data_1
_audit_creation_date 2019-10-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bruker-AXS (2016). APEX3. Version 2016.5-0. Madison, Wisconsin, USA.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
"OLEX2: a complete structure solution, refinement and analysis program".
(2009), J. Appl. Cryst. 42, 339-341.
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015).
J. Appl. Crystallogr. 48, 3-10.
Sheldrick, G.M. (2015a). "SHELXT - Integrated space-group and crystal-structure
determination". Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015b). "Crystal structure refinement with SHELXL".
Acta Cryst. C71, 3-8.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic
;
?
;
_chemical_formula_moiety 'C62 H42 Cd3 N8 O18, 4(H4 O2)'
_chemical_formula_sum 'C62 H58 Cd3 N8 O26'
_chemical_formula_weight 1668.36
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Cd' 'Cd' -0.8075 1.2024
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'triclinic'
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.685(5)
_cell_length_b 10.309(5)
_cell_length_c 16.725(5)
_cell_angle_alpha 92.107(5)
_cell_angle_beta 103.546(5)
_cell_angle_gamma 102.952(5)
_cell_volume 1575.1(12)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 1871
_cell_measurement_temperature 293(2)
_cell_measurement_theta_max 25.127
_cell_measurement_theta_min 1.628
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.098
_exptl_absorpt_correction_T_max 0.803
_exptl_absorpt_correction_T_min 0.768
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour clourless
_exptl_crystal_colour_primary clourless
_exptl_crystal_density_diffrn 1.759
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 838
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.2
_exptl_special_details
;
?
;
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0350
_diffrn_reflns_av_unetI/netI 0.0778
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max 8
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 12
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 20
_diffrn_reflns_limit_l_min -20
_diffrn_reflns_number 10194
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full 25.240
_diffrn_reflns_theta_max 26.454
_diffrn_reflns_theta_min 1.258
_diffrn_ambient_temperature 293(2)
_diffrn_detector 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II Quazar'
_diffrn_measurement_method '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_detector 'Bruker APEX II'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71069
_diffrn_radiation_xray_symbol K-L~3~
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.2
_diffrn_source_type 'Incoatec I\ms'
_diffrn_source_voltage 40.0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4333
_reflns_number_total 6492
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material 'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2015b)'
_computing_structure_solution 'XT (Sheldrick, 2015a)'
_refine_diff_density_max 2.394
_refine_diff_density_min -1.310
_refine_diff_density_rms 0.169
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.033
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 449
_refine_ls_number_reflns 6463
_refine_ls_number_restraints 80
_refine_ls_R_factor_all 0.0922
_refine_ls_R_factor_gt 0.0515
_refine_ls_restrained_S_all 1.090
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0794P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1253
_refine_ls_wR_factor_ref 0.1507
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, {H5WA,H5WB} of O5W, {H4WA,H4WB} of O4W, {H3WA,H3WB} of O3W,
{H2WA,H2WB} of O2W, All N(H) groups
At 1.5 times of:
{H1WA,H1WB} of O1W
2. Restrained distances
H2WA-H5WB
1.98 with sigma of 0.04
3. Rigid bond restraints
O8, C17
with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O7 \\sim O2W \\sim O4 \\sim O3W \\sim O6 \\sim O4W \\sim O1 \\sim O5W \\sim O5
\\sim O3 \\sim O1W \\sim O2 \\sim O8: within 3.8A with sigma of 0.01 and sigma
for terminal atoms of 0.02 within 3.8A
Uanis(O8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01
5.a Riding coordinates:
O2W(H2WA,H2WB), O3W(H3WA,H3WB), O4W(H4WA,H4WB), O5W(H5WA,H5WB)
5.b Rotating group:
O1W(H1WA,H1WB)
5.c Aromatic/amide H refined with riding coordinates:
C9(H9), C28(H28), C22(H22), N3(H3), N2(H2), C21(H21), C15(H15), C4(H4),
C20(H20), C24(H24), C1(H1), C2(H2A), C27(H27), C19(H19), C13(H13), C3(H3A),
C12(H12), C8(H8), C14(H14)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary ?
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cd1 Cd 0.000000 0.500000 0.000000 0.02877(18) Uani 1 2 d S . P . .
C9 C 0.2653(9) -0.0320(8) 0.4252(5) 0.058(2) Uani 1 1 d . . . . .
H9 H 0.366884 -0.011486 0.436675 0.069 Uiso 1 1 calc R U . . .
O7 O -0.1404(6) 0.1604(5) 0.3524(3) 0.0523(14) Uani 1 1 d . . . . .
O2W O 0.2287(7) 0.1199(6) 0.2026(4) 0.0842(18) Uani 1 1 d . U . . .
H2WA H 0.263548 0.057864 0.225554 0.101 Uiso 1 1 d DR U . . .
H2WB H 0.253908 0.128764 0.157374 0.101 Uiso 1 1 d R U . . .
Cd2 Cd -0.52345(5) 0.60390(4) -0.12640(3) 0.02902(16) Uani 1 1 d . . . . .
C28 C -0.7584(7) -0.0547(6) -0.0326(4) 0.0340(15) Uani 1 1 d . . . . .
H28 H -0.794397 -0.139335 -0.017755 0.041 Uiso 1 1 calc R U . . .
O4 O -0.5179(7) 0.3522(5) -0.1516(3) 0.0649(15) Uani 1 1 d . U . . .
O3W O 0.4942(10) 0.0067(8) 0.3004(5) 0.131(2) Uani 1 1 d . U . . .
H3WA H 0.476754 -0.077218 0.288526 0.157 Uiso 1 1 d R U . . .
H3WB H 0.528214 0.045062 0.262616 0.157 Uiso 1 1 d R U . . .
O6 O -0.6468(5) -0.2649(4) -0.0812(3) 0.0391(11) Uani 1 1 d . U . . .
C22 C 0.4102(7) -0.3215(6) 0.6869(4) 0.0342(15) Uani 1 1 d . . . . .
H22 H 0.345556 -0.280269 0.705205 0.041 Uiso 1 1 calc R U . . .
O4W O 0.3463(11) -0.2509(9) 0.2581(6) 0.147(3) Uani 1 1 d . U . . .
H4WA H 0.255844 -0.279036 0.234659 0.176 Uiso 1 1 d R U . . .
H4WB H 0.394214 -0.274996 0.226009 0.176 Uiso 1 1 d R U . . .
O1 O -0.0764(5) 0.6944(4) 0.0175(3) 0.0318(10) Uani 1 1 d . U . . .
O5W O 0.1265(10) -0.1475(8) 0.1632(5) 0.130(2) Uani 1 1 d . U . . .
H5WA H 0.087366 -0.195869 0.117766 0.156 Uiso 1 1 d R U . . .
H5WB H 0.091986 -0.078519 0.160976 0.156 Uiso 1 1 d DR U . . .
C17 C 0.2794(12) -0.2459(10) 0.4822(6) 0.085(3) Uani 1 1 d . U . . .
N1 N -0.0121(6) 0.4624(5) 0.1359(3) 0.0328(12) Uani 1 1 d . . . . .
O5 O -0.5164(6) -0.1371(5) -0.1513(3) 0.0497(13) Uani 1 1 d . U . . .
C5 C -0.0026(7) 0.3235(6) 0.2481(4) 0.0336(15) Uani 1 1 d . . . . .
O3 O -0.6382(6) 0.4295(5) -0.0763(4) 0.0662(15) Uani 1 1 d . U . . .
N3 N 0.3386(7) -0.2312(6) 0.5590(3) 0.0489(17) Uani 1 1 d . . . . .
H3 H 0.325221 -0.163926 0.585571 0.059 Uiso 1 1 calc R U . . .
O1W O 0.2308(5) 0.6362(5) 0.0430(3) 0.0434(12) Uani 1 1 d . U . . .
H1WA H 0.256919 0.669155 0.001477 0.065 Uiso 1 1 d R U . . .
H1WB H 0.291235 0.589252 0.061001 0.065 Uiso 1 1 d R U . . .
C25 C -0.6562(6) 0.1985(6) -0.0779(4) 0.0262(13) Uani 1 1 d . . . . .
N2 N 0.0306(6) 0.2059(6) 0.2793(3) 0.0412(14) Uani 1 1 d . . . . .
H2 H 0.097180 0.177016 0.263062 0.049 Uiso 1 1 calc R U . . .
C21 C 0.5812(7) -0.4462(7) 0.7122(4) 0.0361(16) Uani 1 1 d . . . . .
H21 H 0.636123 -0.493428 0.747911 0.043 Uiso 1 1 calc R U . . .
C15 C -0.1957(9) -0.1304(8) 0.3740(5) 0.054(2) Uani 1 1 d . . . . .
H15 H -0.250766 -0.076478 0.344600 0.064 Uiso 1 1 calc R U . . .
C29 C -0.6603(6) -0.0371(6) -0.0830(4) 0.0259(13) Uani 1 1 d . . . . .
N4 N 0.4859(6) -0.3909(5) 0.7394(3) 0.0297(12) Uani 1 1 d . . . . .
O2 O -0.2853(5) 0.6408(5) -0.0776(3) 0.0510(12) Uani 1 1 d . U . . .
C4 C -0.0438(9) 0.4172(7) 0.2930(5) 0.052(2) Uani 1 1 d . . . . .
H4 H -0.052379 0.403601 0.346467 0.063 Uiso 1 1 calc R U . . .
C20 C 0.6012(8) -0.4364(7) 0.6346(4) 0.0429(17) Uani 1 1 d . . . . .
H20 H 0.667540 -0.477195 0.617842 0.051 Uiso 1 1 calc R U . . .
C26 C -0.7492(7) 0.1814(6) -0.0249(4) 0.0271(13) Uani 1 1 d . . . . .
O8 O 0.3190(13) -0.3163(11) 0.4385(6) 0.186(4) Uani 1 1 d . U . . .
C31 C -0.2025(7) 0.7082(6) -0.0130(4) 0.0294(14) Uani 1 1 d . . . . .
C23 C -0.6020(7) 0.3351(6) -0.1046(4) 0.0346(15) Uani 1 1 d . . . . .
C24 C -0.6127(7) 0.0882(6) -0.1061(3) 0.0266(13) Uani 1 1 d . . . . .
H24 H -0.550260 0.100155 -0.141228 0.032 Uiso 1 1 calc R U . . .
C1 C 0.0125(7) 0.3501(6) 0.1703(4) 0.0331(15) Uani 1 1 d . . . . .
H1 H 0.041020 0.288191 0.139814 0.040 Uiso 1 1 calc R U . . .
C18 C 0.4235(7) -0.3085(7) 0.6080(4) 0.0356(15) Uani 1 1 d . . . . .
C2 C -0.0543(8) 0.5484(7) 0.1804(4) 0.0413(17) Uani 1 1 d . . . . .
H2A H -0.073185 0.625427 0.157535 0.050 Uiso 1 1 calc R U . . .
C27 C -0.8020(7) 0.0544(6) -0.0047(4) 0.0338(15) Uani 1 1 d . . . . .
H27 H -0.868236 0.041566 0.028208 0.041 Uiso 1 1 calc R U . . .
C7 C 0.0399(7) 0.0304(7) 0.3707(4) 0.0360(15) Uani 1 1 d . . . . .
C19 C 0.5217(7) -0.3650(7) 0.5805(4) 0.0383(16) Uani 1 1 d . . . . .
H19 H 0.534408 -0.355795 0.527386 0.046 Uiso 1 1 calc R U . . .
C13 C -0.1900(12) -0.3314(8) 0.4387(6) 0.067(3) Uani 1 1 d . . . . .
H13 H -0.240505 -0.410168 0.454402 0.080 Uiso 1 1 calc R U . . .
C3 C -0.0716(10) 0.5287(8) 0.2589(5) 0.054(2) Uani 1 1 d . . . . .
H3A H -0.101799 0.591062 0.288080 0.065 Uiso 1 1 calc R U . . .
C10 C 0.1918(10) -0.1501(8) 0.4457(4) 0.052(2) Uani 1 1 d . . . . .
C30 C -0.6043(7) -0.1524(6) -0.1078(4) 0.0303(14) Uani 1 1 d . . . . .
C6 C -0.0338(8) 0.1350(7) 0.3326(4) 0.0359(15) Uani 1 1 d . . . . .
C16 C -0.0397(8) -0.0907(7) 0.3920(4) 0.0391(16) Uani 1 1 d . . . . .
C11 C 0.0386(9) -0.1818(7) 0.4316(4) 0.0413(17) Uani 1 1 d . . . . .
C12 C -0.0434(12) -0.3008(8) 0.4547(4) 0.060(2) Uani 1 1 d . . . . .
H12 H 0.006708 -0.359885 0.482048 0.072 Uiso 1 1 calc R U . . .
C8 C 0.1893(9) 0.0574(8) 0.3874(5) 0.052(2) Uani 1 1 d . . . . .
H8 H 0.240660 0.137025 0.373056 0.063 Uiso 1 1 calc R U . . .
C14 C -0.2637(11) -0.2433(9) 0.3984(6) 0.070(3) Uani 1 1 d . . . . .
H14 H -0.365184 -0.263543 0.387910 0.084 Uiso 1 1 calc R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Cd1 0.0383(4) 0.0232(3) 0.0314(4) 0.0055(3) 0.0159(3) 0.0129(3)
C9 0.044(5) 0.052(5) 0.069(6) 0.006(4) -0.008(4) 0.021(4)
O7 0.055(3) 0.062(4) 0.061(3) 0.030(3) 0.032(3) 0.035(3)
O2W 0.110(5) 0.064(4) 0.100(4) 0.009(3) 0.067(4) 0.022(3)
Cd2 0.0381(3) 0.0240(3) 0.0319(3) 0.00667(19) 0.0140(2) 0.0153(2)
C28 0.039(4) 0.019(3) 0.045(4) 0.006(3) 0.014(3) 0.006(3)
O4 0.100(4) 0.040(3) 0.062(3) 0.012(3) 0.041(3) 0.009(3)
O3W 0.162(5) 0.095(5) 0.128(5) 0.005(4) 0.039(4) 0.015(4)
O6 0.048(3) 0.022(2) 0.057(3) 0.008(2) 0.019(2) 0.020(2)
C22 0.044(4) 0.031(4) 0.035(4) 0.008(3) 0.016(3) 0.017(3)
O4W 0.176(6) 0.103(5) 0.151(6) -0.004(5) 0.008(5) 0.050(5)
O1 0.030(2) 0.028(2) 0.041(2) 0.0029(19) 0.007(2) 0.0173(19)
O5W 0.166(5) 0.078(4) 0.126(5) 0.007(4) 0.012(5) 0.011(4)
C17 0.123(9) 0.081(7) 0.049(5) -0.003(5) -0.029(5) 0.072(6)
N1 0.036(3) 0.036(3) 0.031(3) 0.009(2) 0.012(2) 0.012(2)
O5 0.067(3) 0.037(3) 0.061(3) 0.004(2) 0.038(3) 0.022(3)
C5 0.036(4) 0.031(4) 0.039(4) 0.011(3) 0.015(3) 0.012(3)
O3 0.078(4) 0.028(3) 0.115(4) 0.011(3) 0.063(3) 0.018(2)
N3 0.072(4) 0.059(4) 0.035(3) 0.012(3) 0.017(3) 0.048(4)
O1W 0.038(3) 0.044(3) 0.053(3) 0.014(2) 0.013(2) 0.016(2)
C25 0.028(3) 0.022(3) 0.027(3) 0.002(2) 0.002(3) 0.010(3)
N2 0.049(4) 0.050(4) 0.040(3) 0.025(3) 0.022(3) 0.030(3)
C21 0.040(4) 0.041(4) 0.033(4) 0.010(3) 0.008(3) 0.022(3)
C15 0.050(5) 0.058(5) 0.055(5) 0.021(4) 0.015(4) 0.012(4)
C29 0.025(3) 0.022(3) 0.033(3) 0.001(2) 0.005(3) 0.011(3)
N4 0.035(3) 0.031(3) 0.029(3) 0.007(2) 0.011(2) 0.016(2)
O2 0.047(3) 0.044(3) 0.063(3) -0.015(2) 0.005(2) 0.025(2)
C4 0.086(6) 0.049(5) 0.037(4) 0.011(3) 0.030(4) 0.030(4)
C20 0.046(4) 0.050(5) 0.044(4) 0.007(3) 0.019(3) 0.026(4)
C26 0.032(3) 0.023(3) 0.031(3) 0.001(2) 0.005(3) 0.017(3)
O8 0.267(8) 0.171(6) 0.138(7) -0.051(5) -0.020(5) 0.174(6)
C31 0.034(4) 0.023(3) 0.032(3) 0.000(3) 0.008(3) 0.010(3)
C23 0.035(4) 0.026(3) 0.044(4) 0.005(3) 0.006(3) 0.014(3)
C24 0.035(4) 0.027(3) 0.026(3) 0.006(2) 0.018(3) 0.012(3)
C1 0.041(4) 0.036(4) 0.027(3) 0.006(3) 0.010(3) 0.016(3)
C18 0.040(4) 0.038(4) 0.033(4) 0.007(3) 0.008(3) 0.019(3)
C2 0.060(5) 0.027(4) 0.042(4) 0.005(3) 0.016(4) 0.017(3)
C27 0.037(4) 0.028(3) 0.045(4) 0.004(3) 0.022(3) 0.014(3)
C7 0.041(4) 0.040(4) 0.031(3) 0.007(3) 0.010(3) 0.017(3)
C19 0.044(4) 0.046(4) 0.031(4) 0.003(3) 0.015(3) 0.018(3)
C13 0.093(8) 0.036(5) 0.073(6) 0.008(4) 0.037(6) 0.003(5)
C3 0.096(7) 0.043(5) 0.039(4) 0.006(3) 0.032(4) 0.030(4)
C10 0.076(6) 0.052(5) 0.029(4) -0.003(3) -0.005(4) 0.037(5)
C30 0.036(4) 0.025(3) 0.031(3) 0.003(3) 0.005(3) 0.014(3)
C6 0.045(4) 0.040(4) 0.029(3) 0.011(3) 0.010(3) 0.020(3)
C16 0.054(5) 0.038(4) 0.029(4) 0.007(3) 0.011(3) 0.017(3)
C11 0.061(5) 0.038(4) 0.023(3) 0.004(3) 0.004(3) 0.015(4)
C12 0.120(8) 0.035(4) 0.032(4) 0.013(3) 0.021(5) 0.028(5)
C8 0.051(5) 0.040(4) 0.061(5) 0.006(4) 0.003(4) 0.014(4)
C14 0.076(7) 0.063(6) 0.070(6) 0.003(5) 0.031(5) 0.002(5)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cd1 O1 2.318(4) 2_565 ?
Cd1 O1 2.318(4) . ?
Cd1 N1 2.346(5) . ?
Cd1 N1 2.346(5) 2_565 ?
Cd1 O1W 2.291(5) 2_565 ?
Cd1 O1W 2.291(5) . ?
C9 H9 0.9300 . ?
C9 C10 1.365(11) . ?
C9 C8 1.386(10) . ?
O7 C6 1.232(7) . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8500 . ?
Cd2 O4 2.628(5) . ?
Cd2 O6 2.214(4) 1_565 ?
Cd2 O3 2.196(5) . ?
Cd2 N4 2.269(5) 1_464 ?
Cd2 O2 2.198(5) . ?
C28 H28 0.9300 . ?
C28 C29 1.399(8) . ?
C28 C27 1.388(8) . ?
O4 C23 1.249(8) . ?
O3W H3WA 0.8501 . ?
O3W H3WB 0.8501 . ?
O6 C30 1.273(7) . ?
C22 H22 0.9300 . ?
C22 N4 1.342(7) . ?
C22 C18 1.364(8) . ?
O4W H4WA 0.8499 . ?
O4W H4WB 0.8502 . ?
O1 C31 1.251(7) . ?
O5W H5WA 0.8502 . ?
O5W H5WB 0.8499 . ?
C17 N3 1.266(10) . ?
C17 O8 1.194(11) . ?
C17 C10 1.499(10) . ?
N1 C1 1.355(8) . ?
N1 C2 1.327(8) . ?
O5 C30 1.231(7) . ?
C5 N2 1.410(8) . ?
C5 C4 1.384(9) . ?
C5 C1 1.374(8) . ?
O3 C23 1.222(7) . ?
N3 H3 0.8600 . ?
N3 C18 1.417(8) . ?
O1W H1WA 0.8506 . ?
O1W H1WB 0.8504 . ?
C25 C26 1.394(8) . ?
C25 C23 1.511(8) . ?
C25 C24 1.400(8) . ?
N2 H2 0.8600 . ?
N2 C6 1.350(8) . ?
C21 H21 0.9300 . ?
C21 N4 1.342(7) . ?
C21 C20 1.360(9) . ?
C15 H15 0.9300 . ?
C15 C16 1.429(10) . ?
C15 C14 1.332(11) . ?
C29 C24 1.372(8) . ?
C29 C30 1.497(8) . ?
O2 C31 1.257(8) . ?
C4 H4 0.9300 . ?
C4 C3 1.354(10) . ?
C20 H20 0.9300 . ?
C20 C19 1.389(9) . ?
C26 C31 1.496(8) 2_465 ?
C26 C27 1.380(8) . ?
C24 H24 0.9300 . ?
C1 H1 0.9300 . ?
C18 C19 1.375(9) . ?
C2 H2A 0.9300 . ?
C2 C3 1.379(9) . ?
C27 H27 0.9300 . ?
C7 C6 1.504(9) . ?
C7 C16 1.418(9) . ?
C7 C8 1.369(10) . ?
C19 H19 0.9300 . ?
C13 H13 0.9300 . ?
C13 C12 1.342(12) . ?
C13 C14 1.378(12) . ?
C3 H3A 0.9300 . ?
C10 C11 1.405(11) . ?
C16 C11 1.423(9) . ?
C11 C12 1.425(10) . ?
C12 H12 0.9300 . ?
C8 H8 0.9300 . ?
C14 H14 0.9300 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Cd1 O1 180.0 2_565 . ?
O1 Cd1 N1 92.13(16) 2_565 . ?
O1 Cd1 N1 87.87(16) . . ?
O1 Cd1 N1 92.13(16) . 2_565 ?
O1 Cd1 N1 87.87(16) 2_565 2_565 ?
N1 Cd1 N1 180.0 2_565 . ?
O1W Cd1 O1 95.43(16) 2_565 . ?
O1W Cd1 O1 84.57(16) 2_565 2_565 ?
O1W Cd1 O1 95.43(16) . 2_565 ?
O1W Cd1 O1 84.57(16) . . ?
O1W Cd1 N1 92.31(18) 2_565 2_565 ?
O1W Cd1 N1 92.31(18) . . ?
O1W Cd1 N1 87.69(18) . 2_565 ?
O1W Cd1 N1 87.69(18) 2_565 . ?
O1W Cd1 O1W 180.0 2_565 . ?
C10 C9 H9 119.8 . . ?
C10 C9 C8 120.3(8) . . ?
C8 C9 H9 119.8 . . ?
H2WA O2W H2WB 107.7 . . ?
O6 Cd2 O4 142.87(17) 1_565 . ?
O6 Cd2 N4 116.98(17) 1_565 1_464 ?
O3 Cd2 O4 51.93(17) . . ?
O3 Cd2 O6 92.06(17) . 1_565 ?
O3 Cd2 N4 123.9(2) . 1_464 ?
O3 Cd2 O2 111.1(2) . . ?
N4 Cd2 O4 83.37(17) 1_464 . ?
O2 Cd2 O4 85.71(19) . . ?
O2 Cd2 O6 120.27(17) . 1_565 ?
O2 Cd2 N4 94.76(19) . 1_464 ?
C29 C28 H28 120.0 . . ?
C27 C28 H28 120.0 . . ?
C27 C28 C29 119.9(6) . . ?
C23 O4 Cd2 82.9(4) . . ?
H3WA O3W H3WB 107.7 . . ?
