# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2009 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'R Mukherjee' _publ_contact_author_email RNM@IITK.AC.IN _publ_section_title ; Six-coordinate CoIII and four-coordinate MII (M = Co, Zn) mixed-valence dimers supported by a deprotonated pyridine amide ligand: magnetism of a CoIIICoII complex and C-H...O/Cl/Br interactions ; loop_ _publ_author_name 'R Mukherjee' 'Wilson Jacob' 'F Lloret' 'Haritosh Mishra' 'Sharmila Pandey' # Attachment 'B814303J_final.cif' data_8maybm _database_code_depnum_ccdc_archive 'CCDC 639424' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H30 Cl2 Co2 N9 O3' _chemical_formula_sum 'C36 H30 Cl2 Co2 N9 O3' _chemical_formula_weight 825.45 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M p-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.573(5) _cell_length_b 11.596(5) _cell_length_c 16.367(5) _cell_angle_alpha 76.960(5) _cell_angle_beta 81.580(5) _cell_angle_gamma 66.012(5) _cell_volume 1951.3(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 1.96 _cell_measurement_theta_max 28.31 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 1.033 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8200 _exptl_absorpt_correction_T_max 0.9037 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13140 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.96 _diffrn_reflns_theta_max 28.31 _reflns_number_total 9315 _reflns_number_gt 6235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1019P)^2^+6.2353P] 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 9315 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1215 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2465 _refine_ls_wR_factor_gt 0.1973 _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.71993(7) 0.15895(8) 0.26908(4) 0.0205(2) Uani 1 1 d . . . Co2 Co 0.66082(7) 0.14027(8) 0.06322(5) 0.0216(2) Uani 1 1 d . . . Cl1 Cl 0.63510(19) 0.1211(3) -0.06452(12) 0.0589(6) Uani 1 1 d . . . Cl2A Cl 0.8628(7) 0.3623(8) 0.5080(5) 0.085(2) Uani 0.50 1 d P A 1 Cl2B Cl 0.8033(10) 0.4237(7) 0.4748(6) 0.132(4) Uani 0.50 1 d P B 2 O1 O 0.6417(4) 0.5120(4) 0.1340(3) 0.0368(11) Uani 1 1 d . . . O2 O 1.0339(4) -0.1137(5) 0.1890(3) 0.0358(11) Uani 1 1 d . . . O3 O 0.4166(4) 0.0638(4) 0.3070(3) 0.0354(11) Uani 1 1 d . . . N1 N 0.6196(5) 0.3044(6) 0.3229(3) 0.0333(12) Uani 1 1 d . . . N2 N 0.7180(4) 0.2924(5) 0.1726(3) 0.0224(10) Uani 1 1 d . . . N3 N 0.8019(4) 0.2052(5) 0.0501(3) 0.0226(10) Uani 1 1 d . . . N4 N 0.8840(4) 0.1554(5) 0.2877(3) 0.0218(10) Uani 1 1 d . . . N5 N 0.8235(4) 0.0166(4) 0.2134(3) 0.0204(9) Uani 1 1 d . . . N6 N 0.7022(4) -0.0349(4) 0.1354(3) 0.0224(10) Uani 1 1 d . . . N7 N 0.7124(5) 0.0295(6) 0.3656(3) 0.0303(12) Uani 1 1 d . . . N8 N 0.5582(4) 0.1570(4) 0.2483(3) 0.0203(10) Uani 1 1 d . . . N9 N 0.4997(5) 0.2646(5) 0.1114(3) 0.0273(11) Uani 1 1 d . . . C1 C 0.5723(7) 0.2991(9) 0.4027(4) 0.044(2) Uani 1 1 d . . . H1 H 0.5993 0.2193 0.4406 0.053 Uiso 1 1 calc R . . C2 C 0.4853(9) 0.4070(11) 0.4308(7) 0.067(3) Uani 1 1 d . . . H2 H 0.4517 0.4011 0.4875 0.080 Uiso 1 1 calc R . . C3 C 0.4469(8) 0.5238(11) 0.3766(7) 0.073(3) Uani 1 1 d . . . H3 H 0.3869 0.5985 0.3959 0.088 Uiso 1 1 calc R . . C4 C 0.4965(7) 0.5323(8) 0.2931(6) 0.050(2) Uani 1 1 d . . . H4 H 0.4709 0.6114 0.2543 0.060 Uiso 1 1 calc R . . C5 C 0.5848(6) 0.4194(6) 0.2697(4) 0.0324(14) Uani 1 1 d . . . C6 C 0.6491(6) 0.4153(6) 0.1846(4) 0.0305(13) Uani 1 1 d . . . C7 C 0.8100(5) 0.2727(5) 0.1046(3) 0.0203(11) Uani 1 1 d . . . C8 C 0.9068(6) 0.3159(6) 0.0962(4) 0.0274(13) Uani 1 1 d . . . H8 H 0.9077 0.3666 0.1341 0.033 Uiso 1 1 calc R . . C9 C 1.0024(6) 0.2867(6) 0.0335(4) 0.0335(14) Uani 1 1 d . . . C10 C 1.1118(7) 0.3258(8) 0.0276(5) 0.049(2) Uani 1 1 d . . . H10A H 1.1864 0.2511 0.0487 0.074 Uiso 1 1 calc R . . H10B H 1.0908 0.3924 0.0613 0.074 Uiso 1 1 calc R . . H10C H 1.1298 0.3596 -0.0312 0.074 Uiso 1 1 calc R . . C11 C 0.9925(6) 0.2174(6) -0.0215(4) 0.0317(14) Uani 1 1 d . . . H11 H 1.0550 0.1960 -0.0662 0.038 Uiso 1 1 calc R . . C12 C 0.8911(5) 0.1785(6) -0.0119(3) 0.0241(12) Uani 1 1 d . . . H12 H 0.8857 0.1316 -0.0509 0.029 Uiso 1 1 calc R . . C13 C 0.9054(6) 0.2387(6) 0.3242(4) 0.0286(13) Uani 1 1 d . . . H13 H 0.8377 0.2961 0.3538 0.034 Uiso 1 1 calc R . . C14 C 1.0243(6) 0.2405(7) 0.3186(4) 0.0314(14) Uani 1 1 d . . . H14 H 1.0370 0.3011 0.3430 0.038 Uiso 1 1 calc R . . C15 C 1.1247(6) 0.1563(7) 0.2786(4) 0.0354(16) Uani 1 1 d . . . H15 H 1.2068 0.1577 0.2753 0.043 Uiso 1 1 calc R . . C16 C 1.1043(5) 0.0690(7) 0.2428(4) 0.0311(14) Uani 1 1 d . . . H16 H 1.1719 0.0090 0.2147 0.037 Uiso 1 1 calc R . . C17 C 0.9826(5) 0.0715(6) 0.2491(3) 0.0243(12) Uani 1 1 d . . . C18 C 0.9505(5) -0.0208(6) 0.2147(3) 0.0250(13) Uani 1 1 d . . . C19 C 0.7812(5) -0.0745(5) 0.1971(4) 0.0221(11) Uani 1 1 d . . . C20 C 0.8166(5) -0.1973(6) 0.2455(4) 0.0312(14) Uani 1 1 d . . . H20 H 0.8749 -0.2241 0.2878 0.037 Uiso 1 1 calc R . . C21 C 0.7654(7) -0.2807(7) 0.2310(5) 0.0453(19) Uani 1 1 d . . . C22 C 0.7991(8) -0.4112(8) 0.2836(7) 0.067(3) Uani 1 1 d . . . H22A H 0.7268 -0.4139 0.3224 0.100 Uiso 1 1 calc R . . H22B H 0.8721 -0.4311 0.3157 0.100 Uiso 1 1 calc R . . H22C H 0.8205 -0.4745 0.2473 0.100 Uiso 1 1 calc R . . C23 C 0.6820(6) -0.2353(7) 0.1671(5) 0.0407(17) Uani 1 1 d . . . H23 H 0.6457 -0.2895 0.1553 0.049 Uiso 1 1 calc R . . C24 C 0.6515(6) -0.1144(6) 0.1214(4) 0.0332(14) Uani 1 1 d . . . H24 H 0.5933 -0.0853 0.0787 0.040 Uiso 1 1 calc R . . C25 C 0.8018(7) -0.0356(8) 0.4193(4) 0.049(2) Uani 1 1 d . . . H25 H 0.8720 -0.0119 0.4163 0.059 Uiso 1 1 calc R . . C26 C 0.7949(8) -0.1385(10) 0.4804(5) 0.067(3) Uani 1 1 d . . . H26 H 0.8587 -0.1836 0.5195 0.080 Uiso 1 1 calc R . . C27 C 0.6951(8) -0.1733(10) 0.4830(5) 0.066(3) Uani 1 1 d . . . H27 H 0.6908 -0.2453 0.5228 0.079 Uiso 1 1 calc R . . C28 C 0.6006(7) -0.1047(8) 0.4283(4) 0.048(2) Uani 1 1 d . . . H28 H 0.5290 -0.1263 0.4312 0.058 Uiso 1 1 calc R . . C29 C 0.6121(6) -0.0043(7) 0.3693(4) 0.0314(14) Uani 1 1 d . . . C30 C 0.5190(5) 0.0758(6) 0.3056(4) 0.0236(12) Uani 1 1 d . . . C31 C 0.4689(5) 0.2566(5) 0.1930(3) 0.0197(11) Uani 1 1 d . . . C32 C 0.3571(6) 0.3426(6) 0.2250(4) 0.0277(13) Uani 1 1 d . . . H32 H 0.3363 0.3327 0.2838 0.033 Uiso 1 1 calc R . . C33 C 0.2761(6) 0.4431(6) 0.1701(4) 0.0343(15) Uani 1 1 d . . . C34 C 0.1552(7) 0.5386(8) 0.2030(6) 0.052(2) Uani 1 1 d . . . H34C H 0.1557 0.6250 0.1857 0.079 Uiso 1 1 calc R . . H34B H 0.1484 0.5171 0.2645 0.079 Uiso 1 1 calc R . . H34A H 0.0828 0.5358 0.1803 0.079 Uiso 1 1 calc R . . C35 C 0.3104(6) 0.4521(6) 0.0848(4) 0.0326(14) Uani 1 1 d . . . H35 H 0.2574 0.5196 0.0454 0.039 Uiso 1 1 calc R . . C36 C 0.4220(5) 0.3622(6) 0.0578(4) 0.0258(12) Uani 1 1 d . . . H36 H 0.4450 0.3693 -0.0007 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0220(4) 0.0307(4) 0.0169(4) -0.0093(3) 0.0010(3) -0.0166(3) Co2 0.0210(4) 0.0266(4) 0.0202(4) -0.0081(3) -0.0014(3) -0.0103(3) Cl1 0.0480(11) 0.1090(19) 0.0378(10) -0.0235(11) -0.0038(8) -0.0429(12) Cl2A 0.091(4) 0.117(5) 0.095(5) -0.078(4) 0.055(4) -0.080(4) Cl2B 0.166(9) 0.071(4) 0.094(6) -0.003(4) 0.043(5) -0.004(5) O1 0.033(2) 0.024(2) 0.057(3) -0.012(2) -0.005(2) -0.0113(19) O2 0.023(2) 0.049(3) 0.040(3) -0.020(2) 0.0019(19) -0.013(2) O3 0.022(2) 0.040(3) 0.047(3) -0.002(2) -0.0011(19) -0.018(2) N1 0.033(3) 0.048(3) 0.037(3) -0.024(3) 0.007(2) -0.027(3) N2 0.016(2) 0.025(3) 0.026(2) -0.007(2) 0.0062(18) -0.0088(19) N3 0.019(2) 0.022(2) 0.027(2) -0.0003(19) -0.0021(19) -0.0104(19) N4 0.023(2) 0.039(3) 0.018(2) -0.014(2) 0.0000(18) -0.023(2) N5 0.023(2) 0.023(2) 0.022(2) -0.0034(19) -0.0058(18) -0.014(2) N6 0.026(2) 0.017(2) 0.030(3) -0.0131(19) -0.005(2) -0.009(2) N7 0.031(3) 0.056(4) 0.017(2) -0.010(2) 0.0080(19) -0.031(3) N8 0.016(2) 0.020(2) 0.033(3) -0.012(2) -0.0045(18) -0.0116(19) N9 0.024(3) 0.029(3) 0.032(3) -0.002(2) -0.003(2) -0.015(2) C1 0.049(4) 0.088(6) 0.033(3) -0.051(4) 0.030(3) -0.053(4) C2 0.067(6) 0.104(8) 0.076(6) -0.069(6) 0.034(5) -0.065(6) C3 0.043(5) 0.108(9) 0.106(8) -0.095(7) 0.049(5) -0.046(5) C4 0.035(4) 0.053(5) 0.077(6) -0.043(4) -0.002(4) -0.017(4) C5 0.022(3) 0.035(4) 0.048(4) -0.027(3) 0.006(3) -0.012(3) C6 0.025(3) 0.028(3) 0.042(4) -0.009(3) -0.005(3) -0.012(3) C7 0.026(3) 0.016(3) 0.025(3) -0.011(2) -0.001(2) -0.011(2) C8 0.033(3) 0.025(3) 0.026(3) -0.006(2) 0.003(2) -0.014(3) C9 0.026(3) 0.034(3) 0.035(3) 0.000(3) 0.000(3) -0.011(3) C10 0.033(4) 0.064(5) 0.056(5) -0.008(4) 0.004(3) -0.029(4) C11 0.022(3) 0.033(3) 0.034(3) -0.004(3) 0.008(2) -0.009(3) C12 0.026(3) 0.032(3) 0.017(3) -0.010(2) 0.008(2) -0.014(2) C13 0.035(3) 0.032(3) 0.028(3) -0.008(3) -0.006(2) -0.020(3) C14 0.039(4) 0.045(4) 0.023(3) -0.002(3) -0.011(3) -0.028(3) C15 0.029(3) 0.055(4) 0.031(3) 0.006(3) -0.012(3) -0.028(3) C16 0.018(3) 0.056(4) 0.027(3) -0.009(3) 0.000(2) -0.022(3) C17 0.025(3) 0.035(3) 0.022(3) -0.003(2) -0.007(2) -0.020(3) C18 0.023(3) 0.043(4) 0.014(2) -0.011(2) 0.010(2) -0.019(3) C19 0.026(3) 0.021(3) 0.026(3) -0.011(2) -0.001(2) -0.012(2) C20 0.019(3) 0.028(3) 0.050(4) -0.002(3) -0.004(3) -0.014(2) C21 0.031(4) 0.032(4) 0.076(6) -0.008(4) 0.000(4) -0.018(3) C22 0.046(5) 0.038(4) 0.120(8) 0.015(5) -0.022(5) -0.030(4) C23 0.027(3) 0.033(4) 0.069(5) -0.019(3) -0.004(3) -0.014(3) C24 0.026(3) 0.032(3) 0.045(4) -0.021(3) -0.005(3) -0.006(3) C25 0.055(5) 0.090(6) 0.020(3) 0.022(3) -0.024(3) -0.055(5) C26 0.059(5) 0.100(8) 0.050(5) 0.033(5) -0.024(4) -0.057(6) C27 0.068(6) 0.097(7) 0.044(5) 0.037(5) -0.028(4) -0.061(6) C28 0.045(4) 0.072(6) 0.035(4) 0.014(4) -0.008(3) -0.040(4) C29 0.034(3) 0.043(4) 0.025(3) -0.001(3) -0.001(2) -0.026(3) C30 0.015(2) 0.034(3) 0.030(3) -0.011(2) 0.009(2) -0.019(2) C31 0.016(2) 0.024(3) 0.024(3) -0.013(2) 0.002(2) -0.010(2) C32 0.028(3) 0.029(3) 0.033(3) -0.011(3) 0.001(2) -0.017(3) C33 0.026(3) 0.030(3) 0.048(4) -0.015(3) 0.001(3) -0.009(3) C34 0.042(4) 0.039(4) 0.070(6) -0.021(4) 0.001(4) -0.005(3) C35 0.030(3) 0.027(3) 0.043(4) -0.005(3) -0.003(3) -0.013(3) C36 0.020(3) 0.026(3) 0.029(3) 0.003(2) -0.008(2) -0.008(2) _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 N5 1.934(5) . ? Co1 N1 1.936(5) . ? Co1 N7 1.937(5) . ? Co1 N2 1.941(5) . ? Co1 N4 1.949(4) . ? Co1 N8 1.961(4) . ? Co2 N6 2.011(5) . ? Co2 N9 2.019(5) . ? Co2 N3 2.026(5) . ? Co2 Cl1 2.226(2) . ? O1 C6 1.214(8) . ? O2 C18 1.228(7) . ? O3 C30 1.245(6) . ? N1 C1 1.338(8) . ? N1 C5 1.357(9) . ? N2 C6 1.364(8) . ? N2 C7 1.413(7) . ? N3 C12 1.329(7) . ? N3 C7 1.347(7) . ? N4 C17 1.346(8) . ? N4 C13 1.360(7) . ? N5 C18 1.355(7) . ? N5 C19 1.418(7) . ? N6 C19 1.337(7) . ? N6 C24 1.349(8) . ? N7 C25 1.321(8) . ? N7 C29 1.358(7) . ? N8 C30 1.340(7) . ? N8 C31 1.432(7) . ? N9 C31 1.323(7) . ? N9 C36 1.347(7) . ? C1 C2 1.375(12) . ? C1 H1 0.9500 . ? C2 C3 1.380(15) . ? C2 H2 0.9500 . ? C3 C4 1.401(12) . ? C3 H3 0.9500 . ? C4 C5 1.389(9) . ? C4 H4 0.9500 . ? C5 C6 1.480(9) . ? C7 C8 1.381(8) . ? C8 C9 1.383(9) . ? C8 H8 0.9500 . ? C9 C11 1.378(10) . ? C9 C10 1.493(9) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.396(8) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.373(8) . ? C13 H13 0.9500 . ? C14 C15 