# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'Biao Wu' _publ_contact_author_email WUBIAO@LZB.AC.CN _publ_section_title ; Solvent-directed Conformational Variation of Co(II)/(III) Complexes with a Diiminopyridine Ligand ; loop_ _publ_author_name 'Biao Wu' 'Yanyan Liu' 'Ning Tang' 'Xiao-Juan Yang' 'Jin Yang' ; Fuyu Zhuge ; # Attachment 'Co-R.cif' data_L _database_code_depnum_ccdc_archive 'CCDC 754687' #TrackingRef 'Co-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H57 N5 O2' _chemical_formula_weight 699.96 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' _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 8.7594(16) _cell_length_b 15.754(3) _cell_length_c 15.889(3) _cell_angle_alpha 76.862(3) _cell_angle_beta 87.533(4) _cell_angle_gamma 86.832(3) _cell_volume 2131.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.091 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 756 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9834 _exptl_absorpt_correction_T_max 0.9960 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11039 _diffrn_reflns_av_R_equivalents 0.0483 _diffrn_reflns_av_sigmaI/netI 0.1310 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7476 _reflns_number_gt 2848 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0890P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7476 _refine_ls_number_parameters 483 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1948 _refine_ls_R_factor_gt 0.0672 _refine_ls_wR_factor_ref 0.2035 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 0.918 _refine_ls_restrained_S_all 0.918 _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 C1 C 0.8564(5) 0.9332(3) 0.3416(3) 0.0664(13) Uani 1 1 d . . . H1 H 0.9215 0.8835 0.3528 0.080 Uiso 1 1 calc R . . C2 C 0.7010(5) 0.9210(3) 0.3423(2) 0.0519(11) Uani 1 1 d . . . C3 C 0.6076(5) 0.9963(3) 0.3276(3) 0.0649(12) Uani 1 1 d . . . H3 H 0.5019 0.9928 0.3283 0.078 Uiso 1 1 calc R . . C4 C 0.6714(6) 1.0763(3) 0.3120(3) 0.0803(15) Uani 1 1 d . . . H4 H 0.6095 1.1273 0.3018 0.096 Uiso 1 1 calc R . . C5 C 0.8278(7) 1.0802(3) 0.3115(3) 0.0860(16) Uani 1 1 d . . . H5 H 0.8698 1.1348 0.3002 0.103 Uiso 1 1 calc R . . C6 C 0.6410(5) 0.8331(2) 0.3570(2) 0.0454(10) Uani 1 1 d . . . C7 C 0.7154(4) 0.7692(2) 0.3210(3) 0.0529(11) Uani 1 1 d . . . H7 H 0.8074 0.7815 0.2905 0.064 Uiso 1 1 calc R . . C8 C 0.6576(4) 0.6875(2) 0.3289(3) 0.0499(10) Uani 1 1 d . . . C9 C 0.5181(4) 0.6706(2) 0.3742(2) 0.0451(10) Uani 1 1 d . . . C10 C 0.4430(4) 0.7321(2) 0.4148(2) 0.0470(10) Uani 1 1 d . . . C11 C 0.5069(5) 0.8126(2) 0.4046(2) 0.0489(10) Uani 1 1 d . . . H11 H 0.4577 0.8542 0.4307 0.059 Uiso 1 1 calc R . . C12 C 0.7418(5) 0.6192(3) 0.2889(3) 0.0708(14) Uani 1 1 d . . . H12 H 0.6652 0.5799 0.2786 0.085 Uiso 1 1 calc R . . C13 C 0.8203(9) 0.6541(4) 0.2043(4) 0.170(3) Uani 1 1 d . . . H13A H 0.7459 0.6816 0.1629 0.255 Uiso 1 1 calc R . . H13B H 0.8741 0.6072 0.1846 0.255 Uiso 1 1 calc R . . H13C H 0.8916 0.6961 0.2109 0.255 Uiso 1 1 calc R . . C14 C 0.8533(8) 0.5650(5) 0.3504(5) 0.189(4) Uani 1 1 d . . . H14A H 0.9052 0.5222 0.3237 0.284 Uiso 1 1 calc R . . H14B H 0.7995 0.5362 0.4020 0.284 Uiso 1 1 calc R . . H14C H 0.9268 0.6020 0.3650 0.284 Uiso 1 1 calc R . . C15 C 0.2974(5) 0.7102(3) 0.4675(3) 0.0655(12) Uani 1 1 d . . . H15 H 0.2909 0.6466 0.4800 0.079 Uiso 1 1 calc R . . C16 C 0.2974(8) 0.7358(7) 0.5511(4) 0.220(5) Uani 1 1 d . . . H16A H 0.2289 0.7858 0.5495 0.330 Uiso 1 1 calc R . . H16B H 0.3989 0.7499 0.5619 0.330 Uiso 1 1 calc R . . H16C H 0.2644 0.6883 0.5964 0.330 Uiso 1 1 calc R . . C17 C 0.1632(6) 0.7471(5) 0.4226(4) 0.186(4) Uani 1 1 d . . . H17A H 0.1518 0.8080 0.4227 0.279 Uiso 1 1 calc R . . H17B H 0.0753 0.7178 0.4509 0.279 Uiso 1 1 calc R . . H17C H 0.1722 0.7402 0.3641 0.279 Uiso 1 1 calc R . . C18 C 0.3747(4) 0.5717(2) 0.3252(3) 0.0487(10) Uani 1 1 d . . . C19 C 0.3446(5) 0.6324(2) 0.2398(3) 0.0717(14) Uani 1 1 d . . . H19A H 0.3911 0.6867 0.2372 0.108 Uiso 1 1 calc R . . H19B H 0.2362 0.6426 0.2332 0.108 Uiso 1 1 calc R . . H19C H 0.3870 0.6067 0.1942 0.108 Uiso 1 1 calc R . . C20 C 0.3044(4) 0.4853(2) 0.3413(3) 0.0448(10) Uani 1 1 d . . . C21 C 0.3153(5) 0.4262(3) 0.4189(3) 0.0595(12) Uani 1 1 d . . . H21 H 0.3694 0.4381 0.4636 0.071 Uiso 1 1 calc R . . C22 C 0.2441(5) 0.3487(3) 0.4289(3) 0.0682(13) Uani 1 1 d . . . H22 H 0.2495 0.3076 0.4810 0.082 Uiso 1 1 calc R . . C23 C 0.1654(5) 0.3319(3) 0.3623(3) 0.0595(12) Uani 1 1 d . . . H23 H 0.1161 0.2799 0.3685 0.071 Uiso 1 1 calc R . . C24 C 0.1614(4) 0.3940(2) 0.2860(3) 0.0441(10) Uani 1 1 d . . . C25 C 0.0854(4) 0.3795(2) 0.2078(2) 0.0439(10) Uani 1 1 d . . . C26 C 0.1078(5) 0.4466(3) 0.1256(3) 0.0713(13) Uani 1 1 d . . . H26A H 0.0688 0.4264 0.0785 0.107 Uiso 1 1 calc R . . H26B H 0.2149 0.4563 0.1153 0.107 Uiso 1 1 calc R . . H26C H 0.0542 0.5002 0.1303 0.107 Uiso 1 1 calc R . . C27 C -0.0521(4) 0.2878(2) 0.1443(2) 0.0478(10) Uani 1 1 d . . . C28 C -0.1949(4) 0.3215(2) 0.1136(2) 0.0493(10) Uani 1 1 d . . . C29 C -0.2512(4) 0.2904(2) 0.0469(3) 0.0543(11) Uani 1 1 d . . . H29 H -0.3463 0.3121 0.0257 0.065 Uiso 1 1 calc R . . C30 C -0.1722(4) 0.2284(2) 0.0102(2) 0.0480(10) Uani 1 1 d . . . C31 C -0.0321(5) 0.1972(2) 0.0423(2) 0.0526(11) Uani 1 1 d . . . H31 H 0.0224 0.1560 0.0178 0.063 Uiso 1 1 calc R . . C32 C 0.0322(4) 0.2242(2) 0.1095(2) 0.0493(10) Uani 1 1 d . . . C33 C -0.2844(5) 0.3873(3) 0.1537(3) 0.0643(13) Uani 1 1 d . . . H33 H -0.2114 0.4162 0.1815 0.077 Uiso 1 1 calc R . . C34 C -0.3706(7) 0.4568(3) 0.0910(3) 0.122(2) Uani 1 1 d . . . H34A H -0.2998 0.4909 0.0513 0.183 Uiso 1 1 calc R . . H34B H -0.4292 0.4939 0.1220 0.183 Uiso 1 1 calc R . . H34C H -0.4382 0.4302 0.0597 0.183 Uiso 1 1 calc R . . C35 C -0.3925(8) 0.3429(4) 0.2221(4) 0.135(2) Uani 1 1 d . . . H35A H -0.4703 0.3176 0.1962 0.202 Uiso 1 1 calc R . . H35B H -0.4391 0.3846 0.2521 0.202 Uiso 1 1 calc R . . H35C H -0.3380 0.2978 0.2622 0.202 Uiso 1 1 calc R . . C36 C 0.1861(5) 0.1885(3) 0.1439(3) 0.0652(13) Uani 1 1 d . . . H36 H 0.1887 0.1943 0.2039 0.078 Uiso 1 1 calc R . . C37 C 0.3088(6) 0.2425(4) 0.0931(4) 0.125(2) Uani 1 1 d . . . H37A H 0.3064 0.2393 0.0335 0.187 Uiso 1 1 calc R . . H37B H 0.4067 0.2206 0.1157 0.187 Uiso 1 1 calc R . . H37C H 0.2917 0.3021 0.0975 0.187 Uiso 1 1 calc R . . C38 C 0.2177(6) 0.0935(3) 0.1433(4) 0.115(2) Uani 1 1 d . . . H38A H 0.1310 0.0608 0.1681 0.173 Uiso 1 1 calc R . . H38B H 0.3061 0.0716 0.1767 0.173 Uiso 1 1 calc R . . H38C H 0.2362 0.0876 0.0849 0.173 Uiso 1 1 calc R . . C39 C -0.2354(5) 0.1936(2) -0.0595(2) 0.0477(10) Uani 1 1 d . . . C40 C -0.1434(5) 0.1664(2) -0.1218(3) 0.0559(11) Uani 1 1 d . . . H40 H -0.0380 0.1713 -0.1225 0.067 Uiso 1 1 calc R . . C41 C -0.2091(6) 0.1321(3) -0.1828(3) 0.0649(12) Uani 1 1 d . . . H41 H -0.1484 0.1137 -0.2254 0.078 Uiso 1 1 calc R . . C42 C -0.3646(6) 0.1252(3) -0.1807(3) 0.0695(13) Uani 1 1 d . . . H42 H -0.4071 0.1019 -0.2227 0.083 Uiso 1 1 calc R . . C43 C -0.3909(5) 0.1831(3) -0.0632(3) 0.0607(12) Uani 1 1 d . . . H43 H -0.4545 0.2006 -0.0213 0.073 Uiso 1 1 calc R . . N1 N 0.9207(4) 1.0104(3) 0.3263(3) 0.0816(12) Uani 1 1 d . . . N2 N 0.4526(4) 0.58766(19) 0.3845(2) 0.0498(9) Uani 1 1 d . . . N3 N 0.2291(3) 0.46965(19) 0.27487(19) 0.0454(8) Uani 1 1 d . . . N4 N 0.0111(3) 0.31123(19) 0.21681(19) 0.0479(8) Uani 1 1 d . . . N5 N -0.4565(4) 0.1499(2) -0.1221(3) 0.0690(11) Uani 1 1 d . . . C44 C 0.2274(7) 0.0198(3) 0.9112(4) 0.111(2) Uani 1 1 d . . . H44A H 0.3292 -0.0051 0.9066 0.166 Uiso 1 1 calc R . . H44B H 0.1622 -0.0005 0.8736 0.166 Uiso 1 1 calc R . . H44C H 0.1891 0.0025 0.9698 0.166 Uiso 1 1 calc R . . O1 O 0.2302(3) 0.1102(2) 0.8873(3) 0.0938(11) Uani 1 1 d . . . H46 H 0.3187 0.1250 0.8858 0.141 Uiso 1 1 calc R . . C45 C 0.2311(8) 0.0541(5) 0.4351(5) 0.174(3) Uani 1 1 d . . . H45A H 0.2563 0.0119 0.4870 0.261 Uiso 1 1 calc R . . H45B H 0.1316 0.0807 0.4423 0.261 Uiso 1 1 calc R . . H45C H 0.3055 0.0982 0.4233 0.261 Uiso 1 1 calc R . . O2 O 0.2310(4) 0.0144(4) 0.3689(3) 0.1499(18) Uani 1 1 d . . . H47 H 0.1456 0.0203 0.3486 0.225 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 C1 0.055(3) 0.055(3) 0.094(4) -0.026(3) -0.004(3) -0.009(2) C2 0.050(3) 0.055(3) 0.054(3) -0.020(2) -0.008(2) -0.008(2) C3 0.061(3) 0.051(3) 0.086(3) -0.021(2) -0.013(3) -0.005(2) C4 0.080(4) 0.053(3) 0.112(4) -0.026(3) -0.005(3) -0.004(3) C5 0.088(4) 0.060(3) 0.115(4) -0.027(3) 0.000(4) -0.017(3) C6 0.048(3) 0.042(2) 0.050(3) -0.015(2) -0.013(2) -0.001(2) C7 0.041(2) 0.053(3) 0.067(3) -0.017(2) -0.004(2) -0.009(2) C8 0.044(3) 0.051(2) 0.059(3) -0.022(2) -0.002(2) -0.002(2) C9 0.050(3) 0.042(2) 0.046(2) -0.012(2) -0.015(2) -0.004(2) C10 0.048(3) 0.052(2) 0.045(2) -0.017(2) -0.008(2) -0.006(2) C11 0.055(3) 0.048(2) 0.049(3) -0.019(2) -0.005(2) -0.007(2) C12 0.061(3) 0.061(3) 0.100(4) -0.038(3) 0.011(3) -0.005(3) C13 0.257(9) 0.099(4) 0.157(6) -0.061(4) 0.119(6) -0.006(5) C14 0.184(8) 0.197(7) 0.195(8) -0.087(7) -0.046(6) 0.134(7) C15 0.061(3) 0.065(3) 0.075(3) -0.026(3) 0.016(3) -0.012(2) C16 0.120(6) 0.460(15) 0.108(6) -0.112(8) 0.043(5) -0.093(8) C17 0.052(4) 0.308(10) 0.151(6) 0.044(7) -0.002(4) -0.001(5) C18 0.051(3) 0.043(2) 0.057(3) -0.020(2) -0.006(2) -0.003(2) C19 0.102(4) 0.047(2) 0.065(3) -0.001(2) -0.035(3) -0.015(3) C20 0.044(2) 0.043(2) 0.051(3) -0.016(2) -0.007(2) 0.0004(19) C21 0.074(3) 0.050(3) 0.055(3) -0.007(2) -0.022(2) -0.016(2) C22 0.086(4) 0.059(3) 0.058(3) -0.003(2) -0.025(3) -0.016(3) C23 0.073(3) 0.050(3) 0.055(3) -0.004(2) -0.012(2) -0.022(2) C24 0.038(2) 0.044(2) 0.055(3) -0.021(2) -0.005(2) -0.003(2) C25 0.041(2) 0.045(2) 0.049(3) -0.018(2) -0.003(2) 