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 _shelx_hkl_file ; -1 0 0 21.60 0.48 1 0 0 28.06 0.50 -2 0 0 406.67 5.95 -2 0 0 402.54 6.69 -3 0 0 8.31 0.56 -3 0 0 9.00 0.83 -4 0 0 322.10 6.19 -4 0 0 320.40 5.09 -5 0 0 14.53 1.39 -5 0 0 11.54 0.80 -6 0 0 49.50 1.54 -6 0 0 54.72 2.40 -7 0 0 7.04 0.87 -7 0 0 7.10 1.46 -8 0 0 23.61 2.26 -9 0 0 -0.67 1.08 -10 0 0 2.33 1.69 -11 0 0 -0.37 1.69 -11 1 0 3.57 1.99 -10 1 0 4.19 1.74 -9 1 0 14.02 2.13 -8 1 0 1.09 1.17 -7 1 0 16.92 1.80 -6 1 0 1.05 0.84 -6 1 0 0.77 0.40 -5 1 0 3.57 0.95 -5 1 0 2.60 0.37 -4 1 0 38.78 1.61 -4 1 0 40.83 0.85 -3 1 0 54.58 1.71 -2 1 0 261.04 4.59 1 -1 0 16.19 0.37 -1 1 0 17.27 0.64 -1 1 0 16.91 0.37 0 -1 0 236.79 3.59 0 1 0 234.82 3.80 0 1 0 242.64 3.80 -1 -1 0 50.06 1.09 -2 -1 0 845.28 13.29 -2 -1 0 832.50 12.30 -3 -1 0 2.42 0.56 -3 -1 0 2.44 0.49 -4 -1 0 147.10 2.92 -4 -1 0 150.51 3.65 -5 -1 0 0.39 0.65 -5 -1 0 -0.08 0.51 -6 -1 0 71.77 2.84 -6 -1 0 75.09 2.15 -7 -1 0 -0.25 0.77 -7 -1 0 -0.06 1.10 -8 -1 0 25.65 2.46 -9 -1 0 2.82 1.50 -10 -1 0 7.10 1.95 -11 -1 0 0.18 1.72 -11 2 0 7.06 2.21 -10 2 0 -0.62 1.54 -9 2 0 18.86 2.25 -8 2 0 5.55 1.53 -7 2 0 36.13 2.36 -6 2 0 0.83 1.09 -5 2 0 88.70 2.87 -4 2 0 4.37 0.90 -3 2 0 22.81 1.25 2 -2 0 76.31 1.38 -2 2 0 77.29 1.82 -2 2 0 80.82 2.14 1 -2 0 13.43 0.55 -1 2 0 12.79 0.78 -1 2 0 13.48 0.66 0 -2 0 1.71 0.34 -1 -2 0 21.24 0.91 -2 -2 0 173.94 3.29 -3 -2 0 3.85 0.65 -3 -2 0 2.79 0.64 -4 -2 0 147.65 3.20 -4 -2 0 147.36 3.76 -5 -2 0 6.83 1.13 -5 -2 0 8.53 0.96 -6 -2 0 31.06 1.68 -6 -2 0 32.68 2.08 -7 -2 0 4.56 1.09 -7 -2 0 5.93 1.29 -8 -2 0 39.00 2.77 -9 -2 0 3.92 1.44 -10 -2 0 9.13 2.11 -11 3 0 7.67 2.33 -10 3 0 2.66 1.88 -9 3 0 41.54 3.20 -8 3 0 5.64 1.59 -7 3 0 69.82 3.30 -6 3 0 12.25 1.55 -5 3 0 206.75 4.92 4 -3 0 43.02 0.81 4 -3 0 40.88 0.83 -4 3 0 40.31 2.00 3 -3 0 71.37 1.43 -3 3 0 73.32 2.40 -3 3 0 69.66 1.95 2 -3 0 41.82 1.13 -2 3 0 40.71 1.68 -2 3 0 41.67 1.42 1 -3 0 101.27 2.08 -1 3 0 99.32 2.33 -1 3 0 98.63 2.35 0 -3 0 11.72 0.84 -1 -3 0 314.56 5.41 -2 -3 0 7.83 0.83 -3 -3 0 51.53 1.82 -4 -3 0 0.67 