#------------------------------------------------------------------------------ #$Date: 2020-08-14 04:41:46 +0300 (Fri, 14 Aug 2020) $ #$Revision: 255305 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705145.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_7705145 loop_ _publ_author_name 'Laha, Biswajit' 'Khullar, Sadhika' 'Gogia, Alisha' 'Mandal, Sanjay' _publ_section_title ; Effecting structural diversity in a series of Co(II)-organic frameworks by the interplay between rigidity of a dicarboxylate and flexibility of bis(tridentate) spanning ligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02153A _journal_year 2020 _chemical_formula_moiety '2 (C22 H23 Co N3 O5 S), C2H6O, 2 (H2O)' _chemical_formula_sum 'C46 H56 Co2 N6 O13 S2' _chemical_formula_weight 1082.94 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_update_record ; 2020-06-16 deposited with the CCDC. 2020-08-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 92.443(7) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 9.1292(10) _cell_length_b 16.1977(18) _cell_length_c 17.632(2) _cell_measurement_reflns_used 2900 _cell_measurement_temperature 100.(2) _cell_measurement_theta_max 22.3815 _cell_measurement_theta_min 2.2329 _cell_volume 2604.9(5) _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 100.(2) _diffrn_detector_area_resol_mean 8.3333 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker Kappa APEX II' _diffrn_measurement_method 'phi and omega scan' _diffrn_radiation_monochromator Graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0704 _diffrn_reflns_av_unetI/netI 0.0669 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 19903 _diffrn_reflns_theta_full 25.03 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_min 1.71 _diffrn_source 'Sealed tube' _diffrn_source_type 'Fine Focus' _exptl_absorpt_coefficient_mu 0.782 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.59 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/5 (Bruker AXS Inc.)' _exptl_crystal_colour pink _exptl_crystal_density_diffrn 1.381 _exptl_crystal_density_method 'not measured' _exptl_crystal_description rectangular _exptl_crystal_F_000 1128 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _refine_diff_density_max 1.748 _refine_diff_density_min -0.527 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 316 _refine_ls_number_reflns 4591 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.031 _refine_ls_R_factor_all 0.1049 _refine_ls_R_factor_gt 0.0698 _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^)+(0.1250P)^2^+4.3587P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1889 _refine_ls_wR_factor_ref 0.2130 _reflns_number_gt 3192 _reflns_number_total 4591 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02153a2.cif _cod_data_source_block 3 _cod_database_code 7705145 _shelx_res_file ; BL_Co_tpchn_tdc_0m.res created by SHELXL-2014/7 TITL BL_Co_tpchn_tdc_0m in P2(1)/c CELL 0.71073 9.1292 16.1977 17.632 90 92.4428 90 ZERR 2 0.001 0.0018 0.0021 0 0.0066 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H N O S Co UNIT 92 112 12 26 4 4 L.S. 10 ACTA BOND $H FMAP 2 PLAN 25 CONF DFIX 1.54 0.01 C24 C25 DFIX 1.40 0.01 C25 O6 TEMP -173 WGHT 0.124968 4.358730 FVAR 0.13968 CO1 6 0.349421 0.219315 0.192704 11.00000 0.02546 0.02342 = 0.02917 -0.00424 0.00121 0.00281 S1 5 -0.024234 0.426178 0.238629 11.00000 0.02768 0.03106 = 0.03758 -0.00032 -0.00143 0.00616 AFIX 6 O1S 4 0.940828 0.061076 0.949111 11.00000 0.09947 0.07617 = 0.05592 -0.01537 -0.01059 0.01215 H1SA 2 0.920029 0.037878 0.906817 11.00000 -1.50000 H1SB 2 0.899976 0.031033 0.981624 11.00000 -1.50000 AFIX 0 O1 4 0.273958 0.169175 0.086293 11.00000 0.03361 0.03416 = 0.02858 -0.00466 0.00401 0.00392 AFIX 7 H1A 2 0.344882 0.167709 0.056034 11.00000 -1.50000 H1B 2 0.211537 0.201782 0.064369 11.00000 -1.50000 AFIX 0 O2 4 0.078162 0.290728 0.065569 11.00000 0.03906 0.03963 = 0.03856 -0.00831 -0.01059 0.00609 O3 4 0.246553 0.132662 0.257793 11.00000 0.03164 0.02759 = 0.03848 -0.00554 0.00320 -0.00200 O4 4 0.165629 0.047609 0.164474 11.00000 0.04018 0.03155 = 0.04007 -0.00137 -0.00073 -0.00629 N1 3 0.418852 0.289286 0.287047 11.00000 0.03689 0.02007 = 0.02759 0.00099 0.00434 -0.00109 N2 3 0.538100 0.144449 0.180648 11.00000 0.02442 0.02798 = 0.03496 -0.00060 0.00141 0.00228 O8 4 0.162569 0.294326 0.187265 11.00000 0.03774 0.04185 = 0.03833 -0.00430 -0.00631 0.01616 C1 1 0.538358 0.336096 0.279969 11.00000 0.04316 0.02325 = 0.02141 0.00240 -0.00205 -0.00414 C2 1 0.611308 0.331166 0.205744 11.00000 0.03751 0.03454 = 0.03493 0.00392 0.00217 -0.01384 AFIX 23 H2A 2 0.650176 0.385110 0.193702 11.00000 -1.20000 H2B 2 0.693197 0.293118 0.210774 11.00000 -1.20000 AFIX 0 N3 3 0.511815 0.303698 0.142321 11.00000 0.04014 0.02707 = 0.01936 -0.00466 -0.00084 0.00681 C4 1 0.423574 0.372095 0.105558 11.00000 0.04432 0.03839 = 0.03300 -0.00299 -0.00006 0.00939 AFIX 23 H4A 2 0.367426 0.397742 0.144665 11.00000 -1.20000 H4B 2 0.353647 0.346996 0.069571 11.00000 -1.20000 AFIX 0 C5 1 0.501218 0.440729 0.064144 11.00000 0.04046 0.04568 = 0.03047 0.00465 0.00578 0.00587 AFIX 13 H5 2 0.590051 0.456771 0.093679 11.00000 -1.20000 AFIX 0 C6 1 0.396042 0.513978 0.058837 11.00000 0.05270 0.05517 = 0.03889 0.00797 0.01762 0.02178 AFIX 23 H6A 2 0.304779 0.496541 0.033561 11.00000 -1.20000 H6B 2 0.374403 0.531841 0.109662 11.00000 -1.20000 AFIX 0 C7 1 0.542766 0.415123 -0.016571 11.00000 0.06786 0.06605 = 0.04442 0.02126 0.02330 0.03198 AFIX 23 H7A 2 0.614732 0.371081 -0.013077 11.00000 -1.20000 H7B 2 0.456459 0.394216 -0.044251 11.00000 -1.20000 AFIX 0 C8 1 0.569016 0.072541 0.216898 11.00000 0.03417 0.02449 = 0.04101 0.00076 0.00386 0.00530 AFIX 43 H8 2 0.509230 0.055813 