Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2004 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Lawrence Gahan' 'German Cavigliasso' 'Clint A. Sharrad' 'Robert Stranger' _publ_contact_author_name 'Dr Lawrence Gahan' _publ_contact_author_address ; Chemistry Department The University of Queensland Brisbane Queensland 4072 AUSTRALIA ; _publ_contact_author_email GAHAN@MAILBOX.UQ.EDU.AU _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Embracing Ligands. Synthesis, characterisation and the correlation between 59Cobalt NMR and ligand field parameters of cobalt(III) complexes with a new class of nitrogen-thioether multidentate ligand ; data_1709cs10 _database_code_depnum_ccdc_archive 'CCDC 222245' _audit_creation_date 2003-08-26T21:01:03-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common [Co(XyN4S2amp)]Br3.3H2O _chemical_formula_sum 'C36 H80 Br6 Co2 N8 O6 S4' _chemical_formula_weight 1446.64 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 23.719(5) _cell_length_b 9.7912(9) _cell_length_c 24.073(2) _cell_angle_alpha 90 _cell_angle_beta 99.626(7) _cell_angle_gamma 90 _cell_volume 5511.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.33 _exptl_crystal_size_min 0.22 _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2912 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.15 _exptl_absorpt_correction_type psiscans #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_decay_% 'less than 5 %' _diffrn_reflns_av_R_equivalents 0.0585 _diffrn_reflns_av_unetI/netI 0.0978 _diffrn_reflns_number 9941 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 9688 _reflns_number_gt 4281 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction XTAL3.2 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1144P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9688 _refine_ls_number_parameters 559 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1702 _refine_ls_R_factor_obs 0.0591 _refine_ls_wR_factor_all 0.2043 _refine_ls_wR_factor_obs 0.154 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.111 _refine_diff_density_min -0.949 _refine_diff_density_rms 0.164 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Co Co 0.3494 0.9721 '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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.91059(5) 0.86743(13) 0.36625(5) 0.0244(3) Uani 1 1 d . . . N2 N 0.8383(4) 0.8617(8) 0.3110(3) 0.033(2) Uani 1 1 d . . . H2A H 0.8423 0.7974 0.2853 0.039 Uiso 1 1 calc R . . H2B H 0.8105 0.8329 0.3295 0.039 Uiso 1 1 calc R . . N3 N 0.9783(3) 0.8748(8) 0.4249(3) 0.028(2) Uani 1 1 d . . . H3A H 0.9911 0.9615 0.4267 0.034 Uiso 1 1 calc R . . H3B H 0.9669 0.8568 0.458 0.034 Uiso 1 1 calc R . . N4 N 0.9547(3) 0.7686(8) 0.3153(3) 0.0284(19) Uani 1 1 d . . . H4A H 0.9291 0.7403 0.2856 0.034 Uiso 1 1 calc R . . H4B H 0.9768 0.8312 0.3021 0.034 Uiso 1 1 calc R . . N1 N 0.9328(3) 1.0399(8) 0.3306(3) 0.031(2) Uani 1 1 d . . . H1A H 0.9654 1.0697 0.3518 0.037 Uiso 1 1 calc R . . H1B H 0.9415 1.0171 0.2968 0.037 Uiso 1 1 calc R . . N5 N 1.0671(3) 1.0414(8) 0.1645(3) 0.030(2) Uani 1 1 d . . . H5A H 1.0347 1.0699 0.1426 0.036 Uiso 1 1 calc R . . H5B H 1.058 1.0214 0.1984 0.036 Uiso 1 1 calc R . . N6 N 1.1624(3) 0.8645(8) 0.1866(3) 0.029(2) Uani 1 1 d . . . H6A H 1.1585 0.8023 0.2132 0.034 Uiso 1 1 calc R . . H6B H 1.1902 0.8339 0.1684 0.034 Uiso 1 1 calc R . . N7 N 1.0215(3) 0.8694(8) 0.0736(3) 0.029(2) Uani 1 1 d . . . H7A H 1.0085 0.9559 0.0711 0.035 Uiso 1 1 calc R . . H7B H 1.0327 0.8498 0.0406 0.035 Uiso 1 1 calc R . . N8 N 1.0455(3) 0.7711(8) 0.1847(3) 0.032(2) Uani 1 1 d . . . H8A H 1.0708 0.7478 0.2154 0.038 Uiso 1 1 calc R . . H8B H 1.022 0.8337 0.1959 0.038 Uiso 1 1 calc R . . S2 S 0.89158(11) 0.6540(3) 0.39388(10) 0.0288(6) Uani 1 1 d . . . S1 S 0.86738(11) 1.0066(3) 0.42217(10) 0.0306(6) Uani 1 1 d . . . S3 S 1.13191(10) 1.0026(3) 0.07411(9) 0.0282(6) Uani 1 1 d . . . S4 S 1.11007(11) 0.6519(3) 0.10574(10) 0.0294(6) Uani 1 1 d . . . C14 C 0.9611(4) 0.5869(10) 0.4260(4) 0.033(3) Uani 1 1 d . . . H14A H 0.968 0.6094 0.4658 0.039 Uiso 1 1 calc R . . H14B H 0.9607 0.4882 0.4226 0.039 Uiso 1 1 calc R . . C32 C 1.0404(4) 0.5830(11) 0.0749(5) 0.039(3) Uani 1 1 d . . . H32A H 1.0328 0.6047 0.035 0.047 Uiso 1 1 calc R . . H32B H 1.0413 0.4843 0.0785 0.047 Uiso 1 1 calc R . . C6 C 0.8224(4) 0.9301(10) 0.4689(4) 0.034(3) Uani 1 1 d . . . H6C H 0.8469 0.8833 0.4993 0.041 Uiso 1 1 calc R . . H6D H 0.8029 1.0026 0.4854 0.041 Uiso 1 1 calc R . . C13 C 0.8531(4) 0.6412(11) 0.4517(4) 0.034(3) Uani 1 1 d . . . H13A H 0.8518 0.5468 0.4636 0.041 Uiso 1 1 calc R . . H13B H 0.8721 0.6945 0.4833 0.041 Uiso 1 1 calc R . . C12 C 0.7922(4) 0.6949(11) 0.4326(4) 0.032(3) Uani 1 1 d . . . C7 C 0.7785(4) 0.8305(10) 0.4401(4) 0.030(2) Uani 1 1 d . . . C33 C 0.9721(4) 0.7796(10) 0.0785(4) 0.028(2) Uani 1 1 d . . . H33A H 0.9491 0.7675 0.0415 0.033 Uiso 1 1 calc R . . H33B H 0.9484 0.8232 0.1025 0.033 Uiso 1 1 calc R . . C16 C 0.9921(4) 0.6494(10) 0.3339(4) 0.034(3) Uani 1 1 d . . . H16A H 1.0261 0.6544 0.3165 0.041 Uiso 1 1 calc R . . H16B H 0.972 0.5659 0.3212 0.041 Uiso 1 1 calc R . . C34 C 1.0107(5) 0.6489(11) 0.1673(4) 0.039(3) Uani 1 1 d . . . H34A H 0.9771 0.6501 0.1855 0.047 Uiso 1 1 calc R . . H34B H 1.0327 0.5681 0.1801 0.047 Uiso 1 1 calc R . . C15 C 1.0271(4) 0.7862(10) 0.4211(4) 0.032(3) Uani 1 1 d . . . H15A H 1.05 0.7772 0.4583 0.038 Uiso 1 1 calc R . . H15B H 1.0507 0.829 0.3968 0.038 Uiso 1 1 calc R . . C31 C 1.1500(4) 0.6354(10) 0.0466(4) 0.029(2) Uani 1 1 d . . . H31A H 1.1523 0.5401 0.0362 0.035 Uiso 1 1 calc R . . H31B H 1.1305 0.6851 0.0141 0.035 Uiso 1 1 calc R . . C30 C 1.2083(4) 0.6918(10) 0.0643(4) 0.028(2) Uani 1 1 d . . . C8 C 0.7233(5) 0.8754(12) 0.4227(5) 0.043(3) Uani 1 1 d . . . H8 H 0.7139 0.9655 0.4292 0.052 Uiso 1 1 calc R . . C11 C 0.7505(5) 0.6077(12) 0.4056(4) 0.045(3) Uani 1 1 d . . . H11 H 0.7595 0.5169 0.3996 0.054 Uiso 1 1 calc R . . C17 C 1.0099(4) 