Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Samiran Mitra' _publ_contact_author_address ; Department of Chemistry Jadavpur University Kolkata 700 032 INDIA ; _publ_contact_author_email 'SMITRA_2002@YAHOO.COM' _publ_section_title ; Ligating properties of a potentially tetradentate Schiff base [(CH3)2NCH2CH2N=CHC6H3(OH)(OMe)] with zinc(II), cadmium(II), cobalt(II), cobalt(III) and manganese(III) ions: Synthesis and structural studies ; _publ_requested_category FM loop_ _publ_author_name 'Samiran Mitra' 'Subrata Kumar Dey' 'Volker Gramlich' 'David L. Hughes' 'Takayuki Matsushita' 'Guillaume Pilet' ; G.Rosair ; 'Soma Sen' 'Pritha Talukder' 'Glenn P. A. Yap' data_samm003 _database_code_depnum_ccdc_archive 'CCDC 281764' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 1' _chemical_melting_point ? _chemical_formula_moiety 'C25 H36 N5 O4 S1 ZN1, C17 H20 N5 O4 S3 Zn2' _chemical_formula_structural '[Zn(LH)2(NCS)][Zn2(L)(MeCOO)(NCS)3]' _chemical_formula_sum 'C42 H56 N10 O8 S4 Zn3' _chemical_formula_weight 1153.32 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' Zn Zn 0.2839 1.4301 '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' _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 10.5391(16) _cell_length_b 14.630(2) _cell_length_c 17.946(3) _cell_angle_alpha 101.851(2) _cell_angle_beta 94.654(3) _cell_angle_gamma 104.704(2) _cell_volume 2593.2(7) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 1001 _cell_measurement_theta_min 2.92 _cell_measurement_theta_max 28.12 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.477 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1192 _exptl_absorpt_coefficient_mu 1.595 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7622 _exptl_absorpt_correction_T_max 0.8568 _exptl_absorpt_process_details 'SADABS, Bruker (2000)' _exptl_special_details ; Data collection is performed with three batch runs at phi = 0.00 deg (606 frames), at phi = 90.00 deg (600 frames), and at phi = 180 deg (600 frames) A fourth batch run is collected at phi = 0.00 deg (50 frames) to monitor crystal and diffractometer stability. Frame width = 0.30 deg in omega. Data is merged, corrected for decay (if any), and treated with multi-scan absorption corrections (if required). All symmetry-equivalent reflections are merged for centrosymmetric data. Friedel pairs are not merged for noncentrosymmetric data. ; _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 '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_% <1 _diffrn_reflns_number 26646 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0279 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 28.27 _reflns_number_total 11584 _reflns_number_gt 10690 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART, Bruker (2000)' _computing_cell_refinement 'SMART, Bruker (2000)' _computing_data_reduction 'XPREP, Bruker (2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL, Bruker (2000)' _computing_publication_material 'SHELXTL, Bruker (2000)' _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^)+(0.0600P)^2^+1.5665P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11584 _refine_ls_number_parameters 620 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0415 _refine_ls_R_factor_gt 0.0379 _refine_ls_wR_factor_ref 0.1031 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.42433(2) 0.190133(18) 0.411941(15) 0.01789(7) Uani 1 1 d . . . Zn2 Zn 0.18098(3) 0.556626(19) 0.172950(15) 0.02060(7) Uani 1 1 d . . . Zn3 Zn 0.32951(3) 0.723687(19) 0.072387(15) 0.02018(7) Uani 1 1 d . . . N1 N 0.49168(18) 0.06823(14) 0.36766(11) 0.0200(4) Uani 1 1 d . . . N2 N 0.4336(2) 0.09070(14) 0.20610(11) 0.0207(4) Uani 1 1 d . . . H1 H 0.377(3) 0.099(2) 0.2338(17) 0.025 Uiso 1 1 d . . . N3 N 0.3413(2) 0.30290(14) 0.45580(12) 0.0244(4) Uani 1 1 d . . . N4 N 0.3699(2) 0.27374(15) 0.61479(12) 0.0246(4) Uani 1 1 d . . . H2 H 0.343(3) 0.219(2) 0.5797(18) 0.030 Uiso 1 1 d . . . N5 N 0.6045(2) 0.28570(15) 0.42159(13) 0.0277(4) Uani 1 1 d . . . N6 N 0.0327(2) 0.44300(16) 0.10332(13) 0.0265(4) Uani 1 1 d . . . N7 N 0.0567(2) 0.51765(16) 0.26114(12) 0.0273(4) Uani 1 1 d . . . N8 N 0.3101(2) 0.79311(16) -0.00932(12) 0.0280(4) Uani 1 1 d . . . N9 N 0.5007(2) 0.78261(15) 0.13761(13) 0.0278(4) Uani 1 1 d . . . N10 N 0.3326(2) 0.50828(15) 0.20481(12) 0.0259(4) Uani 1 1 d . . . O1 O 0.35713(16) 0.12605(11) 0.49577(9) 0.0211(3) Uani 1 1 d . . . O2 O 0.17340(17) 0.06746(13) 0.57975(10) 0.0293(4) Uani 1 1 d . . . O3 O 0.29742(16) 0.15442(12) 0.31581(9) 0.0231(3) Uani 1 1 d . . . O4 O 0.13819(17) 0.05850(14) 0.18865(10) 0.0308(4) Uani 1 1 d . . . O5 O 0.23318(16) 0.58773(11) 0.06951(9) 0.0214(3) Uani 1 1 d . . . O6 O 0.42892(17) 0.62571(12) -0.00769(10) 0.0259(4) Uani 1 1 d . . . O7 O 0.19837(17) 0.77810(12) 0.13198(10) 0.0269(4) Uani 1 1 d . . . O8 O 0.20510(18) 0.69607(12) 0.22397(10) 0.0262(4) Uani 1 1 d . . . S1 S 0.83200(6) 0.44156(5) 0.44788(4) 0.03284(15) Uani 1 1 d . . . S2 S 0.49700(10) 0.42096(6) 0.27744(4) 0.0485(2) Uani 1 1 d . . . S3 S 0.76093(7) 0.88988(5) 0.19474(4) 0.03368(15) Uani 1 1 d . . . S5 S 0.29464(7) 0.96064(5) -0.05612(4) 0.03084(14) Uani 1 1 d . . . C1 C 0.3097(2) 0.03153(16) 0.48733(12) 0.0178(4) Uani 1 1 d . . . C2 C 0.2120(2) -0.00382(17) 0.53235(13) 0.0221(5) Uani 1 1 d . . . C3 C 0.1602(2) -0.10213(19) 0.52656(15) 0.0281(5) Uani 1 1 d . . . H3A H 0.0941 -0.1237 0.5569 0.034 Uiso 1 1 calc R . . C4 C 0.2044(3) -0.16976(18) 0.47653(17) 0.0323(6) Uani 1 1 d . . . H4A H 0.1698 -0.2373 0.4734 0.039 Uiso 1 1 calc R . . C5 C 0.2980(3) -0.13831(18) 0.43193(16) 0.0294(5) Uani 1 1 d . . . H5A H 0.3281 -0.1846 0.3979 0.035 Uiso 1 1 calc R . . C6 C 0.3508(2) -0.03828(16) 0.43553(14) 0.0215(4) Uani 1 1 d . . . C7 C 0.4470(2) -0.01383(17) 0.38391(14) 0.0240(5) Uani 1 1 d . . . H7A H 0.4806 -0.0650 0.3595 0.029 Uiso 1 1 calc R . . C8 C 0.0609(3) 0.0347(2) 0.61755(17) 0.0366(6) Uani 1 1 d . . . H8A H 0.0365 0.0911 0.6459 0.055 Uiso 1 1 calc R . . H8B H 0.0835 -0.0028 0.6535 0.055 Uiso 1 1 calc R . . H8C H -0.0139 -0.0064 0.5791 0.055 Uiso 1 1 calc R . . C9 C 0.5915(2) 0.0742(2) 0.31447(14) 0.0265(5) Uani 1 1 d . . . H9A H 0.5914 0.0076 0.2885 0.032 Uiso 1 1 calc R . . H9B H 0.6803 0.1071 0.3444 0.032 Uiso 1 1 calc R . . C10 C 0.5660(2) 0.12980(19) 0.25300(15) 0.0276(5) Uani 1 1 d . . . H10A H 0.5770 0.1985 0.2790 0.033 Uiso 1 1 calc R . . H10B H 0.6341 0.1288 0.2182 0.033 Uiso 1 1 calc R . . C11 C 0.4221(3) 0.15021(19) 0.14862(15) 0.0297(5) Uani 1 1 d . . . H11A H 0.3350 0.1237 0.1169 0.044 Uiso 1 1 calc R . . H11B H 0.4915 0.1483 0.1157 0.044 Uiso 1 1 calc R . . H11C H 0.4321 0.2176 0.1756 0.044 Uiso 1 1 calc R . . C12 C 0.4029(3) -0.01362(18) 0.16741(16) 0.0307(5) Uani 1 1 d . . . H12A H 0.4067 -0.0517 0.2061 0.046 Uiso 1 1 calc R . . H12B H 0.4679 -0.0231 0.1326 0.046 Uiso 1 1 calc R . . H12C H 0.3139 -0.0351 0.1379 0.046 Uiso 1 1 calc R . . C13 C 0.1817(2) 0.17275(17) 0.30736(14) 0.0223(5) Uani 1 1 d . . . C14 C 0.0908(2) 0.12169(18) 0.23932(14) 0.0249(5) Uani 1 1 d . . . C15 C -0.0329(2) 0.13602(19) 0.22728(17) 0.0315(6) Uani 1 1 d . . . H15A H -0.0919 0.1008 0.1817 0.038 Uiso 1 1 calc R . . C16 C -0.0713(3) 0.2029(2) 0.28267(19) 0.0362(6) Uani 1 1 d . . . H16A H -0.1572 0.2118 0.2750 0.043 Uiso 1 1 calc R . . C17 C 0.0139(3) 0.25500(19) 0.34716(17) 0.0306(6) Uani 1 1 d . . . H17A H -0.0125 0.3010 0.3837 0.037 Uiso 1 1 calc R . . C18 C 0.1414(2) 0.24158(18) 0.36061(15) 0.0244(5) Uani 1 1 d . . . C19 C 0.2273(3) 0.30679(18) 0.42775(15) 0.0273(5) Uani 1 1 d . . . H19A H 0.1959 0.3582 0.4540 0.033 Uiso 1 1 calc R . . C20 C 0.0595(3) 0.0158(3) 0.11436(17) 0.0427(7) Uani 1 1 d . . . H20A H 0.1034 -0.0265 0.0829 0.064 Uiso 1 1 calc R . . H20B H 0.0498 0.0674 0.0890 0.064 Uiso 1 1 calc R . . H20C H -0.0281 -0.0225 0.1206 0.064 Uiso 1 1 calc R . . C21 C 0.4143(3) 0.38238(17) 0.52116(15) 0.0294(5) Uani 1 1 d . . . H21A H 0.3541 0.4207 0.5411 0.035 Uiso 1 1 calc R . . H21B H 0.4876 0.4261 0.5034 0.035 Uiso 1 1 calc R . . C22 C 0.4707(3) 0.34486(17) 0.58538(14) 0.0259(5) Uani 1 1 d . . . H22A H 0.5386 0.3134 0.5666 0.031 Uiso 1 1 calc R . . H22B H 0.5155 0.4009 0.6286 0.031 Uiso 1 1 calc R . . C23 C 0.4333(3) 0.2529(2) 0.68419(15) 0.0319(6) Uani 1 1 d . . . H23A H 0.3733 0.1975 0.6976 0.048 Uiso 1 1 calc R . . H23B H 0.4523 0.3100 0.7272 0.048 Uiso 1 1 calc R . . H23C H 0.5162 0.2374 0.6734 0.048 Uiso 1 1 calc R . . C24 C 0.2518(3) 0.3075(2) 0.63312(17) 0.0358(6) Uani 1 1 d . . . H24A H 0.1963 0.2629 0.6592 0.054 Uiso 1 1 calc R . . H24B H 0.2006 0.3088 0.5854 0.054 Uiso 1 1 calc R . . H24C H 0.2805 0.3729 0.6668 0.054 Uiso 1 1 calc R . . C25 C 0.6985(2) 0.35091(17) 0.43197(13) 0.0212(4) Uani 1 1 d . . . C26 C 0.2408(2) 0.51635(16) 0.01176(13) 0.0209(4) Uani 1 1 d . . . C27 C 0.1481(2) 0.42375(17) -0.00772(14) 0.0238(5) Uani 1 1 d . . . C28 C 0.1603(3) 0.35379(19) -0.07197(15) 0.0294(5) Uani 1 1 d . . . H28A H 0.0970 0.2918 -0.0859 0.035 Uiso 1 1 calc R . . C29 C 0.2623(3) 0.37379(19) -0.11458(15) 0.0312(6) Uani 1 1 d . . . H29A H 0.2689 0.3258 -0.1575 0.037 Uiso 1 1 calc R . . C30 C 0.3560(3) 0.46448(18) -0.09485(14) 0.0274(5) Uani 1 1 d . . . H30A H 0.4271 0.4783 -0.1238 0.033 Uiso 1 1 calc R . . C31 C 0.3445(2) 0.53366(17) -0.03296(14) 0.0229(5) Uani 1 1 d . . . C32 C 0.0412(2) 0.39531(18) 0.03652(15) 0.0271(5) Uani 1 1 d . . . H32A H -0.0270 0.3372 0.0143 0.033 Uiso 1 1 calc R . . C33 C 0.5354(3) 0.65533(19) -0.05008(16) 0.0292(5) Uani 1 1 d . . . H33A H 0.5950 0.6138 -0.0488 0.044 Uiso 1 1 calc R . . H33B H 0.5847 0.7231 -0.0269 0.044 Uiso 1 1 calc R . . H33C H 0.4994 0.6493 -0.1035 0.044 Uiso 1 1 calc R . . C34 C -0.0763(3) 0.4036(2) 0.14368(17) 0.0366(6) Uani 1 1 d . . . H34A H -0.1178 0.3339 0.1194 0.044 Uiso 1 1 calc R . . H34B H -0.1447 0.4388 0.1412 0.044 Uiso 1 1 calc R . . C35 C -0.0194(3) 0.41587(19) 0.22706(16) 0.0310(6) Uani 1 1 d . . . H35A H -0.0925 0.3965 0.2570 0.037 Uiso 1 1 calc R . . H35B H 0.0390 0.3729 0.2295 0.037 Uiso 1 1 calc R . . C36 C 0.1361(3) 0.5238(2) 0.33467(16) 0.0380(6) Uani 1 1 d . . . H36A H 0.0767 0.5040 0.3713 0.057 Uiso 1 1 calc R . . H36B H 0.1905 0.5909 0.3556 0.057 Uiso 1 1 calc R . . H36C H 0.1937 0.4807 0.3259 0.057 Uiso 1 1 calc R . . C37 C -0.0341(3) 0.5790(2) 0.27797(19) 0.0411(7) Uani 1 1 d . . . H37A H -0.0989 0.5504 0.3088 0.062 Uiso 1 1 calc R . . H37B H -0.0804 0.5829 0.2296 0.062 Uiso 1 1 calc R . . H37C H 0.0168 0.6444 0.3066 0.062 Uiso 1 1 calc R . . C38 C 0.3995(3) 0.47039(17) 0.23420(14) 0.0256(5) Uani 1 1 d . . . C39 C 0.6095(2) 0.82752(17) 0.15990(13) 0.0231(5) Uani 1 1 d . . . C40 C 0.3034(2) 0.86312(18) -0.02818(13) 0.0223(5) Uani 1 1 d . . . C41 C 0.1758(2) 0.76255(17) 0.19665(14) 0.0234(5) Uani 1 1 d . . . C42 C 0.1085(3) 0.8283(2) 0.24493(16) 0.0319(6) Uani 1 1 d . . . H42A H 0.1434 0.8950 0.2394 0.048 Uiso 1 1 calc R . . H42B H 0.1258 0.8265 0.2990 0.048 Uiso 1 1 calc R . . H42C H 0.0128 0.8061 0.2277 0.048 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 Zn1 0.01970(13) 0.01721(13) 0.01712(13) 0.00459(10) 0.00324(10) 0.00508(10) Zn2 0.02214(14) 0.02086(13) 0.02038(14) 0.00645(10) 0.00486(10) 0.00688(10) Zn3 0.02279(14) 0.01846(13) 0.02001(14) 0.00464(10) 0.00447(10) 0.00642(10) N1 0.0178(9) 0.0245(10) 0.0187(9) 0.0042(8) 0.0029(7) 0.0082(7) N2 0.0233(10) 0.0203(9) 0.0186(10) 0.0047(8) 0.0076(8) 0.0048(7) N3 0.0352(11) 0.0180(9) 0.0227(10) 0.0067(8) 0.0064(8) 0.0099(8) N4 0.0322(11) 0.0202(10) 0.0210(10) 0.0015(8) 0.0073(8) 0.0080(8) N5 0.0256(10) 0.0252(10) 0.0296(11) 0.0067(9) 0.0018(8) 0.0027(8) N6 0.0214(10) 0.0297(11) 0.0296(11) 0.0120(9) 0.0022(8) 0.0053(8) N7 0.0294(11) 0.0318(11) 0.0259(11) 0.0121(9) 0.0078(8) 0.0121(9) N8 0.0342(11) 0.0294(11) 0.0235(11) 0.0084(9) 0.0054(9) 0.0121(9) N9 0.0276(11) 0.0264(10) 0.0273(11) 0.0018(9) -0.0012(8) 0.0088(9) N10 0.0253(10) 0.0274(10) 0.0266(11) 0.0068(9) 0.0043(8) 0.0099(8) O1 0.0288(8) 0.0156(7) 0.0194(8) 0.0034(6) 0.0080(6) 0.0061(6) O2 0.0307(9) 0.0325(9) 0.0264(9) 0.0089(8) 0.0131(7) 0.0073(7) O3 0.0220(8) 0.0292(9) 0.0195(8) 0.0034(7) 0.0020(6) 0.0115(7) O4 0.0237(8) 0.0395(10) 0.0234(9) 0.0023(8) -0.0023(7) 0.0043(7) O5 0.0263(8) 0.0177(7) 0.0199(8) 0.0031(6) 0.0061(6) 0.0057(6) O6 0.0290(9) 0.0228(8) 0.0265(9) 0.0048(7) 0.0113(7) 0.0066(7) O7 0.0341(9) 0.0250(9) 0.0281(9) 0.0091(7) 0.0130(7) 0.0144(7) O8 0.0375(10) 0.0221(8) 0.0218(8) 0.0046(7) 0.0084(7) 0.0125(7) S1 0.0252(3) 0.0250(3) 0.0426(4) 0.0019(3) 0.0098(3) 0.0002(2) S2 0.0790(6) 0.0394(4) 0.0310(4) -0.0040(3) -0.0137(4) 0.0399(4) S3 0.0290(3) 0.0297(3) 0.0364(4) 0.0066(3) 0.0015(3) -0.0005(3) S5 0.0331(3) 0.0339(3) 0.0310(3) 0.0159(3) 0.0032(3) 0.0128(3) C1 0.0195(10) 0.0188(10) 0.0162(10) 0.0060(8) 0.0022(8) 0.0055(8) C2 0.0223(11) 0.0253(11) 0.0187(11) 0.0074(9) -0.0008(8) 0.0059(9) C3 0.0231(11) 0.0317(13) 0.0290(13) 0.0145(11) 0.0000(10) 0.0019(10) C4 0.0350(14) 0.0206(12) 0.0410(15) 0.0133(11) 0.0005(11) 0.0040(10) C5 0.0317(13) 0.0195(11) 0.0378(15) 0.0057(10) 0.0058(11) 0.0089(10) C6 0.0228(11) 0.0170(10) 0.0246(12) 0.0048(9) 0.0004(9) 0.0066(8) C7 0.0243(11) 0.0221(11) 0.0256(12) 0.0011(9) 0.0019(9) 0.0109(9) C8 0.0278(13) 0.0538(18) 0.0293(14) 0.0116(13) 0.0126(11) 0.0092(12) C9 0.0215(11) 0.0366(13) 0.0230(12) 0.0064(10) 0.0061(9) 0.0103(10) C10 0.0246(12) 0.0317(13) 0.0234(12) 0.0047(10) 0.0049(9) 0.0033(10) C11 0.0350(13) 0.0292(13) 0.0268(13) 0.0104(11) 0.0069(10) 0.0088(10) C12 0.0371(14) 0.0218(12) 0.0302(14) 0.0021(10) 0.0060(11) 0.0054(10) C13 0.0209(10) 0.0247(11) 0.0259(12) 0.0144(10) 0.0055(9) 0.0070(9) C14 0.0221(11) 0.0265(12) 0.0271(12) 0.0123(10) 0.0033(9) 0.0036(9) C15 0.0195(11) 0.0310(13) 0.0437(16) 0.0201(12) -0.0014(10) -0.0006(10) C16 0.0196(12) 0.0361(14) 0.061(2) 0.0256(14) 0.0083(12) 0.0100(10) C17 0.0280(13) 0.0284(13) 0.0445(16) 0.0178(12) 0.0130(11) 0.0142(10) C18 0.0249(11) 0.0261(12) 0.0299(13) 0.0158(10) 0.0091(9) 0.0118(9) C19 0.0389(14) 0.0225(11) 0.0295(13) 0.0125(10) 0.0134(11) 0.0167(10) C20 0.0245(13) 0.063(2) 0.0275(14) 0.0009(14) -0.0018(11) -0.0017(13) C21 0.0435(15) 0.0166(11) 0.0284(13) 0.0034(10) 0.0069(11) 0.0100(10) C22 0.0327(13) 0.0200(11) 0.0225(12) 0.0011(9) 0.0066(10) 0.0050(9) C23 0.0443(15) 0.0302(13) 0.0227(13) 0.0069(10) 0.0057(11) 0.0120(11) C24 0.0355(14) 0.0391(15) 0.0355(15) 0.0043(12) 0.0120(12) 0.0164(12) C25 0.0240(11) 0.0228(11) 0.0181(11) 0.0035(9) 0.0060(8) 0.0086(9) C26 0.0244(11) 0.0209(11) 0.0202(11) 0.0056(9) 0.0017(9) 0.0111(9) C27 0.0255(11) 0.0230(11) 0.0230(12) 0.0046(9) -0.0025(9) 0.0091(9) C28 0.0333(13) 0.0233(12) 0.0279(13) 0.0011(10) -0.0050(10) 0.0081(10) C29 0.0450(15) 0.0258(12) 0.0236(13) -0.0005(10) 0.0013(11) 0.0172(11) C30 0.0357(13) 0.0293(13) 0.0233(12) 0.0070(10) 0.0071(10) 0.0182(11) C31 0.0289(12) 0.0212(11) 0.0219(11) 0.0061(9) 0.0030(9) 0.0122(9) C32 0.0232(11) 0.0233(12) 0.0325(14) 0.0087(10) -0.0044(10) 0.0031(9) C33 0.0311(13) 0.0318(13) 0.0293(13) 0.0102(11) 0.0141(10) 0.0112(10) C34 0.0252(13) 0.0417(16) 0.0394(16) 0.0135(13) 0.0047(11) -0.0003(11) C35 0.0307(13) 0.0314(13) 0.0341(14) 0.0165(11) 0.0112(11) 0.0050(10) C36 0.0366(15) 0.0527(18) 0.0264(14) 0.0165(13) 0.0077(11) 0.0088(13) C37 0.0410(16) 0.0464(17) 0.0509(19) 0.0224(15) 0.0270(14) 0.0237(14) C38 0.0333(13) 0.0219(11) 0.0195(11) -0.0018(9) 0.0037(9) 0.0093(10) C39 0.0342(13) 0.0208(11) 0.0173(11) 0.0047(9) 0.0048(9) 0.0124(10) C40 0.0209(11) 0.0319(12) 0.0141(10) 0.0050(9) 0.0030(8) 0.0072(9) C41 0.0241(11) 0.0220(11) 0.0238(12) 0.0032(9) 0.0061(9) 0.0064(9) C42 0.0383(14) 0.0309(13) 0.0319(14) 0.0064(11) 0.0124(11) 0.0175(11) _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 Zn1 O3 1.9846(16) . ? Zn1 O1 2.0146(16) . ? Zn1 N5 2.023(2) . ? Zn1 N3 2.102(2) . ? Zn1 N1 2.1138(19) . ? Zn2 N10 1.993(2) . ? Zn2 O8 1.9991(17) . ? Zn2 N6 2.068(2) . ? Zn2 O5 2.0836(16) . ? Zn2 N7 2.207(2) . ? Zn3 N9 1.955(2) . ? Zn3 N8 1.973(2) . ? Zn3 O5 1.9783(16) . ? Zn3 O7 2.0339(17) . ? Zn3 O6 2.3190(17) . ? N1 C7 1.276(3) . ? N1 C9 1.475(3) . ? N2 C10 1.480(3) . ? N2 C12 1.481(3) . ? N2 C11 1.496(3) . ? N2 H1 0.83(3) . ? N3 C19 1.284(3) . ? N3 C21 1.470(3) . ? N4 C24 1.488(3) . ? N4 C23 1.488(3) . ? N4 C22 1.498(3) . ? N4 H2 0.87(3) . ? N5 C25 1.159(3) . ? N6 C32 1.280(3) . ? N6 C34 1.466(3) . ? N7 C35 1.475(3) . ? N7 C37 1.478(3) . ? N7 C36 1.477(3) . ? N8 C40 1.159(3) . ? N9 C39 1.159(3) . ? N10 C38 1.157(3) . ? O1 C1 1.317(3) . ? O2 C2 1.373(3) . ? O2 C8 1.439(3) . ? O3 C13 1.317(3) . ? O4 C14 1.376(3) . ? O4 C20 1.439(3) . ? O5 C26 1.335(3) . ? O6 C31 1.373(3) . ? O6 C33 1.433(3) . ? O7 C41 1.257(3) . ? O8 C41 1.267(3) . ? S1 C25 1.629(2) . ? S2 C38 1.631(3) . ? S3 C39 1.623(3) . ? S5 C40 1.627(2) . ? C1 C6 1.412(3) . ? C1 C2 1.420(3) . ? C2 C3 1.381(3) . ? C3 C4 1.392(4) . ? C3 H3A 0.9500 . ? C4 C5 1.369(4) . ? C4 H4A 0.9500 . ? C5 C6 1.413(3) . ? C5 H5A 0.9500 . ? C6 C7 1.456(3) . ? C7 H7A 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.543(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.413(3) . ? C13 C14 1.428(3) . ? C14 C15 1.379(3) . ? C15 C16 1.406(4) . ? C15 H15A 0.9500 . ? C16 C17 1.359(4) . ? C16 H16A 0.9500 . ? C17 C18 1.416(3) . ? C17 H17A 0.9500 . ? C18 C19 1.447(4) . ? C19 H19A 0.9500 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.515(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C26 C27 1.411(3) . ? C26 C31 1.410(3) . ? C27 C28 1.414(4) . ? C27 C32 1.454(4) . ? C28 C29 1.375(4) . ? C28 H28A 0.9500 . ? C29 C30 1.395(4) . ? C29 H29A 0.9500 . ? C30 C31 1.377(3) . ? C30 H30A 0.9500 . ? C32 H32A 0.9500 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.523(4) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C41 C42 1.511(3) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 O3 Zn1 O1 114.80(7) . . ? O3 Zn1 N5 120.62(8) . . ? O1 Zn1 N5 124.58(8) . . ? O3 Zn1 N3 89.63(7) . . ? O1 Zn1 N3 88.11(7) . . ? N5 Zn1 N3 91.32(9) . . ? O3 Zn1 N1 88.11(7) . . ? O1 Zn1 N1 88.82(7) . . ? N5 Zn1 N1 93.63(8) . . ? N3 Zn1 N1 175.04(8) . . ? N10 Zn2 O8 112.62(8) . . ? N10 Zn2 N6 109.77(8) . . ? O8 Zn2 N6 137.28(8) . . ? N10 Zn2 O5 99.67(8) . . ? O8 Zn2 O5 93.53(7) . . ? N6 Zn2 O5 84.41(7) . . ? N10 Zn2 N7 98.31(8) . . ? O8 Zn2 N7 87.71(8) . . ? N6 Zn2 N7 81.18(8) . . ? O5 Zn2 N7 159.93(7) . . ? N9 Zn3 N8 110.98(9) . . ? N9 Zn3 O5 119.13(8) . . ? N8 Zn3 O5 125.89(8) . . ? N9 Zn3 O7 104.91(8) . . ? N8 Zn3 O7 92.98(8) . . ? O5 Zn3 O7 92.86(7) . . ? N9 Zn3 O6 88.63(8) . . ? N8 Zn3 O6 89.24(8) . . ? O5 Zn3 O6 73.47(6) . . ? O7 Zn3 O6 164.40(7) . . ? C7 N1 C9 116.8(2) . . ? C7 N1 Zn1 122.35(16) . . ? C9 N1 Zn1 120.81(15) . . ? C10 N2 C12 113.5(2) . . ? C10 N2 C11 109.37(19) . . ? C12 N2 C11 110.7(2) . . ? C10 N2 H1 109(2) . . ? C12 N2 H1 109(2) . . ? C11 N2 H1 105(2) . . ? C19 