0.255446 11.00000 -1.20000 AFIX 0 C9 1 0.684529 0.023403 0.199233 11.00000 0.04568 0.03977 = 0.05665 0.00413 -0.00149 0.01386 AFIX 43 H9 2 0.701173 -0.026455 0.224300 11.00000 -1.20000 AFIX 0 C10 1 0.775951 0.049150 0.143529 11.00000 0.05086 0.06288 = 0.05269 0.00314 0.00892 0.03808 AFIX 43 H10 2 0.856063 0.017141 0.131155 11.00000 -1.20000 AFIX 0 C11 1 0.747637 0.122540 0.106452 11.00000 0.04344 0.05601 = 0.04514 0.00349 0.01312 0.01897 AFIX 43 H11 2 0.807527 0.140567 0.068429 11.00000 -1.20000 AFIX 0 C12 1 0.628758 0.168863 0.126740 11.00000 0.03576 0.03706 = 0.02760 -0.00272 -0.00060 0.00624 C13 1 0.590909 0.251269 0.089568 11.00000 0.03648 0.03707 = 0.02844 0.00256 0.00285 0.00427 AFIX 23 H13A 2 0.680101 0.278810 0.075486 11.00000 -1.20000 H13B 2 0.530365 0.242164 0.043783 11.00000 -1.20000 AFIX 0 C14 1 0.084505 0.319924 0.132046 11.00000 0.02285 0.03328 = 0.04180 -0.00540 0.00274 0.00259 C15 1 -0.004187 0.395501 0.146728 11.00000 0.02265 0.02703 = 0.03643 -0.00480 0.00154 -0.00244 C16 1 0.121707 0.012157 0.290935 11.00000 0.02671 0.02348 = 0.04409 -0.00241 0.00153 0.00318 C17 1 -0.135213 0.516196 0.131711 11.00000 0.03090 0.02851 = 0.04277 0.00541 0.00436 0.00029 AFIX 43 H17 2 -0.182850 0.558949 0.105515 11.00000 -1.20000 AFIX 0 C18 1 -0.069783 0.449176 0.095906 11.00000 0.03143 0.03354 = 0.03695 0.00466 0.00399 -0.00013 AFIX 43 H18 2 -0.070853 0.442022 0.043551 11.00000 -1.20000 AFIX 0 C19 1 0.181396 0.068692 0.233195 11.00000 0.02149 0.02627 = 0.04050 -0.00387 -0.00127 0.00286 C20 1 0.593816 0.385406 0.339257 11.00000 0.05435 0.02825 = 0.03124 -0.00063 -0.00590 -0.00842 AFIX 43 H20 2 0.677070 0.417510 0.333509 11.00000 -1.20000 AFIX 0 C21 1 0.522680 0.385532 0.406454 11.00000 0.07192 0.03277 = 0.02712 -0.00447 -0.00603 -0.00328 AFIX 43 H21 2 0.558815 0.417228 0.447061 11.00000 -1.20000 AFIX 0 C22 1 0.399157 0.339231 0.413661 11.00000 0.06490 0.04479 = 0.02360 0.00284 0.00901 0.00593 AFIX 43 H22 2 0.349753 0.339450 0.458710 11.00000 -1.20000 AFIX 0 C23 1 0.349079 0.292107 0.352776 11.00000 0.04349 0.02962 = 0.02863 0.00248 0.00805 0.00246 AFIX 43 H23 2 0.264074 0.261168 0.357270 11.00000 -1.20000 AFIX 0 O6 4 0.120965 0.763887 0.045160 10.50000 0.06131 AFIX 147 H6 2 0.058097 0.800039 0.042266 10.50000 -1.50000 AFIX 0 C25 1 0.104491 0.717491 0.111903 10.50000 0.06135 AFIX 23 H25A 2 0.151987 0.667637 0.094913 10.50000 -1.20000 H25B 2 0.000905 0.705521 0.103758 10.50000 -1.20000 AFIX 0 C24 1 0.114513 0.697994 0.196571 10.50000 0.12148 AFIX 137 H24A 2 0.215533 0.697471 0.214077 10.50000 -1.50000 H24B 2 0.071668 0.644876 0.205223 10.50000 -1.50000 H24C 2 0.062646 0.739360 0.223719 10.50000 -1.50000 AFIX 0 HKLF 4 REM BL_Co_tpchn_tdc_0m in P2(1)/c REM R1 = 0.0698 for 3192 Fo > 4sig(Fo) and 0.1049 for all 4591 data REM 316 parameters refined using 2 restraints END WGHT 0.1242 4.2073 REM Highest