#------------------------------------------------------------------------------ #$Date: 2020-08-18 05:04:26 +0300 (Tue, 18 Aug 2020) $ #$Revision: 255417 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705192.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_7705192 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 geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-05-15 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90.076(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.801(3) _cell_length_b 14.041(3) _cell_length_c 15.332(4) _cell_measurement_reflns_used 4665 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 31.196 _cell_measurement_theta_min 1.967 _cell_volume 2540.5(11) _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-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 296(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.970 _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 0.0679 _diffrn_reflns_av_unetI/netI 0.0612 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 38737 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.196 _diffrn_reflns_theta_min 1.967 _diffrn_source 'sealed tube' _exptl_absorpt_coefficient_mu 0.864 _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 1.379 _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 0.491 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.062 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 298 _refine_ls_number_reflns 7983 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.017 _refine_ls_R_factor_all 0.0988 _refine_ls_R_factor_gt 0.0462 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0470P)^2^+0.4408P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1019 _refine_ls_wR_factor_ref 0.1218 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4665 _reflns_number_total 7983 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02546a2.cif _cod_data_source_block Complex1_296K _cod_original_cell_volume 2540.5(10) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705192 _shelx_shelxl_version_number 2018/3 _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-2018/3 at 20:25:26 on 30-Apr-2020 CELL 0.71073 11.8009 14.0411 15.3322 90.000 90.076 90.000 ZERR 4.00 0.0026 0.0029 0.0037 0.000 0.010 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 SIZE 0.300 0.400 0.600 ACTA BOND $H CONF L.S. 10 TEMP 23.00 WGHT 0.047000 0.440800 FVAR 0.12648 CO1 5 0.573389 0.351057 0.751071 11.00000 0.04168 0.02761 = 0.03257 -0.00024 0.00437 -0.00030 S1 4 0.556098 0.128074 0.984281 11.00000 0.11600 0.06296 = 0.06294 0.02139 0.01690 -0.00351 S2 4 0.646859 0.157506 0.502074 11.00000 0.11440 0.10440 = 0.04298 -0.02083 -0.01402 0.06584 N2 3 0.522484 0.456541 0.836001 11.00000 