1.370(10) . ? C14 H14 0.9500 . ? C15 C16 1.389(9) . ? C15 H15 0.9500 . ? C16 C17 1.385(7) . ? C16 H16 0.9500 . ? C17 C18 1.504(8) . ? C19 C20 1.390(8) . ? C20 C21 1.397(9) . ? C20 H20 0.9500 . ? C21 C23 1.392(11) . ? C21 C22 1.488(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.361(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.395(10) . ? C25 H25 0.9500 . ? C26 C27 1.362(11) . ? C26 H26 0.9500 . ? C27 C28 1.375(10) . ? C27 H27 0.9500 . ? C28 C29 1.374(9) . ? C28 H28 0.9500 . ? C29 C30 1.480(9) . ? C31 C32 1.389(8) . ? C32 C33 1.389(9) . ? C32 H32 0.9500 . ? C33 C35 1.387(9) . ? C33 C34 1.504(9) . ? C34 H34C 0.9800 . ? C34 H34B 0.9800 . ? C34 H34A 0.9800 . ? C35 C36 1.377(9) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 N5 Co1 N1 178.2(2) . . ? N5 Co1 N7 85.9(2) . . ? N1 Co1 N7 95.6(2) . . ? N5 Co1 N2 95.77(19) . . ? N1 Co1 N2 82.8(2) . . ? N7 Co1 N2 177.1(2) . . ? N5 Co1 N4 82.91(19) . . ? N1 Co1 N4 95.8(2) . . ? N7 Co1 N4 97.0(2) . . ? N2 Co1 N4 85.6(2) . . ? N5 Co1 N8 94.97(19) . . ? N1 Co1 N8 86.3(2) . . ? N7 Co1 N8 82.7(2) . . ? N2 Co1 N8 94.7(2) . . ? N4 Co1 N8 177.9(2) . . ? N6 Co2 N9 108.9(2) . . ? N6 Co2 N3 113.70(19) . . ? N9 Co2 N3 110.5(2) . . ? N6 Co2 Cl1 106.29(15) . . ? N9 Co2 Cl1 110.91(16) . . ? N3 Co2 Cl1 106.49(15) . . ? C1 N1 C5 119.3(6) . . ? C1 N1 Co1 126.2(6) . . ? C5 N1 Co1 114.1(4) . . ? C6 N2 C7 118.2(5) . . ? C6 N2 Co1 115.6(4) . . ? C7 N2 Co1 123.2(4) . . ? C12 N3 C7 118.5(5) . . ? C12 N3 Co2 120.0(4) . . ? C7 N3 Co2 121.4(4) . . ? C17 N4 C13 118.5(5) . . ? C17 N4 Co1 113.8(3) . . ? C13 N4 Co1 126.9(4) . . ? C18 N5 C19 116.2(5) . . ? C18 N5 Co1 116.0(4) . . ? C19 N5 Co1 124.4(4) . . ? C19 N6 C24 119.3(5) . . ? C19 N6 Co2 120.4(4) . . ? C24 N6 Co2 120.3(4) . . ? C25 N7 C29 119.7(6) . . ? C25 N7 Co1 125.6(4) . . ? C29 N7 Co1 114.2(4) . . ? C30 N8 C31 119.0(4) . . ? C30 N8 Co1 114.8(4) . . ? C31 N8 Co1 123.8(3) . . ? C31 N9 C36 118.8(5) . . ? C31 N9 Co2 123.1(4) . . ? C36 N9 Co2 118.1(4) . . ? N1 C1 C2 121.3(9) . . ? N1 C1 H1 119.3 . . ? C2 C1 H1 119.3 . . ? C1 C2 C3 119.8(8) . . ? C1 C2 H2 120.1 . . ? C3 C2 H2 120.1 . . ? C2 C3 C4 120.1(8) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C5 C4 C3 116.7(9) . . ? C5 C4 H4 121.7 . . ? C3 C4 H4 121.7 . . ? N1 C5 C4 122.8(7) . . ? N1 C5 C6 114.7(5) . . ? C4 C5 C6 122.5(7) . . ? O1 C6 N2 125.8(6) . . ? O1 C6 C5 122.3(6) . . ? N2 C6 C5 111.9(5) . . ? N3 C7 C8 121.5(5) . . ? N3 C7 N2 116.9(5) . . ? C8 C7 N2 121.5(5) . . ? C7 C8 C9 121.1(6) . . ? C7 C8 H8 119.5 . . ? C9 C8 H8 119.5 . . ? C11 C9 C8 116.4(6) . . ? C11 C9 C10 122.3(6) . . ? C8 C9 C10 121.3(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 C12 120.5(6) . . ? C9 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? N3 C12 C11 121.9(6) . . ? N3 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? N4 C13 C14 120.6(6) . . ? N4 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C15 C14 C13 121.1(6) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 C16 118.7(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C17 C16 C15 118.2(6) . . ? C17 C16 H16 120.9 . . ? C15 C16 H16 120.9 . . ? N4 C17 C16 122.8(5) . . ? N4 C17 C18 114.5(5) . . ? C16 C17 C18 122.7(6) . . ? O2 C18 N5 127.5(6) . . ? O2 C18 C17 121.1(5) . . ? N5 C18 C17 111.3(5) . . ? N6 C19 C20 121.9(5) . . ? N6 C19 N5 116.8(5) . . ? C20 C19 N5 121.3(5) . . ? C19 C20 C21 119.3(6) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C23 C21 C20 117.1(7) . . ? C23 C21 C22 122.6(7) . . ? C20 C21 C22 120.2(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C21 121.0(6) . . ? C24 C23 H23 119.5 . . ? C21 C23 H23 119.5 . . ? N6 C24 C23 121.4(6) . . ? N6 C24 H24 119.3 . . ? C23 C24 H24 119.3 . . ? N7 C25 C26 121.2(6) . . ? N7 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 118.9(7) . . ? C27 C26 H26 120.6 . . ? C25 C26 H26 120.6 . . ? C26 C27 C28 120.3(7) . . ? C26 C27 H27 119.9 . . ? C28 C27 H27 119.9 . . ? C29 C28 C27 118.4(7) . . ? C29 C28 H28 120.8 . . ? C27 C28 H28 120.8 . . ? N7 C29 C28 121.5(6) . . ? N7 C29 C30 114.3(5) . . ? C28 C29 C30 124.1(6) . . ? O3 C30 N8 125.6(6) . . ? O3 C30 C29 121.1(5) . . ? N8 C30 C29 113.3(5) . . ? N9 C31 C32 122.2(5) . . ? N9 C31 N8 117.1(5) . . ? C32 C31 N8 120.6(5) . . ? C33 C32 C31 119.4(6) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C35 C33 C32 118.0(6) . . ? C35 C33 C34 121.5(6) . . ? C32 C33 C34 120.5(6) . . ? C33 C34 H34C 109.5 . . ? C33 C34 H34B 109.5 . . ? H34C C34 H34B 109.5 . . ? C33 C34 H34A 109.5 . . ? H34C C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? C36 C35 C33 119.4(6) . . ? C36 C35 H35 120.3 . . ? C33 C35 H35 120.3 . . ? N9 C36 C35 122.3(6) . . ? N9 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Co1 N1 C1 -142(7) . . . . ? N7 Co1 N1 C1 2.2(6) . . . . ? N2 Co1 N1 C1 179.7(6) . . . . ? N4 Co1 N1 C1 -95.5(5) . . . . ? N8 Co1 N1 C1 84.5(5) . . . . ? N5 Co1 N1 C5 46(7) . . . . ? N7 Co1 N1 C5 -169.9(4) . . . . ? N2 Co1 N1 C5 7.6(4) . . . . ? N4 Co1 N1 C5 92.4(4) . . . . ? N8 Co1 N1 C5 -87.6(4) . . . . ? N5 Co1 N2 C6 178.7(4) . . . . ? N1 Co1 N2 C6 -2.5(4) . . . . ? N7 Co1 N2 C6 55(4) . . . . ? N4 Co1 N2 C6 -98.9(4) . . . . ? N8 Co1 N2 C6 83.2(4) . . . . ? N5 Co1 N2 C7 -21.4(4) . . . . ? N1 Co1 N2 C7 157.5(5) . . . . ? N7 Co1 N2 C7 -145(4) . . . . ? N4 Co1 N2 C7 61.0(4) . . . . ? N8 Co1 N2 C7 -116.9(4) . . . . ? N6 Co2 N3 C12 89.0(5) . . . . ? N9 Co2 N3 C12 -148.3(4) . . . . ? Cl1 Co2 N3 C12 -27.7(5) . . . . ? N6 Co2 N3 C7 -89.3(5) . . . . ? N9 Co2 N3 C7 33.5(5) . . . . ? Cl1 Co2 N3 C7 154.0(4) . . . . ? N5 Co1 N4 C17 5.9(4) . . . . ? N1 Co1 N4 C17 -172.8(4) . . . . ? N7 Co1 N4 C17 90.8(4) . . . . ? N2 Co1 N4 C17 -90.5(4) . . . . ? N8 Co1 N4 C17 8(6) . . . . ? N5 Co1 N4 C13 176.0(5) . . . . ? N1 Co1 N4 C13 -2.6(5) . . . . ? N7 Co1 N4 C13 -99.0(5) . . . . ? N2 Co1 N4 C13 79.6(5) . . . . ? N8 Co1 N4 C13 178(100) . . . . ? N1 Co1 N5 C18 48(7) . . . . ? N7 Co1 N5 C18 -95.6(4) . . . . ? N2 Co1 N5 C18 86.8(4) . . . . ? N4 Co1 N5 C18 2.0(4) . . . . ? N8 Co1 N5 C18 -177.9(4) . . . . ? N1 Co1 N5 C19 -153(7) . . . . ? N7 Co1 N5 C19 62.7(4) . . . . ? N2 Co1 N5 C19 -114.8(4) . . . . ? N4 Co1 N5 C19 160.3(5) . . . . ? N8 Co1 N5 C19 -19.6(4) . . . . ? N9 Co2 N6 C19 -94.4(5) . . . . ? N3 Co2 N6 C19 29.3(5) . . . . ? Cl1 Co2 N6 C19 146.1(4) . . . . ? N9 Co2 N6 C24 86.4(5) . . . . ? N3 Co2 N6 C24 -150.0(4) . . . . ? Cl1 Co2 N6 C24 -33.1(5) . . . . ? N5 Co1 N7 C25 80.0(7) . . . . ? N1 Co1 N7 C25 -98.9(7) . . . . ? N2 Co1 N7 C25 -156(4) . . . . ? N4 Co1 N7 C25 -2.3(7) . . . . ? N8 Co1 N7 C25 175.6(7) . . . . ? N5 Co1 N7 C29 -91.6(5) . . . . ? N1 Co1 N7 C29 89.5(5) . . . . ? N2 Co1 N7 C29 33(4) . . . . ? N4 Co1 N7 C29 -173.9(5) . . . . ? N8 Co1 N7 C29 4.0(5) . . . . ? N5 Co1 N8 C30 86.0(4) . . . . ? N1 Co1 N8 C30 -95.4(4) . . . . ? N7 Co1 N8 C30 0.8(4) . . . . ? N2 Co1 N8 C30 -177.8(4) . . . . ? N4 Co1 N8 C30 84(6) . . . . ? N5 Co1 N8 C31 -111.8(4) . . . . ? N1 Co1 N8 C31 66.9(4) . . . . ? N7 Co1 N8 C31 163.0(4) . . . . ? N2 Co1 N8 C31 -15.6(4) . . . . ? N4 Co1 N8 C31 -114(5) . . . . ? N6 Co2 N9 C31 34.6(5) . . . . ? N3 Co2 N9 C31 -90.9(5) . . . . ? Cl1 Co2 N9 C31 151.2(4) . . . . ? N6 Co2 N9 C36 -147.3(4) . . . . ? N3 Co2 N9 C36 87.1(5) . . . . ? Cl1 Co2 N9 C36 -30.7(5) . . . . ? C5 N1 C1 C2 2.6(9) . . . . ? Co1 N1 C1 C2 -169.2(5) . . . . ? N1 C1 C2 C3 -1.0(11) . . . . ? C1 C2 C3 C4 0.0(12) . . . . ? C2 C3 C4 C5 -0.7(11) . . . . ? C1 N1 C5 C4 -3.4(9) . . . . ? Co1 N1 C5 C4 169.4(5) . . . . ? C1 N1 C5 C6 176.2(5) . . . . ? Co1 N1 C5 C6 -11.0(7) . . . . ? C3 C4 C5 N1 2.4(10) . . . . ? C3 C4 C5 C6 -177.2(6) . . . . ? C7 N2 C6 O1 14.7(9) . . . . ? Co1 N2 C6 O1 175.7(5) . . . . ? C7 N2 C6 C5 -163.6(5) . . . . ? Co1 N2 C6 C5 -2.6(6) . . . . ? N1 C5 C6 O1 -169.5(6) . . . . ? C4 C5 C6 O1 10.2(10) . . . . ? N1 C5 C6 N2 8.9(8) . . . . ? C4 C5 C6 N2 -171.5(6) . . . . ? C12 N3 C7 C8 1.1(8) . . . . ? Co2 N3 C7 C8 179.4(4) . . . . ? C12 N3 C7 N2 -176.2(5) . . . . ? Co2 N3 C7 N2 2.0(7) . . . . ? C6 N2 C7 N3 -125.7(6) . . . . ? Co1 N2 C7 N3 74.8(6) . . . . ? C6 N2 C7 C8 56.9(8) . . . . ? Co1 N2 C7 C8 -102.6(6) . . . . ? N3 C7 C8 C9 -2.8(9) . . . . ? N2 C7 C8 C9 174.4(6) . . . . ? C7 C8 C9 C11 2.6(9) . . . . ? C7 C8 C9 C10 -175.9(6) . . . . ? C8 C9 C11 C12 -0.9(9) . . . . ? C10 C9 C11 C12 177.6(6) . . . . ? C7 N3 C12 C11 0.6(9) . . . . ? Co2 N3 C12 C11 -177.7(4) . . . . ? C9 C11 C12 N3 -0.7(9) . . . . ? C17 N4 C13 C14 2.6(9) . . . . ? Co1 N4 C13 C14 -167.1(4) . . . . ? N4 C13 C14 C15 -1.9(9) . . . . ? C13 C14 C15 C16 0.5(9) . . . . ? C14 C15 C16 C17 0.3(9) . . . . ? C13 N4 C17 C16 -1.9(8) . . . . ? Co1 N4 C17 C16 169.1(5) . . . . ? C13 N4 C17 C18 177.0(5) . . . . ? Co1 N4 C17 C18 -11.9(6) . . . . ? C15 C16 C17 N4 0.5(9) . . . . ? C15 C16 C17 C18 -178.4(6) . . . . ? C19 N5 C18 O2 14.3(8) . . . . ? Co1 N5 C18 O2 174.4(5) . . . . ? C19 N5 C18 C17 -168.6(5) . . . . ? Co1 N5 C18 C17 -8.5(6) . . . . ? N4 C17 C18 O2 -169.3(5) . . . . ? C16 C17 C18 O2 9.6(9) . . . . ? N4 C17 C18 N5 13.4(7) . . . . ? C16 C17 C18 N5 -167.7(5) . . . . ? C24 N6 C19 C20 2.5(8) . . . . ? Co2 N6 C19 C20 -176.8(4) . . . . ? C24 N6 C19 N5 -175.0(5) . . . . ? Co2 N6 C19 N5 5.7(7) . . . . ? C18 N5 C19 N6 -127.7(5) . . . . ? Co1 N5 C19 N6 74.0(6) . . . . ? C18 N5 C19 C20 54.8(7) . . . . ? Co1 N5 C19 C20 -103.5(6) . . . . ? N6 C19 C20 C21 -1.9(9) . . . . ? N5 C19 C20 C21 175.5(6) . . . . ? C19 C20 C21 C23 0.9(10) . . . . ? C19 C20 C21 C22 -178.2(7) . . . . ? C20 C21 C23 C24 -0.4(11) . . . . ? C22 C21 C23 C24 178.7(7) . . . . ? C19 N6 C24 C23 -2.0(9) . . . . ? Co2 N6 C24 C23 177.3(5) . . . . ? C21 C23 C24 N6 0.9(10) . . . . ? C29 N7 C25 C26 -0.3(12) . . . . ? Co1 N7 C25 C26 -171.5(7) . . . . ? N7 C25 C26 C27 1.3(15) . . . . ? C25 C26 C27 C28 -2.4(16) . . . . ? C26 C27 C28 C29 2.5(15) . . . . ? C25 N7 C29 C28 0.4(11) . . . . ? Co1 N7 C29 C28 172.5(6) . . . . ? C25 N7 C29 C30 -179.8(6) . . . . ? Co1 N7 C29 C30 -7.7(7) . . . . ? C27 C28 C29 N7 -1.5(12) . . . . ? C27 C28 C29 C30 178.7(8) . . . . ? C31 N8 C30 O3 13.1(9) . . . . ? Co1 N8 C30 O3 176.2(5) . . . . ? C31 N8 C30 C29 -168.1(5) . . . . ? Co1 N8 C30 C29 -4.9(6) . . . . ? N7 C29 C30 O3 -172.8(6) . . . . ? C28 C29 C30 O3 7.0(10) . . . . ? N7 C29 C30 N8 8.3(8) . . . . ? C28 C29 C30 N8 -171.9(7) . . . . ? C36 N9 C31 C32 2.4(8) . . . . ? Co2 N9 C31 C32 -179.6(4) . . . . ? C36 N9 C31 N8 -175.6(5) . . . . ? Co2 N9 C31 N8 2.4(7) . . . . ? C30 N8 C31 N9 -126.6(5) . . . . ? Co1 N8 C31 N9 71.9(6) . . . . ? C30 N8 C31 C32 55.4(7) . . . . ? Co1 N8 C31 C32 -106.2(5) . . . . ? N9 C31 C32 C33 -2.1(9) . . . . ? N8 C31 C32 C33 175.9(5) . . . . ? C31 C32 C33 C35 0.8(9) . . . . ? C31 C32 C33 C34 -179.3(6) . . . . ? C32 C33 C35 C36 0.1(9) . . . . ? C34 C33 C35 C36 -179.9(6) . . . . ? C31 N9 C36 C35 -1.5(9) . . . . ? Co2 N9 C36 C35 -179.6(5) . . . . ? C33 C35 C36 N9 0.3(9) . . . . ? _diffrn_measured_fraction_theta_max 0.956 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.956 _refine_diff_density_max 1.679 _refine_diff_density_min -1.196 _refine_diff_density_rms 0.157 #===END data_25maybm _database_code_depnum_ccdc_archive 'CCDC 698530' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H34 Br2 Co2 N9 O4' _chemical_formula_sum 'C37 H34 