difference peak 1.748, deepest hole -0.527, 1-sigma level 0.114 Q1 1 0.2357 0.6994 0.1653 11.00000 0.05 1.75 Q2 1 0.0046 0.7806 0.0843 11.00000 0.05 1.53 Q3 1 0.1172 0.6804 0.0461 11.00000 0.05 1.33 Q4 1 0.0927 0.7153 0.2249 11.00000 0.05 0.76 Q5 1 0.4155 0.3913 0.0390 11.00000 0.05 0.69 Q6 1 0.5387 0.3892 0.1068 11.00000 0.05 0.62 Q7 1 0.1464 0.7766 0.0303 11.00000 0.05 0.62 Q8 1 0.1427 0.7086 0.1320 11.00000 0.05 0.60 Q9 1 0.3237 0.4737 0.0338 11.00000 0.05 0.56 Q10 1 0.3979 0.2614 0.1742 11.00000 0.05 0.47 Q11 1 0.1371 0.6652 0.1760 11.00000 0.05 0.47 Q12 1 0.4868 0.3667 -0.0463 11.00000 0.05 0.44 Q13 1 0.2215 0.1212 0.0975 11.00000 0.05 0.43 Q14 1 0.2194 0.3322 0.1684 11.00000 0.05 0.37 Q15 1 0.3477 0.2215 0.2687 11.00000 0.05 0.36 Q16 1 0.0432 0.7220 0.0111 11.00000 0.05 0.34 Q17 1 0.3418 0.2186 0.1235 11.00000 0.05 0.32 Q18 1 -0.0540 0.7067 0.0632 11.00000 0.05 0.32 Q19 1 0.3595 0.2383 0.1474 11.00000 0.05 0.31 Q20 1 0.0871 -0.0207 0.2788 11.00000 0.05 0.29 Q21 1 0.2485 0.1785 0.1322 11.00000 0.05 0.29 Q22 1 0.2720 0.6401 0.0687 11.00000 0.05 0.27 Q23 1 0.3819 0.2847 0.3101 11.00000 0.05 0.27 Q24 1 0.8457 0.1602 0.1155 11.00000 0.05 0.27 Q25 1 0.6425 0.2145 0.1026 11.00000 0.05 0.26 ; _shelx_res_checksum 87814 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co Co1 0.34942(8) 0.21932(4) 0.19270(4) 0.0260(3) Uani d . . . 1 . . S S1 -0.02423(16) 0.42618(9) 0.23863(8) 0.0322(4) Uani d . . . 1 . . O O1S 0.9408(7) 0.0611(4) 0.9491(3) 0.0776(17) Uani d . . G 1 . . H H1SA 0.92 0.0379 0.9068 0.116 Uiso d U . G 1 . . H H1SB 0.9 0.031 0.9816 0.116 Uiso d U . G 1 . . O O1 0.2740(4) 0.1692(2) 0.0863(2) 0.0320(9) Uani d . . . 1 . . H H1A 0.3449 0.1677 0.056 0.048 Uiso d U . R 1 . . H H1B 0.2115 0.2018 0.0644 0.048 Uiso d U . R 1 . . O O2 0.0782(5) 0.2907(2) 0.0656(2) 0.0394(10) Uani d . . . 1 . . O O3 0.2466(4) 0.1327(2) 0.2578(2) 0.0325(9) Uani d . . . 1 . . O O4 0.1656(4) 0.0476(2) 0.1645(2) 0.0373(10) Uani d . . . 1 . . N N1 0.4189(5) 0.2893(3) 0.2870(3) 0.0281(10) Uani d . . . 1 . . N N2 0.5381(5) 0.1444(3) 0.1806(3) 0.0291(11) Uani d . . . 1 . . O O8 0.1626(5) 0.2943(3) 0.1873(2) 0.0395(10) Uani d . . . 1 . . C C1 0.5384(6) 0.3361(3) 0.2800(3) 0.0294(13) Uani d . . . 1 . . C C2 0.6113(7) 0.3312(4) 0.2057(3) 0.0356(14) Uani d . . . 1 . . H H2A 0.6502 0.3851 0.1937 0.043 Uiso calc U . R 1 . . H H2B 0.6932 0.2931 0.2108 0.043 Uiso calc U . R 1 . . N N3 0.5118(5) 0.3037(3) 0.1423(2) 0.0289(11) Uani d . . . 1 . . C C4 0.4236(7) 0.3721(4) 0.1056(3) 0.0386(15) Uani d . . . 1 . . H H4A 0.3674 0.3977 0.1447 0.046 Uiso calc U . R 1 . . H H4B 0.3536 0.347 0.0696 0.046 Uiso calc U . R 1 . . C C5 0.5012(7) 0.4407(4) 0.0641(3) 0.0387(14) Uani d . . . 1 . . H H5 0.5901 0.4568 0.0937 0.046 Uiso calc U . R 1 . . C C6 0.3960(8) 0.5140(4) 0.0588(4) 0.0485(17) Uani d . . . 