C30 O6 Cd2 104.7(4) . 1_545 ?
N4 C22 H22 118.4 . . ?
N4 C22 C18 123.1(6) . . ?
C18 C22 H22 118.4 . . ?
H4WA O4W H4WB 107.7 . . ?
C31 O1 Cd1 124.6(4) . . ?
H5WA O5W H5WB 107.7 . . ?
N3 C17 C10 119.2(8) . . ?
O8 C17 N3 118.8(9) . . ?
O8 C17 C10 120.1(9) . . ?
C1 N1 Cd1 122.6(4) . . ?
C2 N1 Cd1 120.0(4) . . ?
C2 N1 C1 117.2(5) . . ?
C4 C5 N2 123.6(6) . . ?
C1 C5 N2 118.6(6) . . ?
C1 C5 C4 117.8(6) . . ?
C23 O3 Cd2 104.5(4) . . ?
C17 N3 H3 115.0 . . ?
C17 N3 C18 130.0(7) . . ?
C18 N3 H3 115.0 . . ?
Cd1 O1W H1WA 109.2 . . ?
Cd1 O1W H1WB 109.3 . . ?
H1WA O1W H1WB 104.5 . . ?
C26 C25 C23 120.3(5) . . ?
C26 C25 C24 119.6(5) . . ?
C24 C25 C23 120.1(5) . . ?
C5 N2 H2 117.4 . . ?
C6 N2 C5 125.1(5) . . ?
C6 N2 H2 117.4 . . ?
N4 C21 H21 118.6 . . ?
N4 C21 C20 122.9(6) . . ?
C20 C21 H21 118.6 . . ?
C16 C15 H15 119.4 . . ?
C14 C15 H15 119.4 . . ?
C14 C15 C16 121.2(8) . . ?
C28 C29 C30 120.0(5) . . ?
C24 C29 C28 118.8(5) . . ?
C24 C29 C30 121.2(5) . . ?
C22 N4 Cd2 122.4(4) . 1_646 ?
C21 N4 Cd2 120.1(4) . 1_646 ?
C21 N4 C22 117.2(5) . . ?
C31 O2 Cd2 130.5(4) . . ?
C5 C4 H4 120.1 . . ?
C3 C4 C5 119.9(6) . . ?
C3 C4 H4 120.1 . . ?
C21 C20 H20 120.2 . . ?
C21 C20 C19 119.5(6) . . ?
C19 C20 H20 120.2 . . ?
C25 C26 C31 124.9(5) . 2_465 ?
C27 C26 C25 118.8(5) . . ?
C27 C26 C31 116.3(5) . 2_465 ?
O1 C31 O2 122.9(6) . . ?
O1 C31 C26 118.0(5) . 2_465 ?
O2 C31 C26 118.8(6) . 2_465 ?
O4 C23 C25 121.2(6) . . ?
O3 C23 O4 120.7(6) . . ?
O3 C23 C25 118.1(6) . . ?
C25 C24 H24 119.3 . . ?
C29 C24 C25 121.4(5) . . ?
C29 C24 H24 119.3 . . ?
N1 C1 C5 123.1(6) . . ?
N1 C1 H1 118.5 . . ?
C5 C1 H1 118.5 . . ?
C22 C18 N3 117.7(6) . . ?
C22 C18 C19 119.5(6) . . ?
C19 C18 N3 122.8(6) . . ?
N1 C2 H2A 118.5 . . ?
N1 C2 C3 123.0(6) . . ?
C3 C2 H2A 118.5 . . ?
C28 C27 H27 119.3 . . ?
C26 C27 C28 121.4(6) . . ?
C26 C27 H27 119.3 . . ?
C16 C7 C6 122.2(6) . . ?
C8 C7 C6 117.7(6) . . ?
C8 C7 C16 120.0(6) . . ?
C20 C19 H19 121.1 . . ?
C18 C19 C20 117.8(6) . . ?
C18 C19 H19 121.1 . . ?
C12 C13 H13 120.8 . . ?
C12 C13 C14 118.3(8) . . ?
C14 C13 H13 120.8 . . ?
C4 C3 C2 119.0(7) . . ?
C4 C3 H3A 120.5 . . ?
C2 C3 H3A 120.5 . . ?
C9 C10 C17 117.8(8) . . ?
C9 C10 C11 121.1(6) . . ?
C11 C10 C17 121.1(8) . . ?
O6 C30 C29 118.4(5) . . ?
O5 C30 O6 121.3(5) . . ?
O5 C30 C29 120.3(6) . . ?
O7 C6 N2 121.9(6) . . ?
O7 C6 C7 122.4(6) . . ?
N2 C6 C7 115.5(5) . . ?
C7 C16 C15 124.2(6) . . ?
C7 C16 C11 118.8(6) . . ?
C11 C16 C15 117.0(7) . . ?
C10 C11 C16 118.7(7) . . ?
C10 C11 C12 123.6(7) . . ?
C16 C11 C12 117.8(7) . . ?
C13 C12 C11 122.8(7) . . ?
C13 C12 H12 118.6 . . ?
C11 C12 H12 118.6 . . ?
C9 C8 H8 119.5 . . ?
C7 C8 C9 121.0(8) . . ?
C7 C8 H8 119.5 . . ?
C15 C14 C13 122.8(9) . . ?
C15 C14 H14 118.6 . . ?
C13 C14 H14 118.6 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cd1 O1 C31 O2 -25.9(8) . . . . ?
Cd1 O1 C31 C26 159.9(4) . . . 2_465 ?
Cd1 N1 C1 C5 -176.1(5) . . . . ?
Cd1 N1 C2 C3 176.3(6) . . . . ?
C9 C10 C11 C16 2.6(11) . . . . ?
C9 C10 C11 C12 -177.4(7) . . . . ?
Cd2 O4 C23 O3 0.5(7) . . . . ?
Cd2 O4 C23 C25 -176.7(6) . . . . ?
Cd2 O6 C30 O5 2.2(7) 1_545 . . . ?
Cd2 O6 C30 C29 -176.0(4) 1_545 . . . ?
Cd2 O3 C23 O4 -0.6(9) . . . . ?
Cd2 O3 C23 C25 176.6(4) . . . . ?
Cd2 O2 C31 O1 161.8(4) . . . . ?
Cd2 O2 C31 C26 -24.0(9) . . . 2_465 ?
C28 C29 C24 C25 2.3(9) . . . . ?
C28 C29 C30 O6 -0.8(9) . . . . ?
C28 C29 C30 O5 -179.0(6) . . . . ?
C22 C18 C19 C20 1.5(11) . . . . ?
C17 N3 C18 C22 -145.6(10) . . . . ?
C17 N3 C18 C19 37.2(14) . . . . ?
C17 C10 C11 C16 -176.1(7) . . . . ?
C17 C10 C11 C12 3.9(11) . . . . ?
N1 C2 C3 C4 0.3(13) . . . . ?
C5 N2 C6 O7 7.8(11) . . . . ?
C5 N2 C6 C7 -167.8(6) . . . . ?
C5 C4 C3 C2 -1.7(14) . . . . ?
N3 C17 C10 C9 83.9(13) . . . . ?
N3 C17 C10 C11 -97.3(12) . . . . ?
N3 C18 C19 C20 178.7(7) . . . . ?
C25 C26 C27 C28 3.4(10) . . . . ?
N2 C5 C4 C3 178.9(7) . . . . ?
N2 C5 C1 N1 -177.8(6) . . . . ?
C21 C20 C19 C18 -1.0(11) . . . . ?
C15 C16 C11 C10 176.1(6) . . . . ?
C15 C16 C11 C12 -3.9(9) . . . . ?
C29 C28 C27 C26 -0.8(10) . . . . ?
N4 C22 C18 N3 -179.3(6) . . . . ?
N4 C22 C18 C19 -2.0(11) . . . . ?
N4 C21 C20 C19 0.8(11) . . . . ?
C4 C5 N2 C6 33.7(11) . . . . ?
C4 C5 C1 N1 -0.6(10) . . . . ?
C20 C21 N4 Cd2 -174.1(6) . . . 1_646 ?
C20 C21 N4 C22 -1.1(10) . . . . ?
C26 C25 C23 O4 179.5(6) . . . . ?
C26 C25 C23 O3 2.3(9) . . . . ?
C26 C25 C24 C29 0.3(9) . . . . ?
O8 C17 N3 C18 -16.8(19) . . . . ?
O8 C17 C10 C9 -80.2(15) . . . . ?
O8 C17 C10 C11 98.6(14) . . . . ?
C31 C26 C27 C28 -176.4(6) 2_465 . . . ?
C23 C25 C26 C31 -3.1(9) . . . 2_465 ?
C23 C25 C26 C27 177.1(6) . . . . ?
C23 C25 C24 C29 -179.9(6) . . . . ?
C24 C25 C26 C31 176.7(6) . . . 2_465 ?
C24 C25 C26 C27 -3.2(9) . . . . ?
C24 C25 C23 O4 -0.2(10) . . . . ?
C24 C25 C23 O3 -177.4(7) . . . . ?
C24 C29 C30 O6 176.6(6) . . . . ?
C24 C29 C30 O5 -1.6(9) . . . . ?
C1 N1 C2 C3 0.9(11) . . . . ?
C1 C5 N2 C6 -149.2(7) . . . . ?
C1 C5 C4 C3 1.8(12) . . . . ?
C18 C22 N4 Cd2 174.6(5) . . . 1_646 ?
C18 C22 N4 C21 1.7(10) . . . . ?
C2 N1 C1 C5 -0.8(10) . . . . ?
C27 C28 C29 C24 -2.1(9) . . . . ?
C27 C28 C29 C30 175.4(6) . . . . ?
C7 C16 C11 C10 -1.9(10) . . . . ?
C7 C16 C11 C12 178.1(6) . . . . ?
C10 C9 C8 C7 0.8(12) . . . . ?
C10 C17 N3 C18 178.8(8) . . . . ?
C10 C11 C12 C13 -178.1(8) . . . . ?
C30 C29 C24 C25 -175.1(6) . . . . ?
C6 C7 C16 C15 5.2(10) . . . . ?
C6 C7 C16 C11 -177.0(6) . . . . ?
C6 C7 C8 C9 177.7(7) . . . . ?
C16 C15 C14 C13 -3.2(14) . . . . ?
C16 C7 C6 O7 36.7(10) . . . . ?
C16 C7 C6 N2 -147.6(7) . . . . ?
C16 C7 C8 C9 -0.1(11) . . . . ?
C16 C11 C12 C13 1.9(11) . . . . ?
C12 C13 C14 C15 0.9(14) . . . . ?
C8 C9 C10 C17 176.7(8) . . . . ?
C8 C9 C10 C11 -2.1(12) . . . . ?
C8 C7 C6 O7 -141.0(7) . . . . ?
C8 C7 C6 N2 34.6(9) . . . . ?
C8 C7 C16 C15 -177.1(7) . . . . ?
C8 C7 C16 C11 0.7(10) . . . . ?
C14 C15 C16 C7 -177.5(8) . . . . ?
C14 C15 C16 C11 4.7(11) . . . . ?
C14 C13 C12 C11 -0.3(13) . . . . ?
_shelx_res_file
;
TITL 1 in P-1
1.res
created by SHELXL-2018/3 at 10:03:02 on 24-Oct-2019
CELL 0.71069 9.685 10.309 16.725 92.107 103.546 102.952
ZERR 1 0.005 0.005 0.005 0.005 0.005 0.005
LATT 1
SFAC C H Cd N O
UNIT 62 58 3 8 26
DANG 1.98 H2Wa H5Wb
DELU 0.001 0.001 O8 C17
SIMU 0.01 0.02 3.8 $O
ISOR 0.01 0.01 O8
L.S. 20
PLAN 5
CONF
LIST 1
fmap 2
acta
MORE -1
BOND $H
MERG 2
REM
REM
REM
WGHT 0.079400
FVAR 0.13298
CD1 3 0.000000 0.500000 0.000000 10.50000 0.03832 0.02318 =
0.03142 0.00553 0.01586 0.01287
C9 1 0.265294 -0.032017 0.425199 11.00000 0.04427 0.05240 =
0.06903 0.00559 -0.00827 0.02066
AFIX 43
H9 2 0.366884 -0.011486 0.436675 11.00000 -1.20000
AFIX 0
O7 5 -0.140371 0.160447 0.352352 11.00000 0.05474 0.06155 =
0.06146 0.02973 0.03157 0.03459
O2W 5 0.228748 0.119854 0.202644 11.00000 0.11007 0.06409 =
0.10004 0.00904 0.06705 0.02177
AFIX 3
H2WA 2 0.263548 0.057864 0.225554 11.00000 -1.20000
H2WB 2 0.253908 0.128764 0.157374 11.00000 -1.20000
AFIX 0
CD2 3 -0.523445 0.603905 -0.126397 11.00000 0.03806 0.02397 =
0.03194 0.00667 0.01401 0.01532
C28 1 -0.758417 -0.054664 -0.032584 11.00000 0.03941 0.01881 =
0.04507 0.00552 0.01375 0.00564
AFIX 43
H28 2 -0.794397 -0.139335 -0.017755 11.00000 -1.20000
AFIX 0
O4 5 -0.517875 0.352247 -0.151625 11.00000 0.10026 0.03972 =
0.06224 0.01237 0.04138 0.00885
O3W 5 0.494184 0.006702 0.300436 11.00000 0.16221 0.09529 =
0.12845 0.00457 0.03863 0.01468
AFIX 3
H3WA 2 0.476754 -0.077218 0.288526 11.00000 -1.20000
H3WB 2 0.528214 0.045062 0.262616 11.00000 -1.20000
AFIX 0
O6 5 -0.646838 -0.264896 -0.081205 11.00000 0.04789 0.02153 =
0.05723 0.00783 0.01940 0.02017
C22 1 0.410183 -0.321467 0.686923 11.00000 0.04379 0.03128 =
0.03501 0.00757 0.01594 0.01742
AFIX 43
H22 2 0.345556 -0.280269 0.705205 11.00000 -1.20000
AFIX 0
O4W 5 0.346324 -0.250916 0.258079 11.00000 0.17647 0.10286 =
0.15140 -0.00433 0.00813 0.04988
AFIX 3
H4WA 2 0.255844 -0.279036 0.234659 11.00000 -1.20000
H4WB 2 0.394214 -0.274996 0.226009 11.00000 -1.20000
AFIX 0
O1 5 -0.076421 0.694376 0.017455 11.00000 0.02991 0.02825 =
0.04146 0.00291 0.00741 0.01734
O5W 5 0.126546 -0.147529 0.163236 11.00000 0.16624 0.07765 =
0.12553 0.00695 0.01195 0.01147
AFIX 3
H5WA 2 0.087366 -0.195869 0.117766 11.00000 -1.20000
H5WB 2 0.091986 -0.078519 0.160976 11.00000 -1.20000
AFIX 0
C17 1 0.279390 -0.245948 0.482232 11.00000 0.12267 0.08124 =
0.04908 -0.00311 -0.02934 0.07189
N1 4 -0.012087 0.462442 0.135950 11.00000 0.03552 0.03616 =
0.03088 0.00870 0.01202 0.01231
O5 5 -0.516401 -0.137132 -0.151286 11.00000 0.06675 0.03693 =
0.06106 0.00418 0.03790 0.02153
C5 1 -0.002619 0.323486 0.248105 11.00000 0.03576 0.03121 =
0.03914 0.01100 0.01543 0.01150
O3 5 -0.638226 0.429520 -0.076294 11.00000 0.07791 0.02839 =
0.11514 0.01128 0.06327 0.01772
N3 4 0.338603 -0.231227 0.559045 11.00000 0.07158 0.05905 =
0.03471 0.01238 0.01691 0.04848
AFIX 43
H3 2 0.325221 -0.163926 0.585571 11.00000 -1.20000
AFIX 0
O1W 5 0.230756 0.636211 0.043017 11.00000 0.03813 0.04380 =
0.05283 0.01362 0.01291 0.01606
AFIX 7
H1WA 2 0.256919 0.669155 0.001477 11.00000 -1.50000
H1WB 2 0.291235 0.589252 0.061001 11.00000 -1.50000
AFIX 0
C25 1 -0.656219 0.198474 -0.077904 11.00000 0.02841 0.02220 =
0.02740 0.00218 0.00196 0.00987
N2 4 0.030625 0.205877 0.279285 11.00000 0.04926 0.05011 =
0.04010 0.02472 0.02204 0.02952
AFIX 43
H2 2 0.097180 0.177016 0.263062 11.00000 -1.20000
AFIX 0
C21 1 0.581249 -0.446244 0.712166 11.00000 0.04040 0.04118 =
0.03313 0.01002 0.00844 0.02241
AFIX 43
H21 2 0.636123 -0.493428 0.747911 11.00000 -1.20000
AFIX 0
C15 1 -0.195721 -0.130409 0.373971 11.00000 0.05033 0.05758 =
0.05491 0.02149 0.01516 0.01207
AFIX 43
H15 2 -0.250766 -0.076478 0.344600 11.00000 -1.20000
AFIX 0
C29 1 -0.660273 -0.037064 -0.082992 11.00000 0.02494 0.02174 =
0.03251 0.00079 0.00533 0.01083
N4 4 0.485930 -0.390872 0.739412 11.00000 0.03494 0.03073 =
0.02915 0.00698 0.01078 0.01582
O2 5 -0.285325 0.640765 -0.077565 11.00000 0.04748 0.04354 =
0.06253 -0.01528 0.00460 0.02503
C4 1 -0.043800 0.417201 0.293004 11.00000 0.08564 0.04877 =
0.03665 0.01065 0.02968 0.02958
AFIX 43
H4 2 -0.052379 0.403601 0.346467 11.00000 -1.20000
AFIX 0
C20 1 0.601167 -0.436415 0.634565 11.00000 0.04553 0.05035 =
0.04435 0.00739 0.01912 0.02632
AFIX 43
H20 2 0.667540 -0.477195 0.617842 11.00000 -1.20000
AFIX 0
C26 1 -0.749238 0.181449 -0.024870 11.00000 0.03156 0.02284 =
0.03059 0.00085 0.00538 0.01706
O8 5 0.319026 -0.316254 0.438504 11.00000 0.26655 0.17063 =
0.13816 -0.05069 -0.02000 0.17428
C31 1 -0.202544 0.708218 -0.013026 11.00000 0.03441 0.02331 =
0.03183 0.00039 0.00844 0.00960
C23 1 -0.601971 0.335059 -0.104574 11.00000 0.03510 0.02555 =
0.04442 0.00506 0.00604 0.01365
C24 1 -0.612722 0.088227 -0.106093 11.00000 0.03514 0.02678 =
0.02569 0.00630 0.01755 0.01203
AFIX 43
H24 2 -0.550260 0.100155 -0.141228 11.00000 -1.20000
AFIX 0
C1 1 0.012535 0.350126 0.170313 11.00000 0.04122 0.03554 =
0.02704 0.00565 0.01050 0.01557
AFIX 43
H1 2 0.041020 0.288191 0.139814 11.00000 -1.20000
AFIX 0
C18 1 0.423471 -0.308470 0.608031 11.00000 0.04021 0.03771 =
0.03325 0.00661 0.00790 0.01883
C2 1 -0.054337 0.548392 0.180403 11.00000 0.06016 0.02674 =
0.04190 0.00541 0.01563 0.01696
AFIX 43
H2A 2 -0.073185 0.625427 0.157535 11.00000 -1.20000
AFIX 0
C27 1 -0.802030 0.054399 -0.004729 11.00000 0.03719 0.02812 =
0.04530 0.00420 0.02211 0.01422
AFIX 43
H27 2 -0.868236 0.041566 0.028208 11.00000 -1.20000
AFIX 0
C7 1 0.039871 0.030449 0.370719 11.00000 0.04139 0.03983 =
0.03098 0.00702 0.00972 0.01668
C19 1 0.521656 -0.365028 0.580471 11.00000 0.04384 0.04635 =
0.03109 0.00279 0.01520 0.01771
AFIX 43
H19 2 0.534408 -0.355795 0.527386 11.00000 -1.20000
AFIX 0
C13 1 -0.189964 -0.331448 0.438704 11.00000 0.09337 0.03594 =
0.07335 0.00783 0.03703 0.00295
AFIX 43
H13 2 -0.240505 -0.410168 0.454402 11.00000 -1.20000
AFIX 0
C3 1 -0.071561 0.528688 0.258944 11.00000 0.09565 0.04327 =
0.03900 0.00561 0.03154 0.03050
AFIX 43
H3A 2 -0.101799 0.591062 0.288080 11.00000 -1.20000
AFIX 0
C10 1 0.191767 -0.150054 0.445694 11.00000 0.07611 0.05219 =
0.02850 -0.00277 -0.00450 0.03658
C30 1 -0.604297 -0.152447 -0.107828 11.00000 0.03612 0.02500 =
0.03115 0.00255 0.00460 0.01414
C6 1 -0.033803 0.135049 0.332590 11.00000 0.04462 0.03990 =
0.02876 0.01069 0.00963 0.01974
C16 1 -0.039699 -0.090651 0.392047 11.00000 0.05412 0.03796 =
0.02889 0.00746 0.01119 0.01679
C11 1 0.038628 -0.181779 0.431563 11.00000 0.06130 0.03783 =
0.02282 0.00371 0.00403 0.01471
C12 1 -0.043445 -0.300829 0.454687 11.00000 0.11982 0.03465 =
0.03209 0.01270 0.02063 0.02785
AFIX 43
H12 2 0.006708 -0.359885 0.482048 11.00000 -1.20000
AFIX 0
C8 1 0.189329 0.057437 0.387363 11.00000 0.05050 0.04039 =
0.06131 0.00643 0.00274 0.01407
AFIX 43
H8 2 0.240660 0.137025 0.373056 11.00000 -1.20000
AFIX 0
C14 1 -0.263699 -0.243314 0.398437 11.00000 0.07621 0.06290 =
0.07018 0.00306 0.03098 0.00207
AFIX 43
H14 2 -0.365184 -0.263543 0.387910 11.00000 -1.20000
AFIX 0
HKLF 4
REM 1 in P-1
REM wR2 = 0.1507, GooF = S = 1.033, Restrained GooF = 1.090 for all data
REM R1 = 0.0515 for 4333 Fo > 4sig(Fo) and 0.0922 for all 6463 data
REM 449 parameters refined using 80 restraints
END
WGHT 0.0794 0.0000
REM Highest difference peak 2.394, deepest hole -1.310, 1-sigma level 0.169
Q1 1 0.2187 -0.3789 0.4600 11.00000 0.05 2.39
Q2 1 0.4032 -0.2539 0.4401 11.00000 0.05 1.40
Q3 1 -0.3019 -0.2610 0.3488 11.00000 0.05 0.74
Q4 1 0.3335 -0.2232 0.4876 11.00000 0.05 0.64
Q5 1 0.1810 -0.1311 0.4735 11.00000 0.05 0.63
;
_shelx_res_checksum 95018
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-1 3 -18 8.43 1.64
-2 3 -18 0.61 1.15
-3 3 -18 4.56 1.41
7 2 -18 3.50 1.38
6 2 -18 -0.05 0.99
5 2 -18 9.05 1.67
4 2 -18 0.71 0.98
3 2 -18 13.98 1.96
2 2 -18 2.15 1.23
1 2 -18 25.32 2.45
0 2 -18 4.41 1.33
-1 2 -18 13.05 1.92
-2 2 -18 3.42 1.39
-3 2 -18 5.20 1.56
8 1 -18 8.87 1.64
7 1 -18 1.85 1.19
6 1 -18 -0.29 1.03
5 1 -18 -0.76 0.95
4 1 -18 1.07 1.10
3 1 -18 7.21 1.55
2 1 -18 -0.66 1.05
1 1 -18 6.39 1.48
0 1 -18 2.00 1.29
-1 1 -18 9.18 1.72
-2 1 -18 1.74 1.23
-3 1 -18 7.00 1.66
8 0 -18 5.20 1.42
7 0 -18 1.00 1.12
6 0 -18 5.99 1.44
5 0 -18 -0.94 0.96
4 0 -18 -0.12 0.98
3 0 -18 0.11 1.11
2 0 -18 1.70 1.19
1 0 -18 3.75 1.43
0 0 -18 1.68 1.27
-1 0 -18 8.37 1.71
-2 0 -18 1.19 1.35
-3 0 -18 6.65 1.68
8 -1 -18 12.12 1.78
-8 1 18 9.59 2.45
7 -1 -18 4.02 1.36
-7 1 18 0.10 1.80
6 -1 -18 17.24 2.00
-6 1 18 9.69 2.29
5 -1 -18 1.07 1.12
-5 1 18 -2.25 1.60
4 -1 -18 13.32 1.83
-4 1 18 15.81 2.34
3 -1 -18 2.20 1.28
-3 1 18 0.89 1.55
2 -1 -18 7.51 1.61
1 -1 -18 -0.40 0.96
0 -1 -18 5.17 1.57
-1 -1 -18 -0.54 1.20
-2 -1 -18 0.47 1.33
8 -2 -18 7.60 1.50
-8 2 18 10.57 2.44
7 -2 -18 3.92 1.23
-7 2 18 2.69 2.09
6 -2 -18 10.64 1.69
-6 2 18 7.51 2.16
5 -2 -18 1.03 1.08
-5 2 18 -1.82 1.56
4 -2 -18 28.59 2.53
-4 2 18 30.09 2.89
3 -2 -18 4.33 1.40
-3 2 18 1.77 1.56
2 -2 -18 9.72 1.75
1 -2 -18 1.23 1.09
0 -2 -18 9.80 1.75
-1 -2 -18 1.04 1.21
-2 -2 -18 6.86 1.73
-8 3 18 2.34 2.13
7 -3 -18 0.28 1.01
-7 3 18 -1.47 1.96
6 -3 -18 9.41 1.65
-6 3 18 8.31 2.39
5 -3 -18 1.37 1.12
-5 3 18 -0.34 1.78
4 -3 -18 13.41 1.97