0.71 -4 -3 0 1.11 0.77 -5 -3 0 1.17 0.92 -5 -3 0 0.32 0.83 -6 -3 0 35.16 2.40 -6 -3 0 36.29 2.02 -7 -3 0 0.29 1.09 -7 -3 0 -0.84 0.97 -8 -3 0 18.00 2.20 -9 -3 0 0.46 1.19 -10 -3 0 3.12 1.58 -11 4 0 21.25 3.09 -10 4 0 4.24 2.09 -9 4 0 20.40 2.67 -8 4 0 5.77 1.87 -7 4 0 98.77 4.03 -6 4 0 2.63 1.23 -5 4 0 108.12 3.60 -5 4 0 102.74 2.97 4 -4 0 98.27 1.93 -4 4 0 96.50 2.65 -4 4 0 100.10 3.19 3 -4 0 583.56 8.79 -3 4 0 572.02 10.16 -3 4 0 567.58 9.70 2 -4 0 9.74 0.76 -2 4 0 9.45 1.00 -2 4 0 9.39 0.95 1 -4 0 201.35 3.79 -1 4 0 199.44 4.09 -1 4 0 202.93 4.10 0 -4 0 84.11 2.15 -1 -4 0 114.63 2.74 -2 -4 0 107.71 2.82 -3 -4 0 140.94 3.49 -4 -4 0 2.77 0.94 -5 -4 0 8.22 1.25 -5 -4 0 10.35 1.45 -6 -4 0 0.15 1.04 -6 -4 0 0.48 1.06 -7 -4 0 -1.34 0.94 -7 -4 0 -1.22 0.78 -8 -4 0 -2.63 1.01 -8 -4 0 0.04 1.21 -9 -4 0 2.55 1.56 -11 5 0 -3.06 1.92 -10 5 0 5.53 2.29 -9 5 0 13.35 2.31 -8 5 0 5.15 1.25 -8 5 0 2.45 1.85 -7 5 0 19.77 1.82 -7 5 0 19.59 2.50 -6 5 0 20.30 2.32 -6 5 0 18.30 1.66 5 -5 0 99.39 2.07 -5 5 0 103.48 3.64 -5 5 0 98.48 2.98 4 -5 0 -0.24 0.42 -4 5 0 0.40 0.69 -4 5 0 -1.11 0.95 3 -5 0 33.89 1.32 -3 5 0 36.70 1.74 -3 5 0 35.19 1.89 2 -5 0 64.34 1.88 -2 5 0 62.53 2.17 -2 5 0 63.01 2.19 1 -5 0 208.97 4.11 -1 5 0 197.40 4.34 -1 5 0 202.35 4.35 0 -5 0 12.58 1.13 -1 -5 0 222.08 4.70 -2 -5 0 -0.31 0.67 -3 -5 0 135.93 3.68 -4 -5 0 25.33 1.97 -5 -5 0 68.84 2.88 -5 -5 0 73.71 3.22 -6 -5 0 0.14 1.07 -6 -5 0 0.21 1.02 -7 -5 0 9.34 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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 2 -9 0 35.90 11.30 -2 9 0 25.00 9.20 1 -9 0 15.70 11.00 -1 9 0 13.00 9.30 0 -9 0 267.27 22.80 0 9 0 212.18 18.90 1 9 0 264.77 21.20 2 9 0 64.19 13.20 3 9 0 56.39 14.30 4 9 0 151.08 19.10 5 9 0 0.00 12.00 6 9 0 18.80 14.50 7 9 0 2.50 12.40 -10 10 0 7.00 13.60 -9 10 0 31.40 13.50 -8 10 0 4.20 10.90 7 -10 0 -5.80 9.20 -7 10 0 -2.50 9.70 6 -10 0 194.28 20.20 -6 10 0 211.48 21.60 5 -10 0 15.50 10.20 -5 10 0 24.80 11.10 4 -10 0 151.58 18.00 -4 10 0 160.48 17.90 3 -10 0 4.80 10.20 -3 10 0 1.20 8.00 2 -10 0 387.06 25.40 -2 10 0 422.86 24.40 1 -10 0 -14.50 7.70 -1 10 0 21.60 10.50 0 10 0 21.10 11.50 1 10 0 13.90 9.80 2 10 0 153.88 19.20 3 10 0 36.60 12.80 4 10 0 154.48 21.70 5 10 0 -2.40 14.10 6 10 0 22.50 13.10 -9 11 0 88.59 18.60 -8 11 0 22.00 12.90 7 -11 0 31.70 13.70 -7 11 0 23.70 11.80 6 -11 0 18.00 11.80 -6 11 0 -1.70 9.10 5 -11 0 9.30 11.70 -5 11 0 13.50 9.60 4 -11 0 16.80 11.90 -4 11 0 9.90 10.30 3 -11 0 6.90 11.60 -3 11 0 -7.10 7.40 2 -11 0 30.70 13.40 -2 11 0 61.29 13.70 1 -11 0 -12.70 11.00 -1 11 0 4.40 9.60 0 11 0 127.79 17.70 1 11 0 -2.80 10.60 2 11 0 89.29 16.60 3 11 0 70.69 15.80 4 11 0 139.79 21.40 -7 12 0 177.18 22.70 6 -12 0 40.30 15.00 -6 12 0 31.30 14.50 5 -12 0 187.28 22.90 -5 12 0 152.48 20.10 4 -12 0 14.40 12.60 -4 12 0 36.50 12.00 3 -12 0 111.69 19.60 -3 12 0 118.09 18.60 2 -12 0 0.10 12.50 -2 12 0 2.40 9.50 -1 12 0 51.19 14.10 0 12 0 24.50 12.80 1 12 0 7.30 10.80 2 12 0 105.99 19.90 3 12 0 9.20 14.80 5 -13 0 46.60 16.80 -5 13 0 23.90 14.30 4 -13 0 14.10 15.10 -4 13 0 8.10 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160.28 11.90 -4 6 -4 186.88 15.40 4 -6 4 185.38 11.60 -5 6 -4 1.10 6.50 5 -6 4 3.60 5.20 -6 6 -4 10.80 7.40 -7 6 -4 29.60 11.10 -8 6 -4 27.20 10.60 -9 6 -4 108.79 17.10 -10 6 -4 42.20 14.90 11 -6 4 108.69 18.70 10 5 -4 17.90 16.00 10 5 -4 40.80 15.10 9 5 -4 10.20 13.60 9 5 -4 30.40 12.20 8 5 -4 33.10 13.70 8 5 -4 29.70 10.50 7 5 -4 3.50 10.80 7 5 -4 -7.00 7.50 6 5 -4 267.47 17.90 6 5 -4 261.77 21.30 5 5 -4 37.60 10.50 5 5 -4 26.00 8.50 4 5 -4 77.69 11.30 4 5 -4 82.99 9.90 3 5 -4 218.38 12.00 3 5 -4 194.08 14.90 2 5 -4 440.16 15.00 2 5 -4 473.75 18.30 1 5 -4 87.29 9.30 1 5 -4 103.89 7.90 0 5 -4 461.45 13.10 0 5 -4 458.65 16.90 -1 5 -4 90.29 7.20 -1 5 -4 71.29 8.40 -2 5 -4 170.18 8.60 -2 5 -4 180.98 11.40 2 -5 4 172.68 10.10 -3 5 -4 -1.90 3.80 -3 5 -4 7.20 5.30 3 -5 4 6.60 4.30 -4 5 -4 120.59 12.40 -4 5 -4 113.89 10.00 4 -5 4 127.19 8.90 -5 5 -4 60.79 10.50 5 -5 4 56.19 6.70 -6 5 -4 244.68 16.80 -7 5 -4 17.20 8.60 -8 5 -4 16.80 9.30 -9 5 -4 14.80 10.70 10 -5 4 12.50 11.20 11 -5 4 44.70 