#------------------------------------------------------------------------------ #$Date: 2021-10-07 02:05:43 +0300 (Thu, 07 Oct 2021) $ #$Revision: 269801 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/85/7708510.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_7708510 loop_ _publ_author_name 'Elsby, Matthew' 'Kim, Scott Y. H.' 'Steinmann, Stephan' 'Baker, R. Tom' _publ_section_title ; Same ligand, three first-row metals: Comparing M-amido bifunctional reactivity (Mn, Fe, Co) ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02637B _journal_year 2021 _chemical_formula_sum 'C30 H32 Co N2 S4' _chemical_formula_weight 607.74 _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-2014/7 _audit_update_record ; 2021-06-11 deposited with the CCDC. 2021-10-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 107.760(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.3526(5) _cell_length_b 10.3708(4) _cell_length_c 19.8110(6) _cell_measurement_reflns_used 5011 _cell_measurement_temperature 200(2) _cell_measurement_theta_max 25.95 _cell_measurement_theta_min 2.96 _cell_volume 2808.29(17) _computing_cell_refinement 'APEX II, Bruker (2009)' _computing_data_collection 'APEX II, Bruker (2009)' _computing_data_reduction 'XPREP, Bruker (2009)' _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXS-03 (Sheldrick, 2003)' _diffrn_ambient_temperature 200(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.995 _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 0.0516 _diffrn_reflns_av_unetI/netI 0.0523 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.995 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 27717 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.995 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 28.379 _diffrn_reflns_theta_min 2.241 _exptl_absorpt_coefficient_mu 0.932 _exptl_absorpt_correction_T_max 0.7457 _exptl_absorpt_correction_T_min 0.6737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS, Bruker (2003)' _exptl_crystal_colour purple _exptl_crystal_density_diffrn 1.437 _exptl_crystal_description 'hexagonal plate' _exptl_crystal_F_000 1268 _exptl_crystal_size_max 0.542 _exptl_crystal_size_mid 0.211 _exptl_crystal_size_min 0.064 _refine_diff_density_max 0.358 _refine_diff_density_min -0.319 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 338 _refine_ls_number_reflns 7003 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.012 _refine_ls_R_factor_all 0.0783 _refine_ls_R_factor_gt 0.0424 _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^)+(0.0465P)^2^+0.9434P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0920 _refine_ls_wR_factor_ref 0.1076 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4794 _reflns_number_total 7003 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02637b2.cif _cod_data_source_block shelx _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7708510 _shelx_shelxl_version_number 2014/7 _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 0.632 _shelx_estimated_absorpt_t_max 