#------------------------------------------------------------------------------ #$Date: 2024-06-05 05:22:05 +0300 (Wed, 05 Jun 2024) $ #$Revision: 292201 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571777.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_1571777 loop_ _publ_author_name 'Qin, Hui-Yu' 'Zhang, Bing-Guang' 'Sun, Qiao-Zhen' _publ_section_title ; Poly[[{\m2-5-[(dimethylamino)(thioxo)methoxy]benzene-1,3-dicarboxylato-\k4 O 1,O 1′:O 3,O 3′}(\m2-4,4′-dipyridylamine-\k2 N 4:N 4′)cobalt(II)] dimethylformamide hemisolvate monohydrate] ; _journal_coeditor_code WM4212 _journal_issue 6 _journal_name_full IUCrData _journal_paper_doi 10.1107/S2414314624004899 _journal_volume 9 _journal_year 2024 _chemical_formula_iupac '[Co (C11 H9 N1 O5 S1) (C10 H9 N3)], 0.5C3 H7 N O, H2 O' _chemical_formula_moiety 'C21 H18 Co1 N4 O5 S1, 0.5(C3 H7 N O), H2 O' _chemical_formula_sum 'C22.5 H23.5 Co N4.5 O6.5 S' _chemical_formula_weight 551.95 _chemical_name_systematic ;Poly[[{\m~2~-5-[(dimethylamino)(thioxo)methoxy]benzene-1,3-dicarboxylato-\k^4^O^1^,O^1'^:O^3^,O^3'^}(\m~2-~4,4'-dipyridylamine-\k^2^N^4^:N^4'^)cobalt(II)] dimethylformamide hemisolvate monohydrate] ; _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _cell_angle_alpha 90 _cell_angle_beta 103.485(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.2451(14) _cell_length_b 14.4734(17) _cell_length_c 15.232(2) _cell_measurement_reflns_used 4852 _cell_measurement_temperature 298.0 _cell_measurement_theta_max 26.309 _cell_measurement_theta_min 2.922 _cell_volume 2410.7(5) _computing_cell_refinement ; SAINT (Bruker, 2015) ; _computing_data_collection ; APEX2 (Bruker, 2015) ; _computing_data_reduction ; SAINT (Bruker, 2015) ; _computing_molecular_graphics ; Olex2 (Dolomanov et al., 2009), XP (Sheldrick, 2008) ; _computing_publication_material ; publCIF (Westrip, 2010) ; _computing_structure_refinement ; SHELXL (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT (Sheldrick, 2015a) ; _diffrn_ambient_temperature 298.0 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Bruker APEXII CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0685 _diffrn_reflns_av_unetI/netI 0.0532 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 21131 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.021 _diffrn_reflns_theta_min 2.479 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.849 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6430 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.521 _exptl_crystal_description prism _exptl_crystal_F_000 1140 _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _refine_diff_density_max 0.759 _refine_diff_density_min -0.421 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 355 _refine_ls_number_reflns 4711 _refine_ls_number_restraints 64 _refine_ls_restrained_S_all 1.059 _refine_ls_R_factor_all 0.0898 _refine_ls_R_factor_gt 0.0531 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0742P)^2^+2.1129P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1290 _refine_ls_wR_factor_ref 0.1495 _reflns_number_gt 3216 _reflns_number_total 4711 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file wm4212.cif _cod_data_source_block I _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 1571777 _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. ; _shelx_hkl_file ; 2 0 0 1737.03 54.39 -2 0 0 1764.42 54.29 3 0 0 0.70 1.90 -3 0 0 1.30 1.70 -4 0 0 3589.54 111.79 4 0 0 3632.54 112.19 -5 0 0 -5.20 1.80 5 0 0 -1.70 2.70 6 0 0 3093.29 95.59 -6 0 0 2992.80 94.49 -7 0 0 -2.60 1.70 7 0 0 3.40 3.50 8 0 0 72.89 7.40 9 0 0 4.10 4.50 9 0 0 3.90 4.60 10 0 0 161.58 12.00 10 0 0 196.48 12.20 11 0 0 0.40 6.10 12 0 0 34.20 8.30 13 0 0 12.10 8.80 -2 -1 0 104.49 5.20 2 1 0 98.79 5.00 3 -1 0 3.40 1.40 -3 -1 0 2.40 2.40 3 1 0 5.70 2.60 4 -1 0 3.80 1.90 -4 -1 0 2.80 2.50 4 1 0 5.30 2.70 -5 -1 0 443.66 15.80 5 -1 0 445.06 15.40 5 1 0 449.76 16.30 6 -1 0 280.17 11.40 -6 -1 0 307.37 11.60 6 1 0 290.47 12.30 -7 -1 0 26.70 3.50 7 -1 0 38.00 4.20 7 1 0 33.10 4.70 8 -1 0 17.80 4.20 -8 -1 0 9.90 3.20 8 1 0 17.80 4.70 9 -1 0 5.60 4.40 -9 -1 0 7.10 2.90 9 -1 0 7.80 4.30 9 1 0 3.30 4.80 9 1 0 11.90 5.40 10 -1 0 119.49 10.30 10 -1 0 111.39 10.00 10 1 0 109.39 11.30 11 -1 0 31.60 6.60 11 1 0 33.30 7.40 11 1 0 27.60 7.40 12 -1 0 2.00 6.80 12 1 0 0.60 8.30 12 1 0 8.00 7.80 13 -1 0 2.50 8.80 13 -1 0 21.00 8.60 13 1 0 36.30 10.30 13 1 0 28.30 10.10 0 -2 0 15.40 1.70 0 2 0 17.10 1.80 -1 -2 0 4246.88 132.59 1 2 0 4324.37 132.59 -2 -2 0 418.56 14.90 2 2 0 439.36 14.90 -3 -2 0 1446.96 46.80 3 2 0 1493.05 47.00 -4 -2 0 333.97 12.70 4 -2 0 342.07 11.00 4 2 0 325.57 13.10 -5 -2 0 1024.80 33.90 5 -2 0 1034.10 32.60 5 2 0 1019.50 34.10 6 -2 0 39.50 4.30 -6 -2 0 30.00 4.20 6 2 0 49.10 5.10 7 -2 0 344.87 13.00 -7 -2 0 332.37 13.80 7 2 0 344.37 14.40 -8 -2 0 -1.10 3.70 8 -2 0 -2.10 3.20 8 2 0 -1.70 4.60 9 -2 0 27.10 4.60 -9 -2 0 21.60 4.40 9 -2 0 27.20 4.80 9 2 0 14.20 6.00 9 2 0 9.50 5.20 -10 -2 0 5.60 3.90 10 -2 0 10.10 5.20 10 -2 0 6.00 4.70 10 2 0 18.60 6.90 11 -2 0 33.30 6.40 -11 -2 0 30.70 3.80 11 -2 0 36.00 6.50 11 2 0 32.30 8.20 11 2 0 36.90 9.40 12 -2 0 -8.00 6.00 12 2 0 5.50 8.50 13 -2 0 5.40 8.70 13 -2 0 7.60 8.40 13 2 0 1.10 9.00 13 2 0 -22.00 9.70 0 -3 0 0.20 2.00 0 3 0 3.30 2.10 0 3 0 2.40 2.10 1 -3 0 38.90 3.00 -1 -3 0 38.60 4.50 -1 3 0 41.00 2.50 1 3 0 36.50 3.50 -1 3 0 47.40 2.40 -2 -3 0 2.20 3.00 2 3 0 1.10 2.90 -3 -3 0 17.50 3.50 3 3 0 