N3 C21 116.9(2) . . ? C19 N3 Zn1 122.93(17) . . ? C21 N3 Zn1 120.16(16) . . ? C24 N4 C23 109.8(2) . . ? C24 N4 C22 113.4(2) . . ? C23 N4 C22 109.3(2) . . ? C24 N4 H2 107.9(19) . . ? C23 N4 H2 108(2) . . ? C22 N4 H2 109(2) . . ? C25 N5 Zn1 169.6(2) . . ? C32 N6 C34 119.2(2) . . ? C32 N6 Zn2 125.77(17) . . ? C34 N6 Zn2 113.54(17) . . ? C35 N7 C37 110.3(2) . . ? C35 N7 C36 109.7(2) . . ? C37 N7 C36 107.5(2) . . ? C35 N7 Zn2 103.71(15) . . ? C37 N7 Zn2 113.06(16) . . ? C36 N7 Zn2 112.55(16) . . ? C40 N8 Zn3 150.4(2) . . ? C39 N9 Zn3 162.1(2) . . ? C38 N10 Zn2 163.4(2) . . ? C1 O1 Zn1 124.55(14) . . ? C2 O2 C8 116.0(2) . . ? C13 O3 Zn1 127.01(15) . . ? C14 O4 C20 116.5(2) . . ? C26 O5 Zn3 119.52(14) . . ? C26 O5 Zn2 119.89(14) . . ? Zn3 O5 Zn2 117.08(8) . . ? C31 O6 C33 118.51(19) . . ? C31 O6 Zn3 109.99(13) . . ? C33 O6 Zn3 127.88(15) . . ? C41 O7 Zn3 122.35(15) . . ? C41 O8 Zn2 129.45(16) . . ? O1 C1 C6 123.7(2) . . ? O1 C1 C2 119.2(2) . . ? C6 C1 C2 117.1(2) . . ? O2 C2 C3 124.1(2) . . ? O2 C2 C1 114.3(2) . . ? C3 C2 C1 121.6(2) . . ? C2 C3 C4 120.4(2) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 119.6(2) . . ? C5 C4 H4A 120.2 . . ? C3 C4 H4A 120.2 . . ? C4 C5 C6 121.2(2) . . ? C4 C5 H5A 119.4 . . ? C6 C5 H5A 119.4 . . ? C5 C6 C1 120.0(2) . . ? C5 C6 C7 116.2(2) . . ? C1 C6 C7 123.7(2) . . ? N1 C7 C6 127.6(2) . . ? N1 C7 H7A 116.2 . . ? C6 C7 H7A 116.2 . . ? O2 C8 H8A 109.5 . . ? O2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 C10 112.84(19) . . ? N1 C9 H9A 109.0 . . ? C10 C9 H9A 109.0 . . ? N1 C9 H9B 109.0 . . ? C10 C9 H9B 109.0 . . ? H9A C9 H9B 107.8 . . ? N2 C10 C9 114.7(2) . . ? N2 C10 H10A 108.6 . . ? C9 C10 H10A 108.6 . . ? N2 C10 H10B 108.6 . . ? C9 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O3 C13 C18 124.4(2) . . ? O3 C13 C14 118.5(2) . . ? C18 C13 C14 117.0(2) . . ? O4 C14 C15 124.3(2) . . ? O4 C14 C13 114.0(2) . . ? C15 C14 C13 121.7(2) . . ? C14 C15 C16 119.8(3) . . ? C14 C15 H15A 120.1 . . ? C16 C15 H15A 120.1 . . ? C17 C16 C15 120.3(2) . . ? C17 C16 H16A 119.8 . . ? C15 C16 H16A 119.8 . . ? C16 C17 C18 120.8(3) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C13 C18 C17 120.3(2) . . ? C13 C18 C19 123.7(2) . . ? C17 C18 C19 115.8(2) . . ? N3 C19 C18 127.2(2) . . ? N3 C19 H19A 116.4 . . ? C18 C19 H19A 116.4 . . ? O4 C20 H20A 109.5 . . ? O4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? O4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N3 C21 C22 111.93(19) . . ? N3 C21 H21A 109.2 . . ? C22 C21 H21A 109.2 . . ? N3 C21 H21B 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N4 C22 C21 114.4(2) . . ? N4 C22 H22A 108.7 . . ? C21 C22 H22A 108.7 . . ? N4 C22 H22B 108.7 . . ? C21 C22 H22B 108.7 . . ? H22A C22 H22B 107.6 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N5 C25 S1 178.8(2) . . ? O5 C26 C27 123.0(2) . . ? O5 C26 C31 119.2(2) . . ? C27 C26 C31 117.9(2) . . ? C26 C27 C28 119.2(2) . . ? C26 C27 C32 123.0(2) . . ? C28 C27 C32 117.8(2) . . ? C29 C28 C27 121.2(2) . . ? C29 C28 H28A 119.4 . . ? C27 C28 H28A 119.4 . . ? C28 C29 C30 120.1(2) . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 119.4(2) . . ? C31 C30 H30A 120.3 . . ? C29 C30 H30A 120.3 . . ? O6 C31 C30 125.4(2) . . ? O6 C31 C26 112.3(2) . . ? C30 C31 C26 122.3(2) . . ? N6 C32 C27 124.6(2) . . ? N6 C32 H32A 117.7 . . ? C27 C32 H32A 117.7 . . ? O6 C33 H33A 109.5 . . ? O6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? O6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N6 C34 C35 107.9(2) . . ? N6 C34 H34A 110.1 . . ? C35 C34 H34A 110.1 . . ? N6 C34 H34B 110.1 . . ? C35 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? N7 C35 C34 110.7(2) . . ? N7 C35 H35A 109.5 . . ? C34 C35 H35A 109.5 . . ? N7 C35 H35B 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 108.1 . . ? N7 C36 H36A 109.5 . . ? N7 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N7 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N7 C37 H37A 109.5 . . ? N7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N10 C38 S2 177.9(2) . . ? N9 C39 S3 177.6(2) . . ? N8 C40 S5 179.0(2) . . ? O7 C41 O8 124.9(2) . . ? O7 C41 C42 117.2(2) . . ? O8 C41 C42 118.0(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zn1 N1 C7 -95.08(19) . . . . ? O1 Zn1 N1 C7 19.78(19) . . . . ? N5 Zn1 N1 C7 144.35(19) . . . . ? N3 Zn1 N1 C7 -32.1(10) . . . . ? O3 Zn1 N1 C9 83.45(17) . . . . ? O1 Zn1 N1 C9 -161.69(17) . . . . ? N5 Zn1 N1 C9 -37.11(17) . . . . ? N3 Zn1 N1 C9 146.5(8) . . . . ? O3 Zn1 N3 C19 17.5(2) . . . . ? O1 Zn1 N3 C19 -97.4(2) . . . . ? N5 Zn1 N3 C19 138.1(2) . . . . ? N1 Zn1 N3 C19 -45.5(10) . . . . ? O3 Zn1 N3 C21 -162.19(18) . . . . ? O1 Zn1 N3 C21 82.98(18) . . . . ? N5 Zn1 N3 C21 -41.58(18) . . . . ? N1 Zn1 N3 C21 134.8(8) . . . . ? O3 Zn1 N5 C25 93.2(11) . . . . ? O1 Zn1 N5 C25 -85.7(11) . . . . ? N3 Zn1 N5 C25 2.9(11) . . . . ? N1 Zn1 N5 C25 -176.8(11) . . . . ? N10 Zn2 N6 C32 -65.3(2) . . . . ? O8 Zn2 N6 C32 122.2(2) . . . . ? O5 Zn2 N6 C32 33.0(2) . . . . ? N7 Zn2 N6 C32 -161.0(2) . . . . ? N10 Zn2 N6 C34 100.51(19) . . . . ? O8 Zn2 N6 C34 -72.1(2) . . . . ? O5 Zn2 N6 C34 -161.20(18) . . . . ? N7 Zn2 N6 C34 4.79(18) . . . . ? N10 Zn2 N7 C35 -86.26(16) . . . . ? O8 Zn2 N7 C35 161.21(16) . . . . ? N6 Zn2 N7 C35 22.59(15) . . . . ? O5 Zn2 N7 C35 67.2(3) . . . . ? N10 Zn2 N7 C37 154.3(2) . . . . ? O8 Zn2 N7 C37 41.8(2) . . . . ? N6 Zn2 N7 C37 -96.8(2) . . . . ? O5 Zn2 N7 C37 -52.2(3) . . . . ? N10 Zn2 N7 C36 32.3(2) . . . . ? O8 Zn2 N7 C36 -80.24(19) . . . . ? N6 Zn2 N7 C36 141.14(19) . . . . ? O5 Zn2 N7 C36 -174.24(19) . . . . ? N9 Zn3 N8 C40 -62.6(4) . . . . ? O5 Zn3 N8 C40 140.3(4) . . . . ? O7 Zn3 N8 C40 44.6(4) . . . . ? O6 Zn3 N8 C40 -150.8(4) . . . . ? N8 Zn3 N9 C39 -18.4(7) . . . . ? O5 Zn3 N9 C39 140.4(6) . . . . ? O7 Zn3 N9 C39 -117.6(7) . . . . ? O6 Zn3 N9 C39 70.3(7) . . . . ? O8 Zn2 N10 C38 101.8(7) . . . . ? N6 Zn2 N10 C38 -72.7(7) . . . . ? O5 Zn2 N10 C38 -160.2(7) . . . . ? N7 Zn2 N10 C38 10.9(7) . . . . ? O3 Zn1 O1 C1 54.14(18) . . . . ? N5 Zn1 O1 C1 -126.84(17) . . . . ? N3 Zn1 O1 C1 142.86(18) . . . . ? N1 Zn1 O1 C1 -33.24(17) . . . . ? O1 Zn1 O3 C13 64.11(19) . . . . ? N5 Zn1 O3 C13 -114.96(19) . . . . ? N3 Zn1 O3 C13 -23.64(19) . . . . ? N1 Zn1 O3 C13 151.94(19) . . . . ? N9 Zn3 O5 C26 -98.81(17) . . . . ? N8 Zn3 O5 C26 56.60(19) . . . . ? O7 Zn3 O5 C26 152.36(16) . . . . ? O6 Zn3 O5 C26 -20.00(15) . . . . ? N9 Zn3 O5 Zn2 60.05(12) . . . . ? N8 Zn3 O5 Zn2 -144.54(9) . . . . ? O7 Zn3 O5 Zn2 -48.78(9) . . . . ? O6 Zn3 O5 Zn2 138.87(10) . . . . ? N10 Zn2 O5 C26 62.85(17) . . . . ? O8 Zn2 O5 C26 176.51(16) . . . . ? N6 Zn2 O5 C26 -46.30(16) . . . . ? N7 Zn2 O5 C26 -90.5(3) . . . . ? N10 Zn2 O5 Zn3 -95.93(10) . . . . ? O8 Zn2 O5 Zn3 17.73(9) . . . . ? N6 Zn2 O5 Zn3 154.92(10) . . . . ? N7 Zn2 O5 Zn3 110.7(2) . . . . ? N9 Zn3 O6 C31 140.72(15) . . . . ? N8 Zn3 O6 C31 -108.27(15) . . . . ? O5 Zn3 O6 C31 19.72(14) . . . . ? O7 Zn3 O6 C31 -9.9(3) . . . . ? N9 Zn3 O6 C33 -61.4(2) . . . . ? N8 Zn3 O6 C33 49.6(2) . . . . ? O5 Zn3 O6 C33 177.6(2) . . . . ? O7 Zn3 O6 C33 148.0(2) . . . . ? N9 Zn3 O7 C41 -62.4(2) . . . . ? N8 Zn3 O7 C41 -175.04(19) . . . . ? O5 Zn3 O7 C41 58.78(19) . . . . ? O6 Zn3 O7 C41 87.1(3) . . . . ? N10 Zn2 O8 C41 141.2(2) . . . . ? N6 Zn2 O8 C41 -46.4(2) . . . . ? O5 Zn2 O8 C41 39.2(2) . . . . ? N7 Zn2 O8 C41 -120.8(2) . . . . ? Zn1 O1 C1 C6 29.8(3) . . . . ? Zn1 O1 C1 C2 -150.32(16) . . . . ? C8 O2 C2 C3 -7.9(3) . . . . ? C8 O2 C2 C1 170.9(2) . . . . ? O1 C1 C2 O2 2.0(3) . . . . ? C6 C1 C2 O2 -178.05(19) . . . . ? O1 C1 C2 C3 -179.1(2) . . . . ? C6 C1 C2 C3 0.8(3) . . . . ? O2 C2 C3 C4 179.5(2) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? C2 C3 C4 C5 -1.2(4) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C4 C5 C6 C1 1.8(4) . . . . ? C4 C5 C6 C7 -178.4(2) . . . . ? O1 C1 C6 C5 177.9(2) . . . . ? C2 C1 C6 C5 -2.0(3) . . . . ? O1 C1 C6 C7 -1.9(4) . . . . ? C2 C1 C6 C7 178.2(2) . . . . ? C9 N1 C7 C6 178.7(2) . . . . ? Zn1 N1 C7 C6 -2.7(3) . . . . ? C5 C6 C7 N1 167.7(2) . . . . ? C1 C6 C7 N1 -12.5(4) . . . . ? C7 N1 C9 C10 136.2(2) . . . . ? Zn1 N1 C9 C10 -42.4(3) . . . . ? C12 N2 C10 C9 -55.4(3) . . . . ? C11 N2 C10 C9 -179.5(2) . . . . ? N1 C9 C10 N2 -56.1(3) . . . . ? Zn1 O3 C13 C18 16.4(3) . . . . ? Zn1 O3 C13 C14 -164.99(16) . . . . ? C20 O4 C14 C15 9.0(3) . . . . ? C20 O4 C14 C13 -171.1(2) . . . . ? O3 C13 C14 O4 -1.0(3) . . . . ? C18 C13 C14 O4 177.7(2) . . . . ? O3 C13 C14 C15 178.9(2) . . . . ? C18 C13 C14 C15 -2.4(3) . . . . ? O4 C14 C15 C16 -179.6(2) . . . . ? C13 C14 C15 C16 0.5(4) . . . . ? C14 C15 C16 C17 1.4(4) . . . . ? C15 C16 C17 C18 -1.3(4) . . . . ? O3 C13 C18 C17 -178.9(2) . . . . ? C14 C13 C18 C17 2.5(3) . . . . ? O3 C13 C18 C19 5.9(4) . . . . ? C14 C13 C18 C19 -172.8(2) . . . . ? C16 C17 C18 C13 -0.7(4) . . . . ? C16 C17 C18 C19 174.9(2) . . . . ? C21 N3 C19 C18 175.3(2) . . . . ? Zn1 N3 C19 C18 -4.4(4) . . . . ? C13 C18 C19 N3 -11.8(4) . . . . ? C17 C18 C19 N3 172.8(2) . . . . ? C19 N3 C21 C22 133.4(2) . . . . ? Zn1 N3 C21 C22 -46.9(3) . . . . ? C24 N4 C22 C21 -49.3(3) . . . . ? C23 N4 C22 C21 -172.2(2) . . . . ? N3 C21 C22 N4 -56.1(3) . . . . ? Zn1 N5 C25 S1 115(12) . . . . ? Zn3 O5 C26 C27 -160.77(17) . . . . ? Zn2 O5 C26 C27 41.0(3) . . . . ? Zn3 O5 C26 C31 18.3(3) . . . . ? Zn2 O5 C26 C31 -139.96(17) . . . . ? O5 C26 C27 C28 177.2(2) . . . . ? C31 C26 C27 C28 -1.9(3) . . . . ? O5 C26 C27 C32 -4.4(3) . . . . ? C31 C26 C27 C32 176.5(2) . . . . ? C26 C27 C28 C29 1.4(4) . . . . ? C32 C27 C28 C29 -177.1(2) . . . . ? C27 C28 C29 C30 -0.1(4) . . . . ? C28 C29 C30 C31 -0.6(4) . . . . ? C33 O6 C31 C30 2.7(3) . . . . ? Zn3 O6 C31 C30 162.91(19) . . . . ? C33 O6 C31 C26 -176.9(2) . . . . ? Zn3 O6 C31 C26 -16.7(2) . . . . ? C29 C30 C31 O6 -179.5(2) . . . . ? C29 C30 C31 C26 0.0(4) . . . . ? O5 C26 C31 O6 1.7(3) . . . . ? C27 C26 C31 O6 -179.17(19) . . . . ? O5 C26 C31 C30 -177.9(2) . . . . ? C27 C26 C31 C30 1.2(3) . . . . ? C34 N6 C32 C27 -176.6(2) . . . . ? Zn2 N6 C32 C27 -11.5(3) . . . . ? C26 C27 C32 N6 -12.4(4) . . . . ? C28 C27 C32 N6 166.0(2) . . . . ? C32 N6 C34 C35 136.0(2) . . . . ? Zn2 N6 C34 C35 -30.8(3) . . . . ? C37 N7 C35 C34 74.9(3) . . . . ? C36 N7 C35 C34 -166.9(2) . . . . ? Zn2 N7 C35 C34 -46.4(2) . . . . ? N6 C34 C35 N7 52.9(3) . . . . ? Zn2 N10 C38 S2 -109(7) . . . . ? Zn3 N9 C39 S3 166(5) . . . . ? Zn3 N8 C40 S5 162(14) . . . . ? Zn3 O7 C41 O8 -17.1(3) . . . . ? Zn3 O7 C41 C42 162.96(17) . . . . ? Zn2 O8 C41 O7 -44.3(3) . . . . ? Zn2 O8 C41 C42 135.6(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H1 O3 0.83(3) 1.89(3) 2.681(3) 160(3) . N2 H1 O4 0.83(3) 2.46(3) 3.008(3) 125(2) . N4 H2 O1 0.87(3) 1.86(3) 2.676(3) 155(3) . N4 H2 O2 0.87(3) 2.47(3) 3.103(3) 130(2) . _diffrn_measured_fraction_theta_max 0.902 _diffrn_reflns_theta_full 28.27 _diffrn_measured_fraction_theta_full 0.902 _refine_diff_density_max 0.706 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.079 #===END data_sm6 _database_code_depnum_ccdc_archive 'CCDC 281765' _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 2' _chemical_formula_moiety 'C24 H34 Cd2 Cl2 N4 O4' _chemical_formula_structural '[Cd2 (L)2 Cl2]' _chemical_formula_analytical ? _chemical_formula_sum 'C24 H34 Cd2 Cl2 N4 O4' _chemical_formula_weight 738.25 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cd Cd 0.1185 4.6533 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M Cc 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' _cell_length_a 15.373(8) _cell_length_b 14.399(7) _cell_length_c 14.621(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.94(4) _cell_angle_gamma 90.00 _cell_volume 2980.5(28) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 16 _cell_measurement_theta_min 20 _cell_measurement_theta_max 25 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max .09 _exptl_crystal_size_mid .04 _exptl_crystal_size_min .04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.645 _exptl_crystal_density_method ? _exptl_crystal_F_000 1472 _exptl_absorpt_coefficient_mu 13.363 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'PICKER 4-circle Stoe upgrade' _diffrn_measurement_method ' \w scans' _diffrn_standards_number 1 _diffrn_standards_interval_count 120 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 1537 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 4.38 _diffrn_reflns_theta_max 50.00 _reflns_number_total 1537 _reflns_number_observed 1435 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'PICKER STOE DIF4' _computing_cell_refinement 'STOE DIF4' _computing_data_reduction 'STOE REDU4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXLTL-Plus _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.1071P)^2^+2.1018P] 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 ? _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 0.01(2) _refine_ls_number_reflns 1537 _refine_ls_number_parameters 323 _refine_ls_number_restraints 452 _refine_ls_R_factor_all 0.0489 _refine_ls_R_factor_obs 0.0464 _refine_ls_wR_factor_all 0.1227 _refine_ls_wR_factor_obs 0.1193 _refine_ls_goodness_of_fit_all 1.046 _refine_ls_goodness_of_fit_obs 1.062 _refine_ls_restrained_S_all 0.948 _refine_ls_restrained_S_obs 0.954 _refine_ls_shift/esd_max -0.014 _refine_ls_shift/esd_mean 0.001 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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Cd1 Cd 1.0000 0.97808(7) 1.0000 0.0454(4) Uani 1 d U . Cd2 Cd 1.22436(8) 1.01739(8) 1.20975(9) 0.0487(4) Uani 1 d U . Cl1 Cl 0.8597(3) 0.9137(4) 1.0170(4) 0.0724(13) Uani 1 d U . Cl2 Cl 1.2496(3) 1.0751(4) 1.3759(4) 0.0765(14) Uani 1 d U . C12' C 1.3921(11) 1.1275(14) 1.1833(17) 0.075(4) Uani 1 d U . H12A H 1.4268(11) 1.1443(14) 1.2515(17) 0.104 Uiso 1 d R . H12B H 1.4124(11) 1.1671(14) 1.1425(17) 0.104 Uiso 1 d R . C13 C 0.9558(23) 0.9517(18) 0.7792(16) 0.127(7) Uani 1 d U . H13A H 0.9678(23) 0.9749(18) 0.7237(16) 0.178 Uiso 1 d R . H13D H 0.8912(23) 0.9314(18) 0.7525(16) 0.178 Uiso 1 d R . O9' O 1.0988(8) 1.0880(9) 1.0910(9) 0.051(2) Uani 1 d U . O9 O 1.1313(8) 0.9067(10) 1.1179(10) 0.058(3) Uani 1 d U . N14' N 1.3780(10) 0.9648(10) 1.2244(11) 0.066(3) Uani 1 d U . C8' C 1.0821(11) 1.1780(12) 1.0737(10) 0.040(3) Uani 1 d U . N14 N 0.9516(13) 1.0319(11) 0.8317(11) 0.074(3) Uani 1 d U . O2' O 0.9227(8) 1.1416(7) 1.0229(9) 0.064(3) Uani 1 d U . C16' C 1.3704(15) 0.8692(14) 1.1781(17) 0.080(4) Uani 1 d U . H16A H 1.4316(15) 0.8479(14) 1.1840(17) 0.112 Uiso 1 d R . H16B H 1.3446(15) 0.8264(14) 1.2112(17) 0.112 Uiso 1 d R . H16C H 1.3293(15) 0.8730(14) 1.1092(17) 0.112 Uiso 1 d R . C6' C 1.1301(13) 1.3358(11) 1.0685(15) 0.065(4) Uani 1 d U . H6'A H 1.1789(13) 1.3810(11) 1.0788(15) 0.091 Uiso 1 d R . O2 O 1.2163(8) 0.8496(9) 1.2985(8) 0.071(3) Uani 1 d U . C7 C 1.1047(11) 0.7524(11) 1.0525(13) 0.058(3) Uani 1 d U . N11' N 1.2908(9) 1.1417(9) 1.1567(10) 0.056(3) Uani 1 d U . C6 C 1.1132(12) 0.6558(11) 1.0769(14) 0.062(4) Uani 1 d U . H6A H 1.0893(12) 0.6112(11) 1.0240(14) 0.087 Uiso 1 d R . C12 C 1.0025(15) 0.8711(15) 0.8072(13) 0.077(4) Uani 1 d U . H12C H 1.0572(15) 0.8754(15) 0.7910(13) 0.108 Uiso 1 d R . H12D H 0.9654(15) 0.8191(15) 0.7721(13) 0.108 Uiso 1 d R . C7' C 1.1559(11) 1.2418(10) 1.0899(12) 0.050(3) Uani 1 d U . C13' C 1.4145(13) 1.0312(12) 1.1681(16) 0.068(3) Uani 1 d U . H13B H 1.4814(13) 1.0228(12) 1.1883(16) 0.095 Uiso 1 d R . H13C H 1.3849(13) 1.0167(12) 1.0986(16) 0.095 Uiso 1 d R . C4' C 0.9674(12) 1.3037(11) 1.0200(12) 0.059(4) Uani 1 d U . H4'A H 0.9029(12) 1.3239(11) 0.9968(12) 0.082 Uiso 1 d R . C10 C 1.0644(12) 0.7768(11) 0.9512(14) 0.063(4) Uani 1 d U . H10A H 1.0589(12) 0.7278(11) 0.9048(14) 0.088 Uiso 1 d R . C3 C 1.1815(11) 0.7835(13) 1.2287(13) 0.062(4) Uani 1 d U . C5 C 1.1552(13) 0.6248(14) 1.1719(15) 0.069(5) Uani 1 d U . H5A H 1.1616(13) 0.5594(14) 1.1856(15) 0.096 Uiso 1 d R . C5' C 1.0406(14) 1.3645(13) 1.0345(14) 0.065(4) Uani 1 d U . H5'A H 1.0259(14) 1.4290(13) 1.0202(14) 0.091 Uiso 1 d R . N11 N 1.0321(10) 0.8579(9) 0.9130(9) 0.060(3) Uani 1 d U . C3' C 0.9896(11) 1.2088(11) 1.0398(11) 0.048(3) Uani 1 d U . C4 C 1.1887(12) 0.6868(13) 1.2489(14) 0.069(4) Uani 1 d U . H4A H 1.2162(12) 0.6656(13) 1.3164(14) 0.097 Uiso 1 d R . C10' C 1.2541(11) 1.2180(11) 1.1234(11) 0.056(3) Uani 1 d U . H10B H 1.2959(11) 1.2661(11) 1.1197(11) 0.079 Uiso 1 d R . C15' C 1.4442(14) 0.9675(20) 1.3324(17) 0.106(7) Uani 1 d U . H15A H 1.5052(14) 0.9461(20) 1.3379(17) 0.148 Uiso 1 d R . H15B H 1.4498(14) 1.0288(20) 1.3599(17) 0.148 Uiso 1 d R . H15C H 1.4197(14) 0.9261(20) 1.3681(17) 0.148 Uiso 1 d R . C8 C 1.1392(12) 0.8154(14) 1.1301(14) 0.058(4) Uani 1 d U . C1 C 1.2588(15) 0.8251(16) 1.4035(13) 0.095(7) Uani 1 d U . H1A H 1.2803(15) 0.8797(16) 1.4438(13) 0.133 Uiso 1 d R . H1B H 1.2121(15) 0.7940(16) 1.4209(13) 0.133 Uiso 1 d R . H1C H 1.3112(15) 0.7842(16) 1.4147(13) 0.133 Uiso 1 d R . C1' C 0.8276(13) 1.1668(15) 1.0016(19) 0.093(7) Uani 1 d U . H1'A H 0.7908(13) 1.1111(15) 0.9919(19) 0.131 Uiso 1 d R . H1'B H 0.8260(13) 1.2000(15) 1.0578(19) 0.131 Uiso 1 d R . H1'C H 0.8018(13) 1.2051(15) 0.9434(19) 0.131 Uiso 1 d R . C16 C 1.0100(16) 1.0950(17) 0.8166(13) 0.093(5) Uani 1 d U . H16D H 0.9868(16) 1.1137(17) 0.7482(13) 0.131 Uiso 1 d R . H16E H 1.0116(16) 1.1478(17) 0.8573(13) 0.131 Uiso 1 d R . H16F H 1.0725(16) 1.0701(17) 0.8359(13) 0.131 Uiso 1 d R . C15 C 0.8552(18) 1.0624(24) 0.7941(16) 0.135(7) Uani 1 d U . H15D H 0.8369(18) 1.0834(24) 0.7269(16) 0.189 Uiso 1 d R . H15E H 0.8154(18) 1.0118(24) 0.7961(16) 0.189 Uiso 1 d R . H15F H 0.8489(18) 1.1125(24) 0.8345(16) 0.189 Uiso 1 d 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 Cd1 0.0469(8) 0.0436(8) 0.0442(7) 0.0007(6) 0.0161(6) -0.0064(6) Cd2 0.0455(8) 0.0465(8) 0.0507(8) -0.0040(7) 0.0150(6) 0.0019(7) Cl1 0.073(3) 0.078(3) 0.076(3) -0.007(3) 0.039(2) -0.030(3) Cl2 0.069(3) 0.107(4) 0.055(2) -0.018(3) 0.026(2) -0.017(3) C12' 0.047(6) 0.075(7) 0.103(13) 0.003(11) 0.031(9) 0.004(8) C13 0.228(18) 0.078(8) 0.041(7) 0.000(11) 0.014(13) 0.039(15) O9' 0.058(5) 0.036(4) 0.052(5) 0.009(5) 0.012(5) 0.006(6) O9 0.058(5) 0.041(4) 0.061(5) -0.004(6) 0.008(5) 0.002(6) N14' 0.049(5) 0.069(6) 0.067(7) -0.005(7) 0.010(6) 0.004(7) C8' 0.057(5) 0.037(5) 0.028(7) 0.003(7) 0.020(6) 0.022(8) N14 0.110(9) 0.071(7) 0.046(5) 0.019(7) 0.035(7) 0.015(9) O2' 0.056(5) 0.042(5) 0.096(8) 0.002(6) 0.034(6) 0.010(5) C16' 0.079(11) 0.073(8) 0.110(13) -0.008(11) 0.061(11) 0.023(10) C6' 0.075(7) 0.041(6) 0.083(11) 0.007(9) 0.035(8) -0.001(9) O2 0.080(8) 0.077(7) 0.054(5) 0.020(6) 0.023(6) 0.022(7) C7 0.052(9) 0.043(6) 0.064(6) -0.009(8) 0.008(7) -0.005(7) N11' 0.048(5) 0.052(6) 0.067(7) 0.014(7) 0.020(6) -0.010(6) C6 0.061(10) 0.041(6) 0.075(8) -0.004(8) 0.017(8) 0.001(8) C12 0.099(13) 0.088(8) 0.043(6) -0.005(9) 0.027(9) 0.008(11) C7' 0.064(6) 0.036(5) 0.058(9) 0.002(7) 0.031(7) -0.002(7) C13' 0.055(7) 0.074(7) 0.079(9) -0.008(9) 0.031(9) -0.003(8) C4' 0.068(8) 0.044(6) 0.057(9) 0.005(8) 0.017(8) 0.015(8) C10 0.067(10) 0.047(6) 0.064(6) -0.012(8) 0.013(8) -0.013(8) C3 0.054(9) 0.059(6) 0.063(6) -0.004(9) 0.012(8) -0.008(8) C5 0.063(11) 0.050(7) 0.081(9) -0.002(10) 0.014(9) -0.008(9) C5' 0.075(8) 0.040(7) 0.080(12) 0.016(9) 0.030(9) 0.014(9) N11 0.076(8) 0.052(6) 0.046(5) -0.011(6) 0.018(6) -0.014(7) C3' 0.057(5) 0.047(6) 0.044(8) -0.002(7) 0.024(6) 0.011(8) C4 0.067(10) 0.067(6) 0.070(8) 0.028(9) 0.024(8) 0.000(9) C10' 0.062(6) 0.048(7) 0.057(10) 0.011(8) 0.022(7) 0.000(8) C15' 0.055(9) 0.176(22) 0.066(8) 0.010(14) 0.002(9) 0.039(13) C8 0.058(10) 0.044(5) 0.062(6) 0.012(9) 0.011(8) -0.006(8) C1 0.109(16) 0.098(16) 0.056(7) 0.038(11) 0.008(11) -0.017(13) C1' 0.056(7) 0.074(14) 0.141(20) -0.006(14) 0.027(12) -0.007(10) C16 0.114(11) 0.104(11) 0.051(9) 0.025(10) 0.020(10) -0.049(13) C15 0.100(10) 0.231(24) 0.050(11) 0.037(17) 0.005(11) 0.039(20) _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 Cd1 O9' 2.238(13) . ? Cd1 N11 2.312(13) . ? Cd1 O9 2.322(12) . ? Cd1 N14 2.405(14) . ? Cd1 Cl1 2.448(5) . ? Cd2 O9 2.212(13) . ? Cd2 O9' 2.272(11) . ? Cd2 N11' 2.338(12) . ? Cd2 N14' 2.409(14) . ? Cd2 Cl2 2.451(5) . ? C12' N11' 1.46(2) . ? C12' C13' 1.47(3) . ? C13 C12 1.34(3) . ? C13 N14 1.40(3) . ? O9' C8' 1.33(2) . ? O9 C8 1.33(2) . ? N14' C13' 1.51(2) . ? N14' C15' 1.51(3) . ? N14' C16' 1.52(2) . ? C8' C3' 1.38(2) . ? C8' C7' 1.41(2) . ? N14 C16 1.35(2) . ? N14 C15 1.43(3) . ? O2' C3' 1.36(2) . ? O2' C1' 1.42(2) . ? C6' C5' 1.33(3) . ? C6' C7' 1.41(2) . ? O2 C3 1.34(2) . ? O2 C1 1.46(2) . ? C7 C8 1.39(2) . ? C7 C10 1.41(3) . ? C7 C6 1.43(2) . ? N11' C10' 1.24(2) . ? C6 C5 1.36(3) . ? C12 N11 1.44(2) . ? C7' C10' 1.43(2) . ? C4' C5' 1.37(3) . ? C4' C3' 1.41(2) . ? C10 N11 1.31(2) . ? C3 C8 1.41(3) . ? C3 C4 1.42(3) . ? C5 C4 1.37(3) . ? 