0.001(2) C26 0.085(4) 0.069(3) 0.060(3) -0.009(3) -0.017(3) -0.022(3) C27 0.048(3) 0.049(2) 0.052(3) -0.021(2) -0.002(2) -0.008(2) C28 0.041(3) 0.052(2) 0.057(3) -0.019(2) -0.008(2) 0.000(2) C29 0.041(2) 0.059(3) 0.067(3) -0.021(2) -0.010(2) 0.000(2) C30 0.043(3) 0.048(2) 0.056(3) -0.016(2) -0.010(2) -0.004(2) C31 0.049(3) 0.055(3) 0.058(3) -0.022(2) -0.007(2) 0.002(2) C32 0.042(2) 0.053(2) 0.057(3) -0.017(2) -0.012(2) -0.002(2) C33 0.050(3) 0.075(3) 0.076(3) -0.037(3) -0.015(3) 0.011(2) C34 0.165(6) 0.090(4) 0.105(5) -0.025(4) 0.005(4) 0.057(4) C35 0.157(6) 0.128(5) 0.113(5) -0.034(4) 0.047(5) 0.039(5) C36 0.053(3) 0.079(3) 0.075(3) -0.042(3) -0.022(3) 0.017(3) C37 0.046(3) 0.143(5) 0.191(7) -0.049(5) -0.006(4) -0.004(4) C38 0.106(5) 0.099(4) 0.151(5) -0.050(4) -0.054(4) 0.049(4) C39 0.048(3) 0.047(2) 0.049(3) -0.011(2) -0.009(2) -0.003(2) C40 0.055(3) 0.058(3) 0.058(3) -0.019(2) -0.015(2) -0.001(2) C41 0.074(4) 0.065(3) 0.060(3) -0.023(2) -0.008(3) 0.004(3) C42 0.082(4) 0.066(3) 0.067(3) -0.023(3) -0.027(3) -0.008(3) C43 0.049(3) 0.072(3) 0.066(3) -0.025(2) -0.013(2) -0.004(2) N1 0.063(3) 0.069(3) 0.119(4) -0.030(3) -0.001(2) -0.019(2) N2 0.049(2) 0.049(2) 0.053(2) -0.0132(17) -0.0086(17) -0.0069(17) N3 0.045(2) 0.0443(19) 0.050(2) -0.0153(16) -0.0088(17) -0.0011(16) N4 0.044(2) 0.049(2) 0.055(2) -0.0192(17) -0.0068(17) -0.0056(17) N5 0.059(3) 0.076(3) 0.079(3) -0.031(2) -0.023(2) -0.003(2) C44 0.135(6) 0.082(4) 0.112(5) -0.011(4) 0.004(4) -0.029(4) O1 0.060(2) 0.080(2) 0.135(3) -0.007(2) -0.005(2) -0.0117(18) C45 0.145(7) 0.266(10) 0.145(7) -0.118(7) -0.028(5) -0.001(6) O2 0.077(3) 0.237(5) 0.160(4) -0.097(4) -0.017(3) 0.004(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 C1 N1 1.336(5) . ? C1 C2 1.384(5) . ? C2 C3 1.384(5) . ? C2 C6 1.474(5) . ? C3 C4 1.373(6) . ? C4 C5 1.374(6) . ? C5 N1 1.314(6) . ? C6 C11 1.383(5) . ? C6 C7 1.386(5) . ? C7 C8 1.385(5) . ? C8 C9 1.398(5) . ? C8 C12 1.514(5) . ? C9 C10 1.402(5) . ? C9 N2 1.428(4) . ? C10 C11 1.387(5) . ? C10 C15 1.508(5) . ? C12 C13 1.485(7) . ? C12 C14 1.500(7) . ? C15 C17 1.427(6) . ? C15 C16 1.473(7) . ? C18 N2 1.265(4) . ? C18 C20 1.489(5) . ? C18 C19 1.496(5) . ? C20 N3 1.344(4) . ? C20 C21 1.370(5) . ? C21 C22 1.376(5) . ? C22 C23 1.369(5) . ? C23 C24 1.374(5) . ? C24 N3 1.333(4) . ? C24 C25 1.502(5) . ? C25 N4 1.266(4) . ? C25 C26 1.495(5) . ? C27 C28 1.395(5) . ? C27 C32 1.410(5) . ? C27 N4 1.428(4) . ? C28 C29 1.384(5) . ? C28 C33 1.504(5) . ? C29 C30 1.387(5) . ? C30 C31 1.371(5) . ? C30 C39 1.482(5) . ? C31 C32 1.388(5) . ? C32 C36 1.507(5) . ? C33 C35 1.486(7) . ? C33 C34 1.496(6) . ? C36 C37 1.498(6) . ? C36 C38 1.510(6) . ? C39 C40 1.378(5) . ? C39 C43 1.386(5) . ? C40 C41 1.372(5) . ? C41 C42 1.371(6) . ? C42 N5 1.317(5) . ? C43 N5 1.335(5) . ? C44 O1 1.390(5) . ? C45 O2 1.341(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 C1 C2 125.4(4) . . ? C3 C2 C1 115.7(4) . . ? C3 C2 C6 122.8(4) . . ? C1 C2 C6 121.5(4) . . ? C4 C3 C2 119.8(4) . . ? C3 C4 C5 119.3(5) . . ? N1 C5 C4 123.0(5) . . ? C11 C6 C7 118.0(4) . . ? C11 C6 C2 121.2(4) . . ? C7 C6 C2 120.8(4) . . ? C8 C7 C6 122.4(4) . . ? C7 C8 C9 117.9(4) . . ? C7 C8 C12 121.1(4) . . ? C9 C8 C12 121.0(4) . . ? C8 C9 C10 121.3(3) . . ? C8 C9 N2 120.6(3) . . ? C10 C9 N2 118.1(4) . . ? C11 C10 C9 117.9(4) . . ? C11 C10 C15 121.9(4) . . ? C9 C10 C15 120.2(3) . . ? C6 C11 C10 122.3(4) . . ? C13 C12 C14 109.9(5) . . ? C13 C12 C8 114.7(4) . . ? C14 C12 C8 110.9(4) . . ? C17 C15 C16 109.3(6) . . ? C17 C15 C10 113.2(4) . . ? C16 C15 C10 112.4(4) . . ? N2 C18 C20 117.7(4) . . ? N2 C18 C19 125.9(3) . . ? C20 C18 C19 116.4(3) . . ? N3 C20 C21 122.4(4) . . ? N3 C20 C18 115.6(4) . . ? C21 C20 C18 122.0(3) . . ? C20 C21 C22 118.2(4) . . ? C23 C22 C21 120.3(4) . . ? C22 C23 C24 118.1(4) . . ? N3 C24 C23 122.8(4) . . ? N3 C24 C25 115.2(4) . . ? C23 C24 C25 122.0(4) . . ? N4 C25 C26 125.9(4) . . ? N4 C25 C24 117.5(4) . . ? C26 C25 C24 116.6(3) . . ? C28 C27 C32 121.7(3) . . ? C28 C27 N4 121.6(3) . . ? C32 C27 N4 116.5(3) . . ? C29 C28 C27 117.4(4) . . ? C29 C28 C33 121.9(4) . . ? C27 C28 C33 120.6(3) . . ? C28 C29 C30 123.0(4) . . ? C31 C30 C29 117.7(4) . . ? C31 C30 C39 119.7(4) . . ? C29 C30 C39 122.6(4) . . ? C30 C31 C32 123.1(4) . . ? C31 C32 C27 117.1(4) . . ? C31 C32 C36 122.0(4) . . ? C27 C32 C36 120.9(3) . . ? C35 C33 C34 109.1(4) . . ? C35 C33 C28 110.3(4) . . ? C34 C33 C28 114.7(4) . . ? C37 C36 C32 109.3(4) . . ? C37 C36 C38 110.2(4) . . ? C32 C36 C38 113.6(4) . . ? C40 C39 C43 116.2(4) . . ? C40 C39 C30 122.3(4) . . ? C43 C39 C30 121.4(4) . . ? C41 C40 C39 119.3(4) . . ? C42 C41 C40 119.7(4) . . ? N5 C42 C41 123.0(4) . . ? N5 C43 C39 125.2(4) . . ? C5 N1 C1 116.8(4) . . ? C18 N2 C9 120.3(3) . . ? C24 N3 C20 118.3(3) . . ? C25 N4 C27 121.3(3) . . ? C42 N5 C43 116.6(4) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.441 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.038 ############ data_1a _database_code_depnum_ccdc_archive 'CCDC 754688' #TrackingRef 'Co-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H100 Cl4 Co N10' _chemical_formula_weight 1486.50 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' 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.2955(18) _cell_length_b 13.604(3) _cell_length_c 18.883(4) _cell_angle_alpha 80.997(3) _cell_angle_beta 88.164(3) _cell_angle_gamma 81.838(3) _cell_volume 2334.4(8) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 787 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9194 _exptl_absorpt_correction_T_max 0.9348 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15561 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.1143 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8018 _reflns_number_gt 4241 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1727P)^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 8018 _refine_ls_number_parameters 512 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1525 _refine_ls_R_factor_gt 0.0830 _refine_ls_wR_factor_ref 0.2868 _refine_ls_wR_factor_gt 0.2374 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _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 0.5000 1.0000 0.0000 0.0344(3) Uani 1 2 d S . . Cl1 Cl 0.38989(15) 0.95818(10) 0.12067(7) 0.0450(4) Uani 1 1 d . . . N1 N 0.5922(5) 0.8410(3) 0.0017(2) 0.0382(11) Uani 1 1 d . . . N2 N 0.2695(5) 0.3804(3) 0.2137(2) 0.0472(12) Uani 1 1 d . . . N3 N 0.1988(5) 0.2735(3) 0.3920(2) 0.0488(12) Uani 1 1 d . . . N4 N 0.1077(5) 0.1064(4) 0.5439(2) 0.0509(13) Uani 1 1 d . . . N5 N 0.2976(5) -0.0307(3) 0.9511(2) 0.0391(11) Uani 1 1 d . . . C1 C 0.5308(6) 0.7676(4) 0.0405(3) 0.0377(12) Uani 1 1 d . . . H1 H 0.4561 0.7858 0.0718 0.045 Uiso 1 1 calc R . . C2 C 0.5692(6) 0.6662(4) 0.0379(3) 0.0417(13) Uani 1 1 d . . . C3 C 0.6825(7) 0.6410(4) -0.0077(3) 0.0545(16) Uani 1 1 d . . . H3 H 0.7123 0.5740 -0.0121 0.065 Uiso 1 1 calc R . . C4 C 0.7521(7) 0.7159(5) -0.0468(3) 0.0603(18) Uani 1 1 d . . . H4 H 0.8309 0.6996 -0.0764 0.072 Uiso 1 1 calc R . . C5 C 0.7029(7) 0.8138(5) -0.0413(3) 0.0539(16) Uani 1 1 d . . . H5 H 0.7485 0.8638 -0.0686 0.065 Uiso 1 1 calc R . . C6 C 0.4906(6) 0.5915(4) 0.0828(3) 0.0425(14) Uani 1 1 d . . . C7 C 0.3439(6) 0.6124(4) 0.0978(3) 0.0450(14) Uani 1 1 d . . . H7 H 0.2939 0.6739 0.0773 0.054 Uiso 1 1 calc R . . C8 C 0.2682(6) 0.5464(4) 0.1418(3) 0.0421(13) Uani 1 1 d . . . C9 C 0.3446(7) 0.4547(4) 0.1715(3) 0.0450(14) Uani 1 1 d . . . C10 C 0.4940(6) 0.4296(4) 0.1565(3) 0.0457(14) Uani 1 1 d . . . C11 C 0.5629(7) 0.4993(4) 0.1115(3) 0.0459(14) Uani 1 1 d . . . H11 H 0.6608 0.4833 0.1004 0.055 Uiso 1 1 calc R . . C12 C 0.1065(7) 0.5727(5) 0.1569(4) 0.0639(18) Uani 1 1 d . . . H12 H 0.0893 0.5507 0.2080 0.077 Uiso 1 1 calc R . . C13 C 0.0512(10) 0.6838(6) 0.1405(6) 0.106(3) Uani 1 1 d . . . H13A H 0.1182 0.7212 0.1586 0.159 Uiso 1 1 calc R . . H13B H -0.0421 0.6972 0.1630 0.159 Uiso 1 1 calc R . . H13C H 0.0423 0.7036 0.0896 0.159 Uiso 1 1 calc R . . C14 C 0.0148(9) 0.5171(8) 0.1142(6) 0.120(4) Uani 1 1 d . . . H14A H 0.0082 0.5499 0.0653 0.180 Uiso 1 1 calc R . . H14B H -0.0809 0.5180 0.1350 0.180 Uiso 1 1 calc R . . H14C H 0.0599 0.4489 0.1157 0.180 Uiso 1 1 calc R . . C15 C 0.5773(8) 0.3281(5) 0.1890(4) 0.0649(19) Uani 1 1 d . . . H15 H 0.5079 0.2879 0.2157 0.078 Uiso 1 1 calc R . . C16 C 0.6861(18) 0.3411(9) 0.2384(9) 0.235(10) Uani 1 1 d . . . H16A H 0.6410 0.3510 0.2836 0.353 Uiso 1 1 calc R . . H16B H 0.7320 0.3986 0.2193 0.353 Uiso 1 1 calc R . . H16C H 0.7578 0.2823 0.2450 0.353 Uiso 1 1 calc R . . C17 C 0.6447(18) 0.2732(8) 0.1319(6) 0.184(7) Uani 1 1 d . . . H17A H 0.7394 0.2919 0.1203 0.276 Uiso 1 1 calc R . . H17B H 0.5850 0.2900 0.0899 0.276 Uiso 1 1 calc R . . H17C H 0.6533 0.2022 0.1482 0.276 Uiso 1 1 calc R . . C18 C 0.3186(10) 0.4420(6) 0.3277(4) 0.093(3) Uani 1 1 d . . . H18A H 0.3422 0.5014 0.2977 0.140 Uiso 1 1 calc R . . H18B H 0.4043 0.4067 0.3520 0.140 Uiso 1 1 calc R . . H18C H 0.2460 0.4605 0.3624 0.140 Uiso 1 1 calc R . . C19 C 0.2602(7) 0.3740(4) 0.2816(3) 0.0537(16) Uani 1 1 d . . . C20 C 0.1861(7) 0.2894(4) 0.3210(3) 0.0485(15) Uani 1 1 d . . . C21 C 0.1167(8) 0.2316(5) 0.2840(3) 0.0638(19) Uani 1 1 d . . . H21 H 0.1120 0.2445 0.2343 0.077 Uiso 1 1 calc R . . C22 C 0.0531(8) 0.1525(5) 0.3231(3) 0.069(2) Uani 1 1 d . . . H22 H 0.0016 0.1128 0.3003 0.083 Uiso 1 1 calc R . . C23 C 0.0689(7) 0.1351(5) 0.3960(3) 0.0585(17) Uani 1 1 d . . . H23 H 0.0308 0.0816 0.4233 0.070 Uiso 1 1 calc R . . C24 C 0.1410(7) 0.1968(4) 0.4289(3) 0.0470(14) Uani 1 1 d . . . C25 C 0.1620(7) 0.1790(5) 0.5076(3) 0.0539(16) Uani 1 1 d . . . C26 C 0.2441(10) 0.2512(6) 0.5406(4) 