#------------------------------------------------------------------------------ #$Date: 2020-10-06 11:51:45 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257541 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/52/7705241.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_7705241 loop_ _publ_author_name 'Melle, Philipp' 'S\'egaud, Nathalie' 'Albrecht, Martin' _publ_section_title ; Ambidentate bonding and electrochemical implications of pincer-type pyridylidene amide ligands in complexes of nickel, cobalt and zinc. ; _journal_issue 36 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12662 _journal_page_last 12673 _journal_paper_doi 10.1039/d0dt02482a _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C19 H17 Cl2 Co N5 O2, 2(C2 H6 O S)' _chemical_formula_sum 'C23 H29 Cl2 Co N5 O4 S2' _chemical_formula_weight 633.46 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-I 2ya' _space_group_name_H-M_alt 'I 1 2/a 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-09-23 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-07-13 deposited with the CCDC. 2020-08-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 95.0990(10) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 20.84210(10) _cell_length_b 13.98040(10) _cell_length_c 19.00770(10) _cell_measurement_reflns_used 14764 _cell_measurement_temperature 173.01(10) _cell_measurement_theta_max 76.7580 _cell_measurement_theta_min 3.8100 _cell_volume 5516.56(6) _computing_cell_refinement 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 173.01(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.970 _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 -63.00 -5.00 0.50 0.75 -- -18.75 119.00 41.00 116 2 \w 26.00 94.00 0.50 0.75 -- 47.95 77.00 150.00 136 3 \w 96.00 174.00 0.50 2.50 -- 107.11 119.00 41.00 156 4 \w 91.00 174.00 0.50 2.50 -- 107.11 61.00 120.00 166 5 \w 95.00 174.00 0.50 2.50 -- 107.11 45.00-120.00 158 6 \w 92.00 174.00 0.50 2.50 -- 107.11 125.00-150.00 164 7 \w 85.00 174.00 0.50 2.50 -- 107.11 77.00-180.00 178 8 \w 28.00 93.00 0.50 0.75 -- 47.95-119.00 -43.00 130 9 \w 35.00 113.00 0.50 2.50 -- 107.11-119.00 -43.00 156 10 \w 35.00 102.00 0.50 2.50 -- 107.11 -77.00 0.00 134 11 \w 35.00 68.00 0.50 2.50 -- 107.11 -61.00 60.00 66 12 \w 35.00 109.00 0.50 2.50 -- 107.11 -94.00 0.00 148 13 \w 35.00 68.00 0.50 2.50 -- 107.11 -61.00-150.00 66 14 \w 35.00 68.00 0.50 2.50 -- 107.11 -61.00-120.00 66 15 \w 35.00 68.00 0.50 2.50 -- 107.11 -61.00 -60.00 66 16 \w -26.00 23.00 0.50 0.75 -- 47.95 -19.00 120.00 98 17 \w -26.00 23.00 0.50 0.75 -- 47.95 -19.00 30.00 98 18 \w -26.00 23.00 0.50 0.75 -- 47.95 -19.00 -90.00 98 19 \w -26.00 23.00 0.50 0.75 -- 47.95 -19.00-120.00 98 20 \w 26.00 120.00 0.50 0.75 -- 47.95 77.00-120.00 188 21 \w 26.00 120.00 0.50 0.75 -- 47.95 77.00 0.00 188 22 \w 35.00 68.00 0.50 2.50 -- 107.11 -61.00 150.00 66 23 \w -86.00 -26.00 0.50 0.75 -- -18.75 157.00-163.00 120 24 \w -90.00 5.00 0.50 0.75 -- -18.75 -77.00 120.00 190 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0002586000 _diffrn_orient_matrix_UB_12 0.1092757000 _diffrn_orient_matrix_UB_13 0.0105189000 _diffrn_orient_matrix_UB_21 -0.0737303000 _diffrn_orient_matrix_UB_22 -0.0012546000 _diffrn_orient_matrix_UB_23 0.0020013000 _diffrn_orient_matrix_UB_31 0.0084637000 _diffrn_orient_matrix_UB_32 -0.0142128000 _diffrn_orient_matrix_UB_33 0.0806525000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0431 _diffrn_reflns_av_unetI/netI 0.0310 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 27154 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.142 _diffrn_reflns_theta_min 3.812 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'PhotonJet (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 8.409 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.55234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour dark _exptl_crystal_colour_primary dark _exptl_crystal_density_diffrn 1.525 _exptl_crystal_description needle _exptl_crystal_F_000 2616 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _refine_diff_density_max 0.297 _refine_diff_density_min -0.391 _refine_diff_density_rms 0.055 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.043 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 340 _refine_ls_number_reflns 5678 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.043 _refine_ls_R_factor_all 0.0373 _refine_ls_R_factor_gt 0.0339 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+7.0215P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.0849 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5254 _reflns_number_total 5678 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02482a2.cif _cod_data_source_block 19MA104_PM313 _cod_depositor_comments 'Adding full bibliography for 7705237--7705245.cif.' _cod_database_code 7705241 _shelx_shelxl_version_number 2014/7 _chemical_oxdiff_formula C19H17Cl2Co1N5O2 _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 0.679 _shelx_estimated_absorpt_t_min 0.284 _diffrn_oxdiff_digest_frames ; 011c851e1d1ec45d472d3f3824a806a905021868970 ; _diffrn_oxdiff_digest_hkl ; 01c447ac8fb2c419465dcc4695b6df0bbd54c4 ; _reflns_odcompleteness_completeness 99.94 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 66.97 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C12(H12), C16(H16), C6(H6), C23(H23), C13(H13), C19(H19), C20(H20), C4(H4), C22(H22), C15(H15), C5(H5) 2.b Idealised Me refined as rotating group: C24(H24A,H24B,H24C), C17(H17A,H17B,H17C), C26(H26A,H26B,H26C), C28(H28A,H28B, H28C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C) ; _shelx_res_file ; 19ma104.res created by SHELXL-2014/7 TITL 19ma104_a.res in I2/a REM Old TITL 19MA104 in I2/a REM SHELXT solution in I2/a REM R1 0.114, Rweak 0.012, Alpha 0.044, Orientation as input REM Formula found by SHELXT: C15 N5 O2 Cl4 S1 CELL 1.54184 20.8421 13.9804 19.0077 90 95.099 90 ZERR 8 0.0001 0.0001 0.0001 0 0.001 0 LATT 2 SYMM 0.5-X,+Y,-Z SFAC C H Cl Co N O S UNIT 184 232 16 8 40 32 16 L.S. 40 PLAN 10 SIZE 0.2 0.05 0.05 MORE -1 BOND $H CONF fmap 2 acta REM REM REM WGHT 0.037800 7.021500 FVAR 0.10021 CO1 4 0.412640 0.294224 0.431169 11.00000 0.02521 0.01493 = 0.01747 -0.00070 0.00021 0.00065 CL2 3 0.328740 0.198687 0.458500 11.00000 0.02712 0.02770 = 0.02023 -0.00024 -0.00070 -0.00501 CL1 3 0.500858 0.214866 0.393466 11.00000 0.03160 0.02773 = 0.02357 -0.00356 0.00493 0.00433 S1 7 0.354380 -0.077139 0.388557 11.00000 0.03138 0.02907 = 0.03878 0.00303 0.00196 -0.00076 S2 7 0.693056 0.327861 0.301526 11.00000 0.04030 0.02647 = 0.04935 0.00252 0.01202 0.00327 O2 6 0.471773 0.437399 0.623878 11.00000 0.06113 0.02543 = 0.01934 -0.00809 -0.00984 0.00519 N8 5 0.405464 0.436418 0.447491 11.00000 0.02468 0.01544 = 0.01736 0.00013 0.00149 0.00021 N10 5 0.450398 0.311426 0.543777 11.00000 0.02410 0.01771 = 0.01306 -0.00097 -0.00191 0.00108 N21 5 0.315708 0.171201 0.156357 11.00000 0.02417 0.02784 = 0.01617 -0.00476 -0.00048 -0.00031 N14 5 0.493754 0.081665 0.680098 11.00000 0.02699 0.02751 = 0.01614 0.00533 -0.00249 0.00120 N1 5 0.368781 0.347987 0.328168 11.00000 0.03069 0.01862 = 0.01357 0.00007 -0.00202 0.00081 O1 6 0.331558 0.493854 0.279280 11.00000 0.08666 0.02308 = 0.03056 0.00153 -0.02300 0.01321 O3 6 0.345866 -0.181408 0.374734 11.00000 0.06255 0.02789 = 0.04737 -0.00390 -0.00091 0.00948 O4 6 0.646564 0.409655 0.297523 11.00000 0.06091 0.02554 = 0.06568 0.00152 -0.00095 0.01382 C11 1 0.467493 0.239547 0.591032 11.00000 0.01907 0.02143 = 0.01515 0.00128 -0.00034 0.00116 C9 1 0.451901 0.403889 0.566123 11.00000 0.02561 0.02155 = 0.01612 -0.00376 -0.00098 0.00071 C18 1 0.350604 0.293561 0.269512 11.00000 0.02283 0.02151 = 0.01660 0.00063 -0.00044 0.00176 C7 1 0.425566 0.473653 0.510425 11.00000 0.02211 0.01996 = 0.01817 -0.00358 0.00131 -0.00022 C12 1 0.465954 0.144517 0.565750 11.00000 0.03020 0.02256 = 0.01540 -0.00008 -0.00410 0.00091 AFIX 43 H12 2 0.456064 0.133334 0.517780 11.00000 -1.20000 AFIX 0 C3 1 0.380674 0.493090 0.394930 11.00000 0.02728 0.01760 = 0.01979 0.00181 0.00057 0.00169 C16 1 0.485836 0.249627 0.664358 11.00000 0.03206 0.02575 = 0.01563 -0.00158 -0.00254 -0.00052 AFIX 43 H16 2 0.489989 0.310413 0.684112 11.00000 -1.20000 AFIX 0 C6 1 0.421413 0.570777 0.523484 11.00000 0.03120 0.02150 = 0.02272 -0.00592 0.00142 -0.00097 AFIX 43 H6 2 0.434930 0.595651 0.567711 11.00000 -1.20000 AFIX 0 C23 1 0.330489 0.328377 0.201080 11.00000 0.03259 0.02228 = 0.01740 0.00170 -0.00426 0.00433 AFIX 43 H23 2 0.328562 0.393960 0.192978 11.00000 -1.20000 AFIX 0 C13 1 0.478637 0.068696 0.610043 11.00000 0.03318 0.02227 = 0.01801 0.00030 -0.00392 0.00270 AFIX 43 H13 2 0.476855 0.006970 0.591733 11.00000 -1.20000 AFIX 0 C19 1 0.353316 0.193286 0.276357 11.00000 0.04072 0.02257 = 0.01571 0.00208 -0.00144 -0.00092 AFIX 43 H19 2 0.367259 0.166571 0.319858 11.00000 -1.20000 AFIX 0 C2 1 0.358091 0.444061 0.326774 11.00000 0.03578 0.01987 = 0.02060 0.00236 -0.00263 0.00262 C20 1 0.335975 0.134531 0.220689 11.00000 0.03734 0.02224 = 0.01903 0.00120 0.00140 -0.00159 AFIX 43 H20 2 0.338041 0.068570 0.226817 11.00000 -1.20000 AFIX 0 C4 1 0.375513 0.590938 0.404146 11.00000 0.03694 0.01898 = 0.02462 0.00260 0.00103 0.00271 AFIX 43 H4 2 0.358210 0.629696 0.367472 11.00000 -1.20000 AFIX 0 C22 1 0.313916 0.266523 0.146954 11.00000 0.03056 0.02866 = 0.01891 0.00242 -0.00292 0.00420 AFIX 43 H22 2 0.301050 0.290932 0.102409 11.00000 -1.20000 AFIX 0 C24 1 0.294156 0.107196 0.097228 