#------------------------------------------------------------------------------ #$Date: 2020-05-05 15:32:56 +0300 (Tue, 05 May 2020) $ #$Revision: 251537 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/77/1557723.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1557723 loop_ _publ_author_name 'Weder, Nicola' 'Probst, Benjamin' 'S\'every, Laurent' 'Fern\'andez-Ter\'an, Ricardo J.' 'Beckord, Jan' 'Blacque, Olivier' 'Tilley, S. David' 'Hamm, Peter' 'Osterwalder, J\"urg' 'Alberto, Roger' _publ_section_title ; Mechanistic insights into photocatalysis and over two days of stable H2 generation in electrocatalysis by a molecular cobalt catalyst immobilized on TiO2 ; _journal_issue 8 _journal_name_full 'Catalysis Science & Technology' _journal_page_first 2549 _journal_paper_doi 10.1039/D0CY00330A _journal_volume 10 _journal_year 2020 _chemical_formula_moiety 'C24 H20 Br2 Co N4 O2, 0.5(C2 H4 O6 S2), C2 H6 O S, H2 O' _chemical_formula_sum 'C27 H30 Br2 Co N4 O7 S2' _chemical_formula_weight 805.42 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2017-11-20 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-10-08 deposited with the CCDC. 2020-03-16 downloaded from the CCDC. ; _cell_angle_alpha 107.981(3) _cell_angle_beta 96.136(3) _cell_angle_gamma 103.720(3) _cell_formula_units_Z 2 _cell_length_a 8.1545(3) _cell_length_b 11.7917(5) _cell_length_c 16.3115(4) _cell_measurement_reflns_used 10672 _cell_measurement_temperature 160(1) _cell_measurement_theta_max 78.4 _cell_measurement_theta_min 2.9 _cell_volume 1421.47(10) _computing_cell_refinement 'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.39.13a (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015b)' _computing_structure_solution 'ShelXT (Sheldrick, 2015a)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 160(1) _diffrn_detector 'CCD plate' _diffrn_detector_type 'Pilatus 200K' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -73.00 21.00 0.50 8.00 -- -51.81 77.00 0.00 188 2 \w -77.00 -11.00 0.50 32.00 -- -86.25 45.00 -30.00 132 3 \w -90.00 -10.00 0.50 32.00 -- -86.25 111.00 60.00 160 4 \w -95.00 -9.00 0.50 8.00 -- -51.81 125.00 120.00 172 5 \w -131.00 -43.00 0.50 8.00 -- -51.81 -19.00 120.00 176 6 \w -127.00 -82.00 0.50 8.00 -- -51.81 -99.00 90.00 90 7 \w -127.00 -82.00 0.50 8.00 -- -51.81 -99.00 0.00 90 8 \w -127.00 -82.00 0.50 8.00 -- -51.81 -99.00 -60.00 90 9 \w -124.00 -38.00 0.50 8.00 -- -51.81 -57.00-150.00 172 10 \w -126.00 -70.00 0.50 8.00 -- -51.81-125.00-180.00 112 11 \w 35.00 129.00 0.50 32.00 -- 107.75 -77.00 90.00 188 12 \w 72.00 105.00 0.50 32.00 -- 107.75 -94.00 90.00 66 13 \w 71.00 113.00 0.50 32.00 -- 107.75-111.00 60.00 84 14 \w 57.00 106.00 0.50 32.00 -- 107.75-111.00 90.00 98 15 \w 38.00 69.00 0.50 32.00 -- 107.75 -94.00 90.00 62 16 \w 32.00 77.00 0.50 32.00 -- 107.75 -45.00 150.00 90 17 \w 41.00 67.00 0.50 32.00 -- 107.75 -30.00 90.00 52 18 \w 45.00 70.00 0.50 32.00 -- 107.75 -15.00 30.00 50 19 \w 83.00 117.00 0.50 32.00 -- 107.75 -15.00 30.00 68 20 \w 106.00 174.00 0.50 32.00 -- 107.75 15.00 30.00 136 21 \w 121.00 171.00 0.50 32.00 -- 107.75 30.00 60.00 100 22 \w 98.00 178.00 0.50 32.00 -- 107.75 15.00 -60.00 160 23 \w 83.00 117.00 0.50 32.00 -- 107.75 -61.00 -60.00 68 24 \w 82.00 114.00 0.50 32.00 -- 107.75-111.00 -90.00 64 25 \w 69.00 115.00 0.50 32.00 -- 107.75-111.00-180.00 92 26 \w 45.00 127.00 0.50 32.00 -- 107.75 -77.00 -60.00 164 27 \w 48.00 97.00 0.50 32.00 -- 107.75 -94.00 -90.00 98 28 \w 46.00 108.00 0.50 32.00 -- 107.75 -94.00 -60.00 124 29 \w 38.00 65.00 0.50 32.00 -- 107.75 -61.00 -60.00 54 30 \w 34.00 61.00 0.50 32.00 -- 107.75 -30.00-120.00 54 31 \w 34.00 74.00 0.50 32.00 -- 107.75 -45.00 -60.00 80 32 \w 32.00 69.00 0.50 32.00 -- 107.75 -30.00 0.00 74 33 \w 33.00 66.00 0.50 32.00 -- 107.75 -30.00 -60.00 66 34 \w 34.00 66.00 0.50 32.00 -- 107.75 -30.00 -30.00 64 35 \w 33.00 71.00 0.50 32.00 -- 107.75 -94.00-120.00 76 36 \w 32.00 102.00 0.50 32.00 -- 107.75 -94.00-180.00 140 37 \w 38.00 79.00 0.50 32.00 -- 107.75-111.00 -90.00 82 38 \w 35.00 72.00 0.50 32.00 -- 107.75 -45.00 60.00 74 39 \w 32.00 71.00 0.50 32.00 -- 107.75 -45.00 90.00 78 40 \w 36.00 62.00 0.50 32.00 -- 107.75 -30.00 120.00 52 41 \w 35.00 66.00 0.50 32.00 -- 107.75 -30.00 150.00 62 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, Pilatus 200K' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0183580000 _diffrn_orient_matrix_UB_12 0.1329698000 _diffrn_orient_matrix_UB_13 0.0295080000 _diffrn_orient_matrix_UB_21 -0.1876882000 _diffrn_orient_matrix_UB_22 -0.0512202000 _diffrn_orient_matrix_UB_23 0.0077570000 _diffrn_orient_matrix_UB_31 0.0612257000 _diffrn_orient_matrix_UB_32 0.0154552000 _diffrn_orient_matrix_UB_33 0.0965306000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0394 _diffrn_reflns_av_unetI/netI 0.0366 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 21345 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.504 _diffrn_reflns_theta_min 2.904 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 9.878 _exptl_absorpt_correction_T_max 0.877 _exptl_absorpt_correction_T_min 0.477 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.13a (Rigaku Oxford Diffraction, 2015) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.882 _exptl_crystal_description needle _exptl_crystal_F_000 810 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent' _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 1.287 _refine_diff_density_min -0.724 _refine_diff_density_rms 0.103 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 400 _refine_ls_number_reflns 5801 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.030 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0412 _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^)+(0.0510P)^2^+3.0667P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1032 _refine_ls_wR_factor_ref 0.1077 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4879 _reflns_number_total 5801 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0cy00330a2.cif _cod_data_source_block Co(III)-9 _cod_depositor_comments 'Adding full bibliography for 1557722--1557724.cif.' _cod_original_cell_volume 1421.47(9) _cod_database_code 1557723 _shelx_shelxl_version_number 2017/1 _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_estimated_absorpt_t_max 0.827 _shelx_estimated_absorpt_t_min 0.410 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All C(H,H,H,H,H) groups, All O(H) groups 2. Restrained distances O7-H7A 0.82 with sigma of 0.01 O7-H7B 0.82 with sigma of 0.01 3.a Secondary CH2 refined with riding coordinates: C25(H25A,H25B) 3.