Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Cobalt(II) and cobalt(III) complexes of thioether-containing hexadentate pyrazine amide ligands: C-S bond cleavage and cyclometallation reaction ; _publ_contact_author_name 'Prof. R.Mukherjee' _publ_contact_author_email RNM@IITK.AC.IN loop_ _publ_author_name A.K.Singh R.Mukherjee # Attachment 'co-cif.cif' data_co _database_code_depnum_ccdc_archive 'CCDC 652240' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H17 Co N6 O2 S2, C2 H8 O2' _chemical_formula_sum 'C26 H25 Co N6 O4 S2' _chemical_formula_weight 608.57 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pccn #(#56) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y, -z+1/2' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' '-x-1/2, y, z-1/2' 'x, -y-1/2, z-1/2' _cell_length_a 19.135(5) _cell_length_b 10.103(5) _cell_length_c 13.099(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2532.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.596 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_absorpt_coefficient_mu 0.890 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7760 _exptl_absorpt_correction_T_max 0.8420 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15892 _diffrn_reflns_av_R_equivalents 0.0518 _diffrn_reflns_av_sigmaI/netI 0.0435 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3136 _reflns_number_gt 2605 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0349P)^2^+9.8426P] 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_extinction_coef ? _refine_ls_number_reflns 3136 _refine_ls_number_parameters 221 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.1044 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.1856 _refine_ls_wR_factor_gt 0.1803 _refine_ls_goodness_of_fit_ref 1.269 _refine_ls_restrained_S_all 1.271 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Co Co 0.25950(14) 0.7688(2) 0.44197(7) 0.0177(4) Uani 0.50 1 d P . . S1A S 0.27993(14) 0.8526(3) 0.31327(19) 0.0199(5) Uani 0.50 1 d P . 1 S1B S 0.30428(14) 0.8989(3) 0.32194(18) 0.0195(5) Uani 0.50 1 d P . 2 O1 O 0.3889(2) 0.4661(3) 0.5092(3) 0.0486(10) Uani 1 1 d . . . O2 O 0.4069(4) 1.2024(8) 0.4802(6) 0.0489(19) Uani 0.50 1 d P A 1 H2A H 0.4465 1.2121 0.4535 0.073 Uiso 0.50 1 calc PR A 1 O3 O 0.5058(15) 1.059(3) 0.508(2) 0.127(10) Uani 0.50 1 d PDU C -1 H3A H 0.5153 1.0804 0.5681 0.191 Uiso 0.50 1 calc PR C -1 N1 N 0.2243(2) 0.6203(4) 0.5441(3) 0.0372(10) Uani 1 1 d . . . N2 N 0.2013(3) 0.4039(4) 0.6679(4) 0.0476(12) Uani 1 1 d . . . N3 N 0.3375(3) 0.6554(4) 0.4418(3) 0.0444(12) Uani 1 1 d . . . C1 C 0.1643(3) 0.6083(5) 0.5936(4) 0.0417(13) Uani 1 1 d . . . H1 H 0.1292 0.6741 0.5871 0.050 Uiso 1 1 calc R . . C2 C 0.1534(3) 0.4976(5) 0.6554(4) 0.0460(14) Uani 1 1 d . . . H2 H 0.1099 0.4890 0.6899 0.055 Uiso 1 1 calc R . . C3 C 0.2617(3) 0.4209(5) 0.6196(4) 0.0438(14) Uani 1 1 d . . . H3 H 0.2975 0.3567 0.6284 0.053 Uiso 1 1 calc R . . C4 C 0.2745(3) 0.5281(4) 0.5571(4) 0.0380(12) Uani 1 1 d . . . C5 C 0.3406(3) 0.5459(5) 0.4998(4) 0.0385(12) Uani 1 1 d . . . C6 C 0.3915(3) 0.6962(5) 0.3744(4) 0.0406(13) Uani 1 1 d . . . C7 C 0.4596(3) 0.6417(5) 0.3700(4) 0.0435(14) Uani 1 1 d . . . H7 H 0.4726 0.5724 0.4151 0.052 Uiso 1 1 calc R . . C8 C 0.5068(3) 0.6897(6) 0.3000(4) 0.0483(15) Uani 1 1 d . . . H8 H 0.5524 0.6528 0.2978 0.058 Uiso 1 1 calc R . . C9 C 0.4896(3) 0.7897(5) 0.2331(4) 0.0456(14) Uani 1 1 d . . . H9 H 0.5227 0.8199 0.1844 0.055 Uiso 1 1 calc R . . C10 C 0.4236(3) 0.8458(5) 0.2377(4) 0.0435(13) Uani 1 1 d . . . H10 H 0.4114 0.9157 0.1926 0.052 Uiso 1 1 calc R . . C11 C 0.3752(3) 0.7996(5) 0.3085(4) 0.0449(15) Uani 1 1 d . . . C12 C 0.3385(6) 1.0482(8) 0.3770(6) 0.030(2) Uani 0.50 1 d P B 2 H12 H 0.3805 1.0417 0.4154 0.036 Uiso 0.50 1 calc PR B 2 C13 C 0.3104(7) 1.1630(10) 0.3683(9) 0.043(3) Uani 0.50 1 d P B 2 H13A H 0.2684 1.1733 0.3304 0.051 Uiso 0.50 1 calc PR B 2 H13B H 0.3316 1.2377 0.3996 0.051 Uiso 0.50 1 calc PR B 2 C14 C 0.3580(7) 1.1705(14) 0.4042(10) 0.058(3) Uani 0.50 1 d P A 1 H14A H 0.3130 1.1500 0.4360 0.087 Uiso 0.50 1 calc PR A 1 H14B H 0.3745 1.0933 0.3657 0.087 Uiso 0.50 1 calc PR A 1 H14C H 0.3525 1.2458 0.3577 0.087 Uiso 0.50 1 calc PR A 1 C15 C 0.4776(16) 0.937(2) 0.507(3) 0.075(8) Uani 0.50 1 d PDU C -1 H15A H 0.5099 0.8751 0.4735 0.112 Uiso 0.50 1 calc PR C -1 H15B H 0.4334 0.9386 0.4690 0.112 Uiso 0.50 1 calc PR C -1 H15C H 0.4689 0.9076 0.5770 0.112 Uiso 0.50 1 calc PR C -1 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 Co 0.0303(14) 0.0087(12) 0.0140(4) 0.0012(4) 0.0016(5) 0.0058(7) S1A 0.0240(14) 0.0184(13) 0.0173(10) 0.0017(9) -0.0009(9) 0.0057(9) S1B 0.0262(14) 0.0168(13) 0.0156(10) 0.0046(9) 0.0024(9) 0.0044(9) O1 0.051(2) 0.0267(18) 0.068(3) -0.0059(18) -0.027(2) 0.0184(16) O2 