# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 loop_ _publ_author_name 'Dong Mok Shin' 'In Su Lee' 'Young Keun Chung' _publ_contact_author_name 'Prof Young Keun Chung' _publ_contact_author_address ; School of Chemistry Seoul National University College of Natural Sciences Kwanak-Gu,Shilim-9-dong Seoul 151-747 KOREA ; _publ_contact_author_email YKCHUNG@PLAZA.SNU.AC.KR _publ_section_title ; Coordination polymers based on square planar Co(II) node and linear spacer: solvent-dependent polymorphism and an unprecedented interpenetrating structure containing both 2D and 3D topological isomers ; data_compound_1 _database_code_CSD 195591 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H22 Co N8 S2' _chemical_formula_weight 569.57 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' 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 'P2(1)2(1)2 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' _cell_length_a 16.4121(12) _cell_length_b 19.4406(15) _cell_length_c 9.3903(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2996.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5538 _cell_measurement_theta_min 2.41 _cell_measurement_theta_max 26.21 _exptl_crystal_description brick _exptl_crystal_colour brown _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.43 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.263 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1172 _exptl_absorpt_coefficient_mu 0.740 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7085 _exptl_absorpt_correction_T_max 0.7414 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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_% <2.0 _diffrn_reflns_number 18409 _diffrn_reflns_av_R_equivalents 0.0248 _diffrn_reflns_av_sigmaI/netI 0.0426 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 28.27 _reflns_number_total 7029 _reflns_number_gt 4129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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. In the crystal structure, both of the crystallographically unique mppe ligands are disordered in conformation. The refinement of the disordered pyridyl group of one mppe ligand resulted in 0.52 and 0.48 site occupancies for each conformation. The other mppe ligand in two different conformations with 0.63 and 0.37 site occupancies accompanied the disorder in the isothiocyanate ligands. The refinement of the crystal structure did not distinguish the non-coordinating pyrimidyl nitrogen atoms. All N/C disorders in the pyrimidyl group were treated with arbitrary equal site occupancy. ; _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^)+(0.1677P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 7029 _refine_ls_number_parameters 464 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_gt 0.0735 _refine_ls_wR_factor_ref 0.2419 _refine_ls_wR_factor_gt 0.2148 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.987 _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 0.00175(3) 0.71405(3) 0.74615(7) 0.0580(3) Uani 1 1 d . . . N1 N -0.0840(2) 0.6383(2) 0.6733(5) 0.0656(11) Uani 1 1 d . B . C2 C -0.0586(5) 0.5814(3) 0.6046(9) 0.101(2) Uani 1 1 d . . . H2 H -0.0020 0.5766 0.5861 0.121 Uiso 1 1 calc R A 1 C3 C -0.1093(5) 0.5307(3) 0.5602(10) 0.138(4) Uani 0.50 1 d P B 1 H3 H -0.0881 0.4901 0.5180 0.166 Uiso 0.50 1 calc PR B 1 N3 N -0.1093(5) 0.5307(3) 0.5602(10) 0.138(4) Uani 0.50 1 d P B 2 C4 C -0.1897(6) 0.5388(3) 0.5769(9) 0.112(3) Uani 1 1 d . . . C5 C -0.2178(4) 0.5932(4) 0.6455(7) 0.106(2) Uani 0.50 1 d P B 2 H5 H -0.2746 0.5976 0.6623 0.127 Uiso 0.50 1 calc PR B 2 N5 N -0.2178(4) 0.5932(4) 0.6455(7) 0.106(2) Uani 0.50 1 d P B 1 C6 C -0.1644(4) 0.6447(4) 0.6939(7) 0.094(2) Uani 1 1 d . . . H6 H -0.1854 0.6841 0.7413 0.113 Uiso 1 1 calc R B 1 N71 N -0.4294(3) 0.2970(2) 0.3429(6) 0.0789(17) Uani 0.481(8) 1 d P . 1 N72 N -0.4294(3) 0.2970(2) 0.3429(6) 0.0789(17) Uani 0.52 1 d P . 2 C8 C -0.4220(5) 0.3071(4) 0.4810(9) 0.110(3) Uani 1 1 d . . . H8 H -0.4440 0.2729 0.5423 0.132 Uiso 1 1 calc R . 