20.10 3.60 -4 -3 0 622.04 21.70 4 3 0 608.04 21.60 -5 -3 0 295.27 12.40 5 3 0 299.17 12.70 6 -3 0 1.30 1.90 -6 -3 0 3.20 3.60 6 3 0 1.40 3.90 7 -3 0 12.30 2.80 -7 -3 0 17.20 4.40 7 3 0 12.80 4.70 -8 -3 0 2.40 4.30 8 -3 0 4.40 3.20 8 -3 0 2.90 2.90 8 3 0 2.30 5.00 9 -3 0 59.59 5.70 -9 -3 0 65.09 6.70 9 -3 0 61.69 6.80 9 3 0 68.69 7.80 10 -3 0 23.40 5.10 10 -3 0 20.30 4.70 -10 -3 0 9.40 5.20 10 3 0 19.30 6.70 10 3 0 17.10 7.20 11 -3 0 37.30 6.10 -11 -3 0 27.40 5.90 11 -3 0 40.30 6.30 11 3 0 24.40 8.10 12 -3 0 21.10 6.60 12 -3 0 7.30 6.00 -12 -3 0 2.80 4.20 12 3 0 7.40 8.80 12 3 0 14.30 9.40 13 -3 0 -1.50 7.40 13 3 0 13.10 10.90 13 3 0 -9.30 9.90 0 -4 0 50.99 4.40 0 4 0 46.90 4.50 0 4 0 50.29 4.20 -1 -4 0 7.90 3.10 1 -4 0 9.40 2.10 -1 4 0 9.70 1.80 -1 4 0 10.30 1.90 1 4 0 9.80 3.10 2 -4 0 276.07 9.30 -2 -4 0 276.27 11.30 2 4 0 276.67 11.30 -3 -4 0 554.24 20.00 3 4 0 567.74 20.10 -4 -4 0 98.89 7.40 4 4 0 103.79 7.60 -5 -4 0 3.80 3.90 5 4 0 5.80 4.10 -6 -4 0 227.28 11.40 6 4 0 213.68 11.80 -7 -4 0 -2.50 4.20 7 -4 0 0.30 2.10 7 -4 0 1.60 2.00 7 4 0 0.60 4.70 8 -4 0 14.20 3.00 -8 -4 0 11.60 5.20 8 -4 0 14.20 3.20 8 4 0 28.60 5.70 9 -4 0 43.30 4.50 9 -4 0 47.70 4.80 -9 -4 0 44.80 6.50 9 4 0 47.60 7.50 9 4 0 50.09 7.80 10 -4 0 5.60 4.10 10 -4 0 6.50 4.40 -10 -4 0 6.40 6.10 10 4 0 4.70 6.90 10 4 0 3.10 6.70 11 -4 0 -5.80 4.40 -11 -4 0 0.10 6.00 11 -4 0 -4.70 5.10 11 4 0 -1.20 8.60 11 4 0 3.00 7.60 -12 -4 0 2.90 6.50 12 -4 0 -1.30 6.00 12 -4 0 0.30 5.60 12 4 0 7.10 10.00 12 4 0 4.90 9.30 -13 -4 0 6.80 5.60 13 -4 0 -2.10 6.80 13 4 0 3.10 12.20 13 4 0 19.30 11.10 0 -5 0 -1.90 2.60 0 5 0 -1.00 2.60 0 5 0 0.40 2.50 1 -5 0 1.70 2.30 -1 -5 0 0.70 2.90 -1 5 0 1.20 2.00 -1 5 0 0.90 1.90 1 5 0 0.40 3.00 -2 -5 0 4.90 3.50 2 -5 0 4.70 1.90 2 5 0 6.70 3.60 3 -5 0 -0.80 1.40 -3 -5 0 -1.50 3.60 3 5 0 0.00 3.70 4 -5 0 261.87 8.50 -4 -5 0 261.97 12.20 4 5 0 257.67 12.10 -5 -5 0 0.30 4.00 5 -5 0 1.70 0.90 5 5 0 -2.70 4.00 6 -5 0 40.80 2.70 -6 -5 0 35.20 5.60 6 5 0 36.90 5.80 7 -5 0 10.20 2.00 7 -5 0 11.90 2.20 -7 -5 0 3.10 4.90 8 -5 0 18.60 3.00 -8 -5 0 9.20 5.60 8 -5 0 18.70 2.90 8 5 0 14.90 6.40 -9 -5 0 26.40 6.80 9 -5 0 21.60 3.60 9 -5 0 23.80 3.90 9 5 0 7.00 6.60 -10 -5 0 8.50 6.70 10 -5 0 12.10 3.90 10 -5 0 18.60 4.50 10 5 0 -0.30 7.20 -11 -5 0 -6.20 6.90 11 -5 0 0.50 5.00 11 -5 0 7.70 4.70 11 5 0 2.70 8.00 11 5 0 -8.50 8.00 12 -5 0 -5.00 5.70 -12 -5 0 2.20 7.70 12 -5 0 -0.80 5.30 12 5 0 -22.40 9.30 12 5 0 -4.00 10.20 0 -6 0 8.60 3.20 0 6 0 11.00 3.20 0 6 0 6.10 2.80 1 -6 0 8.80 2.80 -1 -6 0 9.80 3.50 -1 6 0 10.80 2.50 -1 6 0 9.10 2.50 1 6 0 13.40 3.50 1 6 0 10.20 3.60 2 -6 0 21.40 2.80 -2 -6 0 14.50 4.10 2 6 0 17.00 4.10 -3 -6 0 637.34 23.10 3 -6 0 632.64 20.80 3 6 0 635.14 23.00 -4 -6 0 538.05 21.10 4 -6 0 557.94 18.00 4 6 0 573.24 21.20 5 -6 0 27.00 2.50 -5 -6 0 30.20 5.50 5 6 0 40.40 5.80 -6 -6 0 16.70 5.30 6 -6 0 16.80 1.80 6 6 0 40.30 5.50 7 -6 0 261.17 9.50 -7 -6 0 271.17 14.70 7 6 0 273.37 14.70 8 -6 0 7.80 2.60 -8 -6 0 5.80 6.10 8 -6 0 2.20 2.30 8 6 0 -1.70 6.20 8 6 0 18.80 6.80 -9 -6 0 28.70 7.50 9 -6 0 21.40 3.50 9 -6 0 20.00 3.40 9 6 0 17.90 7.90 9 6 0 19.80 7.90 10 -6 0 -0.80 3.70 -10 -6 0 -2.20 7.40 10 -6 0 2.10 3.50 10 6 0 5.90 8.00 10 6 0 -0.70 8.30 11 -6 0 15.20 4.60 11 -6 0 15.40 5.30 -11 -6 0 18.60 8.70 11 6 0 29.30 10.10 11 6 0 22.10 9.80 12 -6 0 -15.10 5.50 -12 -6 0 1.30 9.20 12 -6 0 -1.70 5.00 12 6 0 4.10 10.40 12 6 0 3.50 10.30 0 -7 0 -5.80 3.00 0 7 0 2.10 3.00 0 7 0 -3.60 3.10 1 -7 0 82.49 6.20 -1 -7 0 84.49 7.00 -1 7 0 77.29 5.40 -1 7 0 71.49 5.40 1 7 0 81.79 6.60 1 7 0 89.59 6.70 -2 -7 0 5.80 4.30 2 -7 0 4.00 2.70 -2 7 0 5.40 1.60 2 7 0 7.50 4.10 -2 7 0 5.20 1.50 2 7 0 6.30 3.90 3 -7 0 202.18 8.40 -3 -7 0 200.98 11.10 3 7 0 206.38 10.90 3 7 0 191.98 10.70 4 -7 0 10.50 2.20 -4 -7 0 6.40 4.80 4 7 0 11.40 4.50 4 7 0 4.50 4.50 -5 -7 0 -1.70 4.90 5 -7 0 -0.20 1.70 5 7 0 -2.70 4.30 5 7 0 4.20 4.80 6 -7 0 128.79 5.40 -6 -7 0 128.29 11.10 6 7 0 140.69 10.90 6 7 0 87.59 9.30 -7 -7 0 46.20 7.40 7 -7 0 45.00 3.70 7 7 0 52.79 7.70 7 7 0 36.50 7.30 -8 -7 0 15.90 7.10 8 -7 0 19.90 2.70 8 7 0 28.10 7.70 8 7 0 23.30 7.60 9 -7 0 86.59 6.00 9 -7 0 86.49 6.40 -9 -7 0 94.29 10.20 9 7 0 99.49 10.90 9 7 0 76.79 10.30 10 -7 0 67.09 6.80 -10 -7 0 25.50 11.60 10 -7 0 46.30 4.50 10 7 0 29.90 10.00 10 7 0 46.20 10.10 -11 -7 0 14.10 10.70 11 -7 0 8.50 4.80 11 -7 0 9.70 4.00 11 7 0 5.70 10.00 11 7 0 6.50 10.10 12 -7 0 0.70 5.70 -12 -7 0 16.90 10.70 12 -7 0 13.20 5.10 12 7 0 1.80 11.20 12 7 0 0.70 11.50 0 -8 0 25.30 4.40 0 8 0 17.10 3.70 0 8 0 17.10 4.00 1 -8 0 218.58 10.10 -1 -8 0 233.98 11.30 1 8 0 222.18 10.70 1 8 0 210.68 10.60 -1 8 0 227.68 9.50 -1 8 0 215.28 9.50 2 -8 0 80.49 6.30 -2 -8 0 72.89 8.10 -2 8 0 75.49 4.30 2 8 0 58.49 6.20 -2 8 0 77.19 4.20 2 8 0 84.49 7.80 3 -8 0 694.03 23.10 -3 -8 0 680.53 25.30 3 8 0 655.83 25.00 3 8 0 675.43 25.10 -4 -8 0 228.18 12.80 4 -8 0 220.88 9.30 4 8 0 208.58 12.40 4 8 0 247.38 12.80 5 -8 0 51.39 4.40 -5 -8 0 47.50 6.90 5 8 0 43.80 6.60 6 -8 0 5.10 2.20 -6 -8 0 7.50 5.90 6 8 0 1.40 5.80 6 8 0 -1.50 5.40 -7 -8 0 22.50 7.00 7 -8 0 21.60 2.70 7 8 0 14.80 7.10 7 8 0 11.30 11.30 8 -8 0 108.09 5.90 -8 -8 0 110.09 12.50 8 8 0 117.39 13.30 -9 -8 0 298.07 18.30 9 -8 0 282.67 11.30 9 -8 0 298.87 11.80 9 8 0 300.47 19.00 9 8 0 303.87 18.80 10 -8 0 60.09 6.20 10 -8 0 55.09 5.00 -10 -8 0 50.19 10.50 10 8 0 51.49 10.60 10 8 0 61.09 11.20 11 -8 0 12.70 4.80 -11 -8 0 5.30 12.00 11 -8 0 9.00 4.10 11 8 0 