1 . . H H6A 0.3048 0.4965 0.0336 0.058 Uiso calc U . R 1 . . H H6B 0.3744 0.5318 0.1097 0.058 Uiso calc U . R 1 . . C C7 0.5428(9) 0.4151(5) -0.0166(4) 0.059(2) Uani d . . . 1 . . H H7A 0.6147 0.3711 -0.0131 0.071 Uiso calc U . R 1 . . H H7B 0.4565 0.3942 -0.0443 0.071 Uiso calc U . R 1 . . C C8 0.5690(6) 0.0725(3) 0.2169(3) 0.0332(13) Uani d . . . 1 . . H H8 0.5092 0.0558 0.2554 0.04 Uiso calc U . R 1 . . C C9 0.6845(7) 0.0234(4) 0.1992(4) 0.0475(17) Uani d . . . 1 . . H H9 0.7012 -0.0265 0.2243 0.057 Uiso calc U . R 1 . . C C10 0.7760(8) 0.0492(5) 0.1435(4) 0.055(2) Uani d . . . 1 . . H H10 0.8561 0.0171 0.1312 0.066 Uiso calc U . R 1 . . C C11 0.7476(7) 0.1225(4) 0.1065(4) 0.0479(17) Uani d . . . 1 . . H H11 0.8075 0.1406 0.0684 0.057 Uiso calc U . R 1 . . C C12 0.6288(6) 0.1689(4) 0.1267(3) 0.0335(14) Uani d . . . 1 . . C C13 0.5909(7) 0.2513(4) 0.0896(3) 0.0340(14) Uani d . . . 1 . . H H13A 0.6801 0.2788 0.0755 0.041 Uiso calc U . R 1 . . H H13B 0.5304 0.2422 0.0438 0.041 Uiso calc U . R 1 . . C C14 0.0845(6) 0.3199(4) 0.1320(4) 0.0326(13) Uani d . . . 1 . . C C15 -0.0042(6) 0.3955(3) 0.1467(3) 0.0287(12) Uani d . . . 1 . . C C16 0.1217(6) 0.0122(3) 0.2909(3) 0.0314(13) Uani d . . . 1 . . C C17 -0.1352(6) 0.5162(3) 0.1317(3) 0.0340(13) Uani d . . . 1 . . H H17 -0.1828 0.5589 0.1055 0.041 Uiso calc U . R 1 . . C C18 -0.0698(6) 0.4492(3) 0.0959(3) 0.0339(13) Uani d . . . 1 . . H H18 -0.0709 0.442 0.0436 0.041 Uiso calc U . R 1 . . C C19 0.1814(6) 0.0687(3) 0.2332(3) 0.0295(13) Uani d . . . 1 . . C C20 0.5938(7) 0.3854(3) 0.3393(3) 0.0382(15) Uani d . . . 1 . . H H20 0.6771 0.4175 0.3335 0.046 Uiso calc U . R 1 . . C C21 0.5227(8) 0.3855(4) 0.4065(3) 0.0442(17) Uani d . . . 1 . . H H21 0.5588 0.4172 0.4471 0.053 Uiso calc U . R 1 . . C C22 0.3992(8) 0.3392(4) 0.4137(3) 0.0442(16) Uani d . . . 1 . . H H22 0.3498 0.3395 0.4587 0.053 Uiso calc U . R 1 . . C C23 0.3491(7) 0.2921(3) 0.3528(3) 0.0337(13) Uani d . . . 1 . . H H23 0.2641 0.2612 0.3573 0.04 Uiso calc U . R 1 . . O O6 0.1210(12) 0.7639(6) 0.0452(6) 0.061(3) Uiso d . P D 0.5 . . H H6 0.0581 0.8 0.0423 0.092 Uiso calc U P R 0.5 . . C C25 0.1045(18) 0.7175(9) 0.1119(7) 0.061(4) Uiso d . P D 0.5 . . H H25A 0.152 0.6676 0.0949 0.074 Uiso calc U P R 0.5 . . H H25B 0.0009 0.7055 0.1038 0.074 Uiso calc U P R 0.5 . . C C24 0.115(3) 0.6980(16) 0.1966(8) 0.121(8) Uiso d . P D 0.5 . . H H24A 0.2155 0.6975 0.2141 0.182 Uiso calc U P R 0.5 . . H H24B 0.0717 0.6449 0.2052 0.182 Uiso calc U P R 0.5 . . H H24C 0.0626 0.7394 0.2237 0.182 Uiso calc U P R 0.5 . . 