-4 3 18 14.53 2.36
3 -3 -18 1.39 1.21
-3 3 18 -0.08 1.58
2 -3 -18 22.47 2.45
1 -3 -18 2.43 1.22
0 -3 -18 16.55 2.25
-1 -3 -18 1.19 1.40
7 -4 -18 6.61 1.54
-7 4 18 1.49 2.20
6 -4 -18 4.19 1.32
-6 4 18 3.93 2.09
5 -4 -18 1.42 1.11
-5 4 18 -0.85 1.76
4 -4 -18 4.74 1.47
-4 4 18 4.11 2.00
3 -4 -18 1.29 1.29
2 -4 -18 7.28 1.65
1 -4 -18 3.00 1.39
0 -4 -18 1.08 1.40
7 -5 -18 7.65 1.52
6 -5 -18 1.10 1.13
-6 5 18 -1.79 1.89
5 -5 -18 10.70 1.85
-5 5 18 6.97 2.29
4 -5 -18 -0.60 1.14
-4 5 18 -0.44 1.70
3 -5 -18 6.18 1.72
2 -5 -18 0.72 1.32
1 -5 -18 -0.73 1.32
5 -6 -18 26.92 2.68
-5 6 18 23.76 3.23
4 -6 -18 6.87 1.77
-4 6 18 3.54 2.15
3 -6 -18 8.30 1.92
4 5 -19 7.63 1.73
3 5 -19 -1.23 0.99
2 5 -19 1.85 1.37
1 5 -19 1.29 1.31
0 5 -19 11.31 1.93
-1 5 -19 2.06 1.27
5 4 -19 5.21 1.56
4 4 -19 1.80 1.35
3 4 -19 2.24 1.25
2 4 -19 4.07 1.38
1 4 -19 3.39 1.44
0 4 -19 2.73 1.33
-1 4 -19 3.74 1.41
6 3 -19 0.53 1.18
5 3 -19 13.70 1.98
4 3 -19 -0.14 1.05
3 3 -19 10.86 1.92
2 3 -19 2.06 1.37
1 3 -19 5.16 1.58
0 3 -19 1.01 1.14
-1 3 -19 1.52 1.28
-2 3 -19 1.83 1.33
6 2 -19 2.88 1.29
5 2 -19 13.66 1.97
4 2 -19 1.84 1.26
3 2 -19 27.86 2.68
2 2 -19 1.23 1.25
1 2 -19 10.23 1.76
0 2 -19 0.62 1.25
-1 2 -19 9.05 1.78
-2 2 -19 1.69 1.35
7 1 -19 7.46 1.59
6 1 -19 0.10 1.07
5 1 -19 5.19 1.46
4 1 -19 2.04 1.28
3 1 -19 12.29 1.89
2 1 -19 3.88 1.36
1 1 -19 10.39 1.77
0 1 -19 1.34 1.36
-1 1 -19 7.98 1.67
-2 1 -19 2.61 1.42
7 0 -19 1.37 1.19
6 0 -19 0.07 1.18
5 0 -19 6.55 1.48
4 0 -19 1.77 1.25
3 0 -19 2.76 1.29
2 0 -19 -0.90 1.04
1 0 -19 6.90 1.58
0 0 -19 1.72 1.15
-1 0 -19 2.88 1.46
-2 0 -19 0.43 1.22
7 -1 -19 0.23 1.04
6 -1 -19 12.92 1.90
5 -1 -19 -0.93 1.02
4 -1 -19 8.51 1.72
3 -1 -19 -0.35 0.91
2 -1 -19 0.06 0.97
1 -1 -19 1.63 1.19
0 -1 -19 1.38 1.17
-1 -1 -19 1.17 1.37
7 -2 -19 4.38 1.43
-7 2 19 4.15 2.31
6 -2 -19 14.99 1.97
-6 2 19 12.05 2.59
5 -2 -19 3.44 1.27
-5 2 19 2.42 2.03
4 -2 -19 12.19 1.92
-4 2 19 13.77 2.33
3 -2 -19 2.10 1.21
2 -2 -19 3.40 1.50
1 -2 -19 -0.17 1.25
0 -2 -19 8.26 1.91
-1 -2 -19 1.16 1.36
7 -3 -19 0.38 1.18
-7 3 19 -1.30 2.02
6 -3 -19 7.69 1.64
-6 3 19 3.56 2.10
5 -3 -19 2.84 1.27
-5 3 19 2.77 1.90
4 -3 -19 4.99 1.62
-4 3 19 7.72 2.16
3 -3 -19 3.57 1.43
2 -3 -19 13.38 2.07
1 -3 -19 1.86 1.33
0 -3 -19 3.07 1.55
6 -4 -19 5.92 1.55
-6 4 19 9.23 2.55
5 -4 -19 0.70 1.19
-5 4 19 3.53 2.23
4 -4 -19 5.83 1.72
-4 4 19 8.12 2.24
3 -4 -19 2.04 1.37
2 -4 -19 4.07 1.56
1 -4 -19 0.06 1.30
4 -5 -19 2.60 1.42
3 4 -20 0.75 1.22
2 4 -20 6.02 1.67
1 4 -20 -0.74 1.28
4 3 -20 -0.16 1.21
3 3 -20 2.39 1.26
2 3 -20 1.47 1.35
1 3 -20 0.39 1.34
0 3 -20 5.56 1.69
5 2 -20 4.33 1.53
4 2 -20 0.64 1.22
3 2 -20 11.06 1.97
2 2 -20 1.18 1.33
1 2 -20 8.17 1.77
0 2 -20 2.88 1.42
6 1 -20 -0.23 1.20
5 1 -20 10.56 1.92
4 1 -20 1.52 1.34
3 1 -20 19.53 2.37
2 1 -20 0.72 1.35
1 1 -20 9.00 1.83
0 1 -20 0.90 1.28
6 0 -20 0.63 1.26
5 0 -20 12.77 1.95
4 0 -20 0.14 1.17
3 0 -20 2.72 1.41
2 0 -20 0.45 1.27
1 0 -20 7.20 1.87
0 0 -20 1.55 1.46
6 -1 -20 0.91 1.22
5 -1 -20 5.33 1.58
4 -1 -20 -1.70 1.08
3 -1 -20 6.66 1.68
2 -1 -20 2.77 1.31
1 -1 -20 13.04 1.96
0 -1 -20 0.36 1.28
5 -2 -20 3.76 1.43
4 -2 -20 10.16 1.83
3 -2 -20 3.08 1.46
2 -2 -20 0.91 1.33
1 -2 -20 2.14 1.32
5 -3 -20 3.28 1.46
4 -3 -20 10.20 1.88
-4 3 20 12.04 2.50
3 -3 -20 1.70 1.36
2 -3 -20 4.57 1.61
0 0 0 0.00 0.00
;
_shelx_hkl_checksum 32292
_olex2_submission_special_instructions 'No special instructions were received'
################
data_2
_audit_creation_date 2019-10-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bruker-AXS (2016). APEX3. Version 2016.5-0. Madison, Wisconsin, USA.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
"OLEX2: a complete structure solution, refinement and analysis program".
(2009), J. Appl. Cryst. 42, 339-341.
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015).
J. Appl. Crystallogr. 48, 3-10.
Sheldrick, G.M. (2015a). "SHELXT - Integrated space-group and crystal-structure
determination". Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015b). "Crystal structure refinement with SHELXL".
Acta Cryst. C71, 3-8.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C62 H42 N8 O18 Zn3, H4 O2'
_chemical_formula_sum 'C62 H46 N8 O20 Zn3'
_chemical_formula_weight 1419.18
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Zn' 'Zn' 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'triclinic'
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4403(5)
_cell_length_b 10.1765(6)
_cell_length_c 16.5532(9)
_cell_angle_alpha 91.7720(10)
_cell_angle_beta 102.0930(10)
_cell_angle_gamma 101.5010(10)
_cell_volume 1519.35(15)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 1808
_cell_measurement_temperature 296.15
_cell_measurement_theta_max 25.127
_cell_measurement_theta_min 1.628
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 1.259
_exptl_absorpt_correction_T_max 0.777
_exptl_absorpt_correction_T_min 0.747
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour colourless
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.551
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 724
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0332
_diffrn_reflns_av_unetI/netI 0.0824
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -11
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 17
_diffrn_reflns_limit_l_min -22
_diffrn_reflns_number 11345
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 28.355
_diffrn_reflns_theta_min 1.262
_diffrn_ambient_temperature 296.15
_diffrn_detector 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'Bruker APEX II'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II Quazar'
_diffrn_measurement_method '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_detector 'Bruker APEX II'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_xray_symbol K-L~3~
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.2
_diffrn_source_type 'Incoatec I\ms'
_diffrn_source_voltage 40.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4956
_reflns_number_total 7605
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
Structure factors included contributions from the .fab file.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material 'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2015b)'
_computing_structure_solution 'XT (Sheldrick, 2015a)'
_refine_diff_density_max 1.750
_refine_diff_density_min -0.527
_refine_diff_density_rms 0.129
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.014
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 425
_refine_ls_number_reflns 7538
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0943
_refine_ls_R_factor_gt 0.0543
_refine_ls_restrained_S_all 1.014
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0783P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1317
_refine_ls_wR_factor_ref 0.1556
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All O(H,H) groups
2.a Free rotating group:
O2W(H2WA,H2WB)
2.b Rotating group:
O1W(H1WA,H1WB)
2.c Aromatic/amide H refined with riding coordinates:
N2(H2), C6(H6), C10(H10), N3(H3), C8(H8), C5(H5), C31(H31), C12(H12),
C14(H14), C13(H13), C30(H30), C28(H28), C24(H24), C29(H29), C25(H25), C18(H18),
C21(H21), C19(H19), C20(H20)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zn1 Zn 0.000000 1.000000 0.000000 0.02190(16) Uani 1 2 d S . P . .
Zn2 Zn 0.52363(5) 0.89391(4) 0.12414(3) 0.02171(14) Uani 1 1 d . . . . .
O1 O 0.0903(3) 0.8248(3) -0.01257(16) 0.0244(6) Uani 1 1 d . . . . .
O2 O 0.3119(3) 0.8763(3) 0.07253(16) 0.0253(6) Uani 1 1 d . . . . .
O6 O 0.3563(3) 0.2267(3) -0.08647(18) 0.0313(7) Uani 1 1 d . . . . .
O3 O 0.3731(3) 0.9351(3) -0.09180(18) 0.0290(7) Uani 1 1 d . . . . .
O1W O -0.2078(3) 0.8719(3) -0.03462(18) 0.0311(7) Uani 1 1 d . . . . .
H1WA H -0.249399 0.855563 0.008365 0.047 Uiso 1 1 d R U . . .
H1WB H -0.271619 0.910612 -0.067345 0.047 Uiso 1 1 d R U . . .
O4 O 0.5155(4) 0.8385(3) -0.1551(2) 0.0420(8) Uani 1 1 d . . . . .
O5 O 0.5015(4) 0.3624(3) -0.1498(2) 0.0414(8) Uani 1 1 d . . . . .
N1 N 0.5105(4) 0.8930(3) 0.2464(2) 0.0249(7) Uani 1 1 d . . . . .
N4 N 1.0060(4) 0.0347(3) 0.8716(2) 0.0264(7) Uani 1 1 d . . . . .
O8 O 1.1418(4) 0.3420(4) 0.6546(2) 0.0510(10) Uani 1 1 d . . . . .
N2 N 0.6686(5) 0.7460(4) 0.4329(2) 0.0413(10) Uani 1 1 d . . . . .
H2 H 0.714941 0.699315 0.407583 0.050 Uiso 1 1 calc R U . . .
C1 C 0.2203(4) 0.8074(3) 0.0118(2) 0.0199(8) Uani 1 1 d . . . . .
C2 C 0.4208(4) 0.8332(4) -0.1130(2) 0.0235(8) Uani 1 1 d . . . . .
C6 C 0.2432(5) 0.4491(4) -0.0336(3) 0.0278(9) Uani 1 1 d . . . . .
H6 H 0.203487 0.365155 -0.017767 0.033 Uiso 1 1 calc R U . . .
C4 C 0.2601(4) 0.6894(4) -0.0287(2) 0.0210(8) Uani 1 1 d . . . . .
C10 C 0.5925(5) 0.8296(4) 0.3012(2) 0.0267(9) Uani 1 1 d . . . . .
H10 H 0.663665 0.790828 0.284253 0.032 Uiso 1 1 calc R U . . .
C7 C 0.3440(4) 0.4611(4) -0.0845(2) 0.0231(8) Uani 1 1 d . . . . .
C3 C 0.3564(4) 0.7010(4) -0.0830(2) 0.0219(8) Uani 1 1 d . . . . .
N3 N 0.9640(4) 0.2976(4) 0.7281(2) 0.0373(9) Uani 1 1 d . . . . .
H3 H 0.897556 0.329822 0.745793 0.045 Uiso 1 1 calc R U . . .
C23 C 0.9531(5) 0.4708(4) 0.6324(2) 0.0309(10) Uani 1 1 d . . . . .
C8 C 0.3988(5) 0.5857(4) -0.1098(2) 0.0240(8) Uani 1 1 d . . . . .
H8 H 0.464371 0.593034 -0.145046 0.029 Uiso 1 1 calc R U . . .
C22 C 1.0316(5) 0.5934(5) 0.6079(3) 0.0346(10) Uani 1 1 d . . . . .
C5 C 0.2020(5) 0.5638(4) -0.0064(3) 0.0281(9) Uani 1 1 d . . . . .
H5 H 0.133959 0.555681 0.027466 0.034 Uiso 1 1 calc R U . . .
C26 C 1.0308(5) 0.3666(4) 0.6728(3) 0.0336(10) Uani 1 1 d . . . . .
C16 C 0.7895(6) 0.6480(5) 0.5507(3) 0.0368(11) Uani 1 1 d . . . . .
C31 C 0.9853(5) 0.1500(4) 0.8389(3) 0.0289(9) Uani 1 1 d . . . . .
H31 H 0.962703 0.215309 0.871730 0.035 Uiso 1 1 calc R U . . .
C9 C 0.4049(5) 0.3438(4) -0.1090(3) 0.0261(9) Uani 1 1 d . . . . .
C12 C 0.4702(5) 0.8763(4) 0.4075(3) 0.0329(10) Uani 1 1 d . . . . .
H12 H 0.457281 0.871854 0.461626 0.039 Uiso 1 1 calc R U . . .
C14 C 0.4070(5) 0.9467(4) 0.2716(3) 0.0285(9) Uani 1 1 d . . . . .
H14 H 0.347939 0.990461 0.234127 0.034 Uiso 1 1 calc R U . . .
C11 C 0.5767(5) 0.8188(4) 0.3817(2) 0.0298(9) Uani 1 1 d . . . . .
C17 C 0.9465(6) 0.6824(4) 0.5655(3) 0.0368(11) Uani 1 1 d . . . . .
C13 C 0.3852(5) 0.9394(4) 0.3508(3) 0.0331(10) Uani 1 1 d . . . . .
H13 H 0.312105 0.977663 0.366028 0.040 Uiso 1 1 calc R U . . .
C30 C 1.0405(6) -0.0568(5) 0.8238(3) 0.0385(11) Uani 1 1 d . . . . .
H30 H 1.056447 -0.136907 0.845849 0.046 Uiso 1 1 calc R U . . .
C27 C 0.9958(5) 0.1767(4) 0.7587(3) 0.0320(10) Uani 1 1 d . . . . .
C28 C 1.0299(6) 0.0793(5) 0.7095(3) 0.0415(12) Uani 1 1 d . . . . .
H28 H 1.036390 0.093030 0.655048 0.050 Uiso 1 1 calc R U . . .
C24 C 0.8025(5) 0.4426(5) 0.6158(3) 0.0413(11) Uani 1 1 d . . . . .
H24 H 0.753291 0.362508 0.631746 0.050 Uiso 1 1 calc R U . . .
C15 C 0.6929(7) 0.7402(5) 0.5138(3) 0.0492(14) Uani 1 1 d . . . . .
C29 C 1.0537(7) -0.0381(5) 0.7438(3) 0.0488(14) Uani 1 1 d . . . . .
H29 H 1.078526 -0.104424 0.712911 0.059 Uiso 1 1 calc R U . . .
C25 C 0.7194(6) 0.5302(5) 0.5755(3) 0.0474(13) Uani 1 1 d . . . . .
H25 H 0.616497 0.508519 0.565543 0.057 Uiso 1 1 calc R U . . .
O7 O 0.6230(7) 0.7926(6) 0.5572(2) 0.113(2) Uani 1 1 d . . . . .
C18 C 1.0227(7) 0.8035(5) 0.5407(3) 0.0478(13) Uani 1 1 d . . . . .
H18 H 0.968620 0.862116 0.513193 0.057 Uiso 1 1 calc R U . . .
C21 C 1.1884(6) 0.6350(5) 0.6259(3) 0.0509(13) Uani 1 1 d . . . . .
H21 H 1.246239 0.581426 0.656070 0.061 Uiso 1 1 calc R U . . .
C19 C 1.1716(7) 0.8354(6) 0.5562(3) 0.0587(16) Uani 1 1 d . . . . .
H19 H 1.218799 0.914009 0.537507 0.070 Uiso 1 1 calc R U . . .
C20 C 1.2556(7) 0.7523(6) 0.5997(4) 0.0628(16) Uani 1 1 d . . . . .
H20 H 1.358436 0.776886 0.611054 0.075 Uiso 1 1 calc R U . . .
O2W O 0.7710(6) 0.4016(6) 0.8028(4) 0.1023(19) Uani 1 1 d G . . . .
H2WA H 0.678787 0.377284 0.800918 0.154 Uiso 1 1 d G U . . .
H2WB H 0.789582 0.486530 0.812002 0.154 Uiso 1 1 d G U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Zn1 0.0263(4) 0.0186(3) 0.0240(3) 0.0045(2) 0.0083(3) 0.0089(3)
Zn2 0.0256(3) 0.0181(2) 0.0251(3) 0.00519(17) 0.00863(19) 0.00938(18)
O1 0.0241(15) 0.0235(14) 0.0280(15) 0.0014(11) 0.0070(12) 0.0096(12)
O2 0.0260(15) 0.0251(14) 0.0259(14) -0.0020(11) 0.0013(12) 0.0130(12)
O6 0.0361(18) 0.0180(14) 0.0445(18) 0.0041(12) 0.0132(14) 0.0116(13)
O3 0.0349(17) 0.0162(13) 0.0422(17) 0.0081(12) 0.0184(14) 0.0089(12)
O1W 0.0295(17) 0.0303(16) 0.0359(17) 0.0069(13) 0.0092(13) 0.0093(13)
O4 0.055(2) 0.0262(16) 0.057(2) 0.0098(14) 0.0389(18) 0.0095(15)
O5 0.044(2) 0.0275(16) 0.063(2) -0.0029(15) 0.0333(18) 0.0101(14)
N1 0.0315(19) 0.0217(17) 0.0251(17) 0.0037(13) 0.0094(15) 0.0102(15)
N4 0.0289(19) 0.0284(18) 0.0254(18) 0.0052(14) 0.0072(15) 0.0122(15)
O8 0.053(2) 0.063(2) 0.058(2) 0.0296(18) 0.0351(19) 0.0334(19)
N2 0.050(3) 0.058(3) 0.029(2) 0.0133(18) 0.0124(18) 0.036(2)
C1 0.024(2) 0.0150(17) 0.025(2) 0.0074(14) 0.0100(16) 0.0076(15)
C2 0.028(2) 0.0164(18) 0.027(2) 0.0038(15) 0.0061(17) 0.0068(16)
C6 0.035(2) 0.0136(18) 0.040(2) 0.0071(16) 0.016(2) 0.0067(17)
C4 0.022(2) 0.0178(18) 0.024(2) 0.0016(15) 0.0043(16) 0.0072(15)
C10 0.028(2) 0.029(2) 0.027(2) 0.0055(17) 0.0095(18) 0.0126(18)
C7 0.029(2) 0.0139(18) 0.026(2) 0.0000(15) 0.0050(17) 0.0069(16)
C3 0.026(2) 0.0145(17) 0.027(2) 0.0027(15) 0.0078(16) 0.0055(15)
N3 0.044(2) 0.045(2) 0.039(2) 0.0216(17) 0.0241(18) 0.0280(19)
C23 0.039(3) 0.035(2) 0.023(2) 0.0109(17) 0.0062(18) 0.015(2)
C8 0.031(2) 0.0174(18) 0.029(2) 0.0029(15) 0.0131(18) 0.0097(16)
C22 0.038(3) 0.039(3) 0.028(2) 0.0040(19) 0.009(2) 0.009(2)
C5 0.031(2) 0.0181(19) 0.040(2) 0.0048(17) 0.0180(19) 0.0064(17)
C26 0.039(3) 0.038(3) 0.028(2) 0.0108(18) 0.009(2) 0.016(2)
C16 0.049(3) 0.038(3) 0.024(2) 0.0009(18) 0.000(2) 0.018(2)
C31 0.028(2) 0.031(2) 0.032(2) 0.0082(18) 0.0119(18) 0.0110(18)
C9 0.027(2) 0.0187(19) 0.032(2) -0.0025(16) 0.0024(18) 0.0075(17)
C12 0.039(3) 0.037(2) 0.027(2) 0.0039(18) 0.0122(19) 0.012(2)
C14 0.029(2) 0.031(2) 0.030(2) 0.0082(17) 0.0090(18) 0.0136(18)
C11 0.036(2) 0.032(2) 0.024(2) 0.0076(17) 0.0077(18) 0.0121(19)
C17 0.059(3) 0.032(2) 0.023(2) 0.0047(18) 0.012(2) 0.014(2)
C13 0.032(2) 0.037(2) 0.037(2) 0.0060(19) 0.012(2) 0.017(2)
C30 0.058(3) 0.033(2) 0.029(2) 0.0044(19) 0.010(2) 0.020(2)
C27 0.032(2) 0.034(2) 0.034(2) 0.0133(19) 0.0116(19) 0.0103(19)
C28 0.058(3) 0.051(3) 0.021(2) 0.009(2) 0.014(2) 0.020(3)
C24 0.036(3) 0.042(3) 0.044(3) 0.016(2) 0.004(2) 0.006(2)
C15 0.075(4) 0.047(3) 0.030(3) 0.004(2) -0.001(3) 0.038(3)
C29 0.081(4) 0.043(3) 0.031(3) 0.000(2) 0.019(3) 0.028(3)
C25 0.039(3) 0.052(3) 0.050(3) 0.016(2) 0.001(2) 0.014(2)
O7 0.196(6) 0.140(5) 0.040(2) 0.009(3) 0.015(3) 0.135(5)
C18 0.070(4) 0.037(3) 0.037(3) 0.007(2) 0.015(3) 0.008(3)
C21 0.042(3) 0.055(3) 0.060(3) 0.015(3) 0.020(3) 0.009(3)
C19 0.080(5) 0.041(3) 0.057(4) 0.010(3) 0.030(3) 0.002(3)
C20 0.046(4) 0.071(4) 0.071(4) 0.005(3) 0.026(3) -0.001(3)
O2W 0.070(3) 0.141(5) 0.102(4) -0.030(4) 0.062(3) -0.001(3)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Zn1 O1 2.146(2) 2_575 ?