24.80 10.50 11 8 0 7.70 11.10 12 -8 0 11.10 5.80 12 -8 0 8.50 4.90 12 8 0 4.00 12.60 12 8 0 12.10 11.70 0 -9 0 -3.80 3.90 0 9 0 -2.60 3.50 0 9 0 5.10 3.80 -1 -9 0 16.00 4.90 1 -9 0 13.10 4.30 1 9 0 12.10 4.30 -1 9 0 20.10 3.60 -1 9 0 8.40 3.30 1 9 0 9.70 4.50 2 -9 0 228.08 10.90 -2 -9 0 235.98 12.70 -2 9 0 241.08 8.90 -2 9 0 228.98 8.90 2 9 0 237.18 12.00 2 9 0 229.98 12.10 -3 -9 0 73.29 7.70 3 -9 0 92.49 6.90 3 9 0 96.59 8.90 3 9 0 70.39 7.30 4 -9 0 162.38 8.10 -4 -9 0 165.98 11.40 4 9 0 133.49 11.00 5 -9 0 22.30 3.40 -5 -9 0 18.70 6.40 5 9 0 31.00 6.30 5 9 0 24.30 6.30 -6 -9 0 16.90 6.80 6 -9 0 26.00 3.30 6 9 0 35.00 7.10 7 -9 0 222.88 9.20 -7 -9 0 206.88 16.20 -8 -9 0 5.60 7.50 8 -9 0 5.70 2.80 8 9 0 5.60 7.60 9 -9 0 35.60 3.80 9 9 0 27.50 9.50 9 9 0 28.70 9.10 10 -9 0 -4.20 3.70 10 -9 0 0.20 3.30 10 9 0 12.00 10.50 10 9 0 -0.20 9.10 11 -9 0 9.40 4.10 11 -9 0 15.70 4.70 -11 -9 0 18.00 10.60 11 9 0 9.40 11.70 11 9 0 8.40 10.70 0 -10 0 566.84 22.30 0 10 0 571.14 21.20 0 10 0 575.04 21.20 -1 -10 0 169.08 11.10 1 -10 0 169.28 10.00 1 10 0 143.09 10.60 1 10 0 182.48 10.10 -1 10 0 164.28 8.90 -1 10 0 167.38 8.90 2 -10 0 92.09 7.90 -2 -10 0 91.39 9.80 -2 10 0 88.39 5.40 2 10 0 93.49 8.90 2 10 0 99.29 9.20 -2 10 0 87.39 5.30 -3 -10 0 -2.70 5.40 3 -10 0 1.00 3.60 3 10 0 5.20 5.30 -4 -10 0 212.78 13.50 4 -10 0 209.78 10.40 4 10 0 235.88 14.10 4 10 0 214.88 13.40 -5 -10 0 25.90 7.70 5 -10 0 17.80 3.70 5 10 0 19.70 6.70 5 10 0 3.60 6.00 6 -10 0 139.99 7.90 -6 -10 0 139.39 13.40 6 10 0 110.09 13.00 -7 -10 0 3.50 7.70 7 -10 0 7.10 3.30 7 10 0 8.90 8.00 8 -10 0 11.10 3.30 8 10 0 22.40 9.00 -9 -10 0 17.00 9.40 9 -10 0 28.60 3.90 9 10 0 16.60 9.80 9 10 0 37.00 10.80 10 -10 0 110.39 8.40 -10 -10 0 111.39 13.60 10 -10 0 102.69 7.50 10 10 0 99.99 13.90 10 10 0 83.99 13.10 11 -10 0 -1.00 4.60 -11 -10 0 -2.30 11.70 11 -10 0 2.40 4.20 11 10 0 -13.70 12.30 11 10 0 -3.80 11.90 0 -11 0 -1.70 5.00 0 11 0 1.60 4.20 0 11 0 -3.60 4.00 -1 -11 0 -2.50 5.10 1 -11 0 -2.20 4.40 1 11 0 -0.80 4.90 -1 11 0 -2.70 3.50 -1 11 0 5.40 3.80 1 11 0 4.90 5.00 2 -11 0 0.60 4.40 -2 -11 0 0.80 5.60 -2 11 0 -1.10 2.40 -2 11 0 0.70 2.60 2 11 0 -3.10 5.30 -3 -11 0 -0.90 6.00 3 -11 0 3.60 4.20 3 11 0 9.60 5.70 3 11 0 15.80 6.30 4 -11 0 -0.90 3.90 4 11 0 7.30 6.20 4 11 0 -16.70 5.60 5 -11 0 71.89 7.70 5 11 0 79.29 9.00 5 11 0 69.19 9.10 6 -11 0 60.49 7.10 6 11 0 65.59 9.30 7 -11 0 -0.70 3.50 7 11 0 1.70 8.10 -8 -11 0 10.20 8.90 8 -11 0 8.10 3.80 8 11 0 -4.20 8.70 9 -11 0 -2.70 3.60 -9 -11 0 -6.80 9.90 9 11 0 12.10 9.80 9 11 0 31.80 10.50 10 -11 0 10.00 4.20 -10 -11 0 23.00 11.90 10 11 0 15.50 11.50 10 11 0 20.00 12.10 0 -12 0 55.49 7.70 0 12 0 51.39 6.30 0 12 0 60.69 6.60 1 -12 0 180.48 12.50 -1 -12 0 175.58 13.70 1 12 0 183.18 11.60 -1 12 0 174.88 10.20 -1 12 0 168.18 9.90 1 12 0 216.18 11.90 2 -12 0 7.00 5.20 -2 -12 0 12.20 7.50 -2 12 0 11.50 3.00 2 12 0 24.50 6.80 -2 12 0 15.70 3.10 -3 -12 0 119.09 13.40 3 -12 0 123.59 10.20 3 12 0 119.09 12.60 3 12 0 134.39 12.70 4 -12 0 13.00 4.90 4 12 0 8.90 7.20 4 12 0 11.70 7.10 5 -12 0 98.19 9.20 5 12 0 117.69 12.90 5 12 0 95.19 10.60 6 -12 0 -5.40 4.10 6 12 0 -16.60 7.50 7 -12 0 101.09 8.80 -7 -12 0 93.49 12.30 7 12 0 161.88 15.80 7 12 0 98.19 12.00 8 -12 0 3.60 4.30 -8 -12 0 4.10 10.00 8 12 0 17.20 9.70 8 12 0 23.70 10.90 9 -12 0 0.60 4.30 -9 -12 0 11.10 11.50 9 12 0 23.30 11.70 9 12 0 3.10 10.20 10 -12 0 3.10 4.70 -10 -12 0 39.50 14.10 10 12 0 12.20 13.70 10 12 0 7.00 12.30 0 -13 0 -0.30 6.50 0 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25.40 8.50 9 -7 4 20.40 2.80 9 7 4 17.30 9.30 -10 -7 -4 41.90 11.10 10 -7 4 39.60 3.90 10 7 4 45.60 11.10 11 -7 4 -1.20 4.20 -11 -7 -4 -10.10 11.60 11 7 4 11.70 11.30 -12 -8 4 8.30 12.10 12 -8 -4 21.10 7.50 12 -8 -4 -5.10 6.30 12 8 -4 7.50 12.50 12 8 -4 -12.20 10.90 11 -8 -4 28.60 6.60 11 -8 -4 36.30 7.60 -11 -8 4 6.80 11.30 11 8 -4 36.80 11.00 11 8 -4 16.00 11.10 10 -8 -4 4.40 5.20 10 -8 -4 2.40 5.70 10 8 -4 -5.00 9.00 10 8 -4 10.40 9.40 9 -8 -4 86.79 9.90 -9 -8 4 86.99 10.70 9 -8 -4 67.39 6.70 9 8 -4 84.69 10.50 -8 -8 4 66.99 9.30 8 -8 -4 90.69 8.30 8 8 -4 61.89 11.00 7 -8 -4 2.30 4.00 -7 -8 4 0.90 6.40 7 8 -4 4.80 6.30 6 -8 -4 173.18 10.00 -6 -8 4 188.68 13.00 6 8 -4 189.08 12.60 6 8 -4 191.78 12.90 -5 -8 4 64.39 7.30 5 -8 -4 67.39 7.30 5 8 -4 62.89 7.20 4 -8 -4 61.79 7.10 -4 -8 4 53.29 6.90 4 8 -4 46.30 6.40 -4 8 4 60.19 5.20 4 8 -4 61.29 7.00 -3 -8 4 -3.10 4.50 3 -8 -4 -2.40 3.70 -3 -8 4 -9.50 4.30 -3 8 4 -0.10 3.20 3 8 -4 1.20 4.30 3 8 -4 -10.30 4.00 -2 -8 4 361.86 15.80 -2 -8 4 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-2 10 359.66 16.00 1 -2 10 347.77 15.90 -1 -2 -10 346.47 15.70 -1 -2 -10 319.67 15.60 -1 2 -10 342.47 14.80 -1 2 -10 341.17 14.70 -2 -2 -10 312.77 15.00 -2 -2 -10 322.17 15.50 2 -2 10 303.97 15.10 -2 2 -10 320.17 13.70 -2 2 -10 320.47 13.60 -3 -2 -10 208.48 12.60 -3 -2 -10 211.48 12.70 3 -2 10 232.08 12.70 -3 2 -10 230.98 10.30 -3 2 -10 203.98 10.00 -4 -2 -10 7.80 5.50 -4 -2 -10 6.80 5.50 4 -2 10 18.00 6.00 -4 2 -10 11.50 2.70 -4 2 -10 10.30 2.90 4 2 10 31.90 6.70 -5 -2 -10 329.87 15.80 -5 -2 -10 332.37 15.90 5 -2 10 340.17 16.50 5 2 10 327.97 17.90 -6 -2 -10 3.40 5.20 -6 -2 -10 8.30 5.50 6 2 10 9.70 7.10 -7 -2 -10 -1.70 4.80 -7 -2 -10 5.50 4.90 7 2 10 -10.50 8.80 -8 -2 -10 10.80 3.50 8 -2 10 18.70 7.60 -8 -2 -10 15.60 4.10 8 2 10 34.90 9.80 9 -2 10 33.30 9.40 9 2 10 56.59 12.10 12 -3 -10 20.70 10.60 12 -3 -10 24.50 12.10 12 3 -10 31.10 