1 C9 C -0.3846(6) 0.3638(4) 0.5453(9) 0.129(3) Uani 1 1 d . B . H9 H -0.3791 0.3674 0.6457 0.155 Uiso 1 1 calc R C 1 C101 C -0.3562(5) 0.4140(3) 0.4556(9) 0.110(3) Uani 0.481(8) 1 d P B 1 C102 C -0.3562(5) 0.4140(3) 0.4556(9) 0.110(3) Uani 0.52 1 d P B 2 N13 N 0.0761(5) 0.7932(4) 0.8541(13) 0.066(2) Uani 0.631(4) 1 d P D 1 C14 C 0.0943(6) 0.7963(5) 0.9921(13) 0.072(2) Uani 0.631(4) 1 d P D 1 H14 H 0.0740 0.7612 1.0528 0.086 Uiso 0.631(4) 1 calc PR D 1 C15 C 0.1418(7) 0.8484(5) 1.0527(13) 0.094(3) Uani 0.32 1 d P D 1 H15 H 0.1538 0.8499 1.1516 0.113 Uiso 0.32 1 calc PR D 1 N15 N 0.1418(7) 0.8484(5) 1.0527(13) 0.094(3) Uani 0.32 1 d P E 3 C16 C 0.1705(6) 0.8983(5) 0.9570(12) 0.084(3) Uani 0.631(4) 1 d P D 1 C17 C 0.1516(7) 0.8939(5) 0.8157(11) 0.099(4) Uani 0.32 1 d P D 1 H17 H 0.1712 0.9261 0.7478 0.118 Uiso 0.32 1 calc PR D 1 N17 N 0.1516(7) 0.8939(5) 0.8157(11) 0.099(4) Uani 0.32 1 d P F 3 C18 C 0.1043(6) 0.8419(5) 0.7795(14) 0.092(4) Uani 0.631(4) 1 d P D 1 H18 H 0.0889 0.8409 0.6820 0.110 Uiso 0.631(4) 1 calc PR D 1 N19 N 0.4216(2) 1.13543(18) 1.1618(5) 0.0583(10) Uani 1 1 d . . . C20 C 0.3423(3) 1.1329(3) 1.1812(8) 0.090(2) Uani 1 1 d . . . H20 H 0.3178 1.1660 1.2421 0.108 Uiso 1 1 calc R G 1 C21 C 0.2924(3) 1.0840(4) 1.1171(8) 0.0877(19) Uani 0.82 1 d P D 1 H21 H 0.2352 1.0848 1.1325 0.105 Uiso 0.82 1 calc PR D 1 N21 N 0.2924(3) 1.0840(4) 1.1171(8) 0.0877(19) Uani 0.19 1 d P D 2 C22 C 0.3262(4) 1.0353(2) 1.0322(6) 0.0700(14) Uani 1 1 d . . . C23 C 0.4067(3) 1.0369(3) 1.0155(8) 0.087(2) Uani 0.82 1 d P D 1 H23 H 0.4330 1.0025 0.9602 0.104 Uiso 0.82 1 calc PR D 1 N23 N 0.4067(3) 1.0369(3) 1.0155(8) 0.087(2) Uani 0.19 1 d P D 2 C24 C 0.4515(4) 1.0876(3) 1.0770(7) 0.0766(16) Uani 1 1 d . . . H24 H 0.5083 1.0887 1.0576 0.092 Uiso 1 1 calc R D 1 C25 C -0.2419(6) 0.4833(3) 0.5196(11) 0.153(5) Uani 1 1 d . B . H25 H -0.2142 0.4463 0.4748 0.184 Uiso 1 1 calc R . . C26 C -0.3196(5) 0.4790(4) 0.5228(8) 0.105(3) Uani 1 1 d . . . C27 C 0.2175(12) 0.9597(7) 1.0108(14) 0.176(9) Uani 0.631(4) 1 d PD D 1 H27 H 0.1949 0.9837 1.0896 0.211 Uiso 0.631(4) 1 calc PR D 1 C28 C 0.2776(4) 0.9803(3) 0.9662(9) 0.091(2) Uani 0.631(4) 1 d P D 1 C29 C -0.3784(4) 0.5362(5) 0.5655(13) 0.160(7) Uani 0.837(19) 1 d P B . H29A H -0.4204 0.5174 0.6287 0.240 Uiso 0.837(19) 1 calc PR . . H29B H -0.4042 0.5553 0.4800 0.240 Uiso 0.837(19) 1 calc PR . . H29C H -0.3485 0.5726 0.6152 0.240 Uiso 0.837(19) 1 calc PR . . C30 C 0.311(2) 0.9707(18) 0.7859(18) 0.398(7) Uani 0.66(3) 1 d PD D 1 N31 N 0.0710(6) 0.7119(5) 0.5794(11) 0.066(2) Uani 0.631(4) 1 d P D 1 C32 C 0.1090(7) 0.7051(7) 0.476(2) 0.102(4) Uani 0.631(4) 1 d P D 1 S33 S 0.1647(3) 0.6923(3) 0.3237(6) 0.168(2) Uani 0.631(4) 1 d P D 1 N34 N -0.0709(6) 0.7112(5) 0.9413(12) 0.059(2) Uani 0.631(4) 1 d P D 1 C35 C -0.1121(6) 0.7176(6) 1.0428(13) 0.073(3) Uani 0.631(4) 1 d P D 1 S36 S -0.1705(2) 0.7238(3) 1.1819(5) 0.148(2) Uani 0.631(4) 1 d P D 1 N113 N 0.1025(6) 0.7825(5) 0.7805(11) 0.036(2) Uani 0.369(4) 1 d P D 2 C114 C 0.1211(6) 0.7985(6) 0.9163(15) 0.042(3) Uani 0.369(4) 1 d P D 2 H114 H 0.0907 0.7762 0.9889 0.051 Uiso 0.369(4) 1 calc PR D 2 C115 C 0.1810(7) 0.8447(7) 0.9599(14) 0.054(3) Uani 0.369(4) 1 d P D 2 H115 H 0.1899 0.8548 1.0576 0.065 Uiso 0.369(4) 1 calc PR D 2 C116 C 0.2294(6) 0.8767(5) 0.8469(12) 0.050(3) Uani 0.369(4) 1 d P D 2 C117 C 0.2127(8) 0.8622(6) 0.7108(11) 0.055(3) Uani 0.369(4) 1 d P D 2 H117 H 0.2451 0.8801 0.6356 0.065 Uiso 0.369(4) 1 calc PR D 2 C118 C 0.1419(8) 0.8172(6) 0.6818(13) 0.052(3) Uani 0.369(4) 1 d P D 2 H118 H 0.1237 0.8131 0.5861 0.063 Uiso 0.369(4) 1 calc PR D 2 C127 C 0.2776(4) 0.9803(3) 0.9662(9) 0.091(2) Uani 0.37 1 d P D 2 H127 H 0.2214 0.9840 0.9893 0.109 Uiso 0.369(4) 1 calc PR D 2 C128 C 0.2922(7) 0.9279(6) 0.8841(15) 0.059(3) Uani 0.369(4) 1 d P D 2 C130 C 0.3727(11) 0.9138(9) 0.798(2) 0.085(5) Uani 0.369(4) 1 d P D 2 H301 H 0.4181 0.9380 0.8434 0.128 Uiso 0.369(4) 1 calc PR D 2 H302 H 0.3661 0.9302 0.7001 0.128 Uiso 0.369(4) 1 calc PR D 2 H303 H 0.3839 0.8642 0.7974 0.128 Uiso 0.369(4) 1 calc PR D 2 N131 N 0.0571(8) 0.6885(6) 0.5289(18) 0.046(3) Uani 0.369(4) 1 d P D 2 C132 C 0.0753(10) 0.6705(7) 0.4212(17) 0.064(3) Uani 0.369(4) 1 d P D 2 S133 S 0.0941(4) 0.6367(3) 0.2684(6) 0.123(2) Uani 0.369(4) 1 d P D 2 N134 N -0.0557(10) 0.7354(7) 0.912(2) 0.055(4) Uani 0.369(4) 1 d P D 2 C135 C -0.0909(8) 0.7536(8) 1.0140(16) 0.051(3) Uani 0.369(4) 1 d P D 2 S136 S -0.1320(3) 0.7854(3) 1.1564(6) 0.1030(18) Uani 0.369(4) 1 d P D 2 C11 C -0.3377(7) 0.3919(6) 0.3019(12) 0.063(3) Uiso 0.481(8) 1 d P B 1 H11 H -0.3007 0.4174 0.2448 0.076 Uiso 0.481(8) 1 calc PR . 