# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Jose Real' _publ_contact_author_email JOSE.A.REAL@UV.ES _publ_section_title ; Polymorphism and "reverse" spin transition in the spin crossover system [Co(4-terpyridone)2](CF3SO3)2*1H2O ; loop_ _publ_author_name 'Jose Real' 'Gloria Agusti' 'Carlos Bartual' 'Ana B. Gaspar' 'Victor Martinez' 'M. Carmen Munoz' ; F.J.Munoz-Lara ; # Attachment 'polym1_120K.cif' data_polymorph1_120K _database_code_depnum_ccdc_archive 'CCDC 725083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Co F6 N6 O9 S2' _chemical_formula_weight 873.62 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0800(2) _cell_length_b 9.1040(3) _cell_length_c 21.1500(7) _cell_angle_alpha 94.899(3) _cell_angle_beta 94.810(2) _cell_angle_gamma 91.322(2) _cell_volume 1735.02(9) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.672 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.712 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.936 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19738 _diffrn_reflns_av_R_equivalents 0.0690 _diffrn_reflns_av_sigmaI/netI 0.1667 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 30.42 _reflns_number_total 8059 _reflns_number_gt 4043 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8059 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1879 _refine_ls_R_factor_gt 0.1575 _refine_ls_wR_factor_ref 0.4406 _refine_ls_wR_factor_gt 0.4033 _refine_ls_goodness_of_fit_ref 1.354 _refine_ls_restrained_S_all 1.354 _refine_ls_shift/su_max 0.147 _refine_ls_shift/su_mean 0.096 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 0.21194(17) 0.09403(17) 0.75637(7) 0.0133(5) Uani 1 1 d . . . N1 N 0.1284(10) -0.1199(10) 0.7643(4) 0.0135(19) Uani 1 1 d . . . N2 N 0.1901(10) 0.1018(11) 0.8462(4) 0.016(2) Uani 1 1 d . . . N3 N 0.2906(12) 0.3096(12) 0.7856(5) 0.025(2) Uani 1 1 d . . . N4 N 0.0090(13) 0.1695(11) 0.7226(5) 0.024(2) Uani 1 1 d . . . N5 N 0.2362(11) 0.0850(11) 0.6674(5) 0.021(2) Uani 1 1 d . . . N6 N 0.4237(10) 0.0121(10) 0.7559(4) 0.015(2) Uani 1 1 d . . . O1 O 0.2088(12) 0.1021(12) 1.0400(6) 0.045(3) Uiso 1 1 d . . . O2 O 0.2938(11) 0.0670(11) 0.4772(5) 0.035(2) Uiso 1 1 d . . . C1 C 0.0913(13) -0.2285(13) 0.7179(6) 0.020(2) Uiso 1 1 d . . . C2 C 0.0235(16) -0.3604(16) 0.7273(7) 0.033(3) Uiso 1 1 d . . . C3 C -0.0055(16) -0.3831(16) 0.7904(7) 0.035(3) Uiso 1 1 d . . . C4 C 0.0292(14) -0.2699(14) 0.8392(6) 0.026(3) Uiso 1 1 d . . . C5 C 0.0944(13) -0.1441(13) 0.8246(6) 0.019(2) Uiso 1 1 d . . . C6 C 0.1459(12) -0.0186(12) 0.8723(5) 0.013(2) Uiso 1 1 d . . . C7 C 0.1511(13) -0.0270(13) 0.9372(6) 0.019(2) Uiso 1 1 d . . . C8 C 0.2014(16) 0.1030(16) 0.9766(7) 0.032(3) Uiso 1 1 d . . . C9 C 0.2420(19) 0.2297(19) 0.9514(8) 0.045(4) Uiso 1 1 d . . . C10 C 0.2397(16) 0.2226(15) 0.8833(7) 0.031(3) Uiso 1 1 d . . . C11 C 0.2866(16) 0.3475(16) 0.8484(7) 0.032(3) Uiso 1 1 d . . . C12 C 0.337(2) 0.481(2) 0.8793(10) 0.060(5) Uiso 1 1 d . . . C13 C 0.399(2) 0.585(3) 0.8435(12) 0.070(6) Uiso 1 1 d . . . C14 C 0.3999(18) 0.5520(18) 0.7771(8) 0.041(4) Uiso 1 1 d . . . C15 C 0.3414(16) 0.4120(15) 0.7498(7) 0.031(3) Uiso 1 1 d . . . C16 C -0.1066(15) 0.2121(14) 0.7565(6) 0.025(3) Uiso 1 1 d . . . C17 C -0.2348(15) 0.2707(15) 0.7268(7) 0.031(3) Uiso 1 1 d . . . C18 C -0.2457(15) 0.2792(15) 0.6629(7) 0.030(3) Uiso 1 1 d . . . C19 C -0.1276(15) 0.2355(14) 0.6266(6) 0.025(3) Uiso 1 1 d . . . C20 C -0.0024(13) 0.1814(13) 0.6577(6) 0.019(2) Uiso 1 1 d . . . C21 C 0.1256(13) 0.1274(12) 0.6271(5) 0.017(2) Uiso 1 1 d . . . C22 C 0.1418(14) 0.1228(13) 0.5614(6) 0.022(3) Uiso 1 1 d . . . C23 C 0.2686(15) 0.0737(14) 0.5377(6) 0.026(3) Uiso 1 1 d . . . C24 C 0.3815(14) 0.0265(14) 0.5814(6) 0.024(3) Uiso 1 1 d . . . C25 C 0.3623(12) 0.0371(12) 0.6447(5) 0.014(2) Uiso 1 1 d . . . C26 C 0.4677(12) -0.0111(12) 0.6963(5) 0.014(2) Uiso 1 1 d . . . C27 C 0.6038(14) -0.0758(13) 0.6844(6) 0.021(2) Uiso 1 1 d . . . C28 C 0.6905(14) -0.1165(14) 0.7360(6) 0.025(3) Uiso 1 1 d . . . C29 C 0.6483(15) -0.0988(15) 0.7957(6) 0.027(3) Uiso 1 1 d . . . C30 C 0.5100(14) -0.0268(13) 0.8043(6) 0.021(2) Uiso 1 1 d . . . O3 O 0.8688(12) -0.2443(13) 0.5870(6) 0.047(3) Uiso 1 1 d . . . S1 S -0.1517(6) 0.3227(7) 0.9386(3) 0.0686(16) Uani 1 1 d . . . C31 C -0.2872(10) 0.2439(9) 0.9184(4) 0.0000(15) Uiso 1 1 d . . . O4 O -0.1098(12) 0.3710(12) 1.0034(5) 0.042(3) Uiso 1 1 d . . . O5 O -0.246(2) 0.524(2) 0.9436(11) 0.122(7) Uiso 1 1 d . . . O6 O -0.0747(10) 0.4200(10) 0.8996(5) 0.029(2) Uiso 1 1 d . . . F1 F -0.3936(16) 0.2401(17) 0.9689(8) 0.098(4) Uiso 1 1 d . . . F2 F -0.3859(13) 0.2980(14) 0.8631(6) 0.077(3) Uiso 1 1 d . . . F3 F -0.1543(12) 0.1495(12) 0.9144(6) 0.063(3) Uiso 1 1 d . . . S2 S 0.2811(14) -0.3355(14) 0.5508(5) 0.148(4) Uani 1 1 d . . . C32 C 0.388(2) -0.418(2) 0.5773(9) 0.048(4) Uiso 1 1 d . . . O7 O 0.1981(7) -0.4243(7) 0.5396(3) 0.0000(12) Uiso 1 1 d . . . O8 O 0.1507(10) -0.2630(10) 0.5477(4) 0.029(2) Uiso 1 1 d . . . O9 O 0.354(3) -0.335(3) 0.4874(15) 0.159(10) Uiso 1 1 d . . . F4 F 0.4814(13) -0.3307(13) 0.5512(6) 0.065(3) Uiso 1 1 d . . . F5 F 0.3840(14) -0.3512(15) 0.6404(7) 0.074(3) Uiso 1 1 d . . . F6 F 0.487(18) -0.44(2) 