11.00000 0.03306 0.03564 = 0.02056 -0.00904 -0.00066 -0.00375 AFIX 137 H24A 2 0.313694 0.045455 0.104902 11.00000 -1.50000 H24B 2 0.306611 0.133642 0.053861 11.00000 -1.50000 H24C 2 0.248138 0.100837 0.094439 11.00000 -1.50000 AFIX 0 C15 1 0.497442 0.171133 0.706178 11.00000 0.03342 0.03250 = 0.01379 -0.00034 -0.00248 -0.00056 AFIX 43 H15 2 0.508256 0.179750 0.754288 11.00000 -1.20000 AFIX 0 C5 1 0.396740 0.630110 0.469396 11.00000 0.03605 0.01673 = 0.03154 -0.00399 0.00536 0.00272 AFIX 43 H5 2 0.394362 0.695761 0.476617 11.00000 -1.20000 AFIX 0 C17 1 0.505458 -0.000826 0.727677 11.00000 0.04718 0.03213 = 0.02325 0.01122 -0.00325 0.00285 AFIX 137 H17A 2 0.466619 -0.016219 0.748859 11.00000 -1.50000 H17B 2 0.538816 0.014769 0.763971 11.00000 -1.50000 H17C 2 0.518567 -0.054811 0.701219 11.00000 -1.50000 AFIX 0 C26 1 0.277701 -0.022946 0.367522 11.00000 0.03934 0.02774 = 0.04059 -0.00417 -0.00727 0.00199 AFIX 137 H26A 2 0.266625 -0.026330 0.317470 11.00000 -1.50000 H26B 2 0.279379 0.042803 0.382138 11.00000 -1.50000 H26C 2 0.245782 -0.056112 0.391625 11.00000 -1.50000 AFIX 0 C28 1 0.646596 0.222697 0.282974 11.00000 0.04528 0.02798 = 0.04573 -0.00226 0.00905 0.00318 AFIX 137 H28A 2 0.614176 0.217758 0.315647 11.00000 -1.50000 H28B 2 0.674187 0.167654 0.287606 11.00000 -1.50000 H28C 2 0.626346 0.225913 0.235657 11.00000 -1.50000 AFIX 0 C25 1 0.357916 -0.064478 0.482292 11.00000 0.06011 0.03722 = 0.03955 -0.00304 -0.01097 0.00610 AFIX 137 H25A 2 0.321367 -0.095546 0.499592 11.00000 -1.50000 H25B 2 0.357487 0.002199 0.494312 11.00000 -1.50000 H25C 2 0.396796 -0.093280 0.503370 11.00000 -1.50000 AFIX 0 C27 1 0.713142 0.305766 0.393609 11.00000 0.05789 0.05403 = 0.05468 -0.00754 -0.00870 0.01784 AFIX 137 H27A 2 0.732415 0.362001 0.415413 11.00000 -1.50000 H27B 2 0.743008 0.253470 0.399235 11.00000 -1.50000 H27C 2 0.674777 0.289978 0.415567 11.00000 -1.50000 AFIX 0 HKLF 4 REM 19ma104_a.res in I2/a REM R1 = 0.0339 for 5254 Fo > 4sig(Fo) and 0.0373 for all 5678 data REM 340 parameters refined using 0 restraints END WGHT 0.0378 7.0221 REM Highest difference peak 0.297, deepest hole -0.391, 1-sigma level 0.055 Q1 1 0.4731 0.2417 0.6270 11.00000 0.05 0.30 Q2 1 0.3483 -0.0732 0.4346 11.00000 0.05 0.25 Q3 1 0.4720 0.1940 0.5786 11.00000 0.05 0.25 Q4 1 0.3394 0.3137 0.2345 11.00000 0.05 0.25 Q5 1 0.4123 0.3869 0.4360 11.00000 0.05 0.24 Q6 1 0.4659 0.2843 0.5718 11.00000 0.05 0.24 Q7 1 0.3762 0.3165 0.3655 11.00000 0.05 0.23 Q8 1 0.3972 0.6097 0.4309 11.00000 0.05 0.23 Q9 1 0.3804 0.4732 0.3644 11.00000 0.05 0.23 Q10 1 0.3917 0.4625 0.4194 11.00000 0.05 0.22 ; _shelx_res_checksum 84128 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 2.151 _oxdiff_exptl_absorpt_empirical_full_min 0.608 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x, -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 0.41264(2) 0.29422(2) 0.43117(2) 0.01930(9) Uani 1 1 d . . . . . Cl2 Cl 0.32874(2) 0.19869(4) 0.45850(2) 0.02519(11) Uani 1 1 d . . . . . Cl1 Cl 0.50086(2) 0.21487(4) 0.39347(3) 0.02749(12) Uani 1 1 d . . . . . S1 S 0.35438(3) -0.07714(4) 0.38856(3) 0.03315(13) Uani 1 1 d . . . . . S2 S 0.69306(3) 