#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:04:26 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255417 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705195.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_7705195 loop_ _publ_author_name 'Ghosh, Subrata' 'Selvamani, S.' 'Kamilya, Sujit' 'Mehta, Sakshi' 'Mondal, Abhishake' _publ_section_title ; Tuning of Spin Crossover Properties in a Series of Mononuclear Cobalt(II) Complexes Based on Macrocyclic Tetradentate Ligand and Pseudohalide Coligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02546A _journal_year 2020 _chemical_formula_sum 'C24 H32 Co N6 S2' _chemical_formula_weight 527.60 _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 difmap _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2020-05-15 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.056(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.6028(9) _cell_length_b 13.9245(11) _cell_length_c 15.2779(12) _cell_measurement_reflns_used 5246 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.634 _cell_measurement_theta_min 1.979 _cell_volume 2468.3(3) _computing_cell_refinement 'Bruker APEX2' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'CrystalMaker 10.4.2' _computing_publication_material 'Encifer (Allen et al, 2004)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1332 _diffrn_reflns_av_unetI/netI 0.0574 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 106108 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.634 _diffrn_reflns_theta_min 1.979 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.889 _exptl_absorpt_correction_T_max 0.943 _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour Violet _exptl_crystal_density_diffrn 1.420 _exptl_crystal_description Block _exptl_crystal_F_000 1108 _exptl_crystal_size_max 0.600 _exptl_crystal_size_mid 0.400 _exptl_crystal_size_min 0.300 _refine_diff_density_max 0.751 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.085 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_hydrogen_treatment refall _refine_ls_matrix_type full _refine_ls_number_parameters 426 _refine_ls_number_reflns 7597 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.009 _refine_ls_R_factor_all 0.0787 _refine_ls_R_factor_gt 0.0419 _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^)+(0.0373P)^2^+1.7310P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.1026 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5246 _reflns_number_total 7597 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02546a2.cif _cod_data_source_block Complex1_100K _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705195 _shelx_shelxl_version_number 2016/6 _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_min 0.625 _shelx_estimated_absorpt_t_max 0.782 _shelx_res_file ; TITL SIR92 run in space group P 1 21/n 1 shelx.res created by SHELXL-2016/6 at 23:17:10 on 05-May-2020 CELL 0.71073 11.6028 13.9245 15.2779 90.000 90.056 90.000 ZERR 4.00 0.0009 