11.80 12 3 -10 30.00 12.20 11 -3 -10 20.20 9.90 -11 -3 10 -0.80 9.50 11 -3 -10 21.20 9.20 11 3 -10 0.00 10.00 11 3 -10 0.40 9.40 -10 -3 10 -5.80 8.50 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252.97 12.80 0 4 -10 220.38 11.60 -1 -4 -10 415.36 18.40 1 -4 10 380.06 17.40 1 -4 10 429.56 17.70 -1 4 -10 379.86 15.90 1 4 10 413.96 18.30 -1 4 -10 408.36 16.00 2 -4 10 57.99 6.90 2 -4 10 73.79 7.20 -2 -4 -10 73.39 7.90 2 4 10 59.19 7.90 -2 4 -10 63.79 6.00 -2 4 -10 72.49 6.20 3 -4 10 219.18 12.30 -3 -4 -10 223.68 13.40 3 -4 10 205.28 12.50 3 4 10 208.08 14.00 -4 -4 -10 23.50 6.60 4 -4 10 28.90 6.00 4 4 10 38.60 7.90 -5 -4 -10 118.69 12.30 5 -4 10 110.29 10.60 5 4 10 103.89 10.80 7 -4 10 19.80 6.60 -7 -4 -10 15.40 7.40 7 4 10 4.70 8.80 -8 -4 -10 -5.50 6.40 -8 -4 -10 3.30 7.00 8 4 10 13.60 10.20 -9 -4 -10 7.00 6.70 -9 -4 -10 8.40 6.60 9 4 10 16.50 11.40 -12 -5 10 -3.20 11.80 12 -5 -10 -3.00 11.30 12 -5 -10 -2.30 9.60 12 5 -10 11.70 12.80 12 5 -10 -0.90 11.10 11 -5 -10 16.80 9.10 11 -5 -10 5.90 10.40 -11 -5 10 7.50 10.00 11 5 -10 25.50 11.10 11 5 -10 28.60 11.40 10 -5 -10 -1.00 8.30 10 -5 -10 7.20 8.10 10 5 -10 2.20 9.30 -10 5 10 1.80 5.80 10 5 -10 8.40 9.60 -9 -5 10 61.89 10.40 9 -5 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4 14 64.49 10.60 -1 4 -14 57.49 7.30 -1 4 -14 47.70 7.60 -2 -4 -14 13.00 8.40 -2 -4 -14 21.20 9.70 2 4 14 22.20 9.80 -2 4 -14 10.10 5.30 -2 4 -14 23.10 5.60 -3 -4 -14 15.00 9.20 -3 -4 -14 9.60 8.70 3 4 14 8.10 9.10 -3 4 -14 3.20 3.20 -3 4 -14 -6.90 3.40 4 -4 14 18.10 11.60 -4 -4 -14 14.00 8.80 -4 -4 -14 8.40 9.70 4 4 14 9.30 10.10 -5 -4 -14 36.70 11.30 5 -4 14 28.90 11.40 -5 -4 -14 21.10 10.20 5 4 14 27.30 12.00 6 -4 14 23.70 11.70 6 4 14 15.60 12.70 -10 -5 14 -5.50 12.50 -10 -5 14 7.50 12.20 10 -5 -14 -8.90 11.60 10 -5 -14 -2.30 11.50 10 5 -14 10.50 11.40 -10 5 14 8.00 10.80 10 5 -14 -24.90 11.90 9 -5 -14 76.79 13.20 9 -5 -14 117.29 14.60 -9 -5 14 63.39 12.90 -9 -5 14 92.59 14.70 -9 5 14 95.49 12.70 9 5 -14 99.89 13.60 9 5 -14 88.09 13.90 8 -5 -14 0.00 10.50 -8 -5 14 -2.00 11.40 -8 -5 14 17.10 10.10 8 -5 -14 16.70 10.30 8 5 -14 15.70 10.50 -8 5 14 -5.50 8.90 8 5 -14 7.10 10.10 -7 -5 14 87.99 12.90 7 -5 -14 98.69 12.20 -7 -5 14 78.49 11.80 7 -5 -14 91.89 13.00 -7 5 14 94.59 12.30 7 5 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12.50 5 0 -18 -2.70 10.90 -5 0 18 -33.70 10.40 4 0 -18 12.40 11.30 -4 0 18 2.40 11.10 4 0 -18 8.00 11.50 3 0 -18 16.00 11.10 3 0 -18 -13.00 10.90 -3 0 18 -2.10 10.80 -2 0 18 37.30 12.40 2 0 -18 17.50 11.30 2 0 -18 28.80 12.10 1 0 -18 13.80 11.40 1 0 -18 7.00 11.70 -1 0 18 -7.70 11.10 0 0 -18 60.59 13.00 0 0 18 26.10 12.50 0 0 -18 47.30 12.00 6 -1 -18 8.30 12.70 6 -1 -18 23.20 12.90 -6 -1 18 22.00 12.30 6 1 -18 15.00 12.80 6 1 -18 -4.30 11.50 -6 1 18 30.40 12.40 5 -1 -18 7.30 11.90 5 -1 -18 9.70 12.30 -5 -1 18 20.70 12.00 5 1 -18 -17.60 11.10 -5 1 18 17.40 12.40 5 1 -18 4.70 11.40 4 -1 -18 44.70 12.90 4 -1 -18 64.79 13.10 -4 -1 18 60.99 13.20 4 1 -18 35.20 12.60 4 1 -18 41.50 12.60 -4 1 18 62.69 13.10 -3 -1 18 1.50 11.10 3 -1 -18 6.50 11.30 3 -1 -18 5.40 11.00 -3 1 18 -1.20 11.20 3 1 -18 17.40 11.30 3 1 -18 -0.90 11.50 2 -1 -18 -0.60 11.60 -2 -1 18 7.50 10.90 2 -1 -18 14.20 11.60 2 1 -18 0.50 10.80 -2 1 18 -2.40 11.30 2 1 -18 17.80 11.20 1 -1 -18 11.40 12.10 -1 -1 18 36.00 12.10 1 -1 -18 21.10 11.90 -1 1 18 35.60 12.50 1 1 -18 35.40 11.50 1 1 -18 21.60 11.40 0 -1 18 -0.30 11.90 0 -1 -18 12.20 11.90 0 -1 -18 -3.80 11.80 0 1 -18 12.90 12.00 0 1 18 15.90 12.30 0 1 -18 -3.50 17.90 6 -2 -18 -1.40 12.60 6 -2 -18 18.30 13.00 -6 -2 18 -10.30 11.30 6 2 -18 -12.90 12.30 6 2 -18 -2.60 12.30 -6 2 18 18.20 12.30 5 -2 -18 32.80 13.10 5 -2 -18 33.20 12.80 -5 -2 18 35.40 12.70 5 2 -18 39.10 12.80 -5 2 18 27.50 12.20 5 2 -18 77.09 13.30 4 -2 -18 15.10 11.70 4 -2 -18 26.90 12.30 -4 -2 18 11.60 12.00 -4 2 18 0.60 11.50 4 2 -18 1.80 11.20 4 2 -18 28.50 12.10 3 -2 -18 93.29 13.90 -3 -2 18 70.89 13.50 3 -2 -18 86.89 13.80 3 2 -18 94.69 13.30 -3 2 18 77.39 13.90 3 2 -18 100.19 13.70 -2 -2 18 16.70 11.50 2 -2 -18 4.20 11.40 2 -2 -18 15.10 12.30 2 2 -18 -4.90 10.80 2 2 -18 4.30 11.20 -2 2 18 11.50 11.70 -1 -2 18 22.10 11.60 1 -2 -18 -1.60 12.00 1 -2 -18 33.30 12.20 1 2 -18 17.00 12.00 -1 2 18 28.70 12.80 1 2 -18 38.10 11.40 0 -2 -18 45.20 13.20 0 -2 18 69.09 13.20 0 -2 -18 31.60 12.40 0 2 18 57.39 14.20 0 2 -18 47.60 12.00 6 -3 -18 -8.70 12.20 6 -3 -18 -7.80 12.90 -6 -3 18 18.30 12.00 6 3 -18 11.00 12.70 6 3 -18 -12.70 12.00 -6 3 18 -5.80 12.30 -5 -3 18 39.20 12.60 5 -3 -18 15.40 12.60 5 -3 -18 42.00 13.60 5 3 -18 40.30 12.60 -5 3 18 15.60 12.20 5 3 -18 37.30 13.10 -4 -3 18 -15.40 10.70 4 -3 -18 8.10 12.30 4 -3 -18 6.10 12.30 4 3 -18 33.60 11.60 4 3 -18 3.80 11.60 -4 3 18 -2.40 11.20 3 -3 -18 4.30 12.00 -3 -3 18 -16.30 10.60 3 -3 -18 -1.10 12.00 3 3 -18 -9.60 10.80 -3 3 18 6.10 11.50 3 3 -18 -11.70 10.70 -2 -3 18 17.30 11.80 2 -3 -18 9.10 11.70 2 -3 -18 -1.10 11.80 -2 3 18 16.20 12.00 2 3 -18 8.70 11.40 2 3 -18 4.80 10.70 -1 -3 18 33.40 11.80 1 -3 -18 8.40 12.10 1 -3 -18 -5.20 12.00 -1 3 18 4.10 11.70 1 3 -18 11.70 10.80 0 -3 -18 -0.10 12.50 0 -3 -18 -5.40 12.30 0 -3 18 26.40 12.10 0 3 -18 -23.20 10.40 0 3 -18 7.10 10.70 0 3 18 11.80 12.80 5 -4 -18 0.30 12.90 -5 -4 18 2.50 11.70 5 -4 -18 -4.90 12.90 5 4 -18 1.70 11.90 -5 4 18 -11.30 11.50 5 4 -18 10.20 12.50 4 -4 -18 24.10 13.20 -4 -4 18 32.90 12.70 4 -4 -18 33.40 13.50 4 4 -18 21.50 12.20 4 4 -18 53.89 13.80 -4 4 18 19.90 12.30 -3 -4 18 19.50 12.30 3 -4 -18 22.00 13.20 3 -4 -18 5.70 12.60 3 4 -18 18.30 11.70 -3 4 18 38.10 12.40 3 4 -18 33.10 12.90 -2 -4 18 39.60 12.80 2 -4 -18 29.10 12.90 2 -4 -18 28.90 13.10 2 4 -18 82.49 13.30 -2 4 18 38.90 13.20 2 4 -18 63.99 12.40 1 -4 -18 16.90 13.00 1 -4 -18 4.20 12.80 -1 -4 18 24.50 12.30 1 4 -18 22.10 11.50 -1 4 18 36.50 13.10 4 -5 -18 -14.00 13.00 -4 -5 18 -10.20 11.80 -4 -5 18 3.50 14.10 4 -5 -18 -4.20 13.20 -4 5 18 -21.00 11.70 4 5 -18 20.70 12.50 4 5 -18 1.00 12.10 -3 -5 18 29.00 12.70 3 -5 -18 35.90 14.00 3 -5 -18 29.20 14.20 -3 -5 18 25.50 14.00 3 5 -18 0.00 12.00 -3 5 18 38.80 13.10 3 5 -18 34.20 12.