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 O9' Cd1 N11 128.0(5) . . ? O9' Cd1 O9 71.3(4) . . ? N11 Cd1 O9 76.5(5) . . ? O9' Cd1 N14 104.4(5) . . ? N11 Cd1 N14 74.1(5) . . ? O9 Cd1 N14 137.3(5) . . ? O9' Cd1 Cl1 128.9(3) . . ? N11 Cd1 Cl1 99.1(3) . . ? O9 Cd1 Cl1 107.6(4) . . ? N14 Cd1 Cl1 107.0(5) . . ? O9 Cd2 O9' 72.7(4) . . ? O9 Cd2 N11' 127.8(5) . . ? O9' Cd2 N11' 75.8(5) . . ? O9 Cd2 N14' 101.9(5) . . ? O9' Cd2 N14' 136.1(5) . . ? N11' Cd2 N14' 74.4(5) . . ? O9 Cd2 Cl2 131.4(4) . . ? O9' Cd2 Cl2 111.4(4) . . ? N11' Cd2 Cl2 98.5(4) . . ? N14' Cd2 Cl2 104.3(4) . . ? N11' C12' C13' 112.3(16) . . ? C12 C13 N14 132.7(20) . . ? C8' O9' Cd1 122.8(10) . . ? C8' O9' Cd2 128.8(11) . . ? Cd1 O9' Cd2 108.4(5) . . ? C8 O9 Cd2 129.0(11) . . ? C8 O9 Cd1 123.1(11) . . ? Cd2 O9 Cd1 107.5(6) . . ? C13' N14' C15' 108.2(16) . . ? C13' N14' C16' 108.2(14) . . ? C15' N14' C16' 113.1(16) . . ? C13' N14' Cd2 108.2(10) . . ? C15' N14' Cd2 108.8(12) . . ? C16' N14' Cd2 110.1(10) . . ? O9' C8' C3' 118.4(16) . . ? O9' C8' C7' 121.6(14) . . ? C3' C8' C7' 120.0(15) . . ? C16 N14 C13 106.8(22) . . ? C16 N14 C15 112.6(19) . . ? C13 N14 C15 107.7(21) . . ? C16 N14 Cd1 115.0(13) . . ? C13 N14 Cd1 103.5(13) . . ? C15 N14 Cd1 110.6(13) . . ? C3' O2' C1' 119.9(13) . . ? C5' C6' C7' 122.7(17) . . ? C3 O2 C1 120.7(15) . . ? C8 C7 C10 124.6(16) . . ? C8 C7 C6 117.7(16) . . ? C10 C7 C6 117.7(15) . . ? C10' N11' C12' 120.0(15) . . ? C10' N11' Cd2 128.0(11) . . ? C12' N11' Cd2 111.2(11) . . ? C5 C6 C7 122.3(17) . . ? C13 C12 N11 110.3(18) . . ? C8' C7' C6' 116.8(15) . . ? C8' C7' C10' 125.1(14) . . ? C6' C7' C10' 118.1(15) . . ? C12' C13' N14' 111.0(16) . . ? C5' C4' C3' 117.9(15) . . ? N11 C10 C7 127.6(16) . . ? O2 C3 C8 115.7(16) . . ? O2 C3 C4 124.1(16) . . ? C8 C3 C4 120.1(17) . . ? C6 C5 C4 120.2(18) . . ? C6' C5' C4' 121.6(16) . . ? C10 N11 C12 119.0(15) . . ? C10 N11 Cd1 124.1(11) . . ? C12 N11 Cd1 116.5(12) . . ? O2' C3' C8' 115.8(14) . . ? O2' C3' C4' 123.1(14) . . ? C8' C3' C4' 121.1(16) . . ? C5 C4 C3 119.6(17) . . ? N11' C10' C7' 126.9(15) . . ? O9 C8 C7 123.6(17) . . ? O9 C8 C3 116.3(17) . . ? C7 C8 C3 120.0(17) . . ? _refine_diff_density_max 0.714 _refine_diff_density_min -1.130 _refine_diff_density_rms 0.137 #===END data_CRYSTALS_cif _database_code_depnum_ccdc_archive 'CCDC 281766' _audit_creation_date 05-05-02 _audit_creation_method CRYSTALS_ver_12.51 _oxford_structure_analysis_title 'import in P 21/c' _chemical_name_systematic ? _chemical_melting_point ? _cell_length_a 14.590(5) _cell_length_b 15.638(5) _cell_length_c 14.792(5) _cell_angle_alpha 90 _cell_angle_beta 103.911(5) _cell_angle_gamma 90 _cell_volume 3275.9(19) _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1 ' _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz x,y,z -x,-y,-z -x,y+1/2,-z+1/2 x,-y+1/2,z+1/2 loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512 0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4' H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998 0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4' N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826 -11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4' O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089 0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4' S 0.1246 0.1234 6.9053 1.4679 5.2034 22.2151 1.4379 0.2536 1.5863 56.1720 0.8669 'International Tables Vol C 4.2.6.8 and 6.1.1.4' Cd -0.8075 1.2024 19.2214 0.5946 17.6444 6.9089 4.4610 24.7008 1.6029 87.4825 5.0694 'International Tables Vol C 4.2.6.8 and 6.1.1.4' _cell_formula_units_Z 4 # Given Formula = C27 H34 Cd2 N6 O4 S2 # Dc = 1.61 Fooo = 1568.00 Mu = 14.66 M = 795.54 # Found Formula = C26 H34 Cd2 N6 O4 S2 # Dc = 1.59 FOOO = 1568.00 Mu = 14.64 M = 783.53 _chemical_name_common 'Compound 3' _chemical_formula_structural '[Cd2 (L)2 (NCS)2]' _chemical_formula_sum 'C26 H34 Cd2 N6 O4 S2' _chemical_formula_moiety 'C26 H34 Cd2 N6 O4 S2' _chemical_compound_source ? _chemical_formula_weight 783.53 _cell_measurement_reflns_used 7660 _cell_measurement_theta_min 0 _cell_measurement_theta_max 28 _cell_measurement_temperature 293 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_min 0.01 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_max 0.01 _exptl_crystal_density_diffrn 1.589 _exptl_crystal_density_meas ? # Non-dispersive F(000): _exptl_crystal_F_000 1568 _exptl_absorpt_coefficient_mu 1.464 # Sheldrick geometric approximatio 0.99 0.99 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9855 _exptl_absorpt_correction_T_max 0.9855 _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_radiation_monochromator graphite _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71069 _diffrn_measurement_method \w/2\q _computing_data_collection 'COLLECT (Nonius BV, 1997)' _computing_data_reduction 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_cell_refinement 'DENZO/SCALEPACK (Otwinowski & Minor, 1997)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'CRYSTALS (Betteridge et al., 2003)' _computing_publication_material 'CRYSTALS (Betteridge et al., 2003)' _computing_molecular_graphics 'CAMERON (Watkin et al., 1996)' _diffrn_standards_interval_time ? _diffrn_standards_interval_count ? _diffrn_standards_number 0 _diffrn_standards_decay_% ? _diffrn_ambient_temperature 293 _diffrn_reflns_number 8045 _reflns_number_total 7750 _diffrn_reflns_av_R_equivalents 0.060 # Number of reflections with Friedels Law is 7750 # Number of reflections without Friedels Law is 0 # Theoretical number of reflections is about 8017 _diffrn_reflns_theta_min 1.438 _diffrn_reflns_theta_max 28.136 _diffrn_measured_fraction_theta_max 0.966 _diffrn_reflns_theta_full 27.292 _diffrn_measured_fraction_theta_full 0.996 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _reflns_limit_h_min -18 _reflns_limit_h_max 18 _reflns_limit_k_min 0 _reflns_limit_k_max 20 _reflns_limit_l_min 0 _reflns_limit_l_max 19 _oxford_diffrn_Wilson_B_factor 0.00 _oxford_diffrn_Wilson_scale 0.00 _atom_sites_solution_primary direct #heavy,direct,difmap,geom # _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_diff_density_min -0.83 _refine_diff_density_max 0.95 _refine_ls_number_reflns 3579 _refine_ls_number_restraints 0 _refine_ls_number_parameters 361 #_refine_ls_R_factor_ref 0.0555 _refine_ls_wR_factor_ref 0.0549 _refine_ls_goodness_of_fit_ref 1.0311 #_reflns_number_all 7724 _refine_ls_R_factor_all 0.1434 _refine_ls_wR_factor_all 0.0903 # The I/u(I) cutoff below was used for refinement as # well as the _gt R-factors: _reflns_threshold_expression I>3.00u(I) _reflns_number_gt 3579 _refine_ls_R_factor_gt 0.0555 _refine_ls_wR_factor_gt 0.0549 _refine_ls_shift/su_max 0.002239 # choose from: rm (reference molecule of known chirality), # ad (anomolous dispersion - Flack), rmad (rm and ad), # syn (from synthesis), unk (unknown) or . (not applicable). _chemical_absolute_configuration . _refine_ls_structure_factor_coef F _refine_ls_matrix_type full _refine_ls_hydrogen_treatment noref # none, undef, noref, refall, # refxyz, refU, constr or mixed _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) [weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)] where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax Method = Robust Weighting (Prince, 1982) W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^ A~i~ are: 3.58 -0.242 3.25 ; _publ_section_references ; Altomare, A., Burla, M.C., Camalli, M., Cascarano, G.L., Giacovazzo, C., Guagliardi, A., Grazia, A., Moliterni, G., Polidori, G. and Spagna, R. (1999) J. App. Cryst. 32, 115-119 Betteridge, P.W., Carruthers, J.R., Cooper, R.I., Prout, K., Watkin, D.J. (2003). J. Appl. Cryst. 36, 1487. Nonius BV, COLLECT Software, (1997-2001) Otwinowski, Z. & Minor, W. (1997). Methods in Enzymology, Vol. 276, edited by C. W. Carter Jr & R. M. Sweet, pp. 307--326. New York: Academic Press. Prince, E. Mathematical Techniques in Crystallography and Materials Science Springer-Verlag, New York, 1982. Watkin D.J. (1994), Acta Cryst, A50, 411-437 Watkin, D.J., Prout, C.K. & Pearce, L.J. (1996) CAMERON, Chemical Crystallography Laboratory, OXFORD, UK. ; # Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3 # Replace last . with number of unfound hydrogen atoms attached to an atom. # ..._refinement_flags_... # . no refinement constraints S special position constraint on site # G rigid group refinement of site R riding atom # D distance or angle restraint on site T thermal displacement constraints # U Uiso or Uij restraint (rigid bond) P partial occupancy constraint 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_occupancy _atom_site_adp_type _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_attached_hydrogens Cd1 Cd 0.81103(3) 0.02849(3) 0.19717(3) 0.0394 1.0000 Uani . . . . . . Cd2 Cd 0.76361(4) 0.24892(3) 0.11542(4) 0.0491 1.0000 Uani . . . . . . C1 C 0.5498(6) 0.3436(6) 0.1935(7) 0.0758 1.0000 Uani . . . . . . O2 O 0.5978(4) 0.2694(3) 0.1714(4) 0.0582 1.0000 Uani . . . . . . C3 C 0.5473(5) 0.1928(5) 0.1597(5) 0.0487 1.0000 Uani . . . . . . C4 C 0.4525(5) 0.1855(5) 0.1619(6) 0.0588 1.0000 Uani . . . . . . C5 C 0.4092(6) 0.1041(7) 0.1492(7) 0.0733 1.0000 Uani . . . . . . C6 C 0.4570(5) 0.0335(6) 0.1317(6) 0.0612 1.0000 Uani . . . . . . C7 C 0.5545(5) 0.0384(5) 0.1305(5) 0.0478 1.0000 Uani . . . . . . C8 C 0.6003(4) 0.1197(5) 0.1450(4) 0.0417 1.0000 Uani . . . . . . O9 O 0.6919(3) 0.1292(3) 0.1451(3) 0.0451 1.0000 Uani . . . . . . C10 C 0.5979(5) -0.0413(5) 0.1093(6) 0.0506 1.0000 Uani . . . . . . N11 N 0.6857(4) -0.0549(4) 0.1209(5) 0.0513 1.0000 Uani . . . . . . C12 C 0.7174(6) -0.1402(5) 0.0990(7) 0.0673 1.0000 Uani . . . . . . C13 C 0.8044(6) -0.1287(5) 0.0621(6) 0.0591 1.0000 Uani . . . . . . N14 N 0.8834(4) -0.0834(3) 0.1277(4) 0.0384 1.0000 Uani . . . . . . C15 C 0.9477(6) -0.0496(5) 0.0732(6) 0.0576 1.0000 Uani . . . . . . C16 C 0.9370(7) -0.1423(6) 0.1989(6) 0.0712 1.0000 Uani . . . . . . C21 C 1.0398(6) 0.0130(7) 0.3822(7) 0.0798 1.0000 Uani . . . . . . O22 O 0.9847(3) 0.0587(4) 0.3029(4) 0.0632 1.0000 Uani . . . . . . C23 C 1.0328(5) 0.1099(5) 0.2545(6) 0.0578 1.0000 Uani . . . . . . C24 C 1.1296(6) 0.1167(7) 0.2720(7) 0.0784 1.0000 Uani . . . . . . C25 C 1.1700(7) 0.1687(8) 0.2150(9) 0.0886 1.0000 Uani . . . . . . C26 C 1.1133(7) 0.2131(7) 0.1427(8) 0.0748 1.0000 Uani . . . . . . C27 C 1.0141(6) 0.2095(5) 0.1242(6) 0.0563 1.0000 Uani . . . . . . C28 C 0.9712(5) 0.1569(5) 0.1802(5) 0.0482 1.0000 Uani . . . . . . O29 O 0.8798(3) 0.1477(3) 0.1679(4) 0.0531 1.0000 Uani . . . . . . C30 C 0.9627(8) 0.2608(5) 0.0491(7) 0.0712 1.0000 Uani . . . . . . N31 N 0.8741(7) 0.2793(5) 0.0293(5) 0.0703 1.0000 Uani . . . . . . C32 C 0.8336(10) 0.3339(7) -0.0505(8) 0.0962 1.0000 Uani . . . . . . C33 C 0.7329(10) 0.3070(7) -0.0937(6) 0.0935 1.0000 Uani . . . . . . N34 N 0.6720(6) 0.3121(5) -0.0251(5) 0.0730 1.0000 Uani . . . . . . C35 C 0.5849(12) 0.2626(9) -0.0621(8) 0.1205 1.0000 Uani . . . . . . C36 C 0.6498(10) 0.4035(8) -0.0088(9) 0.1078 1.0000 Uani . . . . . . N40 N 0.7956(5) -0.0240(5) 0.3329(5) 0.0608 1.0000 Uani . . . . . . C41 C 0.7661(5) -0.0692(5) 0.3816(5) 0.0472 1.0000 Uani . . . . . . S42 S 0.72744(19) -0.13028(16) 0.45341(19) 0.0736 1.0000 Uani . . . . . . N43 N 0.7994(6) 0.3518(6) 0.2222(6) 0.0808 1.0000 Uani . . . . . . C44 C 0.7899(5) 0.3854(5) 0.2888(7) 0.0593 1.0000 Uani . . . . . . S45 S 0.7771(2) 0.4311(2) 0.3820(2) 0.0945 1.0000 Uani . . . . . . H11 H 0.5926 0.3963 0.1996 0.0819 1.0000 Uiso . . . . . . H12 H 0.5294 0.3369 0.2523 0.0819 1.0000 Uiso . . . . . . H13 H 0.4920 0.3572 0.1412 0.0819 1.0000 Uiso . . . . . . H82 H 0.4149 0.2396 0.1718 0.0738 1.0000 Uiso . . . . . . H83 H 0.3414 0.0984 0.1523 0.0785 1.0000 Uiso . . . . . . H84 H 0.4223 -0.0237 0.1200 0.0706 1.0000 Uiso . . . . . . H101 H 0.5534 -0.0909 0.0835 0.0593 1.0000 Uiso . . . . . . H121 H 0.7346 -0.1774 0.1563 0.0854 1.0000 Uiso . . . . . . H122 H 0.6663 -0.1711 0.0514 0.0854 1.0000 Uiso . . . . . . H131 H 0.8268 -0.1848 0.0431 0.0730 1.0000 Uiso . . . . . . H132 H 0.7846 -0.0923 0.0016 0.0730 1.0000 Uiso . . . . . . H151 H 1.0027 -0.0187 0.1147 0.0705 1.0000 Uiso . . . . . . H152 H 0.9738 -0.0975 0.0408 0.0705 1.0000 Uiso . . . . . . H153 H 0.9142 -0.0081 0.0237 0.0705 1.0000 Uiso . . . . . . H161 H 0.9892 -0.1118 0.2445 0.0852 1.0000 Uiso . . . . . . H162 H 0.9660 -0.1906 0.1700 0.0852 1.0000 Uiso . . . . . . H163 H 0.8943 -0.1695 0.2366 0.0852 1.0000 Uiso . . . . . . H211 H 0.9975 -0.0217 0.4108 0.0912 1.0000 Uiso . . . . . . H212 H 1.0767 0.0542 0.4286 0.0912 1.0000 Uiso . . . . . . H213 H 1.0857 -0.0262 0.3607 0.0912 1.0000 Uiso . . . . . . H282 H 1.1703 0.0851 0.3300 0.0931 1.0000 Uiso . . . . . . H283 H 1.2424 0.1727 0.2273 0.1101 1.0000 Uiso . . . . . . H284 H 1.1438 0.2508 0.0998 0.1003 1.0000 Uiso . . . . . . H301 H 0.9990 0.2858 0.0047 0.0862 1.0000 Uiso . . . . . . H321 H 0.8720 0.3320 -0.0990 0.1117 1.0000 Uiso . . . . . . H322 H 0.8326 0.3962 -0.0299 0.1117 1.0000 Uiso . . . . . . H331 H 0.7040 0.3451 -0.1504 0.1022 1.0000 Uiso . . . . . . H332 H 0.7326 0.2467 -0.1187 0.1022 1.0000 Uiso . . . . . . H361 H 0.6083 0.4055 0.0386 0.1200 1.0000 Uiso . . . . . . H362 H 0.7074 0.4374 0.0170 0.1200 1.0000 Uiso . . . . . . H363 H 0.6120 0.4315 -0.0674 0.1200 1.0000 Uiso . . . . . . H351 H 0.5417 0.2631 -0.0171 0.1251 1.0000 Uiso . . . . . . H352 H 0.5464 0.2847 -0.1240 0.1251 1.0000 Uiso . . . . . . H353 H 0.5986 0.1994 -0.0721 0.1251 1.0000 Uiso . . . . . . 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 Cd1 0.0405(3) 0.0347(2) 0.0443(3) -0.0013(2) 0.01262(18) -0.0036(2) Cd2 0.0622(4) 0.0379(3) 0.0462(3) 0.0042(2) 0.0109(2) -0.0098(3) C1 0.056(5) 0.068(6) 0.089(7) -0.022(5) -0.011(5) 0.005(4) O2 0.048(3) 0.047(3) 0.075(4) -0.007(2) 0.006(3) 0.001(2) C3 0.044(4) 0.054(4) 0.043(4) 0.002(3) 0.001(3) 0.000(3) C4 0.044(4) 0.057(5) 0.073(5) 0.001(4) 0.011(4) 0.006(4) C5 0.035(4) 0.095(7) 0.090(6) -0.010(5) 0.013(4) 0.003(5) C6 0.035(4) 0.065(5) 0.083(6) 0.000(4) 0.012(4) -0.014(4) C7 0.039(4) 0.047(4) 0.056(4) 0.006(3) 0.007(3) -0.006(3) C8 0.030(3) 0.054(4) 0.037(3) -0.001(3) 0.000(3) 0.007(3) O9 0.039(3) 0.029(2) 0.066(3) 0.008(2) 0.012(2) -0.0060(19) C10 0.042(4) 0.042(4) 0.067(5) 0.004(3) 0.011(3) -0.015(3) N11 0.053(4) 0.034(3) 0.068(4) -0.019(3) 0.016(3) -0.012(3) C12 0.065(5) 0.043(4) 0.101(7) -0.014(4) 0.033(5) -0.010(4) C13 0.066(5) 0.051(4) 0.065(5) -0.020(4) 0.025(4) -0.008(4) N14 0.044(3) 0.037(3) 0.039(3) -0.004(2) 0.018(2) 0.000(2) C15 0.061(5) 0.062(5) 0.054(4) -0.001(4) 0.023(4) -0.008(4) C16 0.090(6) 0.058(5) 0.064(5) 0.019(4) 0.015(5) 0.025(5) C21 0.056(5) 0.093(7) 0.082(6) 0.007(5) -0.002(4) 0.013(5) O22 0.034(3) 0.079(4) 0.070(4) 0.005(3) 0.000(2) 0.003(3) C23 0.044(4) 0.058(5) 0.073(5) -0.040(4) 0.019(4) -0.016(4) C24 0.050(5) 0.101(8) 0.088(7) -0.040(6) 0.023(5) 0.009(5) C25 0.060(6) 0.106(9) 0.112(9) -0.069(7) 0.044(6) -0.031(6) C26 0.065(6) 0.076(6) 0.100(7) -0.045(6) 0.051(6) -0.028(5) C27 0.077(5) 0.044(4) 0.060(5) -0.031(4) 0.040(4) -0.032(4) C28 0.038(4) 0.045(4) 0.063(5) -0.029(3) 0.015(3) -0.017(3) O29 0.040(3) 0.048(3) 0.070(3) 0.000(2) 0.011(2) -0.011(2) C30 0.104(8) 0.051(5) 0.087(6) -0.028(5) 0.077(6) -0.040(5) N31 0.108(7) 0.052(4) 0.063(4) -0.003(3) 0.045(4) -0.027(4) C32 0.141(10) 0.086(8) 0.076(7) 0.026(5) 0.054(7) -0.016(7) C33 0.170(12) 0.064(6) 0.041(5) 0.010(4) 0.015(6) -0.015(7) N34 0.110(6) 0.051(4) 0.049(4) 0.012(3) 0.003(4) -0.015(4) C35 0.156(12) 0.120(10) 0.061(6) 0.018(6) -0.021(7) -0.048(9) C36 0.148(11) 0.078(7) 0.094(8) 0.035(6) 0.022(8) 0.007(8) N40 0.074(4) 0.064(4) 0.050(4) -0.006(3) 0.026(3) -0.001(4) C41 0.051(4) 0.044(4) 0.044(4) -0.014(3) 0.007(3) 0.003(3) S42 0.0832(16) 0.0596(13) 0.0876(16) 0.0115(12) 0.0395(13) -0.0030(12) N43 0.083(6) 0.073(5) 0.091(6) -0.020(5) 0.029(5) -0.025(4) C44 0.045(4) 0.046(4) 0.078(6) -0.015(4) -0.002(4) -0.005(3) S45 0.0772(17) 0.0909(19) 0.111(2) -0.0526(17) 0.0149(15) 0.0045(15) _refine_ls_extinction_method None _oxford_refine_ls_scale 0.2400(6) loop_ _geom_bond_atom_site_label_1 _geom_bond_site_symmetry_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cd1 . O9 . 2.335(5) yes Cd1 . N11 . 2.308(6) yes Cd1 . N14 . 2.399(5) yes Cd1 . O22 . 2.680(5) yes Cd1 . O29 . 2.209(5) yes Cd1 . N40 . 2.230(7) yes Cd2 . O2 . 2.757(6) yes Cd2 . O9 . 2.239(4) yes Cd2 . O29 . 2.313(5) yes Cd2 . N31 . 2.331(8) yes Cd2 . N34 . 2.398(7) yes Cd2 . N43 . 2.227(8) yes C1 . O2 . 1.433(11) yes C1 . H11 . 1.025 no C1 . H12 . 0.991 no C1 . H13 . 1.020 no O2 . C3 . 1.396(9) yes C3 . C4 . 1.396(11) yes C3 . C8 . 1.426(10) yes C4 . C5 . 1.413(13) yes C4 . H82 . 