1 C12 C -0.3756(6) 0.3347(5) 0.2486(14) 0.062(3) Uiso 0.481(8) 1 d P B 1 H12 H -0.3668 0.3202 0.1532 0.075 Uiso 0.481(8) 1 calc PR . 1 C112 C -0.4254(8) 0.3574(7) 0.2875(15) 0.094(4) Uiso 0.519(8) 1 d P B 2 H112 H -0.4469 0.3607 0.1938 0.113 Uiso 0.519(8) 1 calc PR . 2 C122 C -0.3945(8) 0.4193(7) 0.3425(15) 0.094(4) Uiso 0.519(8) 1 d P B 2 H122 H -0.4025 0.4623 0.2962 0.113 Uiso 0.519(8) 1 calc PR . 2 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 0.0391(3) 0.0245(3) 0.1104(6) -0.0047(3) -0.0306(3) 0.00094(18) N1 0.062(2) 0.0387(19) 0.096(3) -0.010(2) -0.016(2) -0.0160(17) C2 0.114(5) 0.042(3) 0.145(6) -0.031(3) -0.058(5) 0.000(3) C3 0.146(6) 0.056(3) 0.213(8) -0.029(4) -0.121(6) -0.007(4) N3 0.146(6) 0.056(3) 0.213(8) -0.029(4) -0.121(6) -0.007(4) C4 0.151(7) 0.039(3) 0.146(6) 0.020(4) -0.095(6) -0.036(4) C5 0.085(4) 0.126(6) 0.108(5) 0.012(4) -0.038(4) -0.064(4) N5 0.085(4) 0.126(6) 0.108(5) 0.012(4) -0.038(4) -0.064(4) C6 0.065(3) 0.120(5) 0.098(4) -0.008(4) -0.020(3) -0.046(3) N71 0.080(3) 0.044(2) 0.113(4) 0.019(2) -0.061(3) -0.017(2) N72 0.080(3) 0.044(2) 0.113(4) 0.019(2) -0.061(3) -0.017(2) C8 0.152(7) 0.072(4) 0.107(5) -0.009(4) 0.007(5) -0.061(4) C9 0.195(9) 0.083(5) 0.109(5) -0.016(4) 0.001(6) -0.075(6) C101 0.126(6) 0.063(3) 0.140(6) 0.032(4) -0.067(5) -0.050(4) C102 0.126(6) 0.063(3) 0.140(6) 0.032(4) -0.067(5) -0.050(4) N13 0.057(5) 0.034(4) 0.108(7) -0.011(4) -0.038(5) -0.007(3) C14 0.072(6) 0.046(5) 0.097(7) -0.005(5) -0.004(6) -0.022(4) C15 0.090(6) 0.075(6) 0.116(8) 0.013(5) 0.001(6) -0.029(5) N15 0.090(6) 0.075(6) 0.116(8) 0.013(5) 0.001(6) -0.029(5) C16 0.086(6) 0.068(6) 0.097(7) -0.009(5) -0.010(6) -0.041(5) C17 0.132(8) 0.067(5) 0.097(7) 0.032(5) -0.069(7) -0.042(5) N17 0.132(8) 0.067(5) 0.097(7) 0.032(5) -0.069(7) -0.042(5) C18 0.098(7) 0.061(6) 0.115(9) 0.018(6) -0.062(7) -0.020(5) N19 0.0442(17) 0.0291(16) 0.101(3) -0.0063(18) -0.0094(19) 0.0023(14) C20 0.049(2) 0.086(4) 0.134(5) -0.055(4) 0.009(3) -0.024(3) C21 0.058(3) 0.083(4) 0.122(5) -0.024(4) -0.010(3) -0.027(3) N21 0.058(3) 0.083(4) 0.122(5) -0.024(4) -0.010(3) -0.027(3) C22 0.082(3) 0.040(2) 0.088(4) -0.009(2) -0.032(3) -0.013(2) C23 0.066(3) 0.065(3) 0.130(5) -0.048(3) -0.046(3) 0.016(2) N23 0.066(3) 0.065(3) 0.130(5) -0.048(3) -0.046(3) 0.016(2) C24 0.064(3) 0.069(3) 0.097(4) -0.012(3) -0.027(3) 0.019(3) C25 0.158(7) 0.054(4) 0.248(11) 0.026(5) -0.156(8) -0.031(4) C26 0.124(6) 0.074(4) 0.119(5) 0.027(4) -0.060(5) -0.051(4) C27 0.30(2) 0.138(11) 0.094(8) -0.026(8) 0.034(11) -0.176(15) C28 0.078(4) 0.053(3) 0.142(6) -0.015(3) -0.061(4) -0.012(3) C29 0.062(4) 0.159(9) 0.258(14) -0.155(10) 0.036(6) -0.041(5) C30 0.54(2) 0.54(2) 0.111(13) -0.14(2) 0.113(18) -0.504 N31 0.055(4) 0.049(5) 0.093(6) -0.006(4) 0.003(4) 0.004(4) C32 0.067(7) 0.080(8) 0.158(13) -0.026(8) -0.029(8) 0.005(6) S33 0.119(3) 0.195(5) 0.189(4) -0.017(4) 0.059(3) 0.013(3) N34 0.056(5) 0.044(6) 0.077(6) -0.009(5) 0.001(4) -0.001(4) C35 0.065(5) 0.048(5) 0.106(8) -0.007(6) -0.016(5) 0.001(4) S36 0.096(2) 0.206(5) 0.142(3) -0.049(3) 0.012(2) 0.003(3) N113 0.041(5) 0.018(4) 0.048(6) -0.001(4) -0.015(4) -0.007(3) C114 0.031(5) 0.051(7) 0.044(6) -0.005(5) -0.002(5) -0.026(4) C115 0.056(7) 0.045(7) 0.062(7) 0.000(6) -0.019(6) -0.031(5) C116 0.053(6) 0.042(5) 0.054(6) 0.008(5) -0.027(5) -0.032(5) C117 0.080(7) 0.049(6) 0.034(5) -0.001(5) -0.014(5) -0.031(6) C118 0.073(7) 0.044(6) 0.041(6) 0.018(5) -0.022(6) -0.026(6) C127 0.078(4) 0.053(3) 0.142(6) -0.015(3) -0.061(4) -0.012(3) C128 0.051(6) 0.038(6) 0.088(9) 0.022(6) -0.014(6) -0.032(5) C130 0.089(10) 0.080(11) 0.088(12) 0.004(9) -0.025(9) -0.028(9) N131 0.046(6) 0.013(5) 0.080(10) -0.002(5) -0.017(6) 0.006(4) C132 0.070(9) 0.054(8) 0.069(9) 0.004(7) -0.001(7) 0.029(7) S133 0.165(5) 0.117(4) 0.086(3) 0.005(3) 0.024(3) 0.075(4) N134 0.053(7) 0.027(7) 0.085(11) 0.011(6) -0.028(8) -0.018(5) C135 0.046(6) 0.043(7) 0.064(8) -0.001(6) -0.003(6) 0.010(6) S136 0.099(3) 0.093(3) 0.117(4) -0.047(3) 0.045(3) -0.010(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 Co1 N134 1.86(2) . ? Co1 N31 1.935(10) . ? Co1 N113 2.148(9) . ? Co1 N1 2.148(4) . ? Co1 N19 2.160(4) 3_547 ? Co1 N72 2.170(4) 3_456 ? Co1 N71 2.170(4) 3_456 ? Co1 N34 2.187(12) . ? Co1 N13 2.210(8) . ? Co1 N131 2.288(18) . ? N1 C6 1.340(7) . ? N1 