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 63601 _shelx_res_file ; TITL mo_0322_3_P 1 21/n 1 R = 0.08 mo_0322_3_0m.res created by SHELXL-2018/3 at 13:28:44 on 22-Apr-2024 CELL 0.71073 11.2451 14.4734 15.232 90 103.485 90 ZERR 2 0.0014 0.0017 0.002 0 0.004 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Co N O S UNIT 90 94 4 18 26 4 EQIV $1 -0.5+X,0.5-Y,-0.5+Z EQIV $2 2-X,1-Y,1-Z EQIV $3 0.5+X,0.5-Y,0.5+Z EQIV $4 1+X,+Y,1+Z DFIX 2.4 H7e O2_$1 ISOR 0.01 0.02 C23 SIMU 0.01 0.02 2 N5 O6 C22 C24 C23 DFIX 2.1 H7d O4 DFIX 1.4 C24 N5 N5 C23 DFIX 2.4 C24 C23 DFIX 2.4 C24 C22 C22 C23 DFIX 1.2 C22 O6 DFIX 1.4 N5 C22 ISOR 0.01 0.02 O6 C22 N5 C24 C23 DFIX 2.3 N5 O6 ISOR 0.005 0.01 O6 L.S. 20 0 11 PLAN 5 TEMP 25 CONF HTAB N3 O6 HTAB N3 O8 HTAB C13 O2_$2 HTAB O7 O2_$1 HTAB O7 O4 HTAB O8 O5_$3 HTAB O8 O7_$4 MORE -1 BOND $H fmap 2 acta OMIT 0 1 5 OMIT 0 2 1 OMIT 0 2 2 OMIT 1 0 1 OMIT 1 3 1 OMIT 10 0 4 OMIT 11 0 3 REM REM REM WGHT 0.074200 2.112900 FVAR 0.37468 CO1 3 0.739270 0.606960 0.448751 11.00000 0.04959 0.02677 = 0.02676 -0.00185 0.01366 -0.00251 S1 6 0.212935 0.445894 0.062542 11.00000 0.07048 0.06710 = 0.07502 0.02949 0.00235 0.00371 O1 5 0.579282 0.534363 0.383637 11.00000 0.04471 0.04348 = 0.05236 -0.02070 0.01577 -0.00225 O2 5 0.752858 0.492682 0.354779 11.00000 0.04308 0.07061 = 0.05083 -0.02650 0.01891 -0.01666 O3 5 0.265242 0.322389 0.192962 11.00000 0.02962 0.05166 = 0.05234 0.01369 0.00330 0.00151 O4 5 0.595021 0.180670 0.053986 11.00000 0.05525 0.03901 = 0.04518 -0.01542 0.01465 -0.00383 O5 5 0.760210 0.213397 0.155316 11.00000 0.05051 0.06453 = 0.03979 -0.01092 0.01403 0.01275 N1 4 0.068167 0.355433 0.150053 11.00000 0.03532 0.04917 = 0.04882 -0.00336 -0.00497 0.00628 N2 4 0.811856 0.523883 0.560982 11.00000 0.05291 0.03046 = 0.03214 0.00236 0.01777 -0.00192 N3 4 0.964450 0.379061 0.799984 11.00000 0.05485 0.03753 = 0.03280 0.00846 0.01330 -0.00463 AFIX 43 H3 2 1.042657 0.385181 0.814726 11.00000 -1.20000 AFIX 0 N4 4 0.835027 0.202527 0.975035 11.00000 0.06234 0.03013 = 0.02777 0.00161 0.01545 -0.00278 C1 1 0.639263 0.484383 0.340591 11.00000 0.04424 0.03230 = 0.03029 -0.00281 0.01306 -0.00567 C2 1 0.574523 0.415086 0.273336 11.00000 0.03533 0.03219 = 0.03173 -0.00017 0.00996 -0.00066 C3 1 0.447919 0.406208 0.257373 11.00000 0.03982 0.03286 = 0.03850 -0.00284 0.01195 0.00702 AFIX 43 H3A 2 0.403355 0.444495 0.286860 11.00000 -1.20000 AFIX 0 C4 1 0.389306 0.340158 0.197472 11.00000 0.03442 0.03869 = 0.03704 0.00778 0.00517 0.00134 C5 1 0.178994 0.374064 0.136178 11.00000 0.04615 0.03657 = 0.04045 -0.00924 -0.00763 0.00863 C6 1 -0.038525 0.403471 0.098087 11.00000 0.04289 0.05723 = 0.05897 -0.01087 -0.01043 0.01492 AFIX 137 H6A 2 -0.061594 0.451505 0.134299 11.00000 -1.50000 H6B 2 -0.104911 0.360578 0.080358 11.00000 -1.50000 H6C 2 -0.019640 0.430104 0.045232 11.00000 -1.50000 AFIX 0 C7 1 0.046989 0.290007 0.215735 11.00000 0.04479 0.07760 = 0.07616 0.01527 0.01297 -0.00047 AFIX 137 H7A 2 0.071609 0.229571 0.200946 11.00000 -1.50000 H7B 2 -0.038419 0.289331 0.215602 11.00000 -1.50000 H7C 2 0.093632 0.307415 0.274533 11.00000 -1.50000 AFIX 0 C8 1 0.452662 0.284292 0.150617 11.00000 0.04188 0.03353 = 0.03411 -0.00140 0.00211 -0.00475 AFIX 43 H8 2 0.411067 0.242145 0.108353 11.00000 -1.20000 AFIX 0 C9 1 0.578271 0.291629 0.167133 11.00000 0.03931 0.03367 = 0.02839 -0.00325 0.01202 -0.00106 C10 1 0.648817 0.225613 0.123200 11.00000 0.04553 0.03156 = 0.03348 0.00208 0.01477 -0.00054 C11 1 0.639414 0.356889 0.228857 11.00000 0.03174 0.03680 = 0.03074 -0.00243 0.00911 -0.00093 AFIX 43 H11 2 0.724132 0.361467 0.240303 11.00000 -1.20000 AFIX 0 C12 1 0.931558 0.523976 0.601784 11.00000 0.05214 0.04162 = 0.04273 0.01055 0.02504 -0.00350 AFIX 43 H12 2 0.983755 0.557585 0.574663 11.00000 -1.20000 AFIX 0 C13 1 0.982032 0.478553 0.679814 11.00000 0.04593 0.04334 = 0.04180 0.00593 0.02101 -0.00485 AFIX 43 H13 2 1.065719 0.482183 0.704535 11.00000 -1.20000 AFIX 0 C14 1 0.906938 0.426114 0.722831 11.00000 0.05317 0.02654 = 0.03127 -0.00019 0.01674 0.00029 C15 1 0.916471 0.323445 0.857650 11.00000 0.05809 0.03041 = 0.02495 -0.00116 0.01219 -0.00509 C16 1 0.798439 0.327479 0.868788 11.00000 0.05872 0.03567 = 0.03054 0.00456 0.00959 -0.00026 AFIX 43 H16 2 0.743752 0.371028 0.837599 11.00000 -1.20000 AFIX 0 C17 1 0.762526 0.266005 0.926858 11.00000 0.05132 0.04011 = 0.03351 0.00730 0.00884 -0.00449 AFIX 43 H17 2 0.682131 0.269181 0.932704 11.00000 -1.20000 AFIX 0 C18 1 0.950891 0.202038 0.967004 11.00000 0.06561 0.03429 = 0.04036 0.00772 0.01773 0.01521 AFIX 43 H18 2 1.004311 0.159659 1.001410 11.00000 -1.20000 AFIX 0 C19 1 0.995921 0.259636 0.911640 11.00000 0.05685 0.04111 = 0.03981 0.00364 0.02249 0.00725 AFIX 43 H19 2 1.077847 0.256815 0.909575 11.00000 -1.20000 AFIX 0 C20 1 