0.943 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL tb234 in P2(1)/n CELL 0.71073 14.3526 10.3708 19.8110 90.000 107.760 90.000 ZERR 4.00 0.0005 0.0004 0.0006 0.000 0.002 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N S CO UNIT 120 128 8 16 4 MERG 2 OMIT -3.00 180.00 EQIV $1 -x+1/2, y-1/2, -z+3/2 HTAB C10 S17_$1 HTAB C10 S17_$1 FMAP 2 PLAN 3 SIZE 0.064 0.211 0.542 ACTA BOND $H CONF L.S. 10 TEMP -73.10 WGHT 0.046500 0.943400 FVAR 0.38789 CO1 5 0.497849 0.491952 0.745366 11.00000 0.02458 0.02470 = 0.03512 0.00424 0.00938 -0.00304 C1 1 0.521188 0.168675 0.691900 11.00000 0.06783 0.04012 = 0.05326 -0.01098 0.02865 -0.01244 AFIX 137 H1A 2 0.537985 0.079613 0.707404 11.00000 -1.50000 H1B 2 0.545938 0.188330 0.652097 11.00000 -1.50000 H1C 2 0.449936 0.179098 0.676868 11.00000 -1.50000 AFIX 0 S2 4 0.575607 0.276730 0.763950 11.00000 0.02993 0.02660 = 0.04443 0.00095 0.01720 0.00064 C3 1 0.511249 0.232746 0.823855 11.00000 0.03102 0.02242 = 0.03761 0.00135 0.01420 -0.00076 C4 1 0.546890 0.133780 0.870914 11.00000 0.04171 0.03051 = 0.04117 0.00402 0.01366 0.00868 AFIX 43 H4 2 0.608427 0.096444 0.873794 11.00000 -1.20000 AFIX 0 C5 1 0.495031 0.088046 0.913793 11.00000 0.06008 0.03177 = 0.03919 0.00843 0.01739 0.00721 AFIX 43 H5 2 0.520271 0.020717 0.946830 11.00000 -1.20000 AFIX 0 C6 1 0.404519 0.143257 0.907381 11.00000 0.05617 0.03111 = 0.04163 0.00252 0.02745 -0.00682 AFIX 43 H6 2 0.366031 0.109804 0.934760 11.00000 -1.20000 AFIX 0 C7 1 0.369302 0.245024 0.862431 11.00000 0.03319 0.02851 = 0.04389 -0.00137 0.01901 -0.00163 AFIX 43 H7 2 0.307423 0.280771 0.860008 11.00000 -1.20000 AFIX 0 C8 1 0.422376 0.297851 0.819834 11.00000 0.02755 0.02188 = 0.03332 0.00108 0.00919 -0.00342 N9 3 0.397209 0.402579 0.776512 11.00000 0.02295 0.02244 = 0.04147 0.00346 0.01107 -0.00075 C10 1 0.300061 0.460019 0.766214 11.00000 0.02015 0.03227 = 0.04304 0.00225 0.00777 -0.00108 AFIX 23 H10A 2 0.253450 0.390658 0.767940 11.00000 -1.20000 H10B 2 0.277284 0.499511 0.718486 11.00000 -1.20000 AFIX 0 C11 1 0.298512 0.561256 0.820738 11.00000 0.02286 0.03104 = 0.04486 0.00228 0.00683 0.00611 C12 1 0.250218 0.541663 0.870693 11.00000 0.03536 0.04570 = 0.05208 0.00420 0.01555 0.01122 AFIX 43 H12 2 0.215017 0.463707 0.869566 11.00000 -1.20000 AFIX 0 C13 1 0.251866 0.632723 0.922279 11.00000 0.05380 0.06370 = 0.05052 0.00603 0.02208 0.02286 AFIX 43 H13 2 0.218172 0.617394 0.956000 11.00000 -1.20000 AFIX 0 C14 1 0.302892 0.745494 0.924001 11.00000 0.06267 0.05285 = 0.05026 -0.00974 0.01286 0.01675 AFIX 43 H14 2 0.306080 0.807309 0.960026 11.00000 -1.20000 AFIX 0 C15 1 0.349441 0.769592 0.873911 11.00000 0.04699 0.03461 = 0.05622 -0.00686 0.00433 0.00747 AFIX 43 H15 2 0.383006 0.848833 0.874811 11.00000 -1.20000 AFIX 0 C16 1 0.347496 0.678467 0.822080 11.00000 0.02673 0.02898 = 0.04670 0.00233 0.00577 0.00890 S17 4 0.399523 0.704654 0.753078 11.00000 0.02878 0.02384 = 0.05660 0.00182 0.01116 0.00049 C18 1 0.471013 0.848923 0.777455 11.00000 0.03710 0.02608 = 0.07873 -0.00073 0.01090 -0.00226 AFIX 137 H18A 2 0.427496 0.922420 0.775915 11.00000 -1.50000 H18B 2 0.508408 0.863532 0.744211 11.00000 -1.50000 H18C 2 0.516164 0.839578 0.825546 11.00000 -1.50000 AFIX 0 C21 1 0.439081 0.413235 0.563845 11.00000 0.06310 0.04752 = 0.05021 -0.00401 0.01897 -0.01713 AFIX 137 H21A 2 0.422714 0.447509 0.515534 11.00000 -1.50000 H21B 2 0.404754 0.331367 0.563289 11.00000 -1.50000 H21C 2 0.509831 0.398977 0.582400 11.00000 -1.50000 AFIX 0 S22 4 0.402219 0.526914 0.619557 11.00000 0.03553 0.03864 = 0.03533 0.00411 0.00189 -0.01234 C23 1 0.476231 0.661161 0.612602 11.00000 0.04109 0.03561 = 0.03923 0.00819 0.00182 -0.01382 C24 1 0.442266 0.745794 0.557033 11.00000 0.06155 0.05403 = 0.05454 0.02377 -0.01688 -0.02100 AFIX 43 H24 2 0.377846 0.735622 0.525601 11.00000 -1.20000 AFIX 0 C25 1 0.498990 0.843560 0.546227 11.00000 0.09107 0.05853 = 0.06810 0.04054 -0.02334 -0.03467 AFIX 43 H25 2 0.474358 0.902527 0.508260 11.00000 -1.20000 AFIX 0 C26 1 0.593530 0.855733 0.591635 11.00000 0.07742 0.05235 = 0.05590 0.02102 0.00199 -0.03680 AFIX 43 H26 2 0.634839 0.921422 0.583309 11.00000 -1.20000 AFIX 0 C27 1 0.628203 0.774960 0.648059 11.00000 0.04639 0.03971 = 0.04110 0.00631 0.00371 -0.01805 AFIX 43 H27 2 0.692789 0.787415 0.678803 11.00000 -1.20000 AFIX 0 C28 1 0.571292 0.673220 0.662394 11.00000 0.03145 0.02923 = 0.03330 0.00114 0.00814 -0.00840 N29 3 0.598747 0.590170 0.718321 11.00000 0.02440 0.03015 = 0.02958 0.00394 0.00701 -0.00444 C30 1 0.698612 0.601155 0.766350 11.00000 0.02402 0.02960 = 0.03242 0.00054 0.01134 -0.00096 AFIX 23 H30A 2 0.742230 0.629867 0.739034 11.00000 -1.20000 H30B 2 0.721148 0.515054 0.786293 11.00000 -1.20000 AFIX 0 C31 1 0.707214 0.694932 0.826744 11.00000 0.01829 0.02884 = 0.03203 0.00128 0.00511 0.00120 C32 1 0.750175 0.815982 0.828872 11.00000 0.02824 0.03061 = 0.03427 0.00014 0.00971 -0.00132 AFIX 43 H32 2 0.777186 0.839485 0.792405 11.00000 -1.20000 AFIX 0 C33 1 0.754456 0.902538 0.882618 11.00000 0.03308 0.02852 = 0.04321 0.00075 0.00621 -0.00298 AFIX 43 H33 2 0.784348 0.984391 0.883051 11.00000 -1.20000 AFIX 0 C34 1 0.715301 0.869867 0.935529 11.00000 0.04126 0.03335 = 0.03525 -0.00453 0.00707 0.00276 AFIX 43 H34 2 0.717070 0.929861 0.972137 11.00000 -1.20000 AFIX 0 C35 1 0.673213 0.749522 0.935599 11.00000 0.03664 0.03772 = 0.02976 -0.00071 0.01017 0.00143 AFIX 43 H35 2 0.646830 0.726604 0.972480 11.00000 -1.20000 AFIX 0 C36 1 0.669777 0.662629 0.881552 11.00000 0.02328 0.02880 = 0.02957 0.00239 0.00544 0.00081 S37 4 0.620532 0.505406 0.879236 11.00000 0.03246 0.03192 = 0.03231 0.00268 0.01154 -0.00337 C38 1 0.553399 0.511998 0.941864 11.00000 0.03754 0.05177 = 0.03559 0.00501 0.01495 -0.00700 AFIX 137 H38A 2 0.598415 0.529564 0.989200 11.00000 -1.50000 H38B 2 0.520613 0.429235 0.942249 11.00000 -1.50000 H38C 2 0.504401 0.580807 0.928444 11.00000 -1.50000 AFIX 0 HKLF 4 REM tb234 in P2(1)/n REM R1 = 0.0424 for 4794 Fo > 4sig(Fo) and 0.0783 for all 7003 data REM 338 parameters refined using 0 restraints END WGHT 0.0464 0.9515 REM Highest