Br2 Co2 N9 O4' _chemical_formula_weight 946.41 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' 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 12.340(5) _cell_length_b 16.429(5) _cell_length_c 20.045(5) _cell_angle_alpha 93.162(5) _cell_angle_beta 94.169(5) _cell_angle_gamma 93.594(5) _cell_volume 4038(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.01 _cell_measurement_theta_max 28.32 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.557 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1900 _exptl_absorpt_coefficient_mu 2.850 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5995 _exptl_absorpt_correction_T_max 0.7636 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26746 _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_sigmaI/netI 0.1112 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 28.32 _reflns_number_total 19176 _reflns_number_gt 10026 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1148P)^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_extinction_coef ? _refine_ls_number_reflns 19176 _refine_ls_number_parameters 971 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.0885 _refine_ls_wR_factor_ref 0.2832 _refine_ls_wR_factor_gt 0.2206 _refine_ls_goodness_of_fit_ref 1.230 _refine_ls_restrained_S_all 1.230 _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 Co1 Co 0.77468(8) 0.26126(6) 0.46152(5) 0.0230(2) Uani 1 1 d . . . Co2 Co 0.74458(8) 0.04923(6) 0.40092(5) 0.0253(2) Uani 1 1 d . . . Co1' Co 0.22649(10) 0.74104(7) 0.03314(6) 0.0393(3) Uani 1 1 d . . . Co2' Co 0.24173(9) 0.95018(6) 0.09487(5) 0.0317(3) Uani 1 1 d . . . Br1 Br 0.72303(8) -0.08804(5) 0.35573(5) 0.0455(3) Uani 1 1 d . . . Br2 Br 0.82029(9) 0.59325(6) 0.68695(5) 0.0551(3) Uani 1 1 d . . . Br1' Br 0.24458(8) 1.08634(6) 0.14089(5) 0.0494(3) Uani 1 1 d . . . Br2' Br 0.74357(16) 0.54397(12) 0.15517(8) 0.1182(6) Uani 1 1 d . . . O1 O 0.4589(4) 0.1931(3) 0.4755(3) 0.0313(12) Uani 1 1 d . . . O2 O 0.8351(5) 0.2458(3) 0.2677(3) 0.0375(13) Uani 1 1 d . . . O3 O 0.9608(4) 0.1392(3) 0.5877(2) 0.0298(12) Uani 1 1 d . . . O1' O 0.3348(6) 0.7415(4) 0.2250(4) 0.080(3) Uani 1 1 d . . . O2' O 0.4279(5) 0.8620(4) -0.0809(3) 0.0452(15) Uani 1 1 d . . . O3' O -0.0802(5) 0.8085(4) 0.0177(3) 0.0440(15) Uani 1 1 d . . . N1 N 0.7040(5) 0.3047(3) 0.5386(3) 0.0245(13) Uani 1 1 d . . . N2 N 0.6311(4) 0.2062(3) 0.4371(3) 0.0185(12) Uani 1 1 d . . . N3 N 0.6365(5) 0.1135(4) 0.3451(3) 0.0301(14) Uani 1 1 d . . . N4 N 0.7324(5) 0.3500(3) 0.4055(3) 0.0228(13) Uani 1 1 d . . . N5 N 0.8375(5) 0.2217(4) 0.3798(3) 0.0248(13) Uani 1 1 d . . . N6 N 0.8996(5) 0.0922(4) 0.3905(3) 0.0257(13) Uani 1 1 d . . . N7 N 0.9197(4) 0.3084(4) 0.4913(3) 0.0229(13) Uani 1 1 d . . . N8 N 0.8201(5) 0.1728(3) 0.5177(3) 0.0238(13) Uani 1 1 d . . . N9 N 0.7096(5) 0.0497(3) 0.4975(3) 0.0227(13) Uani 1 1 d . . . N1' N 0.1716(7) 0.6535(5) 0.0868(4) 0.056(2) Uani 1 1 d . . . N2' N 0.3093(6) 0.7779(4) 0.1167(4) 0.0424(18) Uani 1 1 d . . . N3' N 0.3925(5) 0.9083(4) 0.1088(3) 0.0339(15) Uani 1 1 d . . . N4' N 0.3578(8) 0.6910(5) 0.0082(4) 0.062(2) Uani 1 1 d . . . N5' N 0.2835(6) 0.8286(4) -0.0184(3) 0.0374(16) Uani 1 1 d . . . N6' N 0.1956(5) 0.9500(3) -0.0028(3) 0.0262(14) Uani 1 1 d . . . N7' N 0.1333(7) 0.7053(4) -0.0473(3) 0.0422(18) Uani 1 1 d . . . N8' N 0.0989(5) 0.7974(4) 0.0557(3) 0.0326(15) Uani 1 1 d . . . N9' N 0.1358(5) 0.8886(4) 0.1499(3) 0.0323(15) Uani 1 1 d . . . C1 C 0.7466(7) 0.3578(4) 0.5868(4) 0.0292(17) Uani 1 1 d . . . H1 H 0.8200 0.3787 0.5858 0.035 Uiso 1 1 calc R . . C2 C 0.6868(7) 0.3833(5) 0.6382(4) 0.0345(19) Uani 1 1 d . . . H2 H 0.7171 0.4244 0.6706 0.041 Uiso 1 1 calc R . . C3 C 0.5857(7) 0.3502(6) 0.6427(4) 0.045(2) Uani 1 1 d . . . H3 H 0.5453 0.3662 0.6792 0.054 Uiso 1 1 calc R . . C4 C 0.5399(7) 0.2918(5) 0.5931(4) 0.039(2) Uani 1 1 d . . . H4 H 0.4698 0.2656 0.5962 0.047 Uiso 1 1 calc R . . C5 C 0.5986(6) 0.2746(5) 0.5414(4) 0.0299(17) Uani 1 1 d . . . C6 C 0.5545(6) 0.2197(4) 0.4816(3) 0.0273(9) Uani 1 1 d . . . C7 C 0.5952(5) 0.1790(4) 0.3718(3) 0.0192(14) Uani 1 1 d . . . C8 C 0.5223(6) 0.2231(5) 0.3345(4) 0.0322(17) Uani 1 1 d . . . H8 H 0.4892 0.2676 0.3553 0.039 Uiso 1 1 calc R . . C9 C 0.4978(7) 0.2016(5) 0.2658(4) 0.0352(19) Uani 1 1 d . . . C10 C 0.4315(6) 0.2525(5) 0.2235(4) 0.038(2) Uani 1 1 d . . . H10A H 0.4791 0.2924 0.2030 0.057 Uiso 1 1 calc R . . H10B H 0.3817 0.2813 0.2510 0.057 Uiso 1 1 calc R . . H10C H 0.3892 0.2178 0.1882 0.057 Uiso 1 1 calc R . . C11 C 0.5442(6) 0.1321(5) 0.2396(4) 0.0360(19) Uani 1 1 d . . . H11 H 0.5293 0.1140 0.1939 0.043 Uiso 1 1 calc R . . C12 C 0.6103(6) 0.0917(5) 0.2806(4) 0.0332(18) Uani 1 1 d . . . H12 H 0.6404 0.0444 0.2622 0.040 Uiso 1 1 calc R . . C13 C 0.6814(7) 0.4159(4) 0.4245(4) 0.0339(18) Uani 1 1 d . . . H13 H 0.6719 0.4278 0.4705 0.041 Uiso 1 1 calc R . . C14 C 0.6425(7) 0.4667(5) 0.3768(4) 0.040(2) Uani 1 1 d . . . H14 H 0.6089 0.5146 0.3907 0.048 Uiso 1 1 calc R . . C15 C 0.6512(7) 0.4493(6) 0.3097(4) 0.043(2) Uani 1 1 d . . . H15 H 0.6223 0.4835 0.2771 0.052 Uiso 1 1 calc R . . C16 C 0.7035(6) 0.3808(5) 0.2914(4) 0.0327(18) Uani 1 1 d . . . H16 H 0.7106 0.3665 0.2454 0.039 Uiso 1 1 calc R . . C17 C 0.7448(6) 0.3335(4) 0.3396(4) 0.0284(16) Uani 1 1 d . . . C18 C 0.8102(6) 0.2615(4) 0.3255(4) 0.0273(9) Uani 1 1 d . . . C19 C 0.9210(6) 0.1688(4) 0.3781(4) 0.0255(16) Uani 1 1 d . . . C20 C 1.0260(6) 0.1980(5) 0.3650(3) 0.0268(16) Uani 1 1 d . . . H20 H 1.0390 0.2536 0.3554 0.032 Uiso 1 1 calc R . . C21 C 1.1123(6) 0.1460(5) 0.3661(4) 0.0291(17) Uani 1 1 d . . . C22 C 1.2260(6) 0.1728(5) 0.3512(4) 0.0380(19) Uani 1 1 d . . . H22A H 1.2299 0.2312 0.3432 0.057 Uiso 1 1 calc R . . H22B H 1.2457 0.1417 0.3113 0.057 Uiso 1 1 calc R . . H22C H 1.2767 0.1632 0.3894 0.057 Uiso 1 1 calc R . . C23 C 1.0859(6) 0.0647(5) 0.3813(4) 0.0310(17) Uani 1 1 d . . . H23 H 1.1410 0.0269 0.3839 0.037 Uiso 1 1 calc R . . C24 C 0.9786(6) 0.0394(4) 0.3925(4) 0.0304(17) Uani 1 1 d . . . H24 H 0.9613 -0.0159 0.4016 0.036 Uiso 1 1 calc R . . C25 C 0.9681(6) 0.3767(4) 0.4713(3) 0.0273(9) Uani 1 1 d . . . H25 H 0.9270 0.4121 0.4452 0.033 Uiso 1 1 calc R . . C26 C 1.0809(6) 0.3972(5) 0.4887(4) 0.0335(18) Uani 1 1 d . . . H26 H 1.1161 0.4450 0.4735 0.040 Uiso 1 1 calc R . . C27 C 1.1359(7) 0.3473(5) 0.5271(4) 0.0370(19) Uani 1 1 d . . . H27 H 1.2102 0.3617 0.5410 0.044 Uiso 1 1 calc R . . C28 C 1.0879(6) 0.2763(5) 0.5469(4) 0.0314(17) Uani 1 1 d . . . H28 H 1.1284 0.2405 0.5730 0.038 Uiso 1 1 calc R . . C29 C 0.9797(5) 0.2583(4) 0.5279(4) 0.0223(15) Uani 1 1 d . . . C30 C 0.9184(6) 0.1825(4) 0.5482(4) 0.0246(15) Uani 1 1 d . . . C31 C 0.7461(6) 0.1140(4) 0.5413(4) 0.0239(15) Uani 1 1 d . . . C32 C 0.7131(6) 0.1207(5) 0.6063(4) 0.0299(17) Uani 1 1 d . . . H32 H 0.7399 0.1660 0.6356 0.036 Uiso 1 1 calc R . . C33 C 0.6422(6) 0.0622(5) 0.6282(4) 0.0317(18) Uani 1 1 d . . . C34 C 0.6037(7) 0.0679(6) 0.6971(4) 0.042(2) Uani 1 1 d . . . H34A H 0.6104 0.0155 0.7175 0.063 Uiso 1 1 calc R . . H34B H 0.5274 0.0814 0.6946 0.063 Uiso 1 1 calc R . . H34C H 0.6482 0.1107 0.7244 0.063 Uiso 1 1 calc R . . C35 C 0.6064(6) -0.0051(4) 0.5829(4) 0.0308(18) Uani 1 1 d . . . H35 H 0.5578 -0.0474 0.5961 0.037 Uiso 1 1 calc R . . C36 C 0.6424(6) -0.0083(5) 0.5205(3) 0.0276(16) Uani 1 1 d . . . H36 H 0.6188 -0.0544 0.4912 0.033 Uiso 1 1 calc R . . C1' C 0.0971(10) 0.5942(6) 0.0672(5) 0.072(4) Uani 1 1 d . . . H1' H 0.0745 0.5859 0.0208 0.086 Uiso 1 1 calc R . . C2' C 0.0514(11) 0.5443(7) 0.1113(6) 0.077(4) Uani 1 1 d . . . H2' H -0.0050 0.5043 0.0958 0.092 Uiso 1 1 calc R . . C3' C 0.0863(12) 0.5518(8) 0.1771(5) 0.086(4) Uani 1 1 d . . . H3' H 0.0597 0.5147 0.2079 0.103 Uiso 1 1 calc R . . C4' C 0.1619(9) 0.6153(7) 0.1978(5) 0.070(3) Uani 1 1 d . . . H4' H 0.1844 0.6256 0.2439 0.084 Uiso 1 1 calc R . . C5' C 0.2043(8) 0.6634(5) 0.1508(5) 0.050(3) Uani 1 1 d . . . C6' C 0.2930(9) 0.7311(6) 0.1694(4) 0.053(3) Uani 1 1 d . . . C7' C 0.4041(7) 0.8311(5) 0.1208(4) 0.040(2) Uani 1 1 d . . . C8' C 0.5105(8) 0.8027(7) 0.1324(6) 0.072(3) Uani 1 1 d . . . H8' H 0.5194 0.7474 0.1419 0.086 Uiso 1 1 calc R . . C9' C 0.5983(8) 0.8555(6) 0.1298(7) 0.073(4) Uani 1 1 d . . . C10' C 0.7142(10) 0.8257(8) 0.1401(10) 0.118(6) Uani 1 1 d . . . H10D H 0.7098 0.7690 0.1532 0.176 Uiso 1 1 calc R . . H10E H 0.7562 0.8604 0.1755 0.176 Uiso 1 1 calc R . . H10F H 0.7503 0.8287 0.0983 0.176 Uiso 1 1 calc R . . C11' C 0.5847(8) 0.9338(6) 0.1165(5) 0.053(2) Uani 1 1 d . . . H11' H 0.6463 0.9710 0.1142 0.063 Uiso 1 1 calc R . . C12' C 0.4790(8) 0.9603(5) 0.1061(4) 0.043(2) Uani 1 1 d . . . H12' H 0.4693 1.0157 0.0970 0.052 Uiso 1 1 calc R . . C13' C 0.3921(12) 0.6213(8) 0.0323(8) 0.100(5) Uani 1 1 d . . . H13' H 0.3451 0.5866 0.0554 0.121 Uiso 1 1 calc R . . C14' C 0.499(2) 0.6014(12) 0.0225(11) 0.179(11) Uani 1 1 d . . . H14' H 0.5215 0.5500 0.0354 0.215 Uiso 1 1 calc R . . C15' C 0.5721(17) 0.6548(13) -0.0059(13) 0.194(13) Uani 1 1 d . . . H15' H 0.6474 0.6457 -0.0051 0.233 Uiso 1 1 calc R . . C16' C 0.5312(13) 0.7200(10) -0.0346(9) 0.120(6) Uani 1 1 d . . . H16' H 0.5745 0.7519 -0.0620 0.144 Uiso 1 1 calc R . . C17' C 0.4276(9) 0.7404(7) -0.0243(6) 0.066(3) Uani 1 1 d . . . C18' C 0.3796(9) 0.8156(5) -0.0444(4) 0.045(2) Uani 1 1 d . . . C19' C 0.2216(7) 0.8878(5) -0.0463(4) 0.0339(18) Uani 1 1 d . . . C20' C 0.1893(6) 0.8848(4) -0.1143(4) 0.0296(17) Uani 1 1 d . . . H20' H 0.2096 0.8417 -0.1434 0.036 Uiso 1 1 calc R . . C21' C 0.1268(7) 0.9456(5) -0.1392(4) 0.038(2) Uani 1 1 d . . . C22' C 0.0843(8) 0.9420(5) -0.2122(4) 0.048(2) Uani 1 1 d . . . H22D H 0.0988 0.8893 -0.2339 0.071 Uiso 1 1 calc R . . H22E H 0.1209 0.9862 -0.2348 0.071 Uiso 1 1 calc R . . H22F H 0.0056 0.9483 -0.2153 0.071 Uiso 1 1 calc R . . C23' C 0.0978(6) 1.0089(5) -0.0948(4) 0.0326(18) Uani 1 1 d . . . H23' H 0.0531 1.0501 -0.1101 0.039 Uiso 1 1 calc R . . C24' C 0.1361(6) 1.0092(5) -0.0287(4) 0.0345(18) Uani 1 1 d . . . H24' H 0.1201 1.0535 0.0006 0.041 Uiso 1 1 calc R . . C25' C 0.1644(10) 0.6564(5) -0.0993(4) 0.057(3) Uani 1 1 d . . . H25' H 0.2315 0.6309 -0.0966 0.069 Uiso 1 1 calc R . . C26' C 0.0920(12) 0.6462(6) -0.1564(5) 0.070(4) Uani 1 1 d . . . H26' H 0.1113 0.6121 -0.1929 0.084 Uiso 1 1 calc R . . C27' C -0.0033(10) 0.6814(6) -0.1632(4) 0.057(3) Uani 1 1 d . . . H27' H -0.0486 0.6732 -0.2037 0.069 Uiso 1 1 calc R . . C28' C -0.0345(9) 0.7302(5) -0.1097(4) 0.052(3) Uani 1 1 d . . . H28' H -0.1010 0.7564 -0.1121 0.062 Uiso 1 1 calc R . . C29' C 0.0396(8) 0.7385(5) -0.0509(4) 0.042(2) Uani 1 1 d . . . C30' C 0.0080(9) 0.7858(5) 0.0107(4) 0.041(2) Uani 1 1 d . . . C31' C 0.0767(7) 0.8224(5) 0.1221(4) 0.0347(19) Uani 1 1 d . . . C32' C 0.0051(7) 0.7780(5) 0.1592(3) 0.0319(18) Uani 1 1 d . . . H32' H -0.0381 0.7325 0.1383 0.038 Uiso 1 1 calc R . . C33' C -0.0036(7) 0.7994(6) 0.2260(5) 0.043(2) Uani 1 1 d . . . C34' C -0.0731(8) 0.7490(6) 0.2681(5) 0.052(2) Uani 1 1 d . . . H34D H -0.1274 0.7827 0.2871 0.078 Uiso 1 1 calc R . . H34E H -0.0274 0.7281 0.3045 0.078 Uiso 1 1 calc R . . H34F H -0.1102 0.7031 0.2404 0.078 Uiso 1 1 calc R . . C35' C 0.0574(6) 0.8687(5) 0.2532(4) 0.0342(18) Uani 1 1 d . . . H35' H 0.0527 0.8865 0.2988 0.041 