Zn1 O1 2.146(2) . ?
Zn1 O1W 2.083(3) 2_575 ?
Zn1 O1W 2.083(3) . ?
Zn1 N4 2.176(3) 1_464 ?
Zn1 N4 2.176(3) 2_666 ?
Zn2 O2 1.972(3) . ?
Zn2 O6 1.996(3) 2_665 ?
Zn2 O3 1.965(3) 2_675 ?
Zn2 N1 2.054(3) . ?
O1 C1 1.258(4) . ?
O2 C1 1.265(5) . ?
O6 C9 1.285(5) . ?
O3 C2 1.278(4) . ?
O1W H1WA 0.8871 . ?
O1W H1WB 0.8847 . ?
O4 C2 1.237(5) . ?
O5 C9 1.232(5) . ?
N1 C10 1.334(5) . ?
N1 C14 1.341(5) . ?
N4 C31 1.339(5) . ?
N4 C30 1.335(5) . ?
O8 C26 1.218(5) . ?
N2 H2 0.8600 . ?
N2 C11 1.416(5) . ?
N2 C15 1.316(6) . ?
C1 C4 1.506(5) . ?
C2 C3 1.506(5) . ?
C6 H6 0.9300 . ?
C6 C7 1.389(5) . ?
C6 C5 1.393(5) . ?
C4 C3 1.398(5) . ?
C4 C5 1.380(5) . ?
C10 H10 0.9300 . ?
C10 C11 1.377(5) . ?
C7 C8 1.383(5) . ?
C7 C9 1.504(5) . ?
C3 C8 1.402(5) . ?
N3 H3 0.8600 . ?
N3 C26 1.354(5) . ?
N3 C27 1.408(5) . ?
C23 C22 1.434(6) . ?
C23 C26 1.504(5) . ?
C23 C24 1.359(6) . ?
C8 H8 0.9300 . ?
C22 C17 1.432(6) . ?
C22 C21 1.420(7) . ?
C5 H5 0.9300 . ?
C16 C17 1.420(7) . ?
C16 C15 1.493(6) . ?
C16 C25 1.368(7) . ?
C31 H31 0.9300 . ?
C31 C27 1.383(6) . ?
C12 H12 0.9300 . ?
C12 C11 1.391(6) . ?
C12 C13 1.366(6) . ?
C14 H14 0.9300 . ?
C14 C13 1.371(6) . ?
C17 C18 1.416(7) . ?
C13 H13 0.9300 . ?
C30 H30 0.9300 . ?
C30 C29 1.371(6) . ?
C27 C28 1.392(6) . ?
C28 H28 0.9300 . ?
C28 C29 1.376(6) . ?
C24 H24 0.9300 . ?
C24 C25 1.397(6) . ?
C15 O7 1.245(6) . ?
C29 H29 0.9300 . ?
C25 H25 0.9300 . ?
C18 H18 0.9300 . ?
C18 C19 1.345(8) . ?
C21 H21 0.9300 . ?
C21 C20 1.365(7) . ?
C19 H19 0.9300 . ?
C19 C20 1.388(8) . ?
C20 H20 0.9300 . ?
O2W H2WA 0.8502 . ?
O2W H2WB 0.8496 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 Zn1 O1 180.00(6) . 2_575 ?
O1 Zn1 N4 88.92(11) . 1_464 ?
O1 Zn1 N4 91.08(11) 2_575 1_464 ?
O1 Zn1 N4 88.92(11) 2_575 2_666 ?
O1 Zn1 N4 91.08(11) . 2_666 ?
O1W Zn1 O1 93.48(10) . 2_575 ?
O1W Zn1 O1 93.48(10) 2_575 . ?
O1W Zn1 O1 86.52(10) 2_575 2_575 ?
O1W Zn1 O1 86.52(10) . . ?
O1W Zn1 O1W 180.0 . 2_575 ?
O1W Zn1 N4 91.85(12) 2_575 2_666 ?
O1W Zn1 N4 91.85(12) . 1_464 ?
O1W Zn1 N4 88.15(12) . 2_666 ?
O1W Zn1 N4 88.15(12) 2_575 1_464 ?
N4 Zn1 N4 180.00(17) 2_666 1_464 ?
O2 Zn2 O6 121.48(11) . 2_665 ?
O2 Zn2 N1 99.25(12) . . ?
O6 Zn2 N1 116.68(12) 2_665 . ?
O3 Zn2 O2 106.19(12) 2_675 . ?
O3 Zn2 O6 98.56(11) 2_675 2_665 ?
O3 Zn2 N1 115.08(12) 2_675 . ?
C1 O1 Zn1 130.3(2) . . ?
C1 O2 Zn2 136.3(2) . . ?
C9 O6 Zn2 106.0(2) . 2_665 ?
C2 O3 Zn2 113.7(2) . 2_675 ?
Zn1 O1W H1WA 111.7 . . ?
Zn1 O1W H1WB 111.2 . . ?
H1WA O1W H1WB 102.5 . . ?
C10 N1 Zn2 122.4(3) . . ?
C10 N1 C14 117.6(3) . . ?
C14 N1 Zn2 119.7(3) . . ?
C31 N4 Zn1 122.3(3) . 1_646 ?
C30 N4 Zn1 120.2(3) . 1_646 ?
C30 N4 C31 117.4(4) . . ?
C11 N2 H2 115.6 . . ?
C15 N2 H2 115.6 . . ?
C15 N2 C11 128.9(4) . . ?
O1 C1 O2 123.0(3) . . ?
O1 C1 C4 117.1(3) . . ?
O2 C1 C4 119.6(3) . . ?
O3 C2 C3 116.2(3) . . ?
O4 C2 O3 123.9(4) . . ?
O4 C2 C3 119.9(3) . . ?
C7 C6 H6 120.3 . . ?
C7 C6 C5 119.4(3) . . ?
C5 C6 H6 120.3 . . ?
C3 C4 C1 124.0(3) . . ?
C5 C4 C1 116.5(3) . . ?
C5 C4 C3 119.4(3) . . ?
N1 C10 H10 118.4 . . ?
N1 C10 C11 123.2(4) . . ?
C11 C10 H10 118.4 . . ?
C6 C7 C9 122.1(3) . . ?
C8 C7 C6 119.9(3) . . ?
C8 C7 C9 117.9(3) . . ?
C4 C3 C2 123.1(3) . . ?
C4 C3 C8 119.2(3) . . ?
C8 C3 C2 117.6(3) . . ?
C26 N3 H3 117.7 . . ?
C26 N3 C27 124.5(3) . . ?
C27 N3 H3 117.7 . . ?
C22 C23 C26 122.5(4) . . ?
C24 C23 C22 120.0(4) . . ?
C24 C23 C26 117.5(4) . . ?
C7 C8 C3 120.7(4) . . ?
C7 C8 H8 119.7 . . ?
C3 C8 H8 119.7 . . ?
C17 C22 C23 118.0(4) . . ?
C21 C22 C23 124.3(4) . . ?
C21 C22 C17 117.7(4) . . ?
C6 C5 H5 119.4 . . ?
C4 C5 C6 121.3(4) . . ?
C4 C5 H5 119.4 . . ?
O8 C26 N3 122.5(4) . . ?
O8 C26 C23 122.5(4) . . ?
N3 C26 C23 114.9(4) . . ?
C17 C16 C15 122.9(5) . . ?
C25 C16 C17 120.6(4) . . ?
C25 C16 C15 116.3(5) . . ?
N4 C31 H31 118.4 . . ?
N4 C31 C27 123.2(4) . . ?
C27 C31 H31 118.4 . . ?
O6 C9 C7 119.4(4) . . ?
O5 C9 O6 121.4(3) . . ?
O5 C9 C7 119.2(4) . . ?
C11 C12 H12 121.1 . . ?
C13 C12 H12 121.1 . . ?
C13 C12 C11 117.8(4) . . ?
N1 C14 H14 118.9 . . ?
N1 C14 C13 122.2(4) . . ?
C13 C14 H14 118.9 . . ?
C10 C11 N2 117.3(4) . . ?
C10 C11 C12 118.8(4) . . ?
C12 C11 N2 123.9(4) . . ?
C16 C17 C22 119.4(4) . . ?
C18 C17 C22 118.6(5) . . ?
C18 C17 C16 122.1(4) . . ?
C12 C13 C14 120.4(4) . . ?
C12 C13 H13 119.8 . . ?
C14 C13 H13 119.8 . . ?
N4 C30 H30 118.5 . . ?
N4 C30 C29 123.1(4) . . ?
C29 C30 H30 118.5 . . ?
C31 C27 N3 119.2(4) . . ?
C31 C27 C28 118.5(4) . . ?
C28 C27 N3 122.2(4) . . ?
C27 C28 H28 120.9 . . ?
C29 C28 C27 118.1(4) . . ?
C29 C28 H28 120.9 . . ?
C23 C24 H24 119.0 . . ?
C23 C24 C25 122.1(5) . . ?
C25 C24 H24 119.0 . . ?
N2 C15 C16 117.0(4) . . ?
O7 C15 N2 122.3(4) . . ?
O7 C15 C16 119.9(4) . . ?
C30 C29 C28 119.7(4) . . ?
C30 C29 H29 120.2 . . ?
C28 C29 H29 120.2 . . ?
C16 C25 C24 119.9(5) . . ?
C16 C25 H25 120.0 . . ?
C24 C25 H25 120.0 . . ?
C17 C18 H18 119.3 . . ?
C19 C18 C17 121.3(5) . . ?
C19 C18 H18 119.3 . . ?
C22 C21 H21 119.5 . . ?
C20 C21 C22 121.0(5) . . ?
C20 C21 H21 119.5 . . ?
C18 C19 H19 119.6 . . ?
C18 C19 C20 120.7(5) . . ?
C20 C19 H19 119.6 . . ?
C21 C20 C19 120.6(6) . . ?
C21 C20 H20 119.7 . . ?
C19 C20 H20 119.7 . . ?
H2WA O2W H2WB 104.5 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Zn1 O1 C1 O2 25.2(5) . . . . ?
Zn1 O1 C1 C4 -161.3(2) . . . . ?
Zn1 N4 C31 C27 176.7(3) 1_646 . . . ?
Zn1 N4 C30 C29 -176.6(4) 1_646 . . . ?
Zn2 O2 C1 O1 -173.5(3) . . . . ?
Zn2 O2 C1 C4 13.1(5) . . . . ?
Zn2 O6 C9 O5 3.6(5) 2_665 . . . ?
Zn2 O6 C9 C7 -175.7(3) 2_665 . . . ?
Zn2 O3 C2 O4 -4.9(5) 2_675 . . . ?
Zn2 O3 C2 C3 174.4(3) 2_675 . . . ?
Zn2 N1 C10 C11 -174.6(3) . . . . ?
Zn2 N1 C14 C13 174.6(3) . . . . ?
O1 C1 C4 C3 109.5(4) . . . . ?
O1 C1 C4 C5 -73.7(5) . . . . ?
O2 C1 C4 C3 -76.7(5) . . . . ?
O2 C1 C4 C5 100.1(4) . . . . ?
O3 C2 C3 C4 -5.8(6) . . . . ?
O3 C2 C3 C8 175.8(4) . . . . ?
O4 C2 C3 C4 173.5(4) . . . . ?
O4 C2 C3 C8 -5.0(6) . . . . ?
N1 C10 C11 N2 178.6(4) . . . . ?
N1 C10 C11 C12 0.2(7) . . . . ?
N1 C14 C13 C12 0.2(7) . . . . ?
N4 C31 C27 N3 176.4(4) . . . . ?
N4 C31 C27 C28 -0.1(7) . . . . ?
N4 C30 C29 C28 -0.4(8) . . . . ?
C1 C4 C3 C2 -5.6(6) . . . . ?
C1 C4 C3 C8 172.9(4) . . . . ?
C1 C4 C5 C6 -173.6(4) . . . . ?
C2 C3 C8 C7 179.9(4) . . . . ?
C6 C7 C8 C3 1.6(6) . . . . ?
C6 C7 C9 O6 4.2(6) . . . . ?
C6 C7 C9 O5 -175.2(4) . . . . ?
C4 C3 C8 C7 1.3(6) . . . . ?
C10 N1 C14 C13 0.7(6) . . . . ?
C7 C6 C5 C4 -0.4(7) . . . . ?
C3 C4 C5 C6 3.3(6) . . . . ?
N3 C27 C28 C29 -177.5(5) . . . . ?
C23 C22 C17 C16 1.2(6) . . . . ?
C23 C22 C17 C18 -179.7(4) . . . . ?
C23 C22 C21 C20 179.1(5) . . . . ?
C23 C24 C25 C16 0.7(7) . . . . ?
C8 C7 C9 O6 -180.0(4) . . . . ?
C8 C7 C9 O5 0.7(6) . . . . ?
C22 C23 C26 O8 -35.6(7) . . . . ?
C22 C23 C26 N3 147.5(4) . . . . ?
C22 C23 C24 C25 -0.3(7) . . . . ?
C22 C17 C18 C19 0.1(7) . . . . ?
C22 C21 C20 C19 1.4(9) . . . . ?
C5 C6 C7 C8 -2.1(6) . . . . ?
C5 C6 C7 C9 173.7(4) . . . . ?
C5 C4 C3 C2 177.8(4) . . . . ?
C5 C4 C3 C8 -3.8(6) . . . . ?
C26 N3 C27 C31 147.3(5) . . . . ?
C26 N3 C27 C28 -36.3(7) . . . . ?
C26 C23 C22 C17 176.4(4) . . . . ?
C26 C23 C22 C21 -6.2(7) . . . . ?
C26 C23 C24 C25 -177.5(4) . . . . ?
C16 C17 C18 C19 179.2(5) . . . . ?
C31 N4 C30 C29 -0.8(7) . . . . ?
C31 C27 C28 C29 -1.0(7) . . . . ?
C9 C7 C8 C3 -174.4(4) . . . . ?
C14 N1 C10 C11 -0.9(6) . . . . ?
C11 N2 C15 C16 176.5(5) . . . . ?
C11 N2 C15 O7 6.8(10) . . . . ?
C11 C12 C13 C14 -0.9(7) . . . . ?
C17 C22 C21 C20 -3.5(7) . . . . ?
C17 C16 C15 N2 79.6(6) . . . . ?
C17 C16 C15 O7 -110.4(7) . . . . ?
C17 C16 C25 C24 -0.1(7) . . . . ?
C17 C18 C19 C20 -2.3(8) . . . . ?
C13 C12 C11 N2 -177.5(4) . . . . ?
C13 C12 C11 C10 0.8(7) . . . . ?
C30 N4 C31 C27 1.0(6) . . . . ?
C27 N3 C26 O8 -12.3(8) . . . . ?
C27 N3 C26 C23 164.6(4) . . . . ?
C27 C28 C29 C30 1.3(8) . . . . ?
C24 C23 C22 C17 -0.6(6) . . . . ?
C24 C23 C22 C21 176.8(5) . . . . ?
C24 C23 C26 O8 141.5(5) . . . . ?
C24 C23 C26 N3 -35.4(6) . . . . ?
C15 N2 C11 C10 167.5(5) . . . . ?
C15 N2 C11 C12 -14.2(8) . . . . ?
C15 C16 C17 C22 174.4(4) . . . . ?
C15 C16 C17 C18 -4.7(7) . . . . ?
C15 C16 C25 C24 -175.6(4) . . . . ?
C25 C16 C17 C22 -0.8(6) . . . . ?
C25 C16 C17 C18 -179.9(4) . . . . ?
C25 C16 C15 N2 -105.0(6) . . . . ?
C25 C16 C15 O7 65.1(7) . . . . ?
C18 C19 C20 C21 1.6(9) . . . . ?
C21 C22 C17 C16 -176.4(4) . . . . ?
C21 C22 C17 C18 2.7(6) . . . . ?
_smtbx_masks_special_details ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.271 0.360 0.253 74.2 14.9 ?
2 -0.271 0.640 0.747 74.2 15.2 ?