0.32786(4) 0.30153(3) 0.03822(14) Uani 1 1 d . . . . . O2 O 0.47177(9) 0.43740(11) 0.62388(8) 0.0361(4) Uani 1 1 d . . . . . N8 N 0.40546(8) 0.43642(11) 0.44749(8) 0.0192(3) Uani 1 1 d . . . . . N10 N 0.45040(7) 0.31143(12) 0.54378(8) 0.0185(3) Uani 1 1 d . . . . . N21 N 0.31571(8) 0.17120(13) 0.15636(8) 0.0229(3) Uani 1 1 d . . . . . N14 N 0.49375(8) 0.08167(13) 0.68010(8) 0.0238(4) Uani 1 1 d . . . . . N1 N 0.36878(8) 0.34799(12) 0.32817(8) 0.0212(3) Uani 1 1 d . . . . . O1 O 0.33156(10) 0.49385(12) 0.27928(9) 0.0485(5) Uani 1 1 d . . . . . O3 O 0.34587(10) -0.18141(13) 0.37473(10) 0.0463(4) Uani 1 1 d . . . . . O4 O 0.64656(10) 0.40965(13) 0.29752(11) 0.0511(5) Uani 1 1 d . . . . . C11 C 0.46749(8) 0.23955(14) 0.59103(9) 0.0187(4) Uani 1 1 d . . . . . C9 C 0.45190(9) 0.40389(14) 0.56612(10) 0.0213(4) Uani 1 1 d . . . . . C18 C 0.35060(9) 0.29356(14) 0.26951(10) 0.0204(4) Uani 1 1 d . . . . . C7 C 0.42557(9) 0.47365(14) 0.51042(10) 0.0201(4) Uani 1 1 d . . . . . C12 C 0.46595(10) 0.14452(15) 0.56575(10) 0.0231(4) Uani 1 1 d . . . . . H12 H 0.4561 0.1333 0.5178 0.028 Uiso 1 1 calc R . . . . C3 C 0.38067(9) 0.49309(14) 0.39493(10) 0.0216(4) Uani 1 1 d . . . . . C16 C 0.48584(10) 0.24963(16) 0.66436(10) 0.0248(4) Uani 1 1 d . . . . . H16 H 0.4900 0.3104 0.6841 0.030 Uiso 1 1 calc R . . . . C6 C 0.42141(10) 0.57078(15) 0.52348(11) 0.0252(4) Uani 1 1 d . . . . . H6 H 0.4349 0.5957 0.5677 0.030 Uiso 1 1 calc R . . . . C23 C 0.33049(10) 0.32838(16) 0.20108(10) 0.0245(4) Uani 1 1 d . . . . . H23 H 0.3286 0.3940 0.1930 0.029 Uiso 1 1 calc R . . . . C13 C 0.47864(10) 0.06870(15) 0.61004(10) 0.0249(4) Uani 1 1 d . . . . . H13 H 0.4769 0.0070 0.5917 0.030 Uiso 1 1 calc R . . . . C19 C 0.35332(11) 0.19329(15) 0.27636(10) 0.0266(4) Uani 1 1 d . . . . . H19 H 0.3673 0.1666 0.3199 0.032 Uiso 1 1 calc R . . . . C2 C 0.35809(10) 0.44406(15) 0.32677(10) 0.0257(4) Uani 1 1 d . . . . . C20 C 0.33597(10) 0.13453(15) 0.22069(10) 0.0263(4) Uani 1 1 d . . . . . H20 H 0.3380 0.0686 0.2268 0.032 Uiso 1 1 calc R . . . . C4 C 0.37551(10) 0.59094(15) 0.40415(11) 0.0270(4) Uani 1 1 d . . . . . H4 H 0.3582 0.6297 0.3675 0.032 Uiso 1 1 calc R . . . . C22 C 0.31392(10) 0.26652(16) 0.14695(11) 0.0263(4) Uani 1 1 d . . . . . H22 H 0.3010 0.2909 0.1024 0.032 Uiso 1 1 calc R . . . . C24 C 0.29416(11) 0.10720(17) 0.09723(11) 0.0299(5) Uani 1 1 d . . . . . H24A H 0.3137 0.0455 0.1049 0.045 Uiso 1 1 calc GR . . . . H24B H 0.3066 0.1336 0.0539 0.045 Uiso 1 1 calc GR . . . . H24C H 0.2481 0.1008 0.0944 0.045 Uiso 1 1 calc GR . . . . C15 C 0.49744(10) 0.17113(16) 0.70618(10) 0.0268(4) Uani 1 1 d . . . . . H15 H 0.5083 0.1798 0.7543 0.032 Uiso 1 1 calc R . . . . C5 C 0.39674(10) 0.63011(15) 0.46940(11) 0.0280(4) Uani 1 1 d . . . . . H5 H 0.3944 0.6958 0.4766 0.034 Uiso 1 1 calc R . . . . C17 C 0.50546(12) -0.00083(17) 0.72768(11) 0.0346(5) Uani 1 1 d . . . . . H17A H 0.4666 -0.0162 0.7489 0.052 Uiso 1 1 calc GR . . . . H17B H 0.5388 0.0148 0.7640 0.052 Uiso 1 1 calc GR . . . . H17C H 0.5186 -0.0548 0.7012 0.052 Uiso 1 1 calc GR . . . . C26 C 0.27770(12) -0.02295(17) 0.36752(13) 0.0365(5) Uani 1 1 d . . . . . H26A H 0.2666 -0.0263 0.3175 0.055 Uiso 1 1 calc GR . . . . H26B H 0.2794 0.0428 0.3821 0.055 Uiso 1 1 calc GR . . . . H26C H 0.2458 -0.0561 0.3916 0.055 Uiso 1 1 calc GR . . . . C28 C 0.64660(13) 0.22270(17) 0.28297(14) 0.0394(6) Uani 1 1 d . . . . . H28A H 0.6142 0.2178 0.3156 0.059 Uiso 1 1 calc GR . . . . H28B H 0.6742 0.1677 0.2876 0.059 Uiso 1 1 calc GR . . . . H28C H 0.6263 0.2259 0.2357 0.059 Uiso 1 1 calc GR . . . . C25 C 0.35792(14) -0.0645(2) 0.48229(14) 0.0465(6) Uani 1 1 d . . . . . H25A H 0.3214 -0.0955 0.4996 0.070 Uiso 1 1 calc GR . . . . H25B H 0.3575 0.0022 0.4943 0.070 Uiso 1 1 calc GR . . . . H25C H 0.3968 -0.0933 0.5034 0.070 Uiso 1 1 calc GR . . . . C27 C 0.71314(16) 0.3058(2) 0.39361(16) 0.0564(8) Uani 1 1 d . . . . . H27A H 0.7324 0.3620 0.4154 0.085 Uiso 1 1 calc GR . . . . H27B H 0.7430 0.2535 0.3992 0.085 Uiso 1 1 calc GR . . . . H27C H 0.6748 0.2900 0.4156 0.085 Uiso 1 1 calc GR . . . . 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 0.02521(17) 0.01493(16) 0.01747(16) -0.00070(12) 0.00021(12) 0.00065(12) Cl2 0.0271(2) 0.0277(3) 0.0202(2) -0.00024(18) -0.00070(17) -0.00501(19) Cl1 0.0316(2) 0.0277(3) 0.0236(2) -0.00356(18) 0.00493(18) 0.00433(19) S1 0.0314(3) 0.0291(3) 0.0388(3) 0.0030(2) 0.0020(2) -0.0008(2) S2 0.0403(3) 0.0265(3) 0.0494(4) 0.0025(2) 0.0120(3) 0.0033(2) O2 0.0611(10) 0.0254(8) 0.0193(7) -0.0081(6) -0.0098(7) 0.0052(7) N8 0.0247(8) 0.0154(8) 0.0174(7) 0.0001(6) 0.0015(6) 0.0002(6) N10 0.0241(8) 0.0177(8) 0.0131(7) -0.0010(6) -0.0019(6) 0.0011(6) N21 0.0242(8) 0.0278(9) 0.0162(8) -0.0048(7) -0.0005(6) -0.0003(7) N14 0.0270(8) 0.0275(9) 0.0161(8) 0.0053(7) -0.0025(6) 0.0012(7) N1 0.0307(8) 0.0186(8) 0.0136(7) 0.0001(6) -0.0020(6) 0.0008(7) O1 0.0867(14) 0.0231(9) 0.0306(9) 0.0015(7) -0.0230(9) 0.0132(9) O3 0.0626(12) 0.0279(9) 0.0474(10) -0.0039(8) -0.0009(9) 0.0095(8) O4 0.0609(12) 0.0255(9) 0.0657(13) 0.0015(8) -0.0009(10) 0.0138(9) C11 0.0191(8) 0.0214(10) 0.0152(9) 0.0013(7) -0.0003(7) 0.0012(7) C9 0.0256(9) 0.0216(10) 0.0161(9) -0.0038(7) -0.0010(7) 0.0007(8) C18 0.0228(9) 0.0215(10) 0.0166(9) 0.0006(7) -0.0004(7) 0.0018(7) C7 0.0221(9) 0.0200(10) 0.0182(9) -0.0036(7) 0.0013(7) -0.0002(7) C12 0.0302(10) 0.0226(10) 0.0154(9) -0.0001(8) -0.0041(7) 0.0009(8) C3 0.0273(9) 0.0176(10) 0.0198(9) 0.0018(7) 0.0006(7) 0.0017(8) C16 0.0321(10) 0.0258(11) 0.0156(9) -0.0016(8) -0.0025(7) -0.0005(8) C6 0.0312(10) 0.0215(10) 0.0227(10) -0.0059(8) 0.0014(8) -0.0010(8) C23 0.0326(10) 0.0223(10) 0.0174(9) 0.0017(8) -0.0043(8) 0.0043(8) C13 0.0332(10) 0.0223(10) 0.0180(9) 0.0003(8) -0.0039(8) 0.0027(8) C19 0.0407(12) 0.0226(11) 0.0157(9) 0.0021(8) -0.0014(8) -0.0009(9) C2 0.0358(11) 0.0199(10) 0.0206(10) 0.0024(8) -0.0026(8) 0.0026(8) C20 0.0373(11) 0.0222(11) 0.0190(9) 0.0012(8) 0.0014(8) -0.0016(9) C4 0.0369(11) 0.0190(10) 0.0246(10) 0.0026(8) 0.0010(8) 0.0027(9) C22 0.0306(10) 0.0287(11) 0.0189(9) 0.0024(8) -0.0029(7) 0.0042(9) C24 0.0331(11) 0.0356(13) 0.0206(10) -0.0090(9) -0.0007(8) -0.0038(9) C15 0.0334(11) 0.0325(12) 0.0138(9) -0.0003(8) -0.0025(8) -0.0006(9) C5 0.0361(11) 0.0167(10) 0.0315(11) -0.0040(8) 0.0054(9) 0.0027(8) C17 0.0472(13) 0.0321(13) 