0.637(9) 1.10(13) Uiso 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 Co 0.0155(9) 0.0143(7) 0.0104(7) 0.0056(6) -0.0005(5) 0.0009(5) N1 0.015(5) 0.022(5) 0.006(4) 0.006(4) 0.005(3) 0.003(4) N2 0.014(5) 0.022(5) 0.013(4) 0.006(4) -0.004(4) -0.003(4) N3 0.036(7) 0.025(5) 0.019(5) 0.008(5) 0.017(5) 0.005(5) N4 0.048(7) 0.016(5) 0.009(4) 0.007(4) 0.006(4) 0.006(5) N5 0.024(6) 0.024(5) 0.017(5) 0.013(4) -0.003(4) -0.002(4) N6 0.011(5) 0.023(5) 0.011(4) 0.007(4) -0.002(4) -0.001(4) S1 0.068(4) 0.088(4) 0.049(3) 0.010(3) -0.002(3) -0.009(3) S2 0.191(11) 0.171(10) 0.087(6) 0.037(7) 0.008(7) 0.057(9) _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 N1 2.099(9) . ? Co N2 1.922(9) . ? Co N3 2.097(12) . ? Co N4 2.074(11) . ? Co N5 1.909(10) . ? Co N6 2.079(10) . ? N1 C5 1.371(14) . ? N1 C1 1.348(16) . ? N2 C6 1.336(13) . ? N2 C10 1.341(18) . ? N3 C15 1.347(16) . ? N3 C11 1.347(18) . ? N4 C16 1.366(17) . ? N4 C20 1.380(14) . ? N5 C21 1.347(14) . ? N5 C25 1.346(16) . ? N6 C30 1.313(14) . ? N6 C26 1.357(14) . ? O1 C8 1.338(18) . ? O2 C23 1.314(16) . ? C1 C2 1.374(18) . ? C2 C3 1.41(2) . ? C3 C4 1.40(2) . ? C4 C5 1.348(17) . ? C5 C6 1.497(17) . ? C6 C7 1.380(15) . ? C7 C8 1.430(19) . ? C8 C9 1.37(2) . ? C9 C10 1.43(2) . ? C10 C11 1.481(18) . ? C11 C12 1.38(3) . ? C12 C13 1.40(3) . ? C13 C14 1.41(3) . ? C14 C15 1.42(2) . ? C16 C17 1.413(18) . ? C17 C18 1.356(19) . ? C18 C19 1.415(19) . ? C19 C20 1.387(17) . ? C20 C21 1.452(17) . ? C21 C22 1.407(16) . ? C22 C23 1.363(19) . ? C23 C24 1.421(18) . ? C24 C25 1.362(16) . ? C25 C26 1.491(14) . ? C26 C27 1.413(17) . ? C27 C28 1.375(17) . ? C28 C29 1.347(18) . ? C29 C30 1.448(18) . ? S1 C31 1.424(10) . ? S1 O4 1.421(13) . ? S1 O6 1.464(10) . ? S1 F3 1.614(13) . ? S1 O5 2.04(2) . ? C31 F1 1.502(17) . ? C31 F3 1.502(14) . ? C31 F2 1.534(15) . ? S2 O7 1.089(14) . ? S2 O8 1.368(14) . ? S2 C32 1.35(2) . ? S2 O9 1.54(3) . ? S2 F6 2.73(18) . ? S2 F4 1.818(17) . ? S2 F5 2.060(18) . ? C32 F4 1.335(19) . ? C32 F5 1.42(2) . ? C32 F6 1.51(19) . ? C32 O7 1.83(2) . ? O7 O8 1.539(11) . ? O9 F4 1.70(3) . ? F5 F6 1.23(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 N2 Co N1 79.1(4) . . ? N3 Co N1 158.3(4) . . ? N4 Co N1 93.7(4) . . ? N5 Co N1 100.8(4) . . ? N6 Co N1 89.4(4) . . ? N2 Co N3 79.2(4) . . ? N2 Co N4 101.1(4) . . ? N5 Co N2 179.2(4) . . ? N2 Co N6 99.2(4) . . ? N4 Co N3 91.5(4) . . ? N5 Co N3 100.9(4) . . ? N3 Co N6 93.0(4) . . ? N5 Co N4 79.7(4) . . ? N4 Co N6 159.7(4) . . ? N5 Co N6 79.9(4) . . ? C5 N1 C1 117.0(10) . . ? C5 N1 Co 113.8(8) . . ? C1 N1 Co 128.9(7) . . ? C6 N2 C10 120.3(10) . . ? C6 N2 Co 120.2(8) . . ? C10 N2 Co 118.8(8) . . ? C15 N3 C11 117.6(12) . . ? C15 N3 Co 128.4(10) . . ? C11 N3 Co 114.0(8) . . ? C16 N4 C20 118.7(11) . . ? C16 N4 Co 128.2(8) . . ? C20 N4 Co 113.1(8) . . ? C21 N5 C25 120.0(10) . . ? C21 N5 Co 119.4(8) . . ? C25 N5 Co 120.7(7) . . ? C30 N6 C26 119.1(10) . . ? C30 N6 Co 128.3(8) . . ? C26 N6 Co 112.5(7) . . ? C2 C1 N1 124.4(12) . . ? C1 C2 C3 116.9(14) . . ? C4 C3 C2 119.4(13) . . ? C5 C4 C3 118.8(12) . . ? C4 C5 N1 123.4(12) . . ? C4 C5 C6 124.4(11) . . ? N1 C5 C6 112.0(10) . . ? N2 C6 C7 122.8(11) . . ? N2 C6 C5 113.9(9) . . ? C7 C6 C5 123.3(10) . . ? C6 C7 C8 116.6(10) . . ? O1 C8 C9 118.4(14) . . ? O1 C8 C7 119.6(12) . . ? C9 C8 C7 122.0(14) . . ? C10 C9 C8 116.3(15) . . ? N2 C10 C9 121.8(12) . . ? N2 C10 C11 114.8(12) . . ? C9 C10 C11 123.3(14) . . ? C12 C11 N3 124.7(14) . . ? C12 C11 C10 122.3(14) . . ? N3 C11 C10 112.5(12) . . ? C11 C12 C13 118.3(19) . . ? C14 C13 C12 119(2) . . ? C13 C14 C15 118.4(15) . . ? N3 C15 C14 122.1(13) . . ? N4 C16 C17 121.4(12) . . ? C18 C17 C16 119.3(13) . . ? C17 C18 C19 120.4(13) . . ? C20 C19 C18 118.5(12) . . ? C19 C20 N4 121.6(11) . . ? C19 C20 C21 125.2(11) . . ? N4 C20 C21 113.1(10) . . ? N5 C21 C22 120.2(11) . . ? N5 C21 C20 114.5(10) . . ? C22 C21 C20 125.2(10) . . ? C23 C22 C21 120.5(11) . . ? O2 C23 C22 124.6(12) . . ? O2 C23 C24 117.7(12) . . ? C22 C23 C24 117.7(12) . . ? C25 C24 C23 119.6(12) . . ? N5 C25 C24 121.9(10) . . ? N5 C25 C26 111.8(9) . . ? C24 C25 C26 126.2(11) . . ? N6 C26 C27 122.1(10) . . ? N6 C26 C25 115.0(9) . . ? C27 C26 C25 122.9(10) . . ? C28 C27 C26 117.2(11) . . ? C29 C28 C27 122.2(12) . . ? C28 C29 C30 117.2(12) . . ? N6 C30 C29 122.0(11) . . ? C31 S1 O4 122.7(7) . . ? C31 S1 O6 124.6(6) . . ? O4 S1 O6 107.2(7) . . ? C31 S1 F3 58.8(6) . . ? O4 S1 F3 120.6(7) . . ? O6 S1 F3 115.3(7) . . ? C31 S1 O5 94.3(8) . . ? O4 S1 O5 80.1(9) . . ? O6 S1 O5 70.8(8) . . ? F3 S1 O5 151.7(8) . . ? S1 C31 F1 114.3(9) . . ? S1 C31 F3 66.9(6) . . ? F1 C31 F3 124.7(9) . . ? S1 C31 F2 118.4(7) . . ? F1 C31 F2 101.3(9) . . ? F3 C31 F2 127.6(9) . . ? C31 F3 S1 54.2(5) . . ? O7 S2 O8 76.6(9) . . ? O7 S2 C32 96.7(12) . . ? O8 S2 C32 155.8(12) . . ? O7 S2 O9 101.4(14) . . ? O8 S2 O9 111.0(12) . . ? C32 S2 O9 93.0(15) . . ? O7 S2 F6 106(4) . . ? O8 S2 F6 141(4) . . ? C32 S2 F6 19(4) . . ? O9 S2 F6 106(4) . . ? O7 S2 F4 132.4(11) . . ? O8 S2 F4 149.5(11) . . ? C32 S2 F4 47.0(9) . . ? O9 S2 F4 60.1(12) . . ? F6 S2 F4 51(3) . . ? O7 S2 F5 109.7(8) . . ? O8 S2 F5 116.5(9) . . ? C32 S2 F5 43.4(9) . . ? O9 S2 F5 127.6(14) . . ? F6 