0.0011 0.0012 0.000 0.004 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N S CO UNIT 96 128 24 8 4 MERG 2 FMAP 2 PLAN 25 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.037300 1.731000 FVAR 0.12057 CO1 5 0.430976 0.144500 0.749232 11.00000 0.01706 0.01556 = 0.01364 -0.00174 0.00261 -0.00317 S1 4 0.447246 0.371119 0.518734 11.00000 0.04307 0.03074 = 0.03086 0.00225 0.00252 0.00199 S2 4 0.350588 0.339745 0.995573 11.00000 0.04083 0.04099 = 0.02038 -0.00336 -0.00218 0.02483 N1 3 0.634800 0.150431 0.761041 11.00000 0.01493 0.01465 = 0.01415 -0.00085 0.00181 0.00021 N3 3 0.262746 0.053901 0.739275 11.00000 0.01598 0.01348 = 0.01477 -0.00003 0.00038 -0.00022 N2 3 0.479965 0.043425 0.665293 11.00000 0.01668 0.01261 = 0.01531 0.00073 0.00050 0.00230 N4 3 0.459875 0.042408 0.837583 11.00000 0.01745 0.01139 = 0.01476 -0.00048 0.00045 0.00028 C19 1 0.673651 0.256856 0.887892 11.00000 0.01943 0.02975 = 0.02038 -0.00842 0.00390 -0.00577 N6 3 0.385646 0.234666 0.842512 11.00000 0.02057 0.02387 = 0.01899 0.00309 -0.00117 -0.00472 C1 1 0.427721 0.294270 0.597979 11.00000 0.01840 0.02220 = 0.02972 -0.01218 0.00077 -0.00021 C16 1 0.667200 0.067428 0.816926 11.00000 0.01713 0.01886 = 0.02009 0.00152 0.00123 0.00318 C15 1 0.567186 0.013395 0.856493 11.00000 0.02005 0.01276 = 0.01435 -0.00321 -0.00118 0.00053 C6 1 0.558310 -0.101073 0.558342 11.00000 0.02638 0.01795 = 0.01728 -0.00391 -0.00207 0.00825 C8 1 0.410767 -0.030439 0.645904 11.00000 0.01815 0.01211 = 0.01423 0.00076 -0.00266 0.00087 N5 3 0.414753 0.239686 0.654098 11.00000 0.02049 0.02400 = 0.02390 -0.00786 0.00580 -0.00557 C17 1 0.695457 0.242235 0.790093 11.00000 0.01559 0.01778 = 0.01971 -0.00226 0.00171 -0.00245 C4 1 0.589538 0.044999 0.636402 11.00000 0.01636 0.01622 = 0.01362 0.00110 0.00120 0.00313 C21 1 0.152625 0.099821 0.704683 11.00000 0.01502 0.01433 = 0.02221 0.00147 -0.00049 -0.00042 C23 1 0.168020 0.120678 0.606989 11.00000 0.02060 0.02462 = 0.02159 0.00418 -0.00387 -0.00231 C22 1 0.047763 0.034308 0.717121 11.00000 0.01695 0.02132 = 0.03077 -0.00018 0.00042 -0.00423 C24 1 0.133194 0.195122 0.751514 11.00000 0.01875 0.01760 = 0.03017 -0.00112 -0.00176 0.00209 C7 1 0.447836 -0.103919 0.591161 11.00000 0.02282 0.01378 = 0.01733 -0.00156 -0.00561 0.00265 C10 1 0.253387 0.027262 0.833497 11.00000 0.01894 0.01613 = 0.01901 0.00351 0.00250 -0.00259 C3 1 0.661732 0.127194 0.668358 11.00000 0.01712 0.01749 = 0.01653 -0.00187 0.00412 0.00044 C2 1 0.369810 0.278433 0.905927 11.00000 0.01578 0.02283 = 0.02223 0.00674 -0.00222 0.00077 C11 1 0.368165 -0.008198 0.865763 11.00000 0.02196 0.01257 = 0.01568 0.00068 0.00151 -0.00184 C5 1 0.630977 -0.026416 0.582297 11.00000 0.01859 0.01948 = 0.01777 -0.00028 0.00023 0.00540 C9 1 0.293459 -0.033611 0.688116 11.00000 0.01968 0.01176 = 0.02053 -0.00080 -0.00079 -0.00084 C14 1 0.585540 -0.067241 0.908445 11.00000 0.02516 0.01803 = 0.02057 0.00305 -0.00160 0.00399 C20 1 0.824928 0.237784 0.772864 11.00000 0.01557 0.02772 = 0.02170 -0.00493 