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 0.0255(4) 0.0234(4) 0.0292(4) 0.0028(3) 0.0012(3) -0.0042(3) S1 0.0277(8) 0.0311(8) 0.0376(8) 0.0062(6) -0.0014(6) -0.0003(6) O1S 0.099(5) 0.076(4) 0.056(3) 0.012(3) -0.011(4) -0.015(3) O1 0.034(2) 0.034(2) 0.029(2) 0.0039(18) 0.0040(17) -0.0047(17) O2 0.039(2) 0.040(2) 0.039(3) 0.0061(19) -0.0106(19) -0.008(2) O3 0.032(2) 0.028(2) 0.038(2) -0.0020(17) 0.0032(18) -0.0055(17) O4 0.040(2) 0.032(2) 0.040(3) -0.0063(19) -0.0007(19) -0.0014(19) N1 0.037(3) 0.020(2) 0.028(3) -0.001(2) 0.004(2) 0.0010(19) N2 0.024(2) 0.028(2) 0.035(3) 0.002(2) 0.001(2) -0.001(2) O8 0.038(2) 0.042(2) 0.038(2) 0.016(2) -0.006(2) -0.0043(19) C1 0.043(3) 0.023(3) 0.021(3) -0.004(3) -0.002(2) 0.002(2) C2 0.038(3) 0.035(3) 0.035(3) -0.014(3) 0.002(3) 0.004(3) N3 0.040(3) 0.027(2) 0.019(2) 0.007(2) -0.001(2) -0.0047(19) C4 0.044(4) 0.038(3) 0.033(3) 0.009(3) 0.000(3) -0.003(3) C5 0.040(4) 0.046(4) 0.030(3) 0.006(3) 0.006(3) 0.005(3) C6 0.053(4) 0.055(4) 0.039(4) 0.022(3) 0.018(3) 0.008(3) C7 0.068(5) 0.066(5) 0.044(4) 0.032(4) 0.023(4) 0.021(4) C8 0.034(3) 0.024(3) 0.041(3) 0.005(2) 0.004(3) 0.001(2) C9 0.046(4) 0.040(4) 0.057(4) 0.014(3) -0.001(3) 0.004(3) C10 0.051(4) 0.063(5) 0.053(4) 0.038(4) 0.009(4) 0.003(4) C11 0.043(4) 0.056(4) 0.045(4) 0.019(3) 0.013(3) 0.003(3) C12 0.036(3) 0.037(3) 0.028(3) 0.006(3) -0.001(3) -0.003(3) C13 0.036(3) 0.037(3) 0.028(3) 0.004(3) 0.003(3) 0.003(3) C14 0.023(3) 0.033(3) 0.042(4) 0.003(2) 0.003(3) -0.005(3) C15 0.023(3) 0.027(3) 0.036(3) -0.002(2) 0.002(2) -0.005(2) C16 0.027(3) 0.023(3) 0.044(4) 0.003(2) 0.002(3) -0.002(2) C17 0.031(3) 0.029(3) 0.043(4) 0.000(3) 0.004(3) 0.005(3) C18 0.031(3) 0.034(3) 0.037(3) 0.000(3) 0.004(3) 0.005(3) C19 0.021(3) 0.026(3) 0.041(4) 0.003(2) -0.001(2) -0.004(3) C20 0.054(4) 0.028(3) 0.031(3) -0.008(3) -0.006(3) -0.001(3) C21 0.072(5) 0.033(3) 0.027(3) -0.003(3) -0.006(3) -0.004(3) C22 0.065(5) 0.045(4) 0.024(3) 0.006(3) 0.009(3) 0.003(3) C23 0.043(4) 0.030(3) 0.029(3) 0.002(3) 0.008(3) 0.002(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 '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' 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 O3 Co1 N1 . . 93.21(16) ? O3 Co1 O8 . . 91.78(16) ? N1 Co1 O8 . . 86.59(17) ? O3 Co1 N2 . . 93.30(16) ? N1 Co1 N2 . . 99.76(18) ? O8 Co1 N2 . . 171.62(17) ? O3 Co1 O1 . . 95.32(15) ? N1 Co1 O1 . . 169.52(16) ? O8 Co1 O1 . . 87.06(16) ? N2 Co1 O1 . . 85.84(16) ? O3 Co1 N3 . . 164.73(16) ? N1 Co1 N3 . . 78.48(16) ? O8 Co1 N3 . . 100.39(17) ? N2 Co1 N3 . . 75.77(17) ? O1 Co1 N3 . . 94.49(15) ? C15 S1 C16 . 2 91.3(3) ? H1SA O1S H1SB . . 104.5 ? Co1 O1 H1A . . 109.5 ? Co1 O1 H1B . . 110.2 ? H1A O1 H1B . . 104.0 ? C19 O3 Co1 . . 125.9(4) ? C1 N1 C23 . . 118.6(5) ? C1 N1 Co1 . . 117.0(4) ? C23 N1 Co1 . . 124.4(4) ? C12 N2 C8 . . 117.7(5) ? C12 N2 Co1 . . 115.4(4) ? C8 N2 Co1 . . 126.7(4) ? C14 O8 Co1 . . 131.6(4) ? N1 C1 C20 . . 121.7(5) ? N1 C1 C2 . . 116.5(5) ? C20 C1 C2 . . 121.7(5) ? N3 C2 C1 . . 113.3(5) ? N3 C2 H2A . . 108.9 ? C1 C2 H2A . . 108.9 ? N3 C2 H2B . . 108.9 ? C1 C2 H2B . . 108.9 ? H2A C2 H2B . . 107.7 ? C13 N3 C2 . . 110.5(5) ? C13 N3 C4 . . 115.0(4) ? C2 N3 C4 . . 