0.6446(11) 0.3984(4) 0.032(3) Uani 1 1 d . . . C35 C 0.9914(4) 0.6396(10) 0.1030(4) 0.029(2) Uani 1 1 d . . . C3 C 0.8931(4) 1.1585(11) 0.3214(4) 0.035(3) Uani 1 1 d . . . H3C H 0.899 1.2063 0.2875 0.043 Uiso 1 1 calc R . . H3D H 0.9022 1.2213 0.3528 0.043 Uiso 1 1 calc R . . C21 C 1.1073(5) 1.1606(10) 0.1726(5) 0.037(3) Uani 1 1 d . . . H21A H 1.1013 1.2109 0.2058 0.045 Uiso 1 1 calc R . . H21B H 1.0984 1.2212 0.1404 0.045 Uiso 1 1 calc R . . C24 C 1.1763(4) 0.9258(11) 0.0270(4) 0.036(3) Uani 1 1 d . . . H24A H 1.1514 0.8777 -0.0028 0.043 Uiso 1 1 calc R . . H24B H 1.1948 0.9987 0.0095 0.043 Uiso 1 1 calc R . . C22 C 1.1834(4) 0.9949(10) 0.2162(4) 0.032(2) Uani 1 1 d . . . H22A H 1.2245 0.9891 0.2282 0.039 Uiso 1 1 calc R . . H22B H 1.1659 1.0051 0.2497 0.039 Uiso 1 1 calc R . . C25 C 1.2207(5) 0.8300(11) 0.0539(4) 0.035(3) Uani 1 1 d . . . C4 C 0.8176(4) 0.9883(11) 0.2800(4) 0.040(3) Uani 1 1 d . . . H4C H 0.7766 0.982 0.268 0.049 Uiso 1 1 calc R . . H4D H 0.8352 0.9955 0.2465 0.049 Uiso 1 1 calc R . . C36 C 0.9412(4) 0.5415(11) 0.0910(4) 0.042(3) Uani 1 1 d . . . H36A H 0.9525 0.4537 0.1067 0.064 Uiso 1 1 calc R . . H36B H 0.9294 0.5329 0.051 0.064 Uiso 1 1 calc R . . H36C H 0.91 0.5759 0.1076 0.064 Uiso 1 1 calc R . . C26 C 1.2773(5) 0.8757(12) 0.0714(4) 0.037(3) Uani 1 1 d . . . H26 H 1.2868 0.9655 0.0643 0.044 Uiso 1 1 calc R . . C29 C 1.2508(5) 0.6087(11) 0.0907(4) 0.042(3) Uani 1 1 d . . . H29 H 1.2427 0.5175 0.0966 0.051 Uiso 1 1 calc R . . C5 C 0.8135(5) 1.0978(11) 0.3735(4) 0.039(3) Uani 1 1 d . . . H5C H 0.7778 1.0475 0.369 0.047 Uiso 1 1 calc R . . H5D H 0.8071 1.1866 0.3892 0.047 Uiso 1 1 calc R . . C2 C 0.8312(5) 1.1171(10) 0.3157(4) 0.034(3) Uani 1 1 d . . . C23 C 1.1866(4) 1.0926(11) 0.1214(4) 0.033(3) Uani 1 1 d . . . H23A H 1.2216 1.0394 0.1264 0.04 Uiso 1 1 calc R . . H23B H 1.1942 1.1791 0.1045 0.04 Uiso 1 1 calc R . . C10 C 0.6951(5) 0.6552(14) 0.3872(5) 0.050(3) Uani 1 1 d . . . H10 H 0.6674 0.5956 0.3692 0.06 Uiso 1 1 calc R . . C20 C 1.1698(5) 1.1195(11) 0.1792(4) 0.035(3) Uani 1 1 d . . . C28 C 1.3058(5) 0.6575(13) 0.1089(5) 0.049(3) Uani 1 1 d . . . H28 H 1.3338 0.6001 0.128 0.059 Uiso 1 1 calc R . . C9 C 0.6812(5) 0.7865(14) 0.3954(5) 0.049(3) Uani 1 1 d . . . H9 H 0.6442 0.8176 0.383 0.059 Uiso 1 1 calc R . . C18 C 1.0608(5) 0.5507(12) 0.4113(5) 0.050(3) Uani 1 1 d . . . H18A H 1.0729 0.5455 0.4514 0.075 Uiso 1 1 calc R . . H18B H 1.0915 0.5855 0.394 0.075 Uiso 1 1 calc R . . H18C H 1.0504 0.4612 0.3968 0.075 Uiso 1 1 calc R . . C19 C 1.2063(5) 1.2395(11) 0.2073(5) 0.049(3) Uani 1 1 d . . . H19A H 1.2461 1.2153 0.2122 0.074 Uiso 1 1 calc R . . H19B H 1.1958 1.2588 0.2433 0.074 Uiso 1 1 calc R . . H19C H 1.1997 1.3189 0.1837 0.074 Uiso 1 1 calc R . . C1 C 0.7941(5) 1.2349(12) 0.2862(5) 0.058(4) Uani 1 1 d . . . H1C H 0.7544 1.2112 0.2828 0.086 Uiso 1 1 calc R . . H1D H 0.8036 1.25 0.2495 0.086 Uiso 1 1 calc R . . H1E H 0.8014 1.3167 0.3083 0.086 Uiso 1 1 calc R . . C27 C 1.3186(5) 0.7897(14) 0.0986(5) 0.053(3) Uani 1 1 d . . . H27 H 1.3555 0.822 0.1101 0.064 Uiso 1 1 calc R . . Co2 Co 1.09008(5) 0.86660(13) 0.13167(5) 0.0233(3) Uani 1 1 d . . . Br2 Br 0.85879(6) 0.57562(14) 0.22954(5) 0.0565(4) Uani 1 1 d . . . Br3 Br 1.14255(6) 0.57412(14) 0.27022(5) 0.0565(4) Uani 1 1 d . . . Br1 Br 0.97190(6) 0.80772(12) 0.56017(4) 0.0474(3) Uani 1 1 d . . . Br4 Br 0.96792(6) 1.18437(12) 0.06139(4) 0.0488(4) Uani 1 1 d . . . Br5 Br 1.18687(6) 1.28729(14) -0.01088(6) 0.0623(4) Uani 1 1 d . . . Br6 Br 1.06553(5) 0.98634(13) 0.30076(5) 0.0458(3) Uani 1 1 d . . . O1 O 0.9389(3) 0.9565(9) 0.2025(3) 0.056(2) Uani 1 1 d . . . O2 O 1.3221(4) 1.2112(13) 0.0079(6) 0.133(5) Uani 1 1 d . . . O3 O 0.6568(4) 0.3300(9) 0.3577(4) 0.067(3) Uani 1 1 d . . . O4 O 1.0431(5) 0.3350(10) 0.2824(4) 0.083(3) Uani 1 1 d . . . O5 O 1.1701(4) 0.7910(12) 0.3767(5) 0.105(4) Uani 1 1 d . . . O6 O 0.9528(5) 0.2351(13) 0.2034(4) 0.112(4) Uani 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 0.0259(8) 0.0244(8) 0.0223(7) 0.0018(6) 0.0027(6) -0.0001(6) N2 0.043(6) 0.028(5) 0.025(5) -0.005(4) -0.002(4) 0.004(4) N3 0.032(5) 0.022(5) 0.029(5) 0.005(4) 0.003(4) -0.004(4) N4 0.030(5) 0.030(5) 0.025(4) -0.001(4) 0.004(4) -0.005(4) N1 0.041(5) 0.026(5) 0.028(4) 0.008(4) 0.009(4) 0.005(4) N5 0.038(5) 0.034(5) 0.018(4) -0.005(4) 0.005(4) 0.013(4) N6 0.027(5) 0.029(5) 0.030(5) -0.001(4) 0.006(4) -0.003(4) N7 0.039(5) 0.032(5) 0.017(4) -0.005(4) 0.002(4) 0.004(4) N8 0.030(5) 0.040(5) 0.026(4) -0.003(4) 0.007(4) -0.009(4) S2 0.0292(15) 0.0258(14) 0.0312(14) 0.0016(12) 0.0041(12) -0.0028(12) S1 0.0372(14) 0.0282(14) 0.0279(13) 0.0027(13) 0.0096(11) -0.0039(14) S3 0.0370(14) 0.0236(13) 0.0244(12) 0.0025(12) 0.0067(10) 0.0003(13) S4 0.0335(15) 0.0260(14) 0.0282(14) -0.0003(12) 0.0039(12) 0.0024(12) C14 0.030(6) 0.027(6) 0.039(6) 0.002(5) 0.002(5) 0.005(5) C32 0.040(7) 0.030(6) 0.047(7) -0.009(5) 0.004(6) -0.002(5) C6 0.044(7) 0.031(6) 0.031(6) -0.009(5) 0.015(5) 0.000(5) C13 0.049(7) 0.036(6) 0.016(5) 0.002(5) 0.002(5) -0.008(6) C12 0.030(6) 0.049(8) 0.016(5) 0.007(5) 0.006(4) 0.005(6) C7 0.033(6) 0.025(6) 0.035(6) 0.003(5) 0.014(5) -0.001(5) C33 0.018(5) 0.038(6) 0.027(5) -0.007(5) 0.005(4) -0.005(5) C16 0.039(7) 0.030(6) 0.034(6) -0.004(5) 0.010(5) 0.009(5) C34 0.035(7) 0.045(7) 0.037(6) -0.001(6) 0.007(5) -0.007(6) C15 0.026(6) 0.034(6) 0.032(6) 0.009(5) -0.006(5) 0.003(5) C31 0.031(6) 0.024(5) 0.032(6) -0.008(5) 0.008(5) 0.003(5) C30 0.030(6) 0.026(6) 0.028(6) -0.006(5) 0.008(5) 0.002(5) C8 0.048(8) 0.037(7) 0.050(7) -0.001(6) 0.024(6) 0.002(6) C11 0.053(8) 0.048(8) 0.035(6) -0.011(6) 0.012(6) -0.010(7) C17 0.021(6) 0.040(7) 0.034(6) 0.009(5) 0.000(5) 0.002(5) C35 0.036(6) 0.020(6) 0.030(6) -0.004(5) 0.002(5) -0.007(5) C3 0.027(6) 0.040(7) 0.039(6) 0.014(5) 0.005(5) -0.002(5) C21 0.050(7) 0.023(6) 0.038(6) -0.012(5) 0.004(5) -0.007(5) C24 0.049(7) 0.032(6) 0.027(6) 0.004(5) 0.006(5) 0.007(5) C22 0.032(6) 0.042(7) 0.023(5) -0.007(5) 