S2 F5 25(4) . . ? F4 S2 F5 67.8(7) . . ? F4 C32 F5 103.7(14) . . ? F4 C32 S2 85.1(13) . . ? F5 C32 S2 95.7(13) . . ? F4 C32 F6 96(7) . . ? F5 C32 F6 50(6) . . ? S2 C32 F6 145(7) . . ? F4 C32 O7 114.3(12) . . ? F5 C32 O7 107.4(12) . . ? S2 C32 O7 36.2(8) . . ? F6 C32 O7 147(6) . . ? S2 O7 O8 59.8(7) . . ? S2 O7 C32 47.2(8) . . ? O8 O7 C32 103.8(8) . . ? S2 O8 O7 43.5(6) . . ? S2 O9 F4 67.9(14) . . ? C32 F4 O9 87.0(14) . . ? C32 F4 S2 47.9(9) . . ? O9 F4 S2 51.9(10) . . ? F6 F5 C32 69(9) . . ? F6 F5 S2 109(9) . . ? C32 F5 S2 40.8(9) . . ? F5 F6 C32 62(8) . . ? F5 F6 S2 46(7) . . ? C32 F6 S2 17(3) . . ? _diffrn_measured_fraction_theta_max 0.769 _diffrn_reflns_theta_full 30.42 _diffrn_measured_fraction_theta_full 0.769 _refine_diff_density_max 2.850 _refine_diff_density_min -2.035 _refine_diff_density_rms 0.326 # Attachment 'polym1_293K.cif' data_polymorph1_293K _database_code_depnum_ccdc_archive 'CCDC 725084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Co F6 N6 O9 S2' _chemical_formula_weight 873.62 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1020(5) _cell_length_b 9.2410(5) _cell_length_c 21.3860(18) _cell_angle_alpha 94.896(2) _cell_angle_beta 94.487(2) _cell_angle_gamma 90.730(6) _cell_volume 1786.4(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prismatic _exptl_crystal_colour red _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.624 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.691 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.743 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4730 _diffrn_reflns_av_R_equivalents 0.0699 _diffrn_reflns_av_sigmaI/netI 0.0888 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 18.72 _reflns_number_total 2703 _reflns_number_gt 1854 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2703 _refine_ls_number_parameters 486 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.1355 _refine_ls_R_factor_gt 0.0936 _refine_ls_wR_factor_ref 0.3208 _refine_ls_wR_factor_gt 0.2761 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.258 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.023 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 0.1008(2) 0.2102(2) -0.24381(11) 0.0433(11) Uani 1 1 d . . . N1 N -0.1160(15) 0.1246(14) -0.2334(8) 0.044(4) Uani 1 1 d . . . N2 N 0.1065(17) 0.1895(14) -0.1517(6) 0.037(3) Uani 1 1 d . . . N3 N 0.3177(15) 0.2916(16) -0.2114(9) 0.054(4) Uani 1 1 d . . . N4 N 0.1771(14) 0.0090(16) -0.2828(8) 0.049(4) Uani 1 1 d . . . N5 N 0.0911(14) 0.2397(19) -0.3358(6) 0.048(4) Uani 1 1 d . . . N6 N 0.0137(14) 0.4261(16) -0.2491(10) 0.051(4) Uani 1 1 d . . . O1 O 0.1054(16) 0.216(2) 0.0413(7) 0.103(5) Uani 1 1 d . . . O2 O 0.0711(15) 0.2913(14) -0.5243(6) 0.077(4) Uani 1 1 d . . . C1 C -0.219(2) 0.0875(19) -0.2780(10) 0.053(5) Uani 1 1 d . . . H1 H -0.2032 0.1055 -0.3191 0.059(12) Uiso 1 1 calc R . . C2 C -0.353(2) 0.022(2) -0.2668(11) 0.065(5) Uani 1 1 d . . . H2 H -0.4258 0.0008 -0.2993 0.059(12) Uiso 1 1 calc R . . C3 C -0.373(2) -0.009(2) -0.2068(12) 0.077(6) Uani 1 1 d . . . H3 H -0.4606 -0.0537 -0.1984 0.059(12) Uiso 1 1 calc R . . C4 C -0.265(2) 0.023(2) -0.1585(10) 0.063(6) Uani 1 1 d . . . H4 H -0.2776 -0.0006 -0.1179 0.059(12) Uiso 1 1 calc R . . C5 C -0.1359(18) 0.0923(19) -0.1718(9) 0.042(5) Uani 1 1 d . . . C6 C -0.015(2) 0.1422(18) -0.1254(10) 0.053(5) Uani 1 1 d . . . C7 C -0.021(2) 0.150(2) -0.0613(11) 0.063(6) Uani 1 1 d . . . H7 H -0.1052 0.1199 -0.0438 0.059(12) Uiso 1 1 calc R . . C8 C 0.107(3) 0.208(3) -0.0207(11) 0.079(7) Uani 1 1 d . . . C9 C 0.224(3) 0.250(3) -0.0479(12) 0.088(7) Uani 1 1 d . . . H9 H 0.3071 0.2880 -0.0236 0.059(12) Uiso 1 1 calc R . . C10 C 0.222(2) 0.236(2) -0.1160(11) 0.059(5) Uani 1 1 d . . . C11 C 0.348(2) 0.287(2) -0.1507(12) 0.060(5) Uani 1 1 d . . . C12 C 0.483(3) 0.330(2) -0.1200(11) 0.085(7) Uani 1 1 d . . . H12 H 0.5004 0.3262 -0.0768 0.059(12) Uiso 1 1 calc R . . C13 C 0.587(3) 0.380(3) -0.1550(15) 0.103(9) Uani 1 1 d . . . H13 H 0.6793 0.4106 -0.1359 0.059(12) Uiso 1 1 calc R . . C14 C 0.558(2) 0.385(3) -0.2172(15) 0.087(7) Uani 1 1 d . . . H14 H 0.6298 0.4194 -0.2412 0.059(12) Uiso 1 1 calc R . . C15 C 0.425(3) 0.339(2) -0.2453(10) 0.064(6) Uani 1 1 d . . . H15 H 0.4066 0.3412 -0.2886 0.059(12) Uiso 1 1 calc R . . C16 C 0.225(2) -0.104(2) -0.2517(9) 0.057(5) Uani 1 1 d . . . H16 H 0.2193 -0.0991 -0.2083 0.059(12) Uiso 1 1 calc R . . C17 C 0.282(2) -0.226(2) -0.2804(13) 0.071(6) Uani 1 1 d . . . H17 H 0.3161 -0.3009 -0.2570 0.059(12) Uiso 1 1 calc R . . C18 C 0.287(2) -0.236(2) -0.3439(15) 0.084(7) Uani 1 1 d . . . H18 H 0.3210 -0.3198 -0.3649 0.059(12) Uiso 1 1 calc R . . C19 C 0.242(2) -0.121(3) -0.3770(10) 0.075(6) Uani 1 1 d . . . H19 H 0.2475 -0.1244 -0.4203 0.059(12) Uiso 1 1 calc R . . C20 C 0.1887(18) -0.003(2) -0.3450(11) 0.050(5) Uani 1 1 d . . . C21 C 0.1308(17) 0.127(2) -0.3765(10) 0.048(5) Uani 1 1 d . . . C22 C 0.1270(18) 0.138(2) -0.4399(9) 0.053(5) Uani 1 1 d . . . H22 H 0.1558 0.0610 -0.4669 0.059(12) Uiso 1 1 calc R . . C23 C 0.0771(19) 0.272(2) -0.4643(11) 0.062(6) Uani 1 1 d . . . C24 C 0.0353(18) 0.382(2) -0.4188(10) 0.053(5) Uani 1 1 d . . . H24 H 0.0012 0.4695 -0.4321 0.059(12) Uiso 1 1 calc R . . C25 C 0.0438(18) 0.362(2) -0.3565(9) 0.046(5) Uani 1 1 d . . . C26 C -0.0019(19) 0.469(2) -0.3077(10) 0.045(4) Uani 1 1 d . . . C27 C -0.0671(19) 0.595(2) -0.3190(9) 0.058(5) Uani 1 1 d . . . H27 H -0.0847 0.6203 -0.3600 0.059(12) Uiso 1 1 calc R . . C28 C -0.108(2) 0.688(2) -0.2681(13) 0.075(6) Uani 1 1 d . . . H28 H -0.1477 0.7789 -0.2744 0.059(12) Uiso 1 1 calc R . . C29 C -0.089(2) 0.642(3) -0.2097(11) 0.074(6) Uani 1 1 d . . . H29 H -0.1196 0.6993 -0.1754 0.059(12) Uiso 1 1 calc R . . C30 C -0.0227(19) 0.512(3) -0.2009(11) 0.059(5) Uani 1 1 d . . . H30 H -0.0038 0.4835 -0.1603 0.059(12) Uiso 1 1 calc R . . S1 S 0.5778(7) 0.2014(7) 0.5498(3) 0.095(2) Uani 1 1 d . . . S2 S -0.3208(13) 0.1530(12) 0.0664(5) 0.163(4) Uani 1 1 d D . . O3 O 0.2500(17) 0.1309(15) 0.4122(6) 0.093(5) Uani 1 1 d . . . O5 O 0.7303(12) 0.1537(15) 0.5533(7) 0.092(5) Uani 1 1 d . . . O4 O 0.4849(15) 0.1355(19) 0.5928(10) 0.125(7) Uani 1 1 d . . . O6 O 0.510(2) 0.209(2) 0.4882(9) 0.146(8) Uani 1 1 d . . . O7 O -0.4104(16) 0.0620(16) 0.1042(7) 0.094(5) Uani 1 1 d D . . O9 O -0.4605(15) 0.237(2) 0.0605(14) 0.63(9) Uani 1 1 d D . . O8 O -0.3648(17) 0.1106(18) -0.0005(8) 0.107(5) Uiso 1 1 d . . . C31 C 0.609(4) 0.387(4) 0.5803(18) 0.132(10) Uiso 1 1 d . . . C32 C -0.2509(12) 0.2889(14) 0.0878(6) 0.010(3) Uiso 1 1 d D . . F1 F 0.4555(19) 0.443(2) 0.5828(9) 0.155(6) Uiso 1 1 d . . . F4 F -0.313(2) 0.3648(19) 0.1425(8) 0.154(6) Uani 1 1 d . . . F3 F 0.665(2) 0.4659(18) 0.5461(10) 0.168(8) Uani 1 1 d . . . F2 F 0.6618(19) 0.3958(19) 0.6386(8) 0.148(6) Uani 1 1 d . . . F5 F -0.1481(13) 0.1654(17) 0.0896(6) 0.113(5) Uani 1 1 d . . . F6 F -0.254(3) 0.392(2) 0.0433(12) 0.230(11) 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 0.0487(17) 0.0463(17) 0.0358(18) 0.0049(11) 0.0076(11) 0.0038(11) N1 0.039(9) 0.046(9) 0.045(12) -0.001(8) 0.006(9) 0.000(7) N2 0.030(9) 0.047(9) 0.033(10) 0.000(7) -0.008(9) -0.004(7) N3 0.061(11) 0.065(11) 0.038(12) 0.018(8) -0.005(10) 0.002(8) N4 0.055(9) 0.060(12) 0.034(12) 0.014(9) 0.010(7) 0.007(8) N5 0.061(9) 0.058(12) 0.025(10) -0.001(10) 0.008(7) 0.008(8) N6 0.055(9) 0.042(10) 0.052(13) -0.014(11) 0.004(8) 0.012(7) O1 0.104(11) 0.172(17) 0.033(11) 0.016(9) 0.004(8) -0.027(10) O2 0.126(11) 0.084(10) 0.026(9) 0.025(7) 0.013(7) 0.026(8) C1 0.063(14) 0.048(12) 0.048(15) 0.011(10) 0.004(13) -0.008(10) C2 0.078(17) 0.068(14) 0.047(17) -0.004(11) -0.003(11) -0.007(12) C3 0.047(13) 0.12(2) 0.060(17) 0.011(14) -0.003(13) -0.025(11) C4 0.051(13) 0.091(16) 0.049(15) 0.009(11) 0.015(13) -0.002(11) C5 0.017(11) 0.066(13) 0.041(15) -0.010(10) 0.001(10) 0.010(9) C6 0.072(17) 0.037(11) 0.053(17) 0.001(10) 0.028(15) 0.014(10) C7 0.044(13) 0.083(15) 0.067(19) 0.018(12) 0.025(13) 0.000(10) C8 0.074(18) 0.13(2) 0.035(17) 0.020(13) 0.003(15) -0.007(14) C9 0.067(17) 0.13(2) 0.06(2) 0.027(15) -0.026(15) -0.024(14) C10 0.070(16) 0.049(12) 0.057(18) -0.001(11) 0.016(15) -0.002(11) C11 0.051(16) 0.074(15) 0.060(19) 0.022(12) 0.014(13) -0.010(11) C12 0.061(16) 0.115(19) 0.080(17) 0.015(14) 0.019(16) -0.047(13) C13 0.057(17) 0.16(3) 0.09(2) 0.002(18) -0.013(17) -0.020(15) C14 0.023(14) 0.13(2) 0.11(3) 0.011(17) 0.012(13) -0.005(12) C15 0.070(17) 0.071(14) 0.056(14) 0.020(11) 0.029(15) 0.000(11) C16 0.079(13) 0.047(14) 0.044(13) 0.004(13) -0.003(11) 0.004(11) C17 0.074(14) 0.066(18) 0.08(2) 0.027(15) -0.003(12) 0.030(12) C18 0.105(17) 0.051(16) 0.10(2) 0.021(16) 0.044(15) 0.040(12) C19 0.118(17) 0.076(18) 0.035(13) 0.006(15) 0.028(13) 0.002(14) C20 0.065(12) 0.041(14) 0.045(16) 0.013(12) 0.002(10) 0.011(10) C21 0.043(10) 0.060(15) 0.043(15) 0.020(13) 0.005(9) -0.006(10) C22 0.075(12) 0.051(14) 0.037(15) 0.004(10) 0.018(9) 0.028(10) C23 0.067(12) 0.057(15) 0.069(18) 0.019(15) 0.021(11) 0.006(10) C24 0.065(12) 0.042(13) 0.055(16) 0.014(13) 0.008(10) 0.019(9) C25 0.069(12) 0.031(13) 0.042(17) 0.029(12) -0.007(10) -0.001(10) C26 0.070(12) 0.036(14) 0.027(15) -0.009(12) 0.003(10) 0.006(10) C27 0.072(13) 0.064(16) 0.038(14) 0.001(13) 0.005(10) 0.012(12) C28 0.095(15) 0.045(14) 0.09(2) 0.000(16) 0.001(14) 0.002(11) C29 0.089(15) 0.08(2) 0.046(17) -0.006(14) -0.010(11) -0.011(14) C30 0.052(11) 0.048(14) 0.073(18) -0.005(15) -0.006(11) 0.000(10) S1 0.120(6) 0.087(5) 0.081(5) 0.011(4) 0.008(4) 0.024(4) S2 0.207(11) 0.181(10) 0.099(7) 0.004(7) 0.008(7) 0.020(8) O3 0.138(12) 0.088(11) 0.057(10) 0.006(8) 0.033(8) 0.039(9) O5 0.043(8) 0.097(11) 0.142(14) 0.023(10) 0.018(8) 0.034(7) O4 0.073(10) 0.135(15) 0.186(19) 0.075(14) 0.055(11) -0.002(9) O6 0.213(19) 0.113(15) 0.090(15) -0.052(11) -0.051(14) 0.038(14) O7 0.117(11) 0.126(13) 0.049(10) 0.045(9) 0.037(9) -0.030(9) O9 0.29(5) 1.5(3) 0.11(3) -0.08(7) 0.02(3) -0.01(9) F2 0.170(14) 0.142(14) 0.118(14) -0.018(11) -0.031(11) -0.022(11) F3 0.174(14) 0.114(13) 0.23(2) 0.090(14) 0.040(14) -0.025(11) F4 0.212(16) 0.133(14) 0.102(12) -0.038(10) -0.027(11) 0.006(12) F5 0.075(8) 0.166(14) 0.094(10) 0.011(9) -0.009(7) -0.001(8) F6 0.33(3) 0.161(19) 0.20(2) 0.086(17) -0.04(2) -0.058(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 N1 2.151(13) . ? Co1 N2 1.991(13) . ? Co1 N3 2.146(14) . ? Co1 N4 2.120(14) . ? Co1 