0.053(5) 0.043(4) 0.051(5) -0.003(4) -0.003(4) -0.002(4) O3 0.115(14) 0.137(16) 0.130(17) -0.043(12) -0.004(11) -0.092(11) N1 0.058(3) 0.028(2) 0.0255(19) -0.0164(16) -0.0158(19) 0.0191(19) N2 0.062(3) 0.023(2) 0.058(3) -0.011(2) -0.029(2) 0.003(2) N3 0.071(3) 0.043(2) 0.0187(18) -0.0040(18) -0.009(2) 0.039(2) C1 0.058(3) 0.026(2) 0.041(3) -0.017(2) -0.016(3) 0.017(2) C2 0.053(3) 0.036(3) 0.049(3) -0.020(2) -0.015(3) 0.003(2) C3 0.050(3) 0.027(2) 0.054(3) -0.016(2) -0.027(3) 0.008(2) C4 0.057(3) 0.022(2) 0.035(2) -0.013(2) -0.024(2) 0.014(2) C5 0.056(3) 0.030(2) 0.029(2) -0.013(2) -0.020(2) 0.023(2) C6 0.061(3) 0.038(3) 0.023(2) -0.009(2) -0.010(2) 0.029(2) C7 0.061(4) 0.034(3) 0.036(3) -0.013(2) -0.014(3) 0.028(3) C8 0.051(3) 0.047(3) 0.048(3) -0.013(3) -0.008(3) 0.027(3) C9 0.060(4) 0.039(3) 0.038(3) -0.011(2) -0.010(3) 0.017(3) C10 0.065(4) 0.039(3) 0.027(2) -0.010(2) -0.012(2) 0.021(3) C11 0.076(4) 0.040(3) 0.019(2) -0.011(2) -0.009(2) 0.036(3) C12 0.052(6) 0.018(4) 0.020(4) -0.001(3) 0.013(4) 0.005(4) C13 0.059(7) 0.024(5) 0.045(6) 0.003(4) 0.003(6) 0.006(5) C14 0.054(8) 0.072(9) 0.049(7) 0.003(6) -0.004(6) -0.028(7) C15 0.079(16) 0.045(10) 0.100(16) 0.038(10) -0.024(12) -0.014(10) _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 Co Co 0.525(2) 2_565 ? Co N1 1.773(5) 2_565 ? Co N3 1.882(5) . ? Co S1A 1.927(3) . ? Co N3 2.008(5) 2_565 ? Co N1 2.120(5) . ? Co S1A 2.217(3) 2_565 ? Co S1B 2.221(3) . ? Co S1B 2.614(3) 2_565 ? S1A C11 1.901(6) . ? S1A Co 2.217(3) 2_565 ? S1A S1A 2.369(6) 2_565 ? O2 C14 1.403(14) . ? O1 C5 1.232(5) . ? N1 C1 1.323(7) . ? N1 C4 1.349(6) . ? N1 Co 1.773(5) 2_565 ? N2 C2 1.328(7) . ? N2 C3 1.329(8) . ? N3 C5 1.343(6) . ? N3 C6 1.421(7) . ? N3 Co 2.008(5) 2_565 ? C1 C2 1.396(8) . ? C3 C4 1.380(8) . ? C4 C5 1.483(8) . ? C6 C11 1.390(7) . ? C6 C7 1.415(7) . ? C7 C8 1.374(8) . ? C8 C9 1.377(8) . ? C9 C10 1.386(7) . ? C10 C11 1.391(8) . ? C11 S1B 1.697(5) . ? S1B C12 1.795(10) . ? S1B Co 2.614(3) 2_565 ? C12 C13 1.284(13) . ? O3 C15 1.347(13) . ? 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 Co Co N1 125.3(3) 2_565 2_565 ? Co Co N3 96.3(7) 2_565 . ? N1 Co N3 104.3(2) 2_565 . ? Co Co S1A 117.24(17) 2_565 . ? N1 Co S1A 110.28(17) 2_565 . ? N3 Co S1A 96.07(19) . . ? Co Co N3 68.6(7) 2_565 2_565 ? N1 Co N3 85.5(2) 2_565 2_565 ? N3 Co N3 164.93(8) . 2_565 ? S1A Co N3 91.08(18) . 2_565 ? Co Co N1 43.0(3) 2_565 . ? N1 Co N1 91.5(2) 2_565 . ? N3 Co N1 79.8(2) . . ? S1A Co N1 158.09(14) . . ? N3 Co N1 88.65(19) 2_565 . ? Co Co S1A 50.60(13) 2_565 2_565 ? N1 Co S1A 169.5(2) 2_565 2_565 ? N3 Co S1A 86.13(17) . 2_565 ? S1A Co S1A 69.33(16) . 2_565 ? N3 Co S1A 84.01(16) 2_565 2_565 ? N1 Co S1A 88.86(13) . 2_565 ? Co Co S1B 133.96(16) 2_565 . ? N1 Co S1B 95.30(15) 2_565 . ? N3 Co S1B 93.06(18) . . ? S1A Co S1B 16.71(8) . . ? N3 Co S1B 97.48(17) 2_565 . ? N1 Co S1B 171.14(18) . . ? S1A Co S1B 85.44(13) 2_565 . ? Co Co S1B 37.72(13) 2_565 2_565 ? N1 Co S1B 161.0(2) 2_565 2_565 ? N3 Co S1B 88.60(17) . 2_565 ? S1A Co S1B 81.57(13) . 2_565 ? N3 Co S1B 79.33(16) 2_565 2_565 ? N1 Co S1B 76.85(12) . 2_565 ? S1A Co S1B 12.87(8) 2_565 2_565 ? S1B Co S1B 97.93(14) . 2_565 ? C11 S1A Co 95.7(2) . . ? C11 S1A Co 101.3(2) . 2_565 ? Co S1A Co 12.16(7) . 2_565 ? C11 S1A S1A 102.5(2) . 2_565 ? Co S1A S1A 61.12(9) . 2_565 ? Co S1A S1A 49.55(8) 2_565 2_565 ? C1 N1 C4 119.5(5) . . ? C1 N1 Co 125.4(4) . 2_565 ? C4 N1 Co 114.0(4) . 2_565 ? C1 N1 Co 130.5(3) . . ? C4 N1 Co 110.0(4) . . ? Co N1 Co 11.67(9) 2_565 . ? C2 N2 C3 116.7(5) . . ? C5 N3 C6 123.9(4) . . ? C5 N3 Co 122.4(4) . . ? C6 N3 Co 113.7(3) . . ? C5 N3 Co 110.8(4) . 2_565 ? C6 N3 Co 124.2(3) . 2_565 ? Co N3 Co 15.07(8) . 2_565 ? N1 C1 C2 119.2(5) . . ? N2 C2 C1 122.6(6) . . ? N2 C3 C4 122.5(5) . . ? N1 C4 C3 119.4(5) . . ? N1 C4 C5 117.4(5) . . ? C3 C4 C5 123.1(5) . . ? O1 C5 N3 129.0(6) . . ? O1 C5 C4 120.7(5) . . ? N3 C5 C4 110.4(4) . . ? C11 C6 C7 118.3(5) . . ? C11 C6 N3 116.1(5) . . ? C7 C6 N3 125.6(5) . . ? C8 C7 C6 119.6(5) . . ? C7 C8 C9 121.8(5) . . ? C8 C9 C10 119.3(6) . . ? C9 C10 C11 119.9(5) . . ? C6 C11 C10 121.1(5) . . ? C6 C11 S1B 124.0(5) . . ? C10 C11 S1B 113.8(4) . . ? C6 C11 S1A 114.0(5) . . ? C10 C11 S1A 124.4(4) . . ? S1B C11 S1A 20.45(11) . . ? C11 S1B C12 104.3(4) . . ? C11 S1B Co 91.8(2) . . ? C12 S1B Co 110.7(3) . . ? C11 S1B Co 93.0(2) . 2_565 ? C12 S1B Co 118.2(3) . 2_565 ? Co S1B Co 8.32(5) . 