0.03846 0.02832 = 0.03278 -0.00245 0.00039 0.00155 N3 3 0.369666 0.349825 0.740133 11.00000 0.03369 0.03653 = 0.03469 -0.00133 0.00266 -0.00170 N1 3 0.735828 0.446661 0.759389 11.00000 0.03658 0.03037 = 0.03754 0.00177 0.00227 -0.00282 N5 3 0.590244 0.255182 0.849102 11.00000 0.04961 0.04013 = 0.04653 0.00167 0.00177 -0.00489 N6 3 0.618858 0.261281 0.653980 11.00000 0.04720 0.04085 = 0.04661 -0.00494 0.00241 0.00135 N4 3 0.540184 0.457304 0.661384 11.00000 0.03965 0.02951 = 0.03321 0.00167 0.00087 -0.00031 C15 1 0.590493 0.530114 0.853609 11.00000 0.04475 0.02777 = 0.03360 -0.00036 -0.00822 0.00412 C21 1 0.308157 0.259136 0.712195 11.00000 0.03243 0.04722 = 0.04741 -0.00877 0.00239 -0.00647 C6 1 0.505481 0.617899 0.564286 11.00000 0.08014 0.04342 = 0.06122 0.02196 -0.00572 0.00175 AFIX 43 H6 2 0.493656 0.671462 0.529774 11.00000 -1.20000 AFIX 0 C8 1 0.434588 0.485870 0.644219 11.00000 0.04576 0.03258 = 0.03244 -0.00333 -0.00097 0.00426 C11 1 0.414811 0.456145 0.863510 11.00000 0.04093 0.03612 = 0.03317 0.00023 0.00360 0.00572 C3 1 0.742718 0.474750 0.665922 11.00000 0.04289 0.03958 = 0.04445 0.00717 0.00541 -0.00723 AFIX 23 H3A 2 0.766465 0.420578 0.631200 11.00000 -1.20000 H3B 2 0.798500 0.524901 0.658923 11.00000 -1.20000 AFIX 0 C12 1 0.373291 0.527806 0.915971 11.00000 0.04958 0.04813 = 0.04151 -0.00555 0.00271 0.01316 AFIX 43 H12 2 0.298941 0.526176 0.935951 11.00000 -1.20000 AFIX 0 C14 1 0.552797 0.604136 0.906470 11.00000 0.06087 0.03074 = 0.04480 -0.00689 -0.01135 0.00509 AFIX 43 H14 2 0.600735 0.654565 0.920120 11.00000 -1.20000 AFIX 0 C1 1 0.576083 0.202989 0.905396 11.00000 0.05067 0.03451 = 0.04800 -0.00525 0.00286 -0.00146 C13 1 0.444338 0.601993 0.938215 11.00000 0.06856 0.04076 = 0.04565 -0.01302 -0.00254 0.01799 AFIX 43 H13 2 0.418710 0.650369 0.974623 11.00000 -1.20000 AFIX 0 C19 1 0.867420 0.309941 0.743105 11.00000 0.04342 0.04496 = 0.09369 -0.00605 -0.00773 0.00789 AFIX 33 H19A 2 0.936828 0.281830 0.763271 11.00000 -1.50000 H19B 2 0.805793 0.266794 0.753489 11.00000 -1.50000 H19C 2 0.872966 0.322745 0.681753 11.00000 -1.50000 AFIX 0 C16 1 0.705196 0.532744 0.811908 11.00000 0.05007 0.03010 = 0.04924 -0.00327 -0.00338 -0.00479 AFIX 23 H16A 2 0.708982 0.588160 0.774248 11.00000 -1.20000 H16B 2 0.761625 0.540942 0.857351 11.00000 -1.20000 AFIX 0 C10 1 0.344197 0.373659 0.832503 11.00000 0.03832 0.04631 = 0.03951 -0.00505 0.01143 -0.00153 AFIX 23 H10A 2 0.359154 0.318568 0.868914 11.00000 -1.20000 H10B 2 0.264537 0.389561 0.838008 11.00000 -1.20000 AFIX 0 C17 1 0.846298 0.402595 0.791927 11.00000 0.03526 0.03964 = 0.05770 0.00197 -0.00428 -0.00150 C2 1 0.631789 0.218460 0.590774 11.00000 0.03825 0.04293 = 0.04209 0.00461 0.00161 0.01178 C4 1 0.629397 0.509100 