0.00244 -0.00280 C12 1 0.381609 -0.089206 0.916837 11.00000 0.02651 0.01708 = 0.02199 0.00578 0.00018 -0.00423 C13 1 0.492742 -0.118542 0.938947 11.00000 0.03337 0.01657 = 0.02375 0.00721 -0.00034 0.00154 C18 1 0.643684 0.327241 0.741798 11.00000 0.02205 0.01482 = 0.02870 -0.00118 0.00269 -0.00420 H10B 2 0.229614 0.085181 0.866009 11.00000 0.01012 H3B 2 0.649286 0.185426 0.632195 11.00000 0.01278 H9A 2 0.238984 -0.047541 0.641919 11.00000 0.02092 H3A 2 0.745257 0.107702 0.661244 11.00000 0.01413 H18B 2 0.653879 0.325192 0.678936 11.00000 0.01761 H20B 2 0.837680 0.235934 0.712817 11.00000 0.01763 H6 2 0.583537 -0.147953 0.523038 11.00000 0.01365 H18A 2 0.680582 0.385963 0.763108 11.00000 0.02097 H10A 2 0.199599 -0.020272 0.843588 11.00000 0.01754 H16A 2 0.718863 0.086798 0.863706 11.00000 0.02457 H14 2 0.661427 -0.084663 0.922180 11.00000 0.01957 H20A 2 0.858877 0.182290 0.800188 11.00000 0.02499 H22C 2 0.058348 -0.027387 0.692055 11.00000 0.03062 H24C 2 0.197765 0.238125 0.743842 11.00000 0.01697 H18C 2 0.563170 0.333747 0.755629 11.00000 0.02424 H19C 2 0.598162 0.243164 0.903747 11.00000 0.02494 H24B 2 0.118470 0.186243 0.810211 11.00000 0.03083 H16B 2 0.710404 0.019472 0.781845 11.00000 0.04186 H20C 2 0.863617 0.296513 0.797513 11.00000 0.03775 H22A 2 -0.021103 0.065966 0.688753 11.00000 0.02795 H19A 2 0.724551 0.217332 0.921776 11.00000 0.03348 H9B 2 0.293795 -0.089179 0.724753 11.00000 0.02360 H5 2 0.711396 -0.023115 0.562656 11.00000 0.02272 H22B 2 0.028944 0.022405 0.775991 11.00000 0.02487 H23B 2 0.239523 0.157078 0.596222 11.00000 0.03159 H23A 2 0.105748 0.157907 0.589312 11.00000 0.03397 H7 2 0.400879 -0.156297 0.577770 11.00000 0.02209 H19B 2 0.689920 0.321689 0.901243 11.00000 0.03154 H12 2 0.314440 -0.121302 0.937270 11.00000 0.02829 H13 2 0.502361 -0.172817 0.973946 11.00000 0.03790 H23C 2 0.168687 0.062193 0.572097 11.00000 0.03837 H24A 2 0.065611 0.227319 0.722682 11.00000 0.03319 HKLF 4 REM SIR92 run in space group P 1 21/n 1 REM R1 = 0.0419 for 5246 Fo > 4sig(Fo) and 0.0787 for all 7597 data REM 426 parameters refined using 0 restraints END WGHT 0.0359 1.8146 REM Highest difference peak 0.751, deepest hole -0.494, 1-sigma level 0.085 Q1 1 0.5194 0.3492 0.5117 11.00000 0.05 0.75 Q2 1 0.3581 -0.0366 0.6686 11.00000 0.05 0.40 Q3 1 0.4872 0.0987 0.6920 11.00000 0.05 0.40 Q4 1 0.6203 0.0140 0.6072 11.00000 0.05 0.39 Q5 1 0.1210 0.0588 0.7184 11.00000 0.05 0.37 Q6 1 0.4997 -0.1028 0.5616 11.00000 0.05 0.36 Q7 1 0.6217 0.0903 0.6466 11.00000 0.05 0.35 Q8 1 0.7574 0.2412 0.7840 11.00000 0.05 0.34 Q9 1 0.5614 -0.0413 0.8861 11.00000 0.05 0.34 Q10 1 0.8064 -0.1440 0.9959 11.00000 0.05 0.34 Q11 1 0.4566 0.0614 0.7062 11.00000 0.05 0.34 Q12 1 0.4405 0.2217 0.5976 11.00000 0.05 0.34 Q13 1 0.6093 0.0350 0.8333 11.00000 0.05 0.33 Q14 1 0.5263 0.0392 0.6735 11.00000 0.05 0.33 Q15 1 0.1504 0.1399 0.7230 11.00000 0.05 0.33 Q16 1 0.4232 -0.0614 0.6156 11.00000 0.05 0.33 Q17 1 0.3793 0.2601 0.6113 11.00000 0.05 0.33 Q18 1 0.3065 0.3595 