difference peak 0.358, deepest hole -0.319, 1-sigma level 0.068 Q1 1 0.4810 0.9052 0.5708 11.00000 0.05 0.36 Q2 1 0.5804 0.5056 0.8339 11.00000 0.05 0.35 Q3 1 0.5221 0.4778 0.7960 11.00000 0.05 0.35 ; _shelx_res_checksum 27387 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 0.49785(2) 0.49195(3) 0.74537(2) 0.02807(10) Uani 1 1 d . . . . . C1 C 0.5212(3) 0.1687(3) 0.69190(16) 0.0515(8) Uani 1 1 d . . . . . H1A H 0.5380 0.0796 0.7074 0.077 Uiso 1 1 calc R U . . . H1B H 0.5459 0.1883 0.6521 0.077 Uiso 1 1 calc R U . . . H1C H 0.4499 0.1791 0.6769 0.077 Uiso 1 1 calc R U . . . S2 S 0.57561(5) 0.27673(6) 0.76395(4) 0.03234(16) Uani 1 1 d . . . . . C3 C 0.51125(18) 0.2327(2) 0.82385(13) 0.0295(5) Uani 1 1 d . . . . . C4 C 0.5469(2) 0.1338(3) 0.87091(14) 0.0376(6) Uani 1 1 d . . . . . H4 H 0.6084 0.0964 0.8738 0.045 Uiso 1 1 calc R U . . . C5 C 0.4950(2) 0.0880(3) 0.91379(15) 0.0432(7) Uani 1 1 d . . . . . H5 H 0.5203 0.0207 0.9468 0.052 Uiso 1 1 calc R U . . . C6 C 0.4045(2) 0.1433(3) 0.90738(14) 0.0402(7) Uani 1 1 d . . . . . H6 H 0.3660 0.1098 0.9348 0.048 Uiso 1 1 calc R U . . . C7 C 0.3693(2) 0.2450(2) 0.86243(14) 0.0336(6) Uani 1 1 d . . . . . H7 H 0.3074 0.2808 0.8600 0.040 Uiso 1 1 calc R U . . . C8 C 0.42238(17) 0.2979(2) 0.81983(13) 0.0276(5) Uani 1 1 d . . . . . N9 N 0.39721(14) 0.40258(19) 0.77651(11) 0.0287(5) Uani 1 1 d . . . . . C10 C 0.30006(17) 0.4600(2) 0.76621(14) 0.0322(6) Uani 1 1 d . . . . . H10A H 0.2535 0.3907 0.7679 0.039 Uiso 1 1 calc R U . . . H10B H 0.2773 0.4995 0.7185 0.039 Uiso 1 1 calc R U . . . C11 C 0.29851(18) 0.5613(3) 0.82074(14) 0.0337(6) Uani 1 1 d . . . . . C12 C 0.2502(2) 0.5417(3) 0.87069(16) 0.0439(7) Uani 1 1 d . . . . . H12 H 0.2150 0.4637 0.8696 0.053 Uiso 1 1 calc R U . . . C13 C 0.2519(2) 0.6327(3) 0.92228(17) 0.0546(9) Uani 1 1 d . . . . . H13 H 0.2182 0.6174 0.9560 0.066 Uiso 1 1 calc R U . . . C14 C 0.3029(3) 0.7455(3) 0.92400(18) 0.0562(9) Uani 1 1 d . . . . . H14 H 0.3061 0.8073 0.9600 0.067 Uiso 1 1 calc R U . . . C15 C 0.3494(2) 0.7696(3) 0.87391(16) 0.0485(8) Uani 1 1 d . . . . . H15 H 0.3830 0.8488 0.8748 0.058 Uiso 1 1 calc R U . . . C16 C 0.34750(19) 0.6785(3) 0.82208(14) 0.0354(6) Uani 1 1 d . . . . . S17 S 0.39952(5) 0.70465(6) 0.75308(4) 0.03683(17) Uani 1 1 d . . . . . C18 C 0.4710(2) 0.8489(3) 0.77745(18) 0.0488(8) Uani 1 1 d . . . . . H18A H 0.4275 0.9224 0.7759 0.073 Uiso 1 1 calc R U . . . H18B H 0.5084 0.8635 0.7442 0.073 Uiso 1 1 calc R U . . . H18C H 0.5162 0.8396 0.8255 0.073 Uiso 1 1 calc R U . . . C21 C 0.4391(3) 0.4132(3) 0.56385(16) 0.0532(8) Uani 1 1 d . . . . . H21A H 0.4227 0.4475 0.5155 0.080 Uiso 1 1 calc R U . . . H21B H 0.4048 0.3314 0.5633 0.080 Uiso 1 1 calc R U . . . H21C H 0.5098 0.3990 0.5824 0.080 Uiso 1 1 calc R U . . . S22 S 0.40222(5) 0.52691(7) 0.61956(4) 0.03850(17) Uani 1 1 d . . . . . C23 C 0.4762(2) 0.6612(3) 0.61260(14) 0.0410(7) Uani 1 1 d . . . . . C24 C 0.4423(3) 0.7458(3) 0.55703(17) 0.0645(11) Uani 1 1 d . . . . . H24 H 0.3778 0.7356 0.5256 0.077 Uiso 1 1 calc