0.009(4) -0.008(6) C25 0.043(7) 0.050(7) 0.012(5) -0.010(5) 0.007(5) 0.021(6) C4 0.038(6) 0.050(7) 0.031(6) 0.008(6) 0.001(5) -0.011(6) C36 0.043(7) 0.035(7) 0.049(7) -0.016(5) 0.004(5) -0.012(6) C26 0.031(6) 0.040(7) 0.042(6) -0.009(5) 0.013(5) -0.009(6) C29 0.051(8) 0.030(7) 0.046(7) -0.003(5) 0.008(6) -0.001(6) C5 0.043(7) 0.026(6) 0.051(7) 0.009(5) 0.012(6) 0.008(5) C2 0.034(7) 0.029(6) 0.039(6) 0.013(5) 0.008(5) 0.017(5) C23 0.033(6) 0.038(6) 0.033(6) 0.004(5) 0.016(5) -0.010(5) C10 0.045(8) 0.061(9) 0.042(7) -0.006(7) -0.001(6) -0.012(7) C20 0.041(7) 0.036(7) 0.029(6) -0.003(5) 0.008(5) 0.004(5) C28 0.036(8) 0.052(8) 0.054(8) 0.011(6) -0.010(6) 0.003(6) C9 0.027(6) 0.060(9) 0.057(8) 0.011(7) -0.003(6) 0.000(7) C18 0.048(8) 0.044(8) 0.057(8) 0.012(6) 0.005(6) 0.001(6) C19 0.044(7) 0.044(8) 0.061(8) -0.026(6) 0.013(6) -0.013(6) C1 0.061(8) 0.043(8) 0.069(9) 0.025(7) 0.009(7) 0.012(7) C27 0.031(7) 0.069(9) 0.059(8) -0.020(8) 0.007(6) -0.015(7) Co2 0.0261(8) 0.0250(8) 0.0186(7) -0.0005(6) 0.0030(6) 0.0013(6) Br2 0.0619(9) 0.0585(8) 0.0463(7) -0.0099(6) 0.0015(6) -0.0120(7) Br3 0.0572(8) 0.0560(8) 0.0554(8) 0.0166(7) 0.0067(7) 0.0058(7) Br1 0.0701(9) 0.0381(7) 0.0321(6) -0.0005(5) 0.0033(6) -0.0200(6) Br4 0.0656(8) 0.0462(8) 0.0311(6) -0.0030(5) -0.0023(6) 0.0245(6) Br5 0.0753(9) 0.0464(8) 0.0591(8) 0.0139(7) -0.0069(7) -0.0053(7) Br6 0.0441(6) 0.0622(8) 0.0311(5) -0.0037(6) 0.0062(5) -0.0092(6) O1 0.039(5) 0.092(7) 0.039(4) -0.012(5) 0.009(4) -0.003(5) O2 0.060(7) 0.116(10) 0.216(15) 0.077(10) 0.000(8) 0.004(7) O3 0.068(6) 0.066(6) 0.065(6) -0.001(5) 0.003(5) 0.006(5) O4 0.102(8) 0.062(7) 0.085(7) 0.000(5) 0.011(6) 0.005(6) O5 0.066(7) 0.114(9) 0.130(10) -0.010(8) -0.004(7) -0.005(7) O6 0.105(9) 0.150(11) 0.074(7) 0.054(7) -0.004(6) -0.053(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 1.955(7) . ? Co1 N2 1.987(8) . ? Co1 N4 1.991(8) . ? Co1 N1 2.004(7) . ? Co1 S2 2.261(3) . ? Co1 S1 2.276(3) . ? N2 C4 1.487(12) . ? N3 C15 1.461(12) . ? N4 C16 1.489(12) . ? N1 C3 1.488(12) . ? N5 C21 1.499(12) . ? N5 Co2 1.999(7) . ? N6 C22 1.507(11) . ? N6 Co2 1.983(8) . ? N7 C33 1.486(12) . ? N7 Co2 1.959(7) . ? N8 C34 1.474(12) . ? N8 Co2 2.017(8) . ? S2 C13 1.792(10) . ? S2 C14 1.822(9) . ? S1 C5 1.817(10) . ? S1 C6 1.833(10) . ? S3 C23 1.806(10) . ? S3 C24 1.832(10) . ? S3 Co2 2.266(3) . ? S4 C32 1.824(10) . ? S4 C31 1.845(9) . ? S4 Co2 2.265(3) . ? C14 C17 1.535(13) . ? C32 C35 1.542(14) . ? C6 C7 1.508(13) . ? C13 C12 1.532(13) . ? C12 C11 1.385(14) . ? C12 C7 1.386(14) . ? C7 C8 1.378(14) . ? C33 C35 1.532(13) . ? C16 C17 1.542(13) . ? C34 C35 1.542(13) . ? C15 C17 1.520(14) . ? C31 C30 1.483(13) . ? C30 C29 1.366(14) . ? C30 C25 1.416(14) . ? C8 C9 1.404(15) . ? C11 C10 1.395(16) . ? C17 C18 1.508(14) . ? C35 C36 1.519(13) . ? C3 C2 1.507(14) . ? C21 C20 1.519(15) . ? C24 C25 1.477(13) . ? C22 C20 1.514(13) . ? C25 C26 1.412(14) . ? C4 C2 1.529(14) . ? C26 C27 1.371(16) . ? C29 C28 1.390(15) . ? C5 C2 1.532(14) . ? C2 C1 1.549(13) . ? C23 C20 1.533(13) . ? C10 C9 1.350(16) . ? C20 C19 1.546(14) . ? C28 C27 1.362(16) . ? 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 N3 Co1 N2 175.8(4) . . ? N3 Co1 N4 90.6(3) . . ? N2 Co1 N4 93.3(3) . . ? N3 Co1 N1 92.0(3) . . ? N2 Co1 N1 89.8(3) . . ? N4 Co1 N1 86.7(3) . . ? N3 Co1 S2 90.1(2) . . ? N2 Co1 S2 88.7(2) . . ? N4 Co1 S2 83.3(2) . . ? N1 Co1 S2 169.8(2) . . ? N3 Co1 S1 87.0(2) . . ? N2 Co1 S1 89.4(3) . . ? N4 Co1 S1 172.0(2) . . ? N1 Co1 S1 85.7(2) . . ? S2 Co1 S1 104.34(10) . . ? C4 N2 Co1 119.2(6) . . ? C15 N3 Co1 119.8(6) . . ? C16 N4 Co1 123.0(6) . . ? C3 N1 Co1 121.1(6) . . ? C21 N5 Co2 120.5(6) . . ? C22 N6 Co2 119.2(6) . . ? C33 N7 Co2 120.5(6) . . ? C34 N8 Co2 121.7(6) . . ? C13 S2 C14 100.8(5) . . ? C13 S2 Co1 116.5(4) . . ? C14 S2 Co1 104.3(3) . . ? C5 S1 C6 100.2(5) . . ? C5 S1 Co1 104.5(4) . . ? C6 S1 Co1 118.9(3) . . ? C23 S3 C24 99.4(5) . . ? C23 S3 Co2 104.1(3) . . ? C24 S3 Co2 119.5(3) . . ? C32 S4 C31 101.6(5) . . ? C32 S4 Co2 103.8(3) . . ? C31 S4 Co2 116.9(3) . . ? C17 C14 S2 112.2(7) . . ? C35 C32 S4 112.7(7) . . ? C7 C6 S1 114.2(7) . . ? C12 C13 S2 108.6(6) . . ? C11 C12 C7 119.1(10) . . ? C11 C12 C13 119.5(10) . . ? C7 C12 C13 121.3(10) . . ? C8 C7 C12 119.9(10) . . ? C8 C7 C6 118.7(10) . . ? C12 C7 C6 121.3(10) . . ? N7 C33 C35 111.7(8) . . ? N4 C16 C17 112.0(8) . . ? N8 C34 C35 113.0(8) . . ? N3 C15 C17 113.3(8) . . ? C30 C31 S4 108.6(6) . . ? C29 C30 C25 119.5(10) . . ? C29 C30 C31 119.5(9) . . ? C25 C30 C31 121.0(9) . . ? C7 C8 C9 120.7(11) . . ? C12 C11 C10 120.3(11) . . ? C18 C17 C15 108.9(8) . . ? C18 C17 C14 108.8(8) . . ? C15 C17 C14 110.9(9) . . ? C18 C17 C16 107.5(9) . . ? C15 C17 C16 110.3(8) . . ? C14 C17 C16 110.4(8) . . ? C36 C35 C33 108.5(8) . . ? C36 C35 C32 108.2(8) . . ? C33 C35 C32 110.6(8) . . ? C36 C35 C34 108.6(8) . . ? C33 C35 C34 110.7(8) . . ? C32 C35 C34 110.0(8) . . ? N1 C3 C2 112.7(8) . . ? N5 C21 C20 113.4(8) . . ? C25 C24 S3 115.4(7) . . ? N6 C22 C20 112.5(7) . . ? C26 C25 C30 117.8(9) . . ? C26 C25 C24 120.2(11) . . ? C30 C25 C24 122.1(10) . . ? N2 C4 C2 112.6(7) . . ? C27 C26 C25 121.0(11) . . ? C30 C29 C28 121.6(11) . . ? C2 C5 S1 112.1(7) . . ? C3 C2 C4 112.6(9) . . ? C3 C2 C5 111.2(9) . . ? C4 C2 C5 110.1(9) . . ? C3 C2 C1 108.1(9) . . ? C4 C2 C1 107.9(9) . . ? C5 C2 C1 106.6(9) . . ? C20 C23 S3 112.8(7) . . ? C9 C10 C11 120.8(11) . . ? C22 C20 C21 112.5(9) . . ? C22 C20 C23 109.5(8) . . ? C21 C20 C23 110.3(9) . . ? C22 C20 C19 107.9(9) . . ? C21 C20 C19 108.0(9) . . ? C23 C20 C19 108.4(9) . . ? C27 C28 C29 119.6(11) . . ? C10 C9 C8 119.1(11) . . ? C28 C27 C26 120.6(11) . . ? N7 Co2 N6 176.4(3) . . ? N7 Co2 N5 91.2(3) . . ? N6 Co2 N5 90.5(3) . . ? N7 Co2 N8 89.9(3) . . ? N6 Co2 N8 93.4(3) . . ? N5 Co2 N8 86.6(3) . . ? N7 Co2 S4 90.2(2) . . ? N6 Co2 S4 88.6(2) . . ? N5 Co2 S4 170.7(2) . . ? N8 Co2 S4 84.3(3) . . ? N7 Co2 S3 87.2(2) . . ? N6 Co2 S3 89.7(2) . . ? N5 Co2 S3 85.1(2) . . ? N8 Co2 S3 171.1(3) . . ? S4 Co2 S3 104.09(10) . . ? 