_smtbx_masks_void_probe_radius 1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_file
;
TITL 1_a.res in P-1
1.res
created by SHELXL-2018/3 at 10:12:31 on 24-Oct-2019
REM Old TITL 1 in P-1
REM SHELXT solution in P-1: R1 0.135, Rweak 0.007, Alpha 0.077
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C64 N10 O18 Zn3
CELL 0.71073 9.4403 10.1765 16.5532 91.772 102.093 101.501
ZERR 1 0.0005 0.0006 0.0009 0.001 0.001 0.001
LATT 1
SFAC C H N O Zn
UNIT 62 46 8 20 3
L.S. 10
PLAN 5
TEMP 23
CONF
BOND
list 4
ABIN
fmap 2 53
acta
MORE -1
BOND $H
REM
REM
REM
WGHT 0.078300
FVAR 0.51715
ZN1 5 0.000000 1.000000 0.000000 10.50000 0.02626 0.01864 =
0.02401 0.00451 0.00835 0.00885
ZN2 5 0.523635 0.893914 0.124140 11.00000 0.02564 0.01806 =
0.02509 0.00519 0.00863 0.00938
O1 4 0.090340 0.824803 -0.012574 11.00000 0.02415 0.02348 =
0.02796 0.00140 0.00696 0.00964
O2 4 0.311949 0.876273 0.072528 11.00000 0.02605 0.02510 =
0.02587 -0.00203 0.00133 0.01301
O6 4 0.356267 0.226697 -0.086475 11.00000 0.03611 0.01795 =
0.04447 0.00412 0.01320 0.01161
O3 4 0.373146 0.935125 -0.091801 11.00000 0.03489 0.01623 =
0.04224 0.00813 0.01836 0.00890
O1W 4 -0.207779 0.871922 -0.034625 11.00000 0.02952 0.03030 =
0.03593 0.00685 0.00923 0.00929
AFIX 7
H1WA 2 -0.249399 0.855563 0.008365 11.00000 -1.50000
H1WB 2 -0.271619 0.910612 -0.067345 11.00000 -1.50000
AFIX 0
O4 4 0.515519 0.838453 -0.155069 11.00000 0.05534 0.02620 =
0.05723 0.00978 0.03888 0.00946
O5 4 0.501524 0.362411 -0.149754 11.00000 0.04390 0.02750 =
0.06318 -0.00286 0.03330 0.01009
N1 3 0.510468 0.893049 0.246420 11.00000 0.03153 0.02173 =
0.02508 0.00367 0.00943 0.01016
N4 3 1.005968 0.034718 0.871595 11.00000 0.02885 0.02839 =
0.02543 0.00524 0.00724 0.01222
O8 4 1.141815 0.341962 0.654587 11.00000 0.05311 0.06259 =
0.05823 0.02963 0.03509 0.03337
N2 3 0.668635 0.746049 0.432861 11.00000 0.04963 0.05819 =
0.02868 0.01331 0.01236 0.03553
AFIX 43
H2 2 0.714941 0.699315 0.407583 11.00000 -1.20000
AFIX 0
C1 1 0.220281 0.807425 0.011807 11.00000 0.02387 0.01500 =
0.02485 0.00735 0.01003 0.00757
C2 1 0.420834 0.833158 -0.113035 11.00000 0.02766 0.01644 =
0.02744 0.00385 0.00612 0.00677
C6 1 0.243155 0.449062 -0.033553 11.00000 0.03466 0.01357 =
0.03998 0.00713 0.01642 0.00673
AFIX 43
H6 2 0.203487 0.365155 -0.017767 11.00000 -1.20000
AFIX 0
C4 1 0.260128 0.689400 -0.028657 11.00000 0.02227 0.01779 =
0.02398 0.00165 0.00431 0.00719
C10 1 0.592453 0.829613 0.301238 11.00000 0.02812 0.02938 =
0.02717 0.00555 0.00948 0.01258
AFIX 43
H10 2 0.663665 0.790828 0.284253 11.00000 -1.20000
AFIX 0
C7 1 0.344041 0.461148 -0.084467 11.00000 0.02949 0.01395 =
0.02623 0.00004 0.00499 0.00689
C3 1 0.356358 0.701039 -0.082962 11.00000 0.02613 0.01455 =
0.02666 0.00269 0.00781 0.00552
N3 3 0.964014 0.297578 0.728142 11.00000 0.04390 0.04530 =
0.03858 0.02162 0.02406 0.02796
AFIX 43
H3 2 0.897556 0.329822 0.745793 11.00000 -1.20000
AFIX 0
C23 1 0.953124 0.470835 0.632368 11.00000 0.03862 0.03480 =
0.02256 0.01093 0.00621 0.01453
C8 1 0.398760 0.585705 -0.109817 11.00000 0.03063 0.01742 =
0.02883 0.00287 0.01315 0.00967
AFIX 43
H8 2 0.464371 0.593034 -0.145046 11.00000 -1.20000
AFIX 0
C22 1 1.031605 0.593395 0.607949 11.00000 0.03791 0.03949 =
0.02781 0.00402 0.00932 0.00901
C5 1 0.201964 0.563819 -0.006363 11.00000 0.03122 0.01813 =
0.04009 0.00482 0.01797 0.00636
AFIX 43
H5 2 0.133959 0.555681 0.027466 11.00000 -1.20000
AFIX 0
C26 1 1.030844 0.366597 0.672843 11.00000 0.03916 0.03841 =
0.02789 0.01080 0.00891 0.01633
C16 1 0.789525 0.647952 0.550657 11.00000 0.04859 0.03808 =
0.02359 0.00085 -0.00016 0.01781
C31 1 0.985274 0.150014 0.838900 11.00000 0.02800 0.03103 =
0.03241 0.00821 0.01192 0.01095
AFIX 43
H31 2 0.962703 0.215309 0.871730 11.00000 -1.20000
AFIX 0
C9 1 0.404943 0.343826 -0.109032 11.00000 0.02712 0.01867 =
0.03168 -0.00252 0.00237 0.00755
C12 1 0.470194 0.876279 0.407527 11.00000 0.03886 0.03687 =
0.02678 0.00389 0.01220 0.01168
AFIX 43
H12 2 0.457281 0.871854 0.461626 11.00000 -1.20000
AFIX 0
C14 1 0.406971 0.946748 0.271634 11.00000 0.02927 0.03077 =
0.02997 0.00822 0.00902 0.01358
AFIX 43
H14 2 0.347939 0.990461 0.234127 11.00000 -1.20000
AFIX 0
C11 1 0.576688 0.818820 0.381723 11.00000 0.03575 0.03213 =
0.02442 0.00757 0.00770 0.01212
C17 1 0.946545 0.682374 0.565535 11.00000 0.05892 0.03186 =
0.02289 0.00470 0.01212 0.01358
C13 1 0.385203 0.939411 0.350823 11.00000 0.03188 0.03678 =
0.03736 0.00604 0.01248 0.01714
AFIX 43
H13 2 0.312105 0.977663 0.366028 11.00000 -1.20000
AFIX 0
C30 1 1.040532 -0.056762 0.823832 11.00000 0.05812 0.03331 =
0.02903 0.00438 0.01039 0.02028
AFIX 43
H30 2 1.056447 -0.136907 0.845849 11.00000 -1.20000
AFIX 0
C27 1 0.995827 0.176711 0.758720 11.00000 0.03220 0.03400 =
0.03371 0.01331 0.01156 0.01032
C28 1 1.029883 0.079256 0.709548 11.00000 0.05803 0.05126 =
0.02137 0.00917 0.01370 0.01986
AFIX 43
H28 2 1.036390 0.093030 0.655048 11.00000 -1.20000
AFIX 0
C24 1 0.802546 0.442649 0.615771 11.00000 0.03650 0.04177 =
0.04382 0.01647 0.00436 0.00638
AFIX 43
H24 2 0.753291 0.362508 0.631746 11.00000 -1.20000
AFIX 0
C15 1 0.692901 0.740169 0.513766 11.00000 0.07542 0.04746 =
0.03006 0.00368 -0.00053 0.03805
C29 1 1.053667 -0.038108 0.743847 11.00000 0.08147 0.04293 =
0.03112 0.00019 0.01873 0.02847
AFIX 43
H29 2 1.078526 -0.104424 0.712911 11.00000 -1.20000
AFIX 0
C25 1 0.719407 0.530240 0.575476 11.00000 0.03946 0.05174 =
0.04989 0.01604 0.00089 0.01422
AFIX 43
H25 2 0.616497 0.508519 0.565543 11.00000 -1.20000
AFIX 0
O7 4 0.623044 0.792620 0.557163 11.00000 0.19572 0.13976 =
0.04049 0.00931 0.01475 0.13508
C18 1 1.022678 0.803487 0.540725 11.00000 0.06978 0.03725 =
0.03666 0.00701 0.01460 0.00831
AFIX 43
H18 2 0.968620 0.862116 0.513193 11.00000 -1.20000
AFIX 0
C21 1 1.188426 0.634978 0.625946 11.00000 0.04222 0.05479 =
0.06005 0.01524 0.02028 0.00914
AFIX 43
H21 2 1.246239 0.581426 0.656070 11.00000 -1.20000
AFIX 0
C19 1 1.171566 0.835412 0.556178 11.00000 0.08032 0.04144 =
0.05705 0.01040 0.03049 0.00180
AFIX 43
H19 2 1.218799 0.914009 0.537507 11.00000 -1.20000
AFIX 0
C20 1 1.255553 0.752340 0.599696 11.00000 0.04638 0.07098 =
0.07112 0.00476 0.02600 -0.00137
AFIX 43
H20 2 1.358436 0.776886 0.611054 11.00000 -1.20000
AFIX 6
O2W 4 0.771049 0.401559 0.802824 11.00000 0.07020 0.14136 =
0.10226 -0.02995 0.06210 -0.00121
H2WA 2 0.678787 0.377284 0.800918 11.00000 -1.50000
H2WB 2 0.789582 0.486530 0.812002 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1_a.res in P-1
REM wR2 = 0.1556, GooF = S = 1.014, Restrained GooF = 1.014 for all data
REM R1 = 0.0543 for 4956 Fo > 4sig(Fo) and 0.0943 for all 7538 data
REM 425 parameters refined using 0 restraints
END
WGHT 0.0783 0.0000
REM Highest difference peak 1.750, deepest hole -0.527, 1-sigma level 0.129
Q1 1 0.8933 0.6394 0.8613 11.00000 0.05 1.75
Q2 1 0.7600 0.8756 0.5372 11.00000 0.05 1.27
Q3 1 0.5849 0.7648 0.5417 11.00000 0.05 0.68
Q4 1 0.7790 0.7780 0.5001 11.00000 0.05 0.51
Q5 1 0.7651 0.5649 0.5400 11.00000 0.05 0.49
;
_shelx_res_checksum 729
_shelx_hkl_file
;
1 0 0 255.97 5.90
2 0 0 3633.24 50.09
3 0 0 561.24 14.50
4 0 0 2585.44 43.60
5 0 0 453.45 17.10
6 0 0 621.04 21.80
7 0 0 91.39 11.70
8 0 0 227.68 18.50
9 0 0 -0.30 8.00
10 0 0 77.89 16.10
11 0 0 10.70 13.00
12 0 0 -17.50 13.00
12 -1 0 -1.00 13.00
11 -1 0 65.79 16.50
10 -1 0 63.79 14.30
9 -1 0 63.29 13.30
8 -1 0 16.20 7.90
7 -1 0 190.98 15.40
6 -1 0 57.49 8.70
5 -1 0 22.10 6.30
4 -1 0 108.59 8.50
-4 1 0 123.29 9.20
-3 1 0 864.61 19.20
-2 1 0 2350.16 34.60
1 -1 0 164.28 4.30
-1 1 0 158.28 4.90
0 -1 0 2090.99 28.50
0 1 0 2100.79 28.10
1 1 0 502.05 10.70
2 1 0 9999.00 127.19
3 1 0 1.80 4.10
4 1 0 918.81 23.00
5 1 0 22.50 6.90
6 1 0 888.01 27.70
7 1 0 14.60 7.80
8 1 0 307.07 19.70
9 1 0 11.60 9.70
10 1 0 130.89 18.30
11 1 0 -0.40 12.90
12 -2 0 5.20 13.50
11 -2 0 91.89 16.20
10 -2 0 13.60 9.40
9 -2 0 136.09 16.20
8 -2 0 48.40 10.30
7 -2 0 357.56 17.60
6 -2 0 14.90 5.80
-6 2 0 2.00 5.90
-5 2 0 1075.39 26.50
-4 2 0 11.00 4.30
-3 2 0 106.59 7.80
2 -2 0 261.57 7.90
-2 2 0 261.57 9.00
1 -2 0 224.48 7.30
-1 2 0 208.68 6.90
0 -2 0 39.30 4.50
0 2 0 34.50 3.90
1 2 0 652.03 15.20
2 2 0 1020.00 21.60
3 2 0 107.79 9.30
4 2 0 1892.71 38.10
5 2 0 15.40 7.20
6 2 0 193.48 16.00
7 2 0 46.80 11.00
8 2 0 301.17 23.90
9 2 0 42.10 12.40
10 2 0 123.39 20.00
11 2 0 21.90 13.00
12 -3 0 -4.80 9.80
11 -3 0 32.90 13.90
10 -3 0 51.69 12.30
9 -3 0 188.08 18.40
8 -3 0 14.10 8.20
-7 3 0 382.56 19.20
-6 3 0 185.48 14.10
-5 3 0 1689.63 35.10
4 -3 0 309.47 10.90
-4 3 0 300.17 12.80
3 -3 0 230.68 8.90
-3 3 0 212.48 9.90
2 -3 0 646.84 15.40
-2 3 0 624.24 15.50
1 -3 0 276.47 10.40
-1 3 0 274.67 9.70
0 -3 0 267.87 10.90
0 3 0 265.97 10.20
-1 -3 0 3580.54 55.29
1 3 0 3603.64 54.69
2 3 0 295.57 13.10
3 3 0 809.62 22.30
4 3 0 40.50 7.70
5 3 0 28.00 8.50
6 3 0 335.17 19.90
7 3 0 6.50 8.30
8 3 0 213.48 21.10
9 3 0 76.59 15.00
10 3 0 12.20 13.90
11 3 0 -9.10 14.10
12 -4 0 1.50 12.70
11 -4 0 149.39 18.90
10 -4 0 19.20 9.50
9 -4 0 37.80 11.30
-8 4 0 7.00 7.80
7 -4 0 691.33 21.10
-7 4 0 678.43 25.00
6 -4 0 106.39 9.40
-6 4 0 97.59 11.40
5 -4 0 949.80 22.80
-5 4 0 965.60 25.90
4 -4 0 980.60 22.60
-4 4 0 1000.10 24.70
3 -4 0 4504.25 66.59
-3 4 0 4518.15 67.59
2 -4 0 186.98 9.60
-2 4 0 182.58 9.40
1 -4 0 1217.78 25.90
-1 4 0 1217.18 25.20
0 -4 0 1436.36 29.70
0 4 0 1473.15 29.30
0 4 0 1425.56 20.70
-1 -4 0 858.81 22.60
1 4 0 852.01 22.40
2 4 0 2654.03 48.30
3 4 0 2323.37 46.40
4 4 0 22.60 8.00
5 4 0 21.80 9.50
6 4 0 2.30 7.80
7 4 0 10.90 9.30
8 4 0 20.80 12.50
9 4 0 48.30 15.60
10 4 0 -13.00 10.30
12 -5 0 120.49 20.10
11 -5 0 12.10 10.90
10 -5 0 97.09 15.80
-9 5 0 137.59 17.40
8 -5 0 1.30 6.00
-8 5 0 20.50 9.90
7 -5 0 362.56 16.20
-7 5 0 317.17 19.00
6 -5 0 317.87 14.80
-6 5 0 325.87 16.60
5 -5 0 690.23 20.80
-5 5 0 714.73 23.10
4 -5 0 112.29 9.80
-4 5 0 117.19 10.60
3 -5 0 82.29 8.70
-3 5 0 80.09 8.90
2 -5 0 159.58 10.10
-2 5 0 181.68 10.80
1 -5 0 1063.49 26.30
-1 5 0 1036.90 25.40
0 -5 0 68.19 8.50
0 5 0 61.39 3.60
0 5 0 55.99 7.60
-1 -5 0 1546.15 35.70
1 5 0 1580.64 34.50
2 5 0 6.20 6.30
3 5 0 917.81 28.20
4 5 0 359.06 20.60
5 5 0 1004.50 33.50
6 5 0 16.00 9.50
7 5 0 61.59 13.80
8 5 0 4.70 10.20
9 5 0 44.10 17.00
10 5 0 13.80 15.40
11 -6 0 4.20 9.30
-10 6 0 177.18 20.10
-9 6 0 5.50 9.70
8 -6 0 197.88 15.60
-8 6 0 232.28 19.80
7 -6 0 206.48 14.20
-7 6 0 199.08 17.00
6 -6 0 7.80 6.40
-6 6 0 16.10 8.30
5 -6 0 9.70 5.80
-5 6 0 14.10 7.60
4 -6 0 177.08 12.10
-4 6 0 200.38 13.00
3 -6 0 37.30 7.80
3 -6 0 42.20 2.90
-3 6 0 31.80 7.70
2 -6 0 197.58 12.90
-2 6 0 181.08 11.80
1 -6 0 659.23 22.20
-1 6 0 643.74 21.50
0 -6 0 93.49 11.60
0 6 0 84.19 4.30
0 6 0 73.79 9.50
-1 -6 0 1092.79 31.90
1 6 0 1097.79 30.00
1 6 0 1123.99 21.20
2 6 0 35.30 9.00
3 6 0 106.89 13.40
4 6 0 35.00 10.70
5 6 0 377.86 22.60
6 6 0 8.90 9.90
7 6 0 178.48 22.10
8 6 0 58.09 15.30
9 6 0 33.80 15.30
-11 7 0 27.60 14.10
-10 7 0 175.38 20.20
-9 7 0 -1.30 10.00
-8 7 0 178.08 18.70
7 -7 0 18.10 7.80
-7 7 0 26.40 9.10
6 -7 0 92.19 11.80
-6 7 0 99.09 13.30
5 -7 0 54.19 9.70
-5 7 0 55.89 9.90
4 -7 0 413.86 19.10
-4 7 0 437.46 19.90
3 -7 0 10.60 7.20
-3 7 0 8.80 7.10
2 -7 0 1.50 5.80
-2 7 0 -1.60 6.30
1 -7 0 15.30 7.70
-1 7 0 45.00 9.30
0 -7 0 26.80 9.80
0 7 0 26.60 8.10
1 7 0 263.17 16.80
2 7 0 9.70 4.80
2 7 0 16.80 9.50
3 7 0 199.48 18.80
4 7 0 30.80 12.30
5 7 0 112.59 16.40
6 7 0 9.90 11.20
7 7 0 75.59 16.50
8 7 0 48.50 17.50
9 7 0 69.79 18.90
-11 8 0 16.30 12.20
-10 8 0 117.59 18.30
-9 8 0 19.10 10.30
-8 8 0 38.30 12.10
7 -8 0 31.60 9.80
-7 8 0 12.10 9.90
6 -8 0 590.94 25.10
-6 8 0 610.54 26.50
5 -8 0 440.86 21.60
-5 8 0 416.06 22.00
4 -8 0 700.33 26.40
-4 8 0 632.94 24.90
3 -8 0 496.35 22.90
-3 8 0 463.85 22.00
2 -8 0 299.87 19.70
-2 8 0 304.27 17.60
1 -8 0 422.16 21.80
-1 8 0 407.86 20.90
0 -8 0 18.00 9.20
0 8 0 16.50 9.70
1 8 0 49.30 11.90
2 8 0 40.80 10.70
3 8 0 34.90 10.90
4 8 0 126.29 18.30
5 8 0 8.60 10.50
6 8 0 85.49 16.90
7 8 0 2.20 12.90
8 8 0 3.00 15.20
-10 9 0 23.50 14.10
-9 9 0 2.50 11.10
-8 9 0 48.40 13.30
7 -9 0 99.19 14.50
-7 9 0 107.09 16.00
6 -9 0 595.14 26.90
-6 9 0 581.14 27.30
5 -9 0 130.29 15.60
-5 9 0 141.09 16.70
4 -9 0 445.16 23.90
-4 9 0 495.35 23.40
3 -9 0 243.18 21.00
-3 9 0 191.88 17.40
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8 -2 6 1.0394 0.0369
8 -2 7 -0.7455 0.0115
8 -2 8 -0.6311 -0.0120
8 -2 9 0.6205 -0.0378
8 -2 10 -0.0442 -0.0189
8 -2 11 0.5590 0.0413
8 -2 12 0.3060 0.0191
8 -2 13 -1.2116 -0.0284
8 -1 0 0.3642 -0.0262
8 -1 1 -0.2417 0.0107
8 -1 2 -0.3552 0.0089
8 -1 3 -0.2097 -0.0280
8 -1 4 0.3145 0.0195
8 -1 5 0.0422 0.0327
8 -1 6 -0.5840 -0.0161
8 -1 7 0.3464 -0.0217
8 -1 8 0.2724 -0.0166
8 -1 9 -0.1959 0.0001
8 -1 10 0.6532 0.0380
8 -1 11 -0.3127 0.0234
8 -1 12 -0.8890 -0.0308
8 -1 13 0.4462 -0.0332
8 0 0 -0.8110 0.0059
8 0 1 0.3238 0.0065
8 0 2 0.1998 -0.0154
8 0 3 -0.6035 0.0052
8 0 4 0.1430 0.0077
8 0 5 0.4358 -0.0106
8 0 6 0.0384 -0.0120
8 0 7 -0.0795 0.0133
8 0 8 0.0763 0.0148
8 0 9 -0.1508 -0.0124
8 0 10 -0.2295 0.0203
8 0 11 0.2096 -0.0038
8 0 12 -0.2652 -0.0644
8 0 13 -0.0880 0.0218
8 1 0 0.4001 -0.0024
8 1 1 -0.3813 -0.0190
8 1 2 -0.4404 -0.0130
8 1 3 1.0553 0.0043
8 1 4 0.3691 0.0193
8 1 5 -0.8488 0.0028
8 1 6 0.0034 0.0247
8 1 7 0.3108 -0.0085
8 1 8 -0.6011 -0.0589
8 1 9 0.2895 0.0468
8 1 10 0.5489 0.0049
8 1 11 -0.8841 -0.0899
8 1 12 0.2350 0.0733
8 2 0 0.0554 -0.0181
8 2 1 0.0919 0.0130
8 2 2 0.7844 0.0211
8 2 3 -0.0236 0.0422
8 2 4 -1.1556 -0.0050
8 2 5 0.0721 -0.0199
8 2 6 0.6654 -0.0365
8 2 7 -0.5714 -0.0335
8 2 8 0.3101 0.0599
8 2 9 0.6090 -0.0195
8 2 10 -0.8113 -0.0286
8 2 11 0.0901 0.1311
8 2 12 0.5221 -0.0077
8 3 0 -0.5216 0.0317
8 3 1 0.2389 0.0056
8 3 2 0.3799 0.0321
8 3 3 -1.1728 -0.0482
8 3 4 -0.1528 -0.0580
8 3 5 1.0027 0.0126
8 3 6 -0.1500 0.0208
8 3 7 0.2639 0.0220
8 3 8 0.1777 -0.0082
8 3 9 -1.0116 0.0623
8 3 10 0.0722 0.0483
8 3 11 0.6205 -0.1556
8 4 0 0.3597 -0.0232
8 4 1 0.7487 0.0381
8 4 2 -1.2083 -0.0511
8 4 3 -0.3627 -0.0326
8 4 4 1.3068 0.0545
8 4 5 0.4820 0.0154
8 4 6 -0.3845 -0.0021
8 4 7 -1.0451 0.0175
8 4 8 -0.4730 0.0406
8 4 9 1.1301 -0.0745
8 4 10 0.4247 -0.1367
8 5 0 0.5828 0.0672
8 5 1 -0.9720 -0.0307
8 5 2 -0.2752 -0.0431
8 5 3 1.3014 0.0098
8 5 4 0.3919 0.0354
8 5 5 -1.2127 0.0386
8 5 6 -1.1107 -0.0327
8 5 7 0.9473 -0.0258
8 5 8 1.4814 -0.0393
8 6 0 -0.4537 -0.0262
8 6 1 -0.0641 -0.0537
8 6 2 0.7156 0.0030
8 6 3 -0.0402 0.1176
8 6 4 -0.8014 0.0379
8 6 5 -0.3109 -0.1415
8 6 6 1.0126 -0.0149
8 6 7 0.6403 0.0615
8 7 0 -0.1957 0.0197
8 7 1 -0.0189 -0.0040
8 7 2 0.0304 0.0870
8 7 3 -0.0191 -0.0348
8 7 4 -0.3023 -0.1699
8 8 0 -0.0988 -0.1211
8 8 1 0.5069 -0.0082
9 -11 0 0.0589 -0.1323
9 -11 1 0.1435 -0.0786
9 -10 0 0.7932 0.0232
9 -10 1 0.3531 0.1390
9 -10 2 0.0329 -0.0857
9 -10 3 -1.4289 -0.1613
9 -10 4 -0.4925 0.0877
9 -10 5 0.9637 0.1237
9 -9 0 -0.9634 0.0162
9 -9 1 -0.0120 -0.0067
9 -9 2 -0.7867 -0.0641
9 -9 3 0.0586 0.0488
9 -9 4 1.5118 0.0960
9 -9 5 0.1244 -0.0929
9 -9 6 -0.7924 -0.0505
9 -9 7 -0.1760 0.0897
9 -8 0 0.8910 0.0516
9 -8 1 0.2086 -0.0749
9 -8 2 0.1722 0.0020
9 -8 3 0.3104 0.0612
9 -8 4 -0.5335 -0.0842
9 -8 5 -0.0301 0.0189
9 -8 6 -0.1030 0.0821
9 -8 7 -0.4597 -0.0815
9 -8 8 0.5577 -0.0305
9 -7 0 0.1054 -0.0543
9 -7 1 -0.6870 0.0179
9 -7 2 -0.3812 0.0079
9 -7 3 0.2865 -0.0320
9 -7 4 0.5395 0.0693
9 -7 5 -0.6699 -0.0056
9 -7 6 -0.2363 -0.0906
9 -7 7 0.8475 0.0313
9 -7 8 -0.0845 0.0745
9 -7 9 -0.2531 -0.0040
9 -6 0 -0.6512 -0.0087
9 -6 1 0.5648 -0.0362
9 -6 2 0.2545 0.0304
9 -6 3 -0.3615 0.0418
9 -6 4 -0.1149 -0.0576
9 -6 5 0.3435 -0.0092
9 -6 6 -0.1365 0.0427
9 -6 7 0.0556 0.0110
9 -6 8 0.4379 -0.0051
9 -6 9 -0.7246 -0.0523
9 -6 10 -0.3651 -0.0043
9 -5 0 0.6746 -0.0065
9 -5 1 -0.8808 0.0419
9 -5 2 -0.1674 -0.0040
9 -5 3 0.9632 -0.0138
9 -5 4 -0.1552 0.0355
9 -5 5 -0.6789 -0.0218
9 -5 6 0.6172 -0.0139
9 -5 7 -0.1062 0.0201
9 -5 8 -1.0120 -0.0402
9 -5 9 0.8703 0.0120
9 -5 10 0.6301 0.0492
9 -5 11 -0.6269 -0.0160
9 -4 0 -0.6953 0.0015
9 -4 1 0.4765 -0.0021
9 -4 2 0.2575 0.0364
9 -4 3 -0.2571 0.0079
9 -4 4 -0.1328 -0.0533
9 -4 5 -0.1974 -0.0049
9 -4 6 -0.2508 0.0116
9 -4 7 0.6182 -0.0109
9 -4 8 0.7728 0.0418
9 -4 9 -0.7483 0.0138
9 -4 10 -0.6480 -0.0546
9 -4 11 0.4448 -0.0061
9 -3 0 -0.1624 0.0249
9 -3 1 -0.1312 0.0289
9 -3 2 0.8910 -0.0173
9 -3 3 -0.3945 -0.0469
9 -3 4 -1.0020 -0.0227
9 -3 5 1.1081 0.0199
9 -3 6 0.8711 0.0469
9 -3 7 -1.0434 0.0240
9 -3 8 -0.5504 -0.0347
9 -3 9 0.1919 -0.0445
9 -3 10 0.1049 0.0154
9 -3 11 0.5415 0.0461