2_565 ? C13 C12 S1B 124.8(10) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.646 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.094 #===END #===END data_3octb _database_code_depnum_ccdc_archive 'CCDC 652241' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H26 Co N6 O2 S2' _chemical_formula_sum 'C31 H26 Co N6 O2 S2' _chemical_formula_weight 637.63 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c #15) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 21.722(5) _cell_length_b 12.058(5) _cell_length_c 10.524(5) _cell_angle_alpha 90.0 _cell_angle_beta 104.864(5) _cell_angle_gamma 90.0 _cell_volume 2664.2(18) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Dark-brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1316 _exptl_absorpt_coefficient_mu 0.845 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.7856 _exptl_absorpt_correction_T_max 0.9202 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8566 _diffrn_reflns_av_R_equivalents 0.0636 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 28.35 _reflns_number_total 3266 _reflns_number_gt 2579 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0532P)^2^+16.8213P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3266 _refine_ls_number_parameters 211 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0805 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1595 _refine_ls_wR_factor_gt 0.1247 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.088 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 0.0000 0.23267(6) 0.2500 0.01396(19) Uani 1 2 d S . . S1 S -0.07083(5) 0.10127(8) 0.30040(9) 0.0225(2) Uani 1 1 d . . . O1 O -0.06197(12) 0.2998(2) -0.1391(2) 0.0204(6) Uani 1 1 d . . . N1 N 0.04806(14) 0.3470(3) 0.1693(3) 0.0176(6) Uani 1 1 d . . . N2 N 0.10814(15) 0.4713(3) 0.0124(3) 0.0216(7) Uani 1 1 d . . . N3 N -0.05710(14) 0.2366(3) 0.0744(3) 0.0160(6) Uani 1 1 d . . . C1 C 0.09987(17) 0.4062(3) 0.2227(4) 0.0188(7) Uani 1 1 d . . . H1 H 0.1170 0.4052 0.3153 0.023 Uiso 1 1 calc R . . C2 C 0.12945(18) 0.4700(3) 0.1439(4) 0.0209(8) Uani 1 1 d . . . H2 H 0.1656 0.5135 0.1847 0.025 Uiso 1 1 calc R . . C3 C 0.05628(18) 0.4110(3) -0.0397(3) 0.0180(7) Uani 1 1 d . . . H3 H 0.0403 0.4090 -0.1326 0.022 Uiso 1 1 calc R . . C4 C 0.02472(16) 0.3508(3) 0.0377(3) 0.0155(7) Uani 1 1 d . . . C5 C -0.03667(17) 0.2913(3) -0.0182(3) 0.0161(7) Uani 1 1 d . . . C6 C -0.11662(17) 0.1830(3) 0.0491(3) 0.0160(7) Uani 1 1 d . . . C7 C -0.16584(17) 0.1953(3) -0.0673(4) 0.0211(8) Uani 1 1 d . . . H7 H -0.1597 0.2425 -0.1353 0.025 Uiso 1 1 calc R . . C8 C -0.22278(19) 0.1393(4) -0.0832(4) 0.0260(9) Uani 1 1 d . . . H8 H -0.2553 0.1492 -0.1622 0.031 Uiso 1 1 calc R . . C9 C -0.23387(19) 0.0688(4) 0.0134(4) 0.0282(9) Uani 1 1 d . . . H9 H -0.2729 0.0293 -0.0002 0.034 Uiso 1 1 calc R . . C10 C -0.18686(19) 0.0575(3) 0.1298(4) 0.0250(8) Uani 1 1 d . . . H10 H -0.1939 0.0106 0.1973 0.030 Uiso 1 1 calc R . . C11 C -0.12939(18) 0.1144(3) 0.1486(4) 0.0201(8) Uani 1 1 d . . . C12 C -0.0482(2) -0.0444(4) 0.2981(5) 0.0339(11) Uani 1 1 d D . . H12B H -0.083(3) -0.085(5) 0.299(6) 0.06(2) Uiso 1 1 d . . . H12A H -0.031(5) -0.060(9) 0.383(3) 0.15(4) Uiso 1 1 d D . . C13 C -0.0195(4) -0.0747(6) 0.1954(8) 0.0240(16) Uani 0.50 1 d PD . . H13A H -0.044(4) -0.050(7) 0.118(4) 0.02(2) Uiso 0.50 1 d PD . . H13B H -0.025(4) -0.1479(18) 0.180(9) 0.04(3) Uiso 0.50 1 d PD . . C14 C 0.8071(2) 0.2208(4) 0.4712(4) 0.0285(9) Uani 1 1 d . . . H14 H 0.8459 0.2009 0.4512 0.034 Uiso 1 1 calc R . . C15 C 0.8076(2) 0.2684(4) 0.5919(4) 0.0309(10) Uani 1 1 d . . . H15 H 0.8469 0.2811 0.6550 0.037 Uiso 1 1 calc R . . C16 C 0.7510(2) 0.2973(4) 0.6200(4) 0.0285(9) Uani 1 1 d . . . H16 H 0.7517 0.3299 0.7025 0.034 Uiso 1 1 calc R . . 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 0.0172(3) 0.0135(3) 0.0123(3) 0.000 0.0060(3) 0.000 S1 0.0255(5) 0.0256(5) 0.0196(4) 0.0039(4) 0.0114(4) 0.0025(4) O1 0.0221(13) 0.0267(15) 0.0140(11) 0.0018(11) 0.0074(10) 0.0002(11) N1 0.0196(15) 0.0181(16) 0.0153(14) 0.0034(12) 0.0047(12) 0.0026(12) N2 0.0247(17) 0.0210(17) 0.0195(15) 0.0019(13) 0.0065(13) -0.0030(13) N3 0.0182(14) 0.0184(15) 0.0136(13) -0.0015(12) 0.0080(11) -0.0020(12) C1 0.0183(17) 0.0171(18) 0.0221(17) -0.0020(15) 0.0073(14) 0.0024(14) C2 0.0192(18) 0.022(2) 0.0210(17) -0.0023(15) 0.0039(15) -0.0001(15) C3 0.0248(18) 0.0157(18) 0.0134(15) -0.0004(14) 0.0048(14) 0.0000(14) C4 0.0178(16) 0.0167(18) 0.0141(15) 0.0009(13) 0.0079(13) 0.0044(14) C5 0.0216(17) 0.0162(18) 0.0115(15) 0.0007(13) 0.0062(13) 0.0031(14) C6 0.0200(17) 0.0137(17) 0.0164(16) -0.0049(14) 0.0084(14) -0.0017(14) C7 0.0212(18) 0.0233(19) 0.0203(17) -0.0059(15) 0.0082(15) 0.0003(15) C8 0.0217(19) 0.032(2) 0.0234(19) -0.0064(17) 0.0041(16) -0.0007(17) C9 0.023(2) 0.027(2) 0.036(2) -0.0119(19) 0.0100(17) -0.0058(17) C10 0.029(2) 0.021(2) 0.030(2) -0.0021(17) 0.0172(17) -0.0059(17) C11 0.0222(18) 0.0157(18) 0.0249(18) -0.0025(15) 0.0107(15) 0.0013(14) C12 0.042(3) 0.027(2) 0.039(3) 0.017(2) 0.023(2) 0.010(2) C13 0.042(5) 0.009(3) 0.022(3) 0.000(3) 0.010(3) 0.002(3) C14 0.031(2) 0.029(2) 0.028(2) 0.0023(18) 0.0122(17) 