Uiso 1 1 calc R . . C36' C 0.1252(6) 0.9116(5) 0.2137(4) 0.0328(18) Uani 1 1 d . . . H36' H 0.1658 0.9593 0.2327 0.039 Uiso 1 1 calc R . . O1S O 0.9752(6) 0.4532(6) 0.6387(5) 0.095(3) Uani 1 1 d . . . H1S H 0.9366 0.4935 0.6410 0.142 Uiso 1 1 calc R . . O2S O 0.6706(5) 0.5445(3) 0.5476(3) 0.0414(14) Uani 1 1 d . . . H2S H 0.7135 0.5524 0.5822 0.062 Uiso 1 1 calc R . . C1S C 1.0675(9) 0.4714(8) 0.6716(5) 0.071(3) Uani 1 1 d . . . H1S1 H 1.0916 0.5281 0.6648 0.107 Uiso 1 1 calc R . . H1S2 H 1.1213 0.4349 0.6558 0.107 Uiso 1 1 calc R . . H1S3 H 1.0601 0.4650 0.7194 0.107 Uiso 1 1 calc R . . C2S C 0.6029(8) 0.6073(7) 0.5438(6) 0.067(3) Uani 1 1 d . . . H2S1 H 0.5686 0.6147 0.5861 0.101 Uiso 1 1 calc R . . H2S2 H 0.5464 0.5944 0.5070 0.101 Uiso 1 1 calc R . . H2S3 H 0.6451 0.6577 0.5354 0.101 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0273(5) 0.0191(5) 0.0217(5) -0.0010(4) -0.0005(4) -0.0007(4) Co2 0.0273(5) 0.0223(5) 0.0254(5) -0.0023(4) 0.0012(4) -0.0017(4) Co1' 0.0594(8) 0.0257(6) 0.0321(6) 0.0034(5) 0.0007(5) 0.0007(5) Co2' 0.0391(6) 0.0305(6) 0.0241(5) 0.0003(4) -0.0025(4) -0.0033(5) Br1 0.0498(5) 0.0317(5) 0.0523(6) -0.0098(4) -0.0008(4) -0.0027(4) Br2 0.0789(7) 0.0397(5) 0.0411(6) -0.0025(4) -0.0136(5) -0.0146(5) Br1' 0.0609(6) 0.0400(5) 0.0436(5) -0.0073(4) -0.0043(4) -0.0063(4) Br2' 0.1433(16) 0.1265(15) 0.0886(12) 0.0212(10) -0.0018(10) 0.0385(12) O1 0.025(3) 0.036(3) 0.031(3) -0.003(2) 0.004(2) -0.003(2) O2 0.049(4) 0.033(3) 0.030(3) 0.007(2) 0.000(3) 0.000(3) O3 0.033(3) 0.027(3) 0.029(3) 0.005(2) 0.001(2) -0.002(2) O1' 0.099(6) 0.065(5) 0.065(5) 0.039(4) -0.044(4) -0.053(4) O2' 0.044(4) 0.051(4) 0.041(4) 0.002(3) 0.009(3) 0.004(3) O3' 0.055(4) 0.040(4) 0.034(3) 0.000(3) -0.014(3) 0.000(3) N1 0.033(3) 0.019(3) 0.023(3) -0.003(2) 0.004(3) 0.011(3) N2 0.017(3) 0.016(3) 0.021(3) -0.012(2) 0.007(2) -0.013(2) N3 0.028(3) 0.036(4) 0.024(3) 0.001(3) -0.004(3) -0.005(3) N4 0.031(3) 0.018(3) 0.019(3) 0.001(2) -0.001(2) 0.003(2) N5 0.026(3) 0.033(3) 0.016(3) -0.003(2) 0.003(2) 0.007(3) N6 0.023(3) 0.026(3) 0.028(3) -0.003(3) 0.008(2) 0.002(3) N7 0.013(3) 0.031(3) 0.023(3) -0.007(3) 0.002(2) -0.003(2) N8 0.023(3) 0.022(3) 0.024(3) 0.003(2) -0.007(2) -0.003(2) N9 0.038(3) 0.020(3) 0.008(3) -0.003(2) 0.004(2) -0.012(3) N1' 0.096(7) 0.039(4) 0.028(4) 0.005(3) -0.008(4) -0.017(4) N2' 0.044(4) 0.038(4) 0.044(4) 0.012(3) -0.011(3) -0.002(3) N3' 0.030(4) 0.038(4) 0.034(4) 0.006(3) -0.002(3) 0.005(3) N4' 0.088(7) 0.039(5) 0.062(6) 0.022(4) 0.003(5) 0.012(5) N5' 0.051(4) 0.027(4) 0.034(4) -0.003(3) 0.003(3) 0.006(3) N6' 0.041(4) 0.014(3) 0.022(3) 0.007(2) -0.007(3) -0.003(3) N7' 0.067(5) 0.028(4) 0.031(4) 0.006(3) -0.003(3) 0.000(4) N8' 0.044(4) 0.036(4) 0.016(3) 0.002(3) -0.007(3) -0.010(3) N9' 0.048(4) 0.031(3) 0.015(3) -0.004(3) -0.007(3) -0.001(3) C1 0.043(5) 0.015(3) 0.029(4) -0.009(3) 0.002(3) 0.007(3) C2 0.045(5) 0.032(4) 0.025(4) -0.002(3) -0.007(3) 0.004(4) C3 0.041(5) 0.059(6) 0.032(5) -0.019(4) 0.005(4) 0.001(4) C4 0.031(4) 0.048(5) 0.037(5) -0.006(4) 0.002(3) -0.015(4) C5 0.037(4) 0.033(4) 0.019(4) -0.008(3) 0.004(3) 0.000(3) C6 0.037(2) 0.025(2) 0.018(2) -0.0021(17) -0.0001(17) -0.0060(18) C7 0.012(3) 0.019(3) 0.024(4) -0.012(3) -0.006(2) 0.001(2) C8 0.038(4) 0.037(4) 0.022(4) 0.001(3) 0.006(3) 0.004(4) C9 0.041(5) 0.034(4) 0.029(4) 0.008(4) 0.002(3) -0.009(4) C10 0.035(4) 0.035(4) 0.040(5) 0.000(4) -0.014(4) -0.013(3) C11 0.040(5) 0.038(5) 0.027(4) -0.009(4) -0.002(3) -0.010(4) C12 0.033(4) 0.032(4) 0.029(4) -0.009(3) -0.011(3) -0.016(3) C13 0.045(5) 0.017(4) 0.040(5) 0.000(3) 0.005(4) -0.004(3) C14 0.049(5) 0.027(4) 0.045(5) 0.004(4) 0.003(4) 0.021(4) C15 0.049(5) 0.053(6) 0.030(5) 0.006(4) 0.002(4) 0.017(4) C16 0.037(4) 0.044(5) 0.019(4) 0.004(3) 0.006(3) 0.009(4) C17 0.036(4) 0.016(3) 0.033(4) 0.005(3) -0.001(3) 0.000(3) C18 0.037(2) 0.025(2) 0.018(2) -0.0021(17) -0.0001(17) -0.0060(18) C19 0.029(4) 0.018(3) 0.027(4) -0.005(3) -0.001(3) -0.008(3) C20 0.030(4) 0.030(4) 0.021(4) -0.003(3) 0.004(3) 0.003(3) C21 0.018(4) 0.034(4) 0.034(4) 0.001(3) 0.005(3) -0.004(3) C22 0.034(5) 0.038(5) 0.044(5) 0.002(4) 0.014(4) 0.000(4) C23 0.034(4) 0.024(4) 0.036(4) 0.001(3) 0.002(3) 0.007(3) C24 0.037(4) 0.014(3) 0.039(5) 0.004(3) -0.004(3) -0.005(3) C25 0.037(2) 0.025(2) 0.018(2) -0.0021(17) -0.0001(17) -0.0060(18) C26 0.032(4) 0.036(4) 0.033(4) 0.001(4) 0.009(3) -0.003(4) C27 0.034(4) 0.039(5) 0.036(5) -0.005(4) 0.005(3) -0.005(4) C28 0.030(4) 0.028(4) 0.035(4) 0.002(3) 0.002(3) 0.001(3) C29 0.012(3) 0.021(3) 0.033(4) -0.009(3) 0.001(3) 0.005(3) C30 0.021(4) 0.022(4) 0.030(4) -0.004(3) 0.003(3) 0.000(3) C31 0.032(4) 0.012(3) 0.029(4) 0.014(3) -0.002(3) 0.000(3) C32 0.026(4) 0.039(4) 0.022(4) -0.007(3) -0.006(3) -0.003(3) C33 0.021(4) 0.031(4) 0.042(5) 0.005(4) -0.005(3) 0.000(3) C34 0.043(5) 0.048(5) 0.036(5) 0.010(4) 0.007(4) 0.003(4) C35 0.033(4) 0.014(3) 0.044(5) 0.006(3) 0.000(3) -0.010(3) C36 0.029(4) 0.044(5) 0.010(3) -0.001(3) 0.011(3) 0.000(3) C1' 0.121(10) 0.038(5) 0.047(6) 0.020(5) -0.019(6) -0.048(6) C2' 0.105(10) 0.056(7) 0.064(8) 0.011(6) -0.016(7) -0.026(6) C3' 0.136(12) 0.079(8) 0.032(6) 0.018(6) -0.030(6) -0.036(8) C4' 0.087(8) 0.073(7) 0.043(6) 0.028(5) -0.028(5) -0.031(6) C5' 0.080(7) 0.016(4) 0.051(6) 0.026(4) -0.027(5) -0.006(4) C6' 0.076(7) 0.055(6) 0.024(5) 0.012(4) -0.018(4) -0.019(5) C7' 0.042(5) 0.030(4) 0.043(5) 0.005(4) -0.014(4) -0.010(4) C8' 0.040(6) 0.059(7) 0.117(10) 0.028(7) -0.006(6) 0.007(5) C9' 0.036(6) 0.042(6) 0.144(12) 0.024(7) 0.004(6) 0.002(5) C10' 0.052(8) 0.061(8) 0.24(2) 0.049(10) 0.002(10) 0.005(6) C11' 0.040(5) 0.054(6) 0.064(7) 0.018(5) 0.000(4) 0.001(4) C12' 0.058(6) 0.033(5) 0.038(5) 0.010(4) -0.001(4) -0.006(4) C13' 0.105(11) 0.075(9) 0.134(13) 0.051(9) 0.030(10) 0.047(9) C14' 0.25(3) 0.130(16) 0.20(2) 0.095(15) 0.100(19) 0.149(19) C15' 0.147(18) 0.17(2) 0.31(3) 0.15(2) 0.113(19) 0.117(17) C16' 0.116(13) 0.120(13) 0.145(15) 0.048(11) 0.070(11) 0.073(11) C17' 0.059(7) 0.071(8) 0.074(8) 0.019(6) 0.010(6) 0.029(6) C18' 0.076(7) 0.029(4) 0.031(5) 0.000(4) 0.009(5) -0.004(4) C19' 0.043(5) 0.020(4) 0.038(5) 0.002(3) 0.003(4) 0.000(3) C20' 0.046(5) 0.024(4) 0.018(4) 0.004(3) 0.005(3) -0.004(3) C21' 0.048(5) 0.038(5) 0.026(4) -0.002(4) -0.003(4) -0.003(4) C22' 0.084(7) 0.035(5) 0.021(4) 0.000(4) -0.009(4) 0.001(5) C23' 0.028(4) 0.034(4) 0.033(4) -0.002(3) -0.006(3) -0.003(3) C24' 0.042(5) 0.038(5) 0.021(4) -0.008(3) -0.002(3) -0.009(4) C25' 0.130(10) 0.030(5) 0.008(4) -0.004(3) 0.007(5) -0.020(5) C26' 0.133(11) 0.042(6) 0.033(6) -0.008(5) 0.037(7) -0.039(7) C27' 0.100(9) 0.044(6) 0.020(4) -0.003(4) -0.004(5) -0.041(6) C28' 0.087(7) 0.042(5) 0.021(4) -0.001(4) -0.006(4) -0.026(5) C29' 0.067(6) 0.025(4) 0.029(5) 0.005(3) -0.008(4) -0.015(4) C30' 0.074(7) 0.019(4) 0.028(5) 0.005(3) -0.010(4) -0.009(4) C31' 0.046(5) 0.034(4) 0.021(4) 0.000(3) -0.009(3) -0.011(4) C32' 0.044(5) 0.040(5) 0.011(3) -0.001(3) 0.003(3) 0.004(4) C33' 0.032(5) 0.049(5) 0.046(5) 0.006(4) -0.003(4) 0.003(4) C34' 0.064(6) 0.046(6) 0.046(6) 0.006(4) 0.009(5) -0.012(5) C35' 0.036(4) 0.036(4) 0.030(4) 0.002(4) 0.008(3) -0.003(4) C36' 0.042(5) 0.034(4) 0.020(4) -0.009(3) -0.007(3) -0.001(4) O1S 0.057(5) 0.129(8) 0.088(6) -0.058(6) -0.007(5) -0.001(5) O2S 0.051(4) 0.032(3) 0.039(4) -0.010(3) -0.001(3) 0.003(3) C1S 0.062(7) 0.097(9) 0.048(7) -0.012(6) -0.008(5) -0.019(6) C2S 0.042(6) 0.093(9) 0.071(8) -0.004(6) 0.013(5) 0.038(6) _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 N7 1.944(5) . ? Co1 N1 1.953(6) . ? Co1 N2 1.955(5) . ? Co1 N5 1.959(6) . ? Co1 N4 1.962(6) . ? Co1 N8 1.971(6) . ? Co2 N9 2.014(5) . ? Co2 N6 2.027(6) . ? Co2 N3 2.058(6) . ? Co2 Br1 2.3752(14) . ? Co1' N5' 1.942(7) . ? Co1' N2' 1.944(7) . ? Co1' N8' 1.945(7) . ? Co1' N4' 1.947(9) . ? Co1' N7' 1.952(7) . ? Co1' N1' 1.959(8) . ? Co2' N6' 1.998(6) . ? Co2' N9' 2.029(7) . ? Co2' N3' 2.030(6) . ? Co2' Br1' 2.3694(15) . ? O1 C6 1.228(8) . ? O2 C18 1.238(8) . ? O3 C30 1.206(8) . ? O1' C6' 1.193(10) . ? O2' C18' 1.242(10) . ? O3' C30' 1.188(11) . ? N1 C1 1.321(9) . ? N1 C5 1.368(10) . ? N2 C6 1.365(9) . ? N2 C7 1.391(8) . ? N3 C7 1.323(9) . ? N3 C12 1.333(9) . ? N4 C13 1.336(9) . ? N4 C17 1.355(9) . ? N5 C18 1.334(9) . ? N5 C19 1.389(9) . ? N6 C19 1.311(9) . ? N6 C24 1.344(9) . ? N7 C25 1.333(9) . ? N7 C29 1.351(9) . ? N8 C30 1.315(8) . ? N8 C31 1.412(9) . ? N9 C36 1.347(9) . ? N9 C31 1.367(9) . ? N1' C5' 1.315(11) . ? N1' C1' 1.319(11) . ? N2' C6' 1.360(11) . ? N2' C7' 1.410(10) . ? N3' C7' 1.318(10) . ? N3' C12' 1.332(10) . ? N4' C13' 1.346(13) . ? N4' C17' 1.370(14) . ? N5' C18' 1.354(12) . ? N5' C19' 1.391(10) . ? N6' C24' 1.358(10) . ? N6' C19' 1.375(10) . ? N7' C29' 1.308(11) . ? N7' C25' 1.373(11) . ? N8' C30' 1.383(10) . ? N8' C31' 1.422(10) . ? N9' C36' 1.331(9) . ? N9' C31' 1.342(9) . ? C1 C2 1.372(10) . ? C1 H1 0.9500 . ? C2 C3 1.340(12) . ? C2 H2 0.9500 . ? C3 C4 1.405(11) . ? C3 H3 0.9500 . ? C4 C5 1.334(11) . ? C4 H4 0.9500 . ? C5 C6 1.508(10) . ? C7 C8 1.392(10) . ? C8 C9 1.411(10) . ? C8 H8 0.9500 . ? C9 C11 1.401(11) . ? C9 C10 1.467(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.345(11) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.383(11) . ? C13 H13 0.9500 . ? C14 C15 1.372(11) . ? C14 H14 0.9500 . ? C15 C16 1.378(11) . ? C15 H15 0.9500 . ? C16 C17 1.364(10) . ? C16 H16 0.9500 . ? C17 C18 1.498(10) . ? C19 C20 1.401(10) . ? C20 C21 1.406(10) . ? C20 H20 0.9500 . ? C21 C23 1.410(10) . ? C21 C22 1.501(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.400(11) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.425(10) . ? C25 H25 0.9500 . ? C26 C27 1.335(11) . ? C26 H26 0.9500 . ? C27 C28 1.366(11) . ? C27 H27 0.9500 . ? C28 C29 1.371(9) . ? C28 H28 0.9500 . ? C29 C30 1.507(10) . ? C31 C32 1.393(10) . ? C32 C33 1.371(10) . ? C32 H32 0.9500 . ? C33 C35 1.419(10) . ? C33 C34 1.492(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.357(10) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C1' C2' 1.367(14) . ? C1' H1' 0.9500 . ? C2' C3' 1.353(14) . ? C2' H2' 0.9500 . ? C3' C4' 1.381(15) . ? C3' H3' 0.9500 . ? C4' C5' 1.374(13) . ? C4' H4' 0.9500 . ? C5' C6' 1.521(12) . ? C7' C8' 1.428(13) . ? C8' C9' 1.351(14) . ? C8' H8' 0.9500 . ? C9' C11' 1.347(13) . ? C9' C10' 1.545(15) . ? C10' H10D 0.9800 . ? C10' H10E 0.9800 . ? C10' H10F 0.9800 . ? C11' C12' 1.405(12) . ? C11' H11' 0.9500 . ? C12' H12' 0.9500 . ? C13' C14' 1.40(2) . ? C13' H13' 0.9500 . ? C14' C15' 1.39(3) . ? C14' H14' 0.9500 . ? C15' C16' 1.35(2) . ? C15' H15' 0.9500 . ? C16' C17' 1.369(16) . ? C16' H16' 0.9500 . ? C17' C18' 1.467(13) . ? C19' C20' 1.389(10) . ? C20' C21' 1.393(11) . ? C20' H20' 0.9500 . ? C21' C23' 1.413(11) . ? C21' C22' 1.515(11) . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23' C24' 1.373(10) . ? C23' H23' 0.9500 . ? C24' H24' 0.9500 . ? C25' C26' 1.395(15) . ? C25' H25' 0.9500 . ? C26' C27' 1.344(16) . ? C26' H26' 0.9500 . ? C27' C28' 1.394(13) . ? C27' H27' 0.9500 . ? C28' C29' 1.433(12) . ? C28' H28' 0.9500 . ? C29' C30' 1.511(12) . ? C31' C32' 1.392(11) . ? C32' C33' 1.378(11) . ? C32' H32' 0.9500 . ? C33' C35' 1.388(12) . ? C33' C34' 1.494(12) . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C35' C36' 1.381(11) . ? C35' H35' 0.9500 . ? C36' H36' 0.9500 . ? O1S C1S 1.284(11) . ? O1S H1S 0.8400 . ? O2S C2S 1.370(10) . ? O2S H2S 0.8400 . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S H2S1 0.9800 . ? C2S H2S2 0.9800 . ? C2S H2S3 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 N7 Co1 N1 95.7(2) . . ? N7 Co1 N2 174.9(2) . . ? N1 Co1 N2 83.4(2) . . ? N7 Co1 N5 86.8(2) . . ? N1 Co1 N5 175.6(2) . . ? N2 Co1 N5 94.4(2) . . ? N7 Co1 N4 96.7(2) . . ? N1 Co1 N4 93.4(2) . . ? N2 Co1 N4 88.4(2) . . ? N5 Co1 N4 82.7(2) . . ? N7 Co1 N8 82.3(2) . . ? N1 Co1 N8 87.1(2) . . ? N2 Co1 N8 92.6(2) . . ? N5 Co1 N8 96.8(2) . . ? N4 Co1 N8 178.9(3) . . ? N9 Co2 N6 112.4(2) . . ? N9 Co2 N3 111.4(3) . . ? N6 Co2 N3 110.4(3) . . ? N9 Co2 Br1 107.88(16) . . ? N6 Co2 Br1 108.13(17) . . ? N3 Co2 Br1 106.37(18) . . ? N5' Co1' N2' 95.6(3) . . ? N5' Co1' N8' 94.1(3) . . ? N2' Co1' N8' 93.5(3) . . ? N5' Co1' N4' 82.4(3) . . ? N2' Co1' N4' 86.3(4) . . ? N8' Co1' N4' 176.4(3) . . ? N5' Co1' N7' 86.5(3) . . ? N2' Co1' N7' 175.7(3) . . ? N8' Co1' N7' 82.5(3) . . ? N4' Co1' N7' 97.8(4) . . ? N5' Co1' N1' 178.7(3) . . ? N2' Co1' N1' 83.2(3) . . ? N8' Co1' N1' 86.3(3) . . ? N4' Co1' N1' 97.2(4) . . ? N7' Co1' N1' 94.8(3) . . ? N6' Co2' N9' 114.8(2) . . ? N6' Co2' N3' 110.6(3) . . ? N9' Co2' N3' 110.3(3) . . ? N6' Co2' Br1' 108.06(17) . . ? N9' Co2' Br1' 103.31(18) . . ? N3' Co2' Br1' 109.5(2) . . ? C1 N1 C5 118.5(6) . . ? C1 N1 Co1 127.5(6) . . ? C5 N1 Co1 114.0(5) . . ? C6 N2 C7 118.0(5) . . ? C6 N2 Co1 115.3(4) . . ? C7 N2 Co1 123.3(4) . . ? C7 N3 C12 118.8(6) . . ? C7 N3 Co2 120.6(5) . . ? C12 N3 Co2 120.5(5) . . ? C13 N4 C17 119.6(6) . . ? C13 N4 Co1 126.9(5) . . ? C17 N4 Co1 112.9(4) . . ? C18 N5 C19 119.4(6) . . ? C18 N5 Co1 114.7(5) . . ? C19 N5 Co1 124.6(5) . . ? C19 N6 C24 120.9(6) . . ? C19 N6 Co2 120.4(5) . . ? C24 N6 Co2 118.6(5) . . ? C25 N7 C29 118.9(6) . . ? C25 N7 Co1 126.7(5) . . ? C29 N7 Co1 113.5(5) . . ? C30 N8 C31 117.6(6) . . ? C30 N8 Co1 116.5(5) . . ? C31 N8 Co1 123.4(4) . . ? C36 N9 C31 117.0(6) . . ? C36 N9 Co2 122.3(4) . . ? C31 N9 Co2 120.4(5) . . ? C5' N1' C1' 118.6(8) . . ? C5' N1' Co1' 113.8(6) . . ? C1' N1' Co1' 127.0(6) . . ? C6' N2' C7' 117.7(7) . . ? C6' N2' Co1' 115.4(6) . . ? C7' N2' Co1' 123.9(6) . . ? C7' N3' C12' 120.9(7) . . ? C7' N3' Co2' 120.4(6) . . ? C12' N3' Co2' 118.7(6) . . ? C13' N4' C17' 119.6(11) . . ? C13' N4' Co1' 124.2(9) . . ? C17' N4' Co1' 114.7(6) . . ? C18' N5' C19' 117.3(7) . . ? C18' N5' Co1' 115.0(5) . . ? C19' N5' Co1' 124.7(6) . . ? C24' N6' C19' 117.4(6) . . ? C24' N6' Co2' 122.2(5) . . ? C19' N6' Co2' 120.4(5) . . ? C29' N7' C25' 121.4(8) . . ? C29' N7' Co1' 113.7(6) . . ? C25' N7' Co1' 124.6(7) . . ? C30' N8' C31' 114.7(7) . . ? C30' N8' Co1' 116.8(6) . . ? C31' N8' Co1' 124.2(5) . . ? C36' N9' C31' 119.1(7) . . ? C36' N9' Co2' 121.3(5) . . ? C31' N9' Co2' 119.6(5) . . ? N1 C1 C2 121.2(8) . . ? N1 C1 H1 119.4 . . ? C2 C1 H1 119.4 . . ? C3 C2 C1 120.0(8) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C2 C3 C4 119.7(8) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 117.4(8) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C4 C5 N1 122.8(7) . . ? C4 C5 C6 122.7(7) . . ? N1 C5 C6 114.5(6) . . ? O1 C6 N2 126.2(6) . . ? O1 C6 C5 121.2(7) . . ? N2 C6 C5 112.6(6) . . ? N3 C7 N2 118.7(6) . . ? N3 C7 C8 121.1(6) . . ? N2 C7 C8 120.1(6) . . ? C7 C8 C9 119.7(7) . . ? C7 C8 H8 120.1 . . ? C9 C8 H8 120.1 . . ? C11 C9 C8 116.9(7) . . ? C11 C9 C10 122.1(7) . . ? C8 C9 C10 120.9(8) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 118.8(7) . . ? C12 C11 H11 120.6 . . ? C9 C11 H11 120.6 . . ? N3 C12 C11 124.6(8) . . ? N3 C12 H12 117.7 . . ? C11 C12 H12 117.7 . . ? N4 C13 C14 119.7(8) . . ? N4 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 121.4(7) . . ? C15 C14 H14 119.3 . . ? C13 C14 H14 119.3 . . ? C14 C15 C16 117.8(8) . . ? C14 C15 H15 121.1 . . ? C16 C15 H15 121.1 . . ? C17 C16 C15 119.6(7) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? N4 C17 C16 121.9(7) . . ? N4 C17 C18 114.3(6) . . ? C16 C17 C18 123.8(7) . . ? O2 C18 N5 126.9(7) . . ? O2 C18 C17 119.5(7) . . ? N5 C18 C17 113.6(6) . . ? N6 C19 N5 118.6(6) . . ? N6 C19 C20 121.3(7) . . ? N5 C19 C20 120.1(6) . . ? C19 C20 C21 120.7(7) . . ? C19 C20 H20 119.6 . . ? C21 C20 H20 119.6 . . ? C20 C21 C23 115.9(7) . . ? C20 C21 C22 123.4(7) . . ? C23 C21 C22 120.6(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C21 120.2(7) . . ? C24 C23 H23 119.9 . . ? C21 C23 H23 119.9 . . ? N6 C24 C23 121.0(6) . . ? N6 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? N7 C25 C26 120.7(7) . . ? N7 C25 H25 119.7 . . ? C26 C25 H25 119.7 . . ? C27 C26 C25 118.3(7) . . ? C27 C26 H26 120.9 . . ? C25 C26 H26 120.9 . . ? C26 C27 C28 121.7(8) . . ? C26 C27 H27 119.2 . . ? C28 C27 H27 119.2 . . ? C27 C28 C29 118.0(7) . . ? C27 C28 H28 121.0 . . ? C29 C28 H28 121.0 . . ? N7 C29 C28 122.3(7) . . ? N7 C29 C30 115.3(6) . . ? C28 C29 C30 122.3(6) . . ? O3 C30 N8 128.2(7) . . ? O3 C30 C29 120.3(6) . . ? N8 C30 C29 111.6(6) . . ? N9 C31 C32 121.7(6) . . ? N9 C31 N8 116.6(6) . . ? C32 C31 N8 121.7(6) . . ? C33 C32 C31 120.5(7) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C35 117.4(7) . . ? C32 C33 C34 121.9(7) . . ? C35 C33 C34 120.6(7) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C33 119.2(7) . . ? C36 C35 H35 120.4 . . ? C33 C35 H35 120.4 . . ? N9 C36 C35 124.1(7) . . ? N9 C36 H36 117.9 . . ? C35 C36 H36 117.9 . . ? N1' C1' C2' 122.1(10) . . ? N1' C1' H1' 118.9 . . ? C2' C1' H1' 118.9 . . ? C3' C2' C1' 120.2(11) . . ? C3' C2' H2' 119.9 . . ? C1' C2' H2' 119.9 . . ? C2' C3' C4' 117.4(11) . . ? C2' C3' H3' 121.3 . . ? C4' C3' H3' 121.3 . . ? C5' C4' C3' 119.3(9) . . ? C5' C4' H4' 120.4 . . ? C3' C4' H4' 120.4 . . ? N1' C5' C4' 122.2(8) . . ? N1' C5' C6' 115.7(8) . . ? C4' C5' C6' 122.1(8) . . ? O1' C6' N2' 127.3(9) . . ? O1' C6' C5' 121.5(8) . . ? N2' C6' C5' 111.1(7) . . ? N3' C7' N2' 117.6(7) . . ? N3' C7' C8' 120.0(8) . . ? N2' C7' C8' 122.2(8) . . ? C9' C8' C7' 119.1(10) . . ? C9' C8' H8' 120.4 . . ? C7' C8' H8' 120.4 . . ? C11' C9' C8' 119.9(10) . . ? C11' C9' C10' 119.9(10) . . ? C8' C9' C10' 120.1(10) . . ? C9' C10' H10D 109.5 . . ? C9' C10' H10E 109.5 . . ? H10D C10' H10E 109.5 . . ? C9' C10' H10F 109.5 . . ? H10D C10' H10F 109.5 . . ? H10E C10' H10F 109.5 . . ? C9' C11' C12' 119.7(9) . . ? C9' C11' H11' 120.1 . . ? C12' C11' H11' 120.1 . . ? N3' C12' C11' 120.3(8) . . ? N3' C12' H12' 119.8 . . ? C11' C12' H12' 119.8 . . ? N4' C13' C14' 118.3(14) . . ? N4' C13' H13' 120.8 . . ? C14' C13' H13' 120.8 . . ? C15' C14' C13' 121.8(13) . . ? C15' C14' H14' 119.1 . . ? C13' C14' H14' 119.1 . . ? C16' C15' C14' 117.0(17) . . ? C16' C15' H15' 121.5 . . ? C14' C15' H15' 121.5 . . ? C15' C16' C17' 120.3(15) . . ? C15' C16' H16' 119.8 . . ? C17' C16' H16' 119.8 . . ? C16' C17' N4' 121.8(11) . . ? C16' C17' C18' 125.4(12) . . ? N4' C17' C18' 112.8(9) . . ? O2' C18' N5' 125.5(8) . . ? O2' C18' C17' 120.4(10) . . ? N5' C18' C17' 114.2(8) . . ? N6' C19' C20' 122.1(7) . . ? N6' C19' N5' 116.1(7) . . ? C20' C19' N5' 121.8(7) . . ? C19' C20' C21' 119.2(7) . . ? C19' C20' H20' 120.4 . . ? C21' C20' H20' 120.4 . . ? C20' C21' C23' 119.2(7) . . ? C20' C21' C22' 121.0(7) . . ? C23' C21' C22' 119.7(7) . . ? C21' C22' H22D 109.5 . . ? C21' C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C21' C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C24' C23' C21' 118.1(7) . . ? C24' C23' H23' 121.0 . . ? C21' C23' H23' 121.0 . . ? N6' C24' C23' 123.9(7) . . ? N6' C24' H24' 118.0 . . ? C23' C24' H24' 118.0 . . ? N7' C25' C26' 116.2(11) . . ? N7' C25' H25' 121.9 . . ? C26' C25' H25' 121.9 . . ? C27' C26' C25' 124.4(10) . . ? C27' C26' H26' 117.8 . . ? C25' C26' H26' 117.8 . . ? C26' C27' C28' 118.8(9) . . ? C26' C27' H27' 120.6 . . ? C28' C27' H27' 120.6 . . ? C27' C28' C29' 116.1(10) . . ? C27' C28' H28' 121.9 . . ? C29' C28' H28' 121.9 . . ? N7' C29' C28' 123.0(9) . . ? N7' C29' C30' 117.8(7) . . ? C28' C29' C30' 119.2(9) . . ? O3' C30' N8' 127.3(8) . . ? O3' C30' C29' 124.6(8) . . ? N8' C30' C29' 108.1(8) . . ? N9' C31' C32' 120.7(7) . . ? N9' C31' N8' 116.0(7) . . ? C32' C31' N8' 123.0(7) . . ? C33' C32' C31' 120.7(8) . . ? C33' C32' H32' 119.6 . . ? C31' C32' H32' 119.6 . . ? C32' C33' C35' 117.3(8) . . ? C32' C33' C34' 121.6(8) . . ? C35' C33' C34' 121.0(8) . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C36' C35' C33' 119.5(8) . . ? C36' C35' H35' 120.2 . . ? C33' C35' H35' 120.2 . . ? N9' C36' C35' 122.5(7) . . ? N9' C36' H36' 118.7 . . ? C35' C36' H36' 118.7 . . ? C1S O1S H1S 109.5 . . ? C2S O2S H2S 109.5 . . ? O1S C1S H1S1 109.5 . . ? O1S C1S H1S2 109.5 . . ? H1S1 C1S H1S2 109.5 . . ? O1S C1S H1S3 109.5 . . ? H1S1 C1S H1S3 109.5 . . ? H1S2 C1S H1S3 109.5 . . ? O2S C2S H2S1 109.5 . . ? O2S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? O2S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 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 N7 Co1 N1 C1 8.3(6) . . . . ? N2 Co1 N1 C1 -176.8(6) . . . . ? N5 Co1 N1 C1 -116(3) . . . . ? N4 Co1 N1 C1 -88.8(6) . . . . ? N8 Co1 N1 C1 90.2(6) . . . . ? N7 Co1 N1 C5 -171.1(5) . . . . ? N2 Co1 N1 C5 3.8(5) . . . . ? N5 Co1 N1 C5 64(4) . . . . ? N4 Co1 N1 C5 91.8(5) . . . . ? N8 Co1 N1 C5 -89.2(5) . . . . ? N7 Co1 N2 C6 78(3) . . . . ? N1 Co1 N2 C6 -1.7(5) . . . . ? N5 Co1 N2 C6 -177.9(5) . . . . ? N4 Co1 N2 C6 -95.3(5) . . . . ? N8 Co1 N2 C6 85.0(5) . . . . ? N7 Co1 N2 C7 -123(3) . . . . ? N1 Co1 N2 C7 157.0(5) . . . . ? N5 Co1 N2 C7 -19.2(5) . . . . ? N4 Co1 N2 C7 63.4(5) . . . . ? N8 Co1 N2 C7 -116.3(5) . . . . ? N9 Co2 N3 C7 34.3(6) . . . . ? N6 Co2 N3 C7 -91.3(6) . . . . ? Br1 Co2 N3 C7 151.6(5) . . . . ? N9 Co2 N3 C12 -148.5(6) . . . . ? N6 Co2 N3 C12 85.9(6) . . . . ? Br1 Co2 N3 C12 -31.2(6) . . . . ? N7 Co1 N4 C13 -91.2(6) . . . . ? N1 Co1 N4 C13 4.9(6) . . . . ? N2 Co1 N4 C13 88.2(6) . . . . ? N5 Co1 N4 C13 -177.2(6) . . . . ? N8 Co1 N4 C13 -112(13) . . . . ? N7 Co1 N4 C17 98.4(5) . . . . ? N1 Co1 N4 C17 -165.5(5) . . . . ? N2 Co1 N4 C17 -82.2(5) . . . . ? N5 Co1 N4 C17 12.5(5) . . . . ? N8 Co1 N4 C17 78(13) . . . . ? N7 Co1 N5 C18 -106.8(5) . . . . ? N1 Co1 N5 C18 18(4) . . . . ? N2 Co1 N5 C18 78.1(5) . . . . ? N4 Co1 N5 C18 -9.7(5) . . . . ? N8 Co1 N5 C18 171.3(5) . . . . ? N7 Co1 N5 C19 60.2(6) . . . . ? N1 Co1 N5 C19 -175(3) . . . . ? N2 Co1 N5 C19 -114.8(6) . . . . ? N4 Co1 N5 C19 157.4(6) . . . . ? N8 Co1 N5 C19 -21.7(6) . . . . ? N9 Co2 N6 C19 -96.0(6) . . . . ? N3 Co2 N6 C19 29.0(6) . . . . ? Br1 Co2 N6 C19 145.0(5) . . . . ? N9 Co2 N6 C24 88.1(6) . . . . ? N3 Co2 N6 C24 -146.9(5) . . . . ? Br1 Co2 N6 C24 -30.9(6) . . . . ? N1 Co1 N7 C25 -98.9(6) . . . . ? N2 Co1 N7 C25 -178(69) . . . . ? N5 Co1 N7 C25 77.5(6) . . . . ? N4 Co1 N7 C25 -4.8(6) . . . . ? N8 Co1 N7 C25 174.8(6) . . . . ? N1 Co1 N7 C29 91.7(5) . . . . ? N2 Co1 N7 C29 12(3) . . . . ? N5 Co1 N7 C29 -91.9(5) . . . . ? N4 Co1 N7 C29 -174.2(5) . . . . ? N8 Co1 N7 C29 5.4(5) . . . . ? N7 Co1 N8 C30 0.3(5) . . . . ? N1 Co1 N8 C30 -95.9(5) . . . . ? N2 Co1 N8 C30 -179.1(5) . . . . ? N5 Co1 N8 C30 86.1(5) . . . . ? N4 Co1 N8 C30 21(13) . . . . ? N7 