9 -2 0 0.9554 -0.0045
9 -2 1 0.6595 -0.0204
9 -2 2 -1.1587 -0.0348
9 -2 3 -0.2714 -0.0139
9 -2 4 1.2451 0.0520
9 -2 5 -0.5292 0.0427
9 -2 6 -0.8592 -0.0200
9 -2 7 0.7474 -0.0296
9 -2 8 -0.2825 -0.0235
9 -2 9 -0.1845 -0.0014
9 -2 10 1.1476 0.0368
9 -2 11 -0.4822 0.0073
9 -1 0 -0.7722 -0.0201
9 -1 1 -0.5892 -0.0054
9 -1 2 0.1402 0.0191
9 -1 3 0.0447 0.0184
9 -1 4 -0.1245 -0.0028
9 -1 5 0.4247 0.0054
9 -1 6 0.1162 -0.0093
9 -1 7 -0.7996 -0.0405
9 -1 8 0.4680 -0.0101
9 -1 9 0.8176 0.0442
9 -1 10 -0.7194 0.0464
9 -1 11 -0.2849 -0.0177
9 0 0 0.1881 0.0138
9 0 1 -0.5260 0.0174
9 0 2 0.2641 -0.0314
9 0 3 1.2692 0.0078
9 0 4 -0.3369 0.0448
9 0 5 -1.0661 -0.0373
9 0 6 0.2739 -0.0454
9 0 7 0.7168 0.0113
9 0 8 -0.2478 0.0494
9 0 9 -0.2186 0.0686
9 0 10 -0.1148 -0.0614
9 0 11 -0.5223 -0.1202
9 1 0 -0.3719 0.0036
9 1 1 1.1216 -0.0150
9 1 2 0.8390 0.0194
9 1 3 -1.5836 0.0143
9 1 4 -0.7815 -0.0375
9 1 5 1.3103 0.0050
9 1 6 0.2797 0.0120
9 1 7 -0.8479 0.0322
9 1 8 0.2724 0.0409
9 1 9 -0.0153 -0.1221
9 1 10 -0.3595 -0.0629
9 2 0 0.1636 0.0233
9 2 1 -0.1157 -0.0080
9 2 2 -0.8697 -0.0009
9 2 3 -0.2694 0.0260
9 2 4 1.1768 0.0198
9 2 5 0.1694 -0.0507
9 2 6 -0.9925 -0.0025
9 2 7 0.3140 0.0141
9 2 8 0.2852 -0.0780
9 2 9 -0.2467 0.0693
9 3 0 0.5980 -0.0158
9 3 1 0.5513 0.0205
9 3 2 -0.8064 0.0251
9 3 3 0.4827 -0.0417
9 3 4 0.4354 -0.0936
9 3 5 -0.8164 0.0248
9 3 6 0.2317 0.0764
9 3 7 0.3291 0.0040
9 3 8 -0.2504 0.0545
9 4 0 0.6479 0.0050
9 4 1 -1.5948 -0.0234
9 4 2 0.0533 -0.0451
9 4 3 0.8035 -0.0472
9 4 4 -0.2858 0.1039
9 4 5 0.0078 0.1169
9 4 6 -0.0456 -0.0703
9 4 7 -0.1228 -0.0635
9 5 0 -1.4740 0.0159
9 5 1 0.0249 0.0094
9 5 2 0.8782 -0.0392
9 5 3 0.1864 0.1176
9 5 4 -0.2436 0.0525
9 5 5 -0.5313 -0.1885
9 6 0 0.0380 -0.0084
9 6 1 0.6839 -0.1169
9 6 2 0.5489 0.1067
9 6 3 -0.4127 0.0269
9 7 0 0.4799 -0.1550
10 -10 0 1.2002 0.0848
10 -9 0 -1.0740 0.0160
10 -9 1 -1.2876 -0.1317
10 -9 2 0.8288 -0.0045
10 -9 3 1.0102 0.1094
10 -9 4 -0.0353 -0.0207
10 -8 0 0.6179 -0.0704
10 -8 1 1.2220 0.0474
10 -8 2 -0.1223 0.0375
10 -8 3 -0.4101 -0.0170
10 -8 4 0.0083 0.0319
10 -8 5 -0.9087 -0.0622
10 -8 6 -0.0078 -0.0451
10 -7 0 -0.2834 0.0012
10 -7 1 -1.0027 -0.0511
10 -7 2 -0.2259 0.0564
10 -7 3 0.3727 0.0189
10 -7 4 0.0064 -0.1206
10 -7 5 0.3025 0.0525
10 -7 6 -0.0774 0.0824
10 -7 7 -0.1394 -0.0546
10 -6 0 -0.2843 -0.0540
10 -6 1 0.3310 0.0718
10 -6 2 0.8595 -0.0126
10 -6 3 0.1929 -0.0491
10 -6 4 -0.9790 0.0950
10 -6 5 -0.5696 -0.0137
10 -6 6 1.3938 -0.0687
10 -6 7 0.3775 0.0545
10 -6 8 -1.6185 -0.0185
10 -5 0 0.5478 0.0377
10 -5 1 0.0873 0.0412
10 -5 2 -0.8093 0.0309
10 -5 3 -0.4716 -0.0060
10 -5 4 0.6425 -0.0743
10 -5 5 1.0495 0.0014
10 -5 6 -0.8155 0.0466
10 -5 7 -1.1522 -0.0236
10 -5 8 0.9963 -0.0092
10 -4 0 -1.3094 0.0761
10 -4 1 -0.1709 -0.0094
10 -4 2 1.6862 -0.0780
10 -4 3 -0.2692 -0.0224
10 -4 4 -0.8947 0.0257
10 -4 5 0.1945 0.0096
10 -4 6 0.0437 0.0205
10 -4 7 0.2178 0.0095
10 -4 8 0.1878 -0.0167
10 -4 9 -0.2773 -0.0078
10 -3 0 1.7085 -0.0405
10 -3 1 1.4269 -0.0252
10 -3 2 -2.3521 0.0003
10 -3 3 -0.3650 -0.0208
10 -3 4 1.7528 0.0268
10 -3 5 -0.6995 0.0584
10 -3 6 -0.3915 -0.0181
10 -3 7 0.8589 -0.0401
10 -3 8 -0.6621 -0.0149
10 -3 9 -0.2572 -0.0002
10 -2 0 -0.4048 -0.0076
10 -2 1 -1.9766 -0.0362
10 -2 2 0.7955 -0.0048
10 -2 3 1.0312 0.0575
10 -2 4 -1.0709 0.0262
10 -2 5 0.3117 -0.0267
10 -2 6 0.6506 -0.0293
10 -2 7 -1.1503 -0.0295
10 -2 8 0.2253 0.0185
10 -2 9 0.8113 0.0616
10 -1 0 -0.9965 0.0010
10 -1 1 -0.0008 0.0499
10 -1 2 0.9166 -0.0045
10 -1 3 0.1764 -0.0166
10 -1 4 -0.3365 0.0268
10 -1 5 -0.1630 -0.0151
10 -1 6 -0.2223 -0.0484
10 -1 7 0.2618 0.0114
10 -1 8 0.2545 0.0548
10 -1 9 0.0326 0.0117
10 0 0 -0.1159 0.0114
10 0 1 2.3785 -0.0627
10 0 2 0.0073 0.0229
10 0 3 -2.0338 0.0668
10 0 4 0.4685 -0.0281
10 0 5 0.9519 -0.0751
10 0 6 -0.7021 -0.0186
10 0 7 0.0390 0.1001
10 0 8 0.7725 0.0610
10 1 0 2.0241 0.0076
10 1 1 -1.2980 0.0522
10 1 2 -1.8713 0.0041
10 1 3 1.2598 -0.0326
10 1 4 0.8068 -0.0616
10 1 5 -1.1627 -0.0126
10 1 6 0.2451 0.1572
10 1 7 0.8443 0.0212
10 1 8 -1.0016 -0.1947
10 2 0 -0.8806 0.0032
10 2 1 -0.6356 -0.0553
10 2 2 0.4293 0.0212
10 2 3 0.5667 -0.0094
10 2 4 -0.3139 -0.0187
10 2 5 0.1336 0.1126
10 2 6 0.3618 -0.0455
10 2 7 -0.7354 -0.1542
10 3 0 -0.3426 -0.0500
10 3 1 -0.4848 0.0312
10 3 2 1.1172 0.0030
10 3 3 0.3463 -0.0676
10 3 4 -0.6139 0.0497
10 3 5 -0.2526 0.0043
10 4 0 -0.2621 -0.0114
10 4 1 1.0400 0.0257
10 4 2 -0.1664 -0.0714
10 4 3 -0.9350 0.0780
10 4 4 -0.1150 0.0785
10 5 0 -0.0474 0.0730
10 5 1 -0.5398 -0.0668
11 -8 0 0.6169 -0.0300
11 -8 1 0.3503 -0.0521
11 -7 0 -0.6210 -0.0360
11 -7 1 -0.8094 0.1905
11 -7 2 -0.2899 -0.0696
11 -7 3 0.1054 -0.1862
11 -6 0 -0.2106 0.1041
11 -6 1 1.2279 -0.0487
11 -6 2 0.5727 -0.0620
11 -6 3 -0.5214 0.1050
11 -6 4 -0.2134 0.0073
11 -6 5 0.7902 -0.0933
11 -5 0 0.7305 0.0652
11 -5 1 -0.2394 -0.0189
11 -5 2 -0.5693 -0.0300
11 -5 3 -0.7076 -0.0004
11 -5 4 0.6981 -0.0483
11 -5 5 0.3361 0.0018
11 -4 0 0.0409 -0.0612
11 -4 1 -0.2081 -0.0627
11 -4 2 -1.0727 0.0270
11 -4 3 1.5573 -0.0315
11 -4 4 0.8099 0.0391
11 -4 5 -1.8183 0.1031
11 -4 6 -0.1175 -0.0814
11 -3 0 -0.2819 -0.0089
11 -3 1 -0.4553 0.0013
11 -3 2 1.6210 -0.0286
11 -3 3 -0.5282 0.0614
11 -3 4 -1.9228 0.0477
11 -3 5 1.3253 -0.0848
11 -3 6 1.2033 -0.0386
11 -2 0 -0.2372 -0.0420
11 -2 1 -0.1198 -0.0043
11 -2 2 -0.4454 0.0474
11 -2 3 0.0518 0.0267
11 -2 4 1.1032 -0.0269
11 -2 5 -0.2470 -0.0400
11 -2 6 -1.1730 -0.0038
11 -1 0 -0.6903 0.0274
11 -1 1 2.0373 0.0363
11 -1 2 0.2646 0.0323
11 -1 3 -1.3015 -0.0253
11 -1 4 -0.0395 -0.0593
11 -1 5 0.3146 -0.0028
11 -1 6 0.1005 0.0501
11 0 0 2.9285 0.0493
11 0 1 -1.7976 -0.0219
11 0 2 -2.0859 -0.0656
11 0 3 1.7314 0.0242
11 0 4 0.8316 0.0175
11 0 5 -1.0305 -0.0235
11 1 0 -2.2501 -0.0993
11 1 1 -0.7397 -0.0316
11 1 2 2.0350 0.1364
11 1 3 0.2517 -0.0501
11 1 4 -1.4738 -0.1179
11 2 0 -0.2301 0.0320
11 2 1 0.7167 0.1022
11 2 2 0.0908 -0.1172
11 2 3 -0.9933 -0.0884
11 3 0 0.1250 -0.0158
11 3 1 0.5232 -0.0449
12 -5 0 1.6849 -0.1812
12 -5 1 -0.1746 -0.0820
12 -4 0 -2.1514 0.0019
12 -4 1 -1.1485 0.1008
12 -3 0 0.9346 0.0133
12 -3 1 1.6877 -0.0244
12 -3 2 -0.6919 0.0237
12 -2 0 0.0829 -0.0278
12 -2 1 -0.3467 0.0134
12 -2 2 -0.4100 0.0481
12 -1 0 0.7557 0.0848
12 -1 1 -0.8703 0.0680
12 0 0 -1.2635 -0.0624
0 0 0 0.0 0.0
;
_shelx_fab_checksum 54232
_olex2_submission_special_instructions 'No special instructions were received'
################
data_3
_audit_creation_date 2019-10-24
_audit_creation_method
;
Olex2 1.3-alpha
(compiled 2019.10.11 svn.r3662 for OlexSys, GUI svn.r5962)
;
_shelx_SHELXL_version_number '2018/3'
_audit_contact_author_address ?
_audit_contact_author_email ?
_audit_contact_author_name ''
_audit_contact_author_phone ?
_publ_contact_author_id_orcid ?
_publ_section_references
;
Bruker-AXS (2016). APEX3. Version 2016.5-0. Madison, Wisconsin, USA.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
"OLEX2: a complete structure solution, refinement and analysis program".
(2009), J. Appl. Cryst. 42, 339-341.
Krause, L., Herbst-Irmer, R., Sheldrick, G. M. & Stalke, D. (2015).
J. Appl. Crystallogr. 48, 3-10.
Sheldrick, G.M. (2015a). "SHELXT - Integrated space-group and crystal-structure
determination". Acta Cryst. A71, 3-8.
Sheldrick, G.M. (2015b). "Crystal structure refinement with SHELXL".
Acta Cryst. C71, 3-8.
Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H.
(2009), J. Appl. Cryst. 42, 339-341.
Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C62 H42 Co3 N8 O18, 2(H4 O2)'
_chemical_formula_sum 'C62 H50 Co3 N8 O22'
_chemical_formula_weight 1435.89
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'Co' 'Co' 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system 'triclinic'
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.4573(6)
_cell_length_b 10.1544(6)
_cell_length_c 16.5808(10)
_cell_angle_alpha 92.219(2)
_cell_angle_beta 101.8620(10)
_cell_angle_gamma 101.0430(10)
_cell_volume 1524.39(16)
_cell_formula_units_Z 1
_cell_measurement_reflns_used 1496
_cell_measurement_temperature 296.15
_cell_measurement_theta_max 25.127
_cell_measurement_theta_min 1.628
_shelx_estimated_absorpt_T_max ?
_shelx_estimated_absorpt_T_min ?
_exptl_absorpt_coefficient_mu 0.895
_exptl_absorpt_correction_T_max 0.836
_exptl_absorpt_correction_T_min 0.807
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Krause et al., 2015) was used for absorption correction.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour pink
_exptl_crystal_colour_primary pink
_exptl_crystal_density_diffrn 1.564
_exptl_crystal_density_meas ?
_exptl_crystal_density_method 'not measured'
_exptl_crystal_description block
_exptl_crystal_F_000 735
_exptl_crystal_size_max 0.24
_exptl_crystal_size_mid 0.22
_exptl_crystal_size_min 0.2
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0336
_diffrn_reflns_av_unetI/netI 0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max 11
_diffrn_reflns_limit_h_min -10
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min -12
_diffrn_reflns_limit_l_max 19
_diffrn_reflns_limit_l_min -19
_diffrn_reflns_number 8875
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full 25.135
_diffrn_reflns_theta_max 25.135
_diffrn_reflns_theta_min 2.050
_diffrn_ambient_temperature 296.15
_diffrn_detector 'charge-coupled device (CCD) area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type 'Bruker APEX II'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device 'three-circle diffractometer'
_diffrn_measurement_device_type 'Bruker APEX II Quazar'
_diffrn_measurement_method '0.5\% \w and 0.5\% \f scans'
_diffrn_radiation_collimation 'focusing mirrors'
_diffrn_radiation_detector 'Bruker APEX II'
_diffrn_radiation_monochromator 'mirror optics'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type 'Mo K\a'
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_xray_symbol K-L~3~
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_current 30.0
_diffrn_source_power 1.2
_diffrn_source_type 'Incoatec I\ms'
_diffrn_source_voltage 40.0
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 3981
_reflns_number_total 5445
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing_cell_refinement 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_collection 'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction 'SAINT+ Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_molecular_graphics 'OLEX2 (Dolomanov et al., 2009)'
_computing_publication_material 'OLEX2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'XL (Sheldrick, 2015b)'
_computing_structure_solution 'XT (Sheldrick, 2015a)'
_refine_diff_density_max 2.431
_refine_diff_density_min -0.568
_refine_diff_density_rms 0.106
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.032
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 437
_refine_ls_number_reflns 5431
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0886
_refine_ls_R_factor_gt 0.0612
_refine_ls_restrained_S_all 1.032
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0940P)^2^+3.3262P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1645
_refine_ls_wR_factor_ref 0.1838
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups, All N(H) groups
At 1.5 times of:
All O(H,H) groups
2.a Free rotating group:
O3W(H3WA,H3WB), O2W(H2WA,H2WB)
2.b Rotating group:
O1W(H1WA,H1WB)
2.c Aromatic/amide H refined with riding coordinates:
C7(H7), C5(H5), N2(H2), N3(H3), C8(H8), C31(H31), C14(H14), C10(H10),
C30(H30), C12(H12), C11(H11), C28(H28), C18(H18), C17(H17), C29(H29), C24(H24),
C21(H21), C23(H23), C22(H22)
;
_atom_sites_solution_hydrogens mixed
_atom_sites_solution_primary dual
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.000000 1.000000 0.000000 0.0197(3) Uani 1 2 d S . P . .
Co2 Co 0.52312(7) 0.89455(6) 0.12376(4) 0.0210(2) Uani 1 1 d . . . . .
O2 O 0.0918(4) 0.8286(3) -0.0134(2) 0.0234(8) Uani 1 1 d . . . . .
O1 O 0.3119(4) 0.8767(3) 0.0724(2) 0.0258(8) Uani 1 1 d . . . . .
O6 O 0.3484(4) 0.2214(3) -0.0867(2) 0.0291(9) Uani 1 1 d . . . . .
O3 O 0.3754(4) 0.9340(3) -0.0917(2) 0.0293(9) Uani 1 1 d . . . . .
O4 O 0.5202(5) 0.8359(4) -0.1526(3) 0.0388(10) Uani 1 1 d . . . . .
O5 O 0.5054(4) 0.3523(4) -0.1428(3) 0.0392(10) Uani 1 1 d . . . . .
N4 N 1.0033(5) 0.0346(4) 0.8707(3) 0.0269(10) Uani 1 1 d . . . . .
N1 N 0.5113(5) 0.8948(4) 0.2470(3) 0.0251(10) Uani 1 1 d . . . . .
O8 O 1.1428(5) 0.3429(5) 0.6559(3) 0.0527(13) Uani 1 1 d . . . . .
C3 C 0.2599(5) 0.6898(5) -0.0290(3) 0.0211(11) Uani 1 1 d . . . . .
C7 C 0.2405(6) 0.4489(5) -0.0338(3) 0.0276(12) Uani 1 1 d . . . . .
H7 H 0.199109 0.365618 -0.018357 0.033 Uiso 1 1 calc R U . . .
C1 C 0.2200(5) 0.8097(5) 0.0112(3) 0.0200(11) Uani 1 1 d . . . . .
C2 C 0.4234(6) 0.8315(5) -0.1113(3) 0.0250(11) Uani 1 1 d . . . . .
C5 C 0.3999(6) 0.5833(5) -0.1079(3) 0.0230(11) Uani 1 1 d . . . . .
H5 H 0.467155 0.589640 -0.142013 0.028 Uiso 1 1 calc R U . . .
C4 C 0.3587(5) 0.6996(5) -0.0822(3) 0.0214(11) Uani 1 1 d . . . . .
N2 N 0.6683(6) 0.7454(5) 0.4321(3) 0.0410(13) Uani 1 1 d . . . . .
H2 H 0.716861 0.700502 0.406797 0.049 Uiso 1 1 calc R U . . .
C6 C 0.3432(5) 0.4572(5) -0.0838(3) 0.0228(11) Uani 1 1 d . . . . .
N3 N 0.9625(6) 0.2989(5) 0.7281(3) 0.0389(12) Uani 1 1 d . . . . .
H3 H 0.895338 0.331077 0.745361 0.047 Uiso 1 1 calc R U . . .
C9 C 0.4032(5) 0.3389(5) -0.1064(3) 0.0234(11) Uani 1 1 d . . . . .
C8 C 0.1997(6) 0.5645(5) -0.0071(3) 0.0250(11) Uani 1 1 d . . . . .
H8 H 0.130826 0.557696 0.026058 0.030 Uiso 1 1 calc R U . . .
C31 C 0.9834(6) 0.1511(5) 0.8385(3) 0.0275(12) Uani 1 1 d . . . . .
H31 H 0.960500 0.216725 0.871447 0.033 Uiso 1 1 calc R U . . .
C14 C 0.5935(6) 0.8305(5) 0.3011(3) 0.0288(12) Uani 1 1 d . . . . .
H14 H 0.664694 0.791516 0.283809 0.035 Uiso 1 1 calc R U . . .
C26 C 1.0299(6) 0.3679(6) 0.6731(3) 0.0330(13) Uani 1 1 d . . . . .
C10 C 0.4072(6) 0.9479(5) 0.2720(3) 0.0295(12) Uani 1 1 d . . . . .
H10 H 0.347338 0.990425 0.234427 0.035 Uiso 1 1 calc R U . . .
C20 C 1.0297(7) 0.5940(6) 0.6086(3) 0.0368(14) Uani 1 1 d . . . . .
C19 C 0.9526(7) 0.4703(6) 0.6330(3) 0.0319(13) Uani 1 1 d . . . . .
C13 C 0.5771(6) 0.8197(6) 0.3819(3) 0.0291(12) Uani 1 1 d . . . . .
C16 C 0.7864(7) 0.6451(6) 0.5492(3) 0.0381(15) Uani 1 1 d . . . . .
C30 C 1.0376(7) -0.0576(6) 0.8228(4) 0.0389(15) Uani 1 1 d . . . . .
H30 H 1.052567 -0.138272 0.844384 0.047 Uiso 1 1 calc R U . . .
C27 C 0.9956(6) 0.1775(6) 0.7588(3) 0.0314(13) Uani 1 1 d . . . . .
C12 C 0.4703(7) 0.8765(6) 0.4074(4) 0.0349(14) Uani 1 1 d . . . . .
H12 H 0.455974 0.870956 0.461058 0.042 Uiso 1 1 calc R U . . .
C25 C 0.9438(8) 0.6828(6) 0.5648(3) 0.0378(15) Uani 1 1 d . . . . .
C11 C 0.3857(7) 0.9417(6) 0.3509(4) 0.0355(14) Uani 1 1 d . . . . .
H11 H 0.313689 0.981576 0.366484 0.043 Uiso 1 1 calc R U . . .
C28 C 1.0286(8) 0.0794(7) 0.7092(4) 0.0442(16) Uani 1 1 d . . . . .
H28 H 1.034918 0.093308 0.654873 0.053 Uiso 1 1 calc R U . . .
O7 O 0.6130(9) 0.7850(7) 0.5549(3) 0.105(3) Uani 1 1 d . . . . .
C18 C 0.8023(7) 0.4413(6) 0.6145(4) 0.0420(15) Uani 1 1 d . . . . .
H18 H 0.753262 0.360303 0.629098 0.050 Uiso 1 1 calc R U . . .
C17 C 0.7194(7) 0.5291(7) 0.5744(4) 0.0480(17) Uani 1 1 d . . . . .
H17 H 0.616941 0.507443 0.564984 0.058 Uiso 1 1 calc R U . . .
C29 C 1.0518(9) -0.0387(7) 0.7423(4) 0.0513(19) Uani 1 1 d . . . . .
H29 H 1.076846 -0.105126 0.711014 0.062 Uiso 1 1 calc R U . . .
O3W O 0.7646(8) 0.4105(9) 0.7992(5) 0.108(3) Uani 1 1 d G . . . .
H3WA H 0.689127 0.380449 0.818469 0.161 Uiso 1 1 d G U . . .
H3WB H 0.783222 0.494873 0.812122 0.161 Uiso 1 1 d G U . . .
C24 C 1.0172(8) 0.8017(6) 0.5388(4) 0.0461(17) Uani 1 1 d . . . . .
H24 H 0.962621 0.858052 0.509232 0.055 Uiso 1 1 calc R U . . .
C21 C 1.1855(8) 0.6353(7) 0.6262(4) 0.0524(18) Uani 1 1 d . . . . .
H21 H 1.243471 0.581211 0.655508 0.063 Uiso 1 1 calc R U . . .
C15 C 0.6882(9) 0.7362(7) 0.5124(4) 0.0491(18) Uani 1 1 d . . . . .
C23 C 1.1658(10) 0.8353(7) 0.5563(5) 0.061(2) Uani 1 1 d . . . . .
H23 H 1.212476 0.914627 0.538604 0.074 Uiso 1 1 calc R U . . .
C22 C 1.2513(9) 0.7521(8) 0.6009(5) 0.066(2) Uani 1 1 d . . . . .
H22 H 1.353659 0.777569 0.613064 0.080 Uiso 1 1 calc R U . . .
O2W O 0.6540(15) 0.7039(14) -0.2631(8) 0.176(5) Uani 1 1 d G . . . .
H2WA H 0.661761 0.787611 -0.268800 0.264 Uiso 1 1 d G U . . .
H2WB H 0.565094 0.669355 -0.286482 0.264 Uiso 1 1 d G U . . .
O1W O 0.2045(4) 1.1285(4) 0.0342(2) 0.0290(9) Uani 1 1 d . . . . .
H1WA H 0.242171 1.140435 -0.008015 0.044 Uiso 1 1 d R U . . .