C2 1.346(8) . ? C2 C3 1.356(8) . ? C3 C4 1.338(12) . ? C4 C5 1.322(12) . ? C4 C25 1.477(8) . ? C5 C6 1.406(8) . ? N71 C8 1.317(10) . ? N71 C12 1.450(12) . ? N71 Co1 2.170(4) 3_446 ? C8 C9 1.399(9) . ? C9 C101 1.370(10) . ? C101 C26 1.535(9) . ? C101 C11 1.537(15) . ? N13 C18 1.265(14) . ? N13 C14 1.332(15) . ? C14 C15 1.399(13) . ? C15 C16 1.403(14) . ? C16 C17 1.366(14) . ? C16 C27 1.508(13) . ? C17 C18 1.318(12) . ? N19 C20 1.316(6) . ? N19 C24 1.319(7) . ? N19 Co1 2.160(4) 3_557 ? C20 C21 1.390(7) . ? C21 C22 1.357(9) . ? C22 C23 1.332(9) . ? C22 C28 1.470(7) . ? C23 C24 1.358(7) . ? C25 C26 1.278(12) . ? C26 C29 1.526(12) . ? C27 C28 1.144(15) . ? C28 C30 1.787(18) . ? N31 C32 1.16(2) . ? C32 S33 1.716(19) . ? N34 C35 1.175(16) . ? C35 S36 1.625(14) . ? N113 C118 1.315(16) . ? N113 C114 1.347(17) . ? C114 C115 1.392(14) . ? C115 C116 1.465(17) . ? C116 C117 1.337(15) . ? C116 C128 1.473(12) . ? C117 C118 1.481(14) . ? C128 C130 1.57(2) . ? N131 C132 1.11(2) . ? C132 S133 1.608(17) . ? N134 C135 1.18(2) . ? C135 S136 1.621(16) . ? C11 C12 1.368(15) . ? C112 C122 1.405(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 N134 Co1 N31 167.5(5) . . ? N134 Co1 N113 97.3(5) . . ? N31 Co1 N113 71.5(4) . . ? N134 Co1 N1 95.0(4) . . ? N31 Co1 N1 96.4(3) . . ? N113 Co1 N1 167.7(3) . . ? N134 Co1 N19 96.8(5) . 3_547 ? N31 Co1 N19 88.1(3) . 3_547 ? N113 Co1 N19 86.0(3) . 3_547 ? N1 Co1 N19 91.36(19) . 3_547 ? N134 Co1 N72 83.0(5) . 3_456 ? N31 Co1 N72 91.5(3) . 3_456 ? N113 Co1 N72 91.1(3) . 3_456 ? N1 Co1 N72 91.62(16) . 3_456 ? N19 Co1 N72 177.02(16) 3_547 3_456 ? N134 Co1 N71 83.0(5) . 3_456 ? N31 Co1 N71 91.5(3) . 3_456 ? N113 Co1 N71 91.1(3) . 3_456 ? N1 Co1 N71 91.62(16) . 3_456 ? N19 Co1 N71 177.02(16) 3_547 3_456 ? N72 Co1 N71 0.0(2) 3_456 3_456 ? N134 Co1 N34 14.4(4) . . ? N31 Co1 N34 176.0(4) . . ? N113 Co1 N34 108.0(4) . . ? N1 Co1 N34 83.8(3) . . ? N19 Co1 N34 87.9(3) 3_547 . ? N72 Co1 N34 92.5(3) 3_456 . ? N71 Co1 N34 92.5(3) 3_456 . ? N134 Co1 N13 75.1(5) . . ? N31 Co1 N13 93.5(4) . . ? N113 Co1 N13 22.2(3) . . ? N1 Co1 N13 170.0(3) . . ? N19 Co1 N13 89.3(2) 3_547 . ? N72 Co1 N13 87.8(3) 3_456 . ? N71 Co1 N13 87.8(3) 3_456 . ? N34 Co1 N13 86.2(4) . . ? N134 Co1 N131 172.9(5) . . ? N31 Co1 N131 16.4(4) . . ? N113 Co1 N131 87.9(4) . . ? N1 Co1 N131 80.1(3) . . ? N19 Co1 N131 88.4(3) 3_547 . ? N72 Co1 N131 92.0(3) 3_456 . ? N71 Co1 N131 92.0(3) 3_456 . ? N34 Co1 N131 163.4(4) . . ? N13 Co1 N131 109.9(4) . . ? C6 N1 C2 116.8(5) . . ? C6 N1 Co1 122.4(4) . . ? C2 N1 Co1 120.8(4) . . ? N1 C2 C3 123.7(7) . . ? C4 C3 C2 119.0(7) . . ? C5 C4 C3 119.6(6) . . ? C5 C4 C25 124.0(9) . . ? C3 C4 C25 116.3(8) . . ? C4 C5 C6 120.7(7) . . ? N1 C6 C5 120.1(7) . . ? C8 N71 C12 118.0(6) . . ? C8 N71 Co1 122.7(4) . 3_446 ? C12 N71 Co1 118.3(6) . 3_446 ? N71 C8 C9 125.6(7) . . ? C101 C9 C8 116.4(8) . . ? C9 C101 C26 117.8(7) . . ? C9 C101 C11 116.4(7) . . ? C26 C101 C11 122.6(7) . . ? C18 N13 C14 115.0(9) . . ? C18 N13 Co1 118.0(8) . . ? C14 N13 Co1 127.0(7) . . ? N13 C14 C15 123.6(10) . . ? C14 C15 C16 115.3(11) . . ? C17 C16 C15 120.1(9) . . ? C17 C16 C27 119.5(10) . . ? C15 C16 C27 120.3(10) . . ? C18 C17 C16 115.6(9) . . ? N13 C18 C17 130.3(11) . . ? C20 N19 C24 115.1(4) . . ? C20 N19 Co1 123.2(3) . 3_557 ? C24 N19 Co1 121.6(4) . 3_557 ? N19 C20 C21 123.3(6) . . ? C22 C21 C20 119.4(5) . . ? C23 C22 C21 117.3(5) . . ? C23 C22 C28 120.3(6) . . ? C21 C22 C28 122.3(6) . . ? C22 C23 C24 120.3(5) . . ? N19 C24 C23 124.5(5) . . ? C26 C25 C4 128.1(10) . . ? C25 C26 C29 126.1(6) . . ? C25 C26 C101 115.8(8) . . ? C29 C26 C101 117.4(6) . . ? C28 C27 C16 126.5(13) . . ? C27 C28 C22 124.5(9) . . ? C27 C28 C30 124.9(9) . . ? C22 C28 C30 108.1(7) . . ? C32 N31 Co1 173.8(12) . . ? N31 C32 S33 178.2(14) . . ? C35 N34 Co1 172.2(10) . . ? N34 C35 S36 178.0(11) . . ? C118 N113 C114 116.0(9) . . ? C118 N113 Co1 126.1(8) . . ? C114 N113 Co1 117.3(7) . . ? N113 C114 C115 125.9(11) . . ? C114 C115 C116 116.4(11) . . ? C117 C116 C115 119.4(8) . . ? C117 C116 C128 120.8(10) . . ? C115 C116 C128 119.6(10) . . ? C116 C117 C118 117.5(10) . . ? N113 C118 C117 124.0(10) . . ? C116 C128 C130 110.4(12) . . ? C132 N131 Co1 170.7(14) . . ? N131 C132 S133 173.0(17) . . ? C135 N134 Co1 175.4(14) . . ? N134 C135 S136 173.6(16) . . ? C12 C11 C101 118.8(10) . . ? C11 C12 