Co1 N8 C31 161.8(6) . . . . ? N1 Co1 N8 C31 65.7(6) . . . . ? N2 Co1 N8 C31 -17.6(6) . . . . ? N5 Co1 N8 C31 -112.3(6) . . . . ? N4 Co1 N8 C31 -178(100) . . . . ? N6 Co2 N9 C36 -145.3(5) . . . . ? N3 Co2 N9 C36 90.2(6) . . . . ? Br1 Co2 N9 C36 -26.2(6) . . . . ? N6 Co2 N9 C31 40.7(6) . . . . ? N3 Co2 N9 C31 -83.8(6) . . . . ? Br1 Co2 N9 C31 159.8(5) . . . . ? N5' Co1' N1' C5' 19(16) . . . . ? N2' Co1' N1' C5' 6.2(8) . . . . ? N8' Co1' N1' C5' -87.8(8) . . . . ? N4' Co1' N1' C5' 91.5(8) . . . . ? N7' Co1' N1' C5' -170.0(8) . . . . ? N5' Co1' N1' C1' -170(15) . . . . ? N2' Co1' N1' C1' 176.8(11) . . . . ? N8' Co1' N1' C1' 82.8(11) . . . . ? N4' Co1' N1' C1' -97.8(11) . . . . ? N7' Co1' N1' C1' 0.7(11) . . . . ? N5' Co1' N2' C6' -179.9(7) . . . . ? N8' Co1' N2' C6' 85.6(7) . . . . ? N4' Co1' N2' C6' -98.0(8) . . . . ? N7' Co1' N2' C6' 62(4) . . . . ? N1' Co1' N2' C6' -0.2(7) . . . . ? N5' Co1' N2' C7' -20.0(7) . . . . ? N8' Co1' N2' C7' -114.5(7) . . . . ? N4' Co1' N2' C7' 61.9(7) . . . . ? N7' Co1' N2' C7' -138(4) . . . . ? N1' Co1' N2' C7' 159.7(7) . . . . ? N6' Co2' N3' C7' -96.3(6) . . . . ? N9' Co2' N3' C7' 31.7(7) . . . . ? Br1' Co2' N3' C7' 144.8(6) . . . . ? N6' Co2' N3' C12' 84.3(6) . . . . ? N9' Co2' N3' C12' -147.7(6) . . . . ? Br1' Co2' N3' C12' -34.6(6) . . . . ? N5' Co1' N4' C13' 172.5(11) . . . . ? N2' Co1' N4' C13' 76.3(11) . . . . ? N8' Co1' N4' C13' 164(5) . . . . ? N7' Co1' N4' C13' -102.2(11) . . . . ? N1' Co1' N4' C13' -6.3(11) . . . . ? N5' Co1' N4' C17' 6.5(8) . . . . ? N2' Co1' N4' C17' -89.7(8) . . . . ? N8' Co1' N4' C17' -2(6) . . . . ? N7' Co1' N4' C17' 91.8(8) . . . . ? N1' Co1' N4' C17' -172.3(8) . . . . ? N2' Co1' N5' C18' 84.7(6) . . . . ? N8' Co1' N5' C18' 178.7(6) . . . . ? N4' Co1' N5' C18' -0.8(6) . . . . ? N7' Co1' N5' C18' -99.1(6) . . . . ? N1' Co1' N5' C18' 72(15) . . . . ? N2' Co1' N5' C19' -115.3(6) . . . . ? N8' Co1' N5' C19' -21.4(6) . . . . ? N4' Co1' N5' C19' 159.2(7) . . . . ? N7' Co1' N5' C19' 60.8(6) . . . . ? N1' Co1' N5' C19' -128(15) . . . . ? N9' Co2' N6' C24' 90.8(6) . . . . ? N3' Co2' N6' C24' -143.6(6) . . . . ? Br1' Co2' N6' C24' -23.8(6) . . . . ? N9' Co2' N6' C19' -87.8(6) . . . . ? N3' Co2' N6' C19' 37.8(6) . . . . ? Br1' Co2' N6' C19' 157.6(5) . . . . ? N5' Co1' N7' C29' -89.6(6) . . . . ? N2' Co1' N7' C29' 29(4) . . . . ? N8' Co1' N7' C29' 5.0(6) . . . . ? N4' Co1' N7' C29' -171.4(6) . . . . ? N1' Co1' N7' C29' 90.6(6) . . . . ? N5' Co1' N7' C25' 84.3(7) . . . . ? N2' Co1' N7' C25' -158(4) . . . . ? N8' Co1' N7' C25' 178.9(7) . . . . ? N4' Co1' N7' C25' 2.5(7) . . . . ? N1' Co1' N7' C25' -95.5(7) . . . . ? N5' Co1' N8' C30' 87.9(6) . . . . ? N2' Co1' N8' C30' -176.3(6) . . . . ? N4' Co1' N8' C30' 97(5) . . . . ? N7' Co1' N8' C30' 2.0(6) . . . . ? N1' Co1' N8' C30' -93.4(6) . . . . ? N5' Co1' N8' C31' -116.9(6) . . . . ? N2' Co1' N8' C31' -21.0(6) . . . . ? N4' Co1' N8' C31' -108(5) . . . . ? N7' Co1' N8' C31' 157.2(6) . . . . ? N1' Co1' N8' C31' 61.9(6) . . . . ? N6' Co2' N9' C36' -148.6(6) . . . . ? N3' Co2' N9' C36' 85.7(6) . . . . ? Br1' Co2' N9' C36' -31.2(6) . . . . ? N6' Co2' N9' C31' 32.7(7) . . . . ? N3' Co2' N9' C31' -93.0(6) . . . . ? Br1' Co2' N9' C31' 150.1(6) . . . . ? C5 N1 C1 C2 -0.8(10) . . . . ? Co1 N1 C1 C2 179.8(5) . . . . ? N1 C1 C2 C3 4.5(12) . . . . ? C1 C2 C3 C4 -2.5(13) . . . . ? C2 C3 C4 C5 -3.1(13) . . . . ? C3 C4 C5 N1 7.0(13) . . . . ? C3 C4 C5 C6 -173.7(8) . . . . ? C1 N1 C5 C4 -5.1(11) . . . . ? Co1 N1 C5 C4 174.3(7) . . . . ? C1 N1 C5 C6 175.5(6) . . . . ? Co1 N1 C5 C6 -5.1(8) . . . . ? C7 N2 C6 O1 18.1(11) . . . . ? Co1 N2 C6 O1 178.0(6) . . . . ? C7 N2 C6 C5 -160.4(6) . . . . ? Co1 N2 C6 C5 -0.5(8) . . . . ? C4 C5 C6 O1 5.7(12) . . . . ? N1 C5 C6 O1 -174.9(7) . . . . ? C4 C5 C6 N2 -175.7(7) . . . . ? N1 C5 C6 N2 3.7(9) . . . . ? C12 N3 C7 N2 -173.6(6) . . . . ? Co2 N3 C7 N2 3.6(9) . . . . ? C12 N3 C7 C8 2.5(11) . . . . ? Co2 N3 C7 C8 179.8(5) . . . . ? C6 N2 C7 N3 -128.5(7) . . . . ? Co1 N2 C7 N3 73.3(8) . . . . ? C6 N2 C7 C8 55.3(9) . . . . ? Co1 N2 C7 C8 -102.9(7) . . . . ? N3 C7 C8 C9 -4.7(11) . . . . ? N2 C7 C8 C9 171.4(7) . . . . ? C7 C8 C9 C11 4.0(11) . . . . ? C7 C8 C9 C10 -172.8(7) . . . . ? C8 C9 C11 C12 -1.4(12) . . . . ? C10 C9 C11 C12 175.4(7) . . . . ? C7 N3 C12 C11 0.2(12) . . . . ? Co2 N3 C12 C11 -177.0(6) . . . . ? C9 C11 C12 N3 -0.7(12) . . . . ? C17 N4 C13 C14 -0.4(11) . . . . ? Co1 N4 C13 C14 -170.2(6) . . . . ? N4 C13 C14 C15 2.6(13) . . . . ? C13 C14 C15 C16 -2.1(13) . . . . ? C14 C15 C16 C17 -0.5(13) . . . . ? C13 N4 C17 C16 -2.2(11) . . . . ? Co1 N4 C17 C16 169.0(6) . . . . ? C13 N4 C17 C18 175.8(6) . . . . ? Co1 N4 C17 C18 -13.1(8) . . . . ? C15 C16 C17 N4 2.6(12) . . . . ? C15 C16 C17 C18 -175.2(8) . . . . ? C19 N5 C18 O2 15.8(11) . . . . ? Co1 N5 C18 O2 -176.5(6) . . . . ? C19 N5 C18 C17 -162.6(6) . . . . ? Co1 N5 C18 C17 5.1(8) . . . . ? N4 C17 C18 O2 -173.2(6) . . . . ? C16 C17 C18 O2 4.7(11) . . . . ? N4 C17 C18 N5 5.4(9) . . . . ? C16 C17 C18 N5 -176.7(7) . . . . ? C24 N6 C19 N5 -177.0(6) . . . . ? Co2 N6 C19 N5 7.2(9) . . . . ? C24 N6 C19 C20 1.4(11) . . . . ? Co2 N6 C19 C20 -174.4(5) . . . . ? C18 N5 C19 N6 -122.1(8) . . . . ? Co1 N5 C19 N6 71.4(8) . . . . ? C18 N5 C19 C20 59.5(9) . . . . ? Co1 N5 C19 C20 -107.0(7) . . . . ? N6 C19 C20 C21 -1.2(11) . . . . ? N5 C19 C20 C21 177.2(6) . . . . ? C19 C20 C21 C23 -0.4(10) . . . . ? C19 C20 C21 C22 178.7(7) . . . . ? C20 C21 C23 C24 1.6(11) . . . . ? C22 C21 C23 C24 -177.5(7) . . . . ? C19 N6 C24 C23 0.0(11) . . . . ? Co2 N6 C24 C23 175.8(6) . . . . ? C21 C23 C24 N6 -1.5(12) . . . . ? C29 N7 C25 C26 -0.7(10) . . . . ? Co1 N7 C25 C26 -169.6(5) . . . . ? N7 C25 C26 C27 -1.9(11) . . . . ? C25 C26 C27 C28 3.2(12) . . . . ? C26 C27 C28 C29 -2.0(12) . . . . ? C25 N7 C29 C28 1.9(10) . . . . ? Co1 N7 C29 C28 172.3(6) . . . . ? C25 N7 C29 C30 -180.0(6) . . . . ? Co1 N7 C29 C30 -9.6(7) . . . . ? C27 C28 C29 N7 -0.7(11) . . . . ? C27 C28 C29 C30 -178.6(7) . . . . ? C31 N8 C30 O3 12.7(11) . . . . ? Co1 N8 C30 O3 175.4(6) . . . . ? C31 N8 C30 C29 -167.9(6) . . . . ? Co1 N8 C30 C29 -5.2(8) . . . . ? N7 C29 C30 O3 -170.7(6) . . . . ? C28 C29 C30 O3 7.4(11) . . . . ? N7 C29 C30 N8 9.8(9) . . . . ? C28 C29 C30 N8 -172.1(7) . . . . ? C36 N9 C31 C32 -1.8(10) . . . . ? Co2 N9 C31 C32 172.5(5) . . . . ? C36 N9 C31 N8 177.4(6) . . . . ? Co2 N9 C31 N8 -8.2(8) . . . . ? C30 N8 C31 N9 -117.4(7) . . . . ? Co1 N8 C31 N9 81.2(7) . . . . ? C30 N8 C31 C32 61.9(9) . . . . ? Co1 N8 C31 C32 -99.5(7) . . . . ? N9 C31 C32 C33 0.0(11) . . . . ? N8 C31 C32 C33 -179.2(6) . . . . ? C31 C32 C33 C35 1.2(10) . . . . ? C31 C32 C33 C34 -179.1(7) . . . . ? C32 C33 C35 C36 -0.7(11) . . . . ? C34 C33 C35 C36 179.7(7) . . . . ? C31 N9 C36 C35 2.5(11) . . . . ? Co2 N9 C36 C35 -171.7(6) . . . . ? C33 C35 C36 N9 -1.3(11) . . . . ? C5' N1' C1' C2' 1.5(19) . . . . ? Co1' N1' C1' C2' -168.8(9) . . . . ? N1' C1' C2' C3' -4(2) . . . . ? C1' C2' C3' C4' 5(2) . . . . ? C2' C3' C4' C5' -5(2) . . . . ? C1' N1' C5' C4' -1.3(17) . . . . ? Co1' N1' C5' C4' 170.2(9) . . . . ? C1' N1' C5' C6' 178.0(10) . . . . ? Co1' N1' C5' C6' -10.5(12) . . . . ? C3' C4' C5' N1' 3.1(19) . . . . ? C3' C4' C5' C6' -176.1(11) . . . . ? C7' N2' C6' O1' 18.5(17) . . . . ? Co1' N2' C6' O1' 179.7(10) . . . . ? C7' N2' C6' C5' -166.1(8) . . . . ? Co1' N2' C6' C5' -4.9(11) . . . . ? N1' C5' C6' O1' -174.1(11) . . . . ? C4' C5' C6' O1' 5.2(18) . . . . ? N1' C5' C6' N2' 10.2(13) . . . . ? C4' C5' C6' N2' -170.5(10) . . . . ? C12' N3' C7' N2' -174.2(8) . . . . ? Co2' N3' C7' N2' 6.4(10) . . . . ? C12' N3' C7' C8' 1.3(13) . . . . ? Co2' N3' C7' C8' -178.2(8) . . . . ? C6' N2' C7' N3' -128.9(9) . . . . ? Co1' N2' C7' N3' 71.6(10) . . . . ? C6' N2' C7' C8' 55.8(13) . . . . ? Co1' N2' C7' C8' -103.7(10) . . . . ? N3' C7' C8' C9' -1.2(17) . . . . ? N2' C7' C8' C9' 174.1(11) . . . . ? C7' C8' C9' C11' 0(2) . . . . ? C7' C8' C9' C10' -178.2(13) . . . . ? C8' C9' C11' C12' 0.5(19) . . . . ? C10' C9' C11' C12' 179.0(12) . . . . ? C7' N3' C12' C11' -0.5(13) . . . . ? Co2' N3' C12' C11' 179.0(7) . . . . ? C9' C11' C12' N3' -0.4(15) . . . . ? C17' N4' C13' C14' -1(2) . . . . ? Co1' N4' C13' C14' -166.0(15) . . . . ? N4' C13' C14' C15' 6(3) . . . . ? C13' C14' C15' C16' -12(4) . . . . ? C14' C15' C16' C17' 12(4) . . . . ? C15' C16' C17' N4' -8(3) . . . . ? C15' C16' C17' C18' 170.8(19) . . . . ? C13' N4' C17' C16' 2(2) . . . . ? Co1' N4' C17' C16' 168.3(12) . . . . ? C13' N4' C17' C18' -177.2(11) . . . . ? Co1' N4' C17' C18' -10.5(12) . . . . ? C19' N5' C18' O2' 15.6(13) . . . . ? Co1' N5' C18' O2' 177.1(7) . . . . ? C19' N5' C18' C17' -166.2(8) . . . . ? Co1' N5' C18' C17' -4.7(10) . . . . ? C16' C17' C18' O2' 9.5(19) . . . . ? N4' C17' C18' O2' -171.8(9) . . . . ? C16' C17' C18' N5' -168.9(14) . . . . ? N4' C17' C18' N5' 9.9(13) . . . . ? C24' N6' C19' C20' 0.2(11) . . . . ? Co2' N6' C19' C20' 178.8(6) . . . . ? C24' N6' C19' N5' 179.4(7) . . . . ? Co2' N6' C19' N5' -2.0(10) . . . . ? C18' N5' C19' N6' -122.8(8) . . . . ? Co1' N5' C19' N6' 77.6(8) . . . . ? C18' N5' C19' C20' 56.4(11) . . . . ? Co1' N5' C19' C20' -103.2(8) . . . . ? N6' C19' C20' C21' -1.3(12) . . . . ? N5' C19' C20' C21' 179.6(8) . . . . ? C19' C20' C21' C23' 0.0(12) . . . . ? C19' C20' C21' C22' -176.4(8) . . . . ? C20' C21' C23' C24' 2.3(12) . . . . ? C22' C21' C23' C24' 178.7(8) . . . . ? C19' N6' C24' C23' 2.3(11) . . . . ? Co2' N6' C24' C23' -176.3(6) . . . . ? C21' C23' C24' N6' -3.6(12) . . . . ? C29' N7' C25' C26' 1.7(12) . . . . ? Co1' N7' C25' C26' -171.7(6) . . . . ? N7' C25' C26' C27' 0.7(14) . . . . ? C25' C26' C27' C28' -1.4(15) . . . . ? C26' C27' C28' C29' -0.1(13) . . . . ? C25' N7' C29' C28' -3.3(12) . . . . ? Co1' N7' C29' C28' 170.8(6) . . . . ? C25' N7' C29' C30' 175.1(7) . . . . ? Co1' N7' C29' C30' -10.8(9) . . . . ? C27' C28' C29' N7' 2.4(12) . . . . ? C27' C28' C29' C30' -175.9(7) . . . . ? C31' N8' C30' O3' 15.3(12) . . . . ? Co1' N8' C30' O3' 172.9(7) . . . . ? C31' N8' C30' C29' -165.0(6) . . . . ? Co1' N8' C30' C29' -7.4(8) . . . . ? N7' C29' C30' O3' -168.4(8) . . . . ? C28' C29' C30' O3' 10.1(12) . . . . ? N7' C29' C30' N8' 11.9(10) . . . . ? C28' C29' C30' N8' -169.6(7) . . . . ? C36' N9' C31' C32' -0.1(12) . . . . ? Co2' N9' C31' C32' 178.6(6) . . . . ? C36' N9' C31' N8' -174.8(7) . . . . ? Co2' N9' C31' N8' 3.9(10) . . . . ? C30' N8' C31' N9' -128.8(7) . . . . ? Co1' N8' C31' N9' 75.5(8) . . . . ? C30' N8' C31' C32' 56.6(10) . . . . ? Co1' N8' C31' C32' -99.1(8) . . . . ? N9' C31' C32' C33' -2.3(12) . . . . ? N8' C31' C32' C33' 172.1(7) . . . . ? C31' C32' C33' C35' 3.0(12) . . . . ? C31' C32' C33' C34' -175.1(8) . . . . ? C32' C33' C35' C36' -1.5(12) . . . . ? C34' C33' C35' C36' 176.7(8) . . . . ? C31' N9' C36' C35' 1.7(12) . . . . ? Co2' N9' C36' C35' -177.0(6) . . . . ? C33' C35' C36' N9' -0.