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 N3 Co1 N2 C4 97(5) . . . . ? N4 Co1 N2 C4 -105.3(7) . . . . ? N1 Co1 N2 C4 -18.6(7) . . . . ? S2 Co1 N2 C4 171.5(7) . . . . ? S1 Co1 N2 C4 67.1(7) . . . . ? N2 Co1 N3 C15 142(4) . . . . ? N4 Co1 N3 C15 -15.8(7) . . . . ? N1 Co1 N3 C15 -102.5(7) . . . . ? S2 Co1 N3 C15 67.5(7) . . . . ? S1 Co1 N3 C15 171.9(7) . . . . ? N3 Co1 N4 C16 47.2(7) . . . . ? N2 Co1 N4 C16 -131.2(7) . . . . ? N1 Co1 N4 C16 139.1(7) . . . . ? S2 Co1 N4 C16 -42.9(7) . . . . ? S1 Co1 N4 C16 119.4(16) . . . . ? N3 Co1 N1 C3 -124.4(7) . . . . ? N2 Co1 N1 C3 51.8(7) . . . . ? N4 Co1 N1 C3 145.1(8) . . . . ? S2 Co1 N1 C3 133.8(12) . . . . ? S1 Co1 N1 C3 -37.6(7) . . . . ? N3 Co1 S2 C13 83.9(4) . . . . ? N2 Co1 S2 C13 -92.1(4) . . . . ? N4 Co1 S2 C13 174.5(4) . . . . ? N1 Co1 S2 C13 -174.2(14) . . . . ? S1 Co1 S2 C13 -3.0(4) . . . . ? N3 Co1 S2 C14 -26.2(4) . . . . ? N2 Co1 S2 C14 157.8(4) . . . . ? N4 Co1 S2 C14 64.4(4) . . . . ? N1 Co1 S2 C14 75.7(15) . . . . ? S1 Co1 S2 C14 -113.1(4) . . . . ? N3 Co1 S1 C5 153.5(4) . . . . ? N2 Co1 S1 C5 -28.6(4) . . . . ? N4 Co1 S1 C5 81.0(17) . . . . ? N1 Co1 S1 C5 61.3(4) . . . . ? S2 Co1 S1 C5 -117.2(4) . . . . ? N3 Co1 S1 C6 -95.9(4) . . . . ? N2 Co1 S1 C6 82.0(5) . . . . ? N4 Co1 S1 C6 -168.4(17) . . . . ? N1 Co1 S1 C6 171.9(5) . . . . ? S2 Co1 S1 C6 -6.5(4) . . . . ? C13 S2 C14 C17 -152.9(8) . . . . ? Co1 S2 C14 C17 -31.7(8) . . . . ? C31 S4 C32 C35 -154.3(7) . . . . ? Co2 S4 C32 C35 -32.6(8) . . . . ? C5 S1 C6 C7 62.9(8) . . . . ? Co1 S1 C6 C7 -50.1(9) . . . . ? C14 S2 C13 C12 179.7(7) . . . . ? Co1 S2 C13 C12 67.6(8) . . . . ? S2 C13 C12 C11 85.7(10) . . . . ? S2 C13 C12 C7 -92.1(10) . . . . ? C11 C12 C7 C8 2.6(15) . . . . ? C13 C12 C7 C8 -179.6(9) . . . . ? C11 C12 C7 C6 -179.6(9) . . . . ? C13 C12 C7 C6 -1.8(14) . . . . ? S1 C6 C7 C8 -97.7(10) . . . . ? S1 C6 C7 C12 84.5(11) . . . . ? Co2 N7 C33 C35 -37.6(10) . . . . ? Co1 N4 C16 C17 -20.7(11) . . . . ? Co2 N8 C34 C35 -24.4(11) . . . . ? Co1 N3 C15 C17 -38.0(10) . . . . ? C32 S4 C31 C30 178.3(7) . . . . ? Co2 S4 C31 C30 66.2(7) . . . . ? S4 C31 C30 C29 87.9(10) . . . . ? S4 C31 C30 C25 -92.5(9) . . . . ? C12 C7 C8 C9 -2.6(16) . . . . ? C6 C7 C8 C9 179.5(10) . . . . ? C7 C12 C11 C10 -1.3(15) . . . . ? C13 C12 C11 C10 -179.2(9) . . . . ? N3 C15 C17 C18 -164.2(8) . . . . ? N3 C15 C17 C14 -44.5(11) . . . . ? N3 C15 C17 C16 78.1(10) . . . . ? S2 C14 C17 C18 -159.7(7) . . . . ? S2 C14 C17 C15 80.5(9) . . . . ? S2 C14 C17 C16 -42.0(10) . . . . ? N4 C16 C17 C18 -162.6(8) . . . . ? N4 C16 C17 C15 -44.0(11) . . . . ? N4 C16 C17 C14 78.9(10) . . . . ? N7 C33 C35 C36 -163.6(8) . . . . ? N7 C33 C35 C32 -45.0(10) . . . . ? N7 C33 C35 C34 77.2(10) . . . . ? S4 C32 C35 C36 -159.1(7) . . . . ? S4 C32 C35 C33 82.1(9) . . . . ? S4 C32 C35 C34 -40.5(10) . . . . ? N8 C34 C35 C36 -161.3(8) . . . . ? N8 C34 C35 C33 -42.2(11) . . . . ? N8 C34 C35 C32 80.3(10) . . . . ? Co1 N1 C3 C2 -26.2(11) . . . . ? Co2 N5 C21 C20 -25.7(11) . . . . ? C23 S3 C24 C25 61.8(9) . . . . ? Co2 S3 C24 C25 -50.4(9) . . . . ? Co2 N6 C22 C20 -34.7(10) . . . . ? C29 C30 C25 C26 0.4(14) . . . . ? C31 C30 C25 C26 -179.2(9) . . . . ? C29 C30 C25 C24 -178.3(9) . . . . ? C31 C30 C25 C24 2.1(14) . . . . ? S3 C24 C25 C26 -96.4(10) . . . . ? S3 C24 C25 C30 82.3(11) . . . . ? Co1 N2 C4 C2 -34.6(11) . . . . ? C30 C25 C26 C27 -1.5(14) . . . . ? C24 C25 C26 C27 177.2(10) . . . . ? C25 C30 C29 C28 1.5(16) . . . . ? C31 C30 C29 C28 -178.9(10) . . . . ? C6 S1 C5 C2 -153.6(8) . . . . ? Co1 S1 C5 C2 -29.9(8) . . . . ? N1 C3 C2 C4 -41.4(12) . . . . ? N1 C3 C2 C5 82.8(11) . . . . ? N1 C3 C2 C1 -160.5(9) . . . . ? N2 C4 C2 C3 76.2(11) . . . . ? N2 C4 C2 C5 -48.5(11) . . . . ? N2 C4 C2 C1 -164.5(9) . . . . ? S1 C5 C2 C3 -43.0(11) . . . . ? S1 C5 C2 C4 82.5(10) . . . . ? S1 C5 C2 C1 -160.7(8) . . . . ? C24 S3 C23 C20 -156.2(8) . . . . ? Co2 S3 C23 C20 -32.4(8) . . . . ? C12 C11 C10 C9 0.1(17) . . . . ? N6 C22 C20 C21 75.6(10) . . . . ? N6 C22 C20 C23 -47.5(11) . . . . ? N6 C22 C20 C19 -165.3(8) . . . . ? N5 C21 C20 C22 -41.5(12) . . . . ? N5 C21 C20 C23 81.1(11) . . . . ? N5 C21 C20 C19 -160.5(8) . . . . ? S3 C23 C20 C22 83.9(9) . . . . ? S3 C23 C20 C21 -40.5(11) . . . . ? S3 C23 C20 C19 -158.6(8) . . . . ? C30 C29 C28 C27 -2.3(18) . . . . ? C11 C10 C9 C8 0.0(18) . . . . ? C7 C8 C9 C10 1.3(17) . . . . ? C29 C28 C27 C26 1.2(19) . . . . ? C25 C26 C27 C28 0.7(17) . . . . ? C33 N7 Co2 N6 139(5) . . . . ? C33 N7 Co2 N5 -103.0(7) . . . . ? C33 N7 Co2 N8 -16.4(7) . . . . ? C33 N7 Co2 S4 67.9(7) . . . . ? C33 N7 Co2 S3 172.0(7) . . . . ? C22 N6 Co2 N7 99(5) . . . . ? C22 N6 Co2 N5 -18.8(7) . . . . ? C22 N6 Co2 N8 -105.3(7) . . . . ? C22 N6 Co2 S4 170.5(6) . . . . ? C22 N6 Co2 S3 66.4(6) . . . . ? C21 N5 Co2 N7 -125.9(7) . . . . ? C21 N5 Co2 N6 50.9(7) . . . . ? C21 N5 Co2 N8 144.3(7) . . . . ? C21 N5 Co2 S4 135.4(13) . . . . ? C21 N5 Co2 S3 -38.8(7) . . . . ? C34 N8 Co2 N7 49.9(8) . . . . ? C34 N8 Co2 N6 -128.6(7) . . . . ? C34 N8 Co2 N5 141.1(8) . . . . ? C34 N8 Co2 S4 -40.3(7) . . . . ? C34 N8 Co2 S3 120.6(14) . . . . ? C32 S4 Co2 N7 -25.9(5) . . . . ? C31 S4 Co2 N7 84.9(4) . . . . ? C32 S4 Co2 N6 157.5(4) . . . . ? C31 S4 Co2 N6 -91.7(4) . . . . ? C32 S4 Co2 N5 72.9(16) . . . . ? C31 S4 Co2 N5 -176.3(15) . . . . ? C32 S4 Co2 N8 63.9(4) . . . . ? C31 S4 Co2 N8 174.7(4) . . . . ? C32 S4 Co2 S3 -113.1(4) . . . . ? C31 S4 Co2 S3 -2.3(4) . . . . ? C23 S3 Co2 N7 154.9(4) . . . . ? C24 S3 Co2 N7 -95.4(4) . . . . ? C23 S3 Co2 N6 -27.0(4) . . . . ? C24 S3 Co2 N6 82.6(4) . . . . ? C23 S3 Co2 N5 63.5(4) . . . . ? C24 S3 Co2 N5 173.1(4) . . . . ? C23 S3 Co2 N8 84.0(16) . . . . ? C24 S3 Co2 N8 -166.3(15) . . . . ? C23 S3 Co2 S4 -115.6(4) . . . . ? C24 S3 Co2 S4 -5.9(4) . . . . ? data_cs7070 _database_code_depnum_ccdc_archive 'CCDC 222246' _audit_creation_date 2003-08-26T17:18:52-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common [Co(PrN4S2amp)]Cl(ClO4)2.2H2O _chemical_formula_sum 'C13 H36 Cl3 Co N4 O10 S2' _chemical_formula_weight 637.86 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 10.334(1) _cell_length_b 15.389(2) _cell_length_c 16.216(3) _cell_angle_alpha 90 _cell_angle_beta 99.81(1) _cell_angle_gamma 90 _cell_volume 2541.1(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.43 _exptl_crystal_size_min 0.37 _exptl_crystal_density_diffrn 1.667 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.209 _exptl_absorpt_correction_type psiscans #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_decay_% 'less than 5 %' _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_unetI/netI 0.0207 _diffrn_reflns_number 4725 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.97 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4462 _reflns_number_gt 3771 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction XTAL3.2 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1999)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1005P)^2^+9.2048P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4462 _refine_ls_number_parameters 298 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_obs 0.0596 _refine_ls_wR_factor_all 0.1857 _refine_ls_wR_factor_obs 0.1761 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.59 _refine_diff_density_min -1.34 _refine_diff_density_rms 0.116 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19749(6) 0.62839(4) 0.22358(4) 0.0234(2) Uani 1 1 d . . . N3 N 0.2618(4) 0.7313(3) 0.1693(3) 0.0332(9) Uani 1 1 d . . . H3A H 0.2014 0.7735 0.1689 0.04 Uiso 1 1 calc R . . H3B H 0.3352 0.7497 0.2027 0.04 Uiso 1 1 calc R . . N1 N 0.2925(4) 0.6755(3) 0.3305(2) 0.0287(8) Uani 1 1 d . . . H1A H 0.3786 0.6651 0.3322 0.034 Uiso 1 1 calc R . . H1B H 0.2818 0.7336 0.3292 0.034 Uiso 1 1 calc R . . N2 N 0.1476(4) 0.5238(2) 0.2833(3) 0.0295(9) Uani 1 1 d . . . H2A H 0.0919 0.4926 0.246 0.035 Uiso 1 1 calc R . . H2B H 0.2207 0.4915 0.2974 0.035 Uiso 1 1 calc R . . N4 N 0.3506(4) 0.5619(3) 0.2002(2) 0.0286(8) Uani 1 1 d . . . H4A H 0.4104 0.5608 0.2475 0.034 Uiso 1 1 calc R . . H4B H 0.3242 0.5067 0.1892 0.034 Uiso 1 1 calc R . . S1 S 0.02116(11) 0.70331(8) 0.24697(8) 0.0310(3) Uani 1 1 d . . . S2 S 0.08422(12) 0.57715(8) 0.10167(8) 0.0333(3) Uani 1 1 d . . . C6 C -0.1221(5) 0.6406(4) 0.1990(4) 0.0440(13) Uani 1 1 d . . . H6A H -0.1053 0.579 0.2083 0.053 Uiso 1 1 calc R . . H6B H -0.1974 0.6563 0.2242 0.053 Uiso 1 1 calc R . . C3 C 0.2574(5) 0.6437(4) 0.4099(3) 0.0357(11) Uani 1 1 d . . . H3C H 0.2789 0.6883 0.4524 0.043 Uiso 1 1 calc R . . H3D H 0.3102 0.593 0.4282 0.043 Uiso 1 1 calc R . . C5 C 0.0232(5) 0.6917(3) 0.3588(3) 0.0345(11) Uani 1 1 d . . . H5A H 0.0504 0.7467 0.3855 0.041 Uiso 1 1 calc R . . H5B H -0.0659 0.6807 0.3675 0.041 Uiso 1 1 calc R . . C10 C 0.2923(6) 0.7256(4) 0.0827(4) 0.0430(13) Uani 1 1 d . . . H10A H 0.3652 0.764 0.0782 0.052 Uiso 1 1 calc R . . H10B H 0.2168 0.7455 0.0433 0.052 Uiso 1 1 calc R . . C4 C 0.0863(5) 0.5327(3) 0.3600(3) 0.0355(11) Uani 1 1 d . . . H4C H 0.1199 0.4871 0.3991 0.043 Uiso 1 1 calc R . . H4D H -0.0078 0.5245 0.3447 0.043 Uiso 1 1 calc R . . C9 C 0.2024(6) 0.5788(4) 0.0308(3) 0.0420(13) Uani 1 1 d . . . H9A H 0.2288 0.5194 0.0223 0.05 Uiso 1 1 calc R . . H9B H 0.1588 0.6007 -0.0229 0.05 Uiso 1 1 calc R . . C11 C 0.4183(5) 0.5908(4) 0.1318(3) 0.0391(12) Uani 1 1 d . . . H11A H 0.4603 0.541 0.1109 0.047 Uiso 1 1 calc R . . H11B H 0.4866 0.6318 0.1542 0.047 Uiso 1 1 calc R . . C8 C -0.0316(6) 0.6619(4) 0.0617(4) 0.0476(14) Uani 1 1 d . . . H8A H 0.0107 0.7182 0.0707 0.057 Uiso 1 1 calc R . . H8B H -0.0596 0.6542 0.0019 0.057 Uiso 1 1 calc R . . C2 C 0.1121(5) 0.6200(3) 0.4032(3) 0.0343(11) Uani 1 1 d . . . C12 C 0.3273(6) 0.6334(4) 0.0590(3) 0.0413(13) Uani 1 1 d . . . C7 C -0.1508(6) 0.6592(5) 0.1054(4) 0.0533(16) Uani 1 1 d . . . H7A H -0.2106 0.6151 0.0786 0.064 Uiso 1 1 calc R . . H7B H -0.1958 0.7147 0.0968 0.064 Uiso 1 1 calc R . . C1 C 0.0815(6) 0.6131(4) 0.4920(4) 0.0480(14) Uani 1 1 d . . . H1C H 0.0973 0.6681 0.5197 0.072 Uiso 1 1 calc R . . H1D H 0.1368 0.5697 0.5225 0.072 Uiso 1 1 calc R . . H1E H -0.0089 0.5971 0.4894 0.072 Uiso 1 1 calc R . . C13 C 0.4003(8) 0.6378(5) -0.0161(4) 0.0620(18) Uani 1 1 d . . . H13A H 0.4225 0.5801 -0.0313 0.093 Uiso 1 1 calc R . . H13B H 0.4792 0.6713 -0.0011 0.093 Uiso 1 1 calc R . . H13C H 0.3449 0.6647 -0.0626 0.093 Uiso 1 1 calc R . . Cl1 Cl 0.26321(17) 0.37437(9) 0.13265(11) 0.0539(4) Uani 1 1 d . . . Cl2 Cl -0.10952(16) 0.33354(11) 0.22972(13) 0.0636(5) Uani 1 1 d . . . Cl3 Cl 0.63987(17) 0.58550(16) 0.41465(13) 0.0793(7) Uani 1 1 d . . . O1 O -0.2342(6) 0.3005(4) 0.2183(6) 0.123(3) Uani 1 1 d . . . O2 O -0.1080(8) 0.4192(4) 0.2046(6) 0.132(3) Uani 1 1 d . . . O3 O -0.0312(16) 0.3163(13) 0.2958(11) 0.291(10) Uani 1 1 d . . . O4 O -0.0501(16) 0.2889(9) 0.1712(15) 0.302(12) Uani 1 1 d . . . O5 O 0.5624(8) 0.5914(5) 0.3400(5) 0.123(3) Uani 1 1 d . . . O6 O 0.7618(8) 0.6145(8) 0.4265(8) 0.173(5) Uani 1 1 d . . . O7 O 0.6257(9) 0.5006(8) 0.4456(8) 0.189(5) Uani 1 1 d . . . O8 O 0.5635(10) 0.6490(9) 0.4630(7) 0.181(5) Uani 1 1 d . . . O9 O 0.3754(5) 0.4045(3) 0.3515(3) 0.0613(12) Uani 1 1 d . . . O10 O 0.5644(8) 0.4253(5) 0.2433(6) 0.125(3) Uani 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 0.0226(3) 0.0173(3) 0.0299(4) 0.0005(2) 0.0032(2) 0.0001(2) N3 0.034(2) 0.023(2) 0.043(2) 0.0026(17) 0.0043(18) -0.0012(17) N1 0.0246(19) 0.025(2) 0.037(2) -0.0046(17) 0.0058(16) -0.0017(16) N2 0.031(2) 0.0204(19) 0.038(2) 0.0000(16) 0.0091(17) -0.0007(16) N4 0.030(2) 0.0237(19) 0.033(2) -0.0004(16) 0.0058(16) 0.0028(16) S1 0.0263(6) 0.0246(6) 0.0414(7) 0.0004(5) 0.0038(5) 0.0044(5) S2 0.0337(6) 0.0310(6) 0.0333(6) -0.0016(5) -0.0001(5) -0.0022(5) C6 0.024(2) 0.042(3) 0.065(4) -0.007(3) 0.003(2) 0.000(2) C3 0.036(3) 0.037(3) 0.033(3) -0.002(2) 0.004(2) 0.001(2) C5 0.032(3) 0.033(3) 0.040(3) -0.004(2) 0.011(2) 0.003(2) C10 0.051(3) 0.035(3) 0.044(3) 