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-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 ; -1 0 0 226.18 5.20 -2 0 0 3254.27 45.70 -3 0 0 599.54 14.30 -4 0 0 2324.07 39.00 -5 0 0 471.65 15.50 -6 0 0 631.74 20.10 -7 0 0 87.39 10.40 7 0 0 91.49 11.40 -8 0 0 204.78 15.70 8 0 0 183.48 16.70 9 0 0 7.00 6.40 9 0 0 5.20 6.70 9 0 0 2.10 7.50 10 0 0 103.29 14.90 10 0 0 118.89 16.70 10 0 0 101.39 13.60 10 -1 0 54.89 10.80 10 -1 0 45.40 11.70 9 -1 0 52.79 11.00 9 -1 0 52.79 9.90 8 -1 0 15.20 6.50 8 -1 0 6.00 6.00 7 -1 0 150.78 14.30 7 -1 0 198.68 12.70 6 -1 0 51.99 7.50 6 -1 0 53.89 9.10 5 -1 0 37.00 5.90 4 -1 0 105.29 7.80 3 -1 0 739.73 16.30 2 -1 0 2147.69 32.20 1 -1 0 144.19 5.00 1 -1 0 146.19 4.40 0 -1 0 1864.51 26.20 0 1 0 1842.02 28.00 -1 -1 0 459.85 10.00 1 1 0 459.25 10.40 -2 -1 0 9999.00 128.09 2 1 0 9661.63 137.49 -3 -1 0 -1.30 3.00 3 1 0 -1.40 2.70 -4 -1 0 749.03 19.50 4 1 0 792.02 21.90 -5 -1 0 32.30 6.30 5 1 0 50.59 8.00 -6 -1 0 749.42 22.70 6 1 0 725.73 25.40 -7 -1 0 13.80 6.30 7 1 0 17.40 6.90 7 1 0 12.70 7.40 -8 -1 0 238.08 15.60 8 1 0 306.47 17.60 8 1 0 248.78 17.80 -9 -1 0 0.90 6.30 9 1 0 5.50 7.80 9 1 0 16.20 6.80 -10 -1 0 118.99 14.70 10 1 0 92.19 14.50 10 1 0 89.09 15.30 11 -2 0 115.59 17.00 10 -2 0 20.70 10.00 9 -2 0 88.39 13.50 9 -2 0 69.19 11.00 8 -2 0 43.00 8.70 8 -2 0 34.70 9.70 7 -2 0 301.07 15.20 7 -2 0 296.87 18.20 6 -2 0 4.40 4.90 6 -2 0 1.30 4.30 5 -2 0 1080.29 29.00 5 -2 0 1086.09 25.50 4 -2 0 19.40 4.30 4 -2 0 27.20 5.40 3 -2 0 83.19 7.70 3 -2 0 101.59 6.40 2 -2 0 200.28 7.80 2 -2 0 186.38 8.30 1 -2 0 222.38 7.40 1 -2 0 231.58 7.60 0 -2 0 57.79 4.80 0 -2 0 61.39 3.40 -1 -2 0 697.03 15.60 -1 -2 0 706.13 11.80 1 2 0 718.43 16.60 -2 -2 0 825.72 18.90 2 2 0 820.52 19.80 -3 -2 0 107.79 8.30 3 2 0 111.79 9.00 -4 -2 0 1823.12 36.00 4 2 0 1768.82 37.90 -5 -2 0 9.20 4.80 5 2 0 10.70 5.60 -6 -2 0 183.28 14.10 6 2 0 186.78 15.50 -7 -2 0 61.09 9.90 7 2 0 55.79 10.80 7 2 0 47.30 8.60 -8 -2 0 243.78 16.20 8 2 0 238.18 15.30 8 2 0 275.27 18.90 -9 -2 0 64.79 11.20 9 2 0 36.90 11.40 -10 -2 0 149.59 16.90 10 