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C7(H7), C8(H8), C9(H9), C14(H14), C15(H15), C16(H16), C19(H19), C20(H20), C21(H21) 3.c Idealised Me refined as rotating group: C12(H12A,H12B,H12C), C24(H24A,H24B,H24C), C26(H26A,H26B,H26C), C27(H27A,H27B, H27C) 3.d Idealised tetrahedral OH refined as rotating group: O1(H1), O2(H2A) ; _shelx_res_file ; TITL nw1711_a.res in P-1 nw1711.res created by SHELXL-2017/1 at 10:43:26 on 20-Nov-2017 CELL 1.54184 8.1545 11.7917 16.3115 107.981 96.136 103.72 ZERR 2 0.0003 0.0005 0.0004 0.003 0.003 0.003 LATT 1 SFAC C H Br Co N O S UNIT 54 60 4 2 8 14 4 EQIV $1 1-X,1-Y,-Z EQIV $2 1-X,-Y,-Z DFIX 0.82 0.01 O7 H7a DFIX 0.82 0.01 O7 H7b L.S. 10 PLAN 30 SIZE 0.02 0.03 0.11 HTAB O1 O4 HTAB O2 O7_$1 HTAB O7 O5 HTAB O7 O5_$2 BOND $H fmap 2 acta REM REM REM WGHT 0.051000 3.066700 FVAR 0.69568 BR1 3 0.704211 0.607745 0.376864 11.00000 0.02542 0.03532 = 0.02737 0.01059 0.00733 0.01254 BR2 3 0.278461 0.341553 0.120309 11.00000 0.02271 0.02961 = 0.02718 0.01133 0.00675 0.01016 C1 1 0.676457 0.625230 0.154811 11.00000 0.01693 0.02503 = 0.01892 0.00982 0.00306 0.00590 C2 1 0.819301 0.660925 0.119347 11.00000 0.02140 0.02979 = 0.02723 0.01536 0.00814 0.00638 AFIX 43 H2 2 0.839459 0.733610 0.106006 11.00000 -1.20000 AFIX 0 C3 1 0.931542 0.588857 0.103816 11.00000 0.01809 0.03737 = 0.03157 0.01760 0.01153 0.00745 AFIX 43 H3 2 1.027561 0.612708 0.080343 11.00000 -1.20000 AFIX 0 C4 1 0.899001 0.480509 0.123718 11.00000 0.01993 0.03106 = 0.02807 0.01196 0.01099 0.01283 AFIX 43 H4 2 0.970276 0.428858 0.112088 11.00000 -1.20000 AFIX 0 C5 1 0.758332 0.451247 0.161183 11.00000 0.01759 0.02659 = 0.01983 0.00968 0.00617 0.00926 C6 1 0.716743 0.342728 0.189484 11.00000 0.01996 0.02674 = 0.02195 0.01183 0.00800 0.01187 C7 1 0.796237 0.249353 0.168248 11.00000 0.02877 0.03479 = 0.03047 0.01607 0.01725 0.01976 AFIX 43 H7 2 0.878957 0.251367 0.133234 11.00000 -1.20000 AFIX 0 C8 1 0.750352 0.152504 0.200137 11.00000 0.03866 0.03022 = 0.03580 0.01524 0.01455 0.02317 AFIX 43 H8 2 0.800521 0.087647 0.186184 11.00000 -1.20000 AFIX 0 C9 1 0.629025 0.153968 0.252914 11.00000 0.03218 0.02877 = 0.02817 0.01637 0.00903 0.01413 AFIX 43 H9 2 0.598028 0.090025 0.275293 11.00000 -1.20000 AFIX 0 C10 1 0.552977 0.249788 0.272868 11.00000 0.02379 0.02504 = 0.01946 0.01227 0.00619 0.01058 C11 1 0.439215 0.254234 0.341345 11.00000 0.02415 0.02910 = 0.02573 0.01486 0.00950 0.01146 C12 1 0.559731 0.313182 0.432054 11.00000 0.02706 0.04119 = 0.02475 0.01740 0.00601 0.01436 AFIX 137 H12A 2 0.492620 0.315850 0.477154 11.00000 -1.50000 H12B 2 0.624746 0.396172 0.439323 11.00000 -1.50000 H12C 2 0.637006 0.264297 0.436270 11.00000 -1.50000 AFIX 0 C13 1 0.307145 0.327032 0.343852 11.00000 0.01964 0.02872 = 0.02188 0.01358 0.00670 0.00762 C14 1 0.168311 0.294750 0.383387 11.00000 0.02402 0.03976 = 0.03010 0.02118 0.01060 0.00944 AFIX 43 H14 2 0.150411 0.223896 0.398954 11.00000 -1.20000 AFIX 0 C15 1 0.057103 0.367817 0.399525 11.00000 0.02164 0.04660 = 0.03112 0.01875 0.01391 0.01226 AFIX 43 H15 2 -0.036653 0.345961 0.425038 11.00000 -1.20000 AFIX 0 C16 1 0.087664 0.474074 0.377062 11.00000 0.02237 0.04401 = 0.02832 0.01744 0.01317 0.01754 AFIX 43 H16 2 0.016600 0.525907 0.388499 11.00000 -1.20000 AFIX 0 C17 1 0.225622 0.501256 0.337418 11.00000 0.02063 0.03153 = 0.02055 0.01200 0.00806 0.01166 C18 1 0.267326 0.609932 0.309212 11.00000 0.02105 0.02714 = 0.02266 0.00920 0.00695 0.01190 C19 1 0.191340 0.705485 0.332394 11.00000 0.02925 0.03544 = 0.03245 0.01364 0.01672 0.01861 AFIX 43 H19 2 0.110758 0.704971 0.368647 11.00000 -1.20000 AFIX 0 C20 1 0.238031 0.801421 0.300431 11.00000 0.03738 0.03219 = 0.03901 0.01370 0.01594 0.02365 AFIX 43 H20 2 0.189892 0.867293 0.315277 11.00000 -1.20000 AFIX 0 C21 1 0.356889 0.798820 0.246187 11.00000 0.03212 0.02614 = 0.03220 0.01242 0.01044 0.01599 AFIX 43 H21 2 0.387964 0.862734 0.223788 