113.9(4) ? C13 N3 Co1 . . 104.5(3) ? C2 N3 Co1 . . 106.3(3) ? C4 N3 Co1 . . 105.7(3) ? N3 C4 C5 . . 119.6(5) ? N3 C4 H4A . . 107.4 ? C5 C4 H4A . . 107.4 ? N3 C4 H4B . . 107.4 ? C5 C4 H4B . . 107.4 ? H4A C4 H4B . . 106.9 ? C4 C5 C6 . . 107.0(5) ? C4 C5 C7 . . 112.6(6) ? C6 C5 C7 . . 109.3(5) ? C4 C5 H5 . . 109.3 ? C6 C5 H5 . . 109.3 ? C7 C5 H5 . . 109.3 ? C7 C6 C5 3_665 . 112.4(5) ? C7 C6 H6A 3_665 . 109.1 ? C5 C6 H6A . . 109.1 ? C7 C6 H6B 3_665 . 109.1 ? C5 C6 H6B . . 109.1 ? H6A C6 H6B . . 107.9 ? C6 C7 C5 3_665 . 111.4(6) ? C6 C7 H7A 3_665 . 109.3 ? C5 C7 H7A . . 109.3 ? C6 C7 H7B 3_665 . 109.3 ? C5 C7 H7B . . 109.3 ? H7A C7 H7B . . 108.0 ? N2 C8 C9 . . 122.7(6) ? N2 C8 H8 . . 118.6 ? C9 C8 H8 . . 118.6 ? C8 C9 C10 . . 118.8(6) ? C8 C9 H9 . . 120.6 ? C10 C9 H9 . . 120.6 ? C11 C10 C9 . . 119.5(6) ? C11 C10 H10 . . 120.3 ? C9 C10 H10 . . 120.3 ? C10 C11 C12 . . 118.7(6) ? C10 C11 H11 . . 120.6 ? C12 C11 H11 . . 120.6 ? N2 C12 C11 . . 122.5(6) ? N2 C12 C13 . . 115.3(5) ? C11 C12 C13 . . 122.2(6) ? N3 C13 C12 . . 110.1(5) ? N3 C13 H13A . . 109.7 ? C12 C13 H13A . . 109.7 ? N3 C13 H13B . . 109.7 ? C12 C13 H13B . . 109.7 ? H13A C13 H13B . . 108.2 ? O8 C14 O2 . . 126.8(5) ? O8 C14 C15 . . 115.5(5) ? O2 C14 C15 . . 117.6(5) ? C18 C15 C14 . . 129.2(5) ? C18 C15 S1 . . 112.0(4) ? C14 C15 S1 . . 118.8(4) ? C17 C16 C19 2_545 . 129.3(5) ? C17 C16 S1 2_545 2_545 111.4(4) ? C19 C16 S1 . 2_545 119.3(4) ? C16 C17 C18 2 . 113.0(5) ? C16 C17 H17 2 . 123.5 ? C18 C17 H17 . . 123.5 ? C15 C18 C17 . . 112.3(5) ? C15 C18 H18 . . 123.8 ? C17 C18 H18 . . 123.8 ? O4 C19 O3 . . 125.8(5) ? O4 C19 C16 . . 117.4(5) ? O3 C19 C16 . . 116.8(5) ? C21 C20 C1 . . 118.5(6) ? C21 C20 H20 . . 120.7 ? C1 C20 H20 . . 120.7 ? C22 C21 C20 . . 120.1(6) ? C22 C21 H21 . . 119.9 ? C20 C21 H21 . . 119.9 ? C21 C22 C23 . . 118.6(6) ? C21 C22 H22 . . 120.7 ? C23 C22 H22 . . 120.7 ? N1 C23 C22 . . 122.4(6) ? N1 C23 H23 . . 118.8 ? C22 C23 H23 . . 118.8 ? C25 O6 H6 . . 109.5 ? O6 C25 C24 . . 157.5(17) ? O6 C25 H25A . . 96.9 ? C24 C25 H25A . . 96.9 ? O6 C25 H25B . . 96.9 ? C24 C25 H25B . . 96.9 ? H25A C25 H25B . . 103.5 ? C25 C24 H24A . . 109.5 ? C25 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C25 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? 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 O3 . 2.064(4) ? Co1 N1 . 2.089(4) ? Co1 O8 . 2.093(4) ? Co1 N2 . 2.125(4) ? Co1 O1 . 2.132(4) ? Co1 N3 . 2.229(5) ? S1 C15 . 1.712(6) ? S1 C16 2 1.721(6) ? O1S H1SA . 0.8493 ? O1S H1SB . 0.8502 ? O1 H1A . 0.8567 ? O1 H1B . 0.8569 ? O2 C14 . 1.263(7) ? O3 C19 . 1.262(6) ? O4 C19 . 1.261(7) ? N1 C1 . 1.339(7) ? N1 C23 . 1.347(7) ? N2 C12 . 1.346(7) ? N2 C8 . 1.353(7) ? O8 C14 . 1.252(7) ? C1 C20 . 1.394(8) ? C1 C2 . 1.496(8) ? C2 N3 . 1.479(7) ? C2 H2A . 0.97 ? C2 H2B . 0.97 ? N3 C13 . 1.471(7) ? N3 C4 . 1.501(7) ? C4 C5 . 1.522(9) ? C4 H4A . 