0.087(3) Uani 1 1 d . . . H26A H 0.2175 0.2493 0.5903 0.131 Uiso 1 1 calc R . . H26B H 0.2191 0.3183 0.5156 0.131 Uiso 1 1 calc R . . H26C H 0.3469 0.2310 0.5364 0.131 Uiso 1 1 calc R . . C27 C 0.1221(7) 0.0830(4) 0.6196(3) 0.0452(14) Uani 1 1 d . . . C28 C 0.2443(7) 0.0194(5) 0.6481(3) 0.0501(15) Uani 1 1 d . . . C29 C 0.2519(6) -0.0076(5) 0.7231(3) 0.0476(15) Uani 1 1 d . . . H29 H 0.3345 -0.0477 0.7431 0.057 Uiso 1 1 calc R . . C30 C 0.1384(6) 0.0242(4) 0.7683(3) 0.0411(13) Uani 1 1 d . . . C31 C 0.0170(6) 0.0839(4) 0.7370(3) 0.0479(15) Uani 1 1 d . . . H31 H -0.0608 0.1038 0.7662 0.058 Uiso 1 1 calc R . . C32 C 0.0077(7) 0.1150(5) 0.6635(3) 0.0485(15) Uani 1 1 d . . . C33 C 0.3661(8) -0.0231(6) 0.5994(4) 0.073(2) Uani 1 1 d . . . H33 H 0.3823 0.0312 0.5607 0.088 Uiso 1 1 calc R . . C34 C 0.3231(12) -0.1046(9) 0.5665(6) 0.134(4) Uani 1 1 d . . . H34A H 0.4066 -0.1385 0.5447 0.202 Uiso 1 1 calc R . . H34B H 0.2513 -0.0776 0.5306 0.202 Uiso 1 1 calc R . . H34C H 0.2833 -0.1514 0.6026 0.202 Uiso 1 1 calc R . . C35 C 0.5109(10) -0.0570(11) 0.6400(6) 0.144(5) Uani 1 1 d . . . H35A H 0.5169 -0.0159 0.6764 0.215 Uiso 1 1 calc R . . H35B H 0.5908 -0.0503 0.6069 0.215 Uiso 1 1 calc R . . H35C H 0.5150 -0.1260 0.6618 0.215 Uiso 1 1 calc R . . C36 C -0.1274(8) 0.1836(6) 0.6321(4) 0.076(2) Uani 1 1 d . . . H36 H -0.1107 0.1942 0.5801 0.092 Uiso 1 1 calc R . . C37 C -0.1400(17) 0.2880(8) 0.6541(9) 0.214(9) Uani 1 1 d . . . H37A H -0.0534 0.3171 0.6398 0.321 Uiso 1 1 calc R . . H37B H -0.1519 0.2824 0.7052 0.321 Uiso 1 1 calc R . . H37C H -0.2225 0.3300 0.6312 0.321 Uiso 1 1 calc R . . C38 C -0.2578(13) 0.1330(11) 0.6431(10) 0.213(8) Uani 1 1 d . . . H38A H -0.3048 0.1464 0.6872 0.319 Uiso 1 1 calc R . . H38B H -0.2303 0.0619 0.6452 0.319 Uiso 1 1 calc R . . H38C H -0.3233 0.1578 0.6040 0.319 Uiso 1 1 calc R . . C39 C 0.1501(6) -0.0097(4) 0.8452(3) 0.0377(12) Uani 1 1 d . . . C40 C 0.0450(6) -0.0578(5) 0.8856(3) 0.0499(15) Uani 1 1 d . . . H40 H -0.0408 -0.0660 0.8646 0.060 Uiso 1 1 calc R . . C41 C 0.0706(7) -0.0935(5) 0.9580(3) 0.0545(16) Uani 1 1 d . . . H41 H 0.0024 -0.1268 0.9856 0.065 Uiso 1 1 calc R . . C42 C 0.1954(6) -0.0795(4) 0.9880(3) 0.0444(14) Uani 1 1 d . . . H42 H 0.2111 -0.1046 1.0363 0.053 Uiso 1 1 calc R . . C43 C 0.2719(6) 0.0019(4) 0.8822(3) 0.0418(13) Uani 1 1 d . . . H43 H 0.3417 0.0357 0.8563 0.050 Uiso 1 1 calc R . . C44 C 0.821(3) 0.379(2) 0.4246(15) 0.083(9) Uani 0.25 1 d PDU . . H44A H 0.8091 0.4039 0.3739 0.100 Uiso 0.25 1 calc PR . . H44B H 0.8766 0.3119 0.4304 0.100 Uiso 0.25 1 calc PR . . Cl2 Cl 0.907(2) 0.4616(18) 0.4686(13) 0.265(10) Uani 0.25 1 d PDU . . Cl3 Cl 0.6556(18) 0.3784(15) 0.4687(10) 0.205(7) Uani 0.25 1 d PDU . . C45 C 0.283(4) 0.374(2) 0.719(3) 0.166(17) Uani 0.25 1 d PDU . . H45A H 0.1986 0.3830 0.6887 0.200 Uiso 0.25 1 calc PR . . H45B H 0.2730 0.4228 0.7518 0.200 Uiso 0.25 1 calc PR . . Cl4 Cl 0.333(2) 0.2441(15) 0.7634(10) 0.219(8) Uani 0.25 1 d PDU . . Cl5 Cl 0.455(2) 0.3682(17) 0.6691(11) 0.236(8) Uani 0.25 1 d PDU . . 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 0.0449(7) 0.0276(6) 0.0316(6) 0.0017(4) -0.0012(4) -0.0145(5) Cl1 0.0562(9) 0.0455(8) 0.0343(8) -0.0001(6) 0.0011(6) -0.0171(7) N1 0.042(3) 0.034(2) 0.039(3) 0.0041(19) 0.0032(19) -0.015(2) N2 0.067(3) 0.035(3) 0.040(3) 0.007(2) 0.002(2) -0.024(2) N3 0.072(3) 0.039(3) 0.037(3) 0.003(2) -0.003(2) -0.022(3) N4 0.069(3) 0.046(3) 0.039(3) 0.006(2) 0.000(2) -0.027(3) N5 0.050(3) 0.034(2) 0.035(3) -0.0033(19) -0.0011(19) -0.013(2) C1 0.043(3) 0.030(3) 0.040(3) -0.002(2) 0.001(2) -0.012(2) C2 0.044(3) 0.034(3) 0.046(3) 0.002(2) 0.002(2) -0.010(3) C3 0.070(4) 0.033(3) 0.057(4) -0.001(3) 0.009(3) -0.003(3) C4 0.063(4) 0.042(4) 0.071(5) -0.002(3) 0.030(3) -0.007(3) C5 0.054(4) 0.042(4) 0.064(4) 0.004(3) 0.010(3) -0.021(3) C6 0.057(4) 0.028(3) 0.042(3) 0.004(2) -0.002(3) -0.012(3) C7 0.050(4) 0.030(3) 0.050(3) 0.008(2) 0.002(3) -0.002(3) C8 0.050(4) 0.030(3) 0.044(3) 0.005(2) -0.001(2) -0.008(3) C9 0.062(4) 0.036(3) 0.037(3) 0.005(2) -0.003(3) -0.018(3) C10 0.054(4) 0.028(3) 0.053(4) 0.005(2) -0.003(3) -0.009(3) C11 0.054(4) 0.033(3) 0.048(3) 0.002(2) 0.001(3) -0.007(3) C12 0.062(4) 0.055(4) 0.069(5) 0.009(3) 0.010(3) -0.010(3) C13 0.091(6) 0.059(5) 0.158(9) -0.007(5) 0.037(6) -0.001(5) C14 0.072(6) 0.127(9) 0.178(11) -0.075(8) -0.015(6) -0.006(6) C15 0.068(5) 0.038(4) 0.079(5) 0.021(3) -0.011(4) -0.005(3) C16 0.284(18) 0.091(9) 0.32(2) 0.016(10) -0.243(17) 0.012(10) C17 0.324(19) 0.073(7) 0.123(9) -0.026(6) -0.055(10) 0.104(10) C18 0.169(8) 0.081(6) 0.048(4) -0.011(4) 0.015(4) -0.086(6) C19 0.073(4) 0.042(3) 0.047(4) 0.008(3) 0.001(3) -0.028(3) C20 0.067(4) 0.037(3) 0.042(3) 0.003(2) 0.000(3) -0.022(3) C21 0.100(5) 0.061(4) 0.037(3) 0.006(3) -0.008(3) -0.046(4) C22 0.111(6) 0.054(4) 0.049(4) 0.005(3) -0.009(4) -0.048(4) C23 0.082(5) 0.052(4) 0.044(4) 0.010(3) -0.006(3) -0.038(4) C24 0.068(4) 0.036(3) 0.038(3) 0.005(2) 0.000(3) -0.022(3) C25 0.071(4) 0.045(4) 0.049(4) 0.000(3) -0.004(3) -0.025(3) C26 0.137(7) 0.084(6) 0.054(4) 0.005(4) -0.012(4) -0.072(5) C27 0.060(4) 0.042(3) 0.036(3) 0.004(2) -0.006(3) -0.023(3) C28 0.056(4) 0.051(4) 0.044(4) 0.003(3) 0.006(3) -0.025(3) C29 0.048(4) 0.049(4) 0.043(3) 0.008(3) -0.002(3) -0.017(3) C30 0.050(4) 0.038(3) 0.038(3) -0.002(2) -0.004(2) -0.019(3) C31 0.051(4) 0.049(4) 0.041(3) 0.001(3) -0.002(3) -0.006(3) C32 0.057(4) 0.046(4) 0.041(3) 0.001(3) -0.010(3) -0.009(3) C33 0.079(5) 0.080(5) 0.050(4) 0.009(4) 0.017(3) -0.001(4) C34 0.121(8) 0.165(11) 0.144(10) -0.099(8) 0.046(7) -0.036(8) C35 0.073(7) 0.224(14) 0.133(9) -0.043(9) 0.031(6) -0.009(8) C36 0.080(5) 0.089(6) 0.048(4) 0.013(4) -0.012(3) 0.008(5) C37 0.241(16) 0.076(8) 0.32(2) -0.068(10) -0.175(15) 0.065(9) C38 0.087(9) 0.168(14) 0.37(2) 0.025(13) -0.101(11) -0.015(9) C39 0.041(3) 0.034(3) 0.038(3) -0.002(2) -0.003(2) -0.009(2) C40 0.046(4) 0.064(4) 0.042(3) -0.004(3) -0.008(3) -0.021(3) C41 0.051(4) 0.067(4) 0.046(4) 0.005(3) 0.003(3) -0.026(3) C42 0.053(4) 0.043(3) 0.039(3) -0.002(2) 0.001(2) -0.018(3) C43 0.048(3) 0.037(3) 0.040(3) 0.003(2) 0.001(2) -0.017(3) C44 0.083(9) 0.083(9) 0.083(9) -0.0130(17) -0.0013(10) -0.0112(16) Cl2 0.265(10) 0.265(10) 0.266(10) -0.0403(18) -0.0025(10) -0.0364(17) Cl3 0.205(7) 0.205(7) 0.204(7) -0.0312(15) -0.0034(10) -0.0284(14) C45 0.167(17) 0.166(17) 0.166(17) -0.026(3) -0.0016(10) -0.023(3) Cl4 0.219(8) 0.218(8) 0.218(8) -0.0332(15) -0.0025(10) -0.0300(15) Cl5 0.236(8) 0.236(8) 0.236(8) -0.0365(16) -0.0026(10) -0.0331(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 2.206(4) 2_675 ? Co1 N1 2.206(4) . ? Co1 N5 2.241(4) 2_666 ? Co1 N5 2.241(4) 1_564 ? Co1 Cl1 2.4846(13) 2_675 ? Co1 Cl1 2.4847(13) . ? N1 C1 1.329(6) . ? N1 C5 1.337(7) . ? N2 C19 1.271(7) . ? N2 C9 1.434(7) . ? N3 C20 1.331(7) . ? N3 C24 1.331(7) . ? N4 C25 1.268(7) . ? N4 C27 1.421(7) . ? N5 C43 1.325(6) . ? N5 C42 1.349(7) . ? N5 Co1 2.241(4) 1_546 ? C1 C2 1.383(7) . ? C1 H1 0.9300 . ? C2 C3 1.377(8) . ? C2 C6 1.479(7) . ? C3 C4 1.387(8) . ? C3 H3 0.9300 . ? C4 C5 1.365(8) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.376(7) . ? C6 C7 1.382(8) . ? C7 C8 1.379(7) . ? C7 H7 0.9300 . ? C8 C9 1.389(7) . ? C8 C12 1.523(8) . ? C9 C10 1.413(8) . ? C10 C11 1.384(7) . ? C10 C15 1.532(7) . ? C11 H11 0.9300 . ? C12 C13 1.513(10) . ? C12 C14 1.537(11) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.444(12) . ? C15 C17 1.480(12) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.527(9) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.509(7) . ? C20 C21 1.366(8) . ? C21 C22 1.400(8) . ? C21 H21 0.9300 . ? C22 C23 1.369(8) . ? C22 H22 0.9300 . ? C23 C24 1.374(8) . ? C23 H23 0.9300 . ? C24 C25 1.482(8) . ? C25 C26 1.540(9) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.391(8) . ? C27 C28 1.395(8) . ? C28 C29 1.407(8) . ? C28 C33 1.541(9) . ? C29 C30 1.399(8) . ? C29 H29 0.9300 . ? C30 C31 1.383(7) . ? C30 C39 1.457(7) . ? C31 C32 1.388(7) . ? C31 H31 0.9300 . ? C32 C36 1.531(8) . ? C33 C34 1.461(12) . ? C33 C35 1.546(12) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.470(14) . ? C36 C37 1.529(13) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C43 1.389(7) . ? C39 C40 1.394(7) . ? C40 C41 1.393(7) . ? C40 H40 0.9300 . ? C41 C42 1.357(8) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? C44 Cl3 1.728(18) . ? C44 Cl2 1.784(18) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 Cl5 1.826(19) . ? C45 Cl4 1.834(19) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? 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 N1 Co1 N1 180.0 2_675 . ? N1 Co1 N5 89.15(16) 2_675 2_666 ? N1 Co1 N5 90.85(16) . 2_666 ? N1 Co1 N5 90.85(16) 2_675 1_564 ? N1 Co1 N5 89.15(16) . 1_564 ? N5 Co1 N5 180.0 2_666 1_564 ? N1 Co1 Cl1 90.44(11) 2_675 2_675 ? N1 Co1 Cl1 89.56(11) . 2_675 ? N5 Co1 Cl1 89.00(11) 2_666 2_675 ? N5 Co1 Cl1 91.00(11) 1_564 2_675 ? N1 Co1 Cl1 89.56(11) 2_675 . ? N1 Co1 Cl1 90.44(11) . . ? N5 Co1 Cl1 91.00(11) 2_666 . ? N5 Co1 Cl1 89.00(11) 1_564 . ? Cl1 Co1 Cl1 180.0 2_675 . ? C1 N1 C5 116.9(5) . . ? C1 N1 Co1 121.1(3) . . ? C5 N1 Co1 121.7(3) . . ? C19 N2 C9 121.3(5) . . ? C20 N3 C24 118.0(5) . . ? C25 N4 C27 122.0(5) . . ? C43 N5 C42 116.4(5) . . ? C43 N5 Co1 119.6(3) . 1_546 ? C42 N5 Co1 124.0(3) . 