0.634936 11.00000 0.04970 0.03435 = 0.03554 0.00499 0.00087 -0.00352 C22 1 0.180678 0.266269 0.727138 11.00000 0.03627 0.07207 = 0.06098 -0.01200 0.00645 -0.01301 AFIX 33 H22A 2 0.150980 0.319383 0.694984 11.00000 -1.50000 H22B 2 0.144745 0.208720 0.707659 11.00000 -1.50000 H22C 2 0.166076 0.275193 0.788175 11.00000 -1.50000 AFIX 0 C20 1 0.832634 0.378902 0.889256 11.00000 0.05536 0.06666 = 0.06326 0.01675 -0.01822 -0.00645 AFIX 33 H20A 2 0.819198 0.436482 0.921381 11.00000 -1.50000 H20B 2 0.769671 0.336410 0.896784 11.00000 -1.50000 H20C 2 0.900502 0.349021 0.910371 11.00000 -1.50000 AFIX 0 C5 1 0.614665 0.590151 0.585583 11.00000 0.06818 0.04238 = 0.05566 0.01615 -0.00221 -0.01055 AFIX 43 H5 2 0.676740 0.625490 0.566959 11.00000 -1.20000 AFIX 0 C23 1 0.355696 0.175587 0.762645 11.00000 0.05811 0.03693 = 0.08553 -0.00447 -0.00386 -0.01224 AFIX 33 H23A 2 0.435908 0.171445 0.753003 11.00000 -1.50000 H23B 2 0.341342 0.184382 0.823733 11.00000 -1.50000 H23C 2 0.320011 0.117910 0.743217 11.00000 -1.50000 AFIX 0 C9 1 0.337891 0.431627 0.683829 11.00000 0.04322 0.05051 = 0.04784 0.00246 -0.00231 0.00644 AFIX 23 H9A 2 0.292875 0.475556 0.718187 11.00000 -1.20000 H9B 2 0.290087 0.408202 0.636998 11.00000 -1.20000 AFIX 0 C18 1 0.947269 0.469751 0.780194 11.00000 0.03776 0.06102 = 0.08921 0.00451 -0.00226 -0.00895 AFIX 33 H18A 2 0.933364 0.528014 0.811147 11.00000 -1.50000 H18B 2 1.014482 0.440082 0.802756 11.00000 -1.50000 H18C 2 0.957303 0.483285 0.719317 11.00000 -1.50000 AFIX 0 C7 1 0.415118 0.566483 0.594042 11.00000 0.06039 0.04331 = 0.05293 0.00687 -0.00609 0.01171 AFIX 43 H7 2 0.341506 0.585287 0.580826 11.00000 -1.20000 AFIX 0 C24 1 0.331152 0.242379 0.615181 11.00000 0.04930 0.07883 = 0.05503 -0.02356 0.00577 -0.01491 AFIX 33 H24A 2 0.301564 0.294737 0.581944 11.00000 -1.50000 H24B 2 0.411346 0.237447 0.605765 11.00000 -1.50000 H24C 2 0.294969 0.184443 0.596985 11.00000 -1.50000 AFIX 0 HKLF 4 REM SIR92 run in space group P 1 21/n 1 REM wR2 = 0.1218, GooF = S = 1.017, Restrained GooF = 1.017 for all data REM R1 = 0.0462 for 4665 Fo > 4sig(Fo) and 0.0988 for all 7983 data REM 298 parameters refined using 0 restraints END WGHT 0.0468 0.4497 REM Highest difference peak 0.491, deepest hole -0.521, 1-sigma level 0.062 Q1 1 0.4798 0.1576 0.9946 11.00000 0.05 0.49 Q2 1 0.6932 0.2181 0.5017 11.00000 0.05 0.37 Q3 1 0.5897 0.1434 0.5295 11.00000 0.05 0.34 Q4 1 0.5941 0.2790 0.7959 11.00000 0.05 0.31 Q5 1 0.5571 0.4166 0.7002 11.00000 0.05 0.30 Q6 1 0.4000 0.2764 0.5947 11.00000 0.05 0.29 Q7 1 0.4624 0.3563 0.7326 11.00000 0.05 0.26 Q8 1 0.6027 0.4178 0.7953 11.00000 0.05 0.25 Q9 1 0.4172 0.1591 0.8085 11.00000 0.05 0.25 Q10 1 0.3152 0.1410 0.6285 11.00000 0.05 0.23 Q11 1 0.6819 