11.00000 -1.20000 AFIX 0 C22 1 0.430247 0.701329 0.224907 11.00000 0.02090 0.02384 = 0.02447 0.00971 0.00632 0.01056 C23 1 0.541251 0.695890 0.154780 11.00000 0.02132 0.01991 = 0.02588 0.01126 0.00763 0.00674 C24 1 0.416462 0.629312 0.065402 11.00000 0.02641 0.03630 = 0.02522 0.01480 0.00617 0.01564 AFIX 137 H24A 2 0.331576 0.672532 0.061347 11.00000 -1.50000 H24B 2 0.360538 0.545362 0.060289 11.00000 -1.50000 H24C 2 0.479527 0.628565 0.018889 11.00000 -1.50000 AFIX 0 CO1 4 0.490803 0.475356 0.248546 11.00000 0.01469 0.02146 = 0.01855 0.00982 0.00776 0.00950 N1 5 0.650633 0.523918 0.178448 11.00000 0.01632 0.02265 = 0.01860 0.00973 0.00566 0.00900 N2 5 0.594116 0.342817 0.239857 11.00000 0.01678 0.02489 = 0.01898 0.00986 0.00579 0.00972 N3 5 0.332003 0.428201 0.319373 11.00000 0.01557 0.02786 = 0.01882 0.00888 0.00551 0.01032 N4 5 0.388016 0.608883 0.257658 11.00000 0.01678 0.02191 = 0.01928 0.00867 0.00581 0.00845 O1 6 0.355054 0.130241 0.334445 11.00000 0.03188 0.02851 = 0.03409 0.01941 0.01251 0.00901 AFIX 147 H1 2 0.293812 0.093074 0.285569 11.00000 -1.50000 AFIX 0 O2 6 0.626741 0.819302 0.164376 11.00000 0.03202 0.02316 = 0.03743 0.01675 0.01082 0.00862 AFIX 147 H2A 2 0.601918 0.831394 0.118344 11.00000 -1.50000 AFIX 0 C26 1 0.687628 0.928801 0.478035 11.00000 0.06398 0.04925 = 0.05501 0.02328 0.02172 0.01554 AFIX 137 H26A 2 0.783499 0.910584 0.505455 11.00000 -1.50000 H26B 2 0.605999 0.852583 0.439754 11.00000 -1.50000 H26C 2 0.633613 0.971744 0.522390 11.00000 -1.50000 AFIX 0 H7A 2 0.417215 0.111239 0.013967 11.00000 -1.50000 H7B 2 0.538883 0.088480 -0.039558 11.00000 -1.50000 C27 1 0.879547 0.933452 0.354649 11.00000 0.04861 0.06138 = 0.04026 0.00927 0.01273 0.01004 AFIX 137 H27A 2 0.925400 0.970640 0.314178 11.00000 -1.50000 H27B 2 0.805187 0.851204 0.322643 11.00000 -1.50000 H27C 2 0.972273 0.928840 0.393872 11.00000 -1.50000 AFIX 0 O6 6 0.888305 1.139437 0.476960 11.00000 0.06763 0.04554 = 0.06544 0.01722 0.03029 0.01111 S2 7 0.761656 1.024641 0.415694 11.00000 0.04973 0.05155 = 0.04894 0.02829 0.01381 0.02356 C25 1 -0.003008 0.008694 0.047520 11.00000 0.03055 0.03405 = 0.03706 0.01434 0.00957 0.01250 AFIX 23 H25A 2 -0.118086 -0.032663 0.051766 11.00000 -1.20000 H25B 2 0.021050 0.096710 0.080457 11.00000 -1.20000 AFIX 0 O3 6 0.105886 -0.182292 0.045130 11.00000 0.04431 0.03329 = 0.04977 0.01991 0.01226 0.01550 O4 6 0.124191 -0.023834 0.186140 11.00000 0.04192 0.05044 = 0.03949 0.02118 0.00746 0.00853 O5 6 0.316713 0.016657 0.089906 11.00000 0.02620 0.04636 = 0.05500 0.02569 0.00710 0.01047 S1 7 0.147113 -0.051398 0.095315 11.00000 0.02971 0.03328 = 0.03678 0.01877 0.00720 0.00949 O7 6 0.469008 0.127535 -0.023730 11.00000 0.06534 0.07002 = 0.06818 0.04828 0.03530 0.03776 HKLF 4 REM nw1711_a.res in P-1 REM R1 = 0.0412 for 4879 Fo > 4sig(Fo) and 0.0499 for all 5801 data REM 400 parameters refined using 2 restraints END WGHT 0.0503 3.1001 REM Highest difference peak 1.287, deepest hole -0.724, 1-sigma level 0.103 Q1 1 0.7632 0.6776 0.3963 11.00000 0.05 1.29 Q2 1 0.5157 0.5234 0.2526 11.00000 0.05 0.91 Q3 1 0.2975 0.4004 0.1219 11.00000 0.05 0.74 Q4 1 0.3639 0.4213 0.1742 11.00000 0.05 0.69 Q5 1 0.2405 -0.0774 0.0803 11.00000 0.05 0.66 Q6 1 0.1285 -0.1045 0.0315 11.00000 0.05 0.61 Q7 1 0.8644 1.0250 0.3856 11.00000 0.05 0.58 Q8 1 0.2280 0.2332 0.1102 11.00000 0.05 0.56 Q9 1 0.3296 0.3817 0.3341 11.00000 0.05 0.54 Q10 1 0.8675 1.0402 0.4747 11.00000 0.05 0.52 Q11 1 0.5807 0.3032 0.2651 11.00000 0.05 0.48 Q12 1 0.2463 