1.038 no C5 . C6 . 1.363(13) yes C5 . H83 . 1.006 no C6 . C7 . 1.428(10) yes C6 . H84 . 1.023 no C7 . C8 . 1.428(10) yes C7 . C10 . 1.465(11) yes C8 . O9 . 1.344(8) yes C10 . N11 . 1.269(10) yes C10 . H101 . 1.025 no N11 . C12 . 1.473(10) yes C12 . C13 . 1.508(12) yes C12 . H121 . 1.009 no C12 . H122 . 1.016 no C13 . N14 . 1.494(10) yes C13 . H131 . 0.999 no C13 . H132 . 1.042 no N14 . C15 . 1.474(9) yes N14 . C16 . 1.473(9) yes C15 . H151 . 1.008 no C15 . H152 . 1.012 no C15 . H153 . 1.012 no C16 . H161 . 1.008 no C16 . H162 . 1.009 no C16 . H163 . 1.023 no C21 . O22 . 1.442(11) yes C21 . H211 . 0.990 no C21 . H212 . 0.998 no C21 . H213 . 1.014 no O22 . C23 . 1.374(10) yes C23 . C24 . 1.377(12) yes C23 . C28 . 1.442(12) yes C24 . C25 . 1.400(16) yes C24 . H282 . 1.042 no C25 . C26 . 1.373(17) yes C25 . H283 . 1.030 no C26 . C27 . 1.408(13) yes C26 . H284 . 1.042 no C27 . C28 . 1.416(11) yes C27 . C30 . 1.428(15) yes C28 . O29 . 1.309(8) yes C30 . N31 . 1.289(13) yes C30 . H301 . 1.015 no N31 . C32 . 1.461(13) yes C32 . C33 . 1.513(17) yes C32 . H321 . 1.013 no C32 . H322 . 1.022 no C33 . N34 . 1.503(14) yes C33 . H331 . 1.032 no C33 . H332 . 1.013 no N34 . C35 . 1.476(15) yes N34 . C36 . 1.497(15) yes C35 . H351 . 1.021 no C35 . H352 . 1.013 no C35 . H353 . 1.026 no C36 . H361 . 1.032 no C36 . H362 . 0.989 no C36 . H363 . 1.008 no N40 . C41 . 1.163(10) yes C41 . S42 . 1.628(9) yes N43 . C44 . 1.153(11) yes C44 . S45 . 1.604(10) yes loop_ _geom_angle_atom_site_label_1 _geom_angle_site_symmetry_1 _geom_angle_atom_site_label_2 _geom_angle_site_symmetry_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O9 . Cd1 . N11 . 77.31(19) yes O9 . Cd1 . N14 . 136.08(17) yes N11 . Cd1 . N14 . 76.0(2) yes O9 . Cd1 . O22 . 126.72(17) yes N11 . Cd1 . O22 . 155.7(2) yes N14 . Cd1 . O22 . 85.80(18) yes O9 . Cd1 . O29 . 72.74(17) yes N11 . Cd1 . O29 . 136.5(2) yes N14 . Cd1 . O29 . 105.32(19) yes O22 . Cd1 . O29 . 63.59(19) yes O9 . Cd1 . N40 . 108.5(2) yes N11 . Cd1 . N40 . 89.5(3) yes N14 . Cd1 . N40 . 105.5(2) yes O22 . Cd1 . N40 . 80.0(2) yes O29 . Cd1 . N40 . 129.5(2) yes O2 . Cd2 . O9 . 63.47(16) yes O2 . Cd2 . O29 . 127.17(17) yes O9 . Cd2 . O29 . 72.64(16) yes O2 . Cd2 . N31 . 155.8(3) yes O9 . Cd2 . N31 . 134.0(2) yes O29 . Cd2 . N31 . 77.0(3) yes O2 . Cd2 . N34 . 82.3(2) yes O9 . Cd2 . N34 . 109.0(2) yes O29 . Cd2 . N34 . 141.6(2) yes N31 . Cd2 . N34 . 75.9(3) yes O2 . Cd2 . N43 . 77.1(2) yes O9 . Cd2 . N43 . 120.4(3) yes O29 . Cd2 . N43 . 103.2(3) yes N31 . Cd2 . N43 . 99.5(3) yes N34 . Cd2 . N43 . 107.7(3) yes O2 . C1 . H11 . 110.493 no O2 . C1 . H12 . 112.457 no H11 . C1 . H12 . 108.237 no O2 . C1 . H13 . 110.824 no H11 . C1 . H13 . 105.982 no H12 . C1 . H13 . 108.601 no C1 . O2 . Cd2 . 132.5(5) yes C1 . O2 . C3 . 116.8(6) yes Cd2 . O2 . C3 . 109.8(4) yes O2 . C3 . C4 . 124.3(7) yes O2 . C3 . C8 . 114.7(6) yes C4 . C3 . C8 . 121.0(7) yes C3 . C4 . C5 . 118.9(7) yes C3 . C4 . H82 . 119.788 no C5 . C4 . H82 . 121.262 no C4 . C5 . C6 . 121.4(7) yes C4 . C5 . H83 . 119.140 no C6 . C5 . H83 . 119.403 no C5 . C6 . C7 . 121.0(8) yes C5 . C6 . H84 . 119.055 no C7 . C6 . H84 . 119.899 no C6 . C7 . C8 . 118.5(7) yes C6 . C7 . C10 . 116.1(7) yes C8 . C7 . C10 . 125.3(6) yes C7 . C8 . C3 . 119.0(6) yes C7 . C8 . O9 . 121.9(6) yes C3 . C8 . O9 . 119.1(6) yes C8 . O9 . Cd1 . 125.9(4) yes C8 . O9 . Cd2 . 127.2(4) yes Cd1 . O9 . Cd2 . 106.41(18) yes C7 . C10 . N11 . 126.0(6) yes C7 . C10 . H101 . 117.120 no N11 . C10 . H101 . 116.835 no Cd1 . N11 . C10 . 128.8(5) yes Cd1 . N11 . C12 . 111.4(5) yes C10 . N11 . C12 . 118.9(6) yes N11 . C12 . C13 . 108.0(6) yes N11 . C12 . H121 . 111.406 no C13 . C12 . H121 . 108.125 no N11 . C12 . H122 . 111.441 no C13 . C12 . H122 . 110.365 no H121 . C12 . H122 . 107.503 no C12 . C13 . N14 . 114.0(6) yes C12 . C13 . H131 . 110.905 no N14 . C13 . H131 . 110.212 no C12 . C13 . H132 . 106.983 no N14 . C13 . H132 . 108.093 no H131 . C13 . H132 . 106.260 no C13 . N14 . Cd1 . 105.9(4) yes C13 . N14 . C15 . 107.9(5) yes Cd1 . N14 . C15 . 112.1(4) yes C13 . N14 . C16 . 111.2(6) yes Cd1 . N14 . C16 . 111.2(4) yes C15 . N14 . C16 . 108.5(6) yes N14 . C15 . H151 . 110.912 no N14 . C15 . H152 . 110.884 no H151 . C15 . H152 . 107.901 no N14 . C15 . H153 . 111.483 no H151 . C15 . H153 . 107.883 no H152 . C15 . H153 . 107.622 no N14 . C16 . H161 . 111.561 no N14 . C16 . H162 . 111.607 no H161 . C16 . H162 . 108.154 no N14 . C16 . H163 . 111.213 no H161 . C16 . H163 . 107.095 no H162 . C16 . H163 . 106.977 no O22 . C21 . H211 . 109.666 no O22 . C21 . H212 . 110.064 no H211 . C21 . H212 . 110.472 no O22 . C21 . H213 . 108.944 no H211 . C21 . H213 . 109.167 no H212 . C21 . H213 . 108.496 no C21 . O22 . Cd1 . 130.6(5) yes C21 . O22 . C23 . 117.3(6) yes Cd1 . O22 . C23 . 109.2(4) yes O22 . C23 . C24 . 125.2(9) yes O22 . C23 . C28 . 113.0(6) yes C24 . C23 . C28 . 121.8(9) yes C23 . C24 . C25 . 119.5(11) yes C23 . C24 . H282 . 118.286 no C25 . C24 . H282 . 122.150 no C24 . C25 . C26 . 120.1(9) yes C24 . C25 . H283 . 119.435 no C26 . C25 . H283 . 120.472 no C25 . C26 . C27 . 122.0(9) yes C25 . C26 . H284 . 119.692 no C27 . C26 . H284 . 118.316 no C26 . C27 . C28 . 119.2(9) yes C26 . C27 . C30 . 116.8(8) yes C28 . C27 . C30 . 124.0(8) yes C23 . C28 . C27 . 117.4(7) yes C23 . C28 . O29 . 118.5(7) yes C27 . C28 . O29 . 124.1(8) yes C28 . O29 . Cd2 . 127.7(5) yes C28 . O29 . Cd1 . 124.1(5) yes Cd2 . O29 . Cd1 . 108.2(2) yes C27 . C30 . N31 . 127.8(7) yes C27 . C30 . H301 . 117.491 no N31 . C30 . H301 . 114.679 no Cd2 . N31 . C30 . 128.2(6) yes Cd2 . N31 . C32 . 111.2(7) yes C30 . N31 . C32 . 120.2(8) yes N31 . C32 . C33 . 110.0(8) yes N31 . C32 . H321 . 111.784 no C33 . C32 . H321 . 109.780 no N31 . C32 . H322 . 110.463 no C33 . C32 . H322 . 107.947 no H321 . C32 . H322 . 106.716 no C32 . C33 . N34 . 111.8(8) yes C32 . C33 . H331 . 110.446 no N34 . C33 . H331 . 109.000 no C32 . C33 . H332 . 109.384 no N34 . C33 . H332 . 110.111 no H331 . C33 . H332 . 105.967 no C33 . N34 . Cd2 . 105.5(6) yes C33 . N34 . C35 . 108.5(9) yes Cd2 . N34 . C35 . 110.8(6) yes C33 . N34 . C36 . 110.2(8) yes Cd2 . N34 . C36 . 110.5(6) yes C35 . N34 . C36 . 111.1(11) yes N34 . C35 . H351 . 111.449 no N34 . C35 . H352 . 113.437 no H351 . C35 . H352 . 106.847 no N34 . C35 . H353 . 112.288 no H351 . C35 . H353 . 105.878 no H352 . C35 . H353 . 106.455 no N34 . C36 . H361 . 108.880 no N34 . C36 . H362 . 112.133 no H361 . C36 . H362 . 107.778 no N34 . C36 . H363 . 111.760 no H361 . C36 . H363 . 106.349 no H362 . C36 . H363 . 109.693 no Cd1 . N40 . C41 . 156.1(6) yes N40 . C41 . S42 . 177.6(7) yes Cd2 . N43 . C44 . 151.4(7) yes N43 . C44 . S45 . 179.4(9) yes #===END data_ps1 _database_code_depnum_ccdc_archive 'CCDC 281767' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 4' _chemical_melting_point ? _chemical_formula_moiety '2(C25 H36 Co N5 O4 S), C4 Co N4 S4' _chemical_formula_structural '[Co(LH)2(NCS)]2 [Co(NCS)4]' _chemical_formula_sum 'C54 H72 Co3 N14 O8 S6' _chemical_formula_weight 1414.41 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' 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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.227(18) _cell_length_b 19.468(20) _cell_length_c 13.857(18) _cell_angle_alpha 104.05(9) _cell_angle_beta 93.52(11) _cell_angle_gamma 109.48(8) _cell_volume 3467(7) _cell_formula_units_Z 2 _cell_measurement_temperature 296.2 _cell_measurement_reflns_used 5 _cell_measurement_theta_min 11.4 _cell_measurement_theta_max 12.4 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1470 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type 'not applied' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; Intensity data were measured to theta = 25 deg, but there was little of significance beyond theta = 20 deg. Total no. of reflections measured to theta-max = 25 was 10498, comprising 9962 unique (Rint = 0.220) and 2545 observed data. ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'Rigaku rotating anode generator' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Rigaku AFC7R diffractometer' _diffrn_measurement_method 'scintillation counter; \w/2\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 150 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6.38 _diffrn_reflns_number 6804 _diffrn_reflns_av_R_equivalents 0.1902 _diffrn_reflns_av_sigmaI/netI 0.2561 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 20.00 _reflns_number_total 6457 _reflns_number_gt 2520 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'MSC/AFC Diffractometer Software (MSC, 1993)' _computing_cell_refinement 'MSC/AFC Diffractometer Software (MSC, 1993)' _computing_data_reduction 'MSC texSan/PROCESS (MSC, 1993)' _computing_structure_solution 'SHELXS (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL (Sheldrick, 1997)' _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^)+(0.0890P)^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 6457 _refine_ls_number_parameters 796 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2345 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1820 _refine_ls_wR_factor_gt 0.1464 _refine_ls_goodness_of_fit_ref 0.865 _refine_ls_restrained_S_all 0.865 _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 0.27699(12) 0.09691(10) 0.39368(13) 0.0436(5) Uani 1 1 d . . . O11 O 0.3763(6) 0.1879(5) 0.4893(6) 0.046(2) Uani 1 1 d . . . C11 C 0.4571(11) 0.2400(9) 0.4729(11) 0.040(4) Uani 1 1 d . . . C12 C 0.5270(12) 0.2912(9) 0.5542(12) 0.047(4) Uani 1 1 d . . . O12 O 0.5061(6) 0.2833(5) 0.6453(8) 0.055(2) Uani 1 1 d . . . C121 C 0.5718(12) 0.3363(10) 0.7347(11) 0.104(6) Uani 1 1 d . . . H12A H 0.6366 0.3312 0.7368 0.155 Uiso 1 1 calc R . . H12B H 0.5432 0.3260 0.7930 0.155 Uiso 1 1 calc R . . H12C H 0.5793 0.3870 0.7340 0.155 Uiso 1 1 calc R . . C13 C 0.6091(11) 0.3509(8) 0.5430(11) 0.050(4) Uani 1 1 d . . . H13 H 0.6529 0.3866 0.5991 0.059 Uiso 1 1 calc R . . C14 C 0.6242(10) 0.3560(8) 0.4462(14) 0.056(4) Uani 1 1 d . . . H14 H 0.6783 0.3960 0.4379 0.067 Uiso 1 1 calc R . . C15 C 0.5626(11) 0.3048(9) 0.3657(11) 0.049(4) Uani 1 1 d . . . H15 H 0.5751 0.3075 0.3014 0.059 Uiso 1 1 calc R . . C16 C 0.4780(11) 0.2463(8) 0.3787(12) 0.045(4) Uani 1 1 d . . . C17 C 0.4173(12) 0.1975(10) 0.2856(13) 0.060(4) Uani 1 1 d . . . H17 H 0.4359 0.2113 0.2279 0.072 Uiso 1 1 calc R . . N18 N 0.3374(9) 0.1348(6) 0.2719(8) 0.045(3) Uani 1 1 d . . . C19 C 0.2832(11) 0.0994(8) 0.1697(11) 0.069(4) Uani 1 1 d . . . H19A H 0.3279 0.1155 0.1228 0.082 Uiso 1 1 calc R . . H19B H 0.2270 0.1163 0.1619 0.082 Uiso 1 1 calc R . . C110 C 0.2442(10) 0.0146(8) 0.1445(10) 0.065(4) Uani 1 1 d . . . H11A H 0.1948 -0.0005 0.1879 0.078 Uiso 1 1 calc R . . H11B H 0.2088 -0.0053 0.0759 0.078 Uiso 1 1 calc R . . N111 N 0.3177(8) -0.0227(6) 0.1532(8) 0.054(3) Uani 1 1 d . . . H111 H 0.3385 -0.0122 0.2203 0.065 Uiso 1 1 calc R . . C112 C 0.4108(10) 0.0047(8) 0.1080(10) 0.081(5) Uani 1 1 d . . . H11C H 0.4548 -0.0215 0.1202 0.121 Uiso 1 1 calc R . . H11D H 0.4447 0.0583 0.1380 0.121 Uiso 1 1 calc R . . H11E H 0.3929 -0.0050 0.0368 0.121 Uiso 1 1 calc R . . C113 C 0.2688(11) -0.1064(8) 0.1153(10) 0.073(4) Uani 1 1 d . . . H11F H 0.3180 -0.1293 0.1227 0.109 Uiso 1 1 calc R . . H11G H 0.2409 -0.1203 0.0454 0.109 Uiso 1 1 calc R . . H11H H 0.2159 -0.1238 0.1531 0.109 Uiso 1 1 calc R . . O21 O 0.3198(5) 0.0088(4) 0.3565(6) 0.040(2) Uani 1 1 d . . . C21 C 0.3432(8) -0.0272(7) 0.4197(9) 0.033(3) Uani 1 1 d . . . C22 C 0.4007(10) -0.0725(7) 0.3885(11) 0.045(4) Uani 1 1 d . . . O22 O 0.4308(6) -0.0703(5) 0.2990(8) 0.065(3) Uani 1 1 d . . . C221 C 0.4944(11) -0.1129(9) 0.2612(11) 0.097(6) Uani 1 1 d . . . H22A H 0.5425 -0.0849 0.2261 0.145 Uiso 1 1 calc R . . H22B H 0.4531 -0.1612 0.2160 0.145 Uiso 1 1 calc R . . H22C H 0.5295 -0.1207 0.3166 0.145 Uiso 1 1 calc R . . C23 C 0.4308(10) -0.1110(7) 0.4521(16) 0.072(5) Uani 1 1 d . . . H23 H 0.4731 -0.1375 0.4320 0.087 Uiso 1 1 calc R . . C24 C 0.3973(12) -0.1091(8) 0.5434(14) 0.071(5) Uani 1 1 d . . . H24 H 0.4142 -0.1363 0.5839 0.085 Uiso 1 1 calc R . . C25 C 0.3389(11) -0.0666(8) 0.5743(10) 0.061(4) Uani 1 1 d . . . H25 H 0.3176 -0.0640 0.6367 0.073 Uiso 1 1 calc R . . C26 C 0.3112(9) -0.0274(6) 0.5124(10) 0.036(3) Uani 1 1 d . . . C27 C 0.2456(10) 0.0130(8) 0.5530(10) 0.055(4) Uani 1 1 d . . . H27 H 0.2178 0.0017 0.6088 0.067 Uiso 1 1 calc R . . N28 N 0.2221(7) 0.0629(6) 0.5197(7) 0.044(3) Uani 1 1 d . . . C29 C 0.1494(9) 0.0923(7) 0.5728(10) 0.052(4) Uani 1 1 d . . . H29A H 0.0829 0.0676 0.5323 0.063 Uiso 1 1 calc R . . H29B H 0.1452 0.0798 0.6364 0.063 Uiso 1 1 calc R . . C210 C 0.1792(11) 0.1750(8) 0.5919(10) 0.057(4) Uani 1 1 d . . . H21A H 0.1310 0.1910 0.6290 0.068 Uiso 1 1 calc R . . H21B H 0.1745 0.1862 0.5277 0.068 Uiso 1 1 calc R . . N211 N 0.2832(8) 0.2213(6) 0.6492(8) 0.045(3) Uani 1 1 d . . . H211 H 0.3277 0.2127 0.6077 0.10(6) Uiso 1 1 calc R . . C212 C 0.3065(10) 0.2004(8) 0.7424(9) 0.065(4) Uani 1 1 d . . . H21C H 0.3742 0.2318 0.7746 0.098 Uiso 1 1 calc R . . H21D H 0.3004 0.1481 0.7248 0.098 Uiso 1 1 calc R . . H21E H 0.2600 0.2079 0.7875 0.098 Uiso 1 1 calc R . . C213 C 0.2999(9) 0.3047(7) 0.6730(10) 0.057(4) Uani 1 1 d . . . H21F H 0.3668 0.3338 0.7092 0.085 Uiso 1 1 calc R . . H21G H 0.2514 0.3153 0.7136 0.085 Uiso 1 1 calc R . . H21H H 0.2922 0.3180 0.6115 0.085 Uiso 1 1 calc R . . N31 N 0.1358(9) 0.0898(7) 0.3372(10) 0.082(5) Uani 1 1 d . . . C32 C 0.0579(11) 0.0902(8) 0.3250(13) 0.080(5) Uani 1 1 d . . . S33 S -0.0552(3) 0.0910(3) 0.3051(5) 0.136(2) Uani 1 1 d . . . Co2 Co 0.03781(12) 0.38564(9) 0.67195(13) 0.0425(5) Uani 1 1 d . . . O41 O 0.0763(6) 0.3410(5) 0.7769(5) 0.043(2) Uani 1 1 d . . . C41 C 0.0428(10) 0.2670(8) 0.7710(11) 0.043(4) Uani 1 1 d . . . C42 C 0.0926(10) 0.2437(9) 0.8431(11) 0.044(4) Uani 1 1 d . . . O42 O 0.1728(8) 0.3039(5) 0.9085(7) 0.065(3) Uani 1 1 d . . . C421 C 0.2183(11) 0.2876(8) 0.9907(12) 0.096(6) Uani 1 1 d . . . H42A H 0.1700 0.2745 1.0349 0.144 Uiso 1 1 calc R . . H42B H 0.2754 0.3315 1.0271 0.144 Uiso 1 1 calc R . . H42C H 0.2401 0.2459 0.9654 0.144 Uiso 1 1 calc R . . C43 C 0.0687(12) 0.1697(10) 0.8435(12) 0.061(4) Uani 1 1 d . . . H43 H 0.1045 0.1565 0.8899 0.073 Uiso 1 1 calc R . . C44 C -0.0109(12) 0.1146(9) 0.7725(13) 0.067(4) Uani 1 1 d . . . H44 H -0.0286 0.0639 0.7712 0.080 Uiso 1 1 calc R . . C45 C -0.0644(9) 0.1350(8) 0.7029(10) 0.054(4) Uani 1 1 d . . . H45 H -0.1176 0.0981 0.6557 0.064 Uiso 1 1 calc R . . C46 C -0.0375(10) 0.2099(7) 0.7052(11) 0.039(4) Uani 1 1 d . . . C47 C -0.1041(10) 0.2246(9) 0.6328(10) 0.054(4) Uani 1 1 d . . . H47 H -0.1625 0.1843 0.5993 0.064 Uiso 1 1 calc R . . N48 N -0.0889(7) 0.2878(6) 0.6120(7) 0.046(3) Uani 1 1 d . . . C49 C -0.1717(9) 0.2852(7) 0.5409(10) 0.055(4) Uani 1 1 d . . . H49A H -0.1783 0.3346 0.5575 0.066 Uiso 1 1 calc R . . H49B H -0.2341 0.2488 0.5497 0.066 Uiso 1 1 calc R . . C410 C -0.1586(10) 0.2642(8) 0.4319(11) 0.066(4) Uani 1 1 d . . . H41A H -0.1475 0.2164 0.4168 0.079 Uiso 1 1 calc R . . H41B H -0.2210 0.2560 0.3906 0.079 Uiso 1 1 calc R . . N411 N -0.0742(9) 0.3212(6) 0.4026(9) 0.056(3) Uani 1 1 d . . . H411 H -0.0153 0.3270 0.4391 0.22(11) Uiso 1 1 calc R . . C412 C -0.0683(10) 0.2948(8) 0.2957(11) 0.075(5) Uani 1 1 d . . . H41C H -0.0605 0.2464 0.2820 0.112 Uiso 1 1 calc R . . H41D H -0.0114 0.3307 0.2790 0.112 Uiso 1 1 calc R . . H41E H -0.1290 0.2900 0.2560 0.112 Uiso 1 1 calc R . . C413 C -0.0841(10) 0.3975(8) 0.4205(10) 0.071(4) Uani 1 1 d . . . H41F H -0.0870 0.4169 0.4904 0.106 Uiso 1 1 calc R . . H41G H -0.1448 0.3926 0.3805 0.106 Uiso 1 1 calc R . . H41H H -0.0269 0.4319 0.4019 0.106 Uiso 1 1 calc R . . O51 O 0.0908(6) 0.3705(5) 0.5456(6) 0.049(2) Uani 1 1 d . . . C51 C 0.1870(12) 0.3899(8) 0.5313(11) 0.048(4) Uani 1 1 d . . . C52 C 0.2122(12) 0.3518(7) 0.4433(12) 0.050(4) Uani 1 1 d . . . O52 O 0.1326(7) 0.2970(5) 0.3748(7) 0.059(3) Uani 1 1 d . . . C521 C 0.1541(10) 0.2649(7) 0.2809(11) 0.069(4) Uani 1 1 d . . . H52A H 0.1832 0.3040 0.2491 0.104 Uiso 1 1 calc R . . H52B H 0.0930 0.2284 0.2393 0.104 Uiso 1 1 calc R . . H52C H 0.2010 0.2403 0.2900 0.104 Uiso 1 1 calc R . . C53 C 0.3150(13) 0.3670(9) 0.4301(12) 0.061(4) Uani 1 1 d . . . H53 H 0.3301 0.3391 0.3726 0.073 Uiso 1 1 calc R . . C54 C 0.3915(12) 0.4217(10) 0.5000(15) 0.071(5) Uani 1 1 d . . . H54 H 0.4584 0.4315 0.4908 0.085 Uiso 1 1 calc R . . C55 C 0.3679(10) 0.4610(8) 0.5826(13) 0.062(4) Uani 1 1 d . . . H55 H 0.4200 0.4989 0.6300 0.074 Uiso 1 1 calc R . . C56 C 0.2668(10) 0.4471(8) 0.6010(11) 0.049(4) Uani 1 1 d . . . C57 C 0.2507(12) 0.4924(8) 0.6925(11) 0.061(4) Uiso 1 1 d . . . H57 H 0.3069 0.5340 0.7281 0.074 Uiso 1 1 calc R . . N58 N 0.1698(8) 0.4836(6) 0.7319(8) 0.051(3) Uani 1 1 d . . . C59 C 0.1738(11) 0.5431(7) 0.8238(11) 0.069(4) Uani 1 1 d . . . H59A H 0.1419 0.5761 0.8054 0.083 Uiso 1 1 calc R . . H59B H 0.2438 0.5737 0.8514 0.083 Uiso 1 1 calc R . . C510 C 0.1228(10) 0.5119(8) 0.9032(11) 0.066(4) Uani 1 1 d . . . H51A H 0.0516 0.4848 0.8770 0.079 Uiso 1 1 calc R . . H51B H 0.1283 0.5539 0.9605 0.079 Uiso 1 1 calc R . . N511 N 0.1651(9) 0.4585(7) 0.9398(9) 0.063(3) Uani 1 1 d . . . H511 H 0.1508 0.4156 0.8882 0.14(8) Uiso 1 1 calc R . . C512 C 0.2765(12) 0.4931(8) 0.9705(13) 0.110(7) Uani 1 1 d . . . H51C H 0.3004 0.4580 0.9927 0.164 Uiso 1 1 calc R . . H51D H 0.2931 0.5388 1.0244 0.164 Uiso 1 1 calc R . . H51E H 0.3078 0.5048 0.9141 0.164 Uiso 1 1 calc R . . C513 C 0.1107(12) 0.4371(9) 1.0240(11) 0.097(6) Uani 1 1 d . . . H51F H 0.1367 0.4042 1.0492 0.145 Uiso 1 1 calc R . . H51G H 0.0399 0.4115 0.9993 0.145 Uiso 1 1 calc R . . H51H H 0.1210 0.4822 1.0773 0.145 Uiso 1 1 calc R . . N61 N -0.0483(8) 0.4508(7) 0.6966(8) 0.061(3) Uani 1 1 d . . . C62 C -0.1044(10) 0.4817(7) 0.7016(10) 0.049(4) Uani 1 1 d . . . S63 S -0.1778(3) 0.5297(2) 0.7032(3) 0.0820(14) Uani 1 1 d . . . Co3 Co 0.55942(15) 0.26346(11) 0.03832(15) 0.0655(7) Uani 1 1 d . . . N71 N 0.6595(10) 0.2923(7) -0.0488(9) 0.075(4) Uani 1 1 d . . . C72 C 0.7306(12) 0.3031(8) -0.0895(11) 0.062(4) Uani 1 1 d . . . S73 S 0.8245(4) 0.3199(3) -0.1471(4) 0.1079(17) Uani 1 1 d . . . N81 N 0.5249(9) 0.3506(7) 0.1072(10) 0.087(4) Uani 1 1 d . . . C82A C 0.482(2) 0.3865(17) 0.1443(19) 0.053(8) Uiso 0.60 1 d P . . C82B C 0.509(3) 0.412(2) 0.120(3) 0.060(13) Uiso 0.40 1 d P . . S83A S 0.4209(9) 0.4411(8) 0.1927(10) 0.120(5) Uani 0.60 1 d P . . S83B S 0.4732(15) 0.4760(11) 0.1454(17) 0.145(8) Uani 0.40 1 d P . . N91 N 0.6196(10) 0.2191(8) 0.1271(11) 0.090(5) Uani 1 1 d . . . C92 C 0.6502(12) 0.1773(9) 0.1495(12) 0.074(5) Uani 1 1 d . . . S93 S 0.6927(4) 0.1165(3) 0.1764(4) 0.1010(16) Uani 1 1 d . . . N101 N 0.4341(10) 0.1869(7) -0.0334(10) 