0.0019(18) C15 0.035(2) 0.036(2) 0.0205(19) 0.0046(18) 0.0043(17) -0.005(2) C16 0.036(2) 0.033(2) 0.0212(19) -0.0012(17) 0.0156(17) -0.0019(19) _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 1.944(3) . ? Co1 N3 1.944(3) 2 ? Co1 N1 2.041(3) 2 ? Co1 N1 2.041(3) . ? Co1 S1 2.3617(12) . ? Co1 S1 2.3617(12) 2 ? S1 C11 1.776(4) . ? S1 C12 1.826(5) . ? O1 C5 1.254(4) . ? N1 C1 1.329(5) . ? N1 C4 1.348(4) . ? N2 C3 1.335(5) . ? N2 C2 1.342(5) . ? N3 C5 1.343(4) . ? N3 C6 1.408(4) . ? C1 C2 1.402(5) . ? C3 C4 1.395(5) . ? C4 C5 1.495(5) . ? C6 C7 1.412(5) . ? C6 C11 1.417(5) . ? C7 C8 1.381(5) . ? C8 C9 1.393(6) . ? C9 C10 1.386(6) . ? C10 C11 1.393(5) . ? C12 C13 1.427(9) . ? C12 C13 1.501(10) 2 ? C13 C13 1.242(16) 2 ? C13 C12 1.501(10) 2 ? C14 C15 1.392(6) . ? C14 C16 1.393(6) 7_656 ? C15 C16 1.380(6) . ? C16 C14 1.393(6) 7_656 ? 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 N3 177.21(19) . 2 ? N3 Co1 N1 96.29(12) . 2 ? N3 Co1 N1 81.81(12) 2 2 ? N3 Co1 N1 81.81(12) . . ? N3 Co1 N1 96.29(12) 2 . ? N1 Co1 N1 95.03(18) 2 . ? N3 Co1 S1 86.35(9) . . ? N3 Co1 S1 95.53(9) 2 . ? N1 Co1 S1 85.84(9) 2 . ? N1 Co1 S1 168.16(9) . . ? N3 Co1 S1 95.53(9) . 2 ? N3 Co1 S1 86.35(9) 2 2 ? N1 Co1 S1 168.16(9) 2 2 ? N1 Co1 S1 85.84(9) . 2 ? S1 Co1 S1 95.73(6) . 2 ? C11 S1 C12 101.9(2) . . ? C11 S1 Co1 95.49(13) . . ? C12 S1 Co1 116.72(16) . . ? C1 N1 C4 118.1(3) . . ? C1 N1 Co1 130.9(3) . . ? C4 N1 Co1 110.6(2) . . ? C3 N2 C2 116.6(3) . . ? C5 N3 C6 123.1(3) . . ? C5 N3 Co1 116.9(2) . . ? C6 N3 Co1 120.0(2) . . ? N1 C1 C2 120.8(3) . . ? N2 C2 C1 121.8(4) . . ? N2 C3 C4 122.2(3) . . ? N1 C4 C3 120.4(3) . . ? N1 C4 C5 116.8(3) . . ? C3 C4 C5 122.8(3) . . ? O1 C5 N3 129.5(3) . . ? O1 C5 C4 118.3(3) . . ? N3 C5 C4 112.2(3) . . ? N3 C6 C7 124.8(3) . . ? N3 C6 C11 118.2(3) . . ? C7 C6 C11 117.0(3) . . ? C8 C7 C6 120.6(4) . . ? C7 C8 C9 121.8(4) . . ? C10 C9 C8 118.6(4) . . ? C9 C10 C11 120.5(4) . . ? C10 C11 C6 121.4(4) . . ? C10 C11 S1 119.5(3) . . ? C6 C11 S1 119.1(3) . . ? C13 C12 C13 50.1(6) . 2 ? C13 C12 S1 115.3(4) . . ? C13 C12 S1 119.8(4) 2 . ? C13 C13 C12 68.0(7) 2 . ? C13 C13 C12 61.9(7) 2 2 ? C12 C13 C12 121.1(6) . 2 ? C15 C14 C16 119.1(4) . 7_656 ? C16 C15 C14 120.0(4) . . ? C15 C16 C14 120.9(4) . 7_656 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.982 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.140 #===END data_16jancm _database_code_depnum_ccdc_archive 'CCDC 652242' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H20 Cl Co N6 O6 S2' _chemical_formula_sum 'C25 H20 Cl Co N6 O6 S2' _chemical_formula_weight 658.97 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' O O 0.0106 0.0060 '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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.363(5) _cell_length_b 10.980(5) _cell_length_c 15.046(5) _cell_angle_alpha 96.003(5) _cell_angle_beta 95.062(5) _cell_angle_gamma 103.491(5) _cell_volume 1327.0(11) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 672 _exptl_absorpt_coefficient_mu 0.959 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7618 _exptl_absorpt_correction_T_max 0.8313 _exptl_absorpt_process_details Empirical _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8907 _diffrn_reflns_av_R_equivalents 0.0487 _diffrn_reflns_av_sigmaI/netI 0.1292 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 28.32 _reflns_number_total 6337 _reflns_number_gt 4081 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0706P)^2^+8.8755P] 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_extinction_coef ? _refine_ls_number_reflns 6337 _refine_ls_number_parameters 358 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2238 _refine_ls_wR_factor_gt 0.1817 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 Co Co 0.01860(11) 0.38546(8) 0.25676(6) 0.0113(2) Uani 1 1 d . . . S1 S 0.0742(2) 0.19946(15) 0.25764(11) 0.0159(4) Uani 1 1 d . . . S2 S -0.2436(2) 0.33040(16) 0.28675(11) 0.0165(4) Uani 1 1 d . . . Cl Cl 0.4125(2) 0.85467(17) 0.25590(12) 0.0270(4) Uani 1 1 d . . . O1 O 0.1758(6) 0.5953(5) 0.4952(3) 0.0221(11) Uani 1 1 d . . . O2 O 0.0298(7) 0.3559(6) -0.0098(3) 0.0392(15) Uani 1 1 d . . . O3 O 0.3717(11) 0.9564(6) 0.2158(4) 0.067(3) Uani 1 1 d . . . O4 O 0.5797(8) 0.8470(7) 0.2430(5) 0.059(2) Uani 1 1 d . . . O5 O 0.4035(7) 0.8775(6) 0.3502(4) 0.0354(14) Uani 1 1 d . . . O6 O 0.3000(7) 0.7402(5) 0.2169(4) 0.0325(14) Uani 1 1 d . . . N1 N -0.0056(7) 0.5578(5) 0.2706(4) 0.0133(11) Uani 1 1 d . . . N2 N -0.0228(8) 0.8044(6) 0.3146(4) 0.0247(14) Uani 1 1 d . . . N3 N 0.1164(7) 0.4278(5) 0.3801(4) 0.0145(12) Uani 1 1 d . . . N4 N -0.0643(7) 0.3478(5) 0.1307(4) 0.0181(13) Uani 1 1 d . . . N5 N 0.2280(6) 0.4425(5) 0.2115(4) 0.0130(11) Uani 1 1 d . . . N6 N 0.5057(8) 0.5303(6) 