R U . . . C25 C 0.4990(3) 0.8436(3) 0.54623(19) 0.0832(14) Uani 1 1 d . . . . . H25 H 0.4744 0.9025 0.5083 0.100 Uiso 1 1 calc R U . . . C26 C 0.5935(3) 0.8557(3) 0.59164(17) 0.0660(11) Uani 1 1 d . . . . . H26 H 0.6348 0.9214 0.5833 0.079 Uiso 1 1 calc R U . . . C27 C 0.6282(2) 0.7750(3) 0.64806(15) 0.0446(7) Uani 1 1 d . . . . . H27 H 0.6928 0.7874 0.6788 0.053 Uiso 1 1 calc R U . . . C28 C 0.57129(19) 0.6732(2) 0.66239(13) 0.0317(6) Uani 1 1 d . . . . . N29 N 0.59875(14) 0.5902(2) 0.71832(10) 0.0283(5) Uani 1 1 d . . . . . C30 C 0.69861(17) 0.6012(2) 0.76635(12) 0.0281(5) Uani 1 1 d . . . . . H30A H 0.7422 0.6299 0.7390 0.034 Uiso 1 1 calc R U . . . H30B H 0.7211 0.5151 0.7863 0.034 Uiso 1 1 calc R U . . . C31 C 0.70721(17) 0.6949(2) 0.82674(12) 0.0270(5) Uani 1 1 d . . . . . C32 C 0.75017(18) 0.8160(2) 0.82887(13) 0.0310(6) Uani 1 1 d . . . . . H32 H 0.7772 0.8395 0.7924 0.037 Uiso 1 1 calc R U . . . C33 C 0.75446(19) 0.9025(3) 0.88262(14) 0.0362(6) Uani 1 1 d . . . . . H33 H 0.7843 0.9844 0.8831 0.043 Uiso 1 1 calc R U . . . C34 C 0.7153(2) 0.8699(3) 0.93553(14) 0.0376(6) Uani 1 1 d . . . . . H34 H 0.7171 0.9299 0.9721 0.045 Uiso 1 1 calc R U . . . C35 C 0.6732(2) 0.7495(3) 0.93560(13) 0.0347(6) Uani 1 1 d . . . . . H35 H 0.6468 0.7266 0.9725 0.042 Uiso 1 1 calc R U . . . C36 C 0.66978(17) 0.6626(2) 0.88155(13) 0.0278(5) Uani 1 1 d . . . . . S37 S 0.62053(5) 0.50541(6) 0.87924(3) 0.03186(15) Uani 1 1 d . . . . . C38 C 0.5534(2) 0.5120(3) 0.94186(14) 0.0408(7) Uani 1 1 d . . . . . H38A H 0.5984 0.5296 0.9892 0.061 Uiso 1 1 calc R U . . . H38B H 0.5206 0.4292 0.9422 0.061 Uiso 1 1 calc R U . . . H38C H 0.5044 0.5808 0.9284 0.061 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 0.02458(17) 0.02470(18) 0.0351(2) 0.00424(14) 0.00938(14) -0.00304(14) C1 0.068(2) 0.0401(17) 0.0533(19) -0.0110(14) 0.0286(17) -0.0124(16) S2 0.0299(3) 0.0266(3) 0.0444(4) 0.0009(3) 0.0172(3) 0.0006(3) C3 0.0310(13) 0.0224(12) 0.0376(14) 0.0014(10) 0.0142(11) -0.0008(10) C4 0.0417(16) 0.0305(14) 0.0412(15) 0.0040(12) 0.0137(13) 0.0087(12) C5 0.060(2) 0.0318(15) 0.0392(16) 0.0084(12) 0.0174(14) 0.0072(14) C6 0.0562(19) 0.0311(15) 0.0416(16) 0.0025(12) 0.0275(14) -0.0068(13) C7 0.0332(14) 0.0285(14) 0.0439(15) -0.0014(11) 0.0190(12) -0.0016(11) C8 0.0276(13) 0.0219(12) 0.0333(13) 0.0011(10) 0.0092(10) -0.0034(10) N9 0.0229(10) 0.0224(10) 0.0415(12) 0.0035(9) 0.0111(9) -0.0008(8) C10 0.0201(12) 0.0323(14) 0.0430(15) 0.0023(11) 0.0078(11) -0.0011(10) C11 0.0229(12) 0.0310(14) 0.0449(15) 0.0023(12) 0.0068(11) 0.0061(11) C12 0.0354(15) 0.0457(17) 0.0521(18) 0.0042(14) 0.0156(14) 0.0112(13) C13 0.054(2) 0.064(2) 0.0505(19) 0.0060(16) 0.0221(16) 0.0229(18) C14 0.063(2) 0.053(2) 0.0503(19) -0.0097(16) 0.0129(17) 0.0168(17) C15 0.0470(18) 0.0346(16) 0.0562(19) -0.0069(14) 0.0043(15) 0.0075(14) C16 0.0267(13) 0.0290(14) 0.0467(16) 0.0023(12) 0.0058(12) 0.0089(11) S17 0.0288(3) 0.0238(3) 0.0566(4) 0.0018(3) 0.0112(3) 0.0005(3) C18 0.0371(16) 0.0261(14) 0.079(2) -0.0007(14) 0.0109(16) -0.0023(12) C21 