N71 117.6(10) . . ? _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.966 _refine_diff_density_max 1.047 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.090 #============== END data_compound_2 _database_code_CSD 195592 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C83 H86 Co3 N24 O5 S6' _chemical_formula_weight 1868.91 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' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 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 19.965(1) _cell_length_b 18.731(1) _cell_length_c 27.203(1) _cell_angle_alpha 90.00 _cell_angle_beta 110.190(1) _cell_angle_gamma 90.00 _cell_volume 9547.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15236 _cell_measurement_theta_min 2.70 _cell_measurement_theta_max 25.34 _exptl_crystal_description brick _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.300 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3876 _exptl_absorpt_coefficient_mu 0.706 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8716 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details 'DENZO-SMN (Otwinowski & Minor, 1997)' _exptl_special_details ; The program Denzo-SMN (Otwinowski & Minor, 1997) uses a scaling algorithm (Fox & Holmes, 1966) which effectively corrects for absorption effects. High redundancy data were used in the scaling program hence the 'multi-scan' code word was used. No transmission coefficients are available from the program (only scale factors for each frame). The scale factors in the experimental table are calculated from the 'size' command in the SHELXL-97 input file. ; _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_method 'Phi plus Omega scan' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% <2.0 _diffrn_reflns_number 15236 _diffrn_reflns_av_R_equivalents 0.0790 _diffrn_reflns_av_sigmaI/netI 0.1496 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.70 _diffrn_reflns_theta_max 25.34 _reflns_number_total 8685 _reflns_number_gt 4271 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEP3 _computing_publication_material WinGX _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. The bond distances and angles around the ethylene portion of the ligand are abnormal. However, the restraint refinement with ideal geometry resulted in the abnormally high thermal parameters. There might be some minor disorder conformations of the mppe ligand are present in the crystal structure. However, it was not possible to find the proper disorder model because of poor data quality. ; _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 8685 _refine_ls_number_parameters 538 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1864 _refine_ls_R_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.3336 _refine_ls_wR_factor_gt 0.3022 _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_restrained_S_all 1.011 _refine_ls_shift/su_max 0.002 _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 0.35499(5) 1.02671(5) 0.08701(4) 0.0418(4) Uani 1 1 d . . . Co2 Co 0.0000 0.11630(7) 0.2500 0.0425(4) Uani 1 2 d S . . S1 S 0.5255(2) 0.8401(2) 0.1266(3) 0.189(3) Uani 1 1 d . . . S2 S 0.1927(4) 1.2216(3) 0.0547(2) 0.203(3) Uani 1 1 d . . . S3 S -0.1441(2) 0.1381(2) 0.06954(14) 0.1255(14) Uani 1 1 d . . . N1 N 0.2811(3) 0.9380(3) 0.0820(2) 0.0441(15) Uani 1 1 d . . . N2 N -0.0694(4) 0.6121(4) 0.0901(3) 0.0516(17) Uani 1 1 d . . . N3 N 0.3588(4) 1.0420(4) 0.1688(3) 0.0557(18) Uani 1 1 d . . . N4 N 0.3472(4) 0.9978(4) 0.5063(3) 0.0552(18) Uani 1 1 d . . . N5 N 0.4411(4) 0.9581(4) 0.1127(3) 0.061(2) Uani 1 1 d . . . N6 N 0.2749(4) 1.0985(4) 0.0607(3) 0.0572(19) Uani 1 1 d . . . N7 N 0.0763(4) 0.1962(4) 0.2473(3) 0.0570(18) Uani 1 1 d . . . N8 N 0.4287(3) 0.5304(3) 0.2547(3) 0.0517(17) Uani 1 1 d . . . N9 N -0.0466(4) 0.1190(4) 0.1694(3) 0.0577(18) Uani 1 1 d . . . C1 C 0.2165(5) 0.9500(5) 0.0857(4) 0.065(3) Uani 1 1 d . . . H1 H 0.2036 0.9965 0.0904 0.078 Uiso 1 1 calc R . . C2 C 0.1687(5) 0.8954(5) 0.0826(4) 0.067(3) Uani 1 1 d . . . H2 H 0.1254 0.9065 0.0864 0.080 Uiso 1 1 calc R . . C3 C 0.1823(5) 0.8255(5) 0.0740(4) 0.057(2) Uani 1 1 d . . . C4 C 0.2490(5) 0.8137(5) 0.0696(4) 0.062(2) Uani 1 1 d . . . H4 H 0.2620 0.7678 0.0635 0.075 Uiso 1 1 calc R . . C5 C 0.2960(5) 0.8697(4) 0.0744(4) 0.061(2) Uani 1 1 d . . . H5 H 0.3405 