1.0459 11.00000 0.05 0.33 Q19 1 0.1489 0.1083 0.6527 11.00000 0.05 0.32 Q20 1 0.6765 0.2878 0.7756 11.00000 0.05 0.32 Q21 1 0.3374 0.2427 0.8778 11.00000 0.05 0.32 Q22 1 0.8207 -0.0363 0.9583 11.00000 0.05 0.31 Q23 1 0.4976 0.0767 0.6367 11.00000 0.05 0.31 Q24 1 0.0984 0.0172 0.4566 11.00000 0.05 0.31 Q25 1 0.5663 -0.0679 0.9433 11.00000 0.05 0.30 ; _shelx_res_checksum 91833 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_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.43098(2) 0.14450(2) 0.74923(2) 0.01542(8) Uani 1 1 d . . . . . S1 S 0.44725(6) 0.37112(5) 0.51873(4) 0.03489(16) Uani 1 1 d . . . . . S2 S 0.35059(6) 0.33974(5) 0.99557(4) 0.03407(16) Uani 1 1 d . . . . . N1 N 0.63480(14) 0.15043(12) 0.76104(11) 0.0146(3) Uani 1 1 d . . . . . N3 N 0.26275(14) 0.05390(12) 0.73928(11) 0.0147(3) Uani 1 1 d . . . . . N2 N 0.47996(14) 0.04342(12) 0.66529(11) 0.0149(3) Uani 1 1 d . . . . . N4 N 0.45988(15) 0.04241(12) 0.83758(11) 0.0145(3) Uani 1 1 d . . . . . C19 C 0.6737(2) 0.25686(19) 0.88789(15) 0.0232(5) Uani 1 1 d . . . . . N6 N 0.38565(16) 0.23467(14) 0.84251(12) 0.0211(4) Uani 1 1 d . . . . . C1 C 0.42772(19) 0.29427(16) 0.59798(16) 0.0234(5) Uani 1 1 d . . . . . C16 C 0.66720(19) 0.06743(16) 0.81693(15) 0.0187(4) Uani 1 1 d . . . . . C15 C 0.56719(18) 0.01340(14) 0.85649(13) 0.0157(4) Uani 1 1 d . . . . . C6 C 0.5583(2) -0.10107(16) 0.55834(14) 0.0205(4) Uani 1 1 d . . . . . C8 C 0.41077(18) -0.03044(14) 0.64590(13) 0.0148(4) Uani 1 1 d . . . . . N5 N 0.41475(16) 0.23969(14) 0.65410(13) 0.0228(4) Uani 1 1 d . . . . . C17 C 0.69546(18) 0.24224(15) 0.79009(14) 0.0177(4) Uani 1 1 d . . . . . C4 C 0.58954(17) 0.04500(14) 0.63640(13) 0.0154(4) Uani 1 1 d . . . . . C21 C 0.15262(18) 0.09982(14) 0.70468(14) 0.0172(4) Uani 1 1 d . . . . . C23 C 0.1680(2) 0.12068(18) 0.60699(15) 0.0223(5) Uani 1 1 d . . . . . C22 C 0.0478(2) 0.03431(17) 0.71712(17) 0.0230(5) Uani 1 1 d . . . . . C24 C 0.1332(2) 0.19512(16) 0.75151(17) 0.0222(5) Uani 1 1 d . . . . . C7 C 0.44784(19) -0.10392(15) 0.59116(14) 0.0180(4) Uani 1 1 d . . . . . C10 C 0.25339(19) 0.02726(15) 0.83350(14) 0.0180(4) Uani 1 1 d . . . . . C3 C 0.66173(18) 0.12719(15) 0.66836(14) 0.0170(4) Uani 1 1 d . . . . . C2 C 0.36981(18) 0.27843(16) 0.90593(15) 0.0203(4) Uani 1 1 d . . . . . C11 C 0.36817(18) -0.00820(14) 0.86576(13) 0.0167(4) Uani 1 1 d . . . . . C5 C 0.63098(19) -0.02642(15) 0.58230(14) 0.0186(4) Uani 1 1 d . . . . . C9 C 0.29346(19) -0.03361(15) 0.68812(14) 0.0173(4) Uani 1 1 d . . . . . C14 C 0.5855(2) -0.06724(16) 0.90844(15) 0.0213(4) Uani 1 1 d . . . . . C20 C 0.82493(19) 0.23778(18) 0.77286(16) 0.0217(5) Uani 1 1 d . . . . . C12 C 0.3816(2) -0.08921(16) 0.91684(15) 0.0219(5) Uani 1 1 d . . . . . C13 C 0.4927(2) -0.11854(16) 0.93895(16) 0.0246(5) Uani 1 1 d . . . . . C18 C 0.6437(2) 0.32724(16) 0.74180(16) 0.0219(5) Uani 1 1 d . . . . . H10B H 0.2296(18) 0.0852(16) 0.8660(14) 0.010(5) Uiso 1 1 d . . . . . H3B H 0.6493(18) 0.1854(17) 0.6322(14) 0.013(6) Uiso 1 1 d . . . . . H9A H 0.239(2) -0.0475(17) 0.6419(16) 0.021(6) Uiso 1 1 d . . . . . H3A H 0.745(2) 0.1077(16) 0.6612(14) 0.014(6) Uiso 1 1 d . . . . . H18B H 0.654(2) 0.3252(17) 0.6789(16) 0.018(6) Uiso 1 1 d . . . . . H20B H 0.838(2) 0.2359(17) 0.7128(16) 0.018(6) Uiso 1 1 d . . . . . H6 H 0.5835(19) -0.1480(16) 0.5230(15) 0.014(6) Uiso 1 1 d . . . . . H18A H 0.681(2) 0.3860(18) 0.7631(16) 0.021(6) Uiso 1 1 d . . . . . H10A H 0.200(2) -0.0203(17) 0.8436(15) 0.018(6) Uiso 1 1 d . . . . . H16A H 0.719(2) 0.0868(18) 0.8637(17) 0.025(7) Uiso 1 1 d . . . . . H14 H 0.661(2) -0.0847(17) 0.9222(15) 0.020(6) Uiso 1 1 d . . . . . H20A H 0.859(2) 0.1823(19) 0.8002(17) 0.025(7) Uiso 1 1 d . . . . . H22C H 0.058(2) -0.027(2) 0.6921(17) 0.031(7) Uiso 1 1 d . . . . . H24C H 0.198(2) 0.2381(17) 0.7438(15) 0.017(6) Uiso 1 1 d . . . . . H18C H 0.563(2) 0.3337(18) 0.7556(16) 0.024(7) Uiso 1 1 d . . . . . H19C H 0.598(2) 0.2432(18) 0.9037(16) 0.025(7) Uiso 1 1 d . . . . . H24B H 0.118(2) 0.1862(19) 0.8102(18) 0.031(7) Uiso 1 1 d . . . . . H16B H 0.710(2) 0.019(2) 0.7818(19) 0.042(8) Uiso 1 1 d . . . . . H20C H 0.864(2) 0.297(2) 0.7975(18) 0.038(8) Uiso 1 1 d . . . . . H22A H -0.021(2) 0.0660(19) 0.6888(17) 0.028(7) Uiso 1 1 d . . . . . H19A H 0.725(2) 0.217(2) 0.9218(18) 0.033(8) Uiso 1 1 d . . . . . H9B H 0.294(2) -0.0892(18) 0.7248(16) 0.024(7) Uiso 1 1 d . . . . . H5 H 0.711(2) -0.0231(17) 0.5627(16) 0.023(7) Uiso 1 1 d . . . . . H22B H 0.029(2) 0.0224(18) 0.7760(17) 0.025(7) Uiso 1 1 d . . . . . H23B H 0.240(2) 0.1571(19) 0.5962(17) 0.032(7) Uiso 1 1 d . . . . . H23A H 0.106(2) 0.1579(19) 0.5893(18) 0.034(8) Uiso 1 1 d . . . . . H7 H 0.401(2) -0.1563(17) 0.5778(16) 0.022(6) Uiso 1 1 d . . . . . H19B H 0.690(2) 0.322(2) 0.9012(17) 0.032(7) Uiso 1 1 d . . . . . H12 H 0.314(2) -0.1213(19) 0.9373(17) 0.028(7) Uiso 1 1 d . . . . . H13 H 0.502(2) -0.173(2) 0.9739(18) 0.038(8) Uiso 1 1 d . . . . . H23C H 0.169(2) 0.062(2) 0.5721(18) 0.038(8) Uiso 1 1 d . . . . . H24A H 0.066(2) 0.227(2) 0.7227(18) 0.033(7) Uiso 1 1 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 Co1 0.01706(14) 0.01556(13) 0.01364(13) -0.00174(11) 0.00261(10) -0.00317(11) S1 0.0431(4) 0.0307(3) 0.0309(3) 0.0022(3) 0.0025(3) 0.0020(3) S2 0.0408(4) 0.0410(4) 0.0204(3) -0.0034(3) -0.0022(3) 0.0248(3) N1 0.0149(8) 0.0146(8) 0.0141(8) -0.0009(7) 0.0018(6) 0.0002(6) N3 0.0160(8) 0.0135(8) 0.0148(8) 0.0000(6) 0.0004(6) -0.0002(6) N2 0.0167(8) 0.0126(8) 0.0153(8) 0.0007(6) 0.0005(7) 0.0023(6) N4 0.0174(8) 0.0114(8) 0.0148(8) -0.0005(6) 0.0004(7) 0.0003(6) C19 0.0194(11) 0.0298(13) 0.0204(11) -0.0084(9) 0.0039(9) -0.0058(9) N6 0.0206(9) 0.0239(10) 0.0190(9) 0.0031(7) -0.0012(7) -0.0047(7) C1 0.0184(11) 0.0222(11) 0.0297(12) -0.0122(10) 0.0008(9) -0.0002(8) C16 0.0171(10) 0.0189(10) 0.0201(11) 0.0015(8) 0.0012(8) 0.0032(8) C15 0.0201(10) 0.0128(9) 0.0144(9) -0.0032(7) -0.0012(8) 0.0005(7) C6 0.0264(12) 0.0179(10) 0.0173(10) -0.0039(8) -0.0021(9) 0.0083(9) C8 0.0182(10) 0.0121(9) 0.0142(9) 