N5 2.005(14) . ? Co1 N6 2.165(14) . ? N1 C1 1.31(2) . ? N1 C5 1.40(2) . ? N2 C10 1.29(2) . ? N2 C6 1.36(2) . ? N3 C11 1.31(2) . ? N3 C15 1.35(2) . ? N4 C16 1.35(2) . ? N4 C20 1.34(2) . ? N5 C25 1.31(2) . ? N5 C21 1.37(2) . ? N6 C30 1.31(2) . ? N6 C26 1.34(2) . ? O1 C8 1.32(2) . ? O2 C23 1.31(2) . ? C1 C2 1.40(2) . ? C1 H1 0.9300 . ? C2 C3 1.37(3) . ? C2 H2 0.9300 . ? C3 C4 1.38(3) . ? C3 H3 0.9300 . ? C4 C5 1.39(2) . ? C4 H4 0.9300 . ? C5 C6 1.46(2) . ? C7 C6 1.37(2) . ? C7 C8 1.46(3) . ? C7 H7 0.9300 . ? C8 C9 1.32(3) . ? C9 C10 1.45(3) . ? C9 H9 0.9300 . ? C10 C11 1.51(3) . ? C11 C12 1.38(3) . ? C12 C13 1.36(3) . ? C12 H12 0.9300 . ? C14 C15 1.36(3) . ? C14 C13 1.34(3) . ? C14 H14 0.9300 . ? C25 C24 1.36(2) . ? C25 C26 1.46(2) . ? C28 C29 1.35(3) . ? C28 C27 1.41(3) . ? C28 H28 0.9300 . ? C20 C19 1.35(3) . ? C20 C21 1.51(2) . ? C16 C17 1.36(3) . ? C16 H16 0.9300 . ? C26 C27 1.35(2) . ? C24 C23 1.42(3) . ? C24 H24 0.9300 . ? C19 C18 1.38(3) . ? C19 H19 0.9300 . ? C15 H15 0.9300 . ? C23 C22 1.45(2) . ? C17 C18 1.36(3) . ? C17 H17 0.9300 . ? C29 C30 1.38(3) . ? C29 H29 0.9300 . ? C18 H18 0.9300 . ? C21 C22 1.37(2) . ? C22 H22 0.9300 . ? C13 H13 0.9300 . ? C27 H27 0.9300 . ? O9 C32 1.991(11) . ? C30 H30 0.9300 . ? S1 O6 1.418(18) . ? S1 O4 1.461(15) . ? S1 O5 1.460(12) . ? S1 C31 1.79(4) . ? S2 O8 1.474(19) . ? S2 O7 1.492(16) . ? S2 O9 1.501(10) . ? S2 C32 1.424(16) . ? S2 F5 1.611(16) . ? C31 F3 1.21(3) . ? C31 F2 1.29(4) . ? C31 F1 1.50(3) . ? C32 F6 1.40(2) . ? C32 F4 1.47(2) . ? C32 F5 1.487(18) . ? 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 N1 77.6(7) . . ? N3 Co1 N1 155.3(7) . . ? N4 Co1 N1 93.6(5) . . ? N5 Co1 N1 102.2(6) . . ? N1 Co1 N6 90.6(5) . . ? N2 Co1 N3 77.8(7) . . ? N2 Co1 N4 104.4(6) . . ? N5 Co1 N2 177.5(6) . . ? N2 Co1 N6 101.5(6) . . ? N4 Co1 N3 93.9(5) . . ? N5 Co1 N3 102.3(6) . . ? N3 Co1 N6 92.9(5) . . ? N5 Co1 N4 78.1(7) . . ? N4 Co1 N6 154.0(7) . . ? N5 Co1 N6 76.0(7) . . ? C1 N1 C5 119.1(14) . . ? C1 N1 Co1 127.4(13) . . ? C5 N1 Co1 113.1(12) . . ? C10 N2 C6 119.8(16) . . ? C10 N2 Co1 119.1(13) . . ? C6 N2 Co1 120.6(13) . . ? C11 N3 C15 117.7(15) . . ? C11 N3 Co1 113.5(13) . . ? C15 N3 Co1 128.7(15) . . ? C16 N4 C20 116.1(15) . . ? C16 N4 Co1 127.5(14) . . ? C20 N4 Co1 116.2(12) . . ? C25 N5 C21 121.2(15) . . ? C25 N5 Co1 120.8(13) . . ? C21 N5 Co1 118.0(13) . . ? C30 N6 C26 120.9(16) . . ? C30 N6 Co1 125.1(16) . . ? C26 N6 Co1 114.0(13) . . ? N1 C1 C2 123.0(17) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 118.1(18) . . ? C3 C2 H2 121.0 . . ? C1 C2 H2 120.9 . . ? C2 C3 C4 120.9(18) . . ? C2 C3 H3 119.5 . . ? C4 C3 H3 119.5 . . ? C3 C4 C5 118.6(18) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 120.2(15) . . ? N1 C5 C6 114.4(16) . . ? C4 C5 C6 125.4(19) . . ? C6 C7 C8 119.1(17) . . ? C6 C7 H7 120.5 . . ? C8 C7 H7 120.5 . . ? C7 C6 N2 121.2(18) . . ? C7 C6 C5 125.3(19) . . ? N2 C6 C5 113.5(18) . . ? O1 C8 C9 121(2) . . ? O1 C8 C7 121(2) . . ? C9 C8 C7 118.0(19) . . ? C8 C9 C10 119.3(19) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.4 . . ? N2 C10 C9 122.4(16) . . ? N2 C10 C11 115(2) . . ? C9 C10 C11 123(2) . . ? N3 C11 C12 123.4(16) . . ? N3 C11 C10 114(2) . . ? C12 C11 C10 122(2) . . ? C13 C12 C11 118(2) . . ? C13 C12 H12 121.2 . . ? C11 C12 H12 121.1 . . ? C15 C14 C13 120(2) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.8 . . ? N5 C25 C24 121.0(18) . . ? N5 C25 C26 114.6(17) . . ? C24 C25 C26 124.4(19) . . ? C29 C28 C27 117.8(19) . . ? C29 C28 H28 121.1 . . ? C27 C28 H28 121.1 . . ? N4 C20 C19 123.9(16) . . ? N4 C20 C21 112.8(18) . . ? C19 C20 C21 123(2) . . ? N4 C16 C17 123.5(18) . . ? N4 C16 H16 118.3 . . ? C17 C16 H16 118.3 . . ? C27 C26 N6 120.6(16) . . ? C27 C26 C25 124(2) . . ? N6 C26 C25 114.7(18) . . ? C25 C24 C23 121.6(18) . . ? C25 C24 H24 119.2 . . ? C23 C24 H24 119.2 . . ? C18 C19 C20 118.5(19) . . ? C18 C19 H19 120.7 . . ? C20 C19 H19 120.8 . . ? C14 C15 N3 121.2(19) . . ? C14 C15 H15 119.4 . . ? N3 C15 H15 119.4 . . ? O2 C23 C24 121.8(18) . . ? O2 C23 C22 122.4(18) . . ? C24 C23 C22 115.8(19) . . ? C18 C17 C16 118.5(18) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C28 C29 C30 120(2) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C19 C18 C17 119(2) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C22 C21 N5 121.7(16) . . ? C22 C21 C20 124(2) . . ? N5 C21 C20 114.6(18) . . ? C21 C22 C23 118.6(17) . . ? C21 C22 H22 120.7 . . ? C23 C22 H22 120.7 . . ? C14 C13 C12 120(2) . . ? C14 C13 H13 120.2 . . ? C12 C13 H13 120.1 . . ? C26 C27 C28 119.5(18) . . ? C26 C27 H27 120.3 . . ? C28 C27 H27 120.3 . . ? S2 O9 C32 45.5(6) . . ? N6 C30 C29 121(2) . . ? N6 C30 H30 119.6 . . ? C29 C30 H30 119.7 . . ? O6 S1 O4 114.2(14) . . ? O6 S1 O5 115.5(11) . . ? O4 S1 O5 114.6(9) . . ? O6 S1 C31 105.0(15) . . ? O4 S1 C31 106.6(15) . . ? O5 S1 C31 98.7(13) . . ? O8 S2 O7 107.2(12) . . ? O8 S2 O9 81.5(15) . . ? O7 S2 O9 82.7(8) . . ? O8 S2 C32 122.8(11) . . ? O7 S2 C32 126.1(10) . . ? O9 S2 C32 85.7(8) . . ? O8 S2 F5 119.1(10) . . ? O7 S2 F5 114.6(10) . . ? O9 S2 F5 143.9(12) . . ? C32 S2 F5 58.3(8) . . ? F3 C31 F2 117(3) . . ? F3 C31 S1 116(3) . . ? F2 C31 S1 111(3) . . ? F3 