0.783675 0.423815 0.680844 11.00000 0.05789 0.04084 = 0.03589 0.00608 0.01669 -0.01379 AFIX 43 H20 2 0.729663 0.389357 0.705490 11.00000 -1.20000 AFIX 0 C21 1 0.741852 0.472819 0.602536 11.00000 0.04902 0.03921 = 0.03597 0.00280 0.00982 -0.01132 AFIX 43 H21 2 0.658501 0.470415 0.576267 11.00000 -1.20000 AFIX 0 PART -1 O6 5 1.210182 0.365611 0.830351 10.50000 0.13366 0.10762 = 0.10962 -0.00288 0.03134 0.00073 PART 1 O7 5 0.347001 0.202055 -0.069212 10.50000 0.08503 0.07457 = 0.08355 -0.03176 -0.03369 0.02289 AFIX 3 H7D 2 0.414831 0.198915 -0.032112 10.50000 -1.50000 H7E 2 0.317801 0.146795 -0.086502 10.50000 -1.50000 AFIX 0 PART -1 C23 1 1.493459 0.454610 0.945196 10.50000 0.16638 0.20553 = 0.21088 0.08675 0.01756 -0.06399 AFIX 3 H23A 2 1.466619 0.517120 0.949026 10.50000 -1.50000 H23B 2 1.561309 0.453770 0.916886 10.50000 -1.50000 H23C 2 1.518269 0.428940 1.004746 10.50000 -1.50000 AFIX 0 N5 4 1.406006 0.402416 0.899380 10.50000 0.18957 0.19285 = 0.17870 0.02987 0.03080 0.00318 C22 1 1.276712 0.429630 0.868280 10.50000 0.16751 0.16937 = 0.16115 0.02015 0.03963 0.00238 AFIX 43 H22 2 1.247808 0.488525 0.876167 10.50000 -1.20000 AFIX 0 C24 1 1.423796 0.308654 0.879183 10.50000 0.23343 0.24946 = 0.21924 -0.03621 0.03397 0.06738 AFIX 137 H24A 2 1.509290 0.297487 0.884281 10.50000 -1.50000 H24B 2 1.379160 0.295245 0.818744 10.50000 -1.50000 H24C 2 1.394999 0.269661 0.920830 10.50000 -1.50000 AFIX 0 PART 1 O8 5 1.236210 0.381214 0.833076 10.50000 0.09983 0.19239 = 0.03429 0.01991 0.01257 -0.05450 AFIX 3 H8A 2 1.283550 0.349024 0.876365 10.50000 -1.50000 H8B 2 1.255520 0.363564 0.785015 10.50000 -1.50000 AFIX 0 HKLF 4 REM mo_0322_3_P 1 21/n 1 R = 0.08 REM wR2 = 0.1495, GooF = S = 1.036, Restrained GooF = 1.059 for all data REM R1 = 0.0531 for 3216 Fo > 4sig(Fo) and 0.0898 for all 4711 data REM 355 parameters refined using 64 restraints END WGHT 0.0739 2.1454 REM Highest difference peak 0.759, deepest hole -0.421, 1-sigma level 0.076 Q1 1 1.5141 0.4053 0.8930 11.00000 0.05 0.76 Q2 1 0.2434 0.4007 0.1073 11.00000 0.05 0.42 Q3 1 1.4087 0.4412 0.9045 11.00000 0.05 0.39 Q4 1 0.3574 0.1846 -0.1000 11.00000 0.05 0.37 Q5 1 -0.0158 0.4859 0.0976 11.00000 0.05 0.36 ; _shelx_res_checksum 67755 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co Co1 0.73927(5) 0.60696(3) 0.44875(3) 0.03359(18) Uani d 1 . . S S1 0.21293(14) 0.44589(10) 0.06254(10) 0.0733(4) Uani d 1 . . O O1 0.5793(2) 0.53436(19) 0.38364(19) 0.0461(7) Uani d 1 . . O O2 0.7529(3) 0.4927(2) 0.3548(2) 0.0535(8) Uani d 1 . . O O3 0.2652(2) 0.32239(19) 0.19296(19) 0.0456(7) Uani d 1 . . O O4 0.5950(3) 0.18067(18) 0.05399(18) 0.0460(7) Uani d 1 . . O O5 0.7602(3) 0.2134(2) 0.15532(19) 0.0510(8) Uani d 1 . . N N1 0.0682(3) 0.3554(2) 0.1501(2) 0.0469(9) Uani d 1 . . N N2 0.8119(3) 0.5239(2) 0.5610(2) 0.0372(7) Uani d 1 . . N N3 0.9644(3) 0.3791(2) 0.8000(2) 0.0412(8) Uani d 1 . . H H3 1.042657 0.385181 0.814726 0.049 Uiso calc 1 . . N N4 0.8350(3) 0.2025(2) 0.9750(2) 0.0393(8) Uani d 1 . . C C1 0.6393(4) 0.4844(2) 0.3406(2) 0.0349(8) Uani d 1 . . C C2 0.5745(3) 0.4151(2) 0.2733(2) 0.0327(8) Uani d 1 . . C C3 0.4479(4) 0.4062(2) 0.2574(3) 0.0366(9) Uani d 1 . . H H3A 0.403355 0.444495 0.286860 0.044 Uiso calc 1 . . C C4 0.3893(3) 0.3402(3) 0.1975(3) 0.0372(9) Uani d 1 . . C C5 0.1790(4) 0.3741(3) 0.1362(3) 0.0440(10) Uani d 1 . . C C6 -0.0385(4) 0.4035(3) 0.0981(3) 0.0567(12) Uani d 1 . . H H6A -0.061594 0.451505 0.134299 0.085 Uiso calc 1 . . H H6B -0.104911 0.360578 0.080358 0.085 Uiso calc 1 . . H H6C -0.019640 0.430104 0.045232 0.085 Uiso calc 1 . . C C7 0.0470(4) 0.2900(4) 0.2157(4) 0.0664(14) Uani d 1 . . H H7A 0.071609 0.229571 0.200946 0.100 Uiso calc 1 . . H H7B -0.038419 0.289331 0.215602 0.100 Uiso calc 1 . . H H7C 0.093632 0.307415 0.274533 0.100 Uiso calc 1 . . C C8 0.4527(4) 0.2843(3) 0.1506(3) 0.0376(9) Uani d 1 . . H H8 0.411067 0.242145 0.108353 0.045 Uiso calc 1 . . C C9 0.5783(3) 0.2916(2) 0.1671(2) 0.0331(8) Uani d 1 . . C C10 0.6488(4) 0.2256(2) 0.1232(2) 0.0359(9) Uani d 1 . . C C11 0.6394(3) 0.3569(2) 0.2289(2) 0.0328(8) Uani d 1 . . H H11 0.724132 0.361467 0.240303 0.039 Uiso calc 1 . . C C12 0.9316(4) 0.5240(3) 0.6018(3) 0.0432(10) Uani d 1 . . H H12 0.983755 0.557585 0.574663 0.052 Uiso calc 1 . . C C13 0.9820(4) 0.4786(3) 0.6798(3) 0.0419(9) Uani d 1 . . H H13 1.065719 0.482183 0.704535 0.050 Uiso calc 1 . . C C14 0.9069(4) 0.4261(2) 0.7228(2) 0.0359(9) Uani d 1 . . C C15 0.9165(4) 0.3234(2) 0.8576(2) 0.0374(9) Uani d 1 . . C C16 0.7984(4) 0.3275(3) 0.8688(2) 0.0418(9) Uani d 1 . . H H16 0.743752 0.371028 0.837599 0.050 Uiso calc 1 . . C C17 0.7625(4) 0.2660(3) 0.9269(2) 0.0418(9) Uani d 1 . . H H17 0.682131 0.269181 0.932704 0.050 Uiso calc 1 . . C C18 0.9509(4) 0.2020(3) 0.9670(3) 0.0459(10) Uani d 1 . . H H18 1.004311 0.159659 1.001410 0.055 Uiso calc 1 . . C C19 0.9959(4) 0.2596(3) 0.9116(3) 0.0441(10) Uani d 1 . . H H19 1.077847 0.256815 0.909575 0.053 Uiso calc 1 . . C C20 0.7837(4) 0.4238(3) 0.6808(3) 0.0439(10) Uani d 1 . . H H20 0.729663 0.389357 0.705490 0.053 Uiso calc 1 . . C C21 0.7419(4) 0.4728(3) 0.6025(3) 0.0414(9) Uani d 1 . . H H21 0.658501 0.470415 0.576267 0.050 Uiso calc 1 . . O O6 1.2102(17) 0.3656(14) 0.8304(14) 0.116(6) Uani d 0.5 A -1 O O7 0.3470(7) 0.2021(5) -0.0692(5) 0.090(3) Uani d 0.5 B 1 H H7D 0.414831 0.198915 -0.032112 0.135 Uiso d 0.5 B 1 H H7E 0.317801 0.146795 -0.086502 0.135 Uiso d 0.5 B 1 C C23 1.4935(17) 