0.5539 0.3292 11.00000 0.05 0.47 Q13 1 0.6633 0.5786 0.1776 11.00000 0.05 0.45 Q14 1 0.3711 0.2957 0.3403 11.00000 0.05 0.44 Q15 1 0.5740 0.5160 0.3359 11.00000 0.05 0.43 Q16 1 0.1059 0.0230 0.1549 11.00000 0.05 0.42 Q17 1 0.0876 -0.1626 0.0734 11.00000 0.05 0.42 Q18 1 0.4224 0.7534 0.2439 11.00000 0.05 0.42 Q19 1 0.4167 0.6583 0.2439 11.00000 0.05 0.41 Q20 1 0.8605 1.1597 0.4295 11.00000 0.05 0.41 Q21 1 0.6106 0.5373 0.3080 11.00000 0.05 0.41 Q22 1 0.7504 0.4152 0.1794 11.00000 0.05 0.40 Q23 1 0.7571 1.0632 0.4964 11.00000 0.05 0.40 Q24 1 0.9201 0.5371 0.1221 11.00000 0.05 0.40 Q25 1 0.6712 0.5640 0.2945 11.00000 0.05 0.39 Q26 1 0.0705 0.4247 0.3895 11.00000 0.05 0.39 Q27 1 0.2494 0.6582 0.3171 11.00000 0.05 0.39 Q28 1 0.7130 0.4908 0.1733 11.00000 0.05 0.38 Q29 1 0.4065 0.2025 0.3400 11.00000 0.05 0.38 Q30 1 0.4789 0.7024 0.1974 11.00000 0.05 0.37 ; _shelx_res_checksum 40958 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Br1 Br 0.70421(5) 0.60774(4) 0.37686(3) 0.02855(12) Uani 1 1 d . . . . . Br2 Br 0.27846(5) 0.34155(4) 0.12031(2) 0.02550(11) Uani 1 1 d . . . . . C1 C 0.6765(4) 0.6252(3) 0.1548(2) 0.0198(7) Uani 1 1 d . . . . . C2 C 0.8193(5) 0.6609(4) 0.1193(2) 0.0247(7) Uani 1 1 d . . . . . H2 H 0.839459 0.733610 0.106006 0.030 Uiso 1 1 calc R . . . . C3 C 0.9315(5) 0.5889(4) 0.1038(3) 0.0272(8) Uani 1 1 d . . . . . H3 H 1.027561 0.612708 0.080343 0.033 Uiso 1 1 calc R . . . . C4 C 0.8990(5) 0.4805(4) 0.1237(2) 0.0244(7) Uani 1 1 d . . . . . H4 H 0.970276 0.428858 0.112088 0.029 Uiso 1 1 calc R . . . . C5 C 0.7583(4) 0.4512(3) 0.1612(2) 0.0202(7) Uani 1 1 d . . . . . C6 C 0.7167(4) 0.3427(3) 0.1895(2) 0.0208(7) Uani 1 1 d . . . . . C7 C 0.7962(5) 0.2494(4) 0.1682(3) 0.0273(8) Uani 1 1 d . . . . . H7 H 0.878957 0.251367 0.133234 0.033 Uiso 1 1 calc R . . . . C8 C 0.7504(5) 0.1525(4) 0.2001(3) 0.0310(9) Uani 1 1 d . . . . . H8 H 0.800521 0.087647 0.186184 0.037 Uiso 1 1 calc R . . . . C9 C 0.6290(5) 0.1540(4) 0.2529(3) 0.0269(8) Uani 1 1 d . . . . . H9 H 0.598028 0.090025 0.275293 0.032 Uiso 1 1 calc R . . . . C10 C 0.5530(5) 0.2498(3) 0.2729(2) 0.0208(7) Uani 1 1 d . . . . . C11 C 0.4392(5) 0.2542(4) 0.3413(2) 0.0240(7) Uani 1 1 d . . . . . C12 C 0.5597(5) 0.3132(4) 0.4321(2) 0.0286(8) Uani 1 1 d . . . . . H12A H 0.492620 0.315850 0.477154 0.043 Uiso 1 1 calc GR . . . . H12B H 0.624746 0.396172 0.439323 0.043 Uiso 1 1 calc GR . . . . H12C H 0.637006 0.264297 0.436270 0.043 Uiso 1 1 calc GR . . . . C13 C 0.3071(4) 0.3270(3) 0.3439(2) 0.0219(7) Uani 1 1 d . . . . . C14 C 0.1683(5) 0.2948(4) 0.3834(3) 0.0286(8) Uani 1 1 d . . . . . H14 H 0.150411 0.223896 0.398954 0.034 Uiso 1 1 calc R . . . . C15 C 0.0571(5) 0.3678(4) 0.3995(3) 0.0307(9) Uani 1 1 d . . . . . H15 H -0.036653 0.345961 0.425038 0.037 Uiso 1 1 calc R . . . . C16 C 0.0877(5) 0.4741(4) 0.3771(3) 0.0282(8) Uani 1 1 d . . . . . H16 H 0.016600 0.525907 0.388499 0.034 Uiso 1 1 calc R . . . . C17 C 0.2256(5) 0.5013(4) 0.3374(2) 0.0224(7) Uani 1 1 d . . . . . C18 C 0.2673(5) 0.6099(3) 0.3092(2) 0.0223(7) Uani 1 1 d . . . . . C19 C 0.1913(5) 0.7055(4) 0.3324(3) 0.0294(8) Uani 1 1 d . . . . . H19 H 0.110758 0.704971 0.368647 0.035 Uiso 1 1 calc R . . . . C20 C 0.2380(6) 0.8014(4) 0.3004(3) 0.0327(9) Uani 1 1 d . . . . . H20 H 0.189892 0.867293 0.315277 0.039 Uiso 1 1 calc R . . . . C21 C 0.3569(5) 0.7988(4) 0.2462(3) 0.0279(8) Uani 1 1 d . . . . . H21 H 0.387964 0.862734 0.223788 0.033 Uiso 1 1 calc R . . . . C22 C 0.4302(5) 0.7013(3) 0.2249(2) 0.0218(7) Uani 