0.1249(4) 0.0260(14) Uani 1 1 d . . . C1 C -0.0679(9) 0.6184(6) 0.2086(5) 0.0174(14) Uani 1 1 d . . . H1 H -0.1062 0.5772 0.1492 0.021 Uiso 1 1 calc R . . C2 C -0.0757(10) 0.7443(7) 0.2327(6) 0.0284(18) Uani 1 1 d . . . H2 H -0.1202 0.7872 0.1887 0.034 Uiso 1 1 calc R . . C3 C 0.0404(9) 0.7428(6) 0.3743(5) 0.0201(15) Uani 1 1 d . . . H3 H 0.0827 0.7854 0.4329 0.024 Uiso 1 1 calc R . . C4 C 0.0470(9) 0.6179(6) 0.3539(4) 0.0162(14) Uani 1 1 d . . . C5 C 0.1187(9) 0.5452(7) 0.4181(4) 0.0180(10) Uani 1 1 d . . . C6 C 0.1958(9) 0.3452(6) 0.4202(4) 0.0143(13) Uani 1 1 d . . . C7 C 0.2841(9) 0.3658(7) 0.5063(5) 0.0203(15) Uani 1 1 d . . . H7 H 0.2931 0.4424 0.5444 0.024 Uiso 1 1 calc R . . C8 C 0.3584(9) 0.2741(7) 0.5358(5) 0.0250(17) Uani 1 1 d . . . H8 H 0.4171 0.2885 0.5945 0.030 Uiso 1 1 calc R . . C9 C 0.3482(9) 0.1619(7) 0.4810(5) 0.0242(16) Uani 1 1 d . . . H9 H 0.3996 0.1003 0.5024 0.029 Uiso 1 1 calc R . . C10 C 0.2643(9) 0.1395(7) 0.3959(5) 0.0215(15) Uani 1 1 d . . . H10 H 0.2589 0.0635 0.3580 0.026 Uiso 1 1 calc R . . C11 C 0.1876(9) 0.2291(7) 0.3660(5) 0.0185(15) Uani 1 1 d . . . C12 C -0.1061(9) 0.0790(6) 0.2758(5) 0.0209(11) Uani 1 1 d . . . H12A H -0.1892 0.0638 0.2222 0.025 Uiso 1 1 calc R . . H12B H -0.0725 -0.0007 0.2816 0.025 Uiso 1 1 calc R . . C13 C -0.1868(9) 0.1127(6) 0.3585(5) 0.0189(15) Uani 1 1 d . . . H13A H -0.2439 0.0335 0.3799 0.023 Uiso 1 1 calc R . . H13B H -0.0987 0.1589 0.4067 0.023 Uiso 1 1 calc R . . C14 C -0.3087(9) 0.1913(6) 0.3443(5) 0.0209(11) Uani 1 1 d . . . H14A H -0.3385 0.2197 0.4038 0.025 Uiso 1 1 calc R . . H14B H -0.4106 0.1363 0.3094 0.025 Uiso 1 1 calc R . . C15 C -0.3342(9) 0.2733(7) 0.1741(5) 0.0214(16) Uani 1 1 d . . . C16 C -0.5055(9) 0.2190(7) 0.1566(5) 0.0254(17) Uani 1 1 d . . . H16 H -0.5720 0.2068 0.2045 0.030 Uiso 1 1 calc R . . C17 C -0.5743(10) 0.1841(9) 0.0688(6) 0.039(2) Uani 1 1 d . . . H17 H -0.6896 0.1467 0.0558 0.046 Uiso 1 1 calc R . . C18 C -0.4778(12) 0.2027(9) -0.0014(6) 0.043(2) Uani 1 1 d . . . H18 H -0.5285 0.1777 -0.0617 0.051 Uiso 1 1 calc R . . C19 C -0.3086(10) 0.2570(8) 0.0147(5) 0.0312(19) Uani 1 1 d . . . H19 H -0.2438 0.2697 -0.0339 0.037 Uiso 1 1 calc R . . C20 C -0.2349(9) 0.2928(7) 0.1048(5) 0.0207(15) Uani 1 1 d . . . C21 C 0.0499(9) 0.3749(7) 0.0722(4) 0.0180(10) Uani 1 1 d . . . C22 C 0.2162(8) 0.4324(6) 0.1220(4) 0.0167(14) Uani 1 1 d . . . C23 C 0.3566(9) 0.4766(7) 0.0791(5) 0.0241(16) Uani 1 1 d . . . H23 H 0.3457 0.4682 0.0152 0.029 Uiso 1 1 calc R . . C24 C 0.5133(10) 0.5390(7) 0.2136(5) 0.0237(16) Uani 1 1 d . . . H24 H 0.6168 0.5771 0.2482 0.028 Uiso 1 1 calc R . . C25 C 0.3769(8) 0.4951(6) 0.2588(5) 0.0183(14) Uani 1 1 d . . . H25 H 0.3890 0.5023 0.3227 0.022 Uiso 1 1 calc R . . 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 Co 0.0130(5) 0.0106(4) 0.0115(4) 0.0031(3) 0.0029(3) 0.0037(3) S1 0.0207(9) 0.0138(8) 0.0145(8) 0.0035(6) 0.0026(7) 0.0060(7) S2 0.0148(9) 0.0168(8) 0.0183(9) 0.0036(6) 0.0045(7) 0.0028(7) Cl 0.0324(11) 0.0212(9) 0.0241(10) 0.0008(7) 0.0019(8) 0.0014(8) O1 0.029(3) 0.019(3) 0.019(3) 0.004(2) 0.003(2) 0.006(2) O2 0.030(3) 0.071(4) 0.014(3) 0.007(3) 0.007(2) 0.004(3) O3 0.138(8) 0.023(3) 0.037(4) 0.015(3) -0.011(4) 0.018(4) O4 0.030(4) 0.069(5) 0.059(5) -0.026(4) 0.016(3) -0.016(3) O5 0.035(3) 0.054(4) 0.024(3) 0.008(3) 0.002(2) 0.025(3) O6 0.025(3) 0.021(3) 0.047(4) -0.009(2) 0.003(3) 0.004(2) N1 0.015(3) 0.005(3) 0.022(3) 0.006(2) 0.003(2) 0.004(2) N2 0.028(4) 0.017(3) 0.029(4) 0.004(3) 0.000(3) 0.008(3) N3 0.019(3) 0.012(3) 0.015(3) 0.005(2) 0.007(2) 0.005(2) N4 0.022(3) 0.024(3) 0.013(3) 0.012(2) 0.006(2) 0.009(3) N5 0.008(3) 0.020(3) 0.015(3) 0.006(2) 0.006(2) 0.008(2) N6 0.024(4) 0.032(4) 0.027(4) 0.011(3) 0.014(3) 0.011(3) C1 0.028(4) 0.013(3) 0.017(3) 0.006(3) 0.006(3) 0.011(3) C2 0.026(4) 0.018(4) 0.046(5) 0.010(3) 0.003(4) 0.012(3) C3 0.029(4) 0.011(3) 0.025(4) 0.004(3) 0.005(3) 0.013(3) C4 0.020(4) 0.018(3) 0.013(3) 0.000(3) 0.006(3) 0.008(3) C5 0.023(3) 0.022(3) 0.009(2) -0.0010(18) 0.0055(19) 0.007(2) C6 0.024(4) 0.015(3) 0.005(3) 0.004(2) 0.003(3) 0.007(3) C7 0.024(4) 0.022(4) 0.015(3) 0.000(3) 0.000(3) 0.009(3) C8 0.023(4) 0.037(4) 0.019(4) 0.012(3) -0.001(3) 0.012(3) C9 0.021(4) 0.023(4) 0.031(4) 0.012(3) 0.003(3) 0.007(3) C10 0.025(4) 0.020(4) 0.024(4) 0.008(3) 0.005(3) 0.009(3) C11 0.018(4) 0.024(4) 0.015(3) 0.003(3) 0.006(3) 0.009(3) C12 0.018(3) 0.013(2) 0.024(3) 0.0018(19) 0.004(2) -0.0109(19) C13 0.020(4) 0.018(3) 0.017(4) 0.008(3) 0.004(3) -0.001(3) C14 0.018(3) 0.013(2) 0.024(3) 0.0018(19) 0.004(2) -0.0109(19) C15 0.018(4) 0.033(4) 0.020(4) 0.011(3) 0.008(3) 0.013(3) C16 0.019(4) 0.033(4) 0.023(4) 0.014(3) 0.001(3) -0.001(3) C17 0.020(4) 0.052(6) 0.040(5) 0.011(4) -0.011(4) 0.006(4) C18 0.038(5) 0.056(6) 