0.4546(13) 0.9452(13) 0.199(8) Uani d 0.5 A -1 H H23A 1.466619 0.517120 0.949026 0.298 Uiso d 0.5 A -1 H H23B 1.561309 0.453770 0.916886 0.298 Uiso d 0.5 A -1 H H23C 1.518269 0.428940 1.004746 0.298 Uiso d 0.5 A -1 N N5 1.4060(15) 0.4024(12) 0.8994(13) 0.189(6) Uani d 0.5 A -1 C C22 1.2767(15) 0.4296(13) 0.8683(16) 0.166(6) Uani d 0.5 A -1 H H22 1.247808 0.488525 0.876167 0.199 Uiso calc 0.5 A -1 C C24 1.424(2) 0.3087(13) 0.8792(19) 0.237(9) Uani d 0.5 A -1 H H24A 1.509290 0.297487 0.884281 0.356 Uiso calc 0.5 A -1 H H24B 1.379160 0.295245 0.818744 0.356 Uiso calc 0.5 A -1 H H24C 1.394999 0.269661 0.920830 0.356 Uiso calc 0.5 A -1 O O8 1.2362(15) 0.3812(15) 0.8331(9) 0.109(6) Uani d 0.5 A 1 H H8A 1.283550 0.349024 0.876365 0.164 Uiso d 0.5 A 1 H H8B 1.255520 0.363564 0.785015 0.164 Uiso d 0.5 A 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Co1 0.0496(3) 0.0268(3) 0.0268(3) -0.0025(2) 0.0137(2) -0.0018(2) S1 0.0705(9) 0.0671(9) 0.0750(9) 0.0037(7) 0.0023(7) 0.0295(7) O1 0.0447(16) 0.0435(16) 0.0524(17) -0.0023(13) 0.0158(14) -0.0207(13) O2 0.0431(18) 0.071(2) 0.0508(18) -0.0167(15) 0.0189(14) -0.0265(15) O3 0.0296(15) 0.0517(16) 0.0523(17) 0.0015(12) 0.0033(13) 0.0137(13) O4 0.0552(18) 0.0390(15) 0.0452(16) -0.0038(13) 0.0146(14) -0.0154(13) O5 0.0505(19) 0.0645(19) 0.0398(16) 0.0128(15) 0.0140(14) -0.0109(14) N1 0.035(2) 0.049(2) 0.049(2) 0.0063(16) -0.0050(16) -0.0034(17) N2 0.053(2) 0.0305(16) 0.0321(16) -0.0019(15) 0.0178(15) 0.0024(13) N3 0.055(2) 0.0375(18) 0.0328(17) -0.0046(15) 0.0133(15) 0.0085(14) N4 0.062(2) 0.0301(16) 0.0278(16) -0.0028(15) 0.0155(15) 0.0016(13) C1 0.044(2) 0.0323(19) 0.0303(19) -0.0057(17) 0.0131(17) -0.0028(15) C2 0.035(2) 0.0322(19) 0.0317(19) -0.0007(15) 0.0100(16) -0.0002(15) C3 0.040(2) 0.033(2) 0.039(2) 0.0070(16) 0.0119(17) -0.0028(16) C4 0.034(2) 0.039(2) 0.037(2) 0.0013(17) 0.0052(17) 0.0078(17) C5 0.046(3) 0.037(2) 0.040(2) 0.0086(18) -0.0076(19) -0.0092(17) C6 0.043(3) 0.057(3) 0.059(3) 0.015(2) -0.010(2) -0.011(2) C7 0.045(3) 0.078(3) 0.076(3) 0.000(2) 0.013(2) 0.015(3) C8 0.042(2) 0.034(2) 0.034(2) -0.0048(17) 0.0021(17) -0.0014(16) C9 0.039(2) 0.0337(19) 0.0284(18) -0.0011(16) 0.0120(16) -0.0033(15) C10 0.046(2) 0.0316(19) 0.033(2) -0.0005(17) 0.0148(18) 0.0021(16) C11 0.032(2) 0.0368(19) 0.0307(19) -0.0009(16) 0.0091(15) -0.0024(16) C12 0.052(3) 0.042(2) 0.043(2) -0.0035(19) 0.025(2) 0.0106(18) C13 0.046(2) 0.043(2) 0.042(2) -0.0049(18) 0.0210(19) 0.0059(18) C14 0.053(2) 0.0265(18) 0.0313(19) 0.0003(17) 0.0167(18) -0.0002(15) C15 0.058(3) 0.0304(19) 0.0250(18) -0.0051(18) 0.0122(17) -0.0012(15) C16 0.059(3) 0.036(2) 0.031(2) -0.0003(19) 0.0096(18) 0.0046(16) C17 0.051(3) 0.040(2) 0.034(2) -0.0045(19) 0.0088(18) 0.0073(17) C18 0.066(3) 0.034(2) 0.040(2) 0.015(2) 0.018(2) 0.0077(17) C19 0.057(3) 0.041(2) 0.040(2) 0.007(2) 0.022(2) 0.0036(18) C20 0.058(3) 0.041(2) 0.036(2) -0.014(2) 0.0167(19) 0.0061(17) C21 0.049(2) 0.039(2) 0.036(2) -0.0113(18) 0.0098(18) 0.0028(17) O6 0.134(10) 0.108(8) 0.110(9) 0.001(7) 0.031(7) -0.003(6) O7 0.085(6) 0.075(5) 0.084(5) 0.023(4) -0.034(4) -0.032(4) C23 0.166(13) 0.206(13) 0.211(14) -0.064(11) 0.018(11) 0.087(11) N5 0.190(8) 0.193(8) 0.179(8) 0.003(7) 0.031(7) 0.030(7) C22 0.168(9) 0.169(8) 0.161(8) 0.002(7) 0.040(7) 0.020(7) C24 0.233(14) 0.249(15) 0.219(14) 0.067(13) 0.034(12) -0.036(13) O8 0.100(9) 0.192(16) 0.034(5) -0.055(9) 0.013(5) 0.020(7) 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Co1 O2 . . 60.43(10) ? O1 Co1 O4 . 2_655 151.57(11) ? O1 Co1 O5 . 2_655 98.85(11) ? O1 Co1 C1 . . 30.50(11) ? O2 Co1 C1 . . 29.96(11) ? O4 Co1 O2 2_655 . 99.60(11) ? O4 Co1 O5 2_655 2_655 59.65(10) ? O4 Co1 C1 2_655 . 126.57(12) ? O5 Co1 O2 2_655 . 92.57(12) ? O5 Co1 C1 2_655 . 95.62(11) ? N2 Co1 O1 . . 102.95(12) ? N2 Co1 O2 . . 91.51(12) ? N2 Co1 O4 . 2_655 97.23(12) ? N2 Co1 O5 . 2_655 156.87(12) ? N2 Co1 N4 . 2_656 93.24(12) ? N2 Co1 C1 . . 99.22(12) ? N4 Co1 O1 2_656 . 100.46(12) ? N4 Co1 O2 2_656 . 160.89(13) ? N4 Co1 O4 2_656 2_655 98.15(12) ? N4 Co1 O5 2_656 2_655 90.30(11) ? N4 Co1 C1 2_656 . 130.93(14) ? C1 O1 Co1 . . 91.7(2) ? C1 O2 Co1 . . 87.8(2) ? C5 O3 C4 . . 118.8(3) ? C10 O4 Co1 . 2_645 91.3(2) ? C10 O5 Co1 . 2_645 89.3(2) ? C5 N1 C6 . . 119.9(4) ? C5 N1 C7 . . 123.6(3) ? C7 N1 C6 . . 116.4(4) ? C12 N2 Co1 . . 122.3(2) ? C21 N2 Co1 . . 122.8(3) ? C21 N2 C12 . . 114.6(3) ? C14 N3 H3 . . 114.8 ? C14 N3 C15 . . 130.5(4) ? C15 N3 H3 . . 114.8 ? C17 N4 Co1 . 2_646 119.2(3) ? C17 N4 C18 . . 116.0(3) ? C18 N4 Co1 . 2_646 124.7(3) ? O1 C1 Co1 . . 57.84(18) ? O1 C1 C2 . . 120.2(3) ? O2 C1 Co1 . . 62.2(2) ? O2 C1 O1 . . 120.0(3) ? O2 C1 C2 . . 119.8(3) ? C2 C1 Co1 . . 176.8(3) ? C3 C2 C1 . . 119.7(3) ? C11 C2 C1 . . 120.9(3) ? C11 C2 C3 . . 119.4(3) ? C2 C3 H3A . . 120.3 ? C4 C3 C2 . . 119.4(3) ? C4 C3 H3A . . 120.3 ? C3 C4 O3 . . 118.4(3) ? C3 C4 C8 . . 121.6(4) ? C8 C4 O3 . . 119.6(3) ? O3 C5 S1 . . 122.5(3) ? N1 C5 S1 . . 127.6(3) ? N1 C5 O3 . . 109.9(4) ? N1 C6 H6A . . 109.5 ? N1 C6 H6B . . 109.5 ? N1 C6 H6C . . 109.5 ? H6A C6 H6B . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? N1 C7 H7A . . 109.5 ? N1 C7 H7B . . 109.5 ? N1 C7 H7C . . 109.5 ? H7A C7 H7B . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C4 C8 H8 . . 120.3 ? C9 C8 C4 . . 119.4(3) ? C9 C8 H8 . . 120.3 ? C8 C9 C10 . . 119.8(3) ? C8 C9 C11 . . 119.8(3) ? C11 C9 C10 . . 120.3(3) ? O4 C10 C9 . . 120.0(4) ? O5 C10 O4 . . 119.7(4) ? O5 C10 C9 . . 