0.080(5) Uani 1 1 d . . . C502 C 0.3618(13) 0.1352(8) -0.0649(11) 0.061(5) Uani 1 1 d . . . S103 S 0.2530(3) 0.0652(2) -0.1167(3) 0.0831(14) Uani 1 1 d . . . C991 C 0.928(4) 0.267(3) 0.047(4) 0.079(16) Uiso 0.30 1 d P . . C992 C 0.925(6) 0.162(5) 0.084(6) 0.15(3) Uiso 0.30 1 d P . . C993 C 1.012(6) 0.102(4) 0.069(6) 0.14(3) Uiso 0.30 1 d P . . C994 C 0.944(7) 0.118(5) 0.087(6) 0.15(3) Uiso 0.30 1 d P . . C995 C 1.019(6) 0.038(4) 0.044(5) 0.15(3) Uiso 0.30 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 0.0317(12) 0.0481(12) 0.0549(13) 0.0200(10) 0.0072(10) 0.0154(10) O11 0.037(6) 0.061(6) 0.052(6) 0.028(5) 0.024(5) 0.020(5) C11 0.038(10) 0.079(12) 0.025(10) 0.026(9) 0.019(9) 0.040(10) C12 0.051(12) 0.052(11) 0.042(12) 0.005(10) -0.010(10) 0.031(10) O12 0.053(7) 0.073(7) 0.039(7) 0.011(6) -0.007(6) 0.029(6) C121 0.098(15) 0.146(17) 0.054(12) 0.021(12) -0.001(11) 0.034(14) C13 0.036(10) 0.050(11) 0.064(13) 0.007(9) -0.006(9) 0.026(9) C14 0.027(10) 0.055(11) 0.075(12) 0.018(10) 0.010(10) 0.001(8) C15 0.032(10) 0.057(10) 0.061(12) 0.025(10) 0.008(9) 0.012(9) C16 0.036(10) 0.036(10) 0.057(12) -0.001(9) 0.004(9) 0.016(9) C17 0.056(12) 0.064(12) 0.093(15) 0.053(11) 0.041(11) 0.035(10) N18 0.065(9) 0.034(7) 0.041(8) 0.008(6) 0.009(7) 0.026(7) C19 0.075(12) 0.074(12) 0.058(12) 0.024(9) 0.004(10) 0.026(10) C110 0.049(10) 0.071(12) 0.049(10) -0.009(8) -0.007(8) 0.012(10) N111 0.066(9) 0.049(8) 0.044(7) 0.007(6) 0.009(7) 0.021(7) C112 0.056(11) 0.103(13) 0.059(11) 0.008(9) 0.028(9) 0.007(10) C113 0.082(12) 0.063(12) 0.060(10) 0.003(8) 0.003(9) 0.022(10) O21 0.035(5) 0.053(6) 0.031(5) 0.017(5) 0.001(4) 0.013(5) C21 0.004(7) 0.055(9) 0.022(9) -0.008(7) 0.003(6) 0.002(7) C22 0.036(9) 0.037(9) 0.050(10) -0.006(8) 0.020(8) 0.010(8) O22 0.039(6) 0.085(8) 0.082(8) 0.009(6) 0.019(6) 0.044(6) C221 0.084(13) 0.138(16) 0.080(13) 0.012(11) 0.027(10) 0.067(13) C23 0.038(10) 0.027(9) 0.137(17) 0.017(11) -0.019(11) 0.004(8) C24 0.059(12) 0.056(11) 0.088(14) 0.025(10) -0.014(10) 0.009(10) C25 0.068(11) 0.053(10) 0.057(11) 0.010(9) 0.009(9) 0.020(9) C26 0.042(9) 0.029(8) 0.051(10) 0.017(7) 0.013(8) 0.024(7) C27 0.046(10) 0.046(10) 0.061(10) 0.017(8) 0.012(8) -0.003(8) N28 0.031(7) 0.038(7) 0.055(8) 0.010(6) 0.019(6) 0.003(6) C29 0.038(9) 0.059(11) 0.063(10) 0.014(8) 0.025(8) 0.021(8) C210 0.069(12) 0.064(11) 0.062(10) 0.029(9) 0.031(9) 0.042(10) N211 0.039(8) 0.045(8) 0.052(8) 0.006(6) 0.011(7) 0.019(6) C212 0.076(11) 0.119(13) 0.048(9) 0.056(9) 0.041(8) 0.066(10) C213 0.058(10) 0.043(10) 0.075(11) 0.016(8) 0.004(8) 0.027(8) N31 0.022(7) 0.101(11) 0.154(13) 0.080(9) 0.020(8) 0.028(8) C32 0.036(11) 0.083(13) 0.148(16) 0.074(11) 0.033(11) 0.023(10) S33 0.040(3) 0.114(4) 0.279(8) 0.105(5) 0.022(4) 0.025(3) Co2 0.0293(11) 0.0427(12) 0.0542(13) 0.0148(10) 0.0010(9) 0.0115(10) O41 0.039(6) 0.054(6) 0.039(5) 0.019(5) -0.005(4) 0.017(5) C41 0.033(9) 0.041(11) 0.066(11) 0.032(9) 0.024(8) 0.014(9) C42 0.037(10) 0.056(11) 0.055(10) 0.021(9) 0.013(8) 0.030(9) O42 0.070(8) 0.070(8) 0.057(7) 0.020(6) -0.002(6) 0.030(7) C421 0.088(14) 0.096(14) 0.085(14) 0.015(11) -0.031(11) 0.026(11) C43 0.058(12) 0.068(12) 0.087(12) 0.038(11) 0.031(10) 0.047(11) C44 0.052(11) 0.045(10) 0.090(13) 0.018(10) 0.019(10) 0.000(10) C45 0.032(9) 0.057(12) 0.060(10) 0.008(8) -0.001(8) 0.007(9) C46 0.027(9) 0.010(8) 0.077(11) 0.014(8) 0.027(9) -0.004(8) C47 0.031(9) 0.066(12) 0.063(11) 0.016(9) 0.020(8) 0.016(9) N48 0.037(8) 0.044(8) 0.048(8) 0.016(6) 0.003(6) 0.001(6) C49 0.034(9) 0.056(10) 0.050(10) 0.016(8) -0.027(8) -0.011(8) C410 0.040(10) 0.078(12) 0.070(12) 0.035(10) -0.016(9) 0.004(9) N411 0.042(8) 0.065(9) 0.041(8) 0.009(7) -0.009(7) 0.002(7) C412 0.052(11) 0.085(12) 0.088(14) 0.039(10) -0.005(9) 0.017(9) C413 0.074(12) 0.076(12) 0.058(10) 0.024(9) 0.006(9) 0.019(10) O51 0.019(5) 0.062(6) 0.062(6) 0.026(5) 0.003(5) 0.005(5) C51 0.049(12) 0.033(9) 0.063(11) 0.018(9) 0.000(10) 0.012(10) C52 0.068(13) 0.018(8) 0.072(12) 0.014(8) 0.015(10) 0.022(9) O52 0.063(7) 0.052(7) 0.057(7) 0.004(6) 0.007(6) 0.024(6) C521 0.074(12) 0.063(11) 0.078(12) 0.011(9) 0.014(9) 0.039(9) C53 0.051(12) 0.088(13) 0.076(12) 0.043(11) 0.031(10) 0.046(11) C54 0.024(11) 0.091(14) 0.111(15) 0.047(12) 0.028(12) 0.022(11) C55 0.021(10) 0.084(12) 0.098(13) 0.053(10) 0.021(9) 0.018(9) C56 0.028(10) 0.046(9) 0.079(11) 0.033(9) 0.007(9) 0.011(8) N58 0.048(8) 0.046(7) 0.050(8) 0.010(6) -0.009(6) 0.010(6) C59 0.075(12) 0.044(10) 0.068(12) -0.005(9) 0.004(10) 0.013(9) C510 0.056(11) 0.055(11) 0.071(12) -0.011(9) -0.014(9) 0.026(9) N511 0.073(10) 0.058(9) 0.063(9) 0.016(8) 0.003(8) 0.032(8) C512 0.075(14) 0.061(12) 0.164(18) 0.021(11) -0.051(13) 0.007(11) C513 0.111(15) 0.136(16) 0.066(12) 0.042(11) 0.019(11) 0.061(13) N61 0.046(8) 0.072(9) 0.058(8) 0.001(7) 0.004(7) 0.025(7) C62 0.032(9) 0.035(9) 0.062(10) -0.007(7) 0.000(8) 0.006(8) S63 0.066(3) 0.066(3) 0.124(4) 0.025(3) 0.000(3) 0.039(3) Co3 0.0524(14) 0.0760(16) 0.0691(15) 0.0217(12) 0.0148(12) 0.0228(12) N71 0.062(10) 0.081(10) 0.083(11) 0.009(8) 0.015(8) 0.034(8) C72 0.067(12) 0.055(10) 0.052(11) -0.010(8) 0.001(9) 0.025(10) S73 0.082(4) 0.118(4) 0.107(4) 0.004(3) 0.048(3) 0.030(3) N81 0.060(9) 0.075(10) 0.113(12) 0.014(8) 0.008(8) 0.019(8) S83A 0.090(9) 0.146(12) 0.111(9) -0.021(7) -0.012(6) 0.073(9) S83B 0.119(17) 0.125(17) 0.17(2) -0.035(13) -0.043(13) 0.091(14) N91 0.087(11) 0.123(13) 0.096(11) 0.064(10) 0.023(8) 0.057(10) C92 0.058(12) 0.076(13) 0.079(13) 0.037(10) 0.005(9) 0.004(10) S93 0.107(4) 0.105(4) 0.087(4) 0.039(3) -0.014(3) 0.030(3) N101 0.080(11) 0.040(8) 0.089(11) 0.001(8) 0.030(9) -0.009(8) C502 0.098(15) 0.039(10) 0.056(11) 0.021(9) 0.025(11) 0.032(11) S103 0.074(3) 0.078(3) 0.096(3) 0.048(3) -0.003(3) 0.013(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 O11 1.962(9) . ? Co1 O21 1.970(8) . ? Co1 N31 2.058(12) . ? Co1 N28 2.117(10) . ? Co1 N18 2.119(11) . ? O11 C11 1.329(14) . ? C11 C16 1.381(16) . ? C11 C12 1.382(17) . ? C12 O12 1.346(15) . ? C12 C13 1.394(17) . ? O12 C121 1.437(16) . ? C121 H12A 0.9600 . ? C121 H12B 0.9600 . ? C121 H12C 0.9600 . ? C13 C14 1.394(17) . ? C13 H13 0.9300 . ? C14 C15 1.328(17) . ? C14 H14 0.9300 . ? C15 C16 1.411(16) . ? C15 H15 0.9300 . ? C16 C17 1.426(18) . ? C17 N18 1.324(16) . ? C17 H17 0.9300 . ? N18 C19 1.455(15) . ? C19 C110 1.497(17) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C110 N111 1.471(15) . ? C110 H11A 0.9700 . ? C110 H11B 0.9700 . ? N111 C113 1.484(14) . ? N111 C112 1.492(15) . ? N111 H111 0.9100 . ? C112 H11C 0.9600 . ? C112 H11D 0.9600 . ? C112 H11E 0.9600 . ? C113 H11F 0.9600 . ? C113 H11G 0.9600 . ? C113 H11H 0.9600 . ? O21 C21 1.339(13) . ? C21 C26 1.389(15) . ? C21 C22 1.404(16) . ? C22 O22 1.342(14) . ? C22 C23 1.418(18) . ? O22 C221 1.459(14) . ? C221 H22A 0.9600 . ? C221 H22B 0.9600 . ? C221 H22C 0.9600 . ? C23 C24 1.375(19) . ? C23 H23 0.9300 . ? C24 C25 1.375(17) . ? C24 H24 0.9300 . ? C25 C26 1.397(16) . ? C25 H25 0.9300 . ? C26 C27 1.464(16) . ? C27 N28 1.297(14) . ? C27 H27 0.9300 . ? N28 C29 1.492(13) . ? C29 C210 1.470(15) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C210 N211 1.500(15) . ? C210 H21A 0.9700 . ? C210 H21B 0.9700 . ? N211 C212 1.495(13) . ? N211 C213 1.508(13) . ? N211 H211 0.9100 . ? C212 H21C 0.9600 . ? C212 H21D 0.9600 . ? C212 H21E 0.9600 . ? C213 H21F 0.9600 . ? C213 H21G 0.9600 . ? C213 H21H 0.9600 . ? N31 C32 1.114(14) . ? C32 S33 1.622(16) . ? Co2 O51 1.945(9) . ? Co2 O41 2.001(8) . ? Co2 N61 2.025(12) . ? Co2 N48 2.080(11) . ? Co2 N58 2.122(11) . ? O41 C41 1.337(13) . ? C41 C46 1.380(17) . ? C41 C42 1.432(16) . ? C42 C43 1.368(17) . ? C42 O42 1.400(15) . ? O42 C421 1.428(15) . ? C421 H42A 0.9600 . ? C421 H42B 0.9600 . ? C421 H42C 0.9600 . ? C43 C44 1.393(18) . ? C43 H43 0.9300 . ? C44 C45 1.401(17) . ? C44 H44 0.9300 . ? C45 C46 1.370(15) . ? C45 H45 0.9300 . ? C46 C47 1.480(17) . ? C47 N48 1.282(15) . ? C47 H47 0.9300 . ? N48 C49 1.468(14) . ? C49 C410 1.506(17) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C410 N411 1.493(15) . ? C410 H41A 0.9700 . ? C410 H41B 0.9700 . ? N411 C412 1.462(16) . ? N411 C413 1.502(15) . ? N411 H411 0.9100 . ? C412 H41C 0.9600 . ? C412 H41D 0.9600 . ? C412 H41E 0.9600 . ? C413 H41F 0.9600 . ? C413 H41G 0.9600 . ? C413 H41H 0.9600 . ? O51 C51 1.334(15) . ? C51 C52 1.399(17) . ? C51 C56 1.401(17) . ? C52 O52 1.376(15) . ? C52 C53 1.425(18) . ? O52 C521 1.399(14) . ? C521 H52A 0.9600 . ? C521 H52B 0.9600 . ? C521 H52C 0.9600 . ? C53 C54 1.361(19) . ? C53 H53 0.9300 . ? C54 C55 1.342(18) . ? C54 H54 0.9300 . ? C55 C56 1.424(16) . ? C55 H55 0.9300 . ? C56 C57 1.436(17) . ? C57 N58 1.281(15) . ? C57 H57 0.9300 . ? N58 C59 1.484(15) . ? C59 C510 1.495(17) . ? C59 H59A 0.9700 . ? C59 H59B 0.9700 . ? C510 N511 1.528(15) . ? C510 H51A 0.9700 . ? C510 H51B 0.9700 . ? N511 C512 1.488(16) . ? N511 C513 1.505(16) . ? N511 H511 0.9100 . ? C512 H51C 0.9600 . ? C512 H51D 0.9600 . ? C512 H51E 0.9600 . ? C513 H51F 0.9600 . ? C513 H51G 0.9600 . ? C513 H51H 0.9600 . ? N61 C62 1.145(13) . ? C62 S63 1.616(14) . ? Co3 N101 1.918(14) . ? Co3 N71 1.951(14) . ? Co3 N81 1.964(13) . ? Co3 N91 1.967(14) . ? N71 C72 1.172(16) . ? C72 S73 1.579(17) . ? N81 C82A 1.13(3) . ? N81 C82B 1.26(4) . ? C82A C82B 0.69(4) . ? C82A S83A 1.64(3) . ? C82A S83B 1.78(4) . ? C82B S83B 1.48(4) . ? C82B S83A 1.81(5) . ? S83A S83B 1.18(2) . ? N91 C92 1.137(16) . ? C92 S93 1.603(18) . ? N101 C502 1.141(16) . ? C502 S103 1.658(18) . ? C992 C994 0.99(10) . ? C992 C993 1.95(11) . ? C993 C994 1.13(9) . ? C993 C995 1.25(8) . ? C995 C995 1.59(13) 2_755 ? 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 O11 Co1 O21 115.2(3) . . ? O11 Co1 N31 124.0(4) . . ? O21 Co1 N31 120.8(4) . . ? O11 Co1 N28 87.5(4) . . ? O21 Co1 N28 90.0(4) . . ? N31 Co1 N28 91.0(5) . . ? O11 Co1 N18 90.0(4) . . ? O21 Co1 N18 90.7(3) . . ? N31 Co1 N18 90.8(5) . . ? N28 Co1 N18 177.5(5) . . ? C11 O11 Co1 129.5(8) . . ? O11 C11 C16 124.5(14) . . ? O11 C11 C12 119.0(13) . . ? C16 C11 C12 116.5(14) . . ? O12 C12 C11 115.6(14) . . ? O12 C12 C13 122.2(14) . . ? C11 C12 C13 121.9(14) . . ? C12 O12 C121 119.7(12) . . ? O12 C121 H12A 109.5 . . ? O12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? O12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? C14 C13 C12 118.7(13) . . ? C14 C13 H13 120.6 . . ? C12 C13 H13 120.6 . . ? C15 C14 C13 121.0(13) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.3(14) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C11 C16 C15 122.2(14) . . ? C11 C16 C17 125.0(14) . . ? C15 C16 C17 112.8(14) . . ? N18 C17 C16 127.5(13) . . ? N18 C17 H17 116.3 . . ? C16 C17 H17 116.3 . . ? C17 N18 C19 116.3(12) . . ? C17 N18 Co1 122.4(9) . . ? C19 N18 Co1 120.7(9) . . ? N18 C19 C110 112.0(11) . . ? N18 C19 H19A 109.2 . . ? C110 C19 H19A 109.2 . . ? N18 C19 H19B 109.2 . . ? C110 C19 H19B 109.2 . . ? H19A C19 H19B 107.9 . . ? N111 C110 C19 117.9(11) . . ? N111 C110 H11A 107.8 . . ? C19 C110 H11A 107.8 . . ? N111 C110 H11B 107.8 . . ? C19 C110 H11B 107.8 . . ? H11A C110 H11B 107.2 . . ? C110 N111 C113 111.1(10) . . ? C110 N111 C112 116.0(11) . . ? C113 N111 C112 110.6(10) . . ? C110 N111 H111 106.1 . . ? C113 N111 H111 106.1 . . ? C112 N111 H111 106.1 . . ? N111 C112 H11C 109.5 . . ? N111 C112 H11D 109.5 . . ? H11C C112 H11D 109.5 . . ? N111 C112 H11E 109.5 . . ? H11C C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? N111 C113 H11F 109.5 . . ? N111 C113 H11G 109.5 . . ? H11F C113 H11G 109.5 . . ? N111 C113 H11H 109.5 . . ? H11F C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? C21 O21 Co1 125.8(7) . . ? O21 C21 C26 125.8(11) . . ? O21 C21 C22 117.9(11) . . ? C26 C21 C22 116.2(13) . . ? O22 C22 C21 114.4(13) . . ? O22 C22 C23 124.0(14) . . ? C21 C22 C23 121.4(13) . . ? C22 O22 C221 118.9(11) . . ? O22 C221 H22A 109.5 . . ? O22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? O22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? C24 C23 C22 120.0(14) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C25 C24 C23 119.4(15) . . ? C25 C24 H24 120.3 . . ? C23 C24 H24 120.3 . . ? C24 C25 C26 120.4(13) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 122.4(11) . . ? C21 C26 C27 123.0(12) . . ? C25 C26 C27 114.6(13) . . ? N28 C27 C26 127.1(12) . . ? N28 C27 H27 116.4 . . ? C26 C27 H27 116.4 . . ? C27 N28 C29 115.7(10) . . ? C27 N28 Co1 122.6(8) . . ? C29 N28 Co1 121.6(8) . . ? C210 C29 N28 112.1(10) . . ? C210 C29 H29A 109.2 . . ? N28 C29 H29A 109.2 . . ? C210 C29 H29B 109.2 . . ? N28 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? C29 C210 N211 115.6(10) . . ? C29 C210 H21A 108.4 . . ? N211 C210 H21A 108.4 . . ? C29 C210 H21B 108.4 . . ? N211 C210 H21B 108.4 . . ? H21A C210 H21B 107.4 . . ? C212 N211 C210 114.0(10) . . ? C212 N211 C213 110.9(10) . . ? C210 N211 C213 110.1(10) . . ? C212 N211 H211 107.2 . . ? C210 N211 H211 107.2 . . ? C213 N211 H211 107.2 . . ? N211 C212 H21C 109.5 . . ? N211 C212 H21D 109.5 . . ? H21C C212 H21D 109.5 . . ? N211 C212 H21E 109.5 . . ? H21C C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? N211 C213 H21F 109.5 . . ? N211 C213 H21G 109.5 . . ? H21F C213 H21G 109.5 . . ? N211 C213 H21H 109.5 . . ? H21F C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? C32 N31 Co1 166.9(15) . . ? N31 C32 S33 178.9(16) . . ? O51 Co2 O41 118.9(3) . . ? O51 Co2 N61 119.2(4) . . ? O41 Co2 N61 121.9(4) . . ? O51 Co2 N48 90.9(4) . . ? O41 Co2 N48 90.4(4) . . ? N61 Co2 N48 91.6(5) . . ? O51 Co2 N58 88.1(4) . . ? O41 Co2 N58 88.9(4) . . ? N61 Co2 N58 90.1(4) . . ? N48 Co2 N58 178.3(4) . . ? C41 O41 Co2 125.0(8) . . ? O41 C41 C46 127.4(12) . . ? O41 C41 C42 117.1(13) . . ? C46 C41 C42 115.4(13) . . ? C43 C42 O42 123.5(14) . . ? C43 C42 C41 123.3(15) . . ? O42 C42 C41 113.0(13) . . ? C42 O42 C421 116.6(11) . . ? O42 C421 H42A 109.5 . . ? O42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? O42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? C42 C43 C44 118.1(14) . . ? C42 C43 H43 121.0 . . ? C44 C43 H43 121.0 . . ? C43 C44 C45 120.6(13) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C46 C45 C44 119.3(14) . . ? C46 C45 H45 120.4 . . ? C44 C45 H45 120.4 . . ? C45 C46 C41 123.1(14) . . ? C45 C46 C47 114.1(14) . . ? C41 C46 C47 122.8(11) . . ? N48 C47 C46 126.2(13) . . ? N48 C47 H47 116.9 . . ? C46 C47 H47 116.9 . . ? C47 N48 C49 113.1(11) . . ? C47 N48 Co2 124.8(10) . . ? C49 N48 Co2 122.1(8) . . ? N48 C49 C410 114.4(11) . . ? N48 C49 H49A 108.7 . . ? C410 C49 H49A 108.7 . . ? N48 C49 H49B 108.7 . . ? C410 C49 H49B 108.7 . . ? H49A C49 H49B 107.6 . . ? N411 C410 C49 115.3(12) . . ? N411 C410 H41A 108.4 . . ? C49 C410 H41A 108.4 . . ? N411 C410 H41B 108.4 . . ? C49 C410 H41B 108.4 . . ? H41A C410 H41B 107.5 . . ? C412 N411 C410 110.6(11) . . ? C412 N411 C413 107.4(11) . . ? C410 N411 C413 113.5(11) . . ? C412 N411 H411 108.4 . . ? C410 N411 H411 108.4 . . ? C413 N411 H411 108.4 . . ? N411 C412 H41C 109.5 . . ? N411 C412 H41D 109.5 . . ? H41C C412 H41D 109.5 . . ? N411 C412 H41E 109.5 . . ? H41C C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? N411 C413 H41F 109.5 . . ? N411 C413 H41G 109.5 . . ? H41F C413 H41G 109.5 . . ? N411 C413 H41H 109.5 . . ? H41F C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? C51 O51 Co2 128.3(8) . . ? O51 C51 C52 119.8(14) . . ? O51 C51 C56 123.4(13) . . ? C52 C51 C56 116.7(14) . . ? O52 C52 C51 115.9(14) . . ? O52 C52 C53 123.2(14) . . ? C51 C52 C53 120.9(15) . . ? C52 O52 C521 117.0(11) . . ? O52 C521 H52A 109.5 . . ? O52 C521 H52B 109.5 . . ? H52A C521 H52B 109.5 . . ? O52 C521 H52C 109.5 . . ? H52A C521 H52C 109.5 . . ? H52B C521 H52C 109.5 . . ? C54 C53 C52 121.2(14) . . ? C54 C53 H53 119.4 . . ? C52 C53 H53 119.4 . . ? C55 C54 C53 118.4(14) . . ? C55 C54 H54 120.8 . . ? C53 C54 H54 120.8 . . ? C54 C55 C56 122.9(15) . . ? C54 C55 H55 118.5 . . ? C56 C55 H55 118.5 . . ? C51 C56 C55 119.7(14) . . ? C51 C56 C57 122.2(13) . . ? C55 C56 C57 118.0(15) . . ? N58 C57 C56 129.2(14) . . ? N58 C57 H57 115.4 . . ? C56 C57 H57 115.4 . . ? C57 N58 C59 117.2(12) . . ? C57 N58 Co2 121.4(10) . . ? C59 N58 Co2 121.3(9) . . ? N58 C59 C510 113.4(11) . . ? N58 C59 H59A 108.9 . . ? C510 C59 H59A 108.9 . . ? N58 C59 H59B 108.9 . . ? C510 C59 H59B 108.9 . . ? H59A C59 H59B 107.7 . . ? C59 C510 N511 114.8(11) . . ? C59 C510 H51A 108.6 . . ? N511 C510 H51A 108.6 . . ? C59 C510 H51B 108.6 . . ? N511 C510 H51B 108.6 . . ? H51A C510 H51B 107.5 . . ? C512 N511 C513 112.5(12) . . ? C512 N511 C510 111.7(11) . . ? C513 N511 C510 107.7(11) . . ? C512 N511 H511 108.2 . . ? C513 N511 H511 108.2 . . ? C510 N511 H511 108.2 . . ? N511 C512 H51C 109.5 . . ? N511 C512 H51D 109.5 . . ? H51C C512 H51D 109.5 . . ? N511 C512 H51E 109.5 . . ? H51C C512 H51E 109.5 . . ? H51D C512 H51E 109.5 . . ? N511 C513 H51F 109.5 . . ? N511 C513 H51G 109.5 . . ? H51F C513 H51G 109.5 . . ? N511 C513 H51H 109.5 . . ? H51F C513 H51H 109.5 . . ? H51G C513 H51H 109.5 . . ? C62 N61 Co2 172.4(11) . . ? N61 C62 S63 175.1(14) . . ? N101 Co3 N71 113.3(5) . . ? N101 Co3 N81 105.5(5) . . ? N71 Co3 N81 110.9(5) . . ? N101 Co3 N91 107.4(6) . . ? N71 Co3 N91 104.6(5) . . ? N81 Co3 N91 115.4(6) . . ? C72 N71 Co3 165.6(13) . . ? N71 C72 S73 177.3(15) . . ? C82A N81 C82B 33(2) . . ? C82A N81 Co3 162.4(19) . . ? C82B N81 Co3 158(2) . . ? C82B C82A N81 84(5) . . ? C82B C82A S83A 93(6) . . ? N81 C82A S83A 177(3) . . ? C82B C82A S83B 53(5) . . ? N81 C82A S83B 137(3) . . ? S83A C82A S83B 40.0(10) . . ? C82A C82B N81 63(5) . . ? C82A C82B S83B 105(6) . . ? N81 C82B S83B 168(4) . . ? C82A C82B S83A 64(5) . . ? N81 C82B S83A 127(3) . . ? S83B C82B S83A 40.3(14) . . ? S83B S83A C82A 76.8(15) . . ? S83B S83A C82B 54.4(17) . . ? C82A S83A C82B 22.5(15) . . ? S83A S83B C82B 85(2) . . ? S83A S83B C82A 63.2(15) . . ? C82B S83B C82A 22.1(18) . . ? C92 N91 Co3 158.1(16) . . ? N91 C92 S93 177.7(18) . . ? C502 N101 Co3 168.7(14) . . ? N101 C502 S103 174.4(15) . . ? C994 C992 C993 25(7) . . ? C994 C993 C995 129(10) . . ? C994 C993 C992 22(6) . . ? C995 C993 C992 148(8) . . ? C992 C994 C993 133(10) . . ? C993 C995 C995 141(10) . 