0.3993 0.7649 11.00000 0.05 0.23 Q12 1 0.4711 0.4593 0.8536 11.00000 0.05 0.22 Q13 1 0.9998 0.4643 0.7334 11.00000 0.05 0.21 Q14 1 0.5855 0.5464 0.8982 11.00000 0.05 0.21 Q15 1 0.1961 0.2366 0.8013 11.00000 0.05 0.21 Q16 1 0.9561 0.2229 0.7948 11.00000 0.05 0.20 Q17 1 0.7530 0.3956 0.9269 11.00000 0.05 0.20 Q18 1 0.6435 0.2053 0.5448 11.00000 0.05 0.20 Q19 1 0.9732 0.5419 0.8751 11.00000 0.05 0.20 Q20 1 0.7160 0.4785 0.7810 11.00000 0.05 0.20 Q21 1 0.6069 0.2234 0.8160 11.00000 0.05 0.20 Q22 1 0.4197 0.4532 0.9081 11.00000 0.05 0.20 Q23 1 0.5566 0.5603 0.8712 11.00000 0.05 0.20 Q24 1 0.5853 0.4851 0.6314 11.00000 0.05 0.20 Q25 1 0.8741 0.4391 0.9233 11.00000 0.05 0.20 ; _shelx_res_checksum 51075 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 0.57339(3) 0.35106(2) 0.75107(2) 0.03395(10) Uani 1 1 d . . . . . S1 S 0.55610(9) 0.12807(6) 0.98428(6) 0.0806(3) Uani 1 1 d . . . . . S2 S 0.64686(9) 0.15751(7) 0.50207(5) 0.0873(3) Uani 1 1 d . . . . . N2 N 0.52248(15) 0.45654(12) 0.83600(11) 0.0332(4) Uani 1 1 d . . . . . N3 N 0.36967(15) 0.34982(12) 0.74013(11) 0.0350(4) Uani 1 1 d . . . . . N1 N 0.73583(15) 0.44666(12) 0.75939(11) 0.0348(4) Uani 1 1 d . . . . . N5 N 0.59024(18) 0.25518(14) 0.84910(13) 0.0454(5) Uani 1 1 d . . . . . N6 N 0.61886(17) 0.26128(13) 0.65398(13) 0.0449(5) Uani 1 1 d . . . . . N4 N 0.54018(15) 0.45730(12) 0.66138(11) 0.0341(4) Uani 1 1 d . . . . . C15 C 0.59049(19) 0.53011(14) 0.85361(13) 0.0354(5) Uani 1 1 d . . . . . C21 C 0.30816(19) 0.25914(16) 0.71219(15) 0.0424(5) Uani 1 1 d . . . . . C6 C 0.5055(3) 0.61790(19) 0.56429(18) 0.0616(8) Uani 1 1 d . . . . . H6 H 0.493656 0.671462 0.529774 0.074 Uiso 1 1 calc R U . . . C8 C 0.4346(2) 0.48587(15) 0.64422(13) 0.0369(5) Uani 1 1 d . . . . . C11 C 0.4148(2) 0.45614(15) 0.86351(14) 0.0367(5) Uani 1 1 d . . . . . C3 C 0.7427(2) 0.47475(16) 0.66592(14) 0.0423(5) Uani 1 1 d . . . . . H3A H 0.766465 0.420578 0.631200 0.051 Uiso 1 1 calc R U . . . H3B H 0.798500 0.524901 0.658923 0.051 Uiso 1 1 calc R U . . . C12 C 0.3733(2) 0.52781(17) 0.91597(15) 0.0464(6) Uani 1 1 d . . . . . H12 H 0.298941 0.526176 0.935951 0.056 Uiso 1 1 calc R U . . . C14 C 0.5528(2) 0.60414(16) 0.90647(15) 0.0455(6) Uani 1 1 d . . . . . H14 H 0.600735 0.654565 0.920120 0.055 Uiso 1 1 calc R U . . . C1 C 0.5761(2) 0.20299(16) 0.90540(16) 0.0444(6) Uani 1 1 d . . . . . C13 C 0.4443(2) 0.60199(17) 0.93822(16) 0.0517(7) Uani 1 1 d . . . . . H13 H 0.418710 0.650369 0.974623 0.062 Uiso 1 1 calc R U . . . C19 C 0.8674(2) 0.30994(18) 0.7431(2) 0.0607(8) Uani 1 1 d . . . . . H19A H 0.936828 0.281830 0.763271 0.091 Uiso 1 1 calc R U . . . H19B H 0.805793 0.266794 0.753489 0.091 Uiso 1 1 calc R U . . . H19C H 0.872966 0.322745 0.681753 0.091 Uiso 