0.8596 0.0721 0.073 Uiso 1 1 calc R . . C6 C 0.1287(5) 0.7664(6) 0.0665(4) 0.076(3) Uani 1 1 d . . . C7 C 0.0915(6) 0.7644(5) 0.0949(4) 0.078(3) Uani 1 1 d . . . H7 H 0.0988 0.8000 0.1200 0.094 Uiso 1 1 calc R . . C8 C -0.0119(6) 0.6256(5) 0.1317(4) 0.073(3) Uani 1 1 d . . . H8 H -0.0071 0.5996 0.1618 0.088 Uiso 1 1 calc R . . C9 C 0.0402(5) 0.6730(5) 0.1349(4) 0.065(3) Uani 1 1 d . . . H9 H 0.0779 0.6798 0.1662 0.078 Uiso 1 1 calc R . . C10 C 0.0360(5) 0.7097(5) 0.0921(4) 0.067(3) Uani 1 1 d . . . N11 N -0.0183(6) 0.6982(6) 0.0484(5) 0.131(4) Uani 1 1 d . . . C12 C -0.0740(5) 0.6515(5) 0.0483(5) 0.080(3) Uani 1 1 d . . . H12 H -0.1147 0.6484 0.0185 0.096 Uiso 1 1 calc R . . C13 C 0.1262(6) 0.7107(5) 0.0235(4) 0.083(3) Uani 1 1 d . . . H13A H 0.0921 0.6742 0.0227 0.125 Uiso 1 1 calc R . . H13B H 0.1725 0.6896 0.0311 0.125 Uiso 1 1 calc R . . H13C H 0.1123 0.7340 -0.0100 0.125 Uiso 1 1 calc R . . C14 C 0.3192(7) 1.0932(7) 0.1821(4) 0.100(4) Uani 1 1 d . . . H14 H 0.2973 1.1286 0.1579 0.120 Uiso 1 1 calc R . . C15 C 0.3112(8) 1.0937(9) 0.2294(5) 0.127(6) Uani 1 1 d . . . H15 H 0.2836 1.1291 0.2370 0.153 Uiso 1 1 calc R . . C16 C 0.3440(8) 1.0415(10) 0.2675(4) 0.123(7) Uani 1 1 d . . . C17 C 0.3853(9) 0.9891(8) 0.2536(4) 0.120(6) Uani 1 1 d . . . H17 H 0.4088 0.9539 0.2773 0.144 Uiso 1 1 calc R . . C18 C 0.3900(7) 0.9912(7) 0.2051(4) 0.092(4) Uani 1 1 d . . . H18 H 0.4162 0.9557 0.1962 0.110 Uiso 1 1 calc R . . C19 C 0.3190(6) 1.0572(7) 0.3288(7) 0.131(7) Uani 1 1 d . . . C20 C 0.3547(7) 1.0178(7) 0.3437(9) 0.171(10) Uani 1 1 d . . . H20 H 0.3838 0.9905 0.3308 0.205 Uiso 1 1 calc R . . C21 C 0.4045(5) 1.0063(6) 0.4918(4) 0.070(3) Uani 1 1 d . . . H21 H 0.4487 1.0043 0.5184 0.085 Uiso 1 1 calc R . . C22 C 0.4054(6) 1.0171(6) 0.4449(4) 0.075(3) Uani 1 1 d . . . H22 H 0.4480 1.0220 0.4385 0.090 Uiso 1 1 calc R . . C23 C 0.3399(9) 1.0210(7) 0.4049(5) 0.104(5) Uani 1 1 d . . . N24 N 0.2787(7) 1.0163(8) 0.4166(4) 0.141(5) Uani 1 1 d . . . C25 C 0.2848(6) 1.0028(6) 0.4687(4) 0.071(3) Uani 1 1 d . . . H25 H 0.2436 0.9972 0.4768 0.085 Uiso 1 1 calc R . . C26 C 0.2655(6) 1.1141(5) 0.3208(4) 0.078(3) Uani 1 1 d . . . H26A H 0.2267 1.1058 0.2886 0.117 Uiso 1 1 calc R . . H26B H 0.2870 1.1594 0.3191 0.117 Uiso 1 1 calc R . . H26C H 0.2478 1.1142 0.3494 0.117 Uiso 1 1 calc R . . C27 C 0.1019(6) 0.2471(5) 0.2811(5) 0.095(4) Uani 1 1 d . . . H27 H 0.0833 0.2527 0.3078 0.114 Uiso 1 1 calc R . . C28 C 0.1555(7) 0.2935(6) 0.2795(7) 0.125(6) Uani 1 1 d . . . H28 H 0.1720 0.3286 0.3050 0.150 Uiso 1 1 calc R . . C29 C 0.1843(6) 0.2877(8) 0.2400(9) 0.137(8) Uani 1 1 d . . . C30 C 0.1587(5) 0.2375(6) 0.2072(7) 0.113(5) Uani 1 1 d . . . H30 H 0.1768 0.2304 0.1804 0.135 Uiso 1 1 calc R . . C31 C 0.1052(5) 0.1934(5) 0.2103(5) 0.088(4) Uani 1 1 d . . . H31 H 0.0881 0.1589 0.1843 0.105 Uiso 1 1 calc R . . C32 C 0.2470(13) 0.3398(9) 0.2239(8) 0.156(8) Uani 1 1 d . . . C33 C 0.2612(14) 0.3622(11) 0.2617(6) 0.206(14) Uani 1 1 d . . . C34 C 0.4119(7) 0.5116(6) 0.2944(5) 0.094(4) Uani 1 1 d . . . H34 H 0.4342 0.5375 0.3249 0.112 Uiso 1 1 calc R . . C35 C 0.3668(8) 0.4599(8) 0.2988(6) 0.115(5) Uani 1 1 d . . . H35 H 0.3611 0.4497 0.3306 0.137 Uiso 1 1 calc R . . C36 C 0.3304(5) 0.4240(6) 0.2543(6) 0.097(5) Uani 1 1 d . . . N37 N 0.3474(6) 0.4377(6) 0.2092(5) 0.129(5) Uani 1 1 d . . . C38 C 0.3953(6) 0.4918(6) 0.2135(5) 0.090(4) Uani 1 1 d . . . H38 H 0.4052 0.5025 0.1834 0.109 Uiso 1 1 calc R . . C39 C 0.2440(14) 0.3266(14) 0.1706(8) 0.265(16) Uani 1 1 d . . . C40 C 0.4767(5) 0.9090(5) 0.1190(4) 0.066(3) Uani 1 1 d . . . C41 C 0.2409(6) 1.1495(6) 0.0565(4) 0.082(3) Uani 1 1 d . . . C42 C -0.0872(5) 0.1269(4) 0.1280(4) 0.061(2) Uani 1 1 d . . . O1S O 0.0901(10) 0.0801(10) 0.0915(8) 0.231(7) Uiso 1 1 d . . . C11S C 0.029(3) 0.148(3) 0.050(2) 0.09(2) Uiso 0.24(3) 1 d P . . C12S C 0.0457(17) 0.0721(18) 0.0436(13) 0.197(15) Uiso 0.76(3) 1 d P . . O2S O 0.0000 0.6981(17) 0.2500 0.249(11) Uiso 1 2 d S . . C21S C 0.055(3) 0.742(3) 0.263(2) 0.108(17) Uiso 0.25 1 d P . . C22S C 0.0000 0.770(5) 0.2500 0.24(3) Uiso 0.50 2 d SP . . O3S O 0.399(2) 0.3952(19) 0.0913(13) 0.397(16) Uiso 1 1 d . . . C31S C 0.452(3) 0.356(3) 0.134(2) 0.20(3) Uiso 0.53(8) 1 d P . . C32S C 0.471(3) 0.395(3) 0.108(2) 0.19(3) Uiso 0.47(8) 1 d P . . 