0.063(2) 0.0475(19) 0.0502(18) -0.0040(15) 0.0190(16) -0.0171(16) S22 0.0355(4) 0.0386(4) 0.0353(4) 0.0041(3) 0.0019(3) -0.0123(3) C23 0.0411(16) 0.0356(15) 0.0392(15) 0.0082(12) 0.0018(12) -0.0138(13) C24 0.062(2) 0.054(2) 0.055(2) 0.0238(16) -0.0169(16) -0.0210(17) C25 0.091(3) 0.059(2) 0.068(2) 0.0405(19) -0.023(2) -0.035(2) C26 0.077(3) 0.052(2) 0.056(2) 0.0210(16) 0.0020(18) -0.0368(19) C27 0.0464(17) 0.0397(16) 0.0411(16) 0.0063(13) 0.0037(13) -0.0180(14) C28 0.0314(14) 0.0292(14) 0.0333(14) 0.0011(11) 0.0081(11) -0.0084(11) N29 0.0244(11) 0.0302(11) 0.0296(11) 0.0039(9) 0.0070(9) -0.0044(9) C30 0.0240(12) 0.0296(13) 0.0324(13) 0.0005(10) 0.0113(10) -0.0010(10) C31 0.0183(11) 0.0288(13) 0.0320(13) 0.0013(10) 0.0051(10) 0.0012(10) C32 0.0282(13) 0.0306(14) 0.0343(14) 0.0001(11) 0.0097(11) -0.0013(11) C33 0.0331(14) 0.0285(14) 0.0432(16) 0.0007(12) 0.0062(12) -0.0030(11) C34 0.0413(16) 0.0333(15) 0.0352(15) -0.0045(11) 0.0071(12) 0.0028(12) C35 0.0366(15) 0.0377(15) 0.0298(13) -0.0007(11) 0.0102(11) 0.0014(12) C36 0.0233(12) 0.0288(13) 0.0296(13) 0.0024(10) 0.0054(10) 0.0008(10) S37 0.0325(3) 0.0319(3) 0.0323(3) 0.0027(3) 0.0115(3) -0.0034(3) C38 0.0375(15) 0.0518(18) 0.0356(15) 0.0050(13) 0.0150(12) -0.0070(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 N9 Co1 N29 176.46(8) . . ? N9 Co1 S2 82.48(6) . . ? N29 Co1 S2 99.85(6) . . ? N9 Co1 S22 98.63(6) . . ? N29 Co1 S22 83.03(6) . . ? S2 Co1 S22 111.61(3) . . ? N9 Co1 S17 85.36(6) . . ? N29 Co1 S17 91.94(6) . . ? S2 Co1 S17 165.41(3) . . ? S22 Co1 S17 78.15(3) . . ? N9 Co1 S37 92.15(6) . . ? N29 Co1 S37 85.84(6) . . ? S2 Co1 S37 76.77(2) . . ? S22 Co1 S37 167.06(3) . . ? S17 Co1 S37 95.71(2) . . ? S2 C1 H1A 109.5 . . ? S2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? S2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C3 S2 C1 100.52(13) . . ? C3 S2 Co1 91.62(8) . . ? C1 S2 Co1 112.21(12) . . ? C4 C3 C8 122.2(2) . . ? C4 C3 S2 118.9(2) . . ? C8 C3 S2 118.80(18) . . ? C5 C4 C3 121.1(3) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.4 . . ? C4 C5 C6 118.0(3) . . ? C4 C5 H5 121.0 . . ? C6 C5 H5 121.0 . . ? C7 C6 C5 121.6(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C6 C7 C8 121.9(3) . . ? C6 C7 H7 119.1 . . ? C8 C7 H7 119.1 . . ? N9 C8 C7 126.8(2) . . ? N9 C8 C3 118.3(2) . . ? C7 C8 C3 114.9(2) . . ? C8 N9 C10 117.9(2) . . ? C8 N9 Co1 119.61(16) . . ? C10 N9 Co1 121.39(16) . . ? N9 C10 C11 113.7(2) . . ? N9 C10 H10A 108.8 . . ? C11 C10 H10A 108.8 . . ? N9 C10 H10B 108.8 . . ? C11 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 118.1(3) . . ? C12 C11 C10 121.9(3) . . ? C16 C11 C10 120.0(2) . . ? C11 C12 C13 121.8(3) . . ? C11 C12 H12 119.1 . . ? C13 C12 H12 119.1 . . ? C14 C13 C12 119.1(3) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.4 . . ? C13 C14 C15 120.5(3) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 120.3(3) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C11 120.1(3) . . ? C15 C16 S17 123.3(2) . . ? C11 C16 S17 116.5(2) . . ? C16 S17 C18 