0.0008(7) -0.0027(8) 0.0009(7) N5 0.0205(9) 0.0240(10) 0.0239(10) -0.0079(8) 0.0058(8) -0.0056(8) C17 0.0156(10) 0.0178(10) 0.0197(10) -0.0023(8) 0.0017(8) -0.0024(8) C4 0.0164(10) 0.0162(9) 0.0136(9) 0.0011(7) 0.0012(7) 0.0031(7) C21 0.0150(10) 0.0143(9) 0.0222(11) 0.0015(8) -0.0005(8) -0.0004(8) C23 0.0206(11) 0.0246(12) 0.0216(11) 0.0042(9) -0.0039(9) -0.0023(9) C22 0.0170(11) 0.0213(11) 0.0308(13) -0.0002(10) 0.0004(9) -0.0042(9) C24 0.0187(11) 0.0176(10) 0.0302(13) -0.0011(9) -0.0018(9) 0.0021(8) C7 0.0228(11) 0.0138(10) 0.0173(10) -0.0016(8) -0.0056(8) 0.0027(8) C10 0.0189(10) 0.0161(10) 0.0190(10) 0.0035(8) 0.0025(8) -0.0026(8) C3 0.0171(10) 0.0175(10) 0.0165(10) -0.0019(8) 0.0041(8) 0.0004(8) C2 0.0158(10) 0.0228(11) 0.0222(11) 0.0067(9) -0.0022(8) 0.0008(8) C11 0.0220(10) 0.0126(9) 0.0157(10) 0.0007(7) 0.0015(8) -0.0018(8) C5 0.0186(10) 0.0195(10) 0.0178(10) -0.0003(8) 0.0002(8) 0.0054(8) C9 0.0197(10) 0.0118(9) 0.0205(10) -0.0008(8) -0.0008(8) -0.0008(8) C14 0.0252(12) 0.0180(10) 0.0206(11) 0.0030(8) -0.0016(9) 0.0040(9) C20 0.0156(10) 0.0277(12) 0.0217(12) -0.0049(9) 0.0024(8) -0.0028(9) C12 0.0265(12) 0.0171(10) 0.0220(11) 0.0058(8) 0.0002(9) -0.0042(9) C13 0.0334(13) 0.0166(10) 0.0237(12) 0.0072(9) -0.0003(10) 0.0015(9) C18 0.0220(11) 0.0148(10) 0.0287(13) -0.0012(9) 0.0027(9) -0.0042(8) 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' 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 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 Co1 N5 94.55(8) . . ? N6 Co1 N2 173.86(7) . . ? N5 Co1 N2 91.57(7) . . ? N6 Co1 N4 90.55(7) . . ? N5 Co1 N4 174.11(7) . . ? N2 Co1 N4 83.32(7) . . ? N6 Co1 N3 99.67(7) . . ? N5 Co1 N3 103.66(7) . . ? N2 Co1 N3 79.31(6) . . ? N4 Co1 N3 78.34(7) . . ? N6 Co1 N1 100.92(7) . . ? N5 Co1 N1 97.28(7) . . ? N2 Co1 N1 77.76(6) . . ? N4 Co1 N1 78.81(6) . . ? N3 Co1 N1 149.20(6) . . ? C16 N1 C3 108.97(16) . . ? C16 N1 C17 111.62(16) . . ? C3 N1 C17 111.25(15) . . ? C16 N1 Co1 105.56(12) . . ? C3 N1 Co1 97.50(12) . . ? C17 N1 Co1 120.72(12) . . ? C10 N3 C9 108.69(16) . . ? C10 N3 C21 112.19(16) . . ? C9 N3 C21 111.23(16) . . ? C10 N3 Co1 97.68(12) . . ? C9 N3 Co1 106.03(12) . . ? C21 N3 Co1 119.87(12) . . ? C8 N2 C4 120.44(17) . . ? C8 N2 Co1 121.02(14) . . ? C4 N2 Co1 118.08(14) . . ? C15 N4 C11 120.49(18) . . ? C15 N4 Co1 121.18(14) . . ? C11 N4 Co1 117.27(14) . . ? C17 C19 H19C 112.6(16) . . ? C17 C19 H19A 110.4(16) . . ? H19C C19 H19A 109(2) . . ? C17 C19 H19B 107.8(16) . . ? H19C C19 H19B 109(2) . . ? H19A C19 H19B 108(2) . . ? C2 N6 Co1 168.99(18) . . ? N5 C1 S1 179.5(2) . . ? N1 C16 C15 115.07(17) . . ? N1 C16 H16A 111.3(15) . . ? C15 C16 H16A 108.5(15) . . ? N1 C16 H16B 109.9(17) . . ? C15 C16 H16B 105.7(17) . . ? H16A C16 H16B 106(2) . . ? N4 C15 C14 120.52(19) . . ? N4 C15 C16 118.54(18) . . ? C14 C15 C16 120.88(19) . . ? C7 C6 C5 119.4(2) . . ? C7 C6 H6 120.2(15) . . ? C5 C6 H6 120.4(15) . . ? N2 C8 C7 120.87(19) . . ? N2 C8 C9 118.02(17) . . ? C7 C8 C9 121.06(18) . . ? C1 N5 Co1 