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.953 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.953 _refine_diff_density_max 2.580 _refine_diff_density_min -2.168 _refine_diff_density_rms 0.193 #===END data_dec19sq _database_code_depnum_ccdc_archive 'CCDC 698531' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C37 H44 Cl2 Co N9 O9 Zn' _chemical_formula_sum 'C37 H44 Cl2 Co N9 O9 Zn' _chemical_formula_weight 954.02 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' 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' Zn Zn 0.2839 1.4301 '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 11.555(5) _cell_length_b 12.482(5) _cell_length_c 16.117(5) _cell_angle_alpha 78.089(5) _cell_angle_beta 72.040(5) _cell_angle_gamma 86.649(5) _cell_volume 2163.6(14) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.29 _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.46 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 984 _exptl_absorpt_coefficient_mu 1.123 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9031 _exptl_absorpt_correction_T_max 0.9795 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10253 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1641 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.35 _diffrn_reflns_theta_max 28.29 _reflns_number_total 10253 _reflns_number_gt 4663 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT PLUS' _computing_structure_solution 'SIR97(Altomare, et. al. 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1510P)^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_extinction_coef ? _refine_ls_number_reflns 10253 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1527 _refine_ls_R_factor_gt 0.0872 _refine_ls_wR_factor_ref 0.2691 _refine_ls_wR_factor_gt 0.2244 _refine_ls_goodness_of_fit_ref 0.887 _refine_ls_restrained_S_all 0.887 _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 Zn1 Zn 0.17311(7) 0.03200(6) 0.10638(5) 0.0371(2) Uani 1 1 d . . . Co1 Co 0.21572(8) 0.25288(7) 0.20820(6) 0.0342(3) Uani 1 1 d . . . Cl1 Cl 0.15829(12) -0.10308(11) 0.03292(11) 0.0272(3) Uani 1 1 d . . . O1 O 0.1902(5) -0.0215(4) 0.3928(3) 0.0518(13) Uani 1 1 d . . . O2 O -0.0906(4) 0.3200(4) 0.1418(3) 0.0433(12) Uani 1 1 d . . . O3 O 0.5124(4) 0.2583(4) -0.0033(3) 0.0452(12) Uani 1 1 d . . . N1 N 0.1244(5) 0.2575(5) 0.3299(4) 0.0399(14) Uani 1 1 d . . . N2 N 0.2378(5) 0.1012(5) 0.2589(4) 0.0367(13) Uani 1 1 d . . . N3 N 0.3204(5) -0.0029(4) 0.1499(4) 0.0348(13) Uani 1 1 d . . . N4 N 0.3732(5) 0.2800(5) 0.2209(4) 0.0370(13) Uani 1 1 d . . . N5 N 0.3130(5) 0.2420(4) 0.0885(4) 0.0344(13) Uani 1 1 d . . . N6 N 0.1977(5) 0.1736(5) 0.0156(4) 0.0372(13) Uani 1 1 d . . . N7 N 0.1854(5) 0.4026(5) 0.1588(4) 0.0399(14) Uani 1 1 d . . . N8 N 0.0589(4) 0.2273(5) 0.1910(4) 0.0337(12) Uani 1 1 d . . . N9 N 0.0227(5) 0.0376(5) 0.2094(4) 0.0373(13) Uani 1 1 d . . . C1 C 0.0655(7) 0.3446(6) 0.3619(5) 0.0479(19) Uani 1 1 d . . . H1 H 0.0691 0.4132 0.3224 0.057 Uiso 1 1 calc R . . C2 C 0.0015(8) 0.3354(8) 0.4493(6) 0.060(2) Uani 1 1 d . . . H2 H -0.0377 0.3980 0.4701 0.072 Uiso 1 1 calc R . . C3 C -0.0077(8) 0.2379(7) 0.5078(5) 0.061(2) Uani 1 1 d . . . H3 H -0.0542 0.2308 0.5686 0.073 Uiso 1 1 calc R . . C4 C 0.0545(6) 0.1485(6) 0.4743(5) 0.0434(17) Uani 1 1 d . . . H4 H 0.0524 0.0794 0.5129 0.052 Uiso 1 1 calc R . . C5 C 0.1163(6) 0.1605(6) 0.3885(4) 0.0346(15) Uani 1 1 d . . . C6 C 0.1835(6) 0.0704(6) 0.3474(5) 0.0399(16) Uani 1 1 d . . . C7 C 0.3301(6) 0.0338(5) 0.2184(5) 0.0338(15) Uani 1 1 d . . . C8 C 0.4338(6) 0.0150(6) 0.2471(5) 0.0405(17) Uani 1 1 d . . . H8 H 0.4389 0.0426 0.2966 0.049 Uiso 1 1 calc R . . C9 C 0.5292(7) -0.0452(8) 0.2017(6) 0.058(2) Uani 1 1 d . . . C10 C 0.6416(8) -0.0614(9) 0.2288(7) 0.078(3) Uani 1 1 d . . . H10A H 0.6584 -0.1399 0.2423 0.117 Uiso 1 1 calc R . . H10B H 0.6306 -0.0303 0.2818 0.117 Uiso 1 1 calc R . . H10C H 0.7101 -0.0248 0.1802 0.117 Uiso 1 1 calc R . . C11 C 0.5134(7) -0.0884(7) 0.1321(6) 0.053(2) Uani 1 1 d . . . H11 H 0.5756 -0.1315 0.1010 0.063 Uiso 1 1 calc R . . C12 C 0.4096(7) -0.0685(6) 0.1094(5) 0.0456(18) Uani 1 1 d . . . H12 H 0.3985 -0.1010 0.0641 0.055 Uiso 1 1 calc R . . C13 C 0.3960(7) 0.2928(6) 0.2941(5) 0.0434(18) Uani 1 1 d . . . H13 H 0.3294 0.3006 0.3446 0.052 Uiso 1 1 calc R . . C14 C 0.5128(7) 0.2952(6) 0.3000(6) 0.051(2) Uani 1 1 d . . . H14 H 0.5264 0.3073 0.3525 0.062 Uiso 1 1 calc R . . C15 C 0.6092(7) 0.2796(6) 0.2272(5) 0.0467(19) Uani 1 1 d . . . H15 H 0.6900 0.2771 0.2307 0.056 Uiso 1 1 calc R . . C16 C 0.5883(6) 0.2677(6) 0.1484(5) 0.0458(18) Uani 1 1 d . . . H16 H 0.6536 0.2596 0.0972 0.055 Uiso 1 1 calc R . . C17 C 0.4681(6) 0.2680(5) 0.1484(5) 0.0369(16) Uani 1 1 d . . . C18 C 0.4338(6) 0.2570(5) 0.0691(5) 0.0366(16) Uani 1 1 d . . . C19 C 0.2664(6) 0.2537(5) 0.0162(4) 0.0341(15) Uani 1 1 d . . . C20 C 0.2912(7) 0.3439(6) -0.0515(5) 0.0450(18) Uani 1 1 d . . . H20 H 0.3427 0.3999 -0.0503 0.054 Uiso 1 1 calc R . . C21 C 0.2428(7) 0.3554(6) -0.1218(5) 0.0423(17) Uani 1 1 d . . . C22 C 0.2689(8) 0.4537(7) -0.1977(6) 0.061(2) Uani 1 1 d . . . H22A H 0.2430 0.4379 -0.2464 0.092 Uiso 1 1 calc R . . H22B H 0.3563 0.4697 -0.2190 0.092 Uiso 1 1 calc R . . H22C H 0.2242 0.5171 -0.1770 0.092 Uiso 1 1 calc R . . C23 C 0.1629(6) 0.2708(6) -0.1199(5) 0.0427(17) Uani 1 1 d . . . H23 H 0.1256 0.2755 -0.1655 0.051 Uiso 1 1 calc R . . C24 C 0.1419(6) 0.1825(6) -0.0501(5) 0.0386(16) Uani 1 1 d . . . H24 H 0.0878 0.1263 -0.0470 0.046 Uiso 1 1 calc R . . C25 C 0.2607(7) 0.4892(6) 0.1384(5) 0.0437(18) Uani 1 1 d . . . H25 H 0.3325 0.4809 0.1560 0.052 Uiso 1 1 calc R . . C26 C 0.2359(7) 0.5891(7) 0.0928(6) 0.053(2) Uani 1 1 d . . . H26 H 0.2896 0.6492 0.0800 0.063 Uiso 1 1 calc R . . C27 C 0.1354(7) 0.6017(6) 0.0662(6) 0.051(2) Uani 1 1 d . . . H27 H 0.1200 0.6697 0.0323 0.061 Uiso 1 1 calc R . . C28 C 0.0556(7) 0.5161(7) 0.0881(5) 0.053(2) Uani 1 1 d . . . H28 H -0.0184 0.5257 0.0735 0.063 Uiso 1 1 calc R . . C29 C 0.0843(6) 0.4156(6) 0.1320(5) 0.0401(17) Uani 1 1 d . . . C30 C 0.0082(6) 0.3147(6) 0.1557(4) 0.0355(15) Uani 1 1 d . . . C31 C -0.0149(6) 0.1329(6) 0.2377(5) 0.0399(17) Uani 1 1 d . . . C32 C -0.1146(6) 0.1374(6) 0.3068(5) 0.0452(18) Uani 1 1 d . . . H32 H -0.1372 0.2052 0.3252 0.054 Uiso 1 1 calc R . . C33 C -0.1861(7) 0.0438(8) 0.3525(5) 0.053(2) Uani 1 1 d . . . C34 C -0.2958(8) 0.0467(9) 0.4291(6) 0.074(3) Uani 1 1 d . . . H34A H -0.3465 -0.0179 0.4392 0.111 Uiso 1 1 calc R . . H34B H -0.3422 0.1131 0.4166 0.111 Uiso 1 1 calc R . . H34C H -0.2717 0.0466 0.4823 0.111 Uiso 1 1 calc R . . C35 C -0.1433(7) -0.0547(7) 0.3255(5) 0.053(2) Uani 1 1 d . . . H35 H -0.1847 -0.1218 0.3555 0.063 Uiso 1 1 calc R . . C36 C -0.0393(6) -0.0515(6) 0.2539(5) 0.0446(18) Uani 1 1 d . . . H36 H -0.0108 -0.1185 0.2358 0.053 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 0.0313(4) 0.0330(5) 0.0496(5) -0.0038(4) -0.0181(4) -0.0033(3) Co1 0.0268(5) 0.0349(5) 0.0407(5) -0.0047(4) -0.0112(4) -0.0020(4) Cl1 0.0214(7) 0.0181(7) 0.0516(9) -0.0093(6) -0.0230(7) -0.0011(5) O1 0.062(4) 0.039(3) 0.052(3) 0.002(3) -0.021(3) 0.003(3) O2 0.035(3) 0.047(3) 0.052(3) -0.003(2) -0.025(2) 0.004(2) O3 0.032(3) 0.047(3) 0.051(3) -0.008(2) -0.005(2) -0.010(2) N1 0.031(3) 0.045(4) 0.041(3) -0.003(3) -0.010(3) -0.001(3) N2 0.033(3) 0.047(3) 0.035(3) -0.003(3) -0.018(3) -0.008(3) N3 0.028(3) 0.035(3) 0.048(3) -0.015(3) -0.016(3) 0.001(2) N4 0.026(3) 0.045(3) 0.040(3) -0.004(3) -0.012(2) -0.005(2) N5 0.022(3) 0.035(3) 0.044(3) -0.002(3) -0.009(2) -0.007(2) N6 0.037(3) 0.038(3) 0.041(3) -0.009(3) -0.018(3) 0.002(3) N7 0.033(3) 0.041(3) 0.048(4) -0.011(3) -0.015(3) -0.001(3) N8 0.020(3) 0.038(3) 0.043(3) -0.005(3) -0.012(2) 0.004(2) N9 0.027(3) 0.040(3) 0.046(3) -0.002(3) -0.016(3) -0.003(2) C1 0.055(5) 0.042(4) 0.046(4) -0.011(4) -0.016(4) 0.014(4) C2 0.065(6) 0.062(6) 0.060(6) -0.036(5) -0.012(4) 0.006(4) C3 0.077(6) 0.059(6) 0.040(5) -0.015(4) -0.002(4) -0.007(5) C4 0.038(4) 0.051(5) 0.041(4) 0.000(3) -0.016(3) -0.009(3) C5 0.023(3) 0.045(4) 0.034(4) -0.003(3) -0.007(3) -0.008(3) C6 0.038(4) 0.031(4) 0.045(4) 0.001(3) -0.009(3) -0.007(3) C7 0.026(3) 0.035(4) 0.043(4) -0.006(3) -0.015(3) -0.002(3) C8 0.035(4) 0.048(4) 0.046(4) -0.016(3) -0.021(3) 0.004(3) C9 0.044(5) 0.079(6) 0.060(5) -0.022(5) -0.027(4) 0.020(4) C10 0.055(6) 0.117(9) 0.097(7) -0.057(7) -0.053(5) 0.031(5) C11 0.032(4) 0.069(6) 0.068(5) -0.031(5) -0.023(4) 0.021(4) C12 0.041(4) 0.043(4) 0.063(5) -0.016(4) -0.030(4) 0.014(3) C13 0.055(5) 0.038(4) 0.046(4) -0.011(3) -0.025(4) -0.006(3) C14 0.052(5) 0.049(5) 0.065(5) -0.005(4) -0.038(4) -0.008(4) C15 0.031(4) 0.050(5) 0.064(5) -0.002(4) -0.026(4) -0.010(3) C16 0.022(3) 0.055(5) 0.061(5) -0.007(4) -0.015(3) -0.005(3) C17 0.031(4) 0.028(3) 0.053(4) -0.011(3) -0.014(3) 0.004(3) C18 0.029(4) 0.028(3) 0.052(4) -0.001(3) -0.014(3) -0.003(3) C19 0.035(4) 0.030(4) 0.033(4) -0.004(3) -0.005(3) -0.010(3) C20 0.042(4) 0.049(5) 0.043(4) -0.012(4) -0.010(3) 0.001(3) C21 0.041(4) 0.035(4) 0.049(4) -0.005(3) -0.013(3) -0.003(3) C22 0.064(6) 0.051(5) 0.064(5) 0.006(4) -0.022(5) -0.007(4) C23 0.032(4) 0.050(5) 0.050(4) -0.014(4) -0.016(3) 0.006(3) C24 0.029(4) 0.047(4) 0.044(4) -0.003(3) -0.020(3) -0.005(3) C25 0.045(4) 0.030(4) 0.055(5) -0.003(3) -0.015(4) -0.011(3) C26 0.039(4) 0.045(5) 0.066(5) 0.005(4) -0.014(4) -0.009(3) C27 0.048(5) 0.031(4) 0.069(5) 0.004(4) -0.018(4) -0.004(3) C28 0.044(5) 0.055(5) 0.051(5) 0.003(4) -0.013(4) 0.002(4) C29 0.029(4) 0.049(4) 0.038(4) -0.001(3) -0.011(3) 0.010(3) C30 0.025(3) 0.044(4) 0.036(4) -0.014(3) -0.005(3) 0.006(3) C31 0.020(3) 0.053(5) 0.040(4) 0.005(3) -0.009(3) 0.002(3) C32 0.032(4) 0.050(5) 0.045(4) 0.015(4) -0.015(3) 0.001(3) C33 0.030(4) 0.076(6) 0.050(5) 0.009(4) -0.019(4) -0.004(4) C34 0.043(5) 0.115(9) 0.050(5) 0.018(5) -0.015(4) -0.016(5) C35 0.037(4) 0.065(6) 0.053(5) 0.025(4) -0.027(4) -0.025(4) C36 0.031(4) 0.047(4) 0.056(5) 0.010(4) -0.025(3) -0.011(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 Zn1 N9 2.009(6) . ? Zn1 N6 2.020(6) . ? Zn1 N3 2.025(5) . ? Zn1 Cl1 2.2928(17) . ? Co1 N7 1.931(6) . ? Co1 N1 1.931(6) . ? Co1 N2 1.937(6) . ? Co1 N5 1.938(6) . ? Co1 N4 1.948(5) . ? Co1 N8 1.968(5) . ? O1 C6 1.239(8) . ? O2 C30 1.224(8) . ? O3 C18 1.236(8) . ? N1 C1 1.355(9) . ? N1 C5 1.361(9) . ? N2 C6 1.351(9) . ? N2 C7 1.401(9) . ? N3 C7 1.316(8) . ? N3 C12 1.365(9) . ? N4 C13 1.327(8) . ? N4 C17 1.362(8) . ? N5 C18 1.348(8) . ? N5 C19 1.405(8) . ? N6 C19 1.316(8) . ? N6 C24 1.384(8) . ? N7 C25 1.350(8) . ? N7 C29 1.356(8) . ? N8 C30 1.316(8) . ? N8 C31 1.427(8) . ? N9 C36 1.309(8) . ? N9 C31 1.361(9) . ? C1 C2 1.359(11) . ? C1 H1 0.9500 . ? C2 C3 1.364(12) . ? C2 H2 0.9500 . ? C3 C4 1.403(11) . ? C3 H3 0.9500 . ? C4 C5 1.327(9) . ? C4 H4 0.9500 . ? C5 C6 1.481(10) . ? C7 C8 1.404(9) . ? C8 C9 1.396(10) . ? C8 H8 0.9500 . ? C9 C11 1.402(11) . ? C9 C10 1.484(11) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.354(10) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C14 1.384(10) . ? C13 H13 0.9500 . ? C14 C15 1.385(11) . ? C14 H14 0.9500 . ? C15 C16 1.401(10) . ? C15 H15 0.9500 . ? C16 C17 1.389(9) . ? C16 H16 0.9500 . ? C17 C18 1.484(10) . ? C19 C20 1.371(10) . ? C20 C21 1.391(10) . ? C20 H20 0.9500 . ? C21 C23 1.432(9) . ? C21 C22 1.513(10) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.374(10) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.373(10) . ? C25 H25 0.9500 . ? C26 C27 1.347(11) . ? C26 H26 0.9500 . ? C27 C28 1.369(10) . ? C27 H27 0.9500 . ? C28 C29 1.383(10) . ? C28 H28 0.9500 . ? C29 C30 1.493(10) . ? C31 C32 1.340(9) . ? C32 C33 1.405(11) . ? C32 H32 0.9500 . ? C33 C35 1.402(12) . ? C33 C34 1.476(11) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.382(11) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? 