H1WB H 0.263479 1.090257 0.066416 0.044 Uiso 1 1 d R U . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co1 0.0228(5) 0.0167(5) 0.0230(5) 0.0043(4) 0.0077(4) 0.0089(4)
Co2 0.0249(4) 0.0173(4) 0.0246(4) 0.0053(3) 0.0090(3) 0.0089(3)
O2 0.0234(19) 0.0198(18) 0.030(2) 0.0007(15) 0.0068(16) 0.0114(15)
O1 0.0283(19) 0.0229(19) 0.027(2) 0.0000(16) 0.0023(17) 0.0120(16)
O6 0.036(2) 0.0127(18) 0.043(2) 0.0046(16) 0.0138(18) 0.0110(15)
O3 0.036(2) 0.0160(18) 0.043(2) 0.0060(16) 0.0172(18) 0.0108(16)
O4 0.047(2) 0.030(2) 0.049(3) 0.0090(19) 0.029(2) 0.0067(19)
O5 0.040(2) 0.026(2) 0.060(3) -0.0013(19) 0.027(2) 0.0095(18)
N4 0.031(2) 0.030(3) 0.023(2) 0.008(2) 0.006(2) 0.012(2)
N1 0.030(2) 0.020(2) 0.027(2) 0.0040(18) 0.006(2) 0.0077(19)
O8 0.055(3) 0.066(3) 0.061(3) 0.030(3) 0.038(2) 0.037(2)
C3 0.019(2) 0.021(3) 0.024(3) 0.001(2) 0.003(2) 0.008(2)
C7 0.034(3) 0.013(2) 0.040(3) 0.007(2) 0.016(3) 0.007(2)
C1 0.025(3) 0.015(2) 0.024(3) 0.007(2) 0.012(2) 0.006(2)
C2 0.029(3) 0.018(3) 0.029(3) 0.004(2) 0.008(2) 0.006(2)
C5 0.025(3) 0.020(3) 0.029(3) 0.003(2) 0.011(2) 0.010(2)
C4 0.024(3) 0.016(2) 0.026(3) 0.005(2) 0.008(2) 0.009(2)
N2 0.049(3) 0.061(4) 0.026(3) 0.015(2) 0.015(2) 0.034(3)
C6 0.024(3) 0.013(2) 0.030(3) -0.002(2) 0.002(2) 0.006(2)
N3 0.044(3) 0.050(3) 0.035(3) 0.020(2) 0.018(2) 0.028(3)
C9 0.019(3) 0.019(3) 0.031(3) -0.001(2) 0.003(2) 0.005(2)
C8 0.026(3) 0.024(3) 0.030(3) 0.003(2) 0.015(2) 0.008(2)
C31 0.026(3) 0.031(3) 0.031(3) 0.007(2) 0.012(2) 0.012(2)
C14 0.032(3) 0.033(3) 0.026(3) 0.009(2) 0.007(2) 0.014(2)
C26 0.038(3) 0.040(3) 0.027(3) 0.014(3) 0.010(3) 0.017(3)
C10 0.032(3) 0.029(3) 0.032(3) 0.010(2) 0.009(2) 0.013(2)
C20 0.041(3) 0.045(4) 0.026(3) 0.002(3) 0.009(3) 0.011(3)
C19 0.043(3) 0.033(3) 0.024(3) 0.009(2) 0.011(3) 0.013(3)
C13 0.032(3) 0.030(3) 0.026(3) 0.007(2) 0.005(2) 0.010(2)
C16 0.050(4) 0.046(4) 0.021(3) 0.003(3) 0.001(3) 0.023(3)
C30 0.056(4) 0.036(3) 0.031(3) 0.006(3) 0.011(3) 0.024(3)
C27 0.032(3) 0.040(3) 0.025(3) 0.010(3) 0.008(2) 0.012(3)
C12 0.040(3) 0.044(4) 0.026(3) 0.003(3) 0.014(3) 0.015(3)
C25 0.065(4) 0.032(3) 0.022(3) 0.008(2) 0.016(3) 0.016(3)
C11 0.041(3) 0.039(3) 0.037(3) 0.010(3) 0.016(3) 0.023(3)
C28 0.061(4) 0.056(4) 0.025(3) 0.015(3) 0.017(3) 0.023(3)
O7 0.181(7) 0.127(6) 0.044(3) 0.021(3) 0.029(4) 0.114(6)
C18 0.041(4) 0.040(4) 0.045(4) 0.015(3) 0.004(3) 0.011(3)
C17 0.040(4) 0.050(4) 0.052(4) 0.016(3) -0.001(3) 0.015(3)
C29 0.090(6) 0.051(4) 0.027(3) 0.007(3) 0.019(3) 0.040(4)
O3W 0.077(5) 0.140(7) 0.114(5) -0.030(5) 0.072(4) -0.006(4)
C24 0.068(5) 0.036(4) 0.034(3) 0.005(3) 0.013(3) 0.008(3)
C21 0.043(4) 0.058(5) 0.058(4) 0.015(4) 0.012(3) 0.011(3)
C15 0.075(5) 0.053(4) 0.029(3) 0.005(3) 0.008(3) 0.039(4)
C23 0.094(6) 0.040(4) 0.054(5) 0.011(4) 0.034(5) 0.001(4)
C22 0.058(5) 0.067(5) 0.072(5) 0.008(4) 0.028(4) -0.007(4)
O2W 0.246(13) 0.177(10) 0.158(10) 0.015(8) 0.123(10) 0.088(9)
O1W 0.0247(19) 0.030(2) 0.034(2) 0.0057(17) 0.0070(17) 0.0068(16)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 O2 2.112(3) 2_575 ?
Co1 O2 2.112(3) . ?
Co1 N4 2.192(4) 2_666 ?
Co1 N4 2.192(4) 1_464 ?
Co1 O1W 2.072(3) . ?
Co1 O1W 2.072(3) 2_575 ?
Co2 O1 1.974(4) . ?
Co2 O6 2.010(4) 2_665 ?
Co2 O3 1.969(3) 2_675 ?
Co2 N1 2.068(4) . ?
O2 C1 1.251(6) . ?
O1 C1 1.267(6) . ?
O6 C9 1.289(6) . ?
O3 C2 1.268(6) . ?
O4 C2 1.247(6) . ?
O5 C9 1.230(6) . ?
N4 C31 1.346(7) . ?
N4 C30 1.333(7) . ?
N1 C14 1.338(7) . ?
N1 C10 1.336(7) . ?
O8 C26 1.228(7) . ?
C3 C1 1.512(7) . ?
C3 C4 1.404(7) . ?
C3 C8 1.385(7) . ?
C7 H7 0.9300 . ?
C7 C6 1.394(7) . ?
C7 C8 1.388(7) . ?
C2 C4 1.502(7) . ?
C5 H5 0.9300 . ?
C5 C4 1.390(7) . ?
C5 C6 1.396(7) . ?
N2 H2 0.8600 . ?
N2 C13 1.417(7) . ?
N2 C15 1.315(8) . ?
C6 C9 1.490(7) . ?
N3 H3 0.8600 . ?
N3 C26 1.358(7) . ?
N3 C27 1.418(7) . ?
C8 H8 0.9300 . ?
C31 H31 0.9300 . ?
C31 C27 1.382(7) . ?
C14 H14 0.9300 . ?
C14 C13 1.386(7) . ?
C26 C19 1.485(8) . ?
C10 H10 0.9300 . ?
C10 C11 1.367(8) . ?
C20 C19 1.443(8) . ?
C20 C25 1.445(8) . ?
C20 C21 1.418(9) . ?
C19 C18 1.361(8) . ?
C13 C12 1.383(8) . ?
C16 C25 1.430(9) . ?
C16 C17 1.351(9) . ?
C16 C15 1.494(8) . ?
C30 H30 0.9300 . ?
C30 C29 1.386(8) . ?
C27 C28 1.388(8) . ?
C12 H12 0.9300 . ?
C12 C11 1.377(8) . ?
C25 C24 1.402(9) . ?
C11 H11 0.9300 . ?
C28 H28 0.9300 . ?
C28 C29 1.374(9) . ?
O7 C15 1.250(8) . ?
C18 H18 0.9300 . ?
C18 C17 1.397(8) . ?
C17 H17 0.9300 . ?
C29 H29 0.9300 . ?
O3W H3WA 0.8497 . ?
O3W H3WB 0.8500 . ?
C24 H24 0.9300 . ?
C24 C23 1.348(10) . ?
C21 H21 0.9300 . ?
C21 C22 1.354(10) . ?
C23 H23 0.9300 . ?
C23 C22 1.406(11) . ?
C22 H22 0.9300 . ?
O2W H2WA 0.8501 . ?
O2W H2WB 0.8499 . ?
O1W H1WA 0.8510 . ?
O1W H1WB 0.8508 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O2 Co1 O2 180.0 2_575 . ?
O2 Co1 N4 88.93(15) 2_575 2_666 ?
O2 Co1 N4 91.07(15) . 2_666 ?
O2 Co1 N4 88.93(15) . 1_464 ?
O2 Co1 N4 91.07(15) 2_575 1_464 ?
N4 Co1 N4 180.0(2) 1_464 2_666 ?
O1W Co1 O2 86.67(14) . 2_575 ?
O1W Co1 O2 86.67(14) 2_575 . ?
O1W Co1 O2 93.33(14) . . ?
O1W Co1 O2 93.33(14) 2_575 2_575 ?
O1W Co1 N4 88.56(16) . 1_464 ?
O1W Co1 N4 91.45(16) 2_575 1_464 ?
O1W Co1 N4 88.55(16) 2_575 2_666 ?
O1W Co1 N4 91.44(16) . 2_666 ?
O1W Co1 O1W 180.0 2_575 . ?
O1 Co2 O6 123.33(15) . 2_665 ?
O1 Co2 N1 99.68(16) . . ?
O6 Co2 N1 116.46(16) 2_665 . ?
O3 Co2 O1 106.08(15) 2_675 . ?
O3 Co2 O6 96.89(15) 2_675 2_665 ?
O3 Co2 N1 114.73(16) 2_675 . ?
C1 O2 Co1 131.2(3) . . ?
C1 O1 Co2 137.2(3) . . ?
C9 O6 Co2 102.8(3) . 2_665 ?
C2 O3 Co2 114.9(3) . 2_675 ?
C31 N4 Co1 122.5(4) . 1_646 ?
C30 N4 Co1 119.7(4) . 1_646 ?
C30 N4 C31 117.6(5) . . ?
C14 N1 Co2 122.2(4) . . ?
C10 N1 Co2 119.3(4) . . ?
C10 N1 C14 118.1(5) . . ?
C4 C3 C1 124.0(4) . . ?
C8 C3 C1 116.3(4) . . ?
C8 C3 C4 119.5(5) . . ?
C6 C7 H7 119.9 . . ?
C8 C7 H7 119.9 . . ?
C8 C7 C6 120.2(5) . . ?
O2 C1 O1 123.9(5) . . ?
O2 C1 C3 117.2(4) . . ?
O1 C1 C3 118.6(4) . . ?
O3 C2 C4 117.2(5) . . ?
O4 C2 O3 123.3(5) . . ?
O4 C2 C4 119.5(5) . . ?
C4 C5 H5 119.0 . . ?
C4 C5 C6 121.9(5) . . ?
C6 C5 H5 119.0 . . ?
C3 C4 C2 122.4(4) . . ?
C5 C4 C3 118.7(4) . . ?
C5 C4 C2 118.9(4) . . ?
C13 N2 H2 115.8 . . ?
C15 N2 H2 115.8 . . ?
C15 N2 C13 128.4(5) . . ?
C7 C6 C5 118.4(4) . . ?
C7 C6 C9 122.2(4) . . ?
C5 C6 C9 119.1(5) . . ?
C26 N3 H3 117.8 . . ?
C26 N3 C27 124.3(5) . . ?
C27 N3 H3 117.8 . . ?
O6 C9 C6 119.6(5) . . ?
O5 C9 O6 119.7(5) . . ?
O5 C9 C6 120.7(5) . . ?
C3 C8 C7 121.1(5) . . ?
C3 C8 H8 119.4 . . ?
C7 C8 H8 119.4 . . ?
N4 C31 H31 118.5 . . ?
N4 C31 C27 122.9(5) . . ?
C27 C31 H31 118.5 . . ?
N1 C14 H14 118.6 . . ?
N1 C14 C13 122.7(5) . . ?
C13 C14 H14 118.6 . . ?
O8 C26 N3 122.1(5) . . ?
O8 C26 C19 123.1(5) . . ?
N3 C26 C19 114.7(5) . . ?
N1 C10 H10 118.9 . . ?
N1 C10 C11 122.3(5) . . ?
C11 C10 H10 118.9 . . ?
C19 C20 C25 118.5(5) . . ?
C21 C20 C19 123.9(6) . . ?
C21 C20 C25 117.6(6) . . ?
C20 C19 C26 122.8(5) . . ?
C18 C19 C26 117.8(5) . . ?
C18 C19 C20 119.3(5) . . ?
C14 C13 N2 117.0(5) . . ?
C12 C13 N2 124.3(5) . . ?
C12 C13 C14 118.6(5) . . ?
C25 C16 C15 122.4(6) . . ?
C17 C16 C25 120.9(6) . . ?
C17 C16 C15 116.4(6) . . ?
N4 C30 H30 118.6 . . ?
N4 C30 C29 122.9(5) . . ?
C29 C30 H30 118.6 . . ?
C31 C27 N3 119.1(5) . . ?
C31 C27 C28 118.8(5) . . ?
C28 C27 N3 121.9(5) . . ?
C13 C12 H12 121.0 . . ?
C11 C12 C13 118.1(5) . . ?
C11 C12 H12 121.0 . . ?
C16 C25 C20 118.4(5) . . ?
C24 C25 C20 119.1(6) . . ?
C24 C25 C16 122.5(6) . . ?
C10 C11 C12 120.2(5) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
C27 C28 H28 120.7 . . ?
C29 C28 C27 118.5(5) . . ?
C29 C28 H28 120.7 . . ?
C19 C18 H18 118.9 . . ?
C19 C18 C17 122.2(6) . . ?
C17 C18 H18 118.9 . . ?
C16 C17 C18 120.7(6) . . ?
C16 C17 H17 119.6 . . ?
C18 C17 H17 119.6 . . ?
C30 C29 H29 120.4 . . ?
C28 C29 C30 119.3(6) . . ?
C28 C29 H29 120.4 . . ?
H3WA O3W H3WB 104.4 . . ?
C25 C24 H24 119.6 . . ?
C23 C24 C25 120.8(7) . . ?
C23 C24 H24 119.6 . . ?
C20 C21 H21 119.5 . . ?
C22 C21 C20 121.0(7) . . ?
C22 C21 H21 119.5 . . ?
N2 C15 C16 117.1(6) . . ?
O7 C15 N2 122.1(6) . . ?
O7 C15 C16 120.0(6) . . ?
C24 C23 H23 119.5 . . ?
C24 C23 C22 120.9(7) . . ?
C22 C23 H23 119.5 . . ?
C21 C22 C23 120.5(8) . . ?
C21 C22 H22 119.8 . . ?
C23 C22 H22 119.8 . . ?
H2WA O2W H2WB 104.5 . . ?
Co1 O1W H1WA 109.4 . . ?
Co1 O1W H1WB 109.3 . . ?
H1WA O1W H1WB 104.4 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 O2 C1 O1 24.1(7) . . . . ?
Co1 O2 C1 C3 -162.9(3) . . . . ?
Co1 N4 C31 C27 175.3(4) 1_646 . . . ?
Co1 N4 C30 C29 -175.4(5) 1_646 . . . ?
Co2 O1 C1 O2 -172.0(3) . . . . ?
Co2 O1 C1 C3 15.1(7) . . . . ?
Co2 O6 C9 O5 3.0(6) 2_665 . . . ?
Co2 O6 C9 C6 -176.1(4) 2_665 . . . ?
Co2 O3 C2 O4 -4.7(7) 2_675 . . . ?
Co2 O3 C2 C4 175.1(3) 2_675 . . . ?
Co2 N1 C14 C13 -174.0(4) . . . . ?
Co2 N1 C10 C11 174.6(4) . . . . ?
O3 C2 C4 C3 -6.0(8) . . . . ?
O3 C2 C4 C5 175.0(5) . . . . ?
O4 C2 C4 C3 173.8(5) . . . . ?
O4 C2 C4 C5 -5.2(8) . . . . ?
N4 C31 C27 N3 175.5(5) . . . . ?
N4 C31 C27 C28 0.5(9) . . . . ?
N4 C30 C29 C28 -0.6(11) . . . . ?
N1 C14 C13 N2 178.1(5) . . . . ?
N1 C14 C13 C12 0.6(9) . . . . ?
N1 C10 C11 C12 -1.5(9) . . . . ?
O8 C26 C19 C20 -35.2(9) . . . . ?
O8 C26 C19 C18 140.8(7) . . . . ?
C7 C6 C9 O6 7.3(8) . . . . ?
C7 C6 C9 O5 -171.8(5) . . . . ?
C1 C3 C4 C2 -6.4(8) . . . . ?
C1 C3 C4 C5 172.6(5) . . . . ?
C1 C3 C8 C7 -173.5(5) . . . . ?
C5 C6 C9 O6 -177.9(5) . . . . ?
C5 C6 C9 O5 3.0(8) . . . . ?
C4 C3 C1 O2 110.3(6) . . . . ?
C4 C3 C1 O1 -76.3(6) . . . . ?
C4 C3 C8 C7 3.0(8) . . . . ?
C4 C5 C6 C7 1.1(8) . . . . ?
C4 C5 C6 C9 -173.9(5) . . . . ?
N2 C13 C12 C11 -177.5(6) . . . . ?
C6 C7 C8 C3 -0.2(8) . . . . ?
C6 C5 C4 C3 1.6(8) . . . . ?
C6 C5 C4 C2 -179.4(5) . . . . ?
N3 C26 C19 C20 147.5(6) . . . . ?
N3 C26 C19 C18 -36.4(8) . . . . ?
N3 C27 C28 C29 -176.6(6) . . . . ?
C8 C3 C1 O2 -73.4(6) . . . . ?
C8 C3 C1 O1 100.0(5) . . . . ?
C8 C3 C4 C2 177.5(5) . . . . ?
C8 C3 C4 C5 -3.6(7) . . . . ?
C8 C7 C6 C5 -1.8(8) . . . . ?
C8 C7 C6 C9 173.0(5) . . . . ?
C31 N4 C30 C29 -0.6(9) . . . . ?
C31 C27 C28 C29 -1.7(10) . . . . ?
C14 N1 C10 C11 1.9(8) . . . . ?
C14 C13 C12 C11 -0.2(9) . . . . ?
C26 N3 C27 C31 147.5(6) . . . . ?
C26 N3 C27 C28 -37.6(9) . . . . ?
C26 C19 C18 C17 -177.9(6) . . . . ?
C10 N1 C14 C13 -1.5(8) . . . . ?
C20 C19 C18 C17 -1.7(10) . . . . ?
C20 C25 C24 C23 -1.9(9) . . . . ?
C20 C21 C22 C23 -0.1(12) . . . . ?
C19 C20 C25 C16 1.2(8) . . . . ?
C19 C20 C25 C24 -178.4(5) . . . . ?
C19 C20 C21 C22 179.4(7) . . . . ?
C19 C18 C17 C16 2.8(11) . . . . ?
C13 N2 C15 C16 177.3(6) . . . . ?
C13 N2 C15 O7 7.5(13) . . . . ?
C13 C12 C11 C10 0.6(9) . . . . ?
C16 C25 C24 C23 178.6(6) . . . . ?
C30 N4 C31 C27 0.7(8) . . . . ?
C27 N3 C26 O8 -12.7(10) . . . . ?
C27 N3 C26 C19 164.6(5) . . . . ?
C27 C28 C29 C30 1.8(11) . . . . ?
C25 C20 C19 C26 175.7(5) . . . . ?
C25 C20 C19 C18 -0.3(9) . . . . ?
C25 C20 C21 C22 -1.6(10) . . . . ?
C25 C16 C17 C18 -1.7(10) . . . . ?
C25 C16 C15 N2 78.0(9) . . . . ?
C25 C16 C15 O7 -111.9(9) . . . . ?
C25 C24 C23 C22 0.1(11) . . . . ?
C17 C16 C25 C20 -0.2(9) . . . . ?
C17 C16 C25 C24 179.3(6) . . . . ?
C17 C16 C15 N2 -108.0(8) . . . . ?
C17 C16 C15 O7 62.0(10) . . . . ?
C24 C23 C22 C21 1.0(12) . . . . ?
C21 C20 C19 C26 -5.3(9) . . . . ?
C21 C20 C19 C18 178.7(6) . . . . ?
C21 C20 C25 C16 -177.8(6) . . . . ?
C21 C20 C25 C24 2.6(9) . . . . ?
C15 N2 C13 C14 169.7(7) . . . . ?
C15 N2 C13 C12 -12.9(10) . . . . ?
C15 C16 C25 C20 173.5(5) . . . . ?
C15 C16 C25 C24 -6.9(9) . . . . ?
C15 C16 C17 C18 -175.8(6) . . . . ?