167.03(19) . . ? C18 C17 N1 109.25(17) . . ? C18 C17 C20 109.68(19) . . ? N1 C17 C20 111.70(17) . . ? C18 C17 C19 107.77(19) . . ? N1 C17 C19 108.61(17) . . ? C20 C17 C19 109.73(18) . . ? N2 C4 C5 120.95(19) . . ? N2 C4 C3 115.66(17) . . ? C5 C4 C3 123.38(19) . . ? N3 C21 C24 109.09(17) . . ? N3 C21 C23 108.62(17) . . ? C24 C21 C23 108.05(18) . . ? N3 C21 C22 111.90(17) . . ? C24 C21 C22 110.01(18) . . ? C23 C21 C22 109.09(19) . . ? C21 C23 H23B 111.0(16) . . ? C21 C23 H23A 107.3(17) . . ? H23B C23 H23A 109(2) . . ? C21 C23 H23C 112.1(17) . . ? H23B C23 H23C 109(2) . . ? H23A C23 H23C 108(2) . . ? C21 C22 H22C 112.7(16) . . ? C21 C22 H22A 108.4(15) . . ? H22C C22 H22A 109(2) . . ? C21 C22 H22B 114.1(16) . . ? H22C C22 H22B 105(2) . . ? H22A C22 H22B 108(2) . . ? C21 C24 H24C 111.6(14) . . ? C21 C24 H24B 111.6(17) . . ? H24C C24 H24B 110(2) . . ? C21 C24 H24A 107.4(16) . . ? H24C C24 H24A 106(2) . . ? H24B C24 H24A 110(2) . . ? C6 C7 C8 119.1(2) . . ? C6 C7 H7 119.1(15) . . ? C8 C7 H7 121.8(15) . . ? N3 C10 C11 109.46(17) . . ? N3 C10 H10B 107.7(13) . . ? C11 C10 H10B 110.6(13) . . ? N3 C10 H10A 112.9(15) . . ? C11 C10 H10A 108.0(15) . . ? H10B C10 H10A 108.2(19) . . ? N1 C3 C4 111.01(16) . . ? N1 C3 H3B 108.8(13) . . ? C4 C3 H3B 111.2(13) . . ? N1 C3 H3A 111.3(13) . . ? C4 C3 H3A 107.2(13) . . ? H3B C3 H3A 107.4(18) . . ? N6 C2 S2 178.7(2) . . ? N4 C11 C12 121.3(2) . . ? N4 C11 C10 115.04(18) . . ? C12 C11 C10 123.60(19) . . ? C4 C5 C6 119.1(2) . . ? C4 C5 H5 118.8(14) . . ? C6 C5 H5 122.1(14) . . ? N3 C9 C8 114.63(17) . . ? N3 C9 H9A 113.0(14) . . ? C8 C9 H9A 106.5(14) . . ? N3 C9 H9B 110.8(15) . . ? C8 C9 H9B 105.7(15) . . ? H9A C9 H9B 106(2) . . ? C13 C14 C15 119.6(2) . . ? C13 C14 H14 121.7(15) . . ? C15 C14 H14 118.7(15) . . ? C17 C20 H20B 109.2(15) . . ? C17 C20 H20A 111.1(15) . . ? H20B C20 H20A 110(2) . . ? C17 C20 H20C 110.0(16) . . ? H20B C20 H20C 109(2) . . ? H20A C20 H20C 108(2) . . ? C11 C12 C13 118.7(2) . . ? C11 C12 H12 118.5(16) . . ? C13 C12 H12 122.7(16) . . ? C14 C13 C12 119.4(2) . . ? C14 C13 H13 121.5(18) . . ? C12 C13 H13 119.1(18) . . ? C17 C18 H18B 114.2(14) . . ? C17 C18 H18A 108.5(14) . . ? H18B C18 H18A 108(2) . . ? C17 C18 H18C 110.5(15) . . ? H18B C18 H18C 110(2) . . ? H18A C18 H18C 106(2) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N6 1.971(2) . ? Co1 N5 1.976(2) . ? Co1 N2 1.9874(17) . ? Co1 N4 1.9886(17) . ? Co1 N3 2.3290(17) . ? Co1 N1 2.3731(17) . ? S1 C1 1.632(3) . ? S2 C2 1.629(2) . ? N1 C16 1.485(3) . ? N1 C3 1.486(3) . ? N1 C17 1.525(3) . ? N3 C10 1.491(3) . ? N3 C9 1.491(3) . ? N3 C21 1.523(3) . ? N2 C8 1.338(3) . ? N2 C4 1.346(3) . ? N4 C15 1.340(3) . ? N4 C11 1.347(3) . ? C19 C17 1.529(3) . ? C19 H19C 0.93(3) . ? C19 H19A 0.96(3) . ? C19 H19B 0.94(3) . ? N6 C2 1.159(3) . ? C1 N5 1.156(3) . ? C16 C15 1.510(3) . ? C16 H16A 0.97(3) . ? C16 H16B 0.99(3) . ? C15 C14 1.391(3) . ? C6 C7 1.377(3) . ? C6 C5 1.387(3) . ? C6 H6 0.90(2) . ? C8 C7 1.390(3) . ? C8 C9 1.507(3) . ? C17 C18 1.518(3) . ? C17 