1 1 d . . . . . C23 C 0.5413(5) 0.6959(3) 0.1548(2) 0.0212(7) Uani 1 1 d . . . . . C24 C 0.4165(5) 0.6293(4) 0.0654(2) 0.0270(8) Uani 1 1 d . . . . . H24A H 0.331576 0.672532 0.061347 0.040 Uiso 1 1 calc GR . . . . H24B H 0.360538 0.545362 0.060289 0.040 Uiso 1 1 calc GR . . . . H24C H 0.479527 0.628565 0.018889 0.040 Uiso 1 1 calc GR . . . . Co1 Co 0.49080(7) 0.47536(5) 0.24855(4) 0.01638(13) Uani 1 1 d . . . . . N1 N 0.6506(4) 0.5239(3) 0.17845(18) 0.0178(6) Uani 1 1 d . . . . . N2 N 0.5941(4) 0.3428(3) 0.23986(18) 0.0188(6) Uani 1 1 d . . . . . N3 N 0.3320(4) 0.4282(3) 0.31937(18) 0.0196(6) Uani 1 1 d . . . . . N4 N 0.3880(4) 0.6089(3) 0.25766(18) 0.0182(6) Uani 1 1 d . . . . . O1 O 0.3551(4) 0.1302(3) 0.33444(18) 0.0289(6) Uani 1 1 d . . . . . H1 H 0.293812 0.093074 0.285569 0.043 Uiso 1 1 calc GR . . . . O2 O 0.6267(4) 0.8193(2) 0.16438(19) 0.0289(6) Uani 1 1 d . . . . . H2A H 0.601918 0.831394 0.118344 0.043 Uiso 1 1 calc GR . . . . C26 C 0.6876(8) 0.9288(5) 0.4780(4) 0.0541(13) Uani 1 1 d . . . . . H26A H 0.783499 0.910584 0.505455 0.081 Uiso 1 1 calc GR . . . . H26B H 0.605999 0.852583 0.439754 0.081 Uiso 1 1 calc GR . . . . H26C H 0.633613 0.971744 0.522390 0.081 Uiso 1 1 calc GR . . . . H7A H 0.417(8) 0.111(7) 0.014(4) 0.081 Uiso 1 1 d DR . . . . H7B H 0.539(7) 0.088(6) -0.040(5) 0.081 Uiso 1 1 d DR . . . . C27 C 0.8795(7) 0.9335(6) 0.3546(3) 0.0528(13) Uani 1 1 d . . . . . H27A H 0.925400 0.970640 0.314178 0.079 Uiso 1 1 calc GR . . . . H27B H 0.805187 0.851204 0.322643 0.079 Uiso 1 1 calc GR . . . . H27C H 0.972273 0.928840 0.393872 0.079 Uiso 1 1 calc GR . . . . O6 O 0.8883(5) 1.1394(4) 0.4770(3) 0.0596(10) Uani 1 1 d . . . . . S2 S 0.76166(17) 1.02464(12) 0.41569(8) 0.0454(3) Uani 1 1 d . . . . . C25 C -0.0030(5) 0.0087(4) 0.0475(3) 0.0326(9) Uani 1 1 d . . . . . H25A H -0.118086 -0.032663 0.051766 0.039 Uiso 1 1 calc R . . . . H25B H 0.021050 0.096710 0.080457 0.039 Uiso 1 1 calc R . . . . O3 O 0.1059(4) -0.1823(3) 0.0451(2) 0.0401(7) Uani 1 1 d . . . . . O4 O 0.1242(4) -0.0238(3) 0.1861(2) 0.0435(8) Uani 1 1 d . . . . . O5 O 0.3167(4) 0.0167(3) 0.0899(2) 0.0406(7) Uani 1 1 d . . . . . S1 S 0.14711(13) -0.05140(10) 0.09532(7) 0.0315(2) Uani 1 1 d . . . . . O7 O 0.4690(5) 0.1275(4) -0.0237(3) 0.0568(10) Uani 1 1 d D . . . . 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 Br1 0.0254(2) 0.0353(2) 0.0274(2) 0.01059(17) 0.00733(15) 0.01254(17) Br2 0.0227(2) 0.0296(2) 0.0272(2) 0.01133(16) 0.00675(15) 0.01016(15) C1 0.0169(16) 0.0250(18) 0.0189(16) 0.0098(14) 0.0031(13) 0.0059(14) C2 0.0214(18) 0.030(2) 0.0272(18) 0.0154(16) 0.0081(14) 0.0064(15) C3 0.0181(17) 0.037(2) 0.032(2) 0.0176(17) 0.0115(15) 0.0074(15) C4 0.0199(17) 0.031(2) 0.0281(19) 0.0120(16) 0.0110(14) 0.0128(15) C5 0.0176(16) 0.0266(18) 0.0198(16) 0.0097(14) 0.0062(13) 0.0093(14) C6 0.0200(16) 0.0267(18) 0.0220(17) 0.0118(14) 0.0080(13) 0.0119(14) C7 0.029(2) 0.035(2) 0.0305(19) 0.0161(17) 0.0172(16) 0.0198(17) C8 0.039(2) 0.030(2) 0.036(2) 0.0152(17) 0.0145(18) 0.0232(18) C9 0.032(2) 0.029(2) 0.0282(19) 0.0164(16) 0.0090(16) 0.0141(16) C10 0.0238(17) 0.0250(18) 0.0195(16) 0.0123(14) 0.0062(14) 0.0106(14) C11 0.0241(18) 0.0291(19) 0.0257(18) 0.0149(15) 0.0095(15) 0.0115(15) C12 0.0271(19) 0.041(2) 0.0247(19) 0.0174(17) 0.0060(15) 0.0144(17) C13 0.0196(17) 0.0287(19) 0.0219(17) 0.0136(15) 0.0067(14) 0.0076(14) C14 0.0240(19) 0.040(2) 0.030(2) 0.0212(18) 0.0106(15) 0.0094(16) C15 0.0216(18) 0.047(2) 0.031(2) 0.0188(18) 0.0139(16) 0.0123(17) C16 