C31 F1 103(3) . . ? F2 C31 F1 104(3) . . ? S1 C31 F1 103(2) . . ? F6 C32 F4 104.1(16) . . ? F6 C32 F5 124.8(16) . . ? F4 C32 F5 125.7(12) . . ? F6 C32 S2 115.1(14) . . ? F4 C32 S2 114.5(11) . . ? F5 C32 S2 67.2(9) . . ? F6 C32 O9 89.1(13) . . ? F4 C32 O9 83.9(12) . . ? F5 C32 O9 115.9(10) . . ? S2 C32 O9 48.8(5) . . ? C32 F5 S2 54.6(7) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 18.72 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.319 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.125 # Attachment 'polym2_293K.cif' data_polymorph2_293K _database_code_depnum_ccdc_archive 'CCDC 725085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C32 H24 Co F6 N6 O9 S2' _chemical_formula_weight 873.62 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' F F 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5700(4) _cell_length_b 14.3510(9) _cell_length_c 14.9540(8) _cell_angle_alpha 75.456(4) _cell_angle_beta 71.982(4) _cell_angle_gamma 72.274(2) _cell_volume 1832.19(17) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.584 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 886 _exptl_absorpt_coefficient_mu 0.674 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.765 _exptl_absorpt_correction_T_max 0.910 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8534 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0670 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 22.88 _reflns_number_total 4930 _reflns_number_gt 3365 _reflns_threshold_expression >2sigma(I) _computing_data_collection COLLECT _computing_cell_refinement 'HKL DENZO' _computing_data_reduction 'HKL DENZO and SCALEPACK' _computing_structure_solution SHELXS-97 _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^)+(0.2000P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.005(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4930 _refine_ls_number_parameters 462 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_gt 0.0903 _refine_ls_wR_factor_ref 0.3108 _refine_ls_wR_factor_gt 0.2661 _refine_ls_goodness_of_fit_ref 1.263 _refine_ls_restrained_S_all 1.262 _refine_ls_shift/su_max 0.041 _refine_ls_shift/su_mean 0.032 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 -0.00286(13) -0.25521(8) -0.26374(7) 0.0554(5) Uani 1 1 d . . . N1 N -0.2025(8) -0.2129(5) -0.3166(5) 0.0621(18) Uani 1 1 d . . . N2 N -0.1421(9) -0.1459(5) -0.1921(5) 0.0644(19) Uani 1 1 d . . . N3 N 0.1293(9) -0.2400(6) -0.1803(5) 0.070(2) Uani 1 1 d . . . N4 N -0.0609(8) -0.3859(5) -0.1703(4) 0.0631(18) Uani 1 1 d . . . N5 N 0.1230(7) -0.3643(5) -0.3383(4) 0.0525(16) Uani 1 1 d . . . N6 N 0.1223(8) -0.1789(5) -0.3918(5) 0.0597(17) Uani 1 1 d . . . O1 O -0.4037(10) 0.0869(5) -0.0556(5) 0.101(2) Uani 1 1 d . . . O2 O 0.3347(11) -0.5828(5) -0.4991(6) 0.116(3) Uani 1 1 d . . . C1 C -0.2285(12) -0.2518(7) -0.3807(7) 0.074(3) Uani 1 1 d . . . C2 C -0.3610(13) -0.2219(8) -0.4079(8) 0.085(3) Uani 1 1 d . . . C3 C -0.4756(13) -0.1510(8) -0.3652(8) 0.084(3) Uani 1 1 d . . . C4 C -0.4546(12) -0.1097(7) -0.2985(7) 0.073(2) Uani 1 1 d . . . C5 C -0.3155(9) -0.1417(6) -0.2764(5) 0.054(2) Uani 1 1 d . . . C6 C -0.2772(10) -0.0993(6) -0.2068(6) 0.057(2) Uani 1 1 d . . . C7 C -0.3715(11) -0.0215(6) -0.1633(6) 0.067(2) Uani 1 1 d . . . C8 C -0.3235(13) 0.0087(7) -0.0995(7) 0.076(3) Uani 1 1 d . . . C9 C -0.1845(14) -0.0397(7) -0.0817(7) 0.081(3) Uani 1 1 d . . . C10 C -0.0940(12) -0.1179(6) -0.1291(6) 0.065(2) Uani 1 1 d . . . C11 C 0.0602(12) -0.1735(6) -0.1208(6) 0.067(2) Uani 1 1 d . . . C12 C 0.1320(17) -0.1607(8) -0.0587(8) 0.095(4) Uani 1 1 d . . . C13 C 0.2792(18) -0.2137(9) -0.0601(9) 0.098(4) Uani 1 1 d . . . C14 C 0.3491(15) -0.2796(9) -0.1204(9) 0.095(3) Uani 1 1 d . . . C15 C 0.2751(14) -0.2928(9) -0.1791(7) 0.086(3) Uani 1 1 d . . . C16 C -0.1507(12) -0.3924(9) -0.0824(7) 0.085(3) Uani 1 1 d . . . C17 C -0.1759(15) -0.4824(11) -0.0261(7) 0.099(4) Uani 1 1 d . . . C18 C -0.0952(14) -0.5677(9) -0.0617(7) 0.087(3) Uani 1 1 d . . . C19 C -0.0006(12) -0.5630(7) -0.1497(7) 0.077(3) Uani 1 1 d . . . C20 C 0.0146(9) -0.4716(6) -0.2039(5) 0.056(2) Uani 1 1 d . . . C21 C 0.1088(9) -0.4582(6) -0.3027(6) 0.058(2) Uani 1 1 d . . . C22 C 0.1823(11) -0.5330(7) -0.3550(7) 0.070(2) Uani 1 1 d . . . C23 C 0.2657(12) -0.5098(7) -0.4475(7) 0.074(3) Uani 1 1 d . . . C24 C 0.2789(12) -0.4123(7) -0.4825(6) 0.073(3) Uani 1 1 d . . . C25 C 0.2075(10) -0.3440(6) -0.4270(5) 0.056(2) Uani 1 1 d . . . C26 C 0.2140(10) -0.2356(6) -0.4556(6) 0.062(2) Uani 1 1 d . . . C27 C 0.3080(12) -0.2016(7) -0.5392(6) 0.077(3) Uani 1 1 d . . . C28 C 0.3094(14) -0.1017(8) -0.5585(7) 0.094(3) Uani 1 1 d . . . C29 C 0.2121(13) -0.0406(7) -0.4966(7) 0.082(3) Uani 1 1 d . . . C30 C 0.1207(12) -0.0826(7) -0.4115(7) 0.072(2) Uani 1 1 d . . . S1 S 0.1771(6) 0.1218(4) 0.7529(5) 0.168(2) Uani 1 1 d D . . S2 S 0.5016(4) -0.4417(3) -0.7444(2) 0.1033(11) Uani 1 1 d . . . O3 O 0.3629(15) 0.2144(8) 0.8866(10) 0.161(4) Uani 1 1 d . . . O4 O 0.090(4) 0.095(2) 0.8499(13) 0.403(19) Uiso 1 1 d D . . O5 O 0.193(3) 0.0179(10) 0.7521(19) 0.320(12) Uiso 1 1 d D . . O6 O 0.302(3) 0.079(2) 0.797(3) 0.60(3) Uiso 1 1 d D . . O7 O 0.5076(10) -0.5272(7) -0.6716(6) 