0.025(5) 0.006(4) -0.008(4) -0.002(5) C19 0.028(5) 0.047(5) 0.021(4) 0.003(3) 0.003(3) 0.014(4) C20 0.014(4) 0.027(4) 0.020(4) 0.010(3) -0.002(3) 0.001(3) C21 0.023(3) 0.022(3) 0.009(2) -0.0010(18) 0.0055(19) 0.007(2) C22 0.015(3) 0.023(4) 0.011(3) 0.003(3) 0.002(3) 0.002(3) C23 0.019(4) 0.033(4) 0.019(4) 0.000(3) 0.004(3) 0.004(3) C24 0.021(4) 0.020(4) 0.031(4) 0.002(3) 0.001(3) 0.010(3) C25 0.015(4) 0.022(4) 0.020(4) 0.002(3) 0.005(3) 0.006(3) _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 Co N3 1.925(6) . ? Co N5 1.927(5) . ? Co N4 1.928(6) . ? Co N1 1.942(5) . ? Co S1 2.199(2) . ? Co S2 2.234(2) . ? S1 C11 1.771(7) . ? S1 C12 1.821(7) . ? S2 C15 1.780(8) . ? S2 C14 1.831(7) . ? Cl O6 1.416(5) . ? Cl O3 1.418(6) . ? Cl O5 1.426(6) . ? Cl O4 1.449(7) . ? O1 C5 1.234(8) . ? O2 C21 1.220(8) . ? N1 C1 1.338(8) . ? N1 C4 1.339(8) . ? N2 C2 1.322(10) . ? N2 C3 1.325(9) . ? N3 C5 1.349(8) . ? N3 C6 1.397(8) . ? N4 C21 1.359(9) . ? N4 C20 1.415(9) . ? N5 C22 1.333(8) . ? N5 C25 1.347(8) . ? N6 C24 1.323(10) . ? N6 C23 1.341(9) . ? C1 C2 1.410(9) . ? C3 C4 1.389(9) . ? C4 C5 1.487(9) . ? C6 C7 1.402(9) . ? C6 C11 1.424(9) . ? C7 C8 1.391(10) . ? C8 C9 1.391(10) . ? C9 C10 1.373(10) . ? C10 C11 1.384(9) . ? C12 C13 1.519(10) . ? C13 C14 1.497(10) . ? C15 C20 1.394(10) . ? C15 C16 1.407(10) . ? C16 C17 1.371(11) . ? C17 C18 1.389(13) . ? C18 C19 1.390(12) . ? C19 C20 1.415(10) . ? C21 C22 1.484(9) . ? C22 C23 1.401(10) . ? C24 C25 1.395(10) . ? 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 Co N5 92.7(2) . . ? N3 Co N4 176.0(2) . . ? N5 Co N4 83.3(2) . . ? N3 Co N1 83.8(2) . . ? N5 Co N1 89.7(2) . . ? N4 Co N1 96.0(2) . . ? N3 Co S1 88.47(17) . . ? N5 Co S1 87.66(17) . . ? N4 Co S1 91.54(18) . . ? N1 Co S1 171.69(17) . . ? N3 Co S2 96.16(18) . . ? N5 Co S2 169.61(17) . . ? N4 Co S2 87.80(18) . . ? N1 Co S2 85.97(17) . . ? S1 Co S2 97.93(7) . . ? C11 S1 C12 100.7(3) . . ? C11 S1 Co 97.3(2) . . ? C12 S1 Co 111.7(3) . . ? C15 S2 C14 102.1(3) . . ? C15 S2 Co 96.8(2) . . ? C14 S2 Co 118.7(3) . . ? O6 Cl O3 109.2(4) . . ? O6 Cl O5 111.1(4) . . ? O3 Cl O5 107.9(4) . . ? O6 Cl O4 109.3(4) . . ? O3 Cl O4 111.1(5) . . ? O5 Cl O4 108.2(4) . . ? C1 N1 C4 119.3(6) . . ? C1 N1 Co 127.9(5) . . ? C4 N1 Co 112.9(4) . . ? C2 N2 C3 117.8(6) . . ? C5 N3 C6 124.6(6) . . ? C5 N3 Co 115.2(4) . . ? C6 N3 Co 119.8(4) . . ? C21 N4 C20 124.4(6) . . ? C21 N4 Co 116.1(5) . . ? C20 N4 Co 119.5(4) . . ? C22 N5 C25 118.5(6) . . ? C22 N5 Co 113.3(4) . . ? C25 N5 Co 128.1(5) . . ? C24 N6 C23 116.0(7) . . ? N1 C1 C2 119.0(7) . . ? N2 C2 C1 122.0(7) . . ? N2 C3 C4 122.0(7) . . ? N1 C4 C3 119.9(6) . . ? N1 C4 C5 115.9(6) . . ? C3 C4 C5 124.0(6) . . ? O1 C5 N3 127.8(6) . . ? O1 C5 C4 120.1(6) . . ? N3 C5 C4 112.1(6) . . ? N3 C6 C7 127.1(6) . . ? N3 C6 C11 115.5(6) . . ? C7 C6 C11 117.4(6) . . ? C8 C7 C6 120.0(7) . . ? C9 C8 C7 121.1(7) . . ? C10 C9 C8 120.3(7) . . ? C9 C10 C11 119.3(7) . . ? C10 C11 C6 122.0(6) . . ? C10 C11 S1 119.7(5) . . ? C6 C11 S1 118.4(5) . . ? C13 C12 S1 114.2(5) . . ? C14 C13 C12 115.0(6) . . ? C13 C14 S2 117.0(5) . . ? C20 C15 C16 121.6(7) . . ? C20 C15 S2 118.6(6) . . ? C16 C15 S2 119.6(5) . . ? C17 C16 C15 118.5(7) . . ? C16 C17 C18 121.0(8) . . ? C17 C18 C19 121.3(8) . . ? C18 C19 C20 118.7(8) . . ? C15 C20 C19 119.0(7) . . ? C15 C20 N4 116.5(6) . . ? C19 C20 N4 124.6(7) . . ? O2 C21 N4 128.5(7) . . ? O2 C21 C22 121.2(6) . . ? N4 C21 C22 110.3(6) . . ? N5 C22 C23 120.1(6) . . ? N5 C22 C21 116.9(6) . . ? C23 C22 C21 123.0(6) . . ? N6 C23 C22 122.5(7) . . ? N6 C24 C25 123.3(7) . . ? N5 C25 C24 119.6(7) . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.005 _refine_diff_density_min -1.470 _refine_diff_density_rms 0.182 #===END data_15maya _database_code_depnum_ccdc_archive 'CCDC 652243' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H19 Co N6 O2 S2' _chemical_formula_sum 'C25 H19 Co N6 O2 S2' _chemical_formula_weight 558.51 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c #15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 29.151(5) _cell_length_b 7.911(5) _cell_length_c 22.885(5) _cell_angle_alpha 90.000 _cell_angle_beta 120.892(5) _cell_angle_gamma 90.000 _cell_volume 4529(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Block _exptl_crystal_colour Reddish-brown _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.638 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.981 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.8279 _exptl_absorpt_correction_T_max 0.8279 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14707 _diffrn_reflns_av_R_equivalents 0.0682 _diffrn_reflns_av_sigmaI/netI 0.0877 _diffrn_reflns_limit_h_min -38 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 28.37 _reflns_number_total 5583 _reflns_number_gt 3814 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0430P)^2^+11.5704P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5583 _refine_ls_number_parameters 329 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0975 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1321 _refine_ls_wR_factor_gt 0.1106 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.082 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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 Co Co 0.616745(18) 0.04058(6) 0.20932(2) 0.01119(13) Uani 1 1 d . . . S1 S 0.62070(3) 0.29412(12) 0.25134(5) 0.0143(2) Uani 1 1 d . . . S2 S 0.63971(4) -0.21249(13) 0.32805(5) 0.0169(2) Uani 1 1 d . . . O1 O 0.46950(10) -0.0386(4) 0.04842(14) 0.0247(7) Uani 1 1 d . . . O2 O 0.77159(10) -0.0465(3) 0.27144(13) 0.0193(6) Uani 1 1 d . . . C4 C 0.55201(14) -0.1836(5) 0.10684(18) 0.0127(7) Uani 1 1 d . . . N1 N 0.60141(11) -0.1759(4) 0.16249(14) 0.0111(6) Uani 1 1 d . . . N2 N 0.56968(12) -0.4501(4) 0.07408(16) 0.0164(7) Uani 1 1 d . . . N3 N 0.54339(11) 0.0872(4) 0.14149(15) 0.0118(6) Uani 1 1 d . . . N4 N 0.69294(11) 0.0024(4) 0.27213(15) 0.0133(6) Uani 1 1 d . . . N5 N 0.64451(11) 0.1078(4) 0.14669(15) 0.0119(6) Uani 1 1 d . . . N6 N 0.69437(13) 0.1283(4) 0.07035(17) 0.0214(7) Uani 1 1 d . . . C1 C 0.63431(14) -0.3056(5) 0.17489(18) 0.0131(7) Uani 1 1 d . . . H1 H 0.6688 -0.3060 0.2148 0.016 Uiso 1 1 calc R . . C2 C 0.61841(14) -0.4401(5) 0.12970(19) 0.0147(8) Uani 1 1 d . . . H2 H 0.6432 -0.5288 0.1387 0.018 Uiso 1 1 calc R . . C3 C 0.53663(14) -0.3226(5) 0.06344(19) 0.0157(8) Uani 1 1 d . . . H3 H 0.5014 -0.3263 0.0250 0.019 Uiso 1 1 calc R . . C5 C 0.51655(14) -0.0356(5) 0.09535(19) 0.0162(8) Uani 1 1 d . . . C6 C 0.52022(14) 0.2423(5) 0.14165(19) 0.0131(7) Uani 1 1 d . . . C7 C 0.46805(14) 0.2950(5) 0.09391(19) 0.0165(8) Uani 1 1 d . . . H7 H 0.4450 0.2234 0.0570 0.020 Uiso 1 1 calc R . . C8 C 0.45044(14) 0.4529(5) 0.1011(2) 0.0182(8) Uani 1 1 d . . . H8 H 0.4152 0.4880 0.0683 0.022 Uiso 1 1 calc R . . C9 C 0.48259(15) 0.5604(5) 0.1544(2) 0.0205(9) Uani 1 1 d . . . H9 H 0.4695 0.6668 0.1588 0.025 Uiso 1 1 calc R . . C10 C 0.53423(15) 0.5094(5) 0.20125(19) 0.0161(8) Uani 1 1 d . . . H10 H 0.5570 0.5813 0.2382 0.019 Uiso 1 1 calc R . . C11 C 0.55273(14) 0.3544(5) 0.19431(18) 0.0143(8) Uani 1 1 d . . . C12 C 0.61753(15) 0.2364(5) 0.32636(19) 0.0192(8) Uani 1 1 d . . . H12A H 0.6537 0.2085 0.3646 0.023 Uiso 1 1 calc R . . H12B H 0.6034 0.3322 0.3403 0.023 Uiso 1 1 calc R . . C13 C 0.58149(15) 0.0863(5) 0.3088(2) 0.0194(9) Uani 1 1 d . . . H13A H 0.5439 0.1232 0.2795 0.023 Uiso 1 1 calc R . . H13B H 0.5854 0.0388 0.3512 0.023 Uiso 1 1 calc R . . C14 C 0.59394(14) -0.0523(5) 0.27181(19) 0.0136(8) Uani 1 1 d . . . H14 H 0.5646(15) -0.109(5) 0.247(2) 0.018(11) Uiso 1 1 d . . . C15 C 0.69781(14) -0.0889(5) 0.37734(19) 0.0136(8) Uani 1 1 d . . . C16 C 0.72093(15) -0.0789(5) 0.4472(2) 0.0194(8) Uani 1 1 d . . . H16 H 0.7059 -0.1406 0.4690 0.023 Uiso 1 1 calc R . . C17 C 0.76551(16) 0.0197(5) 0.4856(2) 0.0229(9) Uani 1 1 d . . . H17 H 0.7816 0.0237 0.5337 0.028 Uiso 1 1 calc R . . C18 C 0.78671(15) 0.1126(5) 0.4539(2) 0.0226(9) Uani 1 1 d . . . H18 H 0.8171 0.1821 0.4802 0.027 Uiso 1 1 calc R . . C19 C 0.76354(14) 0.1043(5) 0.38383(19) 0.0180(8) Uani 1 1 d . . . H19 H 0.7782 0.1691 0.3623 0.022 Uiso 1 1 calc R . . C20 C 0.71891(13) 0.0018(5) 0.34429(18) 0.0129(7) Uani 1 1 d . . . C21 C 0.72428(13) -0.0015(5) 0.24444(18) 0.0130(8) Uani 1 1 d . . . C22 C 0.69574(14) 0.0600(5) 0.17259(18) 0.0123(7) Uani 1 1 d . . . C23 C 0.71996(15) 0.0717(5) 0.1343(2) 0.0185(8) Uani 1 1 d . . . H23 H 0.7563 0.0381 0.1544 0.022 Uiso 1 1 calc R . . C24 C 0.64343(15) 0.1740(5) 0.04526(19) 0.0181(8) Uani 1 1 d . . . H24 H 0.6236 0.2146 -0.0002 0.022 Uiso 1 1 calc R . . C25 C 0.61838(15) 0.1648(5) 0.08281(18) 0.0155(8) Uani 1 1 d . . . H25 H 0.5822 0.1994 0.0628 0.019 Uiso 1 1 calc R . . 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 Co 0.0091(2) 0.0131(3) 0.0109(2) -0.0008(2) 0.0048(2) -0.00026(19) S1 0.0125(4) 0.0163(5) 0.0143(5) -0.0032(4) 0.0071(4) -0.0011(3) S2 0.0170(5) 0.0183(5) 0.0166(5) 0.0024(4) 0.0095(4) -0.0007(4) O1 0.0136(13) 0.0240(16) 0.0222(15) -0.0047(12) -0.0011(12) 0.0011(12) O2 0.0125(12) 0.0257(16) 0.0192(14) -0.0008(12) 0.0078(11) 0.0004(11) C4 0.0132(17) 0.0146(19) 0.0141(18) 0.0022(15) 0.0096(15) -0.0001(14) N1 0.0104(14) 0.0139(16) 0.0074(14) -0.0005(12) 0.0034(12) -0.0033(12) N2 0.0177(15) 0.0145(17) 0.0195(17) 0.0008(13) 0.0113(14) -0.0001(13) N3 0.0104(14) 0.0111(15) 0.0121(15) 0.0010(12) 0.0044(13) 0.0001(11) N4 0.0143(15) 0.0134(16) 0.0114(15) 0.0009(12) 0.0060(13) 0.0000(12) N5 0.0112(14) 0.0106(15) 0.0121(15) 0.0008(12) 0.0047(13) -0.0016(12) N6 0.0231(17) 