1_546 ? N1 C1 C2 125.2(5) . . ? N1 C1 H1 117.4 . . ? C2 C1 H1 117.4 . . ? C3 C2 C1 116.3(5) . . ? C3 C2 C6 123.6(5) . . ? C1 C2 C6 120.1(5) . . ? C2 C3 C4 119.8(5) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C5 C4 C3 118.9(6) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? N1 C5 C4 122.9(5) . . ? N1 C5 H5 118.6 . . ? C4 C5 H5 118.6 . . ? C11 C6 C7 118.2(5) . . ? C11 C6 C2 120.4(5) . . ? C7 C6 C2 121.4(5) . . ? C8 C7 C6 123.1(5) . . ? C8 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C7 C8 C9 117.5(5) . . ? C7 C8 C12 121.2(5) . . ? C9 C8 C12 121.2(5) . . ? C8 C9 C10 121.2(5) . . ? C8 C9 N2 119.9(5) . . ? C10 C9 N2 118.7(5) . . ? C11 C10 C9 118.2(5) . . ? C11 C10 C15 120.9(5) . . ? C9 C10 C15 120.9(5) . . ? C6 C11 C10 121.8(5) . . ? C6 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C13 C12 C8 114.0(6) . . ? C13 C12 C14 107.9(7) . . ? C8 C12 C14 111.3(6) . . ? C13 C12 H12 107.8 . . ? C8 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 110.5(11) . . ? C16 C15 C10 111.0(7) . . ? C17 C15 C10 110.5(6) . . ? C16 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C10 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C20 116.8(5) . . ? N2 C19 C18 126.8(5) . . ? C20 C19 C18 116.4(5) . . ? N3 C20 C21 123.7(5) . . ? N3 C20 C19 115.8(5) . . ? C21 C20 C19 120.5(5) . . ? C20 C21 C22 118.1(6) . . ? C20 C21 H21 120.9 . . ? C22 C21 H21 120.9 . . ? C23 C22 C21 118.0(6) . . ? C23 C22 H22 121.0 . . ? C21 C22 H22 121.0 . . ? C22 C23 C24 120.0(5) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? N3 C24 C23 122.1(5) . . ? N3 C24 C25 116.6(5) . . ? C23 C24 C25 121.3(5) . . ? N4 C25 C24 117.7(5) . . ? N4 C25 C26 123.9(5) . . ? C24 C25 C26 118.3(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 121.0(5) . . ? C32 C27 N4 119.5(5) . . ? C28 C27 N4 119.1(5) . . ? C27 C28 C29 118.1(6) . . ? C27 C28 C33 121.4(5) . . ? C29 C28 C33 120.5(6) . . ? C30 C29 C28 121.7(5) . . ? C30 C29 H29 119.2 . . ? C28 C29 H29 119.2 . . ? C31 C30 C29 117.9(5) . . ? C31 C30 C39 122.9(5) . . ? C29 C30 C39 119.1(5) . . ? C30 C31 C32 122.0(6) . . ? C30 C31 H31 119.0 . . ? C32 C31 H31 119.0 . . ? C31 C32 C27 119.2(5) . . ? C31 C32 C36 119.8(6) . . ? C27 C32 C36 121.0(5) . . ? C34 C33 C28 111.4(6) . . ? C34 C33 C35 111.0(9) . . ? C28 C33 C35 111.9(6) . . ? C34 C33 H33 107.4 . . ? C28 C33 H33 107.4 . . ? C35 C33 H33 107.4 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 116.3(11) . . ? C38 C36 C32 111.6(7) . . ? C37 C36 C32 111.8(7) . . ? C38 C36 H36 105.3 . . ? C37 C36 H36 105.3 . . ? C32 C36 H36 105.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C39 C40 116.0(5) . . ? C43 C39 C30 120.7(5) . . ? C40 C39 C30 123.2(5) . . ? C41 C40 C39 118.9(5) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C42 C41 C40 119.8(5) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? N5 C42 C41 123.0(5) . . ? N5 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? N5 C43 C39 125.9(5) . . ? N5 C43 H43 117.0 . . ? C39 C43 H43 117.0 . . ? Cl3 C44 Cl2 102.4(12) . . ? Cl3 C44 H44A 111.3 . . ? Cl2 C44 H44A 111.3 . . ? Cl3 C44 H44B 111.3 . . ? Cl2 C44 H44B 111.3 . . ? H44A C44 H44B 109.2 . . ? Cl5 C45 Cl4 90.7(11) . . ? Cl5 C45 H45A 113.5 . . ? Cl4 C45 H45A 113.5 . . ? Cl5 C45 H45B 113.5 . . ? Cl4 C45 H45B 113.5 . . ? H45A C45 H45B 110.8 . . ? 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 N1 Co1 N1 C1 141.2(5) 2_675 . . . ? N5 Co1 N1 C1 117.1(4) 2_666 . . . ? N5 Co1 N1 C1 -62.9(4) 1_564 . . . ? Cl1 Co1 N1 C1 -153.9(4) 2_675 . . . ? Cl1 Co1 N1 C1 26.1(4) . . . . ? N1 Co1 N1 C5 -45.4(4) 2_675 . . . ? N5 Co1 N1 C5 -69.5(4) 2_666 . . . ? N5 Co1 N1 C5 110.5(4) 1_564 . . . ? Cl1 Co1 N1 C5 19.5(4) 2_675 . . . ? Cl1 Co1 N1 C5 -160.5(4) . . . . ? C5 N1 C1 C2 -2.4(8) . . . . ? Co1 N1 C1 C2 171.3(4) . . . . ? N1 C1 C2 C3 1.6(9) . . . . ? N1 C1 C2 C6 -178.8(5) . . . . ? C1 C2 C3 C4 0.9(9) . . . . ? C6 C2 C3 C4 -178.8(6) . . . . ? C2 C3 C4 C5 -2.3(10) . . . . ? C1 N1 C5 C4 0.8(9) . . . . ? Co1 N1 C5 C4 -172.9(5) . . . . ? C3 C4 C5 N1 1.5(10) . . . . ? C3 C2 C6 C11 34.5(8) . . . . ? C1 C2 C6 C11 -145.1(6) . . . . ? C3 C2 C6 C7 -146.3(6) . . . . ? C1 C2 C6 C7 34.0(8) . . . . ? C11 C6 C7 C8 1.9(9) . . . . ? C2 C6 C7 C8 -177.3(5) . . . . ? C6 C7 C8 C9 -0.4(9) . . . . ? C6 C7 C8 C12 -180.0(6) . . . . ? C7 C8 C9 C10 -0.7(8) . . . . ? C12 C8 C9 C10 178.8(6) . . . . ? C7 C8 C9 N2 -175.8(5) . . . . ? C12 C8 C9 N2 3.8(8) . . . . ? C19 N2 C9 C8 -93.7(7) . . . . ? C19 N2 C9 C10 91.1(7) . . . . ? C8 C9 C10 C11 0.3(9) . . . . ? N2 C9 C10 C11 175.5(5) . . . . ? C8 C9 C10 C15 -179.6(6) . . . . ? N2 C9 C10 C15 -4.4(8) . . . . ? C7 C6 C11 C10 -2.3(9) . . . . ? C2 C6 C11 C10 176.9(5) . . . . ? C9 C10 C11 C6 1.3(9) . . . . ? C15 C10 C11 C6 -178.8(6) . . . . ? C7 C8 C12 C13 -18.5(9) . . . . ? C9 C8 C12 C13 161.9(7) . . . . ? C7 C8 C12 C14 103.9(8) . . . . ? C9 C8 C12 C14 -75.7(8) . . . . ? C11 C10 C15 C16 66.1(12) . . . . ? C9 C10 C15 C16 -114.1(11) . . . . ? C11 C10 C15 C17 -57.0(11) . . . . ? C9 C10 C15 C17 122.9(9) . . . . ? C9 N2 C19 C20 -176.6(5) . . . . ? C9 N2 C19 C18 2.2(11) . . . . ? C24 N3 C20 C21 0.2(9) . . . . ? C24 N3 C20 C19 -177.0(5) . . . . ? N2 C19 C20 N3 169.1(6) . . . . ? C18 C19 C20 N3 -9.8(9) . . . . ? N2 C19 C20 C21 -8.2(9) . . . . ? C18 C19 C20 C21 172.9(7) . . . . ? N3 C20 C21 C22 1.3(11) . . . . ? C19 C20 C21 C22 178.4(6) . . . . ? C20 C21 C22 C23 -2.5(11) . . . . ? C21 C22 C23 C24 2.3(11) . . . . ? C20 N3 C24 C23 -0.5(9) . . . . ? C20 N3 C24 C25 177.8(5) . . . . ? C22 C23 C24 N3 -0.8(10) . . . . ? C22 C23 C24 C25 -179.0(7) . . . . ? C27 N4 C25 C24 179.9(5) . . . . ? C27 N4 C25 C26 -1.9(10) . . . . ? N3 C24 C25 N4 179.9(6) . . . . ? C23 C24 C25 N4 -1.8(10) . . . . ? N3 C24 C25 C26 1.6(9) . . . . ? C23 C24 C25 C26 179.9(7) . . . . ? C25 N4 C27 C32 99.5(7) . . . . ? C25 N4 C27 C28 -87.3(7) . . . . ? C32 C27 C28 C29 -3.0(8) . . . . ? N4 C27 C28 C29 -176.1(5) . . . . ? C32 C27 C28 C33 175.1(6) . . . . ? N4 C27 C28 C33 2.0(8) . . . . ? C27 C28 C29 C30 2.6(9) . . . . ? C33 C28 C29 C30 -175.5(6) . . . . ? C28 C29 C30 C31 -0.1(8) . . . . ? C28 C29 C30 C39 177.5(5) . . . . ? C29 C30 C31 C32 -2.2(8) . . . . ? C39 C30 C31 C32 -179.7(5) . . . . ? C30 C31 C32 C27 1.9(9) . . . . ? C30 C31 C32 C36 -178.2(6) . . . . ? C28 C27 C32 C31 0.8(9) . . . . ? N4 C27 C32 C31 173.9(5) . . . . ? C28 C27 C32 C36 -179.1(6) . . . . ? N4 C27 C32 C36 -6.0(9) . . . . ? C27 C28 C33 C34 -76.2(9) . . . . ? C29 C28 C33 C34 101.8(8) . . . . ? C27 C28 C33 C35 158.8(8) . . . . ? C29 C28 C33 C35 -23.1(10) . . . . ? C31 C32 C36 C38 -65.0(12) . . . . ? C27 C32 C36 C38 115.0(10) . . . . ? C31 C32 C36 C37 67.3(11) . . . . ? C27 C32 C36 C37 -112.8(10) . . . . ? C31 C30 C39 C43 -130.2(6) . . . . ? C29 C30 C39 C43 52.4(7) . . . . ? C31 C30 C39 C40 51.9(8) . . . . ? C29 C30 C39 C40 -125.6(6) . . . . ? C43 C39 C40 C41 -2.3(9) . . . . ? C30 C39 C40 C41 175.8(5) . . . . ? C39 C40 C41 C42 1.1(9) . . . . ? C43 N5 C42 C41 -1.3(8) . . . . ? Co1 N5 C42 C41 177.1(5) 1_546 . . . ? C40 C41 C42 N5 0.8(10) . . . . ? C42 N5 C43 C39 -0.1(8) . . . . ? Co1 N5 C43 C39 -178.6(4) 1_546 . . . ? C40 C39 C43 N5 1.9(9) . . . . ? C30 C39 C43 N5 -176.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.804 _refine_diff_density_min -0.420 _refine_diff_density_rms 0.097 ########### data_1b _database_code_depnum_ccdc_archive 'CCDC 754689' #TrackingRef 'Co-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H100 Cl2 Co N12 O6' _chemical_formula_weight 1539.62 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.3682(18) _cell_length_b 13.489(3) _cell_length_c 19.188(4) _cell_angle_alpha 98.737(3) _cell_angle_beta 91.191(4) _cell_angle_gamma 97.732(4) _cell_volume 2372.7(9) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour pink _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 815 _exptl_absorpt_coefficient_mu 0.289 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9312 _exptl_absorpt_correction_T_max 0.9444 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11829 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0737 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.44 _diffrn_reflns_theta_max 25.05 _reflns_number_total 8080 _reflns_number_gt 5327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1642P)^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 8080 _refine_ls_number_parameters 529 _refine_ls_number_restraints 42 _refine_ls_R_factor_all 0.1192 _refine_ls_R_factor_gt 0.0807 _refine_ls_wR_factor_ref 0.2398 _refine_ls_wR_factor_gt 0.2086 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 0.995 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co Co 0.5000 0.0000 -0.5000 0.0360(2) Uani 1 2 d S . . N1 N 0.6976(3) -0.0231(2) -0.44678(15) 0.0401(7) Uani 1 1 d . . . N2 N 0.8863(4) 0.1123(2) -0.03878(16) 0.0465(8) Uani 1 1 d . . . N3 N 0.7960(4) 0.2736(2) 0.11273(16) 0.0450(8) Uani 1 1 d . . . N4 N 0.7257(4) 0.3748(2) 0.28757(16) 0.0440(8) Uani 1 1 d . . . N5 N 0.4150(3) 0.8408(2) 0.49641(15) 0.0393(7) Uani 1 1 d . . . N6 N 0.3433(6) 0.0517(4) -0.3476(2) 0.0820(14) Uani 1 1 d . . . O1 O 0.4043(4) 0.0387(2) -0.40074(15) 0.0671(9) Uani 1 1 d . . . O2 O 0.3161(12) -0.0039(7) -0.3095(3) 0.218(4) Uani 1 1 d . . . O3 O 0.2782(7) 0.1340(4) -0.3425(3) 0.141(2) Uani 1 1 d . . . C1 C 0.8025(4) -0.0701(3) -0.4796(2) 0.0450(9) Uani 1 1 d . . . H1A H 0.7896 -0.0955 -0.5275 0.054 Uiso 1 1 calc R . . C2 C 0.9270(5) -0.0814(3) -0.4446(2) 0.0549(11) Uani 1 1 d . . . H2A H 0.9963 -0.1146 -0.4687 0.066 Uiso 1 1 calc R . . C3 C 0.9497(5) -0.0441(3) -0.3740(2) 0.0482(9) Uani 1 1 d . . . H3A H 1.0356 -0.0497 -0.3506 0.058 Uiso 1 1 calc R . . C4 C 0.8430(4) 0.0024(3) -0.33765(18) 0.0411(9) Uani 1 1 d . . . C5 C 0.7207(4) 0.0121(3) -0.37726(19) 0.0430(9) Uani 1 1 d . . . H5A H 0.6501 0.0452 -0.3541 0.052 Uiso 1 1 calc R . . C6 C 0.8529(4) 0.0362(3) -0.26057(19) 0.0423(9) Uani 1 1 d . . . C7 C 0.7408(5) 0.0008(3) -0.21947(19) 0.0466(9) Uani 1 1 d . . . H7A H 0.6595 -0.0399 -0.2415 0.056 Uiso 1 1 calc R . . C8 C 0.7490(5) 0.0259(3) -0.1457(2) 