0.0224(18) 0.044(2) 0.0283(19) 0.0174(17) 0.0132(15) 0.0175(17) C17 0.0206(17) 0.032(2) 0.0206(17) 0.0120(15) 0.0081(14) 0.0117(15) C18 0.0211(17) 0.0271(19) 0.0227(17) 0.0092(14) 0.0070(14) 0.0119(14) C19 0.029(2) 0.035(2) 0.032(2) 0.0136(17) 0.0167(16) 0.0186(17) C20 0.037(2) 0.032(2) 0.039(2) 0.0137(18) 0.0159(18) 0.0237(18) C21 0.032(2) 0.0261(19) 0.032(2) 0.0124(16) 0.0104(16) 0.0160(16) C22 0.0209(17) 0.0238(18) 0.0245(17) 0.0097(14) 0.0063(14) 0.0106(14) C23 0.0213(17) 0.0199(17) 0.0259(18) 0.0113(14) 0.0076(14) 0.0067(14) C24 0.0264(19) 0.036(2) 0.0252(18) 0.0148(16) 0.0062(15) 0.0156(16) Co1 0.0147(3) 0.0215(3) 0.0185(3) 0.0098(2) 0.0078(2) 0.0095(2) N1 0.0163(13) 0.0226(15) 0.0186(13) 0.0097(11) 0.0057(11) 0.0090(11) N2 0.0168(14) 0.0249(15) 0.0190(14) 0.0099(12) 0.0058(11) 0.0097(12) N3 0.0156(13) 0.0279(16) 0.0188(14) 0.0089(12) 0.0055(11) 0.0103(12) N4 0.0168(13) 0.0219(15) 0.0193(14) 0.0087(11) 0.0058(11) 0.0084(11) O1 0.0319(15) 0.0285(14) 0.0341(15) 0.0194(12) 0.0125(12) 0.0090(12) O2 0.0320(15) 0.0232(13) 0.0374(15) 0.0168(12) 0.0108(12) 0.0086(11) C26 0.064(3) 0.049(3) 0.055(3) 0.023(3) 0.022(3) 0.016(3) C27 0.049(3) 0.061(3) 0.040(3) 0.009(2) 0.013(2) 0.010(3) O6 0.068(3) 0.046(2) 0.065(2) 0.0172(19) 0.030(2) 0.0111(19) S2 0.0497(7) 0.0516(7) 0.0489(7) 0.0283(6) 0.0138(5) 0.0236(6) C25 0.031(2) 0.034(2) 0.037(2) 0.0143(18) 0.0096(17) 0.0125(17) O3 0.0443(18) 0.0333(16) 0.0498(18) 0.0199(14) 0.0123(15) 0.0155(14) O4 0.0419(18) 0.050(2) 0.0395(17) 0.0212(15) 0.0075(14) 0.0085(15) O5 0.0262(15) 0.0464(19) 0.0550(19) 0.0257(16) 0.0071(13) 0.0105(13) S1 0.0297(5) 0.0333(5) 0.0368(5) 0.0188(4) 0.0072(4) 0.0095(4) O7 0.065(3) 0.070(3) 0.068(3) 0.048(2) 0.035(2) 0.038(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 0 0 -1 0.0091 0 0 1 0.0141 0 -1 0 0.0040 0 1 0 0.0110 5 2 -2 0.0374 -5 -2 2 0.0474 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 C2 C1 C23 117.2(3) . . ? N1 C1 C2 120.4(3) . . ? N1 C1 C23 121.9(3) . . ? C1 C2 H2 119.9 . . ? C3 C2 C1 120.3(3) . . ? C3 C2 H2 119.9 . . ? C2 C3 H3 120.5 . . ? C2 C3 C4 119.1(3) . . ? C4 C3 H3 120.5 . . ? C3 C4 H4 120.8 . . ? C5 C4 C3 118.3(3) . . ? C5 C4 H4 120.8 . . ? C4 C5 C6 123.1(3) . . ? N1 C5 C4 122.5(3) . . ? N1 C5 C6 114.4(3) . . ? C7 C6 C5 123.3(3) . . ? N2 C6 C5 114.1(3) . . ? N2 C6 C7 122.5(3) . . ? C6 C7 H7 120.7 . . ? C6 C7 C8 118.7(3) . . ? C8 C7 H7 120.7 . . ? C7 C8 H8 120.6 . . ? C9 C8 C7 118.8(3) . . ? C9 C8 H8 120.6 . . ? C8 C9 H9 119.7 . . ? C8 C9 C10 120.6(3) . . ? C10 C9 H9 119.7 . . ? C9 C10 C11 117.3(3) . . ? N2 C10 C9 120.7(3) . . ? N2 C10 C11 121.6(3) . . ? C10 C11 C12 107.0(3) . . ? C10 C11 C13 119.1(3) . . ? C13 C11 C12 106.3(3) . . ? O1 C11 C10 108.8(3) . . ? O1 C11 C12 105.6(3) . . ? O1 C11 C13 109.3(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12B 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C11 117.0(3) . . ? N3 C13 C11 122.2(3) . . ? N3 C13 C14 120.3(3) . . ? C13 C14 H14 119.9 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C14 C15 H15 120.5 . . ? C14 C15 C16 119.0(3) . . ? C16 C15 H15 120.5 . . ? C15 C16 H16 120.7 . . ? C17 C16 C15 118.6(4) . . ? C17 C16 H16 120.7 . . ? C16 C17 C18 123.0(3) . . ? N3 C17 C16 122.6(3) . . ? N3 C17 C18 114.3(3) . . ? C19 C18 C17 123.5(3) . . ? N4 C18 C17 114.1(3) . . ? N4 C18 C19 122.4(3) . . ? C18 C19 H19 120.8 . . ? C20 C19 C18 118.4(3) . . ? C20 C19 H19 120.8 . . ? C19 C20 H20 120.3 . . ? C19 C20 C21 119.4(4) . . ? C21 C20 H20 120.3 . . ? C20 C21 H21 119.8 . . ? C20 