105.17(15) . . ? C16 S17 Co1 105.96(9) . . ? C18 S17 Co1 116.03(10) . . ? S17 C18 H18A 109.5 . . ? S17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? S17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? S22 C21 H21A 109.5 . . ? S22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? S22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 S22 C21 99.82(15) . . ? C23 S22 Co1 91.82(9) . . ? C21 S22 Co1 110.15(11) . . ? C24 C23 C28 121.9(3) . . ? C24 C23 S22 119.1(2) . . ? C28 C23 S22 118.86(19) . . ? C25 C24 C23 121.3(3) . . ? C25 C24 H24 119.4 . . ? C23 C24 H24 119.4 . . ? C24 C25 C26 118.8(3) . . ? C24 C25 H25 120.6 . . ? C26 C25 H25 120.6 . . ? C27 C26 C25 121.1(3) . . ? C27 C26 H26 119.5 . . ? C25 C26 H26 119.5 . . ? C26 C27 C28 122.3(3) . . ? C26 C27 H27 118.9 . . ? C28 C27 H27 118.9 . . ? N29 C28 C27 126.4(2) . . ? N29 C28 C23 119.1(2) . . ? C27 C28 C23 114.6(2) . . ? C28 N29 C30 117.5(2) . . ? C28 N29 Co1 119.51(17) . . ? C30 N29 Co1 121.20(15) . . ? N29 C30 C31 113.0(2) . . ? N29 C30 H30A 109.0 . . ? C31 C30 H30A 109.0 . . ? N29 C30 H30B 109.0 . . ? C31 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? C36 C31 C32 117.8(2) . . ? C36 C31 C30 120.2(2) . . ? C32 C31 C30 122.0(2) . . ? C33 C32 C31 121.6(2) . . ? C33 C32 H32 119.2 . . ? C31 C32 H32 119.2 . . ? C34 C33 C32 119.7(3) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 120.1(3) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C34 C35 C36 119.8(3) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C35 C36 C31 120.9(2) . . ? C35 C36 S37 122.5(2) . . ? C31 C36 S37 116.57(19) . . ? C36 S37 C38 103.99(13) . . ? C36 S37 Co1 102.02(8) . . ? C38 S37 Co1 110.79(10) . . ? S37 C38 H38A 109.5 . . ? S37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? S37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 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 N9 1.967(2) . ? Co1 N29 1.974(2) . ? Co1 S2 2.4723(7) . ? Co1 S22 2.4780(7) . ? Co1 S17 2.6481(7) . ? Co1 S37 2.7027(7) . ? C1 S2 1.795(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? S2 C3 1.772(3) . ? C3 C4 1.376(3) . ? C3 C8 1.424(3) . ? C4 C5 1.373(4) . ? C4 H4 0.9500 . ? C5 C6 1.390(4) . ? C5 H5 0.9500 . ? C6 C7 1.374(4) . ? C6 H6 0.9500 . ? C7 C8 1.409(3) . ? C7 H7 0.9500 . ? C8 N9 1.363(3) . ? N9 C10 1.472(3) . ? C10 C11 1.511(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.386(4) . ? C11 C16 1.400(4) . ? C12 C13 1.386(4) . ? C12 H12 0.9500 . ? C13 C14 1.375(5) . ? C13 H13 0.9500 . ? C14 C15 1.378(5) . ? C14 H14 0.9500 . ? C15 C16 1.390(4) . ? C15 H15 0.9500 . ? C16 S17 1.767(3) . ? S17 C18 1.795(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C21 S22 1.801(3) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? S22 C23 1.782(3) . ? C23 C24 1.376(4) . ? C23 C28 1.424(4) . ? C24 C25 1.358(4) . ? C24 H24 0.9500 . ? C25 C26 1.386(5) . ? C25 H25 0.9500 . ? C26 C27 1.364(4) . ? C26 H26 0.9500 . ? C27 C28 1.415(4) . ? C27 H27 0.9500 . ? C28 N29 1.363(3) . ? N29 C30 1.463(3) . ? C30 C31 