1 1 calc R U . . . C16 C 0.7052(2) 0.53274(15) 0.81191(15) 0.0431(6) Uani 1 1 d . . . . . H16A H 0.708982 0.588160 0.774248 0.052 Uiso 1 1 calc R U . . . H16B H 0.761625 0.540942 0.857351 0.052 Uiso 1 1 calc R U . . . C10 C 0.3442(2) 0.37366(16) 0.83250(14) 0.0414(5) Uani 1 1 d . . . . . H10A H 0.359154 0.318568 0.868914 0.050 Uiso 1 1 calc R U . . . H10B H 0.264537 0.389561 0.838008 0.050 Uiso 1 1 calc R U . . . C17 C 0.8463(2) 0.40259(16) 0.79193(16) 0.0442(6) Uani 1 1 d . . . . . C2 C 0.6318(2) 0.21846(16) 0.59077(15) 0.0411(5) Uani 1 1 d . . . . . C4 C 0.6294(2) 0.50910(15) 0.63494(14) 0.0399(5) Uani 1 1 d . . . . . C22 C 0.1807(2) 0.2663(2) 0.72714(18) 0.0564(7) Uani 1 1 d . . . . . H22A H 0.150980 0.319383 0.694984 0.085 Uiso 1 1 calc R U . . . H22B H 0.144745 0.208720 0.707659 0.085 Uiso 1 1 calc R U . . . H22C H 0.166076 0.275193 0.788175 0.085 Uiso 1 1 calc R U . . . C20 C 0.8326(2) 0.3789(2) 0.88926(18) 0.0618(8) Uani 1 1 d . . . . . H20A H 0.819198 0.436482 0.921381 0.093 Uiso 1 1 calc R U . . . H20B H 0.769671 0.336410 0.896784 0.093 Uiso 1 1 calc R U . . . H20C H 0.900502 0.349021 0.910371 0.093 Uiso 1 1 calc R U . . . C5 C 0.6147(2) 0.59015(17) 0.58558(17) 0.0554(7) Uani 1 1 d . . . . . H5 H 0.676740 0.625490 0.566959 0.066 Uiso 1 1 calc R U . . . C23 C 0.3557(2) 0.17559(17) 0.76265(19) 0.0602(7) Uani 1 1 d . . . . . H23A H 0.435908 0.171445 0.753003 0.090 Uiso 1 1 calc R U . . . H23B H 0.341342 0.184382 0.823733 0.090 Uiso 1 1 calc R U . . . H23C H 0.320011 0.117910 0.743217 0.090 Uiso 1 1 calc R U . . . C9 C 0.3379(2) 0.43163(17) 0.68383(16) 0.0472(6) Uani 1 1 d . . . . . H9A H 0.292875 0.475556 0.718187 0.057 Uiso 1 1 calc R U . . . H9B H 0.290087 0.408202 0.636998 0.057 Uiso 1 1 calc R U . . . C18 C 0.9473(2) 0.4698(2) 0.7802(2) 0.0627(8) Uani 1 1 d . . . . . H18A H 0.933364 0.528014 0.811147 0.094 Uiso 1 1 calc R U . . . H18B H 1.014482 0.440082 0.802756 0.094 Uiso 1 1 calc R U . . . H18C H 0.957303 0.483285 0.719317 0.094 Uiso 1 1 calc R U . . . C7 C 0.4151(2) 0.56648(17) 0.59404(16) 0.0522(6) Uani 1 1 d . . . . . H7 H 0.341506 0.585287 0.580826 0.063 Uiso 1 1 calc R U . . . C24 C 0.3312(2) 0.2424(2) 0.61518(17) 0.0610(8) Uani 1 1 d . . . . . H24A H 0.301564 0.294737 0.581944 0.092 Uiso 1 1 calc R U . . . H24B H 0.411346 0.237447 0.605765 0.092 Uiso 1 1 calc R U . . . H24C H 0.294969 0.184443 0.596985 0.092 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.04168(19) 0.02761(15) 0.03257(15) -0.00024(12) 0.00437(12) -0.00030(13) S1 0.1160(8) 0.0630(5) 0.0629(5) 0.0214(4) 0.0169(5) -0.0035(5) S2 0.1144(8) 0.1044(7) 0.0430(4) -0.0208(4) -0.0140(4) 0.0658(6) N2 0.0385(11) 0.0283(8) 0.0328(9) -0.0024(7) 0.0004(8) 0.0016(8) N3 0.0337(10) 0.0365(9) 