2 0 172.38 20.60 11 -3 0 22.50 11.00 10 -3 0 57.29 13.00 9 -3 0 168.28 18.30 9 -3 0 125.79 13.80 8 -3 0 3.50 5.90 8 -3 0 0.60 6.10 7 -3 0 282.27 18.20 7 -3 0 246.78 14.30 6 -3 0 101.89 11.80 6 -3 0 94.39 9.80 5 -3 0 1338.17 29.80 5 -3 0 1436.16 35.10 4 -3 0 274.97 13.20 4 -3 0 283.77 11.60 3 -3 0 127.29 8.40 3 -3 0 113.49 8.10 2 -3 0 733.73 18.30 2 -3 0 728.43 17.40 1 -3 0 113.39 6.40 1 -3 0 131.89 8.20 0 -3 0 255.67 7.70 0 -3 0 238.58 10.00 -1 -3 0 3065.59 49.20 -1 -3 0 3128.49 43.80 1 3 0 3136.99 52.89 -2 -3 0 275.37 11.90 2 3 0 267.47 12.00 -3 -3 0 875.21 22.90 3 3 0 863.31 23.80 -4 -3 0 36.10 7.00 4 3 0 42.00 7.80 -5 -3 0 16.50 6.20 5 3 0 15.50 6.90 -6 -3 0 258.27 15.90 6 3 0 263.07 17.00 -7 -3 0 8.10 7.00 7 3 0 8.50 7.60 7 3 0 17.70 5.90 -8 -3 0 259.87 20.30 8 3 0 221.88 20.70 -9 -3 0 105.79 14.20 9 3 0 115.59 16.90 10 -4 0 -5.60 8.00 9 -4 0 66.99 12.60 9 -4 0 47.10 9.80 8 -4 0 19.80 8.00 8 -4 0 3.90 6.70 7 -4 0 557.84 21.00 7 -4 0 547.55 25.00 6 -4 0 91.79 10.00 6 -4 0 98.39 12.10 5 -4 0 743.43 21.50 5 -4 0 724.83 24.50 4 -4 0 800.72 21.40 4 -4 0 797.12 24.10 3 -4 0 3768.02 63.49 3 -4 0 3803.12 60.09 2 -4 0 262.47 11.10 2 -4 0 231.88 10.90 1 -4 0 966.40 20.70 1 -4 0 920.51 22.50 0 -4 0 1403.96 29.70 0 -4 0 1399.16 24.80 -1 -4 0 577.34 12.60 -1 -4 0 593.04 17.90 1 4 0 572.04 18.70 -2 -4 0 2371.56 34.50 -2 -4 0 2430.86 44.60 2 4 0 2241.18 45.90 -3 -4 0 2139.29 42.60 3 4 0 2043.60 44.10 -4 -4 0 13.00 5.80 4 4 0 18.60 7.10 -5 -4 0 8.70 5.70 5 4 0 30.60 8.40 -6 -4 0 -2.60 5.30 6 4 0 3.00 7.40 -7 -4 0 3.60 7.20 7 4 0 4.40 8.20 -8 -4 0 33.80 10.30 8 4 0 17.50 10.30 -9 -4 0 65.09 13.00 9 4 0 67.99 15.30 10 -5 0 112.09 17.60 9 -5 0 160.08 15.80 9 -5 0 157.28 19.20 8 -5 0 17.40 7.20 8 -5 0 21.90 8.50 7 -5 0 413.26 18.90 7 -5 0 394.56 21.70 6 -5 0 404.16 17.70 6 -5 0 319.27 18.40 5 -5 0 643.74 23.70 5 -5 0 631.44 21.10 4 -5 0 166.48 12.50 4 -5 0 151.68 12.50 3 -5 0 61.09 7.60 3 -5 0 64.39 8.60 2 -5 0 131.19 10.70 2 -5 0 128.89 8.80 1 -5 0 935.61 24.60 1 -5 0 858.81 20.70 0 -5 0 63.79 5.90 0 -5 0 81.79 8.80 -1 -5 0 1346.37 31.70 -1 -5 0 1358.96 24.00 1 5 0 1328.27 33.40 -2 -5 0 1.20 4.90 -2 -5 0 8.70 2.40 2 5 0 2.90 6.10 -3 -5 0 809.22 25.70 3 5 0 800.92 26.90 -4 -5 0 322.67 17.20 4 5 0 331.97 18.70 -5 -5 0 804.72 28.20 5 5 0 856.01 30.30 -6 -5 0 12.30 7.20 6 5 0 24.00 10.30 -7 -5 0 51.69 10.90 7 5 0 74.79 13.80 -8 -5 0 14.80 8.80 8 5 0 8.10 10.30 10 -6 0 145.99 20.00 9 -6 0 8.80 7.30 9 -6 0 12.30 8.70 8 -6 0 146.29 14.50 8 -6 0 152.68 17.20 7 -6 0 210.68 16.80 7 -6 0 190.38 18.70 6 -6 0 3.60 6.40 6 -6 0 1.30 6.40 5 -6 0 3.00 6.70 5 -6 0 -2.40 6.30 4 -6 0 161.98 13.80 4 -6 0 173.18 14.40 3 -6 0 21.00 6.00 3 -6 0 33.50 8.20 2 -6 0 224.08 13.50 2 -6 0 218.28 12.30 1 -6 0 510.05 16.30 1 -6 0 502.35 19.30 0 -6 0 116.69 11.60 0 -6 0 111.69 8.50 -1 -6 0 801.42 18.10 -1 -6 0 868.31 26.70 -2 -6 0 66.19 9.80 2 6 0 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15 -9.40 11.60 0 6 15 47.30 15.80 1 6 15 -21.80 10.50 5 -7 -15 39.00 13.20 4 -7 -15 143.29 20.50 3 -7 -15 14.00 12.90 2 -7 -15 53.69 13.70 -2 7 15 63.79 17.40 1 -7 -15 6.20 11.10 -1 7 15 0.60 13.00 -3 -7 16 128.29 18.90 -2 -7 16 7.80 11.60 -1 -7 16 24.90 13.60 0 -7 16 8.00 12.00 1 -7 16 33.70 14.40 -4 -6 16 40.00 13.40 -4 -6 16 59.29 11.80 -3 -6 16 158.68 21.10 -2 -6 16 41.80 14.90 -1 -6 16 148.79 20.90 0 -6 16 -15.20 8.80 1 -6 16 129.49 20.90 2 -6 16 -14.90 11.70 3 -6 16 117.99 21.20 -5 -5 16 256.27 25.60 -5 -5 16 283.87 22.40 -4 -5 16 -1.00 7.70 -4 -5 16 12.10 7.50 -3 -5 16 56.89 10.60 -3 -5 16 42.90 13.70 -2 -5 16 53.69 15.00 -1 -5 16 202.18 24.20 0 -5 16 8.00 10.00 1 -5 16 169.08 22.60 2 -5 16 1.00 12.90 3 -5 16 117.39 16.40 3 -5 16 106.59 21.40 6 4 -16 0.80 6.40 -6 -4 16 2.80 9.20 5 4 -16 49.10 11.20 -5 -4 16 52.69 13.00 4 4 -16 1.90 6.60 -4 -4 16 6.80 9.40 3 4 -16 101.19 12.40 -3 -4 16 97.19 17.00 -2 -4 16 9.20 11.20 -1 -4 16 -4.40 10.70 0 -4 16 10.30 9.90 1 -4 16 180.98 22.20 2 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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 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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