0.112(3) Uani 1 1 d . . . O8 O 0.4558(12) -0.3522(8) -0.7093(6) 0.121(3) Uani 1 1 d . . . O9 O 0.6331(13) -0.4506(12) -0.8212(6) 0.183(6) Uani 1 1 d . . . C31 C 0.060(2) 0.1663(14) 0.6713(15) 0.73(8) Uani 1 1 d D . . C32 C 0.353(4) -0.4428(13) -0.7865(17) 0.190(11) Uani 1 1 d . . . F1 F 0.010(3) 0.2590(14) 0.6732(17) 0.310(9) Uiso 1 1 d D . . F2 F 0.049(4) 0.171(3) 0.5871(14) 0.73(4) Uiso 1 1 d D . . F3 F -0.064(3) 0.1418(16) 0.7150(17) 0.325(11) Uiso 1 1 d D . . F4 F 0.2197(18) -0.4362(11) -0.7195(11) 0.202(5) Uiso 1 1 d . . . F5 F 0.3719(17) -0.5190(12) -0.8255(11) 0.220(5) Uiso 1 1 d . . . F6 F 0.3238(16) -0.3661(11) -0.8554(10) 0.207(5) Uiso 1 1 d . . . H1 H -0.1519 -0.3019 -0.4082 0.089(7) Uiso 1 1 calc R . . H2 H -0.3730 -0.2492 -0.4544 0.089(7) Uiso 1 1 calc R . . H3 H -0.5680 -0.1306 -0.3814 0.089(7) Uiso 1 1 calc R . . H4 H -0.5320 -0.0613 -0.2688 0.089(7) Uiso 1 1 calc R . . H7 H -0.4653 0.0102 -0.1763 0.089(7) Uiso 1 1 calc R . . H9 H -0.1512 -0.0206 -0.0385 0.089(7) Uiso 1 1 calc R . . H12 H 0.0810 -0.1166 -0.0162 0.089(7) Uiso 1 1 calc R . . H13 H 0.3295 -0.2043 -0.0202 0.089(7) Uiso 1 1 calc R . . H14 H 0.4482 -0.3162 -0.1218 0.089(7) Uiso 1 1 calc R . . H15 H 0.3248 -0.3391 -0.2196 0.089(7) Uiso 1 1 calc R . . H16 H -0.1991 -0.3344 -0.0572 0.089(7) Uiso 1 1 calc R . . H17 H -0.2449 -0.4843 0.0335 0.089(7) Uiso 1 1 calc R . . H18 H -0.1058 -0.6290 -0.0249 0.089(7) Uiso 1 1 calc R . . H19 H 0.0542 -0.6209 -0.1738 0.089(7) Uiso 1 1 calc R . . H22 H 0.1761 -0.5980 -0.3286 0.089(7) Uiso 1 1 calc R . . H24 H 0.3370 -0.3953 -0.5438 0.089(7) Uiso 1 1 calc R . . H27 H 0.3692 -0.2439 -0.5817 0.089(7) Uiso 1 1 calc R . . H28 H 0.3759 -0.0768 -0.6128 0.089(7) Uiso 1 1 calc R . . H29 H 0.2061 0.0271 -0.5103 0.089(7) Uiso 1 1 calc R . . H30 H 0.0574 -0.0419 -0.3679 0.089(7) 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 0.0644(8) 0.0560(8) 0.0478(7) -0.0164(5) -0.0094(5) -0.0168(5) N1 0.073(5) 0.058(4) 0.061(4) -0.026(3) -0.013(3) -0.015(4) N2 0.085(6) 0.065(4) 0.050(4) -0.012(3) -0.011(4) -0.032(4) N3 0.073(5) 0.075(5) 0.061(4) -0.007(4) -0.012(4) -0.024(4) N4 0.068(4) 0.071(5) 0.048(4) -0.012(3) -0.005(3) -0.022(4) N5 0.061(4) 0.051(4) 0.043(3) -0.006(3) -0.007(3) -0.018(3) N6 0.070(5) 0.049(4) 0.064(4) -0.009(3) -0.022(4) -0.016(3) O1 0.124(6) 0.080(5) 0.098(5) -0.058(4) -0.006(4) -0.012(4) O2 0.162(8) 0.077(5) 0.096(5) -0.052(4) 0.023(5) -0.039(5) C1 0.082(7) 0.071(6) 0.075(6) -0.036(5) -0.022(5) -0.008(5) C2 0.100(8) 0.076(6) 0.095(7) -0.034(6) -0.037(6) -0.015(6) C3 0.081(7) 0.084(7) 0.094(7) -0.014(6) -0.031(6) -0.022(6) C4 0.076(7) 0.062(5) 0.083(6) -0.019(5) -0.016(5) -0.018(5) C5 0.059(5) 0.049(4) 0.055(4) -0.011(4) -0.008(4) -0.019(4) C6 0.062(6) 0.055(5) 0.057(5) -0.013(4) -0.008(4) -0.024(4) C7 0.079(6) 0.055(5) 0.065(5) -0.026(4) -0.006(4) -0.012(4) C8 0.094(8) 0.067(6) 0.070(6) -0.026(5) -0.009(5) -0.024(5) C9 0.122(9) 0.066(6) 0.072(6) -0.027(5) -0.023(6) -0.036(6) C10 0.097(7) 0.055(5) 0.052(5) -0.014(4) -0.018(5) -0.030(5) C11 0.097(7) 0.058(5) 0.055(5) -0.014(4) -0.018(5) -0.032(5) C12 0.148(12) 0.075(7) 0.084(7) -0.012(5) -0.051(7) -0.039(7) C13 0.147(12) 0.087(8) 0.099(8) 0.005(7) -0.078(8) -0.052(8) C14 0.099(8) 0.096(8) 0.103(8) 0.006(7) -0.042(7) -0.043(7) C15 0.106(9) 0.097(8) 0.067(6) -0.011(5) -0.019(6) -0.046(7) C16 0.091(7) 0.102(8) 0.059(6) -0.027(6) -0.002(5) -0.025(6) C17 0.104(9) 0.138(11) 0.052(5) 0.006(7) -0.005(5) -0.056(8) C18 0.109(8) 0.089(8) 0.065(6) 0.004(6) -0.018(6) -0.046(7) C19 0.088(7) 0.070(6) 0.073(6) 0.007(5) -0.020(5) -0.038(5) C20 0.058(5) 0.061(5) 0.048(4) -0.004(4) -0.009(4) -0.023(4) C21 0.058(5) 0.067(6) 0.053(4) -0.017(4) -0.009(4) -0.022(4) C22 0.083(6) 0.053(5) 0.073(6) -0.020(4) -0.005(5) -0.022(5) C23 0.090(7) 0.060(6) 0.071(6) -0.021(5) -0.004(5) -0.028(5) C24 0.099(7) 0.066(6) 0.049(4) -0.017(4) 0.000(5) -0.027(5) C25 0.071(5) 0.053(5) 0.047(4) -0.009(4) -0.012(4) -0.024(4) C26 0.069(6) 0.060(5) 0.054(5) -0.007(4) -0.009(4) -0.022(4) C27 0.098(7) 0.064(6) 0.057(5) -0.001(4) -0.008(5) -0.025(5) C28 0.116(9) 0.080(7) 0.067(6) 0.013(6) 0.005(6) -0.050(7) C29 0.105(8) 0.056(5) 0.083(7) 0.008(5) -0.026(6) -0.032(5) C30 0.090(7) 0.054(5) 0.073(6) -0.013(4) -0.022(5) -0.015(5) O3 0.181(11) 0.099(7) 0.214(12) -0.036(7) -0.079(10) -0.012(7) S1 0.128(4) 0.137(4) 0.245(6) -0.056(4) -0.076(4) 0.007(3) S2 0.081(2) 0.164(3) 0.0633(17) -0.040(2) -0.0030(14) -0.0268(19) O7 0.110(6) 0.138(7) 0.074(5) -0.036(5) -0.011(4) -0.012(5) O9 0.133(9) 0.309(17) 0.076(5) -0.059(8) 0.024(6) -0.042(10) O8 0.149(8) 0.141(8) 0.076(5) -0.016(5) -0.016(5) -0.055(6) C31 0.90(13) 0.13(2) 1.5(2) 0.32(6) -0.97(15) -0.27(5) C32 0.34(4) 0.095(11) 0.163(17) -0.041(11) -0.12(2) -0.023(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 N1 2.151(7) . ? Co N2 2.018(8) . ? Co N3 2.118(8) . ? Co N4 2.148(7) . ? Co N5 2.011(6) . ? Co N6 2.151(7) . ? N1 C1 1.340(11) . ? N1 C5 1.344(10) . ? N2 C6 1.320(11) . ? N2 C10 1.353(11) . ? N3 C11 1.348(11) . ? N3 C15 1.373(14) . ? N4 C16 1.327(11) . ? N4 C20 1.354(11) . ? N5 C21 1.351(10) . ? N5 C25 1.335(10) . ? N6 C26 1.334(11) . ? N6 C30 1.335(11) . ? C2 C3 1.363(14) . ? C2 