0.0233(11) 0.0112(9) -0.0033(9) 0.0029(10) C26 0.0393(12) 0.0277(12) 0.0406(13) -0.0042(10) -0.0073(10) 0.0020(10) C28 0.0453(13) 0.0280(12) 0.0457(14) -0.0023(10) 0.0090(11) 0.0032(11) C25 0.0601(17) 0.0372(14) 0.0396(14) -0.0030(11) -0.0110(12) 0.0061(13) C27 0.0579(18) 0.0540(19) 0.0547(18) -0.0075(14) -0.0087(14) 0.0178(14) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 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' Cl Cl 0.3639 0.7018 '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_ _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 Cl2 Co1 Cl1 115.66(2) . . ? N8 Co1 Cl2 118.00(5) . . ? N8 Co1 Cl1 126.23(5) . . ? N8 Co1 N10 76.75(6) . . ? N8 Co1 N1 76.80(6) . . ? N10 Co1 Cl2 93.24(4) . . ? N10 Co1 Cl1 97.28(4) . . ? N1 Co1 Cl2 97.73(5) . . ? N1 Co1 Cl1 99.53(5) . . ? N1 Co1 N10 153.49(6) . . ? O3 S1 C26 106.63(11) . . ? O3 S1 C25 105.48(12) . . ? C26 S1 C25 97.96(12) . . ? O4 S2 C28 106.44(12) . . ? O4 S2 C27 106.00(13) . . ? C28 S2 C27 97.30(14) . . ? C7 N8 Co1 119.93(13) . . ? C7 N8 C3 120.36(17) . . ? C3 N8 Co1 119.71(13) . . ? C11 N10 Co1 126.76(12) . . ? C9 N10 Co1 113.52(12) . . ? C9 N10 C11 119.58(15) . . ? C20 N21 C24 120.42(18) . . ? C22 N21 C20 119.77(17) . . ? C22 N21 C24 119.80(17) . . ? C13 N14 C17 120.72(18) . . ? C15 N14 C13 119.21(17) . . ? C15 N14 C17 120.07(17) . . ? C18 N1 Co1 126.21(13) . . ? C2 N1 Co1 113.93(12) . . ? C2 N1 C18 119.83(16) . . ? N10 C11 C12 117.97(16) . . ? N10 C11 C16 126.96(18) . . ? C12 C11 C16 115.06(17) . . ? O2 C9 N10 129.55(18) . . ? O2 C9 C7 116.93(18) . . ? N10 C9 C7 113.51(16) . . ? N1 C18 C23 126.30(18) . . ? N1 C18 C19 118.03(17) . . ? C19 C18 C23 115.65(18) . . ? N8 C7 C9 116.24(17) . . ? N8 C7 C6 121.50(18) . . ? C6 C7 C9 122.25(17) . . ? C11 C12 H12 119.2 . . ? C13 C12 C11 121.56(18) . . ? C13 C12 H12 119.2 . . ? N8 C3 C2 116.27(17) . . ? N8 C3 C4 121.21(18) . . ? C4 C3 C2 122.51(18) . . ? C11 C16 H16 119.6 . . ? C15 C16 C11 120.72(19) . . ? C15 C16 H16 119.6 . . ? C7 C6 H6 120.7 . . ? C5 C6 C7 118.66(18) . . ? C5 C6 H6 120.7 . . ? C18 C23 H23 119.7 . . ? C22 C23 C18 120.58(19) . . ? C22 C23 H23 119.7 . . ? N14 C13 C12 121.23(19) . . ? N14 C13 H13 119.4 . . ? C12 C13 H13 119.4 . . ? C18 C19 H19 119.3 . . ? C20 C19 C18 121.50(19) . . ? C20 C19 H19 119.3 . . ? N1 C2 C3 113.25(16) . . ? O1 C2 N1 129.35(19) . . ? O1 C2 C3 117.36(18) . . ? N21 C20 C19 120.8(2) . . ? N21 C20 H20 119.6 . . ? C19 C20 H20 119.6 . . ? C3 C4 H4 120.7 . . ? C3 C4 C5 118.65(19) . . ? C5 C4 H4 120.7 . . ? N21 C22 C23 121.71(18) . . ? N21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? N21 C24 H24A 109.5 . . ? N21 C24 H24B 109.5 . . ? N21 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N14 C15 C16 122.14(18) . . ? N14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C6 C5 C4 119.60(19) . . ? C6 C5 H5 120.2 . . ? C4 C5 H5 120.2 . . ? N14 C17 H17A 109.5 . . ? N14 C17 H17B 109.5 . . ? N14 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S2 C28 H28A 109.5 . . ? S2 C28 H28B 109.5 . . ? S2 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S2 C27 H27A 109.5 . . ? S2 C27 H27B 109.5 . . ? S2 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 