2_755 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O21 Co1 O11 C11 80.1(9) . . . . ? N31 Co1 O11 C11 -101.6(10) . . . . ? N28 Co1 O11 C11 168.9(9) . . . . ? N18 Co1 O11 C11 -10.7(9) . . . . ? Co1 O11 C11 C16 11.2(16) . . . . ? Co1 O11 C11 C12 -167.6(8) . . . . ? O11 C11 C12 O12 0.0(16) . . . . ? C16 C11 C12 O12 -178.9(10) . . . . ? O11 C11 C12 C13 -174.8(10) . . . . ? C16 C11 C12 C13 6.3(17) . . . . ? C11 C12 O12 C121 -176.9(11) . . . . ? C13 C12 O12 C121 -2.1(17) . . . . ? O12 C12 C13 C14 -178.6(11) . . . . ? C11 C12 C13 C14 -4.1(17) . . . . ? C12 C13 C14 C15 -0.7(18) . . . . ? C13 C14 C15 C16 2.9(19) . . . . ? O11 C11 C16 C15 177.1(11) . . . . ? C12 C11 C16 C15 -4.1(17) . . . . ? O11 C11 C16 C17 -1.0(19) . . . . ? C12 C11 C16 C17 177.8(11) . . . . ? C14 C15 C16 C11 -0.4(18) . . . . ? C14 C15 C16 C17 177.9(11) . . . . ? C11 C16 C17 N18 -7(2) . . . . ? C15 C16 C17 N18 174.9(11) . . . . ? C16 C17 N18 C19 174.3(12) . . . . ? C16 C17 N18 Co1 3.8(17) . . . . ? O11 Co1 N18 C17 3.3(9) . . . . ? O21 Co1 N18 C17 -111.9(9) . . . . ? N31 Co1 N18 C17 127.3(10) . . . . ? N28 Co1 N18 C17 -7(10) . . . . ? O11 Co1 N18 C19 -166.8(9) . . . . ? O21 Co1 N18 C19 78.0(9) . . . . ? N31 Co1 N18 C19 -42.8(9) . . . . ? N28 Co1 N18 C19 -177(100) . . . . ? C17 N18 C19 C110 143.3(11) . . . . ? Co1 N18 C19 C110 -46.0(14) . . . . ? N18 C19 C110 N111 -57.9(16) . . . . ? C19 C110 N111 C113 -173.8(11) . . . . ? C19 C110 N111 C112 -46.3(16) . . . . ? O11 Co1 O21 C21 61.5(8) . . . . ? N31 Co1 O21 C21 -116.9(9) . . . . ? N28 Co1 O21 C21 -25.7(8) . . . . ? N18 Co1 O21 C21 151.8(8) . . . . ? Co1 O21 C21 C26 22.8(15) . . . . ? Co1 O21 C21 C22 -160.8(8) . . . . ? O21 C21 C22 O22 3.8(15) . . . . ? C26 C21 C22 O22 -179.5(10) . . . . ? O21 C21 C22 C23 178.4(10) . . . . ? C26 C21 C22 C23 -4.9(17) . . . . ? C21 C22 O22 C221 177.6(11) . . . . ? C23 C22 O22 C221 3.2(18) . . . . ? O22 C22 C23 C24 178.9(13) . . . . ? C21 C22 C23 C24 4.9(19) . . . . ? C22 C23 C24 C25 -3(2) . . . . ? C23 C24 C25 C26 2(2) . . . . ? O21 C21 C26 C25 179.9(11) . . . . ? C22 C21 C26 C25 3.5(17) . . . . ? O21 C21 C26 C27 0.2(18) . . . . ? C22 C21 C26 C27 -176.2(11) . . . . ? C24 C25 C26 C21 -2.0(19) . . . . ? C24 C25 C26 C27 177.7(12) . . . . ? C21 C26 C27 N28 -12.1(19) . . . . ? C25 C26 C27 N28 168.2(13) . . . . ? C26 C27 N28 C29 177.1(11) . . . . ? C26 C27 N28 Co1 0.0(18) . . . . ? O11 Co1 N28 C27 -100.5(10) . . . . ? O21 Co1 N28 C27 14.7(10) . . . . ? N31 Co1 N28 C27 135.6(10) . . . . ? N18 Co1 N28 C27 -90(9) . . . . ? O11 Co1 N28 C29 82.6(8) . . . . ? O21 Co1 N28 C29 -162.2(8) . . . . ? N31 Co1 N28 C29 -41.4(9) . . . . ? N18 Co1 N28 C29 93(9) . . . . ? C27 N28 C29 C210 136.9(12) . . . . ? Co1 N28 C29 C210 -45.9(13) . . . . ? N28 C29 C210 N211 -55.7(14) . . . . ? C29 C210 N211 C212 -48.7(14) . . . . ? C29 C210 N211 C213 -174.1(10) . . . . ? O11 Co1 N31 C32 -54(6) . . . . ? O21 Co1 N31 C32 124(5) . . . . ? N28 Co1 N31 C32 34(5) . . . . ? N18 Co1 N31 C32 -144(5) . . . . ? Co1 N31 C32 S33 161(76) . . . . ? O51 Co2 O41 C41 -72.0(9) . . . . ? N61 Co2 O41 C41 111.4(9) . . . . ? N48 Co2 O41 C41 19.2(8) . . . . ? N58 Co2 O41 C41 -159.2(9) . . . . ? Co2 O41 C41 C46 -14.3(16) . . . . ? Co2 O41 C41 C42 168.3(7) . . . . ? O41 C41 C42 C43 -177.5(10) . . . . ? C46 C41 C42 C43 4.8(17) . . . . ? O41 C41 C42 O42 -1.7(15) . . . . ? C46 C41 C42 O42 -179.4(10) . . . . ? C43 C42 O42 C421 -12.0(17) . . . . ? C41 C42 O42 C421 172.2(11) . . . . ? O42 C42 C43 C44 -178.0(11) . . . . ? C41 C42 C43 C44 -2.5(19) . . . . ? C42 C43 C44 C45 0(2) . . . . ? C43 C44 C45 C46 0.2(19) . . . . ? C44 C45 C46 C41 2.3(18) . . . . ? C44 C45 C46 C47 -176.0(11) . . . . ? O41 C41 C46 C45 178.0(11) . . . . ? C42 C41 C46 C45 -4.6(17) . . . . ? O41 C41 C46 C47 -3.9(18) . . . . ? C42 C41 C46 C47 173.6(10) . . . . ? C45 C46 C47 N48 -171.4(12) . . . . ? C41 C46 C47 N48 10.2(19) . . . . ? C46 C47 N48 C49 -176.9(11) . . . . ? C46 C47 N48 Co2 2.3(17) . . . . ? O51 Co2 N48 C47 105.2(10) . . . . ? O41 Co2 N48 C47 -13.7(10) . . . . ? N61 Co2 N48 C47 -135.6(10) . . . . ? N58 Co2 N48 C47 52(15) . . . . ? O51 Co2 N48 C49 -75.7(9) . . . . ? O41 Co2 N48 C49 165.5(9) . . . . ? N61 Co2 N48 C49 43.5(9) . . . . ? N58 Co2 N48 C49 -129(14) . . . . ? C47 N48 C49 C410 -92.1(13) . . . . ? Co2 N48 C49 C410 88.6(12) . . . . ? N48 C49 C410 N411 -67.2(15) . . . . ? C49 C410 N411 C412 179.8(11) . . . . ? C49 C410 N411 C413 -59.4(15) . . . . ? O41 Co2 O51 C51 -58.0(10) . . . . ? N61 Co2 O51 C51 118.7(9) . . . . ? N48 Co2 O51 C51 -149.0(10) . . . . ? N58 Co2 O51 C51 29.7(9) . . . . ? Co2 O51 C51 C52 156.6(9) . . . . ? Co2 O51 C51 C56 -22.9(16) . . . . ? O51 C51 C52 O52 2.0(16) . . . . ? C56 C51 C52 O52 -178.6(10) . . . . ? O51 C51 C52 C53 -174.7(10) . . . . ? C56 C51 C52 C53 4.8(17) . . . . ? C51 C52 O52 C521 172.1(10) . . . . ? C53 C52 O52 C521 -11.4(17) . . . . ? O52 C52 C53 C54 -179.8(13) . . . . ? C51 C52 C53 C54 -3.4(19) . . . . ? C52 C53 C54 C55 0(2) . . . . ? C53 C54 C55 C56 1(2) . . . . ? O51 C51 C56 C55 176.1(10) . . . . ? C52 C51 C56 C55 -3.4(17) . . . . ? O51 C51 C56 C57 -2.9(18) . . . . ? C52 C51 C56 C57 177.6(11) . . . . ? C54 C55 C56 C51 0.5(19) . . . . ? C54 C55 C56 C57 179.5(14) . . . . ? C51 C56 C57 N58 10(2) . . . . ? C55 C56 C57 N58 -169.1(13) . . . . ? C56 C57 N58 C59 -175.5(13) . . . . ? C56 C57 N58 Co2 7.2(19) . . . . ? O51 Co2 N58 C57 -21.2(10) . . . . ? O41 Co2 N58 C57 97.8(10) . . . . ? N61 Co2 N58 C57 -140.3(10) . . . . ? N48 Co2 N58 C57 32(15) . . . . ? O51 Co2 N58 C59 161.5(9) . . . . ? O41 Co2 N58 C59 -79.5(9) . . . . ? N61 Co2 N58 C59 42.4(10) . . . . ? N48 Co2 N58 C59 -145(14) . . . . ? C57 N58 C59 C510 -137.1(13) . . . . ? Co2 N58 C59 C510 40.3(15) . . . . ? N58 C59 C510 N511 58.5(16) . . . . ? C59 C510 N511 C512 51.9(16) . . . . ? C59 C510 N511 C513 175.9(12) . . . . ? O51 Co2 N61 C62 63(9) . . . . ? O41 Co2 N61 C62 -121(9) . . . . ? N48 Co2 N61 C62 -29(9) . . . . ? N58 Co2 N61 C62 151(9) . . . . ? Co2 N61 C62 S63 -96(17) . . . . ? N101 Co3 N71 C72 -116(5) . . . . ? N81 Co3 N71 C72 126(5) . . . . ? N91 Co3 N71 C72 1(5) . . . . ? Co3 N71 C72 S73 -172(28) . . . . ? N101 Co3 N81 C82A 24(6) . . . . ? N71 Co3 N81 C82A 147(6) . . . . ? N91 Co3 N81 C82A -94(6) . . . . ? N101 Co3 N81 C82B -90(6) . . . . ? N71 Co3 N81 C82B 33(6) . . . . ? N91 Co3 N81 C82B 152(6) . . . . ? Co3 N81 C82A C82B -141(6) . . . . ? C82B N81 C82A S83A 22(39) . . . . ? Co3 N81 C82A S83A -119(41) . . . . ? C82B N81 C82A S83B 2(3) . . . . ? Co3 N81 C82A S83B -139(5) . . . . ? S83A C82A C82B N81 -179(2) . . . . ? S83B C82A C82B N81 -178(3) . . . . ? N81 C82A C82B S83B 178(3) . . . . ? S83A C82A C82B S83B -1(4) . . . . ? N81 C82A C82B S83A 179(2) . . . . ? S83B C82A C82B S83A 1(4) . . . . ? Co3 N81 C82B C82A 150(4) . . . . ? C82A N81 C82B S83B -8(13) . . . . ? Co3 N81 C82B S83B 141(13) . . . . ? C82A N81 C82B S83A -1(2) . . . . ? Co3 N81 C82B S83A 148(4) . . . . ? C82B C82A S83A S83B 1(5) . . . . ? N81 C82A S83A S83B -22(42) . . . . ? N81 C82A S83A C82B -22(39) . . . . ? S83B C82A S83A C82B -1(5) . . . . ? C82A C82B S83A S83B -179(6) . . . . ? N81 C82B S83A S83B -178(4) . . . . ? N81 C82B S83A C82A 1(2) . . . . ? S83B C82B S83A C82A 179(6) . . . . ? C82A S83A S83B C82B 0(2) . . . . ? C82B S83A S83B C82A 0(2) . . . . ? C82A C82B S83B S83A 1(5) . . . . ? N81 C82B S83B S83A 8(17) . . . . ? N81 C82B S83B C82A 8(12) . . . . ? S83A C82B S83B C82A -1(5) . . . . ? C82B C82A S83B S83A -179(6) . . . . ? N81 C82A S83B S83A 178(3) . . . . ? N81 C82A S83B C82B -3(4) . . . . ? S83A C82A S83B C82B 179(6) . . . . ? N101 Co3 N91 C92 55(4) . . . . ? N71 Co3 N91 C92 -65(4) . . . . ? N81 Co3 N91 C92 173(4) . . . . ? Co3 N91 C92 S93 4(43) . . . . ? N71 Co3 N101 C502 127(6) . . . . ? N81 Co3 N101 C502 -111(6) . . . . ? N91 Co3 N101 C502 12(7) . . . . ? Co3 N101 C502 S103 164(9) . . . . ? C994 C992 C993 C995 37(19) . . . . ? C995 C993 C994 C992 -156(13) . . . . ? C994 C993 C995 C995 67(21) . . . 2_755 ? C992 C993 C995 C995 50(24) . . . 2_755 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.504 _refine_diff_density_min -0.742 _refine_diff_density_rms 0.095 # CIF produced by WinGX routine CIF_UPDATE # Created on 2003-10-20 at 11:38:45 # Using CIFtbx version 2.6.2 16 Jun 1998 # Dictionary name : cif_core.dic # Dictionary vers : 2.2 # Request file : d:\crystal\wingx\files\archive.dat # CIF files read : mitr17 dreduc struct #===END data_mitr17 _database_code_depnum_ccdc_archive 'CCDC 281768' _audit_creation_date 2003-10-20T11:38:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_common 'Insert systematic name here!!!!!' _chemical_name_systematic ; Insert systematic name here!!!!! ; _chemical_formula_moiety 'C25 H36 Co N5 O4 S, Cl O4' _chemical_formula_structural '[Co (LH)2 (NCS)].ClO4' _chemical_formula_sum 'C25 H36 Cl Co N5 O8 S' _chemical_formula_weight 661.03 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.229(4) _cell_length_b 29.702(4) _cell_length_c 10.646(2) _cell_angle_alpha 90 _cell_angle_beta 96.75(2) _cell_angle_gamma 90 _cell_volume 2898.1(14) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 6.8 _cell_measurement_theta_max 11.1 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description platelet _exptl_crystal_colour 'reddish brown' _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.515 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_special_details ; Crystals were grown from methanol. ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.813 _exptl_absorpt_correction_type none _exptl_absorpt_correction_t_min ? _exptl_absorpt_correction_t_max ? #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'scintillation LiI' _diffrn_detector_dtime 1.195 _diffrn_orient_matrix_type ; x-axis points to radiation source the matrix is specified in reciprocal space ; _diffrn_orient_matrix_ub_11 -0.021076 _diffrn_orient_matrix_ub_12 -0.013836 _diffrn_orient_matrix_ub_13 -0.085827 _diffrn_orient_matrix_ub_21 -0.000848 _diffrn_orient_matrix_ub_22 0.030593 _diffrn_orient_matrix_ub_23 -0.039309 _diffrn_orient_matrix_ub_31 0.10705 _diffrn_orient_matrix_ub_32 -0.002484 _diffrn_orient_matrix_ub_33 -0.005873 _diffrn_measurement_device '\k-geometry diffractometer' _diffrn_measurement_device_type 'Enraf Nonius CAD4' _diffrn_measurement_method 'non-profiled omega scans' _diffrn_standards_number 3 _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 2 _diffrn_standards_decay_corr_max 1.048 _diffrn_standards_decay_corr_min 0.988 loop_ _diffrn_standard_refln_index_h _diffrn_standard_refln_index_k _diffrn_standard_refln_index_l 1 3 -2 -1 -2 -1 0 4 0 _diffrn_reflns_av_R_equivalents 0.1217 _diffrn_reflns_av_unetI/netI 0.3853 _diffrn_reflns_number 5522 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.17 _diffrn_reflns_theta_full 25.17 _diffrn_measured_fraction_theta_full 1 _diffrn_measured_fraction_theta_max 1 _reflns_number_total 5187 _reflns_number_gt 1821 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'CAD4 Express (Enraf Nonius, 1994)' _computing_cell_refinement 'CAD4 Express (Enraf Nonius, 1994)' _computing_data_reduction 'XCAD4 (Harms & Wocadlo, 1995)' _computing_structure_solution 'SIR-97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. ; _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^)+(0.0037P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 5187 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.304 _refine_ls_R_factor_gt 0.0964 _refine_ls_wR_factor_ref 0.127 _refine_ls_wR_factor_gt 0.0895 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.438 _refine_diff_density_min -0.547 _refine_diff_density_rms 0.105 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.43586(15) 0.12208(5) 0.65780(13) 0.0291(4) Uani 1 1 d . . . Cl1 Cl 0.1662(4) 0.19619(11) 1.1514(3) 0.0557(9) Uani 1 1 d . . . S1 S 0.7651(4) 0.17254(11) 0.4184(3) 0.0666(11) Uani 1 1 d . . . O1 O 0.6184(8) 0.1047(2) 0.7437(7) 0.037(2) Uani 1 1 d G . . H1 H 0.6603 0.1299 0.759 0.045 Uiso 1 1 d G . . O2 O 0.3494(8) 0.0703(2) 0.7182(6) 0.0355(19) Uani 1 1 d G . . H2 H 0.3543 0.0472 0.6718 0.043 Uiso 1 1 d G . . O3 O 0.8589(7) 0.0911(2) 0.8913(6) 0.039(2) Uani 1 1 d . . . O4 O 0.3005(7) -0.0147(2) 0.7588(6) 0.0397(19) Uani 1 1 d . . . O5 O 0.1355(9) 0.1966(3) 1.0168(7) 0.083(3) Uani 1 1 d . . . O6 O 0.1075(9) 0.2347(3) 1.2033(8) 0.089(3) Uani 1 1 d . . . O7 O 0.3198(9) 0.1955(3) 1.1847(7) 0.086(3) Uani 1 1 d . . . O8 O 0.1045(10) 0.1571(3) 1.1995(7) 0.093(3) Uani 1 1 d . . . N1 N 0.4518(9) 0.0867(3) 0.5122(7) 0.029(2) Uani 1 1 d . . . N2 N 0.2386(9) 0.1411(3) 0.5718(7) 0.033(2) Uani 1 1 d . . . N3 N 0.4179(9) 0.1567(3) 0.8131(7) 0.031(2) Uani 1 1 d . . . N4 N 0.5396(9) 0.1676(3) 0.5717(8) 0.044(3) Uani 1 1 d . . . N5 N 0.7088(10) 0.1885(3) 0.8617(9) 0.047(3) Uani 1 1 d . . . C1 C 0.7061(11) 0.0746(3) 0.7037(9) 0.025(3) Uani 1 1 d . . . C2 C 0.8411(11) 0.0655(3) 0.7822(9) 0.028(3) Uani 1 1 d . . . C3 C 0.9320(11) 0.0338(3) 0.7478(10) 0.038(3) Uani 1 1 d . . . H3 H 1.0168 0.0277 0.8012 0.046 Uiso 1 1 calc R . . C4 C 0.9048(12) 0.0099(4) 0.6360(10) 0.047(3) Uani 1 1 d . . . H4 H 0.9715 -0.0114 0.6144 0.056 Uiso 1 1 calc R . . C5 C 0.7794(11) 0.0177(3) 0.5580(9) 0.041(3) Uani 1 1 d . . . H5 H 0.7605 0.0015 0.4831 0.049 Uiso 1 1 calc R . . C6 C 0.6791(10) 0.0499(3) 0.5892(9) 0.028(3) Uani 1 1 d . . . C7 C 0.9894(10) 0.0844(3) 0.9741(9) 0.056(3) Uani 1 1 d . . . H7A H 0.9954 0.0535 1.0006 0.067 Uiso 1 1 calc R . . H7B H 0.9889 0.1035 1.0468 0.067 Uiso 1 1 calc R . . H7C H 1.0719 0.0916 0.9308 0.067 Uiso 1 1 calc R . . C8 C 0.5507(11) 0.0579(3) 0.5000(9) 0.030(3) Uani 1 1 d . . . H8 H 0.5399 0.0404 0.4271 0.036 Uiso 1 1 calc R . . C9 C 0.3303(11) 0.0948(3) 0.4116(9) 0.042(3) Uani 1 1 d . . . H9A H 0.3137 0.0684 0.3582 0.05 Uiso 1 1 calc R . . H9B H 0.3525 0.12 0.3594 0.05 Uiso 1 1 calc R . . C10 C 0.1996(11) 0.1046(3) 0.4756(9) 0.039(3) Uani 1 1 d . . . H10A H 0.1689 0.0778 0.517 0.047 Uiso 1 1 calc R . . H10B H 0.1199 0.1145 0.4142 0.047 Uiso 1 1 calc R . . C11 C 0.2356(11) 0.1858(3) 0.5073(8) 0.051(3) Uani 1 1 d . . . H11A H 0.2985 0.185 0.4416 0.061 Uiso 1 1 calc R . . H11B H 0.2687 0.2086 0.5677 0.061 Uiso 1 1 calc R . . H11C H 0.1378 0.1924 0.471 0.061 Uiso 1 1 calc R . . C12 C 0.1253(10) 0.1420(3) 0.6604(9) 0.050(3) Uani 1 1 d . . . H12A H 0.0313 0.1471 0.6137 0.06 Uiso 1 1 calc R . . H12B H 0.1466 0.1659 0.7207 0.06 Uiso 1 1 calc R . . H12C H 0.1249 0.1138 0.704 0.06 Uiso 1 1 calc R . . C13 C 0.3496(10) 0.0584(4) 0.8342(9) 0.028(3) Uani 1 1 d . . . C14 C 0.3208(10) 0.0124(3) 0.8637(9) 0.031(3) Uani 1 1 d . . . C15 C 0.3123(10) -0.0007(3) 0.9838(9) 0.036(3) Uani 1 1 d . . . H15 H 0.2925 -0.0307 1.001 0.043 Uiso 1 1 calc R . . C16 C 0.3332(11) 0.0305(3) 1.0826(9) 0.040(3) Uani 1 1 d . . . H16 H 0.3263 0.0214 1.1653 0.048 Uiso 1 1 calc R . . C17 C 0.3627(10) 0.0728(4) 1.0583(9) 0.042(3) Uani 1 1 d . . . H17 H 0.3784 0.093 1.1254 0.05 Uiso 1 1 calc R . . C18 C 0.3713(10) 0.0888(3) 0.9348(9) 0.021(2) Uani 1 1 d . . . C19 C 0.2557(11) -0.0594(3) 0.7764(9) 0.053(3) Uani 1 1 d . . . H19A H 0.3249 -0.074 0.8375 0.063 Uiso 1 1 calc R . . H19B H 0.2502 -0.0753 0.6975 0.063 Uiso 1 1 calc R . . H19C H 0.1615 -0.0593 0.8062 0.063 Uiso 1 1 calc R . . C20 C 0.3968(10) 0.1350(3) 0.9159(10) 0.035(3) Uani 1 1 d . . . H20 H 0.399 0.1528 0.988 0.042 Uiso 1 1 calc R . . C21 C 0.4406(12) 0.2055(3) 0.8272(10) 0.046(3) Uani 1 1 d . . . H21A H 0.4215 0.2144 0.9114 0.056 Uiso 1 1 calc R . . H21B H 0.3706 0.2209 0.7669 0.056 Uiso 1 1 calc R . . C22 C 0.5933(12) 0.2207(3) 0.8069(10) 0.056(4) Uani 1 1 d . . . H22A H 0.5989 0.2238 0.7169 0.067 Uiso 1 1 calc R . . H22B H 0.6118 0.25 0.8455 0.067 Uiso 1 1 calc R . . C23 C 0.7312(11) 0.1907(3) 1.0033(9) 0.065(4) Uani 1 1 d . . . H23A H 0.7522 0.2211 1.0297 0.078 Uiso 1 1 calc R . . H23B H 0.8114 0.1716 1.0346 0.078 Uiso 1 1 calc R . . H23C H 0.6443 0.1807 1.0364 0.078 Uiso 1 1 calc R . . C24 C 0.8495(11) 0.2017(3) 0.8131(10) 0.064(4) Uani 1 1 d . . . H24A H 0.8358 0.2021 0.7223 0.076 Uiso 1 1 calc R . . H24B H 0.924 0.1802 0.8417 0.076 Uiso 1 1 calc R . . H24C H 0.8784 0.231 0.8442 0.076 Uiso 1 1 calc R . . C25 C 0.6351(12) 0.1685(3) 0.5083(10) 0.041(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0299(8) 0.0301(8) 0.0274(8) -0.0020(8) 0.0047(6) 0.0002(9) Cl1 0.068(3) 0.050(2) 0.048(2) -0.0028(19) 0.0017(19) 0.000(2) S1 0.060(2) 0.056(2) 0.089(3) 0.016(2) 0.031(2) 0.010(2) O1 0.040(5) 0.031(5) 0.042(5) -0.021(4) 0.009(4) -0.003(4) O2 0.048(5) 0.026(5) 0.031(5) -0.015(4) -0.002(4) -0.002(4) O3 0.030(5) 0.044(5) 0.040(5) -0.011(4) -0.008(4) -0.005(4) O4 0.052(5) 0.035(5) 0.034(4) 0.001(4) 0.014(4) -0.002(4) O5 0.090(7) 0.115(8) 0.043(6) 0.014(5) -0.003(5) 0.011(6) O6 0.091(7) 0.053(6) 0.132(8) -0.003(6) 0.051(6) 0.019(6) O7 0.061(7) 0.109(8) 0.083(7) -0.023(6) -0.009(6) 0.005(6) O8 0.154(9) 0.057(6) 0.062(6) 0.016(5) -0.010(6) -0.047(7) N1 0.030(6) 0.031(5) 0.025(5) -0.006(4) 0.006(4) 0.004(5) N2 0.029(5) 0.041(6) 0.030(5) 0.008(5) 0.006(4) 0.005(5) N3 0.039(6) 0.028(6) 0.026(5) 0.000(5) -0.001(5) 0.005(5) N4 0.044(7) 0.045(6) 0.042(6) 0.005(5) 0.009(5) 0.003(6) N5 0.033(6) 0.051(7) 0.057(7) -0.017(6) 0.003(5) 0.004(5) C1 0.032(7) 0.025(6) 0.021(6) 0.006(5) 0.008(5) 0.008(6) C2 0.025(7) 0.027(7) 0.031(7) 0.009(5) -0.004(5) -0.010(6) C3 0.029(7) 0.039(8) 0.045(8) 0.001(6) 0.000(6) 0.000(6) C4 0.047(8) 0.050(8) 0.044(8) 0.001(7) 0.011(7) 0.020(7) C5 0.049(8) 0.031(7) 0.042(7) -0.020(6) 0.004(6) 0.013(6) C6 0.026(7) 0.039(7) 0.021(6) 0.000(5) 0.007(5) -0.007(6) C7 0.031(7) 0.078(9) 0.054(8) -0.004(7) -0.011(6) 0.004(7) C8 0.036(7) 0.026(7) 0.029(7) -0.009(5) 0.014(6) 0.001(6) C9 0.049(8) 0.043(7) 0.034(7) -0.016(6) 0.009(6) -0.001(6) C10 0.055(8) 0.031(7) 0.027(6) -0.005(5) -0.015(6) 0.004(6) C11 0.049(8) 0.068(9) 0.035(7) 0.008(7) 0.004(6) 0.015(7) C12 0.027(7) 0.082(10) 0.041(7) -0.001(6) 0.003(6) -0.001(7) C13 0.028(7) 0.050(8) 0.007(6) -0.005(5) 0.001(5) 0.010(6) C14 0.031(7) 0.033(7) 0.030(7) -0.005(6) 0.012(5) 0.006(6) C15 0.043(7) 0.032(7) 0.034(7) 0.012(6) 0.004(6) -0.015(6) C16 0.054(8) 0.048(8) 0.017(6) 0.003(6) 0.001(6) 0.001(7) C17 0.038(8) 0.060(9) 0.026(7) -0.001(6) -0.001(6) 0.012(7) C18 0.018(6) 0.026(6) 0.020(6) -0.012(5) 0.003(5) 0.002(5) C19 0.074(9) 0.034(7) 0.054(8) -0.017(6) 0.019(7) -0.007(7) C20 0.019(6) 0.039(8) 0.045(8) -0.017(6) -0.004(6) 0.010(6) C21 0.050(8) 0.029(8) 0.061(9) -0.005(6) 0.008(7) 0.003(7) C22 0.068(10) 0.040(8) 0.060(9) -0.004(7) 0.015(8) -0.010(7) C23 0.069(10) 0.065(9) 0.062(9) -0.014(8) 0.007(8) -0.013(8) C24 0.049(9) 0.061(10) 0.081(10) -0.025(8) 0.005(8) 0.008(8) C25 0.058(9) 0.030(7) 0.038(8) 0.002(6) 0.012(7) -0.006(7) _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 O2 1.881(7) . ? Co1 O1 1.892(7) . ? Co1 N1 1.894(7) . ? Co1 N4 1.948(9) . ? Co1 N3 1.970(7) . ? Co1 N2 2.020(8) . ? Cl1 O6 1.405(7) . ? Cl1 O8 1.415(7) . ? Cl1 O7 1.420(8) . ? Cl1 O5 1.428(7) . ? S1 C25 1.624(11) . ? O1 C1 1.309(10) . ? O1 H1 0.8499 . ? O2 C13 1.284(10) . ? O2 H2 0.85 . ? O3 C2 1.382(10) . ? O3 C7 1.420(10) . ? O4 C14 1.372(10) . ? O4 C19 1.410(9) . ? N1 C8 1.267(10) . ? N1 C9 1.476(10) . ? N2 C12 1.489(10) . ? N2 C11 1.492(10) . ? N2 C10 1.505(10) . ? N3 C20 1.303(11) . ? N3 C21 1.471(10) . ? N4 C25 1.172(11) . ? N5 C22 1.498(12) . ? N5 C23 1.499(10) . ? N5 C24 1.505(11) . ? C1 C6 1.420(11) . ? C1 C2 1.442(12) . ? C2 C3 1.339(12) . ? C3 C4 1.384(12) . ? C3 H3 0.93 . ? C4 C5 1.363(12) . ? C4 H4 0.93 . ? C5 C6 1.397(11) . ? C5 H5 0.93 . ? C6 C8 1.449(12) . ? C7 H7A 0.96 . ? C7 H7B 0.96 . ? C7 H7C 0.96 . ? C8 H8 0.93 . ? C9 C10 1.483(12) . ? C9 H9A 0.97 . ? C9 H9B 0.97 . ? C10 H10A 0.97 . ? C10 H10B 0.97 . ? C11 H11A 0.96 . ? C11 H11B 0.96 . ? C11 H11C 0.96 . ? C12 H12A 0.96 . ? C12 H12B 0.96 . ? C12 H12C 0.96 . ? C13 C18 1.398(11) . ? C13 C14 1.433(12) . ? C14 C15 1.348(11) . ? C15 C16 1.398(12) . ? C15 H15 0.93 . ? C16 C17 1.320(12) . ? C16 H16 0.93 . ? C17 C18 1.409(12) . ? C17 H17 0.93 . ? C18 C20 1.411(12) . ? C19 H19A 0.96 . ? C19 H19B 0.96 . ? C19 H19C 0.96 . ? C20 H20 0.93 . ? C21 C22 1.519(12) . ? C21 H21A 0.97 . ? C21 H21B 0.97 . ? C22 H22A 0.97 . ? C22 H22B 0.97 . ? C23 H23A 0.96 . ? C23 H23B 0.96 . ? C23 H23C 0.96 . ? C24 H24A 0.96 . ? C24 H24B 0.96 . ? C24 H24C 0.96 . ? 