0.0347(9) -0.0013(8) 0.0027(7) -0.0017(8) N1 0.0366(10) 0.0304(9) 0.0375(9) 0.0018(8) 0.0023(8) -0.0028(8) N5 0.0496(13) 0.0401(11) 0.0465(11) 0.0017(9) 0.0018(10) -0.0049(9) N6 0.0472(13) 0.0409(11) 0.0466(11) -0.0049(9) 0.0024(9) 0.0014(9) N4 0.0397(11) 0.0295(9) 0.0332(9) 0.0017(7) 0.0009(8) -0.0003(8) C15 0.0448(14) 0.0278(10) 0.0336(11) -0.0004(8) -0.0082(9) 0.0041(9) C21 0.0324(13) 0.0472(13) 0.0474(13) -0.0088(11) 0.0024(10) -0.0065(10) C6 0.080(2) 0.0434(14) 0.0612(17) 0.0220(13) -0.0057(15) 0.0017(14) C8 0.0458(14) 0.0326(11) 0.0324(11) -0.0033(9) -0.0010(9) 0.0043(10) C11 0.0409(13) 0.0361(11) 0.0332(11) 0.0002(9) 0.0036(9) 0.0057(10) C3 0.0429(14) 0.0396(12) 0.0444(13) 0.0072(10) 0.0054(10) -0.0072(10) C12 0.0496(15) 0.0481(14) 0.0415(13) -0.0056(11) 0.0027(11) 0.0132(12) C14 0.0609(17) 0.0307(11) 0.0448(13) -0.0069(10) -0.0114(12) 0.0051(11) C1 0.0507(15) 0.0345(12) 0.0480(14) -0.0052(11) 0.0029(11) -0.0015(11) C13 0.0686(19) 0.0408(13) 0.0457(14) -0.0130(11) -0.0025(13) 0.0180(13) C19 0.0434(16) 0.0450(14) 0.094(2) -0.0061(15) -0.0077(14) 0.0079(12) C16 0.0501(15) 0.0301(11) 0.0492(13) -0.0033(10) -0.0034(11) -0.0048(10) C10 0.0383(13) 0.0463(13) 0.0395(12) -0.0050(10) 0.0114(10) -0.0015(10) C17 0.0353(13) 0.0396(12) 0.0577(15) 0.0020(11) -0.0043(11) -0.0015(10) C2 0.0382(13) 0.0429(12) 0.0421(13) 0.0046(11) 0.0016(10) 0.0118(10) C4 0.0497(15) 0.0343(11) 0.0355(11) 0.0050(9) 0.0009(10) -0.0035(10) C22 0.0363(15) 0.0721(18) 0.0610(17) -0.0120(14) 0.0064(12) -0.0130(13) C20 0.0554(18) 0.0667(17) 0.0633(17) 0.0168(14) -0.0182(14) -0.0065(14) C5 0.0682(19) 0.0424(13) 0.0557(16) 0.0161(12) -0.0022(14) -0.0105(13) C23 0.0581(18) 0.0369(13) 0.086(2) -0.0045(13) -0.0039(15) -0.0122(12) C9 0.0432(15) 0.0505(14) 0.0478(14) 0.0025(11) -0.0023(11) 0.0064(11) C18 0.0378(15) 0.0610(17) 0.089(2) 0.0045(16) -0.0023(14) -0.0090(13) C7 0.0604(18) 0.0433(13) 0.0529(15) 0.0069(12) -0.0061(13) 0.0117(12) C24 0.0493(17) 0.0788(19) 0.0550(16) -0.0236(14) 0.0058(13) -0.0149(14) 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 96.08(8) . . ? N6 Co1 N2 171.77(7) . . ? N5 Co1 N2 92.13(8) . . ? N6 Co1 N4 90.60(8) . . ? N5 Co1 N4 172.41(8) . . ? N2 Co1 N4 81.17(7) . . ? N6 Co1 N1 100.32(7) . . ? N5 Co1 N1 105.10(7) . . ? N2 Co1 N1 78.06(7) . . ? N4 Co1 N1 77.12(7) . . ? N6 Co1 N3 102.11(7) . . ? N5 Co1 N3 98.26(7) . . ? N2 Co1 N3 75.98(7) . . ? N4 Co1 N3 76.74(7) . . ? N1 Co1 N3 145.47(6) . . ? C15 N2 C11 120.64(18) . . ? C15 N2 Co1 120.51(15) . . ? C11 N2 Co1 118.24(14) . . ? C9 N3 C10 109.18(18) . . ? C9 N3 C21 111.25(18) . . ? C10 N3 C21 111.01(17) . . ? C9 N3 Co1 106.62(13) . . ? C10 N3 Co1 97.76(13) . . ? C21 N3 Co1 119.96(13) . . ? C3 N1 C16 108.51(17) . . ? C3 N1 C17 111.98(17) . . ? C16 