C20 1.527(3) . ? C4 C5 1.380(3) . ? C4 C3 1.500(3) . ? C21 C24 1.524(3) . ? C21 C23 1.531(3) . ? C21 C22 1.533(3) . ? C23 H23B 0.99(3) . ? C23 H23A 0.93(3) . ? C23 H23C 0.97(3) . ? C22 H22C 0.95(3) . ? C22 H22A 1.01(3) . ? C22 H22B 0.94(3) . ? C24 H24C 0.97(2) . ? C24 H24B 0.92(3) . ? C24 H24A 1.00(3) . ? C7 H7 0.93(2) . ? C10 C11 1.503(3) . ? C10 H10B 0.99(2) . ? C10 H10A 0.92(2) . ? C3 H3B 0.99(2) . ? C3 H3A 1.01(2) . ? C11 C12 1.380(3) . ? C5 H5 0.98(2) . ? C9 H9A 0.97(2) . ? C9 H9B 0.95(3) . ? C14 C13 1.374(3) . ? C14 H14 0.94(2) . ? C20 H20B 0.93(2) . ? C20 H20A 0.96(3) . ? C20 H20C 1.01(3) . ? C12 C13 1.394(3) . ? C12 H12 0.95(3) . ? C13 H13 0.93(3) . ? C18 H18B 0.97(2) . ? C18 H18A 0.98(2) . ? C18 H18C 0.96(3) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 N1 C16 C15 -110.34(19) . . . . ? C17 N1 C16 C15 126.40(19) . . . . ? Co1 N1 C16 C15 -6.5(2) . . . . ? C11 N4 C15 C14 -2.6(3) . . . . ? Co1 N4 C15 C14 -170.47(15) . . . . ? C11 N4 C15 C16 174.72(18) . . . . ? Co1 N4 C15 C16 6.8(2) . . . . ? N1 C16 C15 N4 1.1(3) . . . . ? N1 C16 C15 C14 178.43(19) . . . . ? C4 N2 C8 C7 -4.1(3) . . . . ? Co1 N2 C8 C7 -176.21(15) . . . . ? C4 N2 C8 C9 173.40(18) . . . . ? Co1 N2 C8 C9 1.3(2) . . . . ? C16 N1 C17 C18 -170.03(17) . . . . ? C3 N1 C17 C18 68.0(2) . . . . ? Co1 N1 C17 C18 -45.2(2) . . . . ? C16 N1 C17 C20 68.4(2) . . . . ? C3 N1 C17 C20 -53.5(2) . . . . ? Co1 N1 C17 C20 -166.71(14) . . . . ? C16 N1 C17 C19 -52.7(2) . . . . ? C3 N1 C17 C19 -174.67(17) . . . . ? Co1 N1 C17 C19 72.13(19) . . . . ? C8 N2 C4 C5 3.7(3) . . . . ? Co1 N2 C4 C5 176.01(15) . . . . ? C8 N2 C4 C3 -175.11(18) . . . . ? Co1 N2 C4 C3 -2.8(2) . . . . ? C10 N3 C21 C24 64.9(2) . . . . ? C9 N3 C21 C24 -173.10(17) . . . . ? Co1 N3 C21 C24 -48.7(2) . . . . ? C10 N3 C21 C23 -177.54(17) . . . . ? C9 N3 C21 C23 -55.5(2) . . . . ? Co1 N3 C21 C23 68.84(19) . . . . ? C10 N3 C21 C22 -57.0(2) . . . . ? C9 N3 C21 C22 64.9(2) . . . . ? Co1 N3 C21 C22 -170.67(14) . . . . ? C5 C6 C7 C8 1.6(3) . . . . ? N2 C8 C7 C6 1.5(3) . . . . ? C9 C8 C7 C6 -175.99(19) . . . . ? C9 N3 C10 C11 62.3(2) . . . . ? C21 N3 C10 C11 -174.30(16) . . . . ? Co1 N3 C10 C11 -47.59(16) . . . . ? C16 N1 C3 C4 64.3(2) . . . . ? C17 N1 C3 C4 -172.17(16) . . . . ? Co1 N1 C3 C4 -45.01(17) . . . . ? N2 C4 C3 N1 37.9(2) . . . . ? C5 C4 C3 N1 -140.8(2) . . . . ? C15 N4 C11 C12 2.0(3) . . . . ? Co1 N4 C11 C12 170.34(16) . . . . ? C15 N4 C11 C10 -174.90(18) . . . . ? Co1 N4 C11 C10 -6.5(2) . . . . ? N3 C10 C11 N4 41.7(2) . . . . ? N3 C10 C11 C12 -135.1(2) . . . . ? N2 C4 C5 C6 -0.6(3) . . . . ? C3 C4 C5 C6 178.1(2) . . . . ? C7 C6 C5 C4 -2.0(3) . . . . ? C10 N3 C9 C8 -114.24(19) . . . . ? C21 N3 C9 C8 121.76(19) . . . . ? Co1 N3 C9 C8 -10.1(2) . . . . ? N2 C8 C9 N3 7.1(3) . . . . ? C7 C8 C9 N3 -175.42(18) . . . . ? N4 C15 C14 C13 1.4(3) . . . . ? C16 C15 C14 C13 -175.9(2) . . . . ? N4 C11 C12 C13 -0.2(3) . . . . ? C10 C11 C12 C13 176.4(2) . . . . ? C15 C14 C13 C12 0.4(3) . . . . ? C11 C12 C13 C14 -1.0(3) . . . . ?