0.0476(9) Uani 1 1 d . . . C9 C 0.8709(5) 0.0910(3) -0.11389(19) 0.0436(9) Uani 1 1 d . . . C10 C 0.9842(5) 0.1288(3) -0.1541(2) 0.0470(9) Uani 1 1 d . . . C11 C 0.9720(5) 0.0987(3) -0.2273(2) 0.0456(9) Uani 1 1 d . . . H11A H 1.0466 0.1216 -0.2546 0.055 Uiso 1 1 calc R . . C12 C 0.6309(6) -0.0192(4) -0.1014(2) 0.0649(12) Uani 1 1 d . . . H12A H 0.6143 0.0345 -0.0632 0.078 Uiso 1 1 calc R . . C13 C 0.6755(9) -0.1022(6) -0.0687(4) 0.125(3) Uani 1 1 d . . . H13A H 0.7626 -0.0782 -0.0405 0.188 Uiso 1 1 calc R . . H13B H 0.6922 -0.1564 -0.1049 0.188 Uiso 1 1 calc R . . H13C H 0.6009 -0.1264 -0.0394 0.188 Uiso 1 1 calc R . . C14 C 0.4838(7) -0.0567(7) -0.1434(4) 0.114(2) Uani 1 1 d . . . H14A H 0.4143 -0.0835 -0.1127 0.171 Uiso 1 1 calc R . . H14B H 0.4968 -0.1085 -0.1820 0.171 Uiso 1 1 calc R . . H14C H 0.4501 -0.0009 -0.1614 0.171 Uiso 1 1 calc R . . C15 C 1.1141(6) 0.1993(3) -0.1197(2) 0.0665(13) Uani 1 1 d . . . H15A H 1.0950 0.2184 -0.0698 0.080 Uiso 1 1 calc R . . C16 C 1.2457(8) 0.1453(7) -0.1233(5) 0.138(3) Uani 1 1 d . . . H16A H 1.2227 0.0810 -0.1077 0.207 Uiso 1 1 calc R . . H16B H 1.3223 0.1857 -0.0935 0.207 Uiso 1 1 calc R . . H16C H 1.2758 0.1351 -0.1711 0.207 Uiso 1 1 calc R . . C17 C 1.1424(11) 0.2953(5) -0.1518(6) 0.166(5) Uani 1 1 d . . . H17A H 1.0620 0.3324 -0.1444 0.249 Uiso 1 1 calc R . . H17B H 1.1550 0.2783 -0.2015 0.249 Uiso 1 1 calc R . . H17C H 1.2281 0.3361 -0.1299 0.249 Uiso 1 1 calc R . . C18 C 0.8312(5) 0.1840(3) -0.00347(19) 0.0482(10) Uani 1 1 d . . . C19 C 0.7506(8) 0.2563(4) -0.0331(3) 0.091(2) Uani 1 1 d . . . H19A H 0.7481 0.2419 -0.0837 0.136 Uiso 1 1 calc R . . H19B H 0.7975 0.3242 -0.0177 0.136 Uiso 1 1 calc R . . H19C H 0.6539 0.2498 -0.0170 0.136 Uiso 1 1 calc R . . C20 C 0.8544(5) 0.1970(3) 0.07582(19) 0.0443(9) Uani 1 1 d . . . C21 C 0.9271(5) 0.1328(3) 0.1074(2) 0.0541(11) Uani 1 1 d . . . H21A H 0.9684 0.0817 0.0805 0.065 Uiso 1 1 calc R . . C22 C 0.9374(6) 0.1461(4) 0.1802(2) 0.0732(15) Uani 1 1 d . . . H22A H 0.9855 0.1033 0.2029 0.088 Uiso 1 1 calc R . . C23 C 0.8760(6) 0.2234(3) 0.2194(2) 0.0622(13) Uani 1 1 d . . . H23A H 0.8813 0.2331 0.2685 0.075 Uiso 1 1 calc R . . C24 C 0.8064(5) 0.2858(3) 0.18307(19) 0.0453(9) Uani 1 1 d . . . C25 C 0.7346(5) 0.3709(3) 0.2215(2) 0.0487(10) Uani 1 1 d . . . C26 C 0.6805(7) 0.4424(4) 0.1779(2) 0.0838(18) Uani 1 1 d . . . H26A H 0.6366 0.4925 0.2078 0.126 Uiso 1 1 calc R . . H26B H 0.6106 0.4054 0.1429 0.126 Uiso 1 1 calc R . . H26C H 0.7597 0.4752 0.1551 0.126 Uiso 1 1 calc R . . C27 C 0.6538(5) 0.4498(2) 0.32880(19) 0.0419(9) Uani 1 1 d . . . C28 C 0.7336(4) 0.5430(3) 0.35905(19) 0.0438(9) Uani 1 1 d . . . C29 C 0.6601(4) 0.6112(2) 0.40239(19) 0.0422(9) Uani 1 1 d . . . H29A H 0.7103 0.6735 0.4227 0.051 Uiso 1 1 calc R . . C30 C 0.5150(4) 0.5891(2) 0.41596(19) 0.0413(9) Uani 1 1 d . . . C31 C 0.4416(4) 0.4941(2) 0.3862(2) 0.0441(9) Uani 1 1 d . . . H31A H 0.3451 0.4777 0.3956 0.053 Uiso 1 1 calc R . . C32 C 0.5087(5) 0.4241(2) 0.34304(19) 0.0441(9) Uani 1 1 d . . . C33 C 0.8930(5) 0.5697(3) 0.3464(2) 0.0565(11) Uani 1 1 d . . . H33A H 0.9055 0.5475 0.2961 0.068 Uiso 1 1 calc R . . C34 C 0.9856(6) 0.5109(5) 0.3869(4) 0.102(2) Uani 1 1 d . . . H34A H 0.9501 0.4399 0.3764 0.153 Uiso 1 1 calc R . . H34B H 0.9813 0.5334 0.4366 0.153 Uiso 1 1 calc R . . H34C H 1.0837 0.5224 0.3731 0.153 Uiso 1 1 calc R . . C35 C 0.9477(7) 0.6832(4) 0.3613(4) 0.0935(19) Uani 1 1 d . . . H35A H 1.0485 0.6944 0.3521 0.140 Uiso 1 1 calc R . . H35B H 0.9337 0.7088 0.4098 0.140 Uiso 1 1 calc R . . H35C H 0.8952 0.7178 0.3313 0.140 Uiso 1 1 calc R . . C36 C 0.4216(5) 0.3222(3) 0.3099(2) 0.0591(12) Uani 1 1 d . . . H36A H 0.4896 0.2776 0.2897 0.071 Uiso 1 1 calc R . . C37 C 0.3379(9) 0.2708(4) 0.3659(4) 0.109(2) Uani 1 1 d . . . H37A H 0.2871 0.2065 0.3443 0.163 Uiso 1 1 calc R . . H37B H 0.2701 0.3131 0.3863 0.163 Uiso 1 1 calc R . . H37C H 0.4041 0.2607 0.4022 0.163 Uiso 1 1 calc R . . C38 C 0.3166(11) 0.3309(6) 0.2530(4) 0.151(4) Uani 1 1 d . . . H38A H 0.3661 0.3627 0.2171 0.227 Uiso 1 1 calc R . . H38B H 0.2454 0.3711 0.2722 0.227 Uiso 1 1 calc R . . H38C H 0.2702 0.2646 0.2327 0.227 Uiso 1 1 calc R . . C39 C 0.4381(4) 0.6642(2) 0.45999(19) 0.0402(8) Uani 1 1 d . . . C40 C 0.3292(5) 0.6362(3) 0.5036(2) 0.0511(10) Uani 1 1 d . . . H40A H 0.3007 0.5684 0.5070 0.061 Uiso 1 1 calc R . . C41 C 0.2637(5) 0.7119(3) 0.5421(3) 0.0630(12) Uani 1 1 d . . . H41A H 0.1885 0.6951 0.5709 0.076 Uiso 1 1 calc R . . C42 C 0.3102(5) 0.8118(3) 0.5376(2) 0.0522(10) Uani 1 1 d . . . H42A H 0.2661 0.8613 0.5646 0.063 Uiso 1 1 calc R . . C43 C 0.4767(4) 0.7674(2) 0.45813(19) 0.0406(8) Uani 1 1 d . . . H43A H 0.5495 0.7864 0.4286 0.049 Uiso 1 1 calc R . . C44 C 0.391(4) 0.660(5) 0.2428(17) 0.26(2) Uani 0.25 1 d PDU . . H44A H 0.3905 0.7328 0.2550 0.310 Uiso 0.25 1 calc PR . . H44B H 0.4502 0.6378 0.2778 0.310 Uiso 0.25 1 calc PR . . Cl1 Cl 0.4532(13) 0.6294(9) 0.1576(6) 0.163(4) Uani 0.25 1 d PDU . . Cl2 Cl 0.215(2) 0.5940(17) 0.2358(11) 0.267(8) Uani 0.25 1 d PDU . . C45 C 0.186(3) 0.368(2) 0.0703(17) 0.117(9) Uani 0.25 1 d PDU . . H45A H 0.1422 0.3018 0.0474 0.141 Uiso 0.25 1 calc PR . . H45B H 0.2011 0.3655 0.1200 0.141 Uiso 0.25 1 calc PR . . Cl3 Cl 0.350(2) 0.4001(18) 0.0340(13) 0.298(10) Uani 0.25 1 d PDU . . Cl4 Cl 0.070(3) 0.454(2) 0.0613(17) 0.370(14) Uani 0.25 1 d PDU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co 0.0505(5) 0.0283(3) 0.0298(4) 0.0006(2) 0.0041(3) 0.0112(3) N1 0.054(2) 0.0339(14) 0.0326(16) 0.0024(11) 0.0019(14) 0.0095(13) N2 0.056(2) 0.0504(17) 0.0330(16) 0.0006(13) 0.0071(14) 0.0136(15) N3 0.061(2) 0.0398(15) 0.0360(17) 0.0023(12) 0.0081(15) 0.0175(15) N4 0.057(2) 0.0378(15) 0.0371(17) -0.0027(12) 0.0075(14) 0.0142(14) N5 0.048(2) 0.0329(14) 0.0378(16) 0.0020(12) 0.0039(14) 0.0124(13) N6 0.099(4) 0.100(3) 0.039(2) 0.008(2) 0.003(2) -0.009(3) O1 0.100(3) 0.0707(18) 0.0341(16) -0.0005(13) 0.0290(16) 0.0294(18) O2 0.309(11) 0.244(8) 0.096(4) 0.092(5) -0.002(5) -0.052(7) O3 0.167(5) 0.122(4) 0.141(5) -0.005(3) 0.051(4) 0.068(4) C1 0.052(3) 0.0480(19) 0.0346(19) 0.0004(15) 0.0060(17) 0.0133(18) C2 0.051(3) 0.070(3) 0.044(2) -0.0006(19) 0.0125(19) 0.019(2) C3 0.043(2) 0.060(2) 0.043(2) 0.0035(17) 0.0020(17) 0.0135(19) C4 0.052(2) 0.0388(17) 0.0334(19) 0.0060(14) 0.0029(16) 0.0093(16) C5 0.052(2) 0.0431(18) 0.036(2) 0.0035(15) 0.0069(17) 0.0169(17) C6 0.048(2) 0.0457(19) 0.0353(19) 0.0056(15) 0.0030(17) 0.0147(17) C7 0.048(2) 0.053(2) 0.039(2) 0.0028(16) 0.0041(17) 0.0104(18) C8 0.053(3) 0.053(2) 0.039(2) 0.0047(16) 0.0085(18) 0.0170(19) C9 0.057(3) 0.0406(18) 0.0352(19) 0.0017(15) 0.0020(18) 0.0181(17) C10 0.053(3) 0.0473(19) 0.040(2) -0.0007(16) 0.0049(18) 0.0104(18) C11 0.051(3) 0.0450(19) 0.040(2) 0.0025(16) 0.0064(18) 0.0071(18) C12 0.068(3) 0.072(3) 0.050(3) 0.002(2) 0.013(2) 0.000(2) C13 0.124(6) 0.135(6) 0.136(6) 0.085(5) 0.036(5) 0.007(5) C14 0.063(4) 0.178(7) 0.108(5) 0.051(5) 0.016(4) 0.006(4) C15 0.074(4) 0.071(3) 0.046(3) -0.006(2) 0.009(2) -0.004(3) C16 0.077(5) 0.145(7) 0.177(9) 0.003(6) -0.042(5) -0.006(5) C17 0.180(9) 0.082(4) 0.219(10) 0.053(5) -0.073(8) -0.063(5) C18 0.064(3) 0.0465(19) 0.035(2) 0.0014(16) 0.0048(18) 0.0166(19) C19 0.149(6) 0.091(4) 0.046(3) 0.005(2) 0.001(3) 0.073(4) C20 0.054(3) 0.0403(18) 0.038(2) -0.0015(15) 0.0080(17) 0.0124(17) C21 0.069(3) 0.056(2) 0.040(2) -0.0036(17) 0.0018(19) 0.032(2) C22 0.116(4) 0.067(3) 0.047(2) 0.002(2) -0.006(3) 0.058(3) C23 0.096(4) 0.062(2) 0.034(2) -0.0005(18) 0.002(2) 0.039(2) C24 0.059(3) 0.0375(17) 0.040(2) -0.0009(15) 0.0028(18) 0.0160(17) C25 0.067(3) 0.0401(18) 0.042(2) 0.0029(16) 0.0091(19) 0.0193(18) C26 0.145(5) 0.073(3) 0.048(3) 0.008(2) 0.014(3) 0.066(3) C27 0.056(3) 0.0339(16) 0.0362(19) -0.0002(14) 0.0016(17) 0.0149(17) C28 0.052(3) 0.0392(18) 0.040(2) 0.0031(15) 0.0080(17) 0.0088(17) C29 0.048(2) 0.0288(16) 0.047(2) -0.0032(14) 0.0051(17) 0.0029(15) C30 0.056(3) 0.0299(16) 0.039(2) 0.0001(14) 0.0042(17) 0.0132(16) C31 0.044(2) 0.0356(17) 0.051(2) 0.0011(15) 0.0056(18) 0.0035(16) C32 0.057(3) 0.0334(17) 0.041(2) -0.0011(14) 0.0021(18) 0.0118(17) C33 0.058(3) 0.049(2) 0.061(3) 0.0000(19) 0.015(2) 0.011(2) C34 0.052(4) 0.105(4) 0.155(6) 0.044(4) -0.002(4) 0.009(3) C35 0.077(4) 0.059(3) 0.137(6) 0.003(3) 0.034(4) -0.008(3) C36 0.061(3) 0.041(2) 0.069(3) -0.0132(19) 0.005(2) 0.0082(19) C37 0.140(6) 0.061(3) 0.113(5) 0.016(3) 0.000(4) -0.030(4) C38 0.202(9) 0.106(5) 0.120(6) 0.011(4) -0.087(7) -0.049(5) C39 0.047(2) 0.0348(17) 0.0385(19) 0.0006(14) 0.0034(17) 0.0095(16) C40 0.061(3) 0.0369(18) 0.054(2) 0.0026(16) 0.011(2) 0.0080(18) C41 0.063(3) 0.047(2) 0.076(3) 0.001(2) 0.035(2) 0.005(2) C42 0.058(3) 0.0416(19) 0.057(2) -0.0017(17) 0.018(2) 0.0150(19) C43 0.052(2) 0.0330(16) 0.0371(19) 0.0025(14) 0.0052(16) 0.0097(16) C44 0.26(2) 0.26(2) 0.26(2) 0.040(4) 0.0108(14) 0.036(3) Cl1 0.163(4) 0.164(4) 0.164(4) 0.0258(12) 0.0067(10) 0.0240(11) Cl2 0.267(8) 0.267(8) 0.267(8) 0.0416(16) 0.0114(11) 0.0375(15) C45 0.117(9) 0.117(9) 0.117(9) 0.0183(17) 0.0048(11) 0.0161(16) Cl3 0.298(10) 0.298(10) 0.298(10) 0.0464(18) 0.0122(11) 0.0413(17) Cl4 0.370(14) 0.370(14) 0.370(14) 0.058(2) 0.0156(12) 0.051(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 Co O1 2.144(3) 2_654 ? Co O1 2.144(3) . ? Co N1 2.177(3) . ? Co N1 2.177(3) 2_654 ? Co N5 2.178(3) 1_544 ? Co N5 2.178(3) 2_665 ? N1 C5 1.349(4) . ? N1 C1 1.355(5) . ? N2 C18 1.269(5) . ? N2 C9 1.427(5) . ? N3 C24 1.335(5) . ? N3 C20 1.347(4) . ? N4 C25 1.267(5) . ? N4 C27 1.438(4) . ? N5 C42 1.329(5) . ? N5 C43 1.344(4) . ? N5 Co 2.178(3) 1_566 ? N6 O2 1.133(7) . ? N6 O1 1.181(5) . ? N6 O3 1.330(7) . ? C1 