_shelx_res_file
;
TITL 1_a.res in P-1
1.res
created by SHELXL-2018/3 at 10:21:30 on 24-Oct-2019
REM Old TITL 1 in P-1
REM SHELXT solution in P-1: R1 0.135, Rweak 0.008, Alpha 0.045
REM 0.000 for 0 systematic absences, Orientation as input
REM Formula found by SHELXT: C66 N8 O18 Co3
CELL 0.71073 9.4573 10.1544 16.5808 92.219 101.862 101.043
ZERR 1 0.0006 0.0006 0.001 0.002 0.001 0.001
LATT 1
SFAC C H Co N O
UNIT 62 50 3 8 22
L.S. 5
PLAN 5
TEMP 23
CONF
BOND
list 4
MORE -1
BOND $H
fmap 2
acta
REM
REM
REM
WGHT 0.094000 3.326200
FVAR 0.52936
CO1 3 0.000000 1.000000 0.000000 10.50000 0.02284 0.01668 =
0.02301 0.00435 0.00772 0.00886
CO2 3 0.523116 0.894548 0.123763 11.00000 0.02486 0.01729 =
0.02461 0.00530 0.00895 0.00891
O2 5 0.091831 0.828578 -0.013394 11.00000 0.02342 0.01981 =
0.03018 0.00069 0.00675 0.01144
O1 5 0.311949 0.876651 0.072388 11.00000 0.02826 0.02288 =
0.02728 0.00005 0.00233 0.01196
O6 5 0.348417 0.221358 -0.086681 11.00000 0.03622 0.01274 =
0.04328 0.00459 0.01376 0.01095
O3 5 0.375425 0.933954 -0.091700 11.00000 0.03558 0.01598 =
0.04278 0.00599 0.01724 0.01078
O4 5 0.520238 0.835911 -0.152632 11.00000 0.04656 0.02975 =
0.04850 0.00898 0.02917 0.00665
O5 5 0.505424 0.352342 -0.142765 11.00000 0.03999 0.02551 =
0.05977 -0.00132 0.02662 0.00954
N4 4 1.003328 0.034609 0.870660 11.00000 0.03066 0.03027 =
0.02277 0.00806 0.00639 0.01165
N1 4 0.511301 0.894838 0.246954 11.00000 0.02985 0.01999 =
0.02661 0.00398 0.00618 0.00769
O8 5 1.142773 0.342917 0.655941 11.00000 0.05473 0.06598 =
0.06057 0.03031 0.03792 0.03665
C3 1 0.259916 0.689816 -0.029028 11.00000 0.01928 0.02109 =
0.02378 0.00098 0.00339 0.00792
C7 1 0.240458 0.448873 -0.033834 11.00000 0.03429 0.01321 =
0.03993 0.00666 0.01555 0.00723
AFIX 43
H7 2 0.199109 0.365618 -0.018357 11.00000 -1.20000
AFIX 0
C1 1 0.220025 0.809698 0.011225 11.00000 0.02523 0.01516 =
0.02374 0.00679 0.01177 0.00610
C2 1 0.423363 0.831491 -0.111296 11.00000 0.02914 0.01807 =
0.02939 0.00381 0.00828 0.00643
C5 1 0.399887 0.583309 -0.107856 11.00000 0.02523 0.01969 =
0.02859 0.00292 0.01053 0.01027
AFIX 43
H5 2 0.467155 0.589640 -0.142013 11.00000 -1.20000
AFIX 0
C4 1 0.358728 0.699637 -0.082241 11.00000 0.02446 0.01634 =
0.02638 0.00464 0.00770 0.00888
N2 4 0.668270 0.745380 0.432104 11.00000 0.04872 0.06130 =
0.02646 0.01509 0.01506 0.03431
AFIX 43
H2 2 0.716861 0.700502 0.406797 11.00000 -1.20000
AFIX 0
C6 1 0.343207 0.457245 -0.083810 11.00000 0.02430 0.01256 =
0.03018 -0.00246 0.00184 0.00581
N3 4 0.962518 0.298924 0.728067 11.00000 0.04448 0.04979 =
0.03547 0.01985 0.01841 0.02753
AFIX 43
H3 2 0.895338 0.331077 0.745361 11.00000 -1.20000
AFIX 0
C9 1 0.403183 0.338861 -0.106426 11.00000 0.01881 0.01939 =
0.03120 -0.00142 0.00303 0.00503
C8 1 0.199716 0.564480 -0.007119 11.00000 0.02583 0.02408 =
0.03007 0.00266 0.01471 0.00805
AFIX 43
H8 2 0.130826 0.557696 0.026058 11.00000 -1.20000
AFIX 0
C31 1 0.983443 0.151084 0.838544 11.00000 0.02601 0.03100 =
0.03075 0.00726 0.01186 0.01162
AFIX 43
H31 2 0.960500 0.216725 0.871447 11.00000 -1.20000
AFIX 0
C14 1 0.593533 0.830550 0.301099 11.00000 0.03160 0.03267 =
0.02599 0.00857 0.00712 0.01354
AFIX 43
H14 2 0.664694 0.791516 0.283809 11.00000 -1.20000
AFIX 0
C26 1 1.029903 0.367855 0.673072 11.00000 0.03801 0.03958 =
0.02726 0.01383 0.00981 0.01691
C10 1 0.407209 0.947853 0.271983 11.00000 0.03222 0.02899 =
0.03153 0.01027 0.00922 0.01257
AFIX 43
H10 2 0.347338 0.990425 0.234427 11.00000 -1.20000
AFIX 0
C20 1 1.029671 0.594043 0.608614 11.00000 0.04071 0.04538 =
0.02609 0.00188 0.00922 0.01137
C19 1 0.952562 0.470338 0.633000 11.00000 0.04290 0.03282 =
0.02445 0.00935 0.01115 0.01339
C13 1 0.577098 0.819689 0.381892 11.00000 0.03218 0.02983 =
0.02641 0.00660 0.00456 0.01043
C16 1 0.786385 0.645051 0.549185 11.00000 0.04967 0.04632 =
0.02067 0.00286 0.00105 0.02250
C30 1 1.037579 -0.057632 0.822808 11.00000 0.05601 0.03642 =
0.03119 0.00632 0.01098 0.02384
AFIX 43
H30 2 1.052567 -0.138272 0.844384 11.00000 -1.20000
AFIX 0
C27 1 0.995598 0.177496 0.758843 11.00000 0.03237 0.03980 =
0.02539 0.01012 0.00809 0.01225
C12 1 0.470285 0.876536 0.407356 11.00000 0.03995 0.04420 =
0.02611 0.00315 0.01367 0.01540
AFIX 43
H12 2 0.455974 0.870956 0.461058 11.00000 -1.20000
AFIX 0
C25 1 0.943824 0.682818 0.564834 11.00000 0.06545 0.03184 =
0.02211 0.00832 0.01619 0.01588
C11 1 0.385691 0.941671 0.350876 11.00000 0.04103 0.03886 =
0.03653 0.00983 0.01588 0.02272
AFIX 43
H11 2 0.313689 0.981576 0.366484 11.00000 -1.20000
AFIX 0
C28 1 1.028634 0.079418 0.709247 11.00000 0.06113 0.05558 =
0.02469 0.01508 0.01684 0.02306
AFIX 43
H28 2 1.034918 0.093308 0.654873 11.00000 -1.20000
AFIX 0
O7 5 0.612998 0.784961 0.554890 11.00000 0.18059 0.12668 =
0.04420 0.02149 0.02862 0.11381
C18 1 0.802312 0.441276 0.614531 11.00000 0.04059 0.03970 =
0.04522 0.01482 0.00357 0.01107
AFIX 43
H18 2 0.753262 0.360303 0.629098 11.00000 -1.20000
AFIX 0
C17 1 0.719386 0.529075 0.574418 11.00000 0.04050 0.04953 =
0.05227 0.01571 -0.00101 0.01500
AFIX 43
H17 2 0.616941 0.507443 0.564984 11.00000 -1.20000
AFIX 0
C29 1 1.051845 -0.038678 0.742311 11.00000 0.08980 0.05139 =
0.02662 0.00669 0.01911 0.04048
AFIX 43
H29 2 1.076846 -0.105126 0.711014 11.00000 -1.20000
AFIX 6
O3W 5 0.764584 0.410545 0.799228 11.00000 0.07714 0.13992 =
0.11400 -0.03025 0.07243 -0.00554
H3WA 2 0.689127 0.380449 0.818469 11.00000 -1.50000
H3WB 2 0.783222 0.494873 0.812122 11.00000 -1.50000
AFIX 0
C24 1 1.017155 0.801724 0.538846 11.00000 0.06836 0.03570 =
0.03415 0.00539 0.01337 0.00770
AFIX 43
H24 2 0.962621 0.858052 0.509232 11.00000 -1.20000
AFIX 0
C21 1 1.185499 0.635267 0.626165 11.00000 0.04290 0.05823 =
0.05757 0.01485 0.01236 0.01068
AFIX 43
H21 2 1.243471 0.581211 0.655508 11.00000 -1.20000
AFIX 0
C15 1 0.688170 0.736182 0.512357 11.00000 0.07471 0.05305 =
0.02862 0.00533 0.00758 0.03900
C23 1 1.165804 0.835313 0.556299 11.00000 0.09370 0.04035 =
0.05380 0.01132 0.03388 0.00149
AFIX 43
H23 2 1.212476 0.914627 0.538604 11.00000 -1.20000
AFIX 0
C22 1 1.251269 0.752149 0.600869 11.00000 0.05835 0.06719 =
0.07165 0.00805 0.02781 -0.00747
AFIX 43
H22 2 1.353659 0.777569 0.613064 11.00000 -1.20000
AFIX 6
O2W 5 0.653966 0.703869 -0.263073 11.00000 0.24641 0.17670 =
0.15752 0.01469 0.12273 0.08840
H2WA 2 0.661761 0.787611 -0.268800 11.00000 -1.50000
H2WB 2 0.565094 0.669355 -0.286482 11.00000 -1.50000
AFIX 0
O1W 5 0.204530 1.128546 0.034215 11.00000 0.02467 0.02982 =
0.03354 0.00572 0.00695 0.00676
AFIX 7
H1WA 2 0.242171 1.140435 -0.008015 11.00000 -1.50000
H1WB 2 0.263479 1.090257 0.066416 11.00000 -1.50000
AFIX 0
HKLF 4
REM 1_a.res in P-1
REM wR2 = 0.1838, GooF = S = 1.032, Restrained GooF = 1.032 for all data
REM R1 = 0.0612 for 3981 Fo > 4sig(Fo) and 0.0886 for all 5431 data
REM 437 parameters refined using 0 restraints
END
WGHT 0.0940 3.3262
REM Highest difference peak 2.431, deepest hole -0.568, 1-sigma level 0.106
Q1 1 0.8763 0.6463 0.8367 11.00000 0.05 2.43
Q2 1 0.4748 0.4836 -0.3065 11.00000 0.05 1.27
Q3 1 0.7576 0.8804 0.5339 11.00000 0.05 1.08
Q4 1 0.7765 0.7720 0.5049 11.00000 0.05 0.42
Q5 1 0.3982 0.5267 -0.0617 11.00000 0.05 0.39
;
_shelx_res_checksum 87722
_shelx_hkl_file
;
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9 1 -8 5.70 7.30
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2 -2 16 60.49 12.20
3 -2 16 49.80 14.50
3 -2 16 80.59 14.50
4 -2 16 6.10 12.30
4 -2 16 -6.20 8.20
8 1 -16 196.98 22.30
7 1 -16 28.80 11.30
6 1 -16 121.29 16.70
-6 -1 16 116.29 17.10
5 1 -16 38.10 11.30
-5 -1 16 49.00 13.10
4 1 -16 156.48 16.20
-4 -1 16 128.99 17.40
3 1 -16 13.60 7.60
-3 -1 16 17.50 9.20
-2 -1 16 372.36 23.50
-1 -1 16 3.00 9.20
0 -1 16 168.38 19.30
0 -1 16 175.18 17.50
1 -1 16 -3.20 7.40
1 -1 16 3.80 10.30
2 -1 16 82.99 16.00
2 -1 16 58.39 13.20
3 -1 16 19.50 10.90
3 -1 16 8.80 11.60
4 -1 16 15.20 11.00
4 -1 16 19.90 13.30
8 0 -16 -0.60 7.60
7 0 -16 22.50 11.50
6 0 -16 67.19 13.00
-6 0 16 57.79 13.40
5 0 -16 -7.40 7.10
-5 0 16 0.10 7.60
4 0 -16 28.80 9.50
-4 0 16 19.30 10.40
3 0 -16 16.60 7.80
-3 0 16 10.80 9.70
2 0 -16 75.29 11.10
-2 0 16 98.79 14.70
-1 0 16 4.80 9.10
-1 0 16 3.30 7.80
0 0 16 195.98 20.40
0 0 16 173.48 18.00
1 0 16 6.00 8.50
1 0 16 -3.90 8.10
2 0 16 230.28 22.10
2 0 16 268.47 24.40
3 0 16 -0.20 9.60
3 0 16 8.90 8.40
4 0 16 218.18 24.50
4 0 16 219.08 23.40
8 -1 -16 39.00 12.70
7 -1 -16 150.78 19.60
6 -1 -16 22.20 11.20
5 -1 -16 14.90 8.70
-5 1 16 17.10 9.10
4 -1 -16 267.97 21.30
-4 1 16 239.28 22.30
3 -1 -16 15.60 8.80
-3 1 16 33.40 11.10
2 -1 -16 -8.40 6.40
-2 1 16 4.40 8.70
-1 1 16 8.10 8.90
-1 1 16 1.10 8.00
0 1 16 64.79 12.50
0 1 16 46.30 11.90
1 1 16 14.90 10.20
1 1 16 24.70 9.40
2 1 16 197.68 22.90
2 1 16 164.18 19.40
3 1 16 22.70 11.10
3 1 16 6.40 9.10
4 1 16 29.90 12.70
8 -2 -16 34.10 12.80
7 -2 -16 62.99 14.70
6 -2 -16 4.00 8.30
5 -2 -16 66.29 12.50
-5 2 16 48.50 12.00
4 -2 -16 13.70 9.00
-4 2 16 7.20 7.30
3 -2 -16 104.39 13.90
-3 2 16 84.29 13.50
2 -2 -16 4.70 7.80
-2 2 16 0.80 8.80
-2 2 16 14.70 9.20
-1 2 16 29.10 9.90
-1 2 16 24.90 11.20
0 2 16 26.50 10.00
0 2 16 8.50 10.20
1 2 16 19.80 9.90
1 2 16 25.30 10.30
2 2 16 14.00 11.50
3 2 16 4.60 9.30
8 -3 -16 42.10 14.20
7 -3 -16 65.19 14.10
6 -3 -16 9.90 9.20
5 -3 -16 67.59 13.20
4 -3 -16 5.20 9.20
-4 3 16 6.80 7.60
3 -3 -16 282.17 22.10
-3 3 16 330.17 22.90
-3 3 16 316.17 24.70
2 -3 -16 -0.10 7.70
-2 3 16 -0.20 7.60
-2 3 16 8.10 9.60
-1 3 16 22.60 9.40
-1 3 16 29.30 12.20
0 3 16 0.70 10.10
0 3 16 15.20 8.10
1 3 16 125.59 19.20
2 3 16 26.60 13.10
3 3 16 -11.20 10.70
7 -4 -16 154.38 20.10
6 -4 -16 21.70 12.00
5 -4 -16 169.18 20.20
4 -4 -16 10.20 10.00
3 -4 -16 140.79 17.60
-3 4 16 117.49 17.30
2 -4 -16 53.79 12.60
-2 4 16 57.09 14.80
-2 4 16 52.19 10.90
-1 4 16 352.96 25.30
0 4 16 6.40 11.20
1 4 16 188.58 23.70
2 4 16 6.40 12.20
7 -5 -16 12.40 12.10
6 -5 -16 8.80 9.80
5 -5 -16 90.69 17.00
4 -5 -16 89.09 16.30
3 -5 -16 66.69 13.30
2 -5 -16 104.59 16.20
-2 5 16 71.19 16.40
1 -5 -16 147.19 17.70
-1 5 16 165.28 22.80
0 5 16 0.30 10.10
1 5 16 34.80 15.70
5 -6 -16 15.60 10.90
4 -6 -16 13.20 10.50
3 -6 -16 0.20 9.50
2 -6 -16 -18.50 8.50
-2 6 16 -3.40 11.40
1 -6 -16 69.39 14.40
-1 6 16 59.89 18.20
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-2 -6 17 6.50 12.40
-1 -6 17 0.90 9.80
0 -6 17 -16.90 8.20
1 -6 17 3.60 11.10
4 5 -17 8.60 8.10
-4 -5 17 15.10 10.40
-3 -5 17 60.09 14.00
-2 -5 17 134.49 20.10
-1 -5 17 73.29 16.80
0 -5 17 13.30 11.10
1 -5 17 -7.80 10.30
2 -5 17 33.50 14.00
5 4 -17 251.37 22.10
-5 -4 17 244.38 25.20
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-4 -4 17 4.70 9.70
-3 -4 17 47.70 13.00
-2 -4 17 55.29 14.10
-1 -4 17 89.99 17.20
0 -4 17 -11.80 9.00
1 -4 17 302.67 28.10
2 -4 17 57.59 17.20
3 -4 17 151.18 23.30
3 -4 17 156.28 19.00
6 3 -17 6.50 7.90
-6 -3 17 0.60 9.60
5 3 -17 48.20 12.10
-5 -3 17 37.00 11.40
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-4 -3 17 18.10 10.30
-3 -3 17 36.10 11.70
-2 -3 17 44.30 13.10
-1 -3 17 37.30 12.40
0 -3 17 59.79 14.90
1 -3 17 130.49 19.00
2 -3 17 65.29 13.00
2 -3 17 68.19 17.00
3 -3 17 31.50 11.30
3 -3 17 32.90 14.00
7 2 -17 9.00 9.90
-7 -2 17 -0.90 7.80
6 2 -17 29.00 10.80
-6 -2 17 11.40 10.60
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-5 -2 17 3.80 7.60
4 2 -17 16.00 8.60
-4 -2 17 11.00 8.80
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-2 -2 17 29.90 12.30
-1 -2 17 100.49 16.80
0 -2 17 5.70 9.70
1 -2 17 65.49 14.60
1 -2 17 42.80 11.20
2 -2 17 -5.70 7.80
2 -2 17 19.70 12.90
3 -2 17 73.19 16.40
3 -2 17 44.80 13.00
7 1 -17 65.69 13.80
6 1 -17 100.69 15.90
-6 -1 17 126.09 18.70
5 1 -17 45.30 11.20
-5 -1 17 44.80 12.90
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-4 -1 17 108.39 17.20
3 1 -17 -5.20 6.00
-3 -1 17 15.80 10.60
-2 -1 17 88.19 16.00
-1 -1 17 104.39 17.30
0 -1 17 58.19 14.70
1 -1 17 65.09 15.20
1 -1 17 15.40 10.20
2 -1 17 85.09 17.00
2 -1 17 69.39 14.00
3 -1 17 72.19 15.70
3 -1 17 100.19 17.50
7 0 -17 9.40 10.10
6 0 -17 131.79 17.30
-6 0 17 69.29 14.50
5 0 -17 5.70 8.80
-5 0 17 2.80 9.30
4 0 -17 249.48 21.10
-4 0 17 257.07 23.20
3 0 -17 43.60 10.80
-3 0 17 64.69 14.50
-2 0 17 240.88 22.20
-1 0 17 -4.60 9.10
0 0 17 10.20 8.80
0 0 17 20.70 11.00
1 0 17 1.80 10.30
1 0 17 3.50 8.90
2 0 17 124.99 18.20
2 0 17 199.98 21.90
3 0 17 0.20 9.10
3 0 17 -1.20 8.20
7 -1 -17 1.50 9.70
6 -1 -17 109.99 16.60
5 -1 -17 33.00 11.20
-5 1 17 26.10 11.40
4 -1 -17 321.57 21.20
-4 1 17 355.86 24.50
3 -1 -17 44.60 10.60
-3 1 17 48.70 12.90
-2 1 17 217.48 21.30
-1 1 17 43.00 12.50
-1 1 17 39.70 11.60
0 1 17 298.97 24.80
0 1 17 374.26 24.10
1 1 17 13.50 9.70
1 1 17 5.00 9.60
2 1 17 68.19 14.40
2 1 17 85.59 15.60
3 1 17 2.80 11.10
7 -2 -17 20.80 10.20
6 -2 -17 173.78 20.40
5 -2 -17 13.90 9.30
-5 2 17 1.10 9.10
4 -2 -17 154.78 17.90
-4 2 17 136.19 17.70
3 -2 -17 13.90 9.40
-3 2 17 22.70 10.00
-2 2 17 80.99 14.40
-1 2 17 40.50 11.30
-1 2 17 24.50 11.70
0 2 17 325.97 21.90
0 2 17 236.28 23.70
1 2 17 18.60 9.80
1 2 17 10.60 11.20
2 2 17 54.69 15.20
7 -3 -17 28.00 12.90
6 -3 -17 -16.50 7.90
5 -3 -17 28.90 11.80
4 -3 -17 1.80 8.90
-4 3 17 -2.40 8.20
3 -3 -17 137.69 16.90
-3 3 17 108.79 16.10
-2 3 17 2.00 8.00
-2 3 17 -15.40 8.40
-1 3 17 -1.10 8.20
-1 3 17 -1.70 9.80
0 3 17 2.20 11.00
1 3 17 0.90 10.40
2 3 17 14.40 12.50
6 -4 -17 8.60 11.20
5 -4 -17 113.69 17.60
4 -4 -17 -4.70 9.20
3 -4 -17 27.30 11.20
-3 4 17 9.00 10.70
2 -4 -17 -1.20 9.20
-2 4 17 33.70 10.30
-2 4 17 31.00 12.60
-1 4 17 188.18 23.20
0 4 17 10.70 11.30
1 4 17 32.20 14.70
5 -5 -17 276.17 25.80
4 -5 -17 92.39 15.90
3 -5 -17 242.68 23.40
2 -5 -17 18.20 11.30
-2 5 17 -3.40 11.50
-1 5 17 122.09 21.30
-3 -5 18 -6.20 10.00
-2 -5 18 11.00 10.50
-1 -5 18 19.00 11.60
0 -5 18 127.99 21.40
-4 -4 18 -0.60 9.80
-3 -4 18 22.00 12.00
-2 -4 18 -19.40 6.70
-1 -4 18 41.20 13.90
0 -4 18 33.10 15.50
1 -4 18 22.30 12.70
5 3 -18 108.39 15.70
-5 -3 18 111.29 18.70
-4 -3 18 21.20 10.60
-3 -3 18 136.69 20.00
-2 -3 18 9.00 10.20
-1 -3 18 310.47 27.70
0 -3 18 21.90 13.00
1 -3 18 74.79 17.10
2 -3 18 1.60 10.40
6 2 -18 -1.80 8.40
-6 -2 18 4.20 9.60
5 2 -18 39.60 10.80
-5 -2 18 2.30 9.70
4 2 -18 52.59 12.60
-4 -2 18 40.40 12.60
-3 -2 18 83.99 15.60
-2 -2 18 16.40 10.40
-1 -2 18 116.69 17.90
0 -2 18 146.39 20.40
1 -2 18 77.29 16.40
2 -2 18 41.90 13.80
2 -2 18 28.50 11.40
6 1 -18 15.60 10.20
-6 -1 18 13.30 11.10
5 1 -18 -4.10 7.80
-5 -1 18 -9.40 7.20
4 1 -18 3.60 7.70
-4 -1 18 6.10 8.40
-3 -1 18 28.30 11.40
-2 -1 18 -0.20 9.80
-1 -1 18 59.29 13.90
0 -1 18 8.20 11.00
1 -1 18 42.90 13.10
1 -1 18 48.70 12.70
2 -1 18 12.60 10.20
2 -1 18 -9.00 10.20
6 0 -18 12.80 10.80
-6 0 18 12.10 10.00
5 0 -18 -4.80 7.80
-5 0 18 -2.00 7.50
4 0 -18 25.70 9.80
-4 0 18 20.20 11.30
-3 0 18 11.80 10.70
-2 0 18 7.80 10.30
-1 0 18 27.80 11.00
0 0 18 18.80 10.20
1 0 18 29.30 12.70
1 0 18 18.30 10.50
2 0 18 48.90 14.50
2 0 18 74.79 15.90
6 -1 -18 88.89 15.30
5 -1 -18 68.59 13.50
-5 1 18 81.79 15.60
4 -1 -18 174.48 18.30
-4 1 18 169.38 20.50
-3 1 18 12.40 9.10
-2 1 18 8.90 10.10
-1 1 18 0.40 9.10
0 1 18 70.19 14.10
0 1 18 40.00 13.00
1 1 18 21.90 11.50
1 1 18 9.60 10.50
6 -2 -18 84.19 16.10
5 -2 -18 0.20 9.30
-5 2 18 3.50 9.90
4 -2 -18 342.27 22.70
-4 2 18 338.37 27.30
-3 2 18 9.20 8.00
-2 2 18 75.99 13.50
-1 2 18 58.69 14.40
-1 2 18 72.59 14.10
0 2 18 165.28 19.20
0 2 18 137.59 19.80
1 2 18 0.90 10.00
6 -3 -18 41.40 12.70
5 -3 -18 6.60 10.60
4 -3 -18 44.30 11.60
-4 3 18 35.60 11.90
3 -3 -18 21.90 11.10
-3 3 18 15.30 10.10
-2 3 18 169.08 18.70
-1 3 18 35.80 12.70
-1 3 18 27.50 10.10
5 -4 -18 -12.50 9.40
4 -4 -18 -5.10 9.50
3 -4 -18 23.50 11.50
-2 4 18 21.80 12.40
-1 4 18 54.69 15.50
-3 -3 19 105.59 18.10
-2 -3 19 3.10 10.50
-1 -3 19 41.40 13.70
0 -3 19 4.00 10.30
-4 -2 19 33.00 12.20
-3 -2 19 132.29 19.60
-2 -2 19 32.80 11.60
-1 -2 19 49.30 15.20
0 -2 19 0.40 9.30
5 1 -19 13.70 9.80
-5 -1 19 9.80 10.40
-4 -1 19 7.90 9.40
-3 -1 19 49.60 14.80
-2 -1 19 20.20 10.10
-1 -1 19 63.49 15.50
0 -1 19 15.30 10.70
5 0 -19 7.90 9.20
-5 0 19 -0.10 8.20
-4 0 19 40.30 13.20
-3 0 19 -9.10 7.20
-2 0 19 20.70 11.20
-1 0 19 50.89 14.60
0 0 19 22.50 11.20
5 -1 -19 3.70 10.10
-5 1 19 5.60 8.70
-4 1 19 122.59 19.30
-3 1 19 10.00 9.80
-2 1 19 -5.30 8.80
-1 1 19 7.60 9.40
0 1 19 11.90 10.10
-4 2 19 48.50 13.70
-3 2 19 16.50 9.80
-2 2 19 21.30 10.30
-1 2 19 8.90 9.90
0 0 0 0.00 0.00
_computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)'
;
_shelx_hkl_checksum 69537
_olex2_submission_special_instructions 'No special instructions were received'
################END