C21 C22 120.3(4) . . ? C22 C21 H21 119.8 . . ? C21 C22 C23 117.0(3) . . ? N4 C22 C21 120.5(3) . . ? N4 C22 C23 122.1(3) . . ? C1 C23 C24 106.4(3) . . ? C22 C23 C1 117.7(3) . . ? C22 C23 C24 106.3(3) . . ? O2 C23 C1 108.0(3) . . ? O2 C23 C22 107.4(3) . . ? O2 C23 C24 111.1(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Br2 Co1 Br1 179.50(3) . . ? N1 Co1 Br1 88.11(9) . . ? N1 Co1 Br2 91.90(9) . . ? N1 Co1 N4 95.06(12) . . ? N2 Co1 Br1 90.26(9) . . ? N2 Co1 Br2 89.24(9) . . ? N2 Co1 N1 84.88(12) . . ? N2 Co1 N3 95.37(12) . . ? N2 Co1 N4 179.74(14) . . ? N3 Co1 Br1 91.45(9) . . ? N3 Co1 Br2 88.53(9) . . ? N3 Co1 N1 179.51(14) . . ? N3 Co1 N4 84.69(12) . . ? N4 Co1 Br1 89.48(9) . . ? N4 Co1 Br2 91.01(9) . . ? C1 N1 C5 119.3(3) . . ? C1 N1 Co1 127.4(2) . . ? C5 N1 Co1 112.9(2) . . ? C6 N2 Co1 113.1(2) . . ? C10 N2 C6 118.6(3) . . ? C10 N2 Co1 128.2(2) . . ? C13 N3 C17 119.2(3) . . ? C13 N3 Co1 127.2(2) . . ? C17 N3 Co1 113.2(2) . . ? C18 N4 Co1 112.9(2) . . ? C22 N4 C18 119.0(3) . . ? C22 N4 Co1 127.9(2) . . ? C11 O1 H1 109.5 . . ? C23 O2 H2A 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S2 C26 H26A 109.5 . . ? S2 C26 H26B 109.5 . . ? S2 C26 H26C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S2 C27 H27A 109.5 . . ? S2 C27 H27B 109.5 . . ? S2 C27 H27C 109.5 . . ? C27 S2 C26 98.3(3) . . ? O6 S2 C26 107.4(3) . . ? O6 S2 C27 106.7(3) . . ? C25 C25 H25A 109.1 2 . ? C25 C25 H25B 109.1 2 . ? C25 C25 S1 112.5(4) 2 . ? H25A C25 H25B 107.8 . . ? S1 C25 H25A 109.1 . . ? S1 C25 H25B 109.1 . . ? O3 S1 C25 107.3(2) . . ? O3 S1 O4 114.41(19) . . ? O3 S1 O5 111.9(2) . . ? O4 S1 C25 104.2(2) . . ? O5 S1 C25 106.65(19) . . ? O5 S1 O4 111.6(2) . . ? H7A O7 H7B 117(7) . . ? 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 Br1 Co1 2.4003(7) . ? Br2 Co1 2.3990(7) . ? C1 C2 1.389(5) . ? C1 C23 1.532(5) . ? C1 N1 1.343(4) . ? C2 H2 0.9300 . ? C2 C3 1.382(5) . ? C3 H3 0.9300 . ? C3 C4 1.386(5) . ? C4 H4 0.9300 . ? C4 C5 1.379(5) . ? C5 C6 1.469(5) . ? C5 N1 1.359(4) . ? C6 C7 1.380(5) . ? C6 N2 1.360(4) . ? C7 H7 0.9300 . ? C7 C8 1.386(6) . ? C8 H8 0.9300 . ? C8 C9 1.379(5) . ? C9 H9 0.9300 . ? C9 C10 1.384(5) . ? C10 C11 1.523(5) . ? C10 N2 1.354(4) . ? C11 C12 1.539(5) . ? C11 C13 1.525(5) . ? C11 O1 1.424(5) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.395(5) . ? C13 N3 1.349(5) . ? C14 H14 0.9300 . ? C14 C15 1.384(6) . ? C15 H15 0.9300 . ? C15 C16 1.386(6) . ? C16 H16 0.9300 . ? C16 C17 1.378(5) . ? C17 C18 1.470(5) . ? C17 N3 1.354(4) . ? C18 C19 1.384(5) . ? C18 N4 1.361(4) . ? C19 H19 0.9300 . ? C19 C20 1.378(6) . ? C20 H20 0.9300 . ? C20 C21 1.380(5) . ? C21 H21 0.9300 . ? C21 C22 1.387(5) . ? C22 C23 1.528(5) . ? C22 N4 1.347(5) . ? C23 C24 1.541(5) . ? C23 O2 1.408(4) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? Co1 N1 1.924(3) . ? Co1 N2 1.920(3) . ? Co1 N3 1.922(3) . ? Co1 N4 1.927(3) . ? O1 H1 0.8200 . ? O2 H2A 0.8200 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C26 S2 1.787(5) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C27 S2 1.762(5) . ? O6 S2 1.476(4) . ? C25 C25 1.507(8) 2 ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 S1 1.777(4) . ? O3 S1 1.442(3) . ? O4 S1 1.458(3) . ? O5 S1 1.452(3) . ? O7 H7A 0.827(10) . ? O7 H7B 0.828(10) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O1 H1 O4 0.82 1.92 2.718(4) 164.8 . yes O2 H2A O7 0.82 1.83 2.646(5) 172.3 2_665 yes O7 H7A O5 0.827(10) 2.02(3) 2.812(5) 160(7) . yes O7 H7B O5 0.828(10) 1.967(14) 2.791(5) 173(7) 2_655 yes