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 Cl2 2.2963(6) . ? Co1 Cl1 2.3150(6) . ? Co1 N8 2.0196(16) . ? Co1 N10 2.2269(15) . ? Co1 N1 2.2171(15) . ? S1 O3 1.4890(18) . ? S1 C26 1.782(2) . ? S1 C25 1.785(3) . ? S2 O4 1.4964(18) . ? S2 C28 1.778(3) . ? S2 C27 1.790(3) . ? O2 C9 1.231(2) . ? N8 C7 1.337(2) . ? N8 C3 1.342(2) . ? N10 C11 1.374(2) . ? N10 C9 1.360(2) . ? N21 C20 1.358(3) . ? N21 C22 1.345(3) . ? N21 C24 1.475(2) . ? N14 C13 1.353(3) . ? N14 C15 1.345(3) . ? N14 C17 1.472(3) . ? N1 C18 1.375(2) . ? N1 C2 1.361(3) . ? O1 C2 1.232(2) . ? C11 C12 1.412(3) . ? C11 C16 1.419(3) . ? C9 C7 1.507(3) . ? C18 C23 1.417(3) . ? C18 C19 1.409(3) . ? C7 C6 1.384(3) . ? C12 H12 0.9300 . ? C12 C13 1.365(3) . ? C3 C2 1.504(3) . ? C3 C4 1.385(3) . ? C16 H16 0.9300 . ? C16 C15 1.364(3) . ? C6 H6 0.9300 . ? C6 C5 1.384(3) . ? C23 H23 0.9300 . ? C23 C22 1.365(3) . ? C13 H13 0.9300 . ? C19 H19 0.9300 . ? C19 C20 1.363(3) . ? C20 H20 0.9300 . ? C4 H4 0.9300 . ? C4 C5 1.392(3) . ? C22 H22 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C15 H15 0.9300 . ? C5 H5 0.9300 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 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 Co1 N8 C7 C9 -0.9(2) . . . . ? Co1 N8 C7 C6 179.97(14) . . . . ? Co1 N8 C3 C2 1.5(2) . . . . ? Co1 N8 C3 C4 -179.50(15) . . . . ? Co1 N10 C11 C12 5.1(2) . . . . ? Co1 N10 C11 C16 -173.64(15) . . . . ? Co1 N10 C9 O2 -177.39(19) . . . . ? Co1 N10 C9 C7 2.0(2) . . . . ? Co1 N1 C18 C23 -171.14(15) . . . . ? Co1 N1 C18 C19 7.2(3) . . . . ? Co1 N1 C2 O1 -175.7(2) . . . . ? Co1 N1 C2 C3 2.1(2) . . . . ? O2 C9 C7 N8 178.59(18) . . . . ? O2 C9 C7 C6 -2.3(3) . . . . ? N8 C7 C6 C5 -1.0(3) . . . . ? N8 C3 C2 N1 -2.4(3) . . . . ? N8 C3 C2 O1 175.6(2) . . . . ? N8 C3 C4 C5 0.1(3) . . . . ? N10 C11 C12 C13 -176.17(18) . . . . ? N10 C11 C16 C15 175.50(19) . . . . ? N10 C9 C7 N8 -0.9(2) . . . . ? N10 C9 C7 C6 178.28(18) . . . . ? N1 C18 C23 C22 179.7(2) . . . . ? N1 C18 C19 C20 179.9(2) . . . . ? C11 N10 C9 O2 6.5(3) . . . . ? C11 N10 C9 C7 -174.13(16) . . . . ? C11 C12 C13 N14 -0.5(3) . . . . ? C11 C16 C15 N14 1.7(3) . . . . ? C9 N10 C11 C12 -179.38(18) . . . . ? C9 N10 C11 C16 1.9(3) . . . . ? C9 C7 C6 C5 179.87(18) . . . . ? C18 N1 C2 O1 2.2(4) . . . . ? C18 N1 C2 C3 179.97(17) . . . . ? C18 C23 C22 N21 0.3(3) . . . . ? C18 C19 C20 N21 0.3(3) . . . . ? C7 N8 C3 C2 -178.66(17) . . . . ? C7 N8 C3 C4 0.3(3) . . . . ? C7 C6 C5 C4 1.4(3) . . . . ? C12 C11 C16 C15 -3.3(3) . . . . ? C3 N8 C7 C9 179.32(17) . . . . ? C3 N8 C7 C6 0.2(3) . . . . ? C3 C4 C5 C6 -1.0(3) . . . . ? C16 C11 C12 C13 2.7(3) . . . . ? C23 C18 C19 C20 -1.6(3) . . . . ? C13 N14 C15 C16 0.6(3) . . . . ? C19 C18 C23 C22 1.3(3) . . . . ? C2 N1 C18 C23 11.2(3) . . . . ? C2 N1 C18 C19 -170.44(19) . . . . ? C2 C3 C4 C5 179.0(2) . . . . ? C20 N21 C22 C23 -1.7(3) . . . . ? C4 C3 C2 N1 178.67(19) . . . . ? C4 C3 C2 O1 -3.3(3) . . . . ? C22 N21 C20 C19 1.4(3) . . . . ? C24 N21 C20 C19 -177.15(19) . . . . ? C24 N21 C22 C23 176.83(19) . . . . ? C15 N14 C13 C12 -1.2(3) . . . . ? C17 N14 C13 C12 178.2(2) . . . . ? C17 N14 C15 C16 -178.8(2) . . . . ?