N1 C17 110.99(17) . . ? C3 N1 Co1 98.34(12) . . ? C16 N1 Co1 107.08(13) . . ? C17 N1 Co1 118.93(12) . . ? C1 N5 Co1 165.9(2) . . ? C2 N6 Co1 168.7(2) . . ? C8 N4 C4 120.65(19) . . ? C8 N4 Co1 121.62(15) . . ? C4 N4 Co1 116.36(14) . . ? N2 C15 C14 120.2(2) . . ? N2 C15 C16 118.41(18) . . ? C14 C15 C16 121.3(2) . . ? C23 C21 C22 109.8(2) . . ? C23 C21 N3 109.12(19) . . ? C22 C21 N3 111.82(19) . . ? C23 C21 C24 108.2(2) . . ? C22 C21 C24 109.4(2) . . ? N3 C21 C24 108.42(19) . . ? C7 C6 C5 119.9(2) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? N4 C8 C7 120.5(2) . . ? N4 C8 C9 118.54(19) . . ? C7 C8 C9 120.9(2) . . ? N2 C11 C12 121.2(2) . . ? N2 C11 C10 115.42(18) . . ? C12 C11 C10 123.3(2) . . ? N1 C3 C4 109.92(18) . . ? N1 C3 H3A 109.7 . . ? C4 C3 H3A 109.7 . . ? N1 C3 H3B 109.7 . . ? C4 C3 H3B 109.7 . . ? H3A C3 H3B 108.2 . . ? C11 C12 C13 118.6(2) . . ? C11 C12 H12 120.7 . . ? C13 C12 H12 120.7 . . ? C13 C14 C15 119.3(2) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? N5 C1 S1 179.3(2) . . ? C14 C13 C12 119.8(2) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C16 C15 115.38(17) . . ? N1 C16 H16A 108.4 . . ? C15 C16 H16A 108.4 . . ? N1 C16 H16B 108.4 . . ? C15 C16 H16B 108.4 . . ? H16A C16 H16B 107.5 . . ? N3 C10 C11 111.22(18) . . ? N3 C10 H10A 109.4 . . ? C11 C10 H10A 109.4 . . ? N3 C10 H10B 109.4 . . ? C11 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C19 C17 N1 109.04(19) . . ? C19 C17 C18 109.9(2) . . ? N1 C17 C18 112.13(19) . . ? C19 C17 C20 108.1(2) . . ? N1 C17 C20 108.3(2) . . ? C18 C17 C20 109.3(2) . . ? N6 C2 S2 178.6(2) . . ? N4 C4 C5 121.0(2) . . ? N4 C4 C3 115.45(18) . . ? C5 C4 C3 123.5(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C4 C5 C6 118.6(2) . . ? C4 C5 H5 120.7 . . ? C6 C5 H5 120.7 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N3 C9 C8 115.87(19) . . ? N3 C9 H9A 108.3 . . ? C8 C9 H9A 108.3 . . ? N3 C9 H9B 108.3 . . ? C8 C9 H9B 108.3 . . ? H9A C9 H9B 107.4 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C6 C7 C8 119.2(3) . . ? C6 C7 H7 120.4 . . ? C8 C7 H7 120.4 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N6 2.024(2) . ? Co1 N5 2.027(2) . ? Co1 N2 2.0621(17) . ? Co1 N4 2.0661(17) . ? Co1 N1 2.3435(18) . ? Co1 N3 2.4098(19) . ? S1 C1 1.620(3) . ? S2 C2 1.617(2) . ? N2 C15 1.336(3) . ? N2 C11 1.339(3) . ? N3 C9 1.485(3) . ? N3 C10 1.486(3) . ? N3 C21 1.527(3) . ? N1 C3 1.489(3) . ? N1 C16 1.497(3) . ? N1 C17 1.526(3) . ? N5 C1 1.145(3) . ? N6 C2 1.151(3) . ? N4 C8 1.335(3) . ? N4 C4 1.343(3) . ? C15 C14 1.391(3) . ? C15 C16 1.498(3) . ? C21 C23 1.513(3) . ? C21 C22 1.525(3) . ? C21 C24 1.531(3) . ? C6 C7 1.367(4) . ? C6 C5 1.385(4) . ? C6 H6 0.9300 . ? C8 C7 1.388(3) . ? C8 C9 1.501(3) . ? C11 C12 