C2 1.372(6) . ? C1 H1A 0.9300 . ? C2 C3 1.373(5) . ? C2 H2A 0.9300 . ? C3 C4 1.394(5) . ? C3 H3A 0.9300 . ? C4 C5 1.394(5) . ? C4 C6 1.477(5) . ? C5 H5A 0.9300 . ? C6 C11 1.385(6) . ? C6 C7 1.402(6) . ? C7 C8 1.403(5) . ? C7 H7A 0.9300 . ? C8 C9 1.410(6) . ? C8 C12 1.526(6) . ? C9 C10 1.410(6) . ? C10 C11 1.400(5) . ? C10 C15 1.512(6) . ? C11 H11A 0.9300 . ? C12 C13 1.467(8) . ? C12 C14 1.564(9) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.511(9) . ? C15 C17 1.511(8) . ? C15 H15A 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.482(6) . ? C18 C20 1.512(5) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 C21 1.372(6) . ? C21 C22 1.380(6) . ? C21 H21A 0.9300 . ? C22 C23 1.388(6) . ? C22 H22A 0.9300 . ? C23 C24 1.387(6) . ? C23 H23A 0.9300 . ? C24 C25 1.511(5) . ? C25 C26 1.498(6) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C32 1.400(6) . ? C27 C28 1.409(5) . ? C28 C29 1.405(5) . ? C28 C33 1.522(6) . ? C29 C30 1.390(6) . ? C29 H29A 0.9300 . ? C30 C31 1.402(5) . ? C30 C39 1.490(5) . ? C31 C32 1.384(5) . ? C31 H31A 0.9300 . ? C32 C36 1.540(5) . ? C33 C34 1.526(7) . ? C33 C35 1.530(6) . ? C33 H33A 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.483(9) . ? C36 C37 1.539(8) . ? C36 H36A 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C40 1.382(6) . ? C39 C43 1.397(5) . ? C40 C41 1.387(6) . ? C40 H40A 0.9300 . ? C41 C42 1.376(6) . ? C41 H41A 0.9300 . ? C42 H42A 0.9300 . ? C43 H43A 0.9300 . ? C44 Cl1 1.76(2) . ? C44 Cl2 1.76(2) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 Cl4 1.712(18) . ? C45 Cl3 1.732(18) . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Co O1 180.0 2_654 . ? O1 Co N1 88.90(12) 2_654 . ? O1 Co N1 91.10(12) . . ? O1 Co N1 91.10(12) 2_654 2_654 ? O1 Co N1 88.90(12) . 2_654 ? N1 Co N1 180.00(13) . 2_654 ? O1 Co N5 88.97(12) 2_654 1_544 ? O1 Co N5 91.03(12) . 1_544 ? N1 Co N5 90.29(11) . 1_544 ? N1 Co N5 89.71(11) 2_654 1_544 ? O1 Co N5 91.03(12) 2_654 2_665 ? O1 Co N5 88.97(12) . 2_665 ? N1 Co N5 89.71(11) . 2_665 ? N1 Co N5 90.29(11) 2_654 2_665 ? N5 Co N5 180.0 1_544 2_665 ? C5 N1 C1 116.8(3) . . ? C5 N1 Co 119.4(2) . . ? C1 N1 Co 123.8(2) . . ? C18 N2 C9 121.8(3) . . ? C24 N3 C20 118.4(3) . . ? C25 N4 C27 121.3(3) . . ? C42 N5 C43 117.0(3) . . ? C42 N5 Co 121.4(2) . 1_566 ? C43 N5 Co 121.2(3) . 1_566 ? O2 N6 O1 127.7(7) . . ? O2 N6 O3 119.1(8) . . ? O1 N6 O3 111.7(5) . . ? N6 O1 Co 173.9(4) . . ? N1 C1 C2 122.1(3) . . ? N1 C1 H1A 118.9 . . ? C2 C1 H1A 118.9 . . ? C1 C2 C3 120.4(4) . . ? C1 C2 H2A 119.8 . . ? C3 C2 H2A 119.8 . . ? C2 C3 C4 119.4(4) . . ? C2 C3 H3A 120.3 . . ? C4 C3 H3A 120.3 . . ? C5 C4 C3 116.6(3) . . ? C5 C4 C6 120.4(3) . . ? C3 C4 C6 122.9(3) . . ? N1 C5 C4 124.6(3) . . ? N1 C5 H5A 117.7 . . ? C4 C5 H5A 117.7 . . ? C11 C6 C7 118.9(3) . . ? C11 C6 C4 122.0(4) . . ? C7 C6 C4 119.1(3) . . ? C6 C7 C8 121.2(4) . . ? C6 C7 H7A 119.4 . . ? C8 C7 H7A 119.4 . . ? C7 C8 C9 118.1(4) . . ? C7 C8 C12 120.5(4) . . ? C9 C8 C12 121.3(4) . . ? C10 C9 C8 121.8(3) . . ? C10 C9 N2 118.8(4) . . ? C8 C9 N2 119.2(4) . . ? C11 C10 C9 117.5(4) . . ? C11 C10 C15 121.0(4) . . ? C9 C10 C15 121.5(4) . . ? C6 C11 C10 122.4(4) . . ? C6 C11 H11A 118.8 . . ? C10 C11 H11A 118.8 . . ? C13 C12 C8 111.7(5) . . ? C13 C12 C14 109.3(5) . . ? C8 C12 C14 113.6(4) . . ? C13 C12 H12A 107.3 . . ? C8 C12 H12A 107.3 . . ? C14 C12 H12A 107.3 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C17 110.5(7) . . ? C16 C15 C10 110.3(4) . . ? C17 C15 C10 112.4(5) . . ? C16 C15 H15A 107.8 . . ? C17 C15 H15A 107.8 . . ? C10 C15 H15A 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N2 C18 C19 125.9(4) . . ? N2 C18 C20 116.1(3) . . ? C19 C18 C20 118.0(3) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 C21 122.8(3) . . ? N3 C20 C18 115.6(3) . . ? C21 C20 C18 121.6(3) . . ? C20 C21 C22 118.3(4) . . ? C20 C21 H21A 120.8 . . ? C22 C21 H21A 120.8 . . ? C21 C22 C23 119.9(4) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 117.9(4) . . ? C24 C23 H23A 121.0 . . ? C22 C23 H23A 121.0 . . ? N3 C24 C23 122.6(3) . . ? N3 C24 C25 115.9(3) . . ? C23 C24 C25 121.5(3) . . ? N4 C25 C26 126.2(3) . . ? N4 C25 C24 116.7(3) . . ? C26 C25 C24 117.1(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C32 C27 C28 121.8(3) . . ? C32 C27 N4 118.5(3) . . ? C28 C27 N4 119.4(4) . . ? C29 C28 C27 117.2(4) . . ? C29 C28 C33 120.7(3) . . ? C27 C28 C33 122.1(3) . . ? C30 C29 C28 122.4(3) . . ? C30 C29 H29A 118.8 . . ? C28 C29 H29A 118.8 . . ? C29 C30 C31 118.1(3) . . ? C29 C30 C39 121.4(3) . . ? C31 C30 C39 120.5(4) . . ? C32 C31 C30 121.9(4) . . ? C32 C31 H31A 119.1 . . ? C30 C31 H31A 119.1 . . ? C31 C32 C27 118.6(3) . . ? C31 C32 C36 119.7(4) . . ? C27 C32 C36 121.7(3) . . ? C28 C33 C34 111.4(4) . . ? C28 C33 C35 114.1(4) . . ? C34 C33 C35 110.9(5) . . ? C28 C33 H33A 106.7 . . ? C34 C33 H33A 106.7 . . ? C35 C33 H33A 106.7 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C38 C36 C37 107.7(6) . . ? C38 C36 C32 113.7(4) . . ? C37 C36 C32 111.1(4) . . ? C38 C36 H36A 108.1 . . ? C37 C36 H36A 108.1 . . ? C32 C36 H36A 108.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C43 117.8(3) . . ? C40 C39 C30 122.7(3) . . ? C43 C39 C30 119.5(3) . . ? C39 C40 C41 118.2(3) . . ? C39 C40 H40A 120.9 . . ? C41 C40 H40A 120.9 . . ? C42 C41 C40 119.9(4) . . ? C42 C41 H41A 120.1 . . ? C40 C41 H41A 120.1 . . ? N5 C42 C41 123.1(3) . . ? N5 C42 H42A 118.4 . . ? C41 C42 H42A 118.4 . . ? N5 C43 C39 123.9(4) . . ? N5 C43 H43A 118.0 . . ? C39 C43 H43A 118.0 . . ? Cl1 C44 Cl2 102.5(14) . . ? Cl1 C44 H44A 111.3 . . ? Cl2 C44 H44A 111.3 . . ? Cl1 C44 H44B 111.3 . . ? Cl2 C44 H44B 111.3 . . ? H44A C44 H44B 109.2 . . ? Cl4 C45 Cl3 112.1(14) . . ? Cl4 C45 H45A 109.2 . . ? Cl3 C45 H45A 109.2 . . ? Cl4 C45 H45B 109.2 . . ? Cl3 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? 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 O1 Co N1 C5 165.1(3) 2_654 . . . ? O1 Co N1 C5 -14.9(3) . . . . ? N1 Co N1 C5 11(15) 2_654 . . . ? N5 Co N1 C5 -105.9(3) 1_544 . . . ? N5 Co N1 C5 74.1(3) 2_665 . . . ? O1 Co N1 C1 -13.8(3) 2_654 . . . ? O1 Co N1 C1 166.2(3) . . . . ? N1 Co N1 C1 -168(15) 2_654 . . . ? N5 Co N1 C1 75.2(3) 1_544 . . . ? N5 Co N1 C1 -104.8(3) 2_665 . . . ? O2 N6 O1 Co 47(4) . . . . ? O3 N6 O1 Co -118(3) . . . . ? O1 Co O1 N6 -29(16) 2_654 . . . ? N1 Co O1 N6 -110(3) . . . . ? N1 Co O1 N6 70(3) 2_654 . . . ? N5 Co O1 N6 -20(3) 1_544 . . . ? N5 Co O1 N6 160(3) 2_665 . . . ? C5 N1 C1 C2 -0.3(5) . . . . ? Co N1 C1 C2 178.6(3) . . . . ? N1 C1 C2 C3 -0.5(6) . . . . ? C1 C2 C3 C4 2.2(6) . . . . ? C2 C3 C4 C5 -3.0(6) . . . . ? C2 C3 C4 C6 174.2(4) . . . . ? C1 N1 C5 C4 -0.7(5) . . . . ? Co N1 C5 C4 -179.7(3) . . . . ? C3 C4 C5 N1 2.3(5) . . . . ? C6 C4 C5 N1 -175.0(3) . . . . ? C5 C4 C6 C11 -130.0(4) . . . . ? C3 C4 C6 C11 52.8(5) . . . . ? C5 C4 C6 C7 52.4(5) . . . . ? C3 C4 C6 C7 -124.7(4) . . . . ? C11 C6 C7 C8 -1.5(5) . . . . ? C4 C6 C7 C8 176.2(3) . . . . ? C6 C7 C8 C9 2.4(5) . . . . ? C6 C7 C8 C12 -175.7(4) . . . . ? C7 C8 C9 C10 -1.5(5) . . . . ? C12 C8 C9 C10 176.6(4) . . . . ? C7 C8 C9 N2 -175.9(3) . . . . ? C12 C8 C9 N2 2.2(5) . . . . ? C18 N2 C9 C10 98.1(5) . . . . ? C18 N2 C9 C8 -87.3(5) . . . . ? C8 C9 C10 C11 -0.4(5) . . . . ? N2 C9 C10 C11 174.0(3) . . . . ? C8 C9 C10 C15 179.5(4) . . . . ? N2 C9 C10 C15 -6.0(5) . . . . ? C7 C6 C11 C10 -0.6(5) . . . . ? C4 C6 C11 C10 -178.1(3) . . . . ? C9 C10 C11 C6 1.5(5) . . . . ? C15 C10 C11 C6 -178.5(4) . . . . ? C7 C8 C12 C13 102.0(6) . . . . ? C9 C8 C12 C13 -76.0(6) . . . . ? C7 C8 C12 C14 -22.2(6) . . . . ? C9 C8 C12 C14 159.8(5) . . . . ? C11 C10 C15 C16 -70.6(6) . . . . ? C9 C10 C15 C16 109.4(6) . . . . ? C11 C10 C15 C17 53.2(7) . . . . ? C9 C10 C15 C17 -126.8(6) . . . . ? C9 N2 C18 C19 -2.4(7) . . . . ? C9 N2 C18 C20 179.2(4) . . . . ? C24 N3 C20 C21 -1.7(6) . . . . ? C24 N3 C20 C18 176.6(4) . . . . ? N2 C18 C20 N3 179.7(4) . . . . ? C19 C18 C20 N3 1.2(6) . . . . ? N2 C18 C20 C21 -1.9(6) . . . . ? C19 C18 C20 C21 179.5(5) . . . . ? N3 C20 C21 C22 1.6(7) . . . . ? C18 C20 C21 C22 -176.6(4) . . . . ? C20 C21 C22 C23 -0.5(8) . . . . ? C21 C22 C23 C24 -0.5(8) . . . . ? C20 N3 C24 C23 0.6(6) . . . . ? C20 N3 C24 C25 -178.1(4) . . . . ? C22 C23 C24 N3 0.5(7) . . . . ? C22 C23 C24 C25 179.1(5) . . . . ? C27 N4 C25 C26 2.7(7) . . . . ? C27 N4 C25 C24 -177.1(3) . . . . ? N3 C24 C25 N4 170.4(4) . . . . ? C23 C24 C25 N4 -8.3(6) . . . . ? N3 C24 C25 C26 -9.5(6) . . . . ? C23 C24 C25 C26 171.8(5) . . . . ? C25 N4 C27 C32 94.7(5) . . . . ? C25 N4 C27 C28 -91.2(5) . . . . ? C32 C27 C28 C29 -2.2(5) . . . . ? N4 C27 C28 C29 -176.2(3) . . . . ? C32 C27 C28 C33 177.3(3) . . . . ? N4 C27 C28 C33 3.3(5) . . . . ? C27 C28 C29 C30 0.4(6) . . . . ? C33 C28 C29 C30 -179.1(3) . . . . ? C28 C29 C30 C31 1.4(5) . . . . ? C28 C29 C30 C39 -177.8(3) . . . . ? C29 C30 C31 C32 -1.4(6) . . . . ? C39 C30 C31 C32 177.7(3) . . . . ? C30 C31 C32 C27 -0.3(6) . . . . ? C30 C31 C32 C36 -178.1(4) . . . . ? C28 C27 C32 C31 2.2(5) . . . . ? N4 C27 C32 C31 176.2(3) . . . . ? C28 C27 C32 C36 179.9(4) . . . . ? N4 C27 C32 C36 -6.0(5) . . . . ? C29 C28 C33 C34 106.1(5) . . . . ? C27 C28 C33 C34 -73.4(5) . . . . ? C29 C28 C33 C35 -20.5(6) . . . . ? C27 C28 C33 C35 160.1(4) . . . . ? C31 C32 C36 C38 71.6(7) . . . . ? C27 C32 C36 C38 -106.1(6) . . . . ? C31 C32 C36 C37 -50.0(6) . . . . ? C27 C32 C36 C37 132.3(5) . . . . ? C29 C30 C39 C40 -146.3(4) . . . . ? C31 C30 C39 C40 34.6(6) . . . . ? C29 C30 C39 C43 33.3(5) . . . . ? C31 C30 C39 C43 -145.8(4) . . . . ? C43 C39 C40 C41 0.8(6) . . . . ? C30 C39 C40 C41 -179.6(4) . . . . ? C39 C40 C41 C42 -1.7(7) . . . . ? C43 N5 C42 C41 -0.2(6) . . . . ? Co N5 C42 C41 -173.2(4) 1_566 . . . ? C40 C41 C42 N5 1.4(8) . . . . ? C42 N5 C43 C39 -0.7(6) . . . . ? Co N5 C43 C39 172.3(3) 1_566 . . . ? C40 C39 C43 N5 0.4(6) . . . . ? C30 C39 C43 N5 -179.