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 0.0454(6) 0.0497(6) 0.0339(6) -0.0008(5) 0.0182(5) -0.0126(5) Co2 0.0378(8) 0.0367(8) 0.0515(10) 0.000 0.0138(7) 0.000 S1 0.117(3) 0.079(2) 0.316(8) 0.000(3) 0.004(4) 0.037(2) S2 0.242(6) 0.170(5) 0.173(5) -0.001(4) 0.039(4) 0.129(5) S3 0.128(3) 0.150(3) 0.064(2) 0.017(2) -0.011(2) -0.001(3) N1 0.044(4) 0.055(4) 0.042(4) 0.003(3) 0.026(3) -0.014(3) N2 0.050(4) 0.066(4) 0.039(4) 0.003(3) 0.016(3) -0.007(3) N3 0.075(5) 0.063(4) 0.031(4) -0.002(3) 0.022(4) -0.020(4) N4 0.052(4) 0.084(5) 0.033(4) 0.006(3) 0.019(4) 0.025(4) N5 0.052(4) 0.068(5) 0.064(5) -0.006(4) 0.020(4) -0.019(4) N6 0.052(4) 0.057(4) 0.068(5) 0.002(4) 0.028(4) -0.015(4) N7 0.048(4) 0.047(4) 0.068(5) 0.007(4) 0.009(4) -0.005(3) N8 0.045(4) 0.052(4) 0.065(5) 0.001(4) 0.028(4) 0.002(3) N9 0.057(4) 0.055(4) 0.057(5) 0.007(4) 0.014(4) -0.001(3) C1 0.066(6) 0.059(5) 0.082(7) -0.009(5) 0.040(5) -0.013(5) C2 0.052(5) 0.063(6) 0.099(8) 0.009(5) 0.043(5) -0.011(5) C3 0.050(5) 0.058(5) 0.062(6) 0.007(4) 0.018(4) -0.020(4) C4 0.069(6) 0.052(5) 0.072(7) -0.012(4) 0.033(5) -0.017(4) C5 0.065(6) 0.051(5) 0.064(6) -0.013(4) 0.020(5) -0.011(4) C6 0.054(6) 0.084(7) 0.085(8) 0.006(6) 0.015(6) -0.012(5) C7 0.075(7) 0.070(6) 0.096(9) 0.002(6) 0.039(6) -0.024(5) C8 0.083(7) 0.067(6) 0.063(7) 0.003(5) 0.017(6) -0.026(5) C9 0.048(5) 0.071(6) 0.061(6) 0.012(5) -0.001(4) -0.035(5) C10 0.048(5) 0.065(6) 0.073(7) 0.018(5) 0.001(5) -0.026(4) N11 0.105(8) 0.126(9) 0.159(12) 0.071(8) 0.040(8) -0.028(7) C12 0.056(6) 0.077(6) 0.101(9) 0.023(6) 0.020(6) -0.019(5) C13 0.093(8) 0.078(7) 0.088(8) -0.028(6) 0.044(7) -0.041(6) C14 0.145(11) 0.107(8) 0.064(8) -0.020(6) 0.055(8) 0.013(8) C15 0.132(12) 0.225(17) 0.046(7) -0.019(9) 0.058(8) 0.014(11) C16 0.146(12) 0.207(16) 0.028(6) -0.036(8) 0.044(7) -0.128(12) C17 0.184(15) 0.148(12) 0.034(6) 0.009(7) 0.044(8) -0.063(11) C18 0.116(10) 0.114(9) 0.048(7) 0.005(6) 0.032(6) -0.012(7) C19 0.055(7) 0.074(8) 0.217(19) -0.020(9) -0.011(9) 0.015(7) C20 0.070(9) 0.073(8) 0.35(3) 0.024(12) 0.041(13) 0.025(7) C21 0.048(5) 0.115(8) 0.048(6) 0.006(5) 0.016(5) 0.002(5) C22 0.083(7) 0.107(8) 0.049(6) -0.012(6) 0.043(6) -0.014(6) C23 0.161(13) 0.129(10) 0.059(8) -0.029(7) 0.085(9) -0.049(10) N24 0.130(10) 0.223(14) 0.056(7) -0.005(8) 0.015(7) -0.051(10) C25 0.070(7) 0.106(7) 0.041(6) -0.001(5) 0.024(5) -0.011(6) C26 0.093(8) 0.098(7) 0.051(6) 0.016(5) 0.035(6) 0.038(6) C27 0.093(8) 0.064(6) 0.098(9) 0.018(6) -0.004(7) -0.029(6) C28 0.083(9) 0.052(6) 0.178(16) 0.008(8) -0.034(9) -0.038(7) C29 0.053(7) 0.075(9) 0.27(2) 0.076(12) 0.033(10) -0.028(7) C30 0.044(6) 0.068(7) 0.243(18) 0.050(9) 0.069(8) -0.007(6) C31 0.068(7) 0.064(6) 0.144(12) 0.032(6) 0.053(7) 0.009(5) C32 0.27(2) 0.117(12) 0.125(15) 0.011(11) 0.129(17) 0.045(14) C33 0.32(3) 0.188(19) 0.066(11) -0.004(11) 0.013(14) 0.17(2) C34 0.110(9) 0.081(7) 0.111(10) -0.002(7) 0.066(8) -0.025(7) C35 0.130(12) 0.122(10) 0.110(11) -0.003(9) 0.064(10) -0.059(9) C36 0.054(6) 0.093(8) 0.155(13) 0.069(9) 0.048(8) -0.017(6) N37 0.097(8) 0.132(9) 0.130(10) 0.028(8) 0.003(7) -0.064(7) C38 0.092(8) 0.084(7) 0.085(9) 0.001(6) 0.017(7) -0.046(7) C39 0.34(3) 0.36(3) 0.189(19) -0.19(2) 0.21(2) -0.29(3) C40 0.053(5) 0.042(5) 0.087(8) 0.002(5) 0.005(5) 0.002(4) C41 0.065(7) 0.083(7) 0.080(8) 0.010(6) 0.003(6) -0.004(6) C42 0.073(6) 0.055(5) 0.057(6) 0.003(4) 0.024(6) 0.000(5) _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 N6 2.021(8) . ? Co1 N5 2.065(9) . ? Co1 N2 2.181(7) 3 ? Co1 N4 2.195(7) 6_575 ? Co1 N1 2.195(6) . ? Co1 N3 2.219(6) . ? Co2 N9 2.065(8) . ? Co2 N9 2.065(8) 2 ? Co2 N7 2.155(7) . ? Co2 N7 2.155(7) 2 ? Co2 N8 2.181(7) 3_445 ? Co2 N8 2.181(7) 4_545 ? S1 C40 1.587(10) . ? S2 C41 1.648(12) . ? S3 C42 1.617(11) . ? N1 C5 1.346(10) . ? N1 C1 1.346(10) . ? N2 C8 1.329(12) . ? N2 C12 1.331(11) . ? N2 Co1 2.181(7) 3_445 ? N3 C18 1.359(13) . ? N3 C14 1.368(13) . ? N4 C25 1.315(11) . ? N4 C21 1.343(11) . ? N4 Co1 2.195(7) 6_576 ? N5 C40 1.139(11) . ? N6 C41 1.155(12) . ? N7 C27 1.299(13) . ? N7 C31 1.324(13) . ? N8 C34 1.285(12) . ? N8 C38 1.307(12) . ? N8 Co2 2.181(7) 3 ? N9 C42 1.148(11) . ? C1 C2 1.381(12) . ? C2 C3 1.373(12) . ? C3 C4 1.395(12) . ? C3 C6 1.504(12) . ? C4 C5 1.384(11) . ? C6 C7 1.243(13) . ? C6 C13 1.556(14) . ? C7 C10 1.491(12) . ? C8 C9 1.345(12) . ? C9 C10 1.332(12) . ? C10 N11 