120.3(3) ? C2 C11 C9 . . 120.4(3) ? C2 C11 H11 . . 119.8 ? C9 C11 H11 . . 119.8 ? N2 C12 H12 . . 117.6 ? N2 C12 C13 . . 124.9(4) ? C13 C12 H12 . . 117.6 ? C12 C13 H13 . . 120.2 ? C12 C13 C14 . . 119.6(4) ? C14 C13 H13 . . 120.2 ? N3 C14 C13 . . 116.7(4) ? N3 C14 C20 . . 126.9(4) ? C20 C14 C13 . . 116.3(4) ? N3 C15 C19 . . 117.5(4) ? C16 C15 N3 . . 125.5(4) ? C16 C15 C19 . . 117.0(3) ? C15 C16 H16 . . 120.5 ? C15 C16 C17 . . 119.1(4) ? C17 C16 H16 . . 120.5 ? N4 C17 C16 . . 124.5(4) ? N4 C17 H17 . . 117.8 ? C16 C17 H17 . . 117.8 ? N4 C18 H18 . . 117.9 ? N4 C18 C19 . . 124.3(4) ? C19 C18 H18 . . 117.9 ? C15 C19 H19 . . 120.5 ? C18 C19 C15 . . 119.0(4) ? C18 C19 H19 . . 120.5 ? C14 C20 H20 . . 120.3 ? C21 C20 C14 . . 119.5(4) ? C21 C20 H20 . . 120.3 ? N2 C21 C20 . . 125.1(4) ? N2 C21 H21 . . 117.5 ? C20 C21 H21 . . 117.5 ? H7D O7 H7E . . 111.7 ? H23A C23 H23B . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? N5 C23 H23A . . 111.7 ? N5 C23 H23B . . 109.3 ? N5 C23 H23C . . 107.3 ? C23 N5 C22 . . 125.5(15) ? C23 N5 C24 . . 122.9(15) ? C24 N5 C22 . . 111.4(13) ? O6 C22 N5 . . 113.0(15) ? O6 C22 H22 . . 123.5 ? N5 C22 H22 . . 123.5 ? O8 C22 O6 . . 10.1(19) ? O8 C22 N5 . . 107(2) ? O8 C22 H22 . . 128.6 ? N5 C24 H24A . . 109.5 ? N5 C24 H24B . . 109.5 ? N5 C24 H24C . . 109.5 ? H24A C24 H24B . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? C22 O8 H8A . . 80.7 ? C22 O8 H8B . . 122.1 ? H8A O8 H8B . . 104.8 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Co1 O1 . 2.119(3) ? Co1 O2 . 2.216(3) ? Co1 O4 2_655 2.156(3) ? Co1 O5 2_655 2.211(3) ? Co1 N2 . 2.094(3) ? Co1 N4 2_656 2.100(3) ? Co1 C1 . 2.502(4) ? S1 C5 . 1.638(5) ? O1 C1 . 1.271(4) ? O2 C1 . 1.251(5) ? O3 C4 . 1.404(4) ? O3 C5 . 1.363(4) ? O4 C10 . 1.266(4) ? O5 C10 . 1.247(5) ? N1 C5 . 1.339(6) ? N1 C6 . 1.451(5) ? N1 C7 . 1.437(6) ? N2 C12 . 1.345(5) ? N2 C21 . 1.341(5) ? N3 H3 . 0.8600 ? N3 C14 . 1.382(5) ? N3 C15 . 1.390(5) ? N4 C17 . 1.330(5) ? N4 C18 . 1.337(5) ? C1 C2 . 1.496(5) ? C2 C3 . 1.393(5) ? C2 C11 . 1.390(5) ? C3 H3A . 0.9300 ? C3 C4 . 1.379(5) ? C4 C8 . 1.381(5) ? C6 H6A . 0.9600 ? C6 H6B . 0.9600 ? C6 H6C . 0.9600 ? C7 H7A . 0.9600 ? C7 H7B . 0.9600 ? C7 H7C . 0.9600 ? C8 H8 . 0.9300 ? C8 C9 . 1.380(5) ? C9 C10 . 1.496(5) ? C9 C11 . 1.395(5) ? C11 H11 . 0.9300 ? C12 H12 . 0.9300 ? C12 C13 . 1.361(5) ? C13 H13 . 0.9300 ? C13 C14 . 1.406(5) ? C14 C20 . 1.385(6) ? C15 C16 . 1.378(6) ? C15 C19 . 1.409(5) ? C16 H16 . 0.9300 ? C16 C17 . 1.380(5) ? C17 H17 . 0.9300 ? C18 H18 . 0.9300 ? C18 C19 . 1.364(6) ? C19 H19 . 0.9300 ? C20 H20 . 0.9300 ? C20 C21 . 1.373(5) ? C21 H21 . 0.9300 ? O6 C22 . 1.245(17) ? O7 H7D . 0.8380 ? O7 H7E . 0.8812 ? C23 H23A . 0.9598 ? C23 H23B . 0.9600 ? C23 H23C . 0.9595 ? C23 N5 . 1.306(14) ? N5 C22 . 1.474(15) ? N5 C24 . 1.416(15) ? C22 H22 . 0.9300 ? C22 O8 . 0.93(3) ? C24 H24A . 0.9600 ? C24 H24B . 0.9600 ? C24 H24C . 0.9600 ? O8 H8A . 0.8784 ? O8 H8B . 0.8500 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N3 H3 O6 . 0.86 1.86 2.700(19) 163.5 yes N3 H3 O8 . 0.86 2.13 2.979(17) 169.5 yes C13 H13 O2 3_766 0.93 2.44 3.174(5) 135.4 yes O7 H7D O4 . 0.84 2.16 2.992(7) 174.0 yes O7 H7E O2 4_565 0.88 2.26 3.136(7) 173.1 yes O8 H8A O7 1_656 0.88 2.33 3.10(2) 146.3 yes O8 H8B O5 4_666 0.85 2.28 3.102(17) 162.9 yes 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Co1 O1 C1 O2 . . . . 3.4(4) ? Co1 O1 C1 C2 . . . . -177.0(3) ? Co1 O2 C1 O1 . . . . -3.2(4) ? Co1 O2 C1 C2 . . . . 177.2(3) ? Co1 O4 C10 O5 2_645 . . . 2.2(4) ? Co1 O4 C10 C9 2_645 . . . -176.6(3) ? Co1 O5 C10 O4 2_645 . . . -2.1(4) ? Co1 O5 C10 C9 2_645 . . . 176.7(3) ? Co1 N2 C12 C13 . . . . 173.3(3) ? Co1 N2 C21 C20 . . . . -173.9(3) ? Co1 N4 C17 C16 2_646 . . . -174.6(3) ? Co1 N4 C18 C19 2_646 . . . 174.4(3) ? O1 C1 C2 C3 . . . . 0.7(5) ? O1 C1 C2 C11 . . . . -176.9(3) ? O2 C1 C2 C3 . . . . -179.7(4) ? O2 C1 C2 C11 . . . . 2.7(5) ? O3 C4 C8 C9 . . . . -169.0(3) ? N2 C12 C13 C14 . . . . 0.6(6) ? N3 C14 C20 C21 . . . . -178.0(4) ? N3 C15 C16 C17 . . . . 178.3(4) ? N3 C15 C19 C18 . . . . -178.0(4) ? N4 C18 C19 C15 . . . . -1.1(6) ? C1 C2 C3 C4 . . . . -177.9(3) ? C1 C2 C11 C9 . . . . 179.1(3) ? C2 C3 C4 O3 . . . . 170.1(3) ? C2 C3 C4 C8 . . . . -2.0(6) ? C3 C2 C11 C9 . . . . 1.5(5) ? C3 C4 C8 C9 . . . . 3.1(6) ? C4 O3 C5 S1 . . . . 8.9(5) ? C4 O3 C5 N1 . . . . -171.9(3) ? C4 C8 C9 C10 . . . . 174.4(3) ? C4 C8 C9 C11 . . . . -1.8(5) ? C5 O3 C4 C3 . . . . 87.8(4) ? C5 O3 C4 C8 . . . . -100.0(4) ? C6 N1 C5 S1 . . . . -1.8(6) ? C6 N1 C5 O3 . . . . 179.0(3) ? C7 N1 C5 S1 . . . . 179.1(4) ? C7 N1 C5 O3 . . . . -0.1(6) ? C8 C9 C10 O4 . . . . 19.2(5) ? C8 C9 C10 O5 . . . . -159.6(4) ? C8 C9 C11 C2 . . . . -0.5(5) ? C10 C9 C11 C2 . . . . -176.6(3) ? C11 C2 C3 C4 . . . . -0.3(5) ? C11 C9 C10 O4 . . . . -164.7(3) ? C11 C9 C10 O5 . . . . 16.5(5) ? C12 N2 C21 C20 . . . . 0.5(6) ? C12 C13 C14 N3 . . . . 177.7(4) ? C12 C13 C14 C20 . . . . 0.6(6) ? C13 C14 C20 C21 . . . . -1.2(6) ? C14 N3 C15 C16 . . . . -23.9(6) ? C14 N3 C15 C19 . . . . 158.4(4) ? C14 C20 C21 N2 . . . . 0.6(6) ? C15 N3 C14 C13 . . . . 178.9(4) ? C15 N3 C14 C20 . . . . -4.3(6) ? C15 C16 C17 N4 . . . . 1.0(6) ? C16 C15 C19 C18 . . . . 4.1(6) ? C17 N4 C18 C19 . . . . -2.0(6) ? C18 N4 C17 C16 . . . . 2.0(6) ? C19 C15 C16 C17 . . . . -4.0(5) ? C21 N2 C12 C13 . . . . -1.2(6) ? C23 N5 C22 O6 . . . . -176(2) ? C23 N5 C22 O8 . . . . 175(2) ? C24 N5 C22 O6 . . . . -1(3) ? C24 N5 C22 O8 . . . . -9(3) ?