1.379(3) . ? C11 C10 1.504(3) . ? C3 C4 1.498(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C12 C13 1.380(4) . ? C12 H12 0.9300 . ? C14 C13 1.370(4) . ? C14 H14 0.9300 . ? C13 H13 0.9300 . ? C19 C17 1.522(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C17 C18 1.530(3) . ? C17 C20 1.538(3) . ? C4 C5 1.378(3) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C5 H5 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C7 H7 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? 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 C11 N2 C15 C14 4.9(3) . . . . ? Co1 N2 C15 C14 175.80(15) . . . . ? C11 N2 C15 C16 -172.36(19) . . . . ? Co1 N2 C15 C16 -1.4(3) . . . . ? C9 N3 C21 C23 171.9(2) . . . . ? C10 N3 C21 C23 -66.3(2) . . . . ? Co1 N3 C21 C23 46.6(2) . . . . ? C9 N3 C21 C22 -66.4(3) . . . . ? C10 N3 C21 C22 55.4(3) . . . . ? Co1 N3 C21 C22 168.27(16) . . . . ? C9 N3 C21 C24 54.3(2) . . . . ? C10 N3 C21 C24 176.1(2) . . . . ? Co1 N3 C21 C24 -71.0(2) . . . . ? C4 N4 C8 C7 4.0(3) . . . . ? Co1 N4 C8 C7 170.21(16) . . . . ? C4 N4 C8 C9 -173.11(19) . . . . ? Co1 N4 C8 C9 -6.9(3) . . . . ? C15 N2 C11 C12 -4.8(3) . . . . ? Co1 N2 C11 C12 -175.94(16) . . . . ? C15 N2 C11 C10 174.59(18) . . . . ? Co1 N2 C11 C10 3.5(2) . . . . ? C16 N1 C3 C4 -62.4(2) . . . . ? C17 N1 C3 C4 174.78(17) . . . . ? Co1 N1 C3 C4 48.87(18) . . . . ? N2 C11 C12 C13 1.6(3) . . . . ? C10 C11 C12 C13 -177.8(2) . . . . ? N2 C15 C14 C13 -1.8(3) . . . . ? C16 C15 C14 C13 175.4(2) . . . . ? C15 C14 C13 C12 -1.4(4) . . . . ? C11 C12 C13 C14 1.5(4) . . . . ? C3 N1 C16 C15 112.8(2) . . . . ? C17 N1 C16 C15 -123.8(2) . . . . ? Co1 N1 C16 C15 7.5(2) . . . . ? N2 C15 C16 N1 -4.9(3) . . . . ? C14 C15 C16 N1 177.93(19) . . . . ? C9 N3 C10 C11 -63.6(2) . . . . ? C21 N3 C10 C11 173.40(18) . . . . ? Co1 N3 C10 C11 47.09(19) . . . . ? N2 C11 C10 N3 -39.7(3) . . . . ? C12 C11 C10 N3 139.7(2) . . . . ? C3 N1 C17 C19 -64.4(2) . . . . ? C16 N1 C17 C19 174.13(19) . . . . ? Co1 N1 C17 C19 49.3(2) . . . . ? C3 N1 C17 C18 57.5(3) . . . . ? C16 N1 C17 C18 -63.9(3) . . . . ? Co1 N1 C17 C18 171.25(16) . . . . ? C3 N1 C17 C20 178.21(19) . . . . ? C16 N1 C17 C20 56.8(2) . . . . ? Co1 N1 C17 C20 -68.1(2) . . . . ? C8 N4 C4 C5 -3.5(3) . . . . ? Co1 N4 C4 C5 -170.33(18) . . . . ? C8 N4 C4 C3 174.07(19) . . . . ? Co1 N4 C4 C3 7.2(2) . . . . ? N1 C3 C4 N4 -42.6(3) . . . . ? N1 C3 C4 C5 134.8(2) . . . . ? N4 C4 C5 C6 0.6(4) . . . . ? C3 C4 C5 C6 -176.7(2) . . . . ? C7 C6 C5 C4 1.6(4) . . . . ? C10 N3 C9 C8 109.4(2) . . . . ? C21 N3 C9 C8 -127.7(2) . . . . ? Co1 N3 C9 C8 4.8(2) . . . . ? N4 C8 C9 N3 0.4(3) . . . . ? C7 C8 C9 N3 -176.7(2) . . . . ? C5 C6 C7 C8 -1.1(4) . . . . ? N4 C8 C7 C6 -1.8(4) . . . . ? C9 C8 C7 C6 175.3(2) . . . . ?