1.321(14) . ? N11 C12 1.414(13) . ? C14 C15 1.351(14) . ? C15 C16 1.41(2) . ? C16 C17 1.41(2) . ? C16 C19 1.92(2) . ? C17 C18 1.354(15) . ? C19 C20 1.009(15) . ? C19 C26 1.471(15) . ? C20 C23 1.79(2) . ? C21 C22 1.297(12) . ? C22 C23 1.384(17) . ? C23 N24 1.367(16) . ? N24 C25 1.403(13) . ? C27 C28 1.391(17) . ? C28 C29 1.39(2) . ? C29 C30 1.28(2) . ? C29 C32 1.76(2) . ? C29 C33 2.01(3) . ? C30 C31 1.374(13) . ? C32 C33 1.05(2) . ? C32 C39 1.45(2) . ? C33 C36 1.87(3) . ? C34 C35 1.355(15) . ? C35 C36 1.356(18) . ? C36 N37 1.405(16) . ? N37 C38 1.370(13) . ? O1S C12S 1.31(3) . ? O1S C11S 1.86(6) . ? C11S C12S 1.49(6) . ? O2S C21S 1.31(6) 2 ? O2S C21S 1.31(6) . ? O2S C22S 1.35(9) . ? C21S C22S 1.15(7) . ? C22S C21S 1.15(7) 2 ? O3S C32S 1.35(6) . ? O3S C31S 1.47(6) . ? C31S C32S 1.17(6) . ? 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 N6 Co1 N5 176.2(3) . . ? N6 Co1 N2 88.8(3) . 3 ? N5 Co1 N2 87.6(3) . 3 ? N6 Co1 N4 90.6(3) . 6_575 ? N5 Co1 N4 88.4(3) . 6_575 ? N2 Co1 N4 90.0(2) 3 6_575 ? N6 Co1 N1 92.8(3) . . ? N5 Co1 N1 90.8(3) . . ? N2 Co1 N1 177.5(2) 3 . ? N4 Co1 N1 88.1(2) 6_575 . ? N6 Co1 N3 91.1(3) . . ? N5 Co1 N3 90.3(3) . . ? N2 Co1 N3 94.8(2) 3 . ? N4 Co1 N3 174.9(2) 6_575 . ? N1 Co1 N3 87.1(2) . . ? N9 Co2 N9 177.2(4) . 2 ? N9 Co2 N7 90.7(3) . . ? N9 Co2 N7 87.4(3) 2 . ? N9 Co2 N7 87.4(3) . 2 ? N9 Co2 N7 90.7(3) 2 2 ? N7 Co2 N7 92.0(4) . 2 ? N9 Co2 N8 90.9(3) . 3_445 ? N9 Co2 N8 91.1(3) 2 3_445 ? N7 Co2 N8 176.2(2) . 3_445 ? N7 Co2 N8 91.5(3) 2 3_445 ? N9 Co2 N8 91.1(3) . 4_545 ? N9 Co2 N8 90.9(3) 2 4_545 ? N7 Co2 N8 91.5(3) . 4_545 ? N7 Co2 N8 176.2(2) 2 4_545 ? N8 Co2 N8 85.0(3) 3_445 4_545 ? C5 N1 C1 116.0(7) . . ? C5 N1 Co1 123.3(5) . . ? C1 N1 Co1 120.7(6) . . ? C8 N2 C12 114.0(8) . . ? C8 N2 Co1 123.8(6) . 3_445 ? C12 N2 Co1 122.1(6) . 3_445 ? C18 N3 C14 117.4(9) . . ? C18 N3 Co1 119.2(7) . . ? C14 N3 Co1 122.2(7) . . ? C25 N4 C21 115.9(7) . . ? C25 N4 Co1 121.0(6) . 6_576 ? C21 N4 Co1 123.1(6) . 6_576 ? C40 N5 Co1 163.1(7) . . ? C41 N6 Co1 162.1(8) . . ? C27 N7 C31 113.5(10) . . ? C27 N7 Co2 126.5(8) . . ? C31 N7 Co2 119.8(7) . . ? C34 N8 C38 111.4(9) . . ? C34 N8 Co2 128.1(7) . 3 ? C38 N8 Co2 120.5(7) . 3 ? C42 N9 Co2 162.1(8) . . ? N1 C1 C2 122.1(8) . . ? C3 C2 C1 122.9(8) . . ? C2 C3 C4 114.6(7) . . ? C2 C3 C6 123.5(8) . . ? C4 C3 C6 121.8(8) . . ? C5 C4 C3 120.5(8) . . ? N1 C5 C4 123.8(8) . . ? C7 C6 C3 119.2(10) . . ? C7 C6 C13 125.2(10) . . ? C3 C6 C13 115.6(9) . . ? C6 C7 C10 125.6(11) . . ? N2 C8 C9 127.1(9) . . ? C10 C9 C8 117.9(9) . . ? N11 C10 C9 119.2(8) . . ? N11 C10 C7 121.5(9) . . ? C9 C10 C7 119.3(9) . . ? C10 N11 C12 120.2(10) . . ? N2 C12 N11 121.2(10) . . ? C15 C14 N3 121.7(13) . . ? C14 C15 C16 121.3(14) . . ? C15 C16 C17 116.7(10) . . ? C15 C16 C19 109.8(14) . . ? C17 C16 C19 133.5(13) . . ? C18 C17 C16 118.9(14) . . ? C17 C18 N3 124.0(13) . . ? C20 C19 C26 165(2) . . ? C20 C19 C16 83.1(19) . . ? C26 C19 C16 112.1(13) . . ? C19 C20 C23 91.8(19) . . ? C22 C21 N4 127.6(10) . . ? C21 C22 C23 116.8(10) . . ? N24 C23 C22 119.5(10) . . ? N24 C23 C20 131.4(13) . . ? C22 C23 C20 108.3(11) . . ? C23 N24 C25 118.1(11) . . ? N4 C25 N24 122.0(10) . . ? N7 C27 C28 123.8(14) . . ? C29 C28 C27 120.3(14) . . ? C30 C29 C28 115.2(11) . . ? C30 C29 C32 112.6(18) . . ? C28 C29 C32 132.2(18) . . ? C30 C29 C33 143.1(16) . . ? C28 C29 C33 101.4(16) . . ? C32 C29 C33 31.7(7) . . ? C29 C30 C31 122.3(15) . . ? N7 C31 C30 124.9(13) . . ? C33 C32 C39 161(3) . . ? C33 C32 C29 87(2) . . ? C39 C32 C29 111.5(17) . . ? C32 C33 C36 96(2) . . ? C32 C33 C29 61(2) . . ? C36 C33 C29 156.9(13) . . ? N8 C34 C35 130.1(13) . . ? C34 C35 C36 116.4(12) . . ? C35 C36 N37 118.2(10) . . ? C35 C36 C33 113.6(11) . . ? N37 C36 C33 128.2(13) . . ? C38 N37 C36 115.6(11) . . ? N8 C38 N37 128.1(11) . . ? N5 C40 S1 178.8(11) . . ? N6 C41 S2 176.2(11) . . ? N9 C42 S3 179.7(10) . . ? C12S O1S C11S 53(2) . . ? C12S C11S O1S 44.3(19) . . ? O1S C12S C11S 83(3) . . ? C21S O2S C21S 103(5) 2 . ? C21S O2S C22S 51(3) 2 . ? C21S O2S C22S 51(3) . . ? C22S C21S O2S 66(5) . . ? C21S C22S C21S 125(10) 2 . ? C21S C22S O2S 62(5) 2 . ? C21S C22S O2S 62(5) . . ? C32S O3S C31S 49(3) . . ? C32S C31S O3S 60(4) . . ? C31S C32S O3S 71(5) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.990 _refine_diff_density_min -0.563 _refine_diff_density_rms 0.144