0.009(2) 0.011(3) -0.006(2) C4 0.037(3) 0.027(3) 0.045(3) 0.004(2) 0.014(2) -0.002(2) C9 0.050(3) 0.042(3) 0.034(3) 0.000(2) 0.008(2) 0.000(3) C11 0.034(3) 0.041(3) 0.045(3) 0.002(2) 0.017(2) 0.001(2) C8 0.042(3) 0.049(3) 0.045(3) 0.002(3) -0.011(3) 0.006(3) C2 0.033(3) 0.034(3) 0.037(3) 0.000(2) 0.011(2) 0.001(2) C12 0.048(3) 0.042(3) 0.037(3) 0.005(2) 0.015(2) -0.004(2) C7 0.034(3) 0.061(4) 0.059(4) -0.006(3) -0.010(3) 0.008(3) C1 0.051(3) 0.054(4) 0.042(3) 0.001(3) 0.016(3) 0.002(3) C13 0.074(5) 0.070(5) 0.050(4) 0.009(3) 0.031(3) -0.005(4) Cl1 0.0636(10) 0.0260(7) 0.0657(10) 0.0000(6) -0.0070(8) -0.0034(6) Cl2 0.0434(8) 0.0432(9) 0.0994(14) -0.0008(8) -0.0014(8) -0.0009(7) Cl3 0.0452(9) 0.1125(17) 0.0700(12) 0.0359(11) -0.0194(8) -0.0206(10) O1 0.058(4) 0.075(4) 0.238(10) 0.024(5) 0.029(5) -0.014(3) O2 0.119(6) 0.061(4) 0.201(9) 0.020(5) -0.018(6) -0.028(4) O3 0.234(16) 0.35(2) 0.241(16) 0.110(16) -0.111(13) 0.087(16) O4 0.235(15) 0.174(11) 0.56(3) -0.173(17) 0.26(2) -0.044(11) O5 0.130(6) 0.097(5) 0.112(5) -0.035(4) -0.069(5) 0.031(4) O6 0.058(4) 0.233(12) 0.224(11) 0.067(9) 0.009(6) -0.029(6) O7 0.118(7) 0.205(10) 0.235(11) 0.159(10) 0.005(7) 0.004(7) O8 0.114(7) 0.264(14) 0.171(10) -0.087(9) 0.042(7) 0.022(8) O9 0.059(3) 0.045(2) 0.077(3) 0.001(2) 0.004(2) -0.005(2) O10 0.107(6) 0.088(5) 0.186(8) -0.022(5) 0.040(5) 0.011(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N4 1.974(4) . ? Co1 N1 1.979(4) . ? Co1 N3 1.982(4) . ? Co1 N2 1.990(4) . ? Co1 S1 2.2426(13) . ? Co1 S2 2.2608(14) . ? N3 C10 1.493(7) . ? N1 C3 1.480(6) . ? N2 C4 1.495(6) . ? N4 C11 1.476(6) . ? S1 C5 1.819(5) . ? S1 C6 1.826(5) . ? S2 C9 1.814(6) . ? S2 C8 1.814(6) . ? C6 C7 1.524(9) . ? C3 C2 1.531(7) . ? C5 C2 1.535(7) . ? C10 C12 1.529(8) . ? C4 C2 1.517(7) . ? C9 C12 1.543(8) . ? C11 C12 1.527(8) . ? C8 C7 1.522(9) . ? C2 C1 1.529(7) . ? C12 C13 1.540(8) . ? Cl2 O3 1.256(11) . ? Cl2 O1 1.369(6) . ? Cl2 O2 1.381(7) . ? Cl2 O4 1.395(12) . ? Cl3 O6 1.319(8) . ? Cl3 O5 1.335(6) . ? Cl3 O7 1.415(9) . ? Cl3 O8 1.551(9) . ? 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 N4 Co1 N1 93.69(17) . . ? N4 Co1 N3 89.36(17) . . ? N1 Co1 N3 86.72(17) . . ? N4 Co1 N2 87.51(16) . . ? N1 Co1 N2 90.06(17) . . ? N3 Co1 N2 175.35(18) . . ? N4 Co1 S1 178.61(13) . . ? N1 Co1 S1 87.67(12) . . ? N3 Co1 S1 90.44(13) . . ? N2 Co1 S1 92.77(12) . . ? N4 Co1 S2 87.91(12) . . ? N1 Co1 S2 178.37(12) . . ? N3 Co1 S2 93.03(13) . . ? N2 Co1 S2 90.28(13) . . ? S1 Co1 S2 90.73(5) . . ? C10 N3 Co1 120.7(3) . . ? C3 N1 Co1 118.9(3) . . ? C4 N2 Co1 120.8(3) . . ? C11 N4 Co1 119.1(3) . . ? C5 S1 C6 104.1(3) . . ? C5 S1 Co1 104.28(17) . . ? C6 S1 Co1 106.21(19) . . ? C9 S2 C8 103.8(3) . . ? C9 S2 Co1 104.19(19) . . ? C8 S2 Co1 105.9(2) . . ? C7 C6 S1 109.3(4) . . ? N1 C3 C2 113.6(4) . . ? C2 C5 S1 116.2(3) . . ? N3 C10 C12 112.8(4) . . ? N2 C4 C2 113.5(4) . . ? C12 C9 S2 116.0(4) . . ? N4 C11 C12 113.7(4) . . ? C7 C8 S2 110.5(4) . . ? C4 C2 C1 109.0(4) . . ? C4 C2 C3 109.7(4) . . ? C1 C2 C3 107.9(5) . . ? C4 C2 C5 112.1(4) . . ? C1 C2 C5 106.7(4) . . ? C3 C2 C5 111.3(4) . . ? C11 C12 C10 110.2(5) . . ? C11 C12 C13 108.1(5) . . ? C10 C12 C13 109.1(5) . . ? C11 C12 C9 111.6(4) . . ? C10 C12 C9 111.0(5) . . ? C13 C12 C9 106.7(5) . . ? C8 C7 C6 115.6(5) . . ? O3 Cl2 O1 119.5(10) . . ? O3 Cl2 O2 114.6(10) . . ? O1 Cl2 O2 111.9(5) . . ? O3 Cl2 O4 100.4(12) . . ? O1 Cl2 O4 103.7(8) . . ? O2 Cl2 O4 104.0(9) . . ? O6 Cl3 O5 121.3(7) . . ? O6 Cl3 O7 114.5(6) . . ? O5 Cl3 O7 107.6(6) . . ? O6 Cl3 O8 105.6(8) . . ? O5 Cl3 O8 97.8(6) . . ? O7 Cl3 O8 108.1(8) . . ? 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 N4 Co1 N3 C10 53.6(4) . . . . ? N1 Co1 N3 C10 147.3(4) . . . . ? N2 Co1 N3 C10 101(2) . . . . ? S1 Co1 N3 C10 -125.0(4) . . . . ? S2 Co1 N3 C10 -34.3(4) . . . . ? N4 Co1 N1 C3 -109.2(4) . . . . ? N3 Co1 N1 C3 161.6(4) . . . . ? N2 Co1 N1 C3 -21.7(4) . . . . ? S1 Co1 N1 C3 71.0(3) . . . . ? S2 Co1 N1 C3 80(4) . . . . ? N4 Co1 N2 C4 144.2(4) . . . . ? N1 Co1 N2 C4 50.5(4) . . . . ? N3 Co1 N2 C4 97(2) . . . . ? S1 Co1 N2 C4 -37.1(4) . . . . ? S2 Co1 N2 C4 -127.9(4) . . . . ? N1 Co1 N4 C11 -109.3(4) . . . . ? N3 Co1 N4 C11 -22.6(4) . . . . ? N2 Co1 N4 C11 160.8(4) . . . . ? S1 Co1 N4 C11 59(5) . . . . ? S2 Co1 N4 C11 70.4(4) . . . . ? N4 Co1 S1 C5 152(5) . . . . ? N1 Co1 S1 C5 -39.5(2) . . . . ? N3 Co1 S1 C5 -126.2(2) . . . . ? N2 Co1 S1 C5 50.5(2) . . . . ? S2 Co1 S1 C5 140.79(18) . . . . ? N4 Co1 S1 C6 42(5) . . . . ? N1 Co1 S1 C6 -149.1(2) . . . . ? N3 Co1 S1 C6 124.2(2) . . . . ? N2 Co1 S1 C6 -59.2(2) . . . . ? S2 Co1 S1 C6 31.2(2) . . . . ? N4 Co1 S2 C9 -39.0(2) . . . . ? N1 Co1 S2 C9 131(4) . . . . ? N3 Co1 S2 C9 50.3(2) . . . . ? N2 Co1 S2 C9 -126.5(2) . . . . ? S1 Co1 S2 C9 140.8(2) . . . . ? N4 Co1 S2 C8 -148.1(3) . . . . ? N1 Co1 S2 C8 22(4) . . . . ? N3 Co1 S2 C8 -58.8(3) . . . . ? N2 Co1 S2 C8 124.5(3) . . . . ? S1 Co1 S2 C8 31.7(2) . . . . ? C5 S1 C6 C7 169.0(4) . . . . ? Co1 S1 C6 C7 -81.2(4) . . . . ? Co1 N1 C3 C2 -32.5(5) . . . . ? C6 S1 C5 C2 95.9(4) . . . . ? Co1 S1 C5 C2 -15.3(4) . . . . ? Co1 N3 C10 C12 -25.2(6) . . . . ? Co1 N2 C4 C2 -21.0(6) . . . . ? C8 S2 C9 C12 95.1(5) . . . . ? Co1 S2 C9 C12 -15.6(5) . . . . ? Co1 N4 C11 C12 -32.2(6) . . . . ? C9 S2 C8 C7 170.4(4) . . . . ? Co1 S2 C8 C7 -80.2(4) . . . . ? N2 C4 C2 C1 -163.6(4) . . . . ? N2 C4 C2 C3 -45.7(6) . . . . ? N2 C4 C2 C5 78.5(5) . . . . ? N1 C3 C2 C4 77.0(5) . . . . ? N1 C3 C2 C1 -164.4(4) . . . . ? N1 C3 C2 C5 -47.7(6) . . . . ? S1 C5 C2 C4 -52.0(5) . . . . ? S1 C5 C2 C1 -171.3(4) . . . . ? S1 C5 C2 C3 71.3(5) . . . . ? N4 C11 C12 C10 75.8(6) . . . . ? N4 C11 C12 C13 -165.1(5) . . . . ? N4 C11 C12 C9 -48.0(6) . . . . ? N3 C10 C12 C11 -42.8(6) . . . . ? N3 C10 C12 C13 -161.2(5) . . . . ? N3 C10 C12 C9 81.4(6) . . . . ? S2 C9 C12 C11 71.4(6) . . . . ? S2 C9 C12 C10 -51.9(6) . . . . ? S2 C9 C12 C13 -170.7(4) . . . . ? S2 C8 C7 C6 39.8(7) . . . . ? S1 C6 C7 C8 43.1(7) . . . . ? data_1843cs18 _database_code_depnum_ccdc_archive 'CCDC 222247' _audit_creation_date 2003-08-26T18:01:36-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common [Co(BuN4S2amp)]Cl2(ClO4).2H2O _chemical_formula_sum 'C14 H38 Cl3 Co N4 O6 S2' _chemical_formula_weight 587.88 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 10.873(1) _cell_length_b 18.484(1) _cell_length_c 13.636(2) _cell_angle_alpha 90 _cell_angle_beta 112.311(9) _cell_angle_gamma 90 _cell_volume 2535.