0.97 ? C4 H4B . 0.97 ? C5 C6 . 1.527(8) ? C5 C7 . 1.545(9) ? C5 H5 . 0.98 ? C6 C7 3_665 1.491(10) ? C6 H6A . 0.97 ? C6 H6B . 0.97 ? C7 C6 3_665 1.491(10) ? C7 H7A . 0.97 ? C7 H7B . 0.97 ? C8 C9 . 1.368(8) ? C8 H8 . 0.93 ? C9 C10 . 1.380(10) ? C9 H9 . 0.93 ? C10 C11 . 1.376(9) ? C10 H10 . 0.93 ? C11 C12 . 1.379(8) ? C11 H11 . 0.93 ? C12 C13 . 1.520(8) ? C13 H13A . 0.97 ? C13 H13B . 0.97 ? C14 C15 . 1.496(8) ? C15 C18 . 1.368(8) ? C16 C17 2_545 1.366(8) ? C16 C19 . 1.490(8) ? C16 S1 2_545 1.722(6) ? C17 C16 2 1.366(8) ? C17 C18 . 1.402(8) ? C17 H17 . 0.93 ? C18 H18 . 0.93 ? C20 C21 . 1.375(9) ? C20 H20 . 0.93 ? C21 C22 . 1.365(10) ? C21 H21 . 0.93 ? C22 C23 . 1.379(9) ? C22 H22 . 0.93 ? C23 H23 . 0.93 ? O6 C25 . 1.410(9) ? O6 H6 . 0.82 ? C25 C24 . 1.525(10) ? C25 H25A . 0.97 ? C25 H25B . 0.97 ? C24 H24A . 0.96 ? C24 H24B . 0.96 ? C24 H24C . 0.96 ? 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 C23 N1 C1 C20 . . . . 1.8(8) ? Co1 N1 C1 C20 . . . . 179.8(4) ? C23 N1 C1 C2 . . . . -179.6(5) ? Co1 N1 C1 C2 . . . . -1.7(6) ? N1 C1 C2 N3 . . . . 23.6(7) ? C20 C1 C2 N3 . . . . -157.8(5) ? C1 C2 N3 C13 . . . . -143.8(5) ? C1 C2 N3 C4 . . . . 85.0(6) ? C1 C2 N3 Co1 . . . . -31.0(5) ? C13 N3 C4 C5 . . . . -64.3(7) ? C2 N3 C4 C5 . . . . 64.6(7) ? Co1 N3 C4 C5 . . . . -179.1(4) ? N3 C4 C5 C6 . . . . -159.8(5) ? N3 C4 C5 C7 . . . . 80.1(7) ? C4 C5 C6 C7 . . . 3_665 -177.8(6) ? C7 C5 C6 C7 . . . 3_665 -55.7(9) ? C4 C5 C7 C6 . . . 3_665 173.9(6) ? C6 C5 C7 C6 . . . 3_665 55.1(9) ? C12 N2 C8 C9 . . . . -2.1(8) ? Co1 N2 C8 C9 . . . . 172.1(5) ? N2 C8 C9 C10 . . . . 1.8(10) ? C8 C9 C10 C11 . . . . -1.0(11) ? C9 C10 C11 C12 . . . . 0.6(11) ? C8 N2 C12 C11 . . . . 1.7(9) ? Co1 N2 C12 C11 . . . . -173.2(5) ? C8 N2 C12 C13 . . . . -178.3(5) ? Co1 N2 C12 C13 . . . . 6.8(6) ? C10 C11 C12 N2 . . . . -1.0(10) ? C10 C11 C12 C13 . . . . 179.0(6) ? C2 N3 C13 C12 . . . . 69.9(6) ? C4 N3 C13 C12 . . . . -159.5(5) ? Co1 N3 C13 C12 . . . . -44.1(5) ? N2 C12 C13 N3 . . . . 27.1(7) ? C11 C12 C13 N3 . . . . -153.0(6) ? Co1 O8 C14 O2 . . . . 18.6(9) ? Co1 O8 C14 C15 . . . . -158.2(4) ? O8 C14 C15 C18 . . . . 162.2(6) ? O2 C14 C15 C18 . . . . -15.0(9) ? O8 C14 C15 S1 . . . . -14.2(7) ? O2 C14 C15 S1 . . . . 168.6(4) ? C16 S1 C15 C18 2 . . . 0.0(4) ? C16 S1 C15 C14 2 . . . 177.0(4) ? C14 C15 C18 C17 . . . . -175.9(5) ? S1 C15 C18 C17 . . . . 0.7(6) ? C16 C17 C18 C15 2 . . . -1.3(7) ? Co1 O3 C19 O4 . . . . -1.4(8) ? Co1 O3 C19 C16 . . . . 176.8(3) ? C17 C16 C19 O4 2_545 . . . 173.5(6) ? S1 C16 C19 O4 2_545 . . . -4.6(7) ? C17 C16 C19 O3 2_545 . . . -4.9(9) ? S1 C16 C19 O3 2_545 . . . 177.0(4) ? N1 C1 C20 C21 . . . . -0.1(9) ? C2 C1 C20 C21 . . . . -178.6(6) ? C1 C20 C21 C22 . . . . -1.1(9) ? C20 C21 C22 C23 . . . . 0.7(10) ? C1 N1 C23 C22 . . . . -2.2(8) ? Co1 N1 C23 C22 . . . . 180.0(4) ? C21 C22 C23 N1 . . . . 1.0(9) ?