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 N9 Zn1 N6 111.1(2) . . ? N9 Zn1 N3 110.4(2) . . ? N6 Zn1 N3 111.0(2) . . ? N9 Zn1 Cl1 111.18(17) . . ? N6 Zn1 Cl1 106.18(16) . . ? N3 Zn1 Cl1 106.85(15) . . ? N7 Co1 N1 96.3(2) . . ? N7 Co1 N2 177.2(2) . . ? N1 Co1 N2 82.7(2) . . ? N7 Co1 N5 86.5(2) . . ? N1 Co1 N5 176.8(2) . . ? N2 Co1 N5 94.6(2) . . ? N7 Co1 N4 96.4(2) . . ? N1 Co1 N4 95.2(2) . . ? N2 Co1 N4 86.3(2) . . ? N5 Co1 N4 83.0(2) . . ? N7 Co1 N8 82.6(2) . . ? N1 Co1 N8 86.6(2) . . ? N2 Co1 N8 94.7(2) . . ? N5 Co1 N8 95.3(2) . . ? N4 Co1 N8 178.1(2) . . ? C1 N1 C5 117.6(6) . . ? C1 N1 Co1 127.3(5) . . ? C5 N1 Co1 115.0(5) . . ? C6 N2 C7 117.4(6) . . ? C6 N2 Co1 115.5(5) . . ? C7 N2 Co1 124.3(4) . . ? C7 N3 C12 119.2(6) . . ? C7 N3 Zn1 121.1(4) . . ? C12 N3 Zn1 119.6(4) . . ? C13 N4 C17 119.0(6) . . ? C13 N4 Co1 127.3(5) . . ? C17 N4 Co1 113.0(4) . . ? C18 N5 C19 116.9(6) . . ? C18 N5 Co1 116.0(5) . . ? C19 N5 Co1 124.1(4) . . ? C19 N6 C24 120.5(6) . . ? C19 N6 Zn1 122.3(5) . . ? C24 N6 Zn1 117.2(4) . . ? C25 N7 C29 118.4(6) . . ? C25 N7 Co1 127.0(5) . . ? C29 N7 Co1 114.0(5) . . ? C30 N8 C31 118.8(5) . . ? C30 N8 Co1 115.4(4) . . ? C31 N8 Co1 122.8(4) . . ? C36 N9 C31 117.9(6) . . ? C36 N9 Zn1 120.8(5) . . ? C31 N9 Zn1 121.3(4) . . ? N1 C1 C2 121.1(7) . . ? N1 C1 H1 119.5 . . ? C2 C1 H1 119.5 . . ? C1 C2 C3 121.3(8) . . ? C1 C2 H2 119.3 . . ? C3 C2 H2 119.3 . . ? C2 C3 C4 117.1(7) . . ? C2 C3 H3 121.4 . . ? C4 C3 H3 121.4 . . ? C5 C4 C3 119.9(7) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 N1 123.0(7) . . ? C4 C5 C6 123.4(7) . . ? N1 C5 C6 113.6(6) . . ? O1 C6 N2 125.5(7) . . ? O1 C6 C5 121.4(7) . . ? N2 C6 C5 113.1(6) . . ? N3 C7 N2 118.4(6) . . ? N3 C7 C8 122.1(6) . . ? N2 C7 C8 119.2(6) . . ? C9 C8 C7 118.7(6) . . ? C9 C8 H8 120.7 . . ? C7 C8 H8 120.7 . . ? C8 C9 C11 117.8(7) . . ? C8 C9 C10 119.2(7) . . ? C11 C9 C10 122.9(7) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 120.0(7) . . ? C12 C11 H11 120.0 . . ? C9 C11 H11 120.0 . . ? C11 C12 N3 121.9(7) . . ? C11 C12 H12 119.1 . . ? N3 C12 H12 119.1 . . ? N4 C13 C14 122.8(7) . . ? N4 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C13 C14 C15 118.2(7) . . ? C13 C14 H14 120.9 . . ? C15 C14 H14 120.9 . . ? C14 C15 C16 120.3(6) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 117.3(7) . . ? C17 C16 H16 121.4 . . ? C15 C16 H16 121.4 . . ? N4 C17 C16 122.3(6) . . ? N4 C17 C18 115.1(6) . . ? C16 C17 C18 122.6(6) . . ? O3 C18 N5 127.4(6) . . ? O3 C18 C17 120.7(6) . . ? N5 C18 C17 111.9(6) . . ? N6 C19 C20 120.7(6) . . ? N6 C19 N5 117.2(6) . . ? C20 C19 N5 122.0(6) . . ? C19 C20 C21 121.5(7) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C23 117.6(7) . . ? C20 C21 C22 122.8(7) . . ? C23 C21 C22 119.6(7) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C21 118.0(7) . . ? C24 C23 H23 121.0 . . ? C21 C23 H23 121.0 . . ? C23 C24 N6 121.5(6) . . ? C23 C24 H24 119.2 . . ? N6 C24 H24 119.2 . . ? N7 C25 C26 121.5(7) . . ? N7 C25 H25 119.3 . . ? C26 C25 H25 119.3 . . ? C27 C26 C25 120.0(7) . . ? C27 C26 H26 120.0 . . ? C25 C26 H26 120.0 . . ? C26 C27 C28 119.8(7) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C27 C28 C29 119.0(7) . . ? C27 C28 H28 120.5 . . ? C29 C28 H28 120.5 . . ? N7 C29 C28 121.2(7) . . ? N7 C29 C30 114.5(6) . . ? C28 C29 C30 124.3(6) . . ? O2 C30 N8 127.3(6) . . ? O2 C30 C29 119.7(6) . . ? N8 C30 C29 113.0(6) . . ? C32 C31 N9 121.7(7) . . ? C32 C31 N8 121.8(7) . . ? N9 C31 N8 116.4(6) . . ? C31 C32 C33 121.3(8) . . ? C31 C32 H32 119.3 . . ? C33 C32 H32 119.3 . . ? C35 C33 C32 116.3(7) . . ? C35 C33 C34 121.3(8) . . ? C32 C33 C34 122.2(9) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C33 118.2(7) . . ? C36 C35 H35 120.9 . . ? C33 C35 H35 120.9 . . ? N9 C36 C35 124.4(8) . . ? N9 C36 H36 117.8 . . ? C35 C36 H36 117.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N7 Co1 N1 C1 -1.9(6) . . . . ? N2 Co1 N1 C1 -179.2(6) . . . . ? N5 Co1 N1 C1 150(4) . . . . ? N4 Co1 N1 C1 95.2(6) . . . . ? N8 Co1 N1 C1 -84.0(6) . . . . ? N7 Co1 N1 C5 175.9(5) . . . . ? N2 Co1 N1 C5 -1.5(4) . . . . ? N5 Co1 N1 C5 -32(4) . . . . ? N4 Co1 N1 C5 -87.1(5) . . . . ? N8 Co1 N1 C5 93.7(5) . . . . ? N7 Co1 N2 C6 -68(5) . . . . ? N1 Co1 N2 C6 0.7(5) . . . . ? N5 Co1 N2 C6 179.1(5) . . . . ? N4 Co1 N2 C6 96.4(5) . . . . ? N8 Co1 N2 C6 -85.3(5) . . . . ? N7 Co1 N2 C7 131(5) . . . . ? N1 Co1 N2 C7 -160.1(5) . . . . ? N5 Co1 N2 C7 18.2(5) . . . . ? N4 Co1 N2 C7 -64.4(5) . . . . ? N8 Co1 N2 C7 113.9(5) . . . . ? N9 Zn1 N3 C7 -35.0(6) . . . . ? N6 Zn1 N3 C7 88.7(5) . . . . ? Cl1 Zn1 N3 C7 -156.0(5) . . . . ? N9 Zn1 N3 C12 143.0(5) . . . . ? N6 Zn1 N3 C12 -93.3(6) . . . . ? Cl1 Zn1 N3 C12 22.0(6) . . . . ? N7 Co1 N4 C13 98.5(6) . . . . ? N1 Co1 N4 C13 1.6(6) . . . . ? N2 Co1 N4 C13 -80.8(6) . . . . ? N5 Co1 N4 C13 -175.8(6) . . . . ? N8 Co1 N4 C13 158(7) . . . . ? N7 Co1 N4 C17 -91.5(5) . . . . ? N1 Co1 N4 C17 171.5(5) . . . . ? N2 Co1 N4 C17 89.2(5) . . . . ? N5 Co1 N4 C17 -5.8(5) . . . . ? N8 Co1 N4 C17 -32(7) . . . . ? N7 Co1 N5 C18 96.7(5) . . . . ? N1 Co1 N5 C18 -55(4) . . . . ? N2 Co1 N5 C18 -85.9(5) . . . . ? N4 Co1 N5 C18 -0.3(5) . . . . ? N8 Co1 N5 C18 178.9(5) . . . . ? N7 Co1 N5 C19 -63.0(5) . . . . ? N1 Co1 N5 C19 145(4) . . . . ? N2 Co1 N5 C19 114.4(5) . . . . ? N4 Co1 N5 C19 -159.9(5) . . . . ? N8 Co1 N5 C19 19.3(5) . . . . ? N9 Zn1 N6 C19 93.8(6) . . . . ? N3 Zn1 N6 C19 -29.5(6) . . . . ? Cl1 Zn1 N6 C19 -145.2(5) . . . . ? N9 Zn1 N6 C24 -88.2(5) . . . . ? N3 Zn1 N6 C24 148.6(5) . . . . ? Cl1 Zn1 N6 C24 32.9(5) . . . . ? N1 Co1 N7 C25 99.0(6) . . . . ? N2 Co1 N7 C25 168(5) . . . . ? N5 Co1 N7 C25 -79.5(6) . . . . ? N4 Co1 N7 C25 3.1(6) . . . . ? N8 Co1 N7 C25 -175.2(6) . . . . ? N1 Co1 N7 C29 -90.2(5) . . . . ? N2 Co1 N7 C29 -22(5) . . . . ? N5 Co1 N7 C29 91.3(5) . . . . ? N4 Co1 N7 C29 173.8(5) . . . . ? N8 Co1 N7 C29 -4.5(5) . . . . ? N7 Co1 N8 C30 0.9(5) . . . . ? N1 Co1 N8 C30 97.6(5) . . . . ? N2 Co1 N8 C30 -180.0(5) . . . . ? N5 Co1 N8 C30 -84.9(5) . . . . ? N4 Co1 N8 C30 -59(7) . . . . ? N7 Co1 N8 C31 -159.5(5) . . . . ? N1 Co1 N8 C31 -62.7(5) . . . . ? N2 Co1 N8 C31 19.7(5) . . . . ? N5 Co1 N8 C31 114.7(5) . . . . ? N4 Co1 N8 C31 140(7) . . . . ? N6 Zn1 N9 C36 150.3(5) . . . . ? N3 Zn1 N9 C36 -86.1(5) . . . . ? Cl1 Zn1 N9 C36 32.3(5) . . . . ? N6 Zn1 N9 C31 -32.7(6) . . . . ? N3 Zn1 N9 C31 90.9(5) . . . . ? Cl1 Zn1 N9 C31 -150.7(4) . . . . ? C5 N1 C1 C2 0.4(11) . . . . ? Co1 N1 C1 C2 178.1(6) . . . . ? N1 C1 C2 C3 -1.1(13) . . . . ? C1 C2 C3 C4 1.7(13) . . . . ? C2 C3 C4 C5 -1.6(12) . . . . ? C3 C4 C5 N1 1.0(11) . . . . ? C3 C4 C5 C6 -179.4(7) . . . . ? C1 N1 C5 C4 -0.4(10) . . . . ? Co1 N1 C5 C4 -178.3(5) . . . . ? C1 N1 C5 C6 180.0(6) . . . . ? Co1 N1 C5 C6 2.0(7) . . . . ? C7 N2 C6 O1 -15.1(10) . . . . ? Co1 N2 C6 O1 -177.3(6) . . . . ? C7 N2 C6 C5 162.4(5) . . . . ? Co1 N2 C6 C5 0.2(7) . . . . ? C4 C5 C6 O1 -3.5(10) . . . . ? N1 C5 C6 O1 176.2(6) . . . . ? C4 C5 C6 N2 178.9(6) . . . . ? N1 C5 C6 N2 -1.5(8) . . . . ? C12 N3 C7 N2 179.8(6) . . . . ? Zn1 N3 C7 N2 -2.1(8) . . . . ? C12 N3 C7 C8 5.0(10) . . . . ? Zn1 N3 C7 C8 -177.0(5) . . . . ? C6 N2 C7 N3 125.2(7) . . . . ? Co1 N2 C7 N3 -74.3(7) . . . . ? C6 N2 C7 C8 -59.8(8) . . . . ? Co1 N2 C7 C8 100.7(7) . . . . ? N3 C7 C8 C9 -0.3(11) . . . . ? N2 C7 C8 C9 -175.1(7) . . . . ? C7 C8 C9 C11 -3.1(12) . . . . ? C7 C8 C9 C10 177.2(8) . . . . ? C8 C9 C11 C12 1.9(13) . . . . ? C10 C9 C11 C12 -178.5(9) . . . . ? C9 C11 C12 N3 2.9(13) . . . . ? C7 N3 C12 C11 -6.4(11) . . . . ? Zn1 N3 C12 C11 175.6(6) . . . . ? C17 N4 C13 C14 0.5(10) . . . . ? Co1 N4 C13 C14 169.9(6) . . . . ? N4 C13 C14 C15 -2.4(11) . . . . ? C13 C14 C15 C16 3.3(11) . . . . ? C14 C15 C16 C17 -2.3(11) . . . . ? C13 N4 C17 C16 0.6(10) . . . . ? Co1 N4 C17 C16 -170.3(5) . . . . ? C13 N4 C17 C18 -178.6(6) . . . . ? Co1 N4 C17 C18 10.5(7) . . . . ? C15 C16 C17 N4 0.3(11) . . . . ? C15 C16 C17 C18 179.5(6) . . . . ? C19 N5 C18 O3 -15.6(10) . . . . ? Co1 N5 C18 O3 -176.8(6) . . . . ? C19 N5 C18 C17 166.9(5) . . . . ? Co1 N5 C18 C17 5.7(7) . . . . ? N4 C17 C18 O3 171.6(6) . . . . ? C16 C17 C18 O3 -7.5(10) . . . . ? N4 C17 C18 N5 -10.7(8) . . . . ? C16 C17 C18 N5 170.1(6) . . . . ? C24 N6 C19 C20 -4.8(10) . . . . ? Zn1 N6 C19 C20 173.3(5) . . . . ? C24 N6 C19 N5 175.6(6) . . . . ? Zn1 N6 C19 N5 -6.4(8) . . . . ? C18 N5 C19 N6 128.6(7) . . . . ? Co1 N5 C19 N6 -71.9(7) . . . . ? C18 N5 C19 C20 -51.0(9) . . . . ? Co1 N5 C19 C20 108.5(7) . . . . ? N6 C19 C20 C21 1.5(11) . . . . ? N5 C19 C20 C21 -178.8(6) . . . . ? C19 C20 C21 C23 1.7(11) . . . . ? C19 C20 C21 C22 -179.7(7) . . . . ? C20 C21 C23 C24 -1.7(10) . . . . ? C22 C21 C23 C24 179.7(7) . . . . ? C21 C23 C24 N6 -1.4(10) . . . . ? C19 N6 C24 C23 4.7(10) . . . . ? Zn1 N6 C24 C23 -173.4(5) . . . . ? C29 N7 C25 C26 0.9(11) . . . . ? Co1 N7 C25 C26 171.3(6) . . . . ? N7 C25 C26 C27 -1.0(12) . . . . ? C25 C26 C27 C28 2.9(13) . . . . ? C26 C27 C28 C29 -4.6(12) . . . . ? C25 N7 C29 C28 -2.8(10) . . . . ? Co1 N7 C29 C28 -174.4(6) . . . . ? C25 N7 C29 C30 178.6(6) . . . . ? Co1 N7 C29 C30 7.0(7) . . . . ? C27 C28 C29 N7 4.6(12) . . . . ? C27 C28 C29 C30 -176.9(7) . . . . ? C31 N8 C30 O2 -15.9(10) . . . . ? Co1 N8 C30 O2 -177.0(5) . . . . ? C31 N8 C30 C29 163.8(6) . . . . ? Co1 N8 C30 C29 2.6(7) . . . . ? N7 C29 C30 O2 173.3(6) . . . . ? C28 C29 C30 O2 -5.2(11) . . . . ? N7 C29 C30 N8 -6.3(8) . . . . ? C28 C29 C30 N8 175.1(7) . . . . ? C36 N9 C31 C32 -2.4(10) . . . . ? Zn1 N9 C31 C32 -179.5(5) . . . . ? C36 N9 C31 N8 176.3(6) . . . . ? Zn1 N9 C31 N8 -0.7(8) . . . . ? C30 N8 C31 C32 -56.8(9) . . . . ? Co1 N8 C31 C32 102.9(7) . . . . ? C30 N8 C31 N9 124.5(7) . . . . ? Co1 N8 C31 N9 -75.8(7) . . . . ? N9 C31 C32 C33 -1.0(11) . . . . ? N8 C31 C32 C33 -179.7(6) . . . . ? C31 C32 C33 C35 3.9(10) . . . . ? C31 C32 C33 C34 179.6(7) . . . . ? C32 C33 C35 C36 -3.4(10) . . . . ? C34 C33 C35 C36 -179.2(7) . . . . ? C31 N9 C36 C35 2.8(10) . . . . ? Zn1 N9 C36 C35 179.9(5) . . . . ? C33 C35 C36 N9 0.2(11) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 1.764 _refine_diff_density_min -0.996 _refine_diff_density_rms 0.158 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.043 0.500 0.500 571 171 ' ' 2 0.500 0.500 1.000 12 3 ' ' _platon_squeeze_details ; The data-set of 3 was treated with the SQUEEZE filter due to the presence of severely disordered solvent molecules and counter anion which could not be modeled satisfactorily. The SQUEEZE process reported that the disordered solvent and chloride components accounted for 171 electrons per unit cell or half that number that is 85.5 (one methanol, five water and one chloride) per cation in a volume of 571.0 \%A3 out of a unit volume of 2163.6 \%A3. These disordered molecules were included in the final chemical formula (Table 4). The values of f(000), Dcalc, M and Mu have been calculated on this assumption. ; #===END