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.54 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.194 _exptl_absorpt_correction_type psiscans #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device CAD4 _diffrn_measurement_method 'omega-2theta scans' _diffrn_standards_decay_% 'less than 5 %' _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_unetI/netI 0.0218 _diffrn_reflns_number 4695 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 24.98 _diffrn_reflns_theta_full 24.98 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 4450 _reflns_number_gt 3605 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection CAD4 _computing_cell_refinement SET4 _computing_data_reduction XTAL3.2 _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1179P)^2^+4.5255P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 4450 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_obs 0.0542 _refine_ls_wR_factor_all 0.1797 _refine_ls_wR_factor_obs 0.1667 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.149 _refine_diff_density_min -0.972 _refine_diff_density_rms 0.11 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Co Co 0.3494 0.9721 '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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.19526(5) 0.65725(3) 0.16838(4) 0.0227(2) Uani 1 1 d . . . S2 S 0.21106(11) 0.64898(6) 0.33837(8) 0.0322(3) Uani 1 1 d . . . S1 S 0.27051(10) 0.54411(5) 0.16367(8) 0.0308(3) Uani 1 1 d . . . N4 N 0.1295(3) 0.75725(18) 0.1672(3) 0.0297(7) Uani 1 1 d . . . H4A H 0.1855 0.7798 0.2256 0.036 Uiso 1 1 calc R . . H4B H 0.1352 0.7802 0.1109 0.036 Uiso 1 1 calc R . . N2 N 0.3768(3) 0.69785(18) 0.2142(3) 0.0290(7) Uani 1 1 d . . . H2A H 0.3685 0.745 0.1966 0.035 Uiso 1 1 calc R . . H2B H 0.4127 0.6957 0.2855 0.035 Uiso 1 1 calc R . . N3 N 0.0109(3) 0.61935(18) 0.1155(3) 0.0281(7) Uani 1 1 d . . . H3A H -0.0279 0.6322 0.0469 0.034 Uiso 1 1 calc R . . H3B H 0.0164 0.5708 0.1171 0.034 Uiso 1 1 calc R . . N1 N 0.1743(3) 0.66658(18) 0.0180(3) 0.0272(7) Uani 1 1 d . . . H1A H 0.1283 0.6278 -0.017 0.033 Uiso 1 1 calc R . . H1B H 0.1234 0.7057 -0.0088 0.033 Uiso 1 1 calc R . . C1 C 0.5163(5) 0.6214(4) 0.0165(5) 0.0567(14) Uani 1 1 d . . . H1C H 0.5485 0.6686 0.0092 0.085 Uiso 1 1 calc R . . H1D H 0.4768 0.5992 -0.052 0.085 Uiso 1 1 calc R . . H1E H 0.589 0.5922 0.0612 0.085 Uiso 1 1 calc R . . C14 C -0.1672(6) 0.7387(4) 0.2493(5) 0.0639(16) Uani 1 1 d . . . H14A H -0.1914 0.7036 0.2907 0.096 Uiso 1 1 calc R . . H14B H -0.2401 0.7455 0.1827 0.096 Uiso 1 1 calc R . . H14C H -0.1464 0.7838 0.2869 0.096 Uiso 1 1 calc R . . C4 C 0.4750(4) 0.6662(3) 0.1746(4) 0.0378(10) Uani 1 1 d . . . H4C H 0.5298 0.6316 0.2262 0.045 Uiso 1 1 calc R . . H4D H 0.5327 0.7045 0.1684 0.045 Uiso 1 1 calc R . . C5 C 0.3638(5) 0.5521(3) 0.0777(4) 0.0405(11) Uani 1 1 d . . . H5A H 0.4408 0.5206 0.1048 0.049 Uiso 1 1 calc R . . H5B H 0.3084 0.5347 0.0076 0.049 Uiso 1 1 calc R . . C3 C 0.2951(4) 0.6730(3) -0.0074(3) 0.0361(10) Uani 1 1 d . . . H3C H 0.3216 0.7234 -0.0026 0.043 Uiso 1 1 calc R . . H3D H 0.2742 0.6573 -0.0798 0.043 Uiso 1 1 calc R . . C7 C 0.3452(6) 0.4703(3) 0.3554(4) 0.0495(13) Uani 1 1 d . . . H7A H 0.2739 0.4402 0.3087 0.059 Uiso 1 1 calc R . . H7B H 0.415 0.4383 0.3996 0.059 Uiso 1 1 calc R . . C8 C 0.2927(6) 0.5130(3) 0.4264(4) 0.0541(14) Uani 1 1 d . . . H8A H 0.2729 0.4793 0.473 0.065 Uiso 1 1 calc R . . H8B H 0.3627 0.5448 0.4706 0.065 Uiso 1 1 calc R . . C6 C 0.4001(5) 0.5155(3) 0.2877(4) 0.0444(11) Uani 1 1 d . . . H6A H 0.4659 0.4873 0.2722 0.053 Uiso 1 1 calc R . . H6B H 0.4442 0.5579 0.3275 0.053 Uiso 1 1 calc R . . C9 C 0.1696(5) 0.5581(3) 0.3698(4) 0.0481(12) Uani 1 1 d . . . H9A H 0.1183 0.562 0.4143 0.058 Uiso 1 1 calc R . . H9B H 0.1149 0.5339 0.3047 0.058 Uiso 1 1 calc R . . C2 C 0.4111(4) 0.6282(2) 0.0668(4) 0.0357(10) Uani 1 1 d . . . C10 C 0.0690(5) 0.7013(3) 0.3379(4) 0.0414(11) Uani 1 1 d . . . H10A H 0.0331 0.6779 0.3849 0.05 Uiso 1 1 calc R . . H10B H 0.1003 0.7488 0.3671 0.05 Uiso 1 1 calc R . . C11 C -0.0825(4) 0.6400(3) 0.1679(4) 0.0409(11) Uani 1 1 d . . . H11A H -0.0835 0.6018 0.2164 0.049 Uiso 1 1 calc R . . H11B H -0.1716 0.6442 0.1143 0.049 Uiso 1 1 calc R . . C12 C -0.0072(4) 0.7674(3) 0.1635(4) 0.0409(11) Uani 1 1 d . . . H12A H -0.0694 0.7643 0.0904 0.049 Uiso 1 1 calc R . . H12B H -0.0148 0.8153 0.1895 0.049 Uiso 1 1 calc R . . C13 C -0.0447(4) 0.7115(3) 0.2291(4) 0.0391(10) Uani 1 1 d . . . Cl1 Cl 0.31559(15) 0.83997(7) 0.38082(10) 0.0567(4) Uani 1 1 d . . . Cl2 Cl 0.59878(13) 0.66901(6) 0.44720(9) 0.0448(3) Uani 1 1 d . . . Cl3 Cl 0.22198(15) 0.53768(10) 0.69930(13) 0.0651(4) Uani 1 1 d . . . O1 O 0.1397(11) 0.5786(7) 0.7347(9) 0.214(5) Uani 1 1 d . . . O3 O 0.1516(17) 0.4907(11) 0.6299(10) 0.326(12) Uani 1 1 d . . . O4 O 0.2948(10) 0.5782(4) 0.6595(9) 0.180(4) Uani 1 1 d . . . O2 O 0.2995(12) 0.5040(9) 0.7883(10) 0.260(7) Uani 1 1 d . . . O5 O 0.0249(4) 0.54392(19) 0.8792(3) 0.0520(9) Uani 1 1 d . . . O6 O 0.4027(7) 0.8383(3) 0.1130(8) 0.156(4) Uani 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 0.0221(3) 0.0219(3) 0.0239(3) -0.00129(19) 0.0085(2) -0.00148(19) S2 0.0340(6) 0.0362(6) 0.0269(5) -0.0014(4) 0.0122(4) -0.0058(4) S1 0.0312(5) 0.0232(5) 0.0354(6) 0.0007(4) 0.0097(4) 0.0005(4) N4 0.0339(19) 0.0255(17) 0.0313(17) -0.0023(14) 0.0141(15) 0.0012(14) N2 0.0251(17) 0.0298(18) 0.0312(18) -0.0029(14) 0.0096(14) -0.0043(14) N3 0.0233(17) 0.0292(17) 0.0296(17) -0.0041(14) 