C1 1.363(14) . ? C4 C3 1.372(14) . ? C5 C4 1.384(13) . ? C5 C6 1.510(12) . ? C7 C6 1.369(12) . ? C7 C8 1.382(13) . ? C9 C10 1.392(14) . ? C9 C8 1.374(16) . ? C11 C12 1.388(14) . ? C11 C10 1.476(14) . ? C13 C12 1.378(18) . ? C13 C14 1.350(18) . ? C14 C15 1.364(16) . ? C16 C17 1.398(16) . ? C17 C18 1.368(16) . ? C19 C18 1.346(15) . ? C20 C19 1.381(12) . ? C20 C21 1.474(11) . ? C21 C22 1.370(12) . ? C23 C22 1.382(13) . ? C26 C27 1.369(12) . ? C26 C25 1.522(11) . ? C24 C25 1.329(12) . ? C24 C23 1.396(13) . ? C28 C27 1.393(14) . ? C29 C28 1.367(15) . ? C30 C29 1.412(14) . ? O1 C8 1.346(12) . ? O2 C23 1.341(11) . ? C24 H24 0.9300 . ? C7 H7 0.9300 . ? C30 H30 0.9300 . ? C29 H29 0.9300 . ? C16 H16 0.9300 . ? C19 H19 0.9300 . ? C28 H28 0.9300 . ? C22 H22 0.9300 . ? C27 H27 0.9300 . ? C13 H13 0.9300 . ? C4 H4 0.9300 . ? C9 H9 0.9300 . ? C14 H14 0.9300 . ? C2 H2 0.9300 . ? C12 H12 0.9300 . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C15 H15 0.9300 . ? C1 H1 0.9300 . ? C3 H3 0.9300 . ? S2 O9 1.414(10) . ? S2 O8 1.404(10) . ? S2 O7 1.421(9) . ? S2 C32 1.73(3) . ? C32 F5 1.30(2) . ? C32 F6 1.33(2) . ? C32 F4 1.35(3) . ? S1 O6 1.445(10) . ? S1 O4 1.455(10) . ? S1 O5 1.455(10) . ? S1 C31 1.782(10) . ? C31 F1 1.273(10) . ? C31 F3 1.273(10) . ? C31 F2 1.278(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 N2 Co N1 76.2(3) . . ? N3 Co N1 153.0(3) . . ? N1 Co N4 93.7(3) . . ? N5 Co N1 99.8(3) . . ? N1 Co N6 92.4(3) . . ? N2 Co N3 76.9(3) . . ? N2 Co N4 102.3(3) . . ? N5 Co N2 175.9(3) . . ? N2 Co N6 104.4(3) . . ? N3 Co N4 93.9(3) . . ? N5 Co N3 107.1(3) . . ? N3 Co N6 92.3(3) . . ? N5 Co N4 77.0(3) . . ? N4 Co N6 153.4(3) . . ? N5 Co N6 76.4(3) . . ? C26 N6 C30 117.7(7) . . ? C26 N6 Co 115.6(5) . . ? C30 N6 Co 126.6(6) . . ? C16 N4 C20 117.5(8) . . ? C16 N4 Co 127.8(7) . . ? C20 N4 Co 114.4(5) . . ? C21 N5 C25 119.0(7) . . ? C21 N5 Co 119.5(5) . . ? C25 N5 Co 121.0(5) . . ? C1 N1 C5 117.3(8) . . ? C1 N1 Co 127.7(6) . . ? C5 N1 Co 114.9(5) . . ? N4 C20 C19 121.8(8) . . ? N4 C20 C21 114.4(7) . . ? C19 C20 C21 123.7(8) . . ? C6 N2 C10 119.1(8) . . ? C6 N2 Co 121.8(6) . . ? C10 N2 Co 119.1(7) . . ? N6 C26 C27 124.2(8) . . ? N6 C26 C25 113.8(7) . . ? C27 C26 C25 122.0(8) . . ? C25 C24 C23 119.1(8) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C11 N3 C15 117.6(9) . . ? C11 N3 Co 115.9(6) . . ? C15 N3 Co 126.5(7) . . ? N1 C5 C4 122.3(8) . . ? N1 C5 C6 114.5(7) . . ? C4 C5 C6 123.2(8) . . ? C24 C25 N5 122.9(7) . . ? C24 C25 C26 124.5(7) . . ? N5 C25 C26 112.6(7) . . ? N5 C21 C22 121.3(7) . . ? N5 C21 C20 113.9(7) . . ? C22 C21 C20 124.7(8) . . ? C6 C7 C8 118.1(9) . . ? C6 C7 H7 121.0 . . ? C8 C7 H7 120.9 . . ? N6 C30 C29 122.0(9) . . ? N6 C30 H30 119.0 . . ? C29 C30 H30 119.0 . . ? N2 C6 C7 123.5(8) . . ? N2 C6 C5 112.4(7) . . ? C7 C6 C5 124.1(8) . . ? C28 C29 C30 118.6(9) . . ? C28 C29 H29 120.7 . . ? C30 C29 H29 120.7 . . ? N4 C16 C17 123.1(11) . . ? N4 C16 H16 118.5 . . ? C17 C16 H16 118.4 . . ? C20 C19 C18 119.6(10) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? N3 C11 C12 121.3(10) . . ? N3 C11 C10 113.9(8) . . ? C12 C11 C10 124.8(9) . . ? O2 C23 C22 118.6(8) . . ? O2 C23 C24 122.5(8) . . ? C22 C23 C24 118.8(8) . . ? C29 C28 C27 119.2(9) . . ? C29 C28 H28 120.4 . . ? C27 C28 H28 120.4 . . ? C21 C22 C23 118.7(8) . . ? C21 C22 H22 120.6 . . ? C23 C22 H22 120.6 . . ? C26 C27 C28 118.1(10) . . ? C26 C27 H27 121.0 . . ? C28 C27 H27 121.0 . . ? C12 C13 C14 118.9(10) . . ? C12 C13 H13 120.5 . . ? C14 C13 H13 120.6 . . ? C5 C4 C3 118.3(9) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? C10 C9 C8 119.2(9) . . ? C10 C9 H9 120.4 . . ? C8 C9 H9 120.4 . . ? N2 C10 C9 120.5(9) . . ? N2 C10 C11 114.1(8) . . ? C9 C10 C11 125.3(8) . . ? C15 C14 C13 120.3(12) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.8 . . ? C3 C2 C1 118.4(10) . . ? C3 C2 H2 120.8 . . ? C1 C2 H2 120.8 . . ? O1 C8 C7 123.3(10) . . ? O1 C8 C9 117.1(9) . . ? C7 C8 C9 119.5(9) . . ? C13 C12 C11 119.8(11) . . ? C13 C12 H12 120.1 . . ? C11 C12 H12 120.1 . . ? C18 C17 C16 117.6(10) . . ? C18 C17 H17 121.2 . . ? C16 C17 H17 121.2 . . ? C17 C18 C19 120.2(10) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? N3 C15 C14 122.1(11) . . ? N3 C15 H15 118.9 . . ? C14 C15 H15 119.0 . . ? N1 C1 C2 123.6(9) . . ? N1 C1 H1 118.2 . . ? C2 C1 H1 118.2 . . ? C2 C3 C4 120.0(10) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? O9 S2 O8 114.8(8) . . ? O9 S2 O7 112.6(7) . . ? O8 S2 O7 113.5(5) . . ? O9 S2 C32 107.4(11) . . ? O8 S2 C32 105.0(8) . . ? O7 S2 C32 102.1(9) . . ? F5 C32 F6 102.8(16) . . ? F5 C32 F4 106(2) . . ? F6 C32 F4 104(2) . . ? F5 C32 S2 116.0(19) . . ? F6 C32 S2 112.6(19) . . ? F4 C32 S2 113.6(14) . . ? O6 S1 O4 81.8(7) . . ? O6 S1 O5 81.9(7) . . ? O4 S1 O5 81.3(7) . . ? O6 S1 C31 165.3(18) . . ? O4 S1 C31 111.4(18) . . ? O5 S1 C31 93.7(14) . . ? F1 C31 F3 97.2(10) . . ? F1 C31 F2 96.3(10) . . ? F3 C31 F2 96.3(10) . . ? F1 C31 S1 104.6(16) . . ? F3 C31 S1 106.2(18) . . ? F2 C31 S1 147(2) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 22.88 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 1.216 _refine_diff_density_min -0.740 _refine_diff_density_rms 0.119