0.026(2) 0.0195(18) -0.0012(15) 0.0141(15) -0.0062(15) C1 0.0117(17) 0.015(2) 0.0135(18) 0.0036(15) 0.0076(15) -0.0002(14) C2 0.0116(17) 0.016(2) 0.0172(19) 0.0042(15) 0.0082(15) -0.0018(15) C3 0.0116(17) 0.019(2) 0.0129(19) 0.0017(15) 0.0036(15) -0.0020(15) C5 0.0140(18) 0.018(2) 0.0148(19) 0.0004(15) 0.0061(15) -0.0024(15) C6 0.0131(17) 0.0145(19) 0.0153(19) 0.0020(14) 0.0099(16) 0.0018(14) C7 0.0152(18) 0.019(2) 0.018(2) 0.0040(16) 0.0098(16) -0.0015(15) C8 0.0116(17) 0.023(2) 0.021(2) 0.0105(17) 0.0094(16) 0.0077(16) C9 0.023(2) 0.017(2) 0.027(2) 0.0027(17) 0.0163(18) 0.0018(16) C10 0.0237(19) 0.0087(19) 0.020(2) -0.0020(15) 0.0139(17) -0.0017(15) C11 0.0128(17) 0.0145(19) 0.0155(19) 0.0026(15) 0.0072(16) -0.0015(14) C12 0.0184(19) 0.028(2) 0.0116(19) -0.0012(16) 0.0082(16) 0.0031(17) C13 0.0188(19) 0.024(2) 0.020(2) 0.0031(16) 0.0137(18) 0.0017(16) C14 0.0105(17) 0.018(2) 0.0145(19) 0.0007(15) 0.0081(15) -0.0024(15) C15 0.0118(17) 0.0131(19) 0.0163(19) -0.0012(15) 0.0074(15) 0.0034(14) C16 0.025(2) 0.021(2) 0.018(2) 0.0011(16) 0.0151(18) 0.0034(16) C17 0.024(2) 0.026(2) 0.016(2) -0.0027(17) 0.0083(17) 0.0049(18) C18 0.019(2) 0.025(2) 0.016(2) -0.0067(17) 0.0029(17) 0.0010(17) C19 0.0175(19) 0.018(2) 0.019(2) 0.0009(16) 0.0096(17) -0.0008(15) C20 0.0109(16) 0.0153(19) 0.0118(18) 0.0016(14) 0.0052(15) 0.0033(14) C21 0.0129(17) 0.0117(19) 0.0133(18) -0.0026(14) 0.0060(15) -0.0021(13) C22 0.0135(17) 0.0127(19) 0.0135(18) -0.0037(14) 0.0090(15) -0.0051(14) C23 0.0186(19) 0.021(2) 0.020(2) -0.0044(16) 0.0122(17) -0.0063(16) C24 0.024(2) 0.018(2) 0.0104(19) 0.0013(15) 0.0077(17) -0.0039(16) C25 0.0206(19) 0.0130(19) 0.0146(19) -0.0029(15) 0.0102(16) -0.0011(15) _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 Co N3 1.926(3) . ? Co N1 1.946(3) . ? Co N4 1.952(3) . ? Co C14 2.001(4) . ? Co N5 2.046(3) . ? Co S1 2.2017(16) . ? S1 C11 1.789(4) . ? S1 C12 1.824(4) . ? S2 C15 1.771(4) . ? S2 C14 1.811(4) . ? O1 C5 1.234(4) . ? O2 C21 1.239(4) . ? C4 N1 1.348(4) . ? C4 C3 1.393(5) . ? C4 C5 1.493(5) . ? N1 C1 1.332(4) . ? N2 C3 1.329(5) . ? N2 C2 1.337(4) . ? N3 C5 1.350(5) . ? N3 C6 1.401(5) . ? N4 C21 1.353(5) . ? N4 C20 1.420(4) . ? N5 C25 1.333(4) . ? N5 C22 1.347(4) . ? N6 C23 1.334(5) . ? N6 C24 1.338(5) . ? C1 C2 1.388(5) . ? C6 C11 1.401(5) . ? C6 C7 1.405(5) . ? C7 C8 1.391(5) . ? C8 C9 1.384(6) . ? C9 C10 1.386(5) . ? C10 C11 1.382(5) . ? C12 C13 1.497(5) . ? C13 C14 1.538(5) . ? C15 C16 1.383(5) . ? C15 C20 1.394(5) . ? C16 C17 1.377(6) . ? C17 C18 1.381(6) . ? C18 C19 1.386(5) . ? C19 C20 1.400(5) . ? C21 C22 1.492(5) . ? C22 C23 1.382(5) . ? C24 C25 1.386(5) . ? 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 Co N1 83.04(12) . . ? N3 Co N4 174.58(13) . . ? N1 Co N4 97.02(12) . . ? N3 Co C14 90.43(14) . . ? N1 Co C14 90.23(14) . . ? N4 Co C14 94.99(14) . . ? N3 Co N5 93.47(12) . . ? N1 Co N5 84.52(12) . . ? N4 Co N5 81.15(12) . . ? C14 Co N5 173.03(14) . . ? N3 Co S1 87.99(9) . . ? N1 Co S1 171.00(9) . . ? N4 Co S1 91.98(9) . . ? C14 Co S1 89.10(12) . . ? N5 Co S1 96.80(9) . . ? C11 S1 C12 100.43(17) . . ? C11 S1 Co 97.70(13) . . ? C12 S1 Co 99.58(14) . . ? C15 S2 C14 100.43(18) . . ? N1 C4 C3 120.4(3) . . ? N1 C4 C5 116.0(3) . . ? C3 C4 C5 123.6(3) . . ? C1 N1 C4 118.0(3) . . ? C1 N1 Co 128.6(2) . . ? C4 N1 Co 113.1(2) . . ? C3 N2 C2 116.5(3) . . ? C5 N3 C6 123.1(3) . . ? C5 N3 Co 116.7(2) . . ? C6 N3 Co 120.2(2) . . ? C21 N4 C20 117.4(3) . . ? C21 N4 Co 116.4(2) . . ? C20 N4 Co 125.6(2) . . ? C25 N5 C22 117.3(3) . . ? C25 N5 Co 130.3(2) . . ? C22 N5 Co 111.5(2) . . ? C23 N6 C24 115.7(3) . . ? N1 C1 C2 120.2(3) . . ? N2 C2 C1 122.7(3) . . ? N2 C3 C4 122.1(3) . . ? O1 C5 N3 129.3(4) . . ? O1 C5 C4 119.9(3) . . ? N3 C5 C4 110.8(3) . . ? N3 C6 C11 116.2(3) . . ? N3 C6 C7 126.1(3) . . ? C11 C6 C7 117.7(3) . . ? C8 C7 C6 119.5(4) . . ? C9 C8 C7 122.1(3) . . ? C8 C9 C10 118.6(4) . . ? C11 C10 C9 120.1(4) . . ? C10 C11 C6 122.0(3) . . ? C10 C11 S1 120.3(3) . . ? C6 C11 S1 117.7(3) . . ? C13 C12 S1 108.3(3) . . ? C12 C13 C14 112.4(3) . . ? C13 C14 S2 113.8(3) . . ? C13 C14 Co 113.0(3) . . ? S2 C14 Co 111.78(18) . . ? C16 C15 C20 120.6(3) . . ? C16 C15 S2 120.5(3) . . ? C20 C15 S2 118.9(3) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C18 119.8(4) . . ? C17 C18 C19 119.9(4) . . ? C18 C19 C20 121.0(4) . . ? C15 C20 C19 118.0(3) . . ? C15 C20 N4 120.8(3) . . ? C19 C20 N4 120.9(3) . . ? O2 C21 N4 128.2(3) . . ? O2 C21 C22 119.4(3) . . ? N4 C21 C22 112.3(3) . . ? N5 C22 C23 120.9(3) . . ? N5 C22 C21 116.2(3) . . ? C23 C22 C21 122.9(3) . . ? N6 C23 C22 122.6(4) . . ? N6 C24 C25 122.8(4) . . ? N5 C25 C24 120.7(3) . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.847 _refine_diff_density_min -0.688 _refine_diff_density_rms 0.138 #===END