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 O2 Co1 O1 90.0(3) . . ? O2 Co1 N1 84.4(3) . . ? O1 Co1 N1 95.4(3) . . ? O2 Co1 N4 168.8(3) . . ? O1 Co1 N4 87.6(3) . . ? N1 Co1 N4 84.9(3) . . ? O2 Co1 N3 93.4(3) . . ? O1 Co1 N3 84.0(3) . . ? N1 Co1 N3 177.7(4) . . ? N4 Co1 N3 97.3(4) . . ? O2 Co1 N2 89.3(3) . . ? O1 Co1 N2 178.1(3) . . ? N1 Co1 N2 86.4(3) . . ? N4 Co1 N2 93.4(3) . . ? N3 Co1 N2 94.3(3) . . ? O6 Cl1 O8 109.6(6) . . ? O6 Cl1 O7 109.5(6) . . ? O8 Cl1 O7 109.2(6) . . ? O6 Cl1 O5 110.3(5) . . ? O8 Cl1 O5 109.3(5) . . ? O7 Cl1 O5 108.9(5) . . ? C1 O1 Co1 125.3(6) . . ? C1 O1 H1 112.3 . . ? Co1 O1 H1 102.2 . . ? C13 O2 Co1 126.9(7) . . ? C13 O2 H2 110 . . ? Co1 O2 H2 114.1 . . ? C2 O3 C7 116.9(8) . . ? C14 O4 C19 117.3(8) . . ? C8 N1 C9 122.0(8) . . ? C8 N1 Co1 125.8(7) . . ? C9 N1 Co1 112.2(6) . . ? C12 N2 C11 107.4(8) . . ? C12 N2 C10 108.3(8) . . ? C11 N2 C10 109.7(7) . . ? C12 N2 Co1 112.3(6) . . ? C11 N2 Co1 115.1(6) . . ? C10 N2 Co1 103.7(6) . . ? C20 N3 C21 115.8(8) . . ? C20 N3 Co1 118.9(7) . . ? C21 N3 Co1 125.1(6) . . ? C25 N4 Co1 137.0(9) . . ? C22 N5 C23 111.9(8) . . ? C22 N5 C24 107.7(8) . . ? C23 N5 C24 108.2(8) . . ? O1 C1 C6 125.4(9) . . ? O1 C1 C2 117.7(9) . . ? C6 C1 C2 116.9(9) . . ? C3 C2 O3 126.9(10) . . ? C3 C2 C1 120.0(10) . . ? O3 C2 C1 113.1(9) . . ? C2 C3 C4 122.7(11) . . ? C2 C3 H3 118.7 . . ? C4 C3 H3 118.7 . . ? C5 C4 C3 119.4(10) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 120.7(10) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 120.2(9) . . ? C5 C6 C8 118.1(9) . . ? C1 C6 C8 121.7(9) . . ? O3 C7 H7A 109.5 . . ? O3 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O3 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N1 C8 C6 126.0(9) . . ? N1 C8 H8 117 . . ? C6 C8 H8 117 . . ? N1 C9 C10 106.8(8) . . ? N1 C9 H9A 110.4 . . ? C10 C9 H9A 110.4 . . ? N1 C9 H9B 110.4 . . ? C10 C9 H9B 110.4 . . ? H9A C9 H9B 108.6 . . ? C9 C10 N2 108.2(8) . . ? C9 C10 H10A 110.1 . . ? N2 C10 H10A 110.1 . . ? C9 C10 H10B 110.1 . . ? N2 C10 H10B 110.1 . . ? H10A C10 H10B 108.4 . . ? N2 C11 H11A 109.5 . . ? N2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N2 C12 H12A 109.5 . . ? N2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O2 C13 C18 122.9(10) . . ? O2 C13 C14 119.6(9) . . ? C18 C13 C14 117.4(9) . . ? C15 C14 O4 125.7(10) . . ? C15 C14 C13 121.2(10) . . ? O4 C14 C13 113.1(9) . . ? C14 C15 C16 120.2(10) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.9(10) . . ? C17 C16 H16 120.1 . . ? C15 C16 H16 120.1 . . ? C16 C17 C18 122.6(10) . . ? C16 C17 H17 118.7 . . ? C18 C17 H17 118.7 . . ? C13 C18 C17 118.7(10) . . ? C13 C18 C20 122.0(10) . . ? C17 C18 C20 119.3(10) . . ? O4 C19 H19A 109.5 . . ? O4 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? O4 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C18 130.1(10) . . ? N3 C20 H20 115 . . ? C18 C20 H20 115 . . ? N3 C21 C22 113.7(9) . . ? N3 C21 H21A 108.8 . . ? C22 C21 H21A 108.8 . . ? N3 C21 H21B 108.8 . . ? C22 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? N5 C22 C21 112.6(9) . . ? N5 C22 H22A 109.1 . . ? C21 C22 H22A 109.1 . . ? N5 C22 H22B 109.1 . . ? C21 C22 H22B 109.1 . . ? H22A C22 H22B 107.8 . . ? N5 C23 H23A 109.5 . . ? N5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N5 C24 H24A 109.5 . . ? N5 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N5 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 S1 176.9(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 Co1 O1 C1 79.8(8) . . . . ? N1 Co1 O1 C1 -4.5(8) . . . . ? N4 Co1 O1 C1 -89.2(8) . . . . ? N3 Co1 O1 C1 173.2(8) . . . . ? N2 Co1 O1 C1 150(10) . . . . ? O1 Co1 O2 C13 56.6(8) . . . . ? N1 Co1 O2 C13 151.9(9) . . . . ? N4 Co1 O2 C13 134.4(17) . . . . ? N3 Co1 O2 C13 -27.4(9) . . . . ? N2 Co1 O2 C13 -121.6(8) . . . . ? O2 Co1 N1 C8 -81.5(8) . . . . ? O1 Co1 N1 C8 8.0(8) . . . . ? N4 Co1 N1 C8 95.1(8) . . . . ? N3 Co1 N1 C8 -65(9) . . . . ? N2 Co1 N1 C8 -171.2(8) . . . . ? O2 Co1 N1 C9 96.3(6) . . . . ? O1 Co1 N1 C9 -174.2(6) . . . . ? N4 Co1 N1 C9 -87.1(7) . . . . ? N3 Co1 N1 C9 113(9) . . . . ? N2 Co1 N1 C9 6.6(6) . . . . ? O2 Co1 N2 C12 53.1(7) . . . . ? O1 Co1 N2 C12 -17(10) . . . . ? N1 Co1 N2 C12 137.5(7) . . . . ? N4 Co1 N2 C12 -137.8(7) . . . . ? N3 Co1 N2 C12 -40.2(7) . . . . ? O2 Co1 N2 C11 176.5(6) . . . . ? O1 Co1 N2 C11 106(10) . . . . ? N1 Co1 N2 C11 -99.1(7) . . . . ? N4 Co1 N2 C11 -14.4(7) . . . . ? N3 Co1 N2 C11 83.2(7) . . . . ? O2 Co1 N2 C10 -63.6(6) . . . . ? O1 Co1 N2 C10 -134(10) . . . . ? N1 Co1 N2 C10 20.8(6) . . . . ? N4 Co1 N2 C10 105.4(6) . . . . ? N3 Co1 N2 C10 -157.0(6) . . . . ? O2 Co1 N3 C20 18.3(8) . . . . ? O1 Co1 N3 C20 -71.4(8) . . . . ? N1 Co1 N3 C20 2(9) . . . . ? N4 Co1 N3 C20 -158.2(8) . . . . ? N2 Co1 N3 C20 107.9(8) . . . . ? O2 Co1 N3 C21 -168.1(8) . . . . ? O1 Co1 N3 C21 102.3(8) . . . . ? N1 Co1 N3 C21 175(8) . . . . ? N4 Co1 N3 C21 15.5(8) . . . . ? N2 Co1 N3 C21 -78.5(8) . . . . ? O2 Co1 N4 C25 -21(3) . . . . ? O1 Co1 N4 C25 56.9(13) . . . . ? N1 Co1 N4 C25 -38.7(13) . . . . ? N3 Co1 N4 C25 140.5(13) . . . . ? N2 Co1 N4 C25 -124.8(13) . . . . ? Co1 O1 C1 C6 -0.1(14) . . . . ? Co1 O1 C1 C2 -179.8(6) . . . . ? C7 O3 C2 C3 2.1(15) . . . . ? C7 O3 C2 C1 -179.9(8) . . . . ? O1 C1 C2 C3 177.5(9) . . . . ? C6 C1 C2 C3 -2.2(14) . . . . ? O1 C1 C2 O3 -0.6(13) . . . . ? C6 C1 C2 O3 179.7(8) . . . . ? O3 C2 C3 C4 -179.9(10) . . . . ? C1 C2 C3 C4 2.3(16) . . . . ? C2 C3 C4 C5 -1.4(17) . . . . ? C3 C4 C5 C6 0.5(17) . . . . ? C4 C5 C6 C1 -0.5(16) . . . . ? C4 C5 C6 C8 177.6(9) . . . . ? O1 C1 C6 C5 -178.4(9) . . . . ? C2 C1 C6 C5 1.3(14) . . . . ? O1 C1 C6 C8 3.6(15) . . . . ? C2 C1 C6 C8 -176.7(8) . . . . ? C9 N1 C8 C6 175.4(9) . . . . ? Co1 N1 C8 C6 -7.0(14) . . . . ? C5 C6 C8 N1 -177.9(9) . . . . ? C1 C6 C8 N1 0.2(15) . . . . ? C8 N1 C9 C10 144.6(9) . . . . ? Co1 N1 C9 C10 -33.3(9) . . . . ? N1 C9 C10 N2 51.5(10) . . . . ? C12 N2 C10 C9 -163.9(8) . . . . ? C11 N2 C10 C9 79.1(9) . . . . ? Co1 N2 C10 C9 -44.4(8) . . . . ? Co1 O2 C13 C18 22.1(14) . . . . ? Co1 O2 C13 C14 -160.4(7) . . . . ? C19 O4 C14 C15 5.3(15) . . . . ? C19 O4 C14 C13 -173.2(9) . . . . ? O2 C13 C14 C15 -176.4(9) . . . . ? C18 C13 C14 C15 1.2(15) . . . . ? O2 C13 C14 O4 2.1(14) . . . . ? C18 C13 C14 O4 179.8(8) . . . . ? O4 C14 C15 C16 -179.0(9) . . . . ? C13 C14 C15 C16 -0.7(16) . . . . ? C14 C15 C16 C17 -0.6(17) . . . . ? C15 C16 C17 C18 1.4(17) . . . . ? O2 C13 C18 C17 177.0(9) . . . . ? C14 C13 C18 C17 -0.5(14) . . . . ? O2 C13 C18 C20 -0.9(16) . . . . ? C14 C13 C18 C20 -178.5(9) . . . . ? C16 C17 C18 C13 -0.8(16) . . . . ? C16 C17 C18 C20 177.2(10) . . . . ? C21 N3 C20 C18 179.6(10) . . . . ? Co1 N3 C20 C18 -6.2(15) . . . . ? C13 C18 C20 N3 -6.9(17) . . . . ? C17 C18 C20 N3 175.2(10) . . . . ? C20 N3 C21 C22 113.1(11) . . . . ? Co1 N3 C21 C22 -60.7(11) . . . . ? C23 N5 C22 C21 -72.9(11) . . . . ? C24 N5 C22 C21 168.4(9) . . . . ? N3 C21 C22 N5 -38.9(13) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N5 0.85 2.08 2.869(10) 154.8 . O2 H2 O4 0.85 2.14 2.609(9) 114.3 . #===END data_smitra4 _database_code_depnum_ccdc_archive 'CCDC 281769' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 6' _chemical_melting_point ? _chemical_formula_moiety 'C20 H24 Co N5 O5, 0.5(C H4 O)' _chemical_formula_structural '[Co (L) (N3) (o-vanillinate)].0.5(MeOH)' _chemical_formula_sum 'C20.50 H26 Co N5 O5.50' _chemical_formula_weight 489.39 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M A-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, y+1/2, z+1/2' '-x, -y, -z' '-x, -y+1/2, -z+1/2' _cell_length_a 10.031(3) _cell_length_b 10.612(2) _cell_length_c 20.996(3) _cell_angle_alpha 94.152(15) _cell_angle_beta 80.05(2) _cell_angle_gamma 84.45(2) _cell_volume 2181.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 8 _cell_measurement_theta_max 10 _exptl_crystal_description parallelipiped _exptl_crystal_colour 'very deep red' _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1020 _exptl_absorpt_coefficient_mu 0.832 _exptl_absorpt_correction_type 'semi-empirical psi-scans' _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details 'EMPABS, (Sheldrick et al, 1977)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type Mo-K\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'Enraf-Nonius CAD4 diffractometer' _diffrn_measurement_method 'scintillation counter; \w/\q scans' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time '10000 s' _diffrn_standards_decay_% 0 _diffrn_reflns_number 4249 _diffrn_reflns_av_R_equivalents 0.019 _diffrn_reflns_av_sigmaI/netI 0.0577 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3828 _reflns_number_gt 2807 _reflns_threshold_expression I>2sigma(I) _computing_data_collection 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_cell_refinement 'CAD4/EXPRESS (Enraf-Nonius, 1992)' _computing_data_reduction 'CAD4 (Hursthouse, 1976)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1971)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0315P)^2^+0.9493P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3828 _refine_ls_number_parameters 299 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0593 _refine_ls_R_factor_gt 0.0390 _refine_ls_wR_factor_ref 0.0956 _refine_ls_wR_factor_gt 0.0833 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.17777(4) 0.26146(4) 0.387080(19) 0.03162(14) Uani 1 1 d . . . O1 O 0.26052(19) 0.40668(18) 0.40901(9) 0.0358(5) Uani 1 1 d . . . C1 C 0.3912(3) 0.4160(3) 0.39567(14) 0.0350(7) Uani 1 1 d . . . O2 O 0.3367(2) 0.6156(2) 0.45462(12) 0.0580(7) Uani 1 1 d . . . C21 C 0.3733(5) 0.7318(4) 0.4802(2) 0.0827(14) Uani 1 1 d . . . H21A H 0.2928 0.7841 0.5023 0.124 Uiso 1 1 calc R . . H21B H 0.4181 0.7751 0.4454 0.124 Uiso 1 1 calc R . . H21C H 0.4337 0.7151 0.5101 0.124 Uiso 1 1 calc R . . C2 C 0.4377(4) 0.5287(3) 0.42092(16) 0.0467(8) Uani 1 1 d . . . C3 C 0.5743(4) 0.5425(4) 0.41099(19) 0.0630(11) Uani 1 1 d . . . H3 H 0.6031 0.6151 0.4293 0.076 Uiso 1 1 calc R . . C4 C 0.6705(4) 0.4504(4) 0.3741(2) 0.0681(11) Uani 1 1 d . . . H4 H 0.7625 0.4618 0.3676 0.082 Uiso 1 1 calc R . . C5 C 0.6291(3) 0.3441(4) 0.34789(17) 0.0540(9) Uani 1 1 d . . . H5 H 0.6932 0.2829 0.3229 0.065 Uiso 1 1 calc R . . C6 C 0.4907(3) 0.3246(3) 0.35765(14) 0.0385(7) Uani 1 1 d . . . C7 C 0.4552(3) 0.2095(3) 0.32937(14) 0.0391(7) Uani 1 1 d . . . H7 H 0.5252 0.1557 0.3032 0.047 Uiso 1 1 calc R . . N8 N 0.3360(2) 0.1730(2) 0.33645(11) 0.0335(6) Uani 1 1 d . . . C9 C 0.3173(4) 0.0467(3) 0.30829(18) 0.0523(9) Uani 1 1 d . . . H9A H 0.3407 -0.0177 0.3362 0.063 Uiso 1 1 calc R . . H9B H 0.3754 0.0274 0.2660 0.063 Uiso 1 1 calc R . . C10 C 0.1697(4) 0.0491(3) 0.30199(17) 0.0569(10) Uani 1 1 d . . . H10A H 0.1526 0.0971 0.2661 0.068 Uiso 1 1 calc R . . H10B H 0.1480 -0.0369 0.2933 0.068 Uiso 1 1 calc R . . N11 N 0.0839(3) 0.1085(2) 0.36290(12) 0.0417(6) Uani 1 1 d . . . C12 C -0.0549(4) 0.1428(4) 0.3487(2) 0.0660(11) Uani 1 1 d . . . H12A H -0.1139 0.1817 0.3874 0.099 Uiso 1 1 calc R . . H12B H -0.0902 0.0674 0.3336 0.099 Uiso 1 1 calc R . . H12C H -0.0499 0.2013 0.3157 0.099 Uiso 1 1 calc R . . C13 C 0.0685(4) 0.0197(4) 0.41398(19) 0.0695(12) Uani 1 1 d . . . H13A H 0.0129 0.0624 0.4528 0.104 Uiso 1 1 calc R . . H13B H 0.1566 -0.0094 0.4228 0.104 Uiso 1 1 calc R . . H13C H 0.0261 -0.0517 0.3995 0.104 Uiso 1 1 calc R . . N31 N 0.1296(3) 0.3363(3) 0.31078(13) 0.0448(7) Uani 1 1 d . . . N32 N 0.1963(3) 0.4133(3) 0.28667(12) 0.0405(6) Uani 1 1 d . . . N33 N 0.2556(4) 0.4888(3) 0.26077(15) 0.0659(9) Uani 1 1 d . . . O51 O 0.23291(19) 0.18758(18) 0.45925(9) 0.0335(5) Uani 1 1 d . . . C51 C 0.1778(3) 0.2211(3) 0.51977(14) 0.0323(7) Uani 1 1 d . . . C52 C 0.2411(3) 0.1651(3) 0.56851(14) 0.0375(7) Uani 1 1 d . . . O52 O 0.3525(2) 0.0802(2) 0.54435(10) 0.0485(6) Uani 1 1 d . . . C521 C 0.4148(4) 0.0129(4) 0.58934(17) 0.0609(10) Uani 1 1 d . . . H52A H 0.4917 -0.0432 0.5664 0.091 Uiso 1 1 calc R . . H52B H 0.3503 -0.0359 0.6129 0.091 Uiso 1 1 calc R . . H52C H 0.4446 0.0721 0.6192 0.091 Uiso 1 1 calc R . . C53 C 0.1899(4) 0.1976(3) 0.63316(15) 0.0502(9) Uani 1 1 d . . . H53 H 0.2335 0.1617 0.6643 0.060 Uiso 1 1 calc R . . C54 C 0.0724(4) 0.2846(3) 0.65298(17) 0.0602(10) Uani 1 1 d . . . H54 H 0.0396 0.3067 0.6970 0.072 Uiso 1 1 calc R . . C55 C 0.0067(4) 0.3365(3) 0.60806(17) 0.0547(9) Uani 1 1 d . . . H55 H -0.0721 0.3925 0.6214 0.066 Uiso 1 1 calc R . . C56 C 0.0580(3) 0.3052(3) 0.54101(15) 0.0385(7) Uani 1 1 d . . . C57 C -0.0187(3) 0.3598(3) 0.49705(16) 0.0428(8) Uani 1 1 d . . . H57 H -0.0993 0.4101 0.5152 0.051 Uiso 1 1 calc R . . O58 O 0.0112(2) 0.3470(2) 0.43558(11) 0.0455(5) Uani 1 1 d . . . O61 O 0.3400(14) 0.7458(8) 0.3031(6) 0.180(5) Uani 0.50 1 d P . . C62 C 0.449(2) 0.735(2) 0.2666(15) 0.232(19) Uani 0.50 1 d P . . H62A H 0.4410 0.7791 0.2289 0.348 Uiso 0.50 1 calc PR . . H62B H 0.4782 0.6464 0.2535 0.348 Uiso 0.50 1 calc PR . . H62C H 0.5156 0.7703 0.2885 0.348 Uiso 0.50 1 calc PR . . 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 0.0295(2) 0.0355(2) 0.0322(2) 0.00748(17) -0.00914(16) -0.00535(16) O1 0.0302(11) 0.0361(12) 0.0407(12) 0.0012(9) -0.0052(9) -0.0056(9) C1 0.0336(17) 0.0438(18) 0.0324(16) 0.0121(14) -0.0102(13) -0.0136(14) O2 0.0524(16) 0.0483(14) 0.0718(17) -0.0105(13) -0.0063(13) -0.0186(12) C21 0.101(4) 0.062(3) 0.085(3) -0.016(2) -0.009(3) -0.037(3) C2 0.047(2) 0.053(2) 0.0430(19) 0.0080(16) -0.0085(16) -0.0165(17) C3 0.057(3) 0.073(3) 0.065(3) 0.005(2) -0.014(2) -0.033(2) C4 0.037(2) 0.094(3) 0.076(3) 0.011(2) -0.006(2) -0.026(2) C5 0.036(2) 0.069(2) 0.055(2) 0.0087(19) -0.0006(16) -0.0076(18) C6 0.0309(17) 0.051(2) 0.0359(17) 0.0114(15) -0.0077(13) -0.0067(14) C7 0.0364(18) 0.0470(19) 0.0320(16) 0.0074(14) -0.0040(14) 0.0042(15) N8 0.0360(15) 0.0362(14) 0.0289(13) 0.0051(11) -0.0083(11) 0.0000(11) C9 0.056(2) 0.044(2) 0.056(2) -0.0033(17) -0.0144(18) -0.0002(17) C10 0.067(3) 0.051(2) 0.055(2) -0.0038(18) -0.0143(19) -0.0150(19) N11 0.0427(16) 0.0469(16) 0.0400(15) 0.0073(12) -0.0142(13) -0.0140(13) C12 0.057(2) 0.078(3) 0.075(3) 0.013(2) -0.033(2) -0.024(2) C13 0.101(3) 0.060(2) 0.066(3) 0.028(2) -0.037(2) -0.047(2) N31 0.0499(17) 0.0489(17) 0.0434(16) 0.0186(13) -0.0202(13) -0.0125(14) N32 0.0445(16) 0.0454(17) 0.0304(14) 0.0058(13) -0.0074(12) 0.0046(14) N33 0.078(2) 0.068(2) 0.0531(19) 0.0248(17) -0.0049(17) -0.0153(19) O51 0.0319(11) 0.0399(12) 0.0290(11) 0.0052(9) -0.0083(9) 0.0020(9) C51 0.0342(17) 0.0321(16) 0.0332(17) 0.0045(13) -0.0074(13) -0.0126(13) C52 0.0424(19) 0.0394(18) 0.0343(17) 0.0079(14) -0.0097(14) -0.0149(15) O52 0.0448(14) 0.0641(15) 0.0392(13) 0.0183(11) -0.0131(11) 0.0011(12) C521 0.057(2) 0.083(3) 0.050(2) 0.029(2) -0.0237(18) -0.003(2) C53 0.067(3) 0.055(2) 0.0340(18) 0.0106(16) -0.0158(17) -0.0206(19) C54 0.086(3) 0.057(2) 0.0320(19) -0.0063(17) 0.0017(19) -0.011(2) C55 0.063(2) 0.048(2) 0.047(2) -0.0030(17) 0.0051(18) -0.0042(18) C56 0.0410(19) 0.0336(17) 0.0395(18) 0.0049(14) -0.0009(14) -0.0071(14) C57 0.0363(18) 0.0367(18) 0.053(2) 0.0015(15) -0.0004(15) -0.0045(14) O58 0.0370(13) 0.0492(14) 0.0514(14) 0.0084(11) -0.0089(11) -0.0062(10) O61 0.242(15) 0.064(6) 0.226(13) -0.008(7) -0.032(10) -0.016(7) C62 0.20(4) 0.148(19) 0.29(4) -0.12(2) -0.01(3) 0.11(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co N8 1.875(2) . ? Co O1 1.885(2) . ? Co O51 1.8958(19) . ? Co O58 1.907(2) . ? Co N31 1.951(3) . ? Co N11 2.030(3) . ? O1 C1 1.307(3) . ? C1 C6 1.414(4) . ? C1 C2 1.425(4) . ? O2 C2 1.362(4) . ? O2 C21 1.416(4) . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C2 C3 1.373(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9300 . ? C4 C5 1.352(5) . ? C4 H4 0.9300 . ? C5 C6 1.405(4) . ? C5 H5 0.9300 . ? C6 C7 1.423(4) . ? C7 N8 1.280(4) . ? C7 H7 0.9300 . ? N8 C9 1.467(4) . ? C9 C10 1.506(5) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N11 1.474(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N11 C13 1.476(4) . ? N11 C12 1.490(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? N31 N32 1.191(3) . ? N32 N33 1.155(4) . ? O51 C51 1.304(3) . ? C51 C56 1.410(4) . ? C51 C52 1.429(4) . ? C52 O52 1.364(4) . ? C52 C53 1.372(4) . ? O52 C521 1.417(3) . ? C521 H52A 0.9600 . ? C521 H52B 0.9600 . ? C521 H52C 0.9600 . ? C53 C54 1.407(5) . ? C53 H53 0.9300 . ? C54 C55 1.359(5) . ? C54 H54 0.9300 . ? C55 C56 1.416(4) . ? C55 H55 0.9300 . ? C56 C57 1.420(4) . ? C57 O58 1.268(4) . ? C57 H57 0.9300 . ? O61 C62 1.216(19) . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? 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 N8 Co O1 95.42(10) . . ? N8 Co O51 86.94(9) . . ? O1 Co O51 88.62(9) . . ? N8 Co O58 176.89(10) . . ? O1 Co O58 87.24(9) . . ? O51 Co O58 94.75(9) . . ? N8 Co N31 90.67(11) . . ? O1 Co N31 90.60(10) . . ? O51 Co N31 177.40(10) . . ? O58 Co N31 87.69(11) . . ? N8 Co N11 85.79(11) . . ? O1 Co N11 178.29(10) . . ? O51 Co N11 92.66(9) . . ? O58 Co N11 91.52(10) . . ? N31 Co N11 88.18(11) . . ? C1 O1 Co 124.83(19) . . ? O1 C1 C6 125.7(3) . . ? O1 C1 C2 117.4(3) . . ? C6 C1 C2 116.9(3) . . ? C2 O2 C21 118.1(3) . . ? O2 C21 H21A 109.5 . . ? O2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? O2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? O2 C2 C3 125.4(3) . . ? O2 C2 C1 114.2(3) . . ? C3 C2 C1 120.4(3) . . ? C2 C3 C4 121.5(4) . . ? C2 C3 H3 119.2 . . ? C4 C3 H3 119.2 . . ? C5 C4 C3 119.4(3) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C4 C5 C6 121.2(4) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C5 C6 C1 120.5(3) . . ? C5 C6 C7 117.9(3) . . ? C1 C6 C7 121.5(3) . . ? N8 C7 C6 126.2(3) . . ? N8 C7 H7 116.9 . . ? C6 C7 H7 116.9 . . ? C7 N8 C9 119.8(3) . . ? C7 N8 Co 125.7(2) . . ? C9 N8 Co 114.2(2) . . ? N8 C9 C10 107.3(3) . . ? N8 C9 H9A 110.3 . . ? C10 C9 H9A 110.3 . . ? N8 C9 H9B 110.3 . . ? C10 C9 H9B 110.3 . . ? H9A C9 H9B 108.5 . . ? N11 C10 C9 109.1(3) . . ? N11 C10 H10A 109.9 . . ? C9 C10 H10A 109.9 . . ? N11 C10 H10B 109.9 . . ? C9 C10 H10B 109.9 . . ? H10A C10 H10B 108.3 . . ? C10 N11 C13 112.2(3) . . ? C10 N11 C12 107.1(3) . . ? C13 N11 C12 106.5(3) . . ? C10 N11 Co 104.40(19) . . ? C13 N11 Co 113.0(2) . . ? C12 N11 Co 113.5(2) . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N32 N31 Co 119.1(2) . . ? N33 N32 N31 175.9(3) . . ? C51 O51 Co 124.81(18) . . ? O51 C51 C56 125.2(3) . . ? O51 C51 C52 117.5(3) . . ? C56 C51 C52 117.3(3) . . ? O52 C52 C53 125.3(3) . . ? O52 C52 C51 114.0(3) . . ? C53 C52 C51 120.7(3) . . ? C52 O52 C521 117.5(3) . . ? O52 C521 H52A 109.5 . . ? O52 C521 H52B 109.5 . . ? H52A C521 H52B 109.5 . . ? O52 C521 H52C 109.5 . . ? H52A C521 H52C 109.5 . . ? H52B C521 H52C 109.5 . . ? C52 C53 C54 120.8(3) . . ? C52 C53 H53 119.6 . . ? C54 C53 H53 119.6 . . ? C55 C54 C53 120.2(3) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 120.0(3) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C51 C56 C55 120.9(3) . . ? C51 C56 C57 122.3(3) . . ? C55 C56 C57 116.8(3) . . ? O58 C57 C56 126.8(3) . . ? O58 C57 H57 116.6 . . ? C56 C57 H57 116.6 . . ? C57 O58 Co 124.5(2) . . ? O61 C62 H62A 109.5 . . ? O61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? O61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N8 Co O1 C1 -7.7(2) . . . . ? O51 Co O1 C1 79.1(2) . . . . ? O58 Co O1 C1 173.9(2) . . . . ? N31 Co O1 C1 -98.4(2) . . . . ? N11 Co O1 C1 -143(3) . . . . ? Co O1 C1 C6 6.3(4) . . . . ? Co O1 C1 C2 -174.5(2) . . . . ? C21 O2 C2 C3 2.0(5) . . . . ? C21 O2 C2 C1 -178.5(3) . . . . ? O1 C1 C2 O2 -2.1(4) . . . . ? C6 C1 C2 O2 177.2(3) . . . . ? O1 C1 C2 C3 177.4(3) . . . . ? C6 C1 C2 C3 -3.3(5) . . . . ? O2 C2 C3 C4 -178.0(3) . . . . ? C1 C2 C3 C4 2.6(6) . . . . ? C2 C3 C4 C5 -0.6(6) . . . . ? C3 C4 C5 C6 -0.5(6) . . . . ? C4 C5 C6 C1 -0.3(5) . . . . ? C4 C5 C6 C7 -179.0(3) . . . . ? O1 C1 C6 C5 -178.5(3) . . . . ? C2 C1 C6 C5 2.2(4) . . . . ? O1 C1 C6 C7 0.1(5) . . . . ? C2 C1 C6 C7 -179.2(3) . . . . ? C5 C6 C7 N8 175.6(3) . . . . ? C1 C6 C7 N8 -3.1(5) . . . . ? C6 C7 N8 C9 -175.1(3) . . . . ? C6 C7 N8 Co -0.9(4) . . . . ? O1 Co N8 C7 5.1(2) . . . . ? O51 Co N8 C7 -83.2(2) . . . . ? O58 Co N8 C7 153.9(18) . . . . ? N31 Co N8 C7 95.8(2) . . . . ? N11 Co N8 C7 -176.1(2) . . . . ? O1 Co N8 C9 179.7(2) . . . . ? O51 Co N8 C9 91.4(2) . . . . ? O58 Co N8 C9 -32(2) . . . . ? N31 Co N8 C9 -89.7(2) . . . . ? N11 Co N8 C9 -1.5(2) . . . . ? C7 N8 C9 C10 -159.1(3) . . . . ? Co N8 C9 C10 26.0(3) . . . . ? N8 C9 C10 N11 -46.1(4) . . . . ? C9 C10 N11 C13 -79.4(3) . . . . ? C9 C10 N11 C12 164.0(3) . . . . ? C9 C10 N11 Co 43.4(3) . . . . ? N8 Co N11 C10 -23.5(2) . . . . ? O1 Co N11 C10 111(3) . . . . ? O51 Co N11 C10 -110.2(2) . . . . ? O58 Co N11 C10 155.0(2) . . . . ? N31 Co N11 C10 67.3(2) . . . . ? N8 Co N11 C13 98.8(3) . . . . ? O1 Co N11 C13 -126(3) . . . . ? O51 Co N11 C13 12.0(3) . . . . ? O58 Co N11 C13 -82.8(3) . . . . ? N31 Co N11 C13 -170.4(3) . . . . ? N8 Co N11 C12 -139.8(2) . . . . ? O1 Co N11 C12 -5(3) . . . . ? O51 Co N11 C12 133.5(2) . . . . ? O58 Co N11 C12 38.7(2) . . . . ? N31 Co N11 C12 -49.0(2) . . . . ? N8 Co N31 N32 -69.7(3) . . . . ? O1 Co N31 N32 25.7(3) . . . . ? O51 Co N31 N32 -47(2) . . . . ? O58 Co N31 N32 113.0(3) . . . . ? N11 Co N31 N32 -155.4(3) . . . . ? Co N31 N32 N33 -176(5) . . . . ? N8 Co O51 C51 169.1(2) . . . . ? O1 Co O51 C51 73.6(2) . . . . ? O58 Co O51 C51 -13.5(2) . . . . ? N31 Co O51 C51 146(2) . . . . ? N11 Co O51 C51 -105.3(2) . . . . ? Co O51 C51 C56 8.7(4) . . . . ? Co O51 C51 C52 -173.41(18) . . . . ? O51 C51 C52 O52 -1.1(4) . . . . ? C56 C51 C52 O52 177.0(2) . . . . ? O51 C51 C52 C53 178.9(3) . . . . ? C56 C51 C52 C53 -3.0(4) . . . . ? C53 C52 O52 C521 5.0(4) . . . . ? C51 C52 O52 C521 -175.1(3) . . . . ? O52 C52 C53 C54 -178.7(3) . . . . ? C51 C52 C53 C54 1.4(5) . . . . ? C52 C53 C54 C55 0.9(5) . . . . ? C53 C54 C55 C56 -1.4(5) . . . . ? O51 C51 C56 C55 -179.5(3) . . . . ? C52 C51 C56 C55 2.5(4) . . . . ? O51 C51 C56 C57 2.3(5) . . . . ? C52 C51 C56 C57 -175.6(3) . . . . ? C54 C55 C56 C51 -0.4(5) . . . . ? C54 C55 C56 C57 177.9(3) . . . . ? C51 C56 C57 O58 -3.8(5) . . . . ? C55 C56 C57 O58 177.9(3) . . . . ? C56 C57 O58 Co -5.8(4) . . . . ? N8 Co O58 C57 135.0(18) . . . . ? O1 Co O58 C57 -76.2(2) . . . . ? O51 Co O58 C57 12.2(2) . . . . ? N31 Co O58 C57 -166.9(2) . . . . ? N11 Co O58 C57 105.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.502 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.057 #===END data_x80097 _database_code_depnum_ccdc_archive 'CCDC 281770' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 'Compound 7' _chemical_melting_point ? _chemical_formula_structural '[Mn (LH)2 )MeOH)2]. (ClO4)3' _chemical_formula_moiety 'C26 H44 Mn N4 O6, 3(Cl O4)' _chemical_formula_sum 'C26 H44 Cl3 Mn N4 O18' _chemical_formula_weight 861.94 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' Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 27.105(7) _cell_length_b 15.978(4) _cell_length_c 8.482(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.566(13) _cell_angle_gamma 90.00 _cell_volume 3649.5(17) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6662 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 27.06 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.662 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.581 _exptl_absorpt_correction_T_max 0.887 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BrukerNonius X8Apex2' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19581 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -34 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.34 _reflns_number_total 4090 _reflns_number_gt 3017 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0864P)^2^+15.9538P] 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 4090 _refine_ls_number_parameters 257 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0570 _refine_ls_wR_factor_ref 0.1769 _refine_ls_wR_factor_gt 0.1519 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Mn1 Mn 0.2500 0.2500 0.5000 0.0191(2) Uani 1 2 d S . . C1 C 0.19375(12) 0.1519(2) 0.2534(4) 0.0201(7) Uani 1 1 d . . . O1 O 0.20091(9) 0.18019(16) 0.4015(3) 0.0230(5) Uani 1 1 d . . . C2 C 0.14747(13) 0.1134(2) 0.2019(4) 0.0215(7) Uani 1 1 d . . . O2 O 0.28126(10) 0.14355(18) 0.6492(3) 0.0275(6) Uani 1 1 d . . . H2O H 0.3019(17) 0.154(3) 0.706(5) 0.027(13) Uiso 1 1 d . . . C3 C 0.13780(14) 0.0846(2) 0.0471(4) 0.0268(8) Uani 1 1 d . . . H3A H 0.1066 0.0597 0.0124 0.032 Uiso 1 1 calc R . . C4 C 0.17387(15) 0.0920(2) -0.0587(4) 0.0296(8) Uani 1 1 d . . . H4A H 0.1669 0.0725 -0.1646 0.036 Uiso 1 1 calc R . . C5 C 0.21881(14) 0.1272(2) -0.0100(4) 0.0255(8) Uani 1 1 d . . . H5A H 0.2431 0.1315 -0.0820 0.031 Uiso 1 1 calc R . . C6 C 0.22974(13) 0.1576(2) 0.1477(4) 0.0214(7) Uani 1 1 d . . . C7 C 0.27879(13) 0.1896(2) 0.1945(4) 0.0221(7) Uani 1 1 d . . . H7A H 0.3016 0.1866 0.1175 0.027 Uiso 1 1 calc R . . N8 N 0.29525(10) 0.22197(19) 0.3296(3) 0.0202(6) Uani 1 1 d . . . C9 C 0.34895(12) 0.2430(2) 0.3512(4) 0.0230(7) Uani 1 1 d . . . H9A H 0.3552 0.2902 0.4264 0.028 Uiso 1 1 calc R . . H9B H 0.3601 0.2595 0.2485 0.028 Uiso 1 1 calc R . . C10 C 0.37688(12) 0.1653(2) 0.4161(5) 0.0269(8) Uani 1 1 d . . . H10A H 0.3673 0.1522 0.5226 0.032 Uiso 1 1 calc R . . H10B H 0.3674 0.1171 0.3457 0.032 Uiso 1 1 calc R . . N11 N 0.43245(11) 0.1776(2) 0.4281(4) 0.0251(6) Uani 1 1 d . . . H11N H 0.4391(16) 0.204(3) 0.346(5) 0.030 Uiso 1 1 d . . . C12 C 0.45122(14) 0.2345(3) 0.5611(5) 0.0305(8) Uani 1 1 d . . . H12A H 0.4873 0.2409 0.5637 0.046 Uiso 1 1 calc R . . H12B H 0.4435 0.2105 0.6618 0.046 Uiso 1 1 calc R . . H12C H 0.4352 0.2893 0.5452 0.046 Uiso 1 1 calc R . . C13 C 0.45856(15) 0.0953(3) 0.4437(6) 0.0395(10) Uani 1 1 d . . . H13A H 0.4945 0.1044 0.4511 0.059 Uiso 1 1 calc R . . H13B H 0.4479 0.0607 0.3506 0.059 Uiso 1 1 calc R . . H13C H 0.4504 0.0668 0.5397 0.059 Uiso 1 1 calc R . . O14 O 0.11530(9) 0.10821(16) 0.3132(3) 0.0257(6) Uani 1 1 d . . . C15 C 0.06909(13) 0.0663(3) 0.2672(5) 0.0310(8) Uani 1 1 d . . . H15A H 0.0491 0.0664 0.3563 0.046 Uiso 1 1 calc R . . H15B H 0.0756 0.0085 0.2371 0.046 Uiso 1 1 calc R . . H15C H 0.0510 0.0955 0.1767 0.046 Uiso 1 1 calc R . . C16 C 0.27088(16) 0.0565(2) 0.6244(5) 0.0336(9) Uani 1 1 d . . . H16A H 0.2898 0.0238 0.7084 0.050 Uiso 0.50 1 calc PR . . H16B H 0.2804 0.0395 0.5210 0.050 Uiso 0.50 1 calc PR . . H16C H 0.2353 0.0464 0.6267 0.050 Uiso 0.50 1 calc PR . . H16D H 0.2472 0.0494 0.5290 0.050 Uiso 0.50 1 calc PR . . H16E H 0.2566 0.0337 0.7164 0.050 Uiso 0.50 1 calc PR . . H16F H 0.3017 0.0267 0.6107 0.050 Uiso 0.50 1 calc PR . . O1A O 0.14256(12) 0.3183(2) 0.1152(4) 0.0490(9) Uani 1 1 d . . . Cl1 Cl 0.10904(3) 0.38360(6) 0.05687(11) 0.0306(3) Uani 1 1 d . . . Cl2 Cl 0.0000 0.14586(9) 0.7500 0.0377(4) Uani 1 2 d S . . O2A O 0.07521(15) 0.4038(2) 0.1646(4) 0.0575(10) Uani 1 1 d . . . O3A O 0.1406(2) 0.4612(4) 0.0715(10) 0.0830(19) Uani 0.75 1 d P . . O3B O 0.1271(4) 0.4443(6) -0.0358(12) 0.069(2) Uiso 0.50 1 d P . . O4A O 0.0833(2) 0.3566(5) -0.0845(6) 0.120(3) Uani 0.75 1 d P . . O5S O -0.00163(19) 0.0999(2) 0.6112(4) 0.0457(12) Uani 0.75 1 d P . . O6A O 0.0579(2) 0.1593(4) 0.7503(8) 0.0465(16) Uani 0.50 1 d P . . O7A O 0.0196(2) 0.2275(4) 0.7842(7) 0.0803(19) Uani 0.75 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 Mn1 0.0142(3) 0.0303(4) 0.0132(3) -0.0015(3) 0.0029(2) -0.0021(3) C1 0.0198(16) 0.0255(17) 0.0150(15) -0.0002(13) 0.0019(12) 0.0017(13) O1 0.0179(11) 0.0373(14) 0.0141(11) -0.0039(10) 0.0030(9) -0.0057(10) C2 0.0197(16) 0.0256(16) 0.0189(16) 0.0018(13) 0.0004(13) 0.0001(13) O2 0.0244(13) 0.0368(15) 0.0201(13) 0.0022(11) -0.0020(11) 0.0000(12) C3 0.0258(18) 0.0321(19) 0.0215(18) -0.0030(15) -0.0021(14) -0.0042(15) C4 0.034(2) 0.037(2) 0.0180(17) -0.0041(15) -0.0001(15) -0.0002(17) C5 0.0288(18) 0.0328(19) 0.0157(16) 0.0009(14) 0.0060(14) 0.0008(15) C6 0.0211(16) 0.0275(17) 0.0161(15) 0.0005(13) 0.0040(13) 0.0015(14) C7 0.0207(16) 0.0289(17) 0.0180(16) 0.0007(14) 0.0073(13) 0.0015(14) N8 0.0162(13) 0.0287(14) 0.0160(13) 0.0006(11) 0.0033(10) 0.0001(11) C9 0.0172(16) 0.0327(18) 0.0200(16) -0.0001(14) 0.0061(13) -0.0040(14) C10 0.0152(16) 0.0357(19) 0.0300(19) 0.0015(16) 0.0037(14) -0.0015(14) N11 0.0182(14) 0.0331(16) 0.0246(15) 0.0005(13) 0.0048(12) -0.0015(12) C12 0.0245(18) 0.043(2) 0.0240(18) -0.0031(16) 0.0007(15) -0.0047(16) C13 0.0217(19) 0.041(2) 0.055(3) -0.004(2) -0.0012(18) 0.0019(17) O14 0.0190(12) 0.0390(14) 0.0193(12) -0.0033(10) 0.0030(9) -0.0063(11) C15 0.0205(17) 0.044(2) 0.0277(19) -0.0013(17) 0.0009(14) -0.0102(16) C16 0.038(2) 0.032(2) 0.032(2) 0.0005(16) 0.0090(17) 0.0018(17) O1A 0.0463(19) 0.0455(18) 0.050(2) -0.0049(15) -0.0179(15) 0.0131(15) Cl1 0.0232(4) 0.0460(6) 0.0233(5) 0.0058(4) 0.0056(3) 0.0060(4) Cl2 0.0483(8) 0.0313(7) 0.0300(7) 0.000 -0.0111(6) 0.000 O2A 0.078(3) 0.063(2) 0.0383(18) 0.0098(16) 0.0367(18) 0.022(2) O3A 0.051(3) 0.068(4) 0.128(6) 0.020(4) 0.003(4) -0.012(3) O4A 0.100(4) 0.208(7) 0.037(3) -0.079(4) -0.057(3) 0.124(5) O5S 0.094(3) 0.036(2) 0.0123(17) 0.0021(15) 0.0250(19) 0.023(2) O6A 0.028(3) 0.053(4) 0.055(4) 0.015(3) -0.008(3) -0.007(3) O7A 0.103(6) 0.086(4) 0.056(4) -0.008(3) 0.022(3) -0.022(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 Mn1 O1 1.860(2) 7_556 ? Mn1 O1 1.860(2) . ? Mn1 N8 2.049(3) . ? Mn1 N8 2.049(3) 7_556 ? Mn1 O2 2.229(3) 7_556 ? Mn1 O2 2.229(3) . ? C1 O1 1.328(4) . ? C1 C6 1.402(5) . ? C1 C2 1.420(5) . ? C2 O14 1.359(4) . ? C2 C3 1.388(5) . ? O2 C16 1.431(5) . ? O2 H2O 0.71(5) . ? C3 C4 1.405(5) . ? C3 H3A 0.9500 . ? C4 C5 1.362(5) . ? C4 H4A 0.9500 . ? C5 C6 1.422(5) . ? C5 H5A 0.9500 . ? C6 C7 1.437(5) . ? C7 N8 1.290(4) . ? C7 H7A 0.9500 . ? N8 C9 1.484(4) . ? C9 C10 1.524(5) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N11 1.511(4) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? N11 C13 1.491(5) . ? N11 C12 1.492(5) . ? N11 H11N 0.86(5) . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? O14 C15 1.434(4) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C16 H16D 0.9800 . ? C16 H16E 0.9800 . ? C16 H16F 0.9800 . ? O1A Cl1 1.434(3) . ? Cl1 O3B 1.374(9) . ? Cl1 O4A 1.386(4) . ? Cl1 O2A 1.404(3) . ? Cl1 O3A 1.503(6) . ? Cl2 O5S 1.385(4) . ? Cl2 O5S 1.385(4) 2_556 ? Cl2 O7A 1.426(6) 2_556 ? Cl2 O7A 1.426(6) . ? Cl2 O6A 1.584(6) 2_556 ? Cl2 O6A 1.584(6) . ? O3A O3B 0.979(10) . ? O6A O7A 1.555(9) . ? O7A O7A 1.151(12) 2_556 ? 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 O1 Mn1 O1 180.0 7_556 . ? O1 Mn1 N8 89.59(11) 7_556 . ? O1 Mn1 N8 90.42(11) . . ? O1 Mn1 N8 90.42(11) 7_556 7_556 ? O1 Mn1 N8 89.58(11) . 7_556 ? N8 Mn1 N8 180.0 . 7_556 ? O1 Mn1 O2 90.20(11) 7_556 7_556 ? O1 Mn1 O2 89.81(11) . 7_556 ? N8 Mn1 O2 89.18(11) . 7_556 ? N8 Mn1 O2 90.82(11) 7_556 7_556 ? O1 Mn1 O2 89.81(11) 7_556 . ? O1 Mn1 O2 90.19(11) . . ? N8 Mn1 O2 90.82(11) . . ? N8 Mn1 O2 89.18(11) 7_556 . ? O2 Mn1 O2 180.0 7_556 . ? O1 C1 C6 123.1(3) . . ? O1 C1 C2 117.8(3) . . ? C6 C1 C2 119.1(3) . . ? C1 O1 Mn1 130.4(2) . . ? O14 C2 C3 124.8(3) . . ? O14 C2 C1 115.3(3) . . ? C3 C2 C1 120.0(3) . . ? C16 O2 Mn1 127.1(2) . . ? C16 O2 H2O 116(4) . . ? Mn1 O2 H2O 115(4) . . ? C2 C3 C4 120.4(3) . . ? C2 C3 H3A 119.8 . . ? C4 C3 H3A 119.8 . . ? C5 C4 C3 120.3(3) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C6 120.6(3) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C1 C6 C5 119.6(3) . . ? C1 C6 C7 122.4(3) . . ? C5 C6 C7 117.9(3) . . ? N8 C7 C6 127.1(3) . . ? N8 C7 H7A 116.4 . . ? C6 C7 H7A 116.4 . . ? C7 N8 C9 115.8(3) . . ? C7 N8 Mn1 122.7(2) . . ? C9 N8 Mn1 121.4(2) . . ? N8 C9 C10 107.5(3) . . ? N8 C9 H9A 110.2 . . ? C10 C9 H9A 110.2 . . ? N8 C9 H9B 110.2 . . ? C10 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? N11 C10 C9 111.6(3) . . ? N11 C10 H10A 109.3 . . ? C9 C10 H10A 109.3 . . ? N11 C10 H10B 109.3 . . ? C9 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C13 N11 C12 110.6(3) . . ? C13 N11 C10 110.5(3) . . ? C12 N11 C10 112.4(3) . . ? C13 N11 H11N 112(3) . . ? C12 N11 H11N 103(3) . . ? C10 N11 H11N 108(3) . . ? N11 C12 H12A 109.5 . . ? N11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N11 C13 H13A 109.5 . . ? N11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C2 O14 C15 116.7(3) . . ? O14 C15 H15A 109.5 . . ? O14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? O14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O2 C16 H16A 109.5 . . ? O2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? O2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C16 H16D 109.5 . . ? H16A C16 H16D 141.1 . . ? H16B C16 H16D 56.3 . . ? H16C C16 H16D 56.3 . . ? O2 C16 H16E 109.5 . . ? H16A C16 H16E 56.3 . . ? H16B C16 H16E 141.1 . . ? H16C C16 H16E 56.3 . . ? H16D C16 H16E 109.5 . . ? O2 C16 H16F 109.5 . . ? H16A C16 H16F 56.3 . . ? H16B C16 H16F 56.3 . . ? H16C C16 H16F 141.1 . . ? H16D C16 H16F 109.5 . . ? H16E C16 H16F 109.5 . . ? O3B Cl1 O4A 84.4(6) . . ? O3B Cl1 O2A 120.8(4) . . ? O4A Cl1 O2A 109.4(3) . . ? O3B Cl1 O1A 117.2(4) . . ? O4A Cl1 O1A 108.0(3) . . ? O2A Cl1 O1A 112.2(2) . . ? O3B Cl1 O3A 39.5(4) . . ? O4A Cl1 O3A 123.6(5) . . ? O2A Cl1 O3A 99.4(3) . . ? O1A Cl1 O3A 103.9(3) . . ? O5S Cl2 O5S 115.9(3) . 2_556 ? O5S Cl2 O7A 109.7(3) . 2_556 ? O5S Cl2 O7A 129.3(3) 2_556 2_556 ? O5S Cl2 O7A 129.3(3) . . ? O5S Cl2 O7A 109.7(3) 2_556 . ? O7A Cl2 O7A 47.6(5) 2_556 . ? O5S Cl2 O6A 97.8(3) . 2_556 ? O5S Cl2 O6A 90.5(3) 2_556 2_556 ? O7A Cl2 O6A 62.0(4) 2_556 2_556 ? O7A Cl2 O6A 102.9(4) . 2_556 ? O5S Cl2 O6A 90.5(3) . . ? O5S Cl2 O6A 97.8(3) 2_556 . ? O7A Cl2 O6A 102.9(4) 2_556 . ? O7A Cl2 O6A 62.0(4) . . ? O6A Cl2 O6A 164.5(5) 2_556 . ? O3B O3A Cl1 63.1(7) . . ? O3A O3B Cl1 77.4(7) . . ? O7A O6A Cl2 54.0(3) . . ? O7A O7A Cl2 66.2(3) 2_556 . ? O7A O7A O6A 120.3(5) 2_556 . ? Cl2 O7A O6A 64.0(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 O1 Mn1 13.4(5) . . . . ? C2 C1 O1 Mn1 -167.3(2) . . . . ? O1 Mn1 O1 C1 -121(12) 7_556 . . . ? N8 Mn1 O1 C1 -20.8(3) . . . . ? N8 Mn1 O1 C1 159.2(3) 7_556 . . . ? O2 Mn1 O1 C1 68.4(3) 7_556 . . . ? O2 Mn1 O1 C1 -111.6(3) . . . . ? O1 C1 C2 O14 -1.2(5) . . . . ? C6 C1 C2 O14 178.1(3) . . . . ? O1 C1 C2 C3 178.5(3) . . . . ? C6 C1 C2 C3 -2.1(5) . . . . ? O1 Mn1 O2 C16 -164.9(3) 7_556 . . . ? O1 Mn1 O2 C16 15.1(3) . . . . ? N8 Mn1 O2 C16 -75.4(3) . . . . ? N8 Mn1 O2 C16 104.6(3) 7_556 . . . ? O2 Mn1 O2 C16 41(7) 7_556 . . . ? O14 C2 C3 C4 -179.2(3) . . . . ? C1 C2 C3 C4 1.0(5) . . . . ? C2 C3 C4 C5 0.4(6) . . . . ? C3 C4 C5 C6 -0.6(6) . . . . ? O1 C1 C6 C5 -178.8(3) . . . . ? C2 C1 C6 C5 1.9(5) . . . . ? O1 C1 C6 C7 4.3(5) . . . . ? C2 C1 C6 C7 -175.0(3) . . . . ? C4 C5 C6 C1 -0.5(5) . . . . ? C4 C5 C6 C7 176.5(3) . . . . ? C1 C6 C7 N8 -5.3(6) . . . . ? C5 C6 C7 N8 177.7(3) . . . . ? C6 C7 N8 C9 174.6(3) . . . . ? C6 C7 N8 Mn1 -9.1(5) . . . . ? O1 Mn1 N8 C7 -162.1(3) 7_556 . . . ? O1 Mn1 N8 C7 17.9(3) . . . . ? N8 Mn1 N8 C7 26.8(11) 7_556 . . . ? O2 Mn1 N8 C7 -71.9(3) 7_556 . . . ? O2 Mn1 N8 C7 108.1(3) . . . . ? O1 Mn1 N8 C9 14.0(3) 7_556 . . . ? O1 Mn1 N8 C9 -166.0(3) . . . . ? N8 Mn1 N8 C9 -157.1(11) 7_556 . . . ? O2 Mn1 N8 C9 104.2(3) 7_556 . . . ? O2 Mn1 N8 C9 -75.8(3) . . . . ? C7 N8 C9 C10 -88.1(4) . . . . ? Mn1 N8 C9 C10 95.6(3) . . . . ? N8 C9 C10 N11 174.7(3) . . . . ? C9 C10 N11 C13 -162.8(3) . . . . ? C9 C10 N11 C12 73.0(4) . . . . ? C3 C2 O14 C15 2.9(5) . . . . ? C1 C2 O14 C15 -177.3(3) . . . . ? O4A Cl1 O3A O3B -6.9(9) . . . . ? O2A Cl1 O3A O3B -127.9(7) . . . . ? O1A Cl1 O3A O3B 116.2(7) . . . . ? O4A Cl1 O3B O3A 174.2(7) . . . . ? O2A Cl1 O3B O3A 64.9(8) . . . . ? O1A Cl1 O3B O3A -78.4(7) . . . . ? O5S Cl2 O6A O7A 135.5(3) . . . . ? O5S Cl2 O6A O7A -108.2(3) 2_556 . . . ? O7A Cl2 O6A O7A 25.2(6) 2_556 . . . ? O6A Cl2 O6A O7A 13.2(3) 2_556 . . . ? O5S Cl2 O7A O7A 80.9(7) . . . 2_556 ? O5S Cl2 O7A O7A -125.8(6) 2_556 . . 2_556 ? O6A Cl2 O7A O7A -30.5(7) 2_556 . . 2_556 ? O6A Cl2 O7A O7A 145.8(8) . . . 2_556 ? O5S Cl2 O7A O6A -64.9(5) . . . . ? O5S Cl2 O7A O6A 88.4(4) 2_556 . . . ? O7A Cl2 O7A O6A -145.8(8) 2_556 . . . ? O6A Cl2 O7A O6A -176.40(14) 2_556 . . . ? Cl2 O6A O7A O7A -36.5(6) . . . 2_556 ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2O O1A 0.71(5) 2.06(5) 2.772(4) 175(5) 7_556 N11 H11N O7A 0.86(5) 1.98(5) 2.787(7) 156(4) 7_556 N11 H11N O6A 0.86(5) 2.33(5) 3.040(7) 141(4) 7_556 N11 H11N O4A 0.86(5) 2.44(4) 2.948(5) 119(4) 7 N11 H11N O7A 0.86(5) 2.54(5) 3.167(8) 130(4) 8 N11 H11N Cl2 0.86(5) 3.07(5) 3.772(3) 141(4) 7_556 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.404 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.111