1.517(3) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C36 1.391(3) . ? C31 C32 1.394(3) . ? C32 C33 1.380(4) . ? C32 H32 0.9500 . ? C33 C34 1.374(4) . ? C33 H33 0.9500 . ? C34 C35 1.387(4) . ? C34 H34 0.9500 . ? C35 C36 1.389(3) . ? C35 H35 0.9500 . ? C36 S37 1.772(3) . ? S37 C38 1.789(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C10 H10A S17 0.99 2.86 3.834(3) 169.5 2_546 C10 H10A S17 0.99 2.86 3.834(3) 169.5 2_546 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 C1 S2 C3 C4 87.8(2) . . . . ? Co1 S2 C3 C4 -159.3(2) . . . . ? C1 S2 C3 C8 -89.9(2) . . . . ? Co1 S2 C3 C8 23.0(2) . . . . ? C8 C3 C4 C5 3.7(4) . . . . ? S2 C3 C4 C5 -173.8(2) . . . . ? C3 C4 C5 C6 1.1(4) . . . . ? C4 C5 C6 C7 -3.3(4) . . . . ? C5 C6 C7 C8 0.8(4) . . . . ? C6 C7 C8 N9 -176.1(2) . . . . ? C6 C7 C8 C3 3.8(4) . . . . ? C4 C3 C8 N9 173.9(2) . . . . ? S2 C3 C8 N9 -8.5(3) . . . . ? C4 C3 C8 C7 -6.0(4) . . . . ? S2 C3 C8 C7 171.57(18) . . . . ? C7 C8 N9 C10 -7.1(4) . . . . ? C3 C8 N9 C10 173.0(2) . . . . ? C7 C8 N9 Co1 161.0(2) . . . . ? C3 C8 N9 Co1 -18.9(3) . . . . ? C8 N9 C10 C11 88.2(3) . . . . ? Co1 N9 C10 C11 -79.7(3) . . . . ? N9 C10 C11 C12 -111.8(3) . . . . ? N9 C10 C11 C16 67.7(3) . . . . ? C16 C11 C12 C13 -1.9(4) . . . . ? C10 C11 C12 C13 177.6(3) . . . . ? C11 C12 C13 C14 -0.1(5) . . . . ? C12 C13 C14 C15 1.9(5) . . . . ? C13 C14 C15 C16 -1.7(5) . . . . ? C14 C15 C16 C11 -0.3(4) . . . . ? C14 C15 C16 S17 176.5(2) . . . . ? C12 C11 C16 C15 2.0(4) . . . . ? C10 C11 C16 C15 -177.4(2) . . . . ? C12 C11 C16 S17 -174.99(19) . . . . ? C10 C11 C16 S17 5.5(3) . . . . ? C15 C16 S17 C18 11.5(3) . . . . ? C11 C16 S17 C18 -171.6(2) . . . . ? C15 C16 S17 Co1 134.9(2) . . . . ? C11 C16 S17 Co1 -48.2(2) . . . . ? C21 S22 C23 C24 86.2(3) . . . . ? Co1 S22 C23 C24 -163.0(3) . . . . ? C21 S22 C23 C28 -90.1(3) . . . . ? Co1 S22 C23 C28 20.7(2) . . . . ? C28 C23 C24 C25 1.4(6) . . . . ? S22 C23 C24 C25 -174.7(3) . . . . ? C23 C24 C25 C26 1.3(7) . . . . ? C24 C25 C26 C27 -2.8(7) . . . . ? C25 C26 C27 C28 1.6(6) . . . . ? C26 C27 C28 N29 -178.1(3) . . . . ? C26 C27 C28 C23 1.0(5) . . . . ? C24 C23 C28 N29 176.7(3) . . . . ? S22 C23 C28 N29 -7.1(4) . . . . ? C24 C23 C28 C27 -2.5(4) . . . . ? S22 C23 C28 C27 173.6(2) . . . . ? C27 C28 N29 C30 -3.9(4) . . . . ? C23 C28 N29 C30 176.9(2) . . . . ? C27 C28 N29 Co1 161.2(2) . . . . ? C23 C28 N29 Co1 -17.9(3) . . . . ? C28 N29 C30 C31 89.2(3) . . . . ? Co1 N29 C30 C31 -75.6(2) . . . . ? N29 C30 C31 C36 72.2(3) . . . . ? N29 C30 C31 C32 -106.3(3) . . . . ? C36 C31 C32 C33 -1.0(4) . . . . ? C30 C31 C32 C33 177.6(2) . . . . ? C31 C32 C33 C34 -0.3(4) . . . . ? C32 C33 C34 C35 1.1(4) . . . . ? C33 C34 C35 C36 -0.7(4) . . . . ? C34 C35 C36 C31 -0.6(4) . . . . ? C34 C35 C36 S37 178.1(2) . . . . ? C32 C31 C36 C35 1.5(3) . . . . ? C30 C31 C36 C35 -177.2(2) . . . . ? C32 C31 C36 S37 -177.32(18) . . . . ? C30 C31 C36 S37 4.1(3) . . . . ? C35 C36 S37 C38 15.4(2) . . . . ? C31 C36 S37 C38 -165.87(19) . . . . ? C35 C36 S37 Co1 130.7(2) . . . . ? C31 C36 S37 Co1 -50.59(19) . . . . ?