0.0077(14) -0.0045(13) N1 0.0294(18) 0.0271(17) 0.0250(17) 0.0000(13) 0.0103(14) 0.0012(13) C1 0.044(3) 0.075(4) 0.063(3) -0.006(3) 0.034(3) 0.005(3) C14 0.043(3) 0.083(4) 0.077(4) -0.019(3) 0.036(3) 0.004(3) C4 0.028(2) 0.043(3) 0.046(3) -0.002(2) 0.017(2) -0.0011(18) C5 0.042(3) 0.040(3) 0.044(3) -0.005(2) 0.021(2) 0.007(2) C3 0.039(2) 0.042(2) 0.034(2) -0.0009(19) 0.022(2) -0.0018(19) C7 0.062(3) 0.032(2) 0.042(3) 0.013(2) 0.005(2) -0.001(2) C8 0.074(4) 0.046(3) 0.038(3) 0.012(2) 0.016(3) -0.004(3) C6 0.041(3) 0.037(2) 0.047(3) 0.011(2) 0.007(2) 0.004(2) C9 0.061(3) 0.046(3) 0.045(3) 0.007(2) 0.028(2) -0.011(2) C2 0.035(2) 0.038(2) 0.041(2) -0.002(2) 0.0222(19) 0.0017(19) C10 0.044(3) 0.049(3) 0.040(2) -0.011(2) 0.027(2) -0.005(2) C11 0.030(2) 0.050(3) 0.047(3) -0.010(2) 0.021(2) -0.006(2) C12 0.033(2) 0.042(3) 0.047(3) -0.006(2) 0.015(2) 0.0106(19) C13 0.028(2) 0.049(3) 0.044(3) -0.009(2) 0.0181(19) 0.0001(19) Cl1 0.0628(9) 0.0510(8) 0.0398(7) -0.0025(5) 0.0011(6) -0.0209(6) Cl2 0.0562(7) 0.0323(6) 0.0368(6) -0.0033(4) 0.0074(5) 0.0007(5) Cl3 0.0518(8) 0.0854(11) 0.0660(9) -0.0046(8) 0.0314(7) -0.0021(7) O1 0.227(10) 0.250(12) 0.265(12) 0.066(9) 0.208(10) 0.098(9) O3 0.350(18) 0.50(3) 0.201(11) -0.200(14) 0.183(13) -0.311(19) O4 0.247(10) 0.104(5) 0.296(12) -0.028(6) 0.224(10) -0.044(6) O2 0.189(11) 0.355(18) 0.197(11) 0.147(12) 0.029(9) 0.112(11) O5 0.051(2) 0.0416(19) 0.065(2) -0.0120(17) 0.0233(18) -0.0101(16) O6 0.102(5) 0.068(4) 0.231(9) 0.037(4) -0.011(5) -0.019(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 1.978(3) . ? Co1 N4 1.980(3) . ? Co1 N1 1.982(3) . ? Co1 N3 1.983(3) . ? Co1 S1 2.2552(11) . ? Co1 S2 2.2636(12) . ? S2 C10 1.821(5) . ? S2 C9 1.832(5) . ? S1 C6 1.822(5) . ? S1 C5 1.825(5) . ? N4 C12 1.480(5) . ? N2 C4 1.488(5) . ? N3 C11 1.496(5) . ? N1 C3 1.486(5) . ? C1 C2 1.546(6) . ? C14 C13 1.543(6) . ? C4 C2 1.536(7) . ? C5 C2 1.523(7) . ? C3 C2 1.528(6) . ? C7 C8 1.518(8) . ? C7 C6 1.525(7) . ? C8 C9 1.516(8) . ? C10 C13 1.540(7) . ? C11 C13 1.534(7) . ? C12 C13 1.520(7) . ? Cl3 O3 1.299(10) . ? Cl3 O2 1.339(9) . ? Cl3 O4 1.344(7) . ? Cl3 O1 1.390(8) . ? 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 N2 Co1 N4 87.83(14) . . ? N2 Co1 N1 90.19(14) . . ? N4 Co1 N1 90.63(14) . . ? N2 Co1 N3 177.06(14) . . ? N4 Co1 N3 90.84(14) . . ? N1 Co1 N3 87.20(14) . . ? N2 Co1 S1 91.82(10) . . ? N4 Co1 S1 177.84(11) . . ? N1 Co1 S1 87.24(10) . . ? N3 Co1 S1 89.42(10) . . ? N2 Co1 S2 91.33(10) . . ? N4 Co1 S2 87.59(10) . . ? N1 Co1 S2 177.62(10) . . ? N3 Co1 S2 91.24(10) . . ? S1 Co1 S2 94.55(4) . . ? C10 S2 C9 101.8(2) . . ? C10 S2 Co1 103.06(16) . . ? C9 S2 Co1 111.82(17) . . ? C6 S1 C5 101.4(2) . . ? C6 S1 Co1 113.84(17) . . ? C5 S1 Co1 103.85(15) . . ? C12 N4 Co1 118.2(3) . . ? C4 N2 Co1 120.3(3) . . ? C11 N3 Co1 120.8(3) . . ? C3 N1 Co1 118.9(3) . . ? N2 C4 C2 113.6(4) . . ? C2 C5 S1 115.3(3) . . ? N1 C3 C2 112.5(3) . . ? C8 C7 C6 115.5(4) . . ? C9 C8 C7 115.7(4) . . ? C7 C6 S1 112.2(4) . . ? C8 C9 S2 112.1(4) . . ? C5 C2 C3 110.0(4) . . ? C5 C2 C4 112.1(4) . . ? C3 C2 C4 110.2(4) . . ? C5 C2 C1 107.6(4) . . ? C3 C2 C1 108.3(4) . . ? C4 C2 C1 108.6(4) . . ? C13 C10 S2 116.0(3) . . ? N3 C11 C13 112.9(3) . . ? N4 C12 C13 112.6(4) . . ? C12 C13 C11 110.0(4) . . ? C12 C13 C10 110.7(4) . . ? C11 C13 C10 111.8(4) . . ? C12 C13 C14 109.0(4) . . ? C11 C13 C14 107.8(4) . . ? C10 C13 C14 107.4(4) . . ? O3 Cl3 O2 110.1(13) . . ? O3 Cl3 O4 110.7(7) . . ? O2 Cl3 O4 111.1(8) . . ? O3 Cl3 O1 109.8(10) . . ? O2 Cl3 O1 101.8(8) . . ? O4 Cl3 O1 113.1(6) . . ? 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 N2 Co1 S2 C10 123.50(19) . . . . ? N4 Co1 S2 C10 35.73(19) . . . . ? N1 Co1 S2 C10 -6(3) . . . . ? N3 Co1 S2 C10 -55.06(19) . . . . ? S1 Co1 S2 C10 -144.57(17) . . . . ? N2 Co1 S2 C9 -127.9(2) . . . . ? N4 Co1 S2 C9 144.3(2) . . . . ? N1 Co1 S2 C9 103(3) . . . . ? N3 Co1 S2 C9 53.6(2) . . . . ? S1 Co1 S2 C9 -36.0(2) . . . . ? N2 Co1 S1 C6 55.1(2) . . . . ? N4 Co1 S1 C6 136(3) . . . . ? N1 Co1 S1 C6 145.2(2) . . . . ? N3 Co1 S1 C6 -127.6(2) . . . . ? S2 Co1 S1 C6 -36.42(18) . . . . ? N2 Co1 S1 C5 -54.27(19) . . . . ? N4 Co1 S1 C5 26(3) . . . . ? N1 Co1 S1 C5 35.83(19) . . . . ? N3 Co1 S1 C5 123.05(19) . . . . ? S2 Co1 S1 C5 -145.75(17) . . . . ? N2 Co1 N4 C12 -164.8(3) . . . . ? N1 Co1 N4 C12 105.0(3) . . . . ? N3 Co1 N4 C12 17.8(3) . . . . ? S1 Co1 N4 C12 115(3) . . . . ? S2 Co1 N4 C12 -73.4(3) . . . . ? N4 Co1 N2 C4 -143.1(3) . . . . ? N1 Co1 N2 C4 -52.4(3) . . . . ? N3 Co1 N2 C4 -80(3) . . . . ? S1 Co1 N2 C4 34.8(3) . . . . ? S2 Co1 N2 C4 129.4(3) . . . . ? N2 Co1 N3 C11 -113(3) . . . . ? N4 Co1 N3 C11 -50.2(3) . . . . ? N1 Co1 N3 C11 -140.8(3) . . . . ? S1 Co1 N3 C11 132.0(3) . . . . ? S2 Co1 N3 C11 37.4(3) . . . . ? N2 Co1 N1 C3 19.9(3) . . . . ? N4 Co1 N1 C3 107.7(3) . . . . ? N3 Co1 N1 C3 -161.5(3) . . . . ? S1 Co1 N1 C3 -71.9(3) . . . . ? S2 Co1 N1 C3 149(2) . . . . ? Co1 N2 C4 C2 25.8(5) . . . . ? C6 S1 C5 C2 -96.7(4) . . . . ? Co1 S1 C5 C2 21.6(4) . . . . ? Co1 N1 C3 C2 35.3(5) . . . . ? C6 C7 C8 C9 66.5(6) . . . . ? C8 C7 C6 S1 -85.4(5) . . . . ? C5 S1 C6 C7 -151.8(4) . . . . ? Co1 S1 C6 C7 97.3(4) . . . . ? C7 C8 C9 S2 -88.5(5) . . . . ? C10 S2 C9 C8 -152.0(4) . . . . ? Co1 S2 C9 C8 98.6(4) . . . . ? S1 C5 C2 C3 -76.6(4) . . . . ? S1 C5 C2 C4 46.3(5) . . . . ? S1 C5 C2 C1 165.7(4) . . . . ? N1 C3 C2 C5 47.4(5) . . . . ? N1 C3 C2 C4 -76.7(5) . . . . ? N1 C3 C2 C1 164.7(4) . . . . ? N2 C4 C2 C5 -80.6(5) . . . . ? N2 C4 C2 C3 42.2(5) . . . . ? N2 C4 C2 C1 160.7(4) . . . . ? C9 S2 C10 C13 -94.5(4) . . . . ? Co1 S2 C10 C13 21.5(4) . . . . ? Co1 N3 C11 C13 23.3(5) . . . . ? Co1 N4 C12 C13 37.6(5) . . . . ? N4 C12 C13 C11 -79.2(5) . . . . ? N4 C12 C13 C10 44.8(5) . . . . ? N4 C12 C13 C14 162.8(4) . . . . ? N3 C11 C13 C12 43.9(5) . . . . ? N3 C11 C13 C10 -79.4(5) . . . . ? N3 C11 C13 C14 162.7(4) . . . . ? S2 C10 C13 C12 -75.7(5) . . . . ? S2 C10 C13 C11 47.3(5) . . . . ? S2 C10 C13 C14 165.4(4) . . . . ?