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.962 _diffrn_reflns_theta_full 25.05 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.896 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.093 ########## data_2 _database_code_depnum_ccdc_archive 'CCDC 754690' #TrackingRef 'Co-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H49 Cl5 Co2 N5' _chemical_formula_weight 930.98 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' 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 Orthorhombic _symmetry_space_group_name_H-M Cmcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x, y, -z+1/2' 'x, -y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x, y, -z-1/2' 'x, -y, z-1/2' '-x, y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' 'x+1/2, -y+1/2, z-1/2' '-x+1/2, y+1/2, z' _cell_length_a 23.382(3) _cell_length_b 22.002(3) _cell_length_c 21.936(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 11285(2) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3848 _exptl_absorpt_coefficient_mu 0.853 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7839 _exptl_absorpt_correction_T_max 0.8479 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29421 _diffrn_reflns_av_R_equivalents 0.0710 _diffrn_reflns_av_sigmaI/netI 0.0602 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.44 _reflns_number_total 5487 _reflns_number_gt 3082 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1325P)^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 5487 _refine_ls_number_parameters 267 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1075 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.2101 _refine_ls_wR_factor_gt 0.1901 _refine_ls_goodness_of_fit_ref 0.958 _refine_ls_restrained_S_all 0.958 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 1 0.000 0.000 -0.004 1816.3 101.8 2 0.500 0.500 -0.012 1809.8 102.6 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 0.30667(4) 0.33745(4) 0.2500 0.0434(3) Uani 1 2 d S . . Co2 Co 0.0000 0.45934(5) -0.07344(5) 0.0654(4) Uani 1 2 d S . . Cl1 Cl 0.39478(9) 0.38312(11) 0.2500 0.0818(7) Uani 1 2 d S . . Cl2 Cl 0.23863(10) 0.40894(9) 0.2500 0.0737(6) Uani 1 2 d S . . Cl3 Cl 0.0000 0.56397(10) -0.04303(10) 0.0714(6) Uani 1 2 d S . . Cl4 Cl 0.0000 0.35683(18) -0.0943(2) 0.1723(18) Uani 1 2 d S . . Cl5 Cl 0.0000 0.4613(3) -0.1842(2) 0.206(2) Uani 1 2 d S . . N1 N 0.09266(17) 0.46110(17) -0.07621(19) 0.0549(10) Uani 1 1 d . . . N2 N 0.30183(16) 0.30598(16) 0.15469(15) 0.0455(9) Uani 1 1 d . . . N3 N 0.3395(2) 0.2505(2) 0.2500 0.0483(13) Uani 1 2 d S . . C1 C 0.1244(2) 0.4308(2) -0.0352(2) 0.0485(11) Uani 1 1 d . . . H1 H 0.1053 0.4101 -0.0044 0.058 Uiso 1 1 calc R . . C2 C 0.18267(18) 0.42796(19) -0.03559(19) 0.0409(10) Uani 1 1 d . . . C3 C 0.2104(2) 0.4581(2) -0.0836(2) 0.0500(12) Uani 1 1 d . . . H3 H 0.2500 0.4561 -0.0876 0.060 Uiso 1 1 calc R . . C4 C 0.1787(2) 0.4903(3) -0.1241(2) 0.0654(15) Uani 1 1 d . . . H4 H 0.1965 0.5118 -0.1553 0.078 Uiso 1 1 calc R . . C5 C 0.1207(2) 0.4908(2) -0.1188(2) 0.0627(14) Uani 1 1 d . . . H5 H 0.0998 0.5134 -0.1469 0.075 Uiso 1 1 calc R . . C6 C 0.21490(18) 0.39602(18) 0.01278(18) 0.0394(10) Uani 1 1 d . . . C7 C 0.1877(2) 0.3532(2) 0.0506(2) 0.0524(12) Uani 1 1 d . . . H7 H 0.1494 0.3443 0.0438 0.063 Uiso 1 1 calc R . . C8 C 0.2158(2) 0.3239(2) 0.09727(19) 0.0511(12) Uani 1 1 d . . . C9 C 0.2730(2) 0.33675(19) 0.10686(18) 0.0441(11) Uani 1 1 d . . . C10 C 0.30232(19) 0.38044(19) 0.0717(2) 0.0459(11) Uani 1 1 d . . . C11 C 0.27157(19) 0.40810(19) 0.0261(2) 0.0473(11) Uani 1 1 d . . . H11 H 0.2902 0.4370 0.0024 0.057 Uiso 1 1 calc R . . C12 C 0.1835(3) 0.2778(3) 0.1359(3) 0.0829(19) Uani 1 1 d . . . H12 H 0.2081 0.2661 0.1700 0.100 Uiso 1 1 calc R . . C13 C 0.1298(3) 0.3022(4) 0.1612(3) 0.125(3) Uani 1 1 d . . . H13A H 0.1356 0.3435 0.1737 0.187 Uiso 1 1 calc R . . H13B H 0.1185 0.2782 0.1957 0.187 Uiso 1 1 calc R . . H13C H 0.1004 0.3006 0.1307 0.187 Uiso 1 1 calc R . . C14 C 0.1706(4) 0.2204(3) 0.0987(4) 0.133(3) Uani 1 1 d . . . H14A H 0.1487 0.2312 0.0632 0.199 Uiso 1 1 calc R . . H14B H 0.1492 0.1924 0.1232 0.199 Uiso 1 1 calc R . . H14C H 0.2059 0.2018 0.0862 0.199 Uiso 1 1 calc R . . C15 C 0.3632(2) 0.3978(2) 0.0834(2) 0.0636(14) Uani 1 1 d . . . H15 H 0.3776 0.3710 0.1157 0.076 Uiso 1 1 calc R . . C16 C 0.3666(3) 0.4623(3) 0.1071(3) 0.094(2) Uani 1 1 d . . . H16A H 0.3551 0.4900 0.0756 0.141 Uiso 1 1 calc R . . H16B H 0.4052 0.4711 0.1192 0.141 Uiso 1 1 calc R . . H16C H 0.3416 0.4666 0.1416 0.141 Uiso 1 1 calc R . . C17 C 0.4017(2) 0.3892(4) 0.0282(3) 0.107(2) Uani 1 1 d . . . H17A H 0.4047 0.3466 0.0189 0.160 Uiso 1 1 calc R . . H17B H 0.4390 0.4051 0.0370 0.160 Uiso 1 1 calc R . . H17C H 0.3857 0.4103 -0.0061 0.160 Uiso 1 1 calc R . . C18 C 0.3397(3) 0.2311(3) 0.0822(2) 0.086(2) Uani 1 1 d . . . H18A H 0.3254 0.2584 0.0517 0.129 Uiso 1 1 calc R . . H18B H 0.3203 0.1928 0.0791 0.129 Uiso 1 1 calc R . . H18C H 0.3800 0.2250 0.0761 0.129 Uiso 1 1 calc R . . C19 C 0.3299(2) 0.2573(2) 0.1430(2) 0.0560(13) Uani 1 1 d . . . C20 C 0.3517(2) 0.2237(2) 0.1978(2) 0.0529(12) Uani 1 1 d . . . C21 C 0.3786(3) 0.1670(2) 0.1963(3) 0.0766(17) Uani 1 1 d . . . H21 H 0.3875 0.1486 0.1593 0.092 Uiso 1 1 calc R . . C22 C 0.3915(4) 0.1393(4) 0.2500 0.084(3) Uani 1 2 d S . . H22 H 0.4092 0.1014 0.2500 0.100 Uiso 1 2 calc SR . . 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 0.0611(6) 0.0376(5) 0.0314(4) 0.000 0.000 0.0078(4) Co2 0.0407(6) 0.0748(8) 0.0808(8) -0.0027(6) 0.000 0.000 Cl1 0.0808(15) 0.0963(16) 0.0682(13) 0.000 0.000 -0.0220(12) Cl2 0.1044(16) 0.0693(13) 0.0476(10) 0.000 0.000 0.0409(11) Cl3 0.0553(11) 0.0815(14) 0.0776(14) -0.0001(10) 0.000 0.000 Cl4 0.117(3) 0.140(3) 0.260(5) -0.068(3) 0.000 0.000 Cl5 0.098(3) 0.375(8) 0.144(4) -0.015(4) 0.000 0.000 N1 0.051(2) 0.052(2) 0.062(3) 0.001(2) -0.002(2) 0.0003(19) N2 0.061(2) 0.044(2) 0.0317(19) -0.0031(16) -0.0009(18) 0.0041(18) N3 0.072(4) 0.040(3) 0.034(3) 0.000 0.000 0.004(3) C1 0.050(3) 0.050(3) 0.045(3) -0.002(2) -0.001(2) 0.001(2) C2 0.043(3) 0.042(2) 0.038(2) -0.0117(19) 0.0024(19) -0.0022(19) C3 0.036(2) 0.060(3) 0.054(3) 0.013(2) -0.003(2) 0.001(2) C4 0.053(3) 0.080(4) 0.063(3) 0.025(3) 0.002(3) -0.006(3) C5 0.055(3) 0.066(3) 0.067(4) 0.017(3) -0.015(3) -0.001(3) C6 0.048(3) 0.039(2) 0.032(2) -0.0049(17) 0.0039(19) 0.0010(19) C7 0.053(3) 0.069(3) 0.036(2) -0.001(2) -0.001(2) -0.009(2) C8 0.065(3) 0.058(3) 0.030(2) 0.000(2) 0.004(2) -0.017(2) C9 0.062(3) 0.040(2) 0.030(2) -0.0038(19) -0.001(2) 0.003(2) C10 0.051(3) 0.042(3) 0.044(3) -0.0006(19) 0.000(2) 0.005(2) C11 0.050(3) 0.048(3) 0.044(3) 0.007(2) 0.007(2) -0.003(2) C12 0.083(4) 0.109(5) 0.057(3) 0.033(3) -0.013(3) -0.034(4) C13 0.103(6) 0.193(9) 0.078(5) 0.010(5) 0.024(4) -0.058(6) C14 0.188(8) 0.086(5) 0.125(7) 0.022(5) 0.023(6) -0.065(6) C15 0.055(3) 0.070(4) 0.065(3) 0.024(3) -0.008(3) -0.001(3) C16 0.090(5) 0.078(4) 0.114(5) 0.007(4) -0.038(4) -0.018(3) C17 0.053(4) 0.157(7) 0.110(6) 0.014(5) 0.010(4) -0.005(4) C18 0.149(6) 0.067(4) 0.041(3) -0.019(3) 0.004(3) 0.027(4) C19 0.088(4) 0.045(3) 0.035(2) -0.010(2) 0.006(2) 0.007(3) C20 0.066(3) 0.044(3) 0.048(3) -0.004(2) 0.001(2) 0.012(2) C21 0.103(5) 0.060(4) 0.066(4) -0.006(3) 0.015(3) 0.029(3) C22 0.119(8) 0.063(5) 0.069(6) 0.000 0.000 0.051(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.061(5) . ? Co1 N2 2.205(3) . ? Co1 N2 2.205(3) 10_556 ? Co1 Cl2 2.2373(19) . ? Co1 Cl1 2.292(2) . ? Co2 N1 2.168(4) 12 ? Co2 N1 2.168(4) . ? Co2 Cl4 2.302(4) . ? Co2 Cl3 2.397(2) . ? Co2 Cl5 2.431(5) . ? Co2 Cl3 2.606(2) 9_565 ? Cl3 Co2 2.606(2) 9_565 ? N1 C5 1.316(6) . ? N1 C1 1.344(6) . ? N2 C19 1.283(6) . ? N2 C9 1.419(5) . ? N3 C20 1.318(5) . ? N3 C20 1.318(5) 10_556 ? C1 C2 1.363(6) . ? C1 H1 0.9300 . ? C2 C3 1.404(6) . ? C2 C6 1.479(6) . ? C3 C4 1.356(6) . ? C3 H3 0.9300 . ? C4 C5 1.362(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.383(6) . ? C6 C7 1.408(6) . ? C7 C8 1.375(6) . ? C7 H7 0.9300 . ? C8 C9 1.384(6) . ? C8 C12 1.522(7) . ? C9 C10 1.410(6) . ? C10 C11 1.375(6) . ? C10 C15 1.497(7) . ? C11 H11 0.9300 . ? C12 C13 1.473(9) . ? C12 C14 1.532(9) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.513(8) . ? C15 C17 1.520(8) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.472(6) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.499(6) . ? C20 C21 1.399(7) . ? C21 C22 1.360(7) . ? C21 H21 0.9300 . ? C22 C21 1.360(7) 10_556 ? C22 H22 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 N2 74.20(10) . . ? N3 Co1 N2 74.20(10) . 10_556 ? N2 Co1 N2 142.89(19) . 10_556 ? N3 Co1 Cl2 156.52(17) . . ? N2 Co1 Cl2 100.62(10) . . ? N2 Co1 Cl2 100.62(10) 10_556 . ? N3 Co1 Cl1 94.15(17) . . ? N2 Co1 Cl1 100.59(10) . . ? N2 Co1 Cl1 100.60(10) 10_556 . ? Cl2 Co1 Cl1 109.33(9) . . ? N1 Co2 N1 176.2(2) 12 . ? N1 Co2 Cl4 90.69(11) 12 . ? N1 Co2 Cl4 90.68(11) . . ? N1 Co2 Cl3 89.46(11) 12 . ? N1 Co2 Cl3 89.46(11) . . ? Cl4 Co2 Cl3 175.34(15) . . ? N1 Co2 Cl5 88.37(11) 12 . ? N1 Co2 Cl5 88.37(11) . . ? Cl4 Co2 Cl5 79.5(2) . . ? Cl3 Co2 Cl5 105.13(16) . . ? N1 Co2 Cl3 91.78(11) 12 9_565 ? N1 Co2 Cl3 91.78(11) . 9_565 ? Cl4 Co2 Cl3 90.15(15) . 9_565 ? Cl3 Co2 Cl3 85.19(8) . 9_565 ? Cl5 Co2 Cl3 169.67(16) . 9_565 ? Co2 Cl3 Co2 94.81(8) . 9_565 ? C5 N1 C1 116.5(4) . . ? C5 N1 Co2 121.8(3) . . ? C1 N1 Co2 121.7(3) . . ? C19 N2 C9 119.6(4) . . ? C19 N2 Co1 115.2(3) . . ? C9 N2 Co1 125.1(3) . . ? C20 N3 C20 120.5(5) . 10_556 ? C20 N3 Co1 119.7(3) . . ? C20 N3 Co1 119.7(3) 10_556 . ? N1 C1 C2 124.8(4) . . ? N1 C1 H1 117.6 . . ? C2 C1 H1 117.6 . . ? C1 C2 C3 116.4(4) . . ? C1 C2 C6 121.8(4) . . ? C3 C2 C6 121.8(4) . . ? C4 C3 C2 119.0(4) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 123.5(5) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C11 C6 C7 115.9(4) . . ? C11 C6 C2 123.2(4) . . ? C7 C6 C2 120.7(4) . . ? C8 C7 C6 122.5(4) . . ? C8 C7 H7 118.8 . . ? C6 C7 H7 118.8 . . ? C7 C8 C9 118.6(4) . . ? C7 C8 C12 119.3(4) . . ? C9 C8 C12 122.1(4) . . ? C8 C9 C10 121.8(4) . . ? C8 C9 N2 118.3(4) . . ? C10 C9 N2 119.9(4) . . ? C11 C10 C9 116.5(4) . . ? C11 C10 C15 120.6(4) . . ? C9 C10 C15 122.9(4) . . ? C10 C11 C6 124.7(4) . . ? C10 C11 H11 117.6 . . ? C6 C11 H11 117.6 . . ? C13 C12 C8 112.9(6) . . ? C13 C12 C14 109.5(6) . . ? C8 C12 C14 110.5(5) . . ? C13 C12 H12 107.9 . . ? C8 C12 H12 107.9 . . ? C14 C12 H12 107.9 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 C16 110.3(5) . . ? C10 C15 C17 113.3(5) . . ? C16 C15 C17 111.1(5) . . ? C10 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C18 126.0(5) . . ? N2 C19 C20 115.1(4) . . ? C18 C19 C20 118.8(4) . . ? N3 C20 C21 121.1(5) . . ? N3 C20 C19 113.8(4) . . ? C21 C20 C19 124.9(4) . . ? C22 C21 C20 118.6(5) . . ? C22 C21 H21 120.7 . . ? C20 C21 H21 120.7 . . ? C21 C22 C21 120.0(7) . 10_556 ? C21 C22 H22 120.0 . . ? C21 C22 H22 120.0 10_556 . ? 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 N1 Co2 Cl3 Co2 91.84(11) 12 . . 9_565 ? N1 Co2 Cl3 Co2 -91.83(11) . . . 9_565 ? Cl4 Co2 Cl3 Co2 0.000(2) . . . 9_565 ? Cl5 Co2 Cl3 Co2 180.0 . . . 9_565 ? Cl3 Co2 Cl3 Co2 0.0 9_565 . . 9_565 ? N1 Co2 N1 C5 2(4) 12 . . . ? Cl4 Co2 N1 C5 113.5(4) . . . . ? Cl3 Co2 N1 C5 -71.2(4) . . . . ? Cl5 Co2 N1 C5 34.0(4) . . . . ? Cl3 Co2 N1 C5 -156.3(4) 9_565 . . . ? N1 Co2 N1 C1 -176(3) 12 . . . ? Cl4 Co2 N1 C1 -65.0(4) . . . . ? Cl3 Co2 N1 C1 110.4(3) . . . . ? Cl5 Co2 N1 C1 -144.5(4) . . . . ? Cl3 Co2 N1 C1 25.2(3) 9_565 . . . ? N3 Co1 N2 C19 -12.5(4) . . . . ? N2 Co1 N2 C19 -45.0(6) 10_556 . . . ? Cl2 Co1 N2 C19 -169.0(3) . . . . ? Cl1 Co1 N2 C19 78.8(4) . . . . ? N3 Co1 N2 C9 170.6(4) . . . . ? N2 Co1 N2 C9 138.1(3) 10_556 . . . ? Cl2 Co1 N2 C9 14.2(4) . . . . ? Cl1 Co1 N2 C9 -98.0(3) . . . . ? N2 Co1 N3 C20 12.1(4) . . . . ? N2 Co1 N3 C20 172.4(5) 10_556 . . . ? Cl2 Co1 N3 C20 92.3(5) . . . . ? Cl1 Co1 N3 C20 -87.7(5) . . . . ? N2 Co1 N3 C20 -172.4(5) . . . 10_556 ? N2 Co1 N3 C20 -12.1(4) 10_556 . . 10_556 ? Cl2 Co1 N3 C20 -92.3(5) . . . 10_556 ? Cl1 Co1 N3 C20 87.7(5) . . . 10_556 ? C5 N1 C1 C2 -1.1(7) . . . . ? Co2 N1 C1 C2 177.4(3) . . . . ? N1 C1 C2 C3 -1.6(7) . . . . ? N1 C1 C2 C6 177.0(4) . . . . ? C1 C2 C3 C4 3.4(7) . . . . ? C6 C2 C3 C4 -175.3(4) . . . . ? C2 C3 C4 C5 -2.5(8) . . . . ? C1 N1 C5 C4 2.3(8) . . . . ? Co2 N1 C5 C4 -176.3(4) . . . . ? C3 C4 C5 N1 -0.5(9) . . . . ? C1 C2 C6 C11 -157.9(4) . . . . ? C3 C2 C6 C11 20.7(6) . . . . ? C1 C2 C6 C7 18.5(6) . . . . ? C3 C2 C6 C7 -162.9(4) . . . . ? C11 C6 C7 C8 -1.3(7) . . . . ? C2 C6 C7 C8 -177.9(4) . . . . ? C6 C7 C8 C9 -0.7(7) . . . . ? C6 C7 C8 C12 -179.5(5) . . . . ? C7 C8 C9 C10 2.5(7) . . . . ? C12 C8 C9 C10 -178.7(5) . . . . ? C7 C8 C9 N2 -179.4(4) . . . . ? C12 C8 C9 N2 -0.6(7) . . . . ? C19 N2 C9 C8 94.5(6) . . . . ? Co1 N2 C9 C8 -88.8(5) . . . . ? C19 N2 C9 C10 -87.3(5) . . . . ? Co1 N2 C9 C10 89.4(4) . . . . ? C8 C9 C10 C11 -2.2(6) . . . . ? N2 C9 C10 C11 179.7(4) . . . . ? C8 C9 C10 C15 176.4(4) . . . . ? N2 C9 C10 C15 -1.7(6) . . . . ? C9 C10 C11 C6 0.0(7) . . . . ? C15 C10 C11 C6 -178.6(4) . . . . ? C7 C6 C11 C10 1.6(7) . . . . ? C2 C6 C11 C10 178.2(4) . . . . ? C7 C8 C12 C13 -52.8(7) . . . . ? C9 C8 C12 C13 128.4(6) . . . . ? C7 C8 C12 C14 70.2(7) . . . . ? C9 C8 C12 C14 -108.6(6) . . . . ? C11 C10 C15 C16 67.1(6) . . . . ? C9 C10 C15 C16 -111.4(5) . . . . ? C11 C10 C15 C17 -58.2(7) . . . . ? C9 C10 C15 C17 123.3(5) . . . . ? C9 N2 C19 C18 5.2(8) . . . . ? Co1 N2 C19 C18 -171.8(5) . . . . ? C9 N2 C19 C20 -171.7(4) . . . . ? Co1 N2 C19 C20 11.3(6) . . . . ? C20 N3 C20 C21 -1.1(10) 10_556 . . . ? Co1 N3 C20 C21 174.3(4) . . . . ? C20 N3 C20 C19 174.3(4) 10_556 . . . ? Co1 N3 C20 C19 -10.2(7) . . . . ? N2 C19 C20 N3 -1.5(7) . . . . ? C18 C19 C20 N3 -178.6(5) . . . . ? N2 C19 C20 C21 173.8(5) . . . . ? C18 C19 C20 C21 -3.3(9) . . . . ? N3 C20 C21 C22 0.8(10) . . . . ? C19 C20 C21 C22 -174.1(7) . . . . ? C20 C21 C22 C21 -0.5(14) . . . 10_556 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.44 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.845 _refine_diff_density_min -1.246 _refine_diff_density_rms 0.082 ########### data_3 _database_code_depnum_ccdc_archive 'CCDC 754691' #TrackingRef 'Co-R.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C90 H104 Co4 N20 O24' _chemical_formula_weight 2085.65 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3784(13) _cell_length_b 24.485(2) _cell_length_c 18.8723(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.633(2) _cell_angle_gamma 90.00 _cell_volume 6075.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2168 _exptl_absorpt_coefficient_mu 0.603 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8167 _exptl_absorpt_correction_T_max 0.8399 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 31983 _diffrn_reflns_av_R_equivalents 0.0701 _diffrn_reflns_av_sigmaI/netI 0.1006 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.49 _reflns_number_total 11217 _reflns_number_gt 5891 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART APEX II' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0764P)^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 11217 _refine_ls_number_parameters 633 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1141 _refine_ls_R_factor_gt 0.0580 _refine_ls_wR_factor_ref 0.1561 _refine_ls_wR_factor_gt 0.1389 _refine_ls_goodness_of_fit_ref 0.901 _refine_ls_restrained_S_all 0.903 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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 1 -0.001 0.000 0.000 712.0 98.4 2 0.009 0.500 0.500 712.0 98.8 3 0.411 0.480 0.003 8.8 0.0 4 0.411 0.020 0.503 8.8 0.1 5 0.589 0.520 -0.003 8.9 0.2 6 0.589 0.980 0.497 8.9 0.2 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 0.47621(4) 0.46887(2) 0.75817(3) 0.04260(16) Uani 1 1 d . . . Co2 Co -0.03350(4) 0.21987(2) 0.48292(3) 0.05130(19) Uani 1 1 d . . . O1 O 0.1152(3) 0.23309(17) 0.4479(2) 0.0872(11) Uani 1 1 d . . . O2 O 0.0316(3) 0.30218(15) 0.46988(19) 0.0810(10) Uani 1 1 d . . . O3 O 0.1723(3) 0.3137(2) 0.4294(2) 0.1206(16) Uani 1 1 d . . . O4 O -0.1871(3) 0.20228(18) 0.5005(2) 0.0887(12) Uani 1 1 d . . . O5 O -0.3041(3) 0.2530(3) 0.5271(3) 0.153(2) Uani 1 1 d . . . O6 O -0.1588(4) 0.28398(19) 0.5200(2) 0.1166(15) Uani 1 1 d . . . O7 O -0.0242(2) 0.13711(12) 0.46909(17) 0.0654(9) Uani 1 1 d . . . O8 O 0.1250(2) 0.12765(14) 0.53632(19) 0.0768(10) Uani 1 1 d . . . O9 O 0.0406(3) 0.05878(16) 0.4951(3) 0.153(2) Uani 1 1 d . . . O10 O 0.3465(3) 0.47501(17) 0.6812(2) 0.0898(11) Uani 1 1 d . . . O11 O 0.3305(2) 0.47137(13) 0.79169(19) 0.0688(9) Uani 1 1 d . . . O12 O 0.1969(3) 0.4801(3) 0.7109(3) 0.181(3) Uani 1 1 d . . . N1 N 0.0248(2) 0.21639(14) 0.59476(18) 0.0477(8) Uani 1 1 d . . . N2 N 0.4895(2) 0.38373(12) 0.79086(16) 0.0386(7) Uani 1 1 d . . . N3 N 0.6065(2) 0.46495(13) 0.83406(15) 0.0364(7) Uani 1 1 d . . . N4 N 0.5068(2) 0.55282(13) 0.79482(16) 0.0411(8) Uani 1 1 d . . . N5 N 0.0994(2) 0.77141(14) 0.6299(2) 0.0549(9) Uani 1 1 d . . . N6 N 0.1086(3) 0.2836(2) 0.4475(2) 0.0724(12) Uani 1 1 d . . . N7 N -0.2192(3) 0.2464(3) 0.5168(2) 0.0770(13) Uani 1 1 d . . . N8 N 0.0495(3) 0.10661(17) 0.5018(2) 0.0663(11) Uani 1 1 d . . . N9 N 0.2876(3) 0.4757(2) 0.7283(3) 0.0920(15) Uani 1 1 d . . . C1 C 0.1046(3) 0.24543(17) 0.6250(2) 0.0487(10) Uani 1 1 d . . . H1 H 0.1297 0.2711 0.5964 0.058 Uiso 1 1 calc R . . C2 C 0.1537(3) 0.24061(17) 0.6959(2) 0.0480(10) Uani 1 1 d . . . C3 C 0.1144(3) 0.20417(19) 0.7391(2) 0.0583(12) Uani 1 1 d . . . H3 H 0.1445 0.1997 0.7872 0.070 Uiso 1 1 calc R . . C4 C 0.0288(3) 0.1742(2) 0.7094(3) 0.0674(13) Uani 1 1 d . . . H4 H -0.0005 0.1499 0.7375 0.081 Uiso 1 1 calc R . . C5 C -0.0119(3) 0.18118(18) 0.6372(3) 0.0604(12) Uani 1 1 d . . . H5 H -0.0679 0.1602 0.6172 0.072 Uiso 1 1 calc R . . C6 C 0.2447(3) 0.27524(16) 0.7228(2) 0.0458(10) Uani 1 1 d . . . C7 C 0.3146(3) 0.28607(16) 0.6789(2) 0.0469(10) Uani 1 1 d . . . H7 H 0.3055 0.2702 0.6334 0.056 Uiso 1 1 calc R . . C8 C 0.3980(3) 0.32007(17) 0.7008(2) 0.0445(10) Uani 1 1 d . . . C9 C 0.4097(3) 0.34337(16) 0.76940(19) 0.0391(9) Uani 1 1 d . . . C10 C 0.3428(3) 0.33240(16) 0.8156(2) 0.0462(10) Uani 1 1 d . . . C11 C 0.2601(3) 0.29756(16) 0.7910(2) 0.0470(10) Uani 1 1 d . . . H11 H 0.2148 0.2894 0.8214 0.056 Uiso 1 1 calc R . . C12 C 0.4737(3) 0.3273(2) 0.6515(2) 0.0632(13) Uani 1 1 d . . . H12 H 0.5266 0.3524 0.6750 0.076 Uiso 1 1 calc R . . C13 C 0.5252(4) 0.2729(3) 0.6395(4) 0.107(2) Uani 1 1 d . . . H13A H 0.5541 0.2572 0.6853 0.160 Uiso 1 1 calc R . . H13B H 0.5780 0.2792 0.6123 0.160 Uiso 1 1 calc R . . H13C H 0.4757 0.2483 0.6135 0.160 Uiso 1 1 calc R . . C14 C 0.4263(4) 0.3518(3) 0.5800(3) 0.0982(19) Uani 1 1 d . . . H14A H 0.3797 0.3261 0.5533 0.147 Uiso 1 1 calc R . . H14B H 0.4786 0.3605 0.5531 0.147 Uiso 1 1 calc R . . H14C H 0.3903 0.3845 0.5879 0.147 Uiso 1 1 calc R . . C15 C 0.3553(3) 0.35408(19) 0.8925(2) 0.0610(13) Uani 1 1 d . . . H15 H 0.4133 0.3792 0.9006 0.073 Uiso 1 1 calc R . . C16 C 0.3785(4) 0.3071(2) 0.9464(2) 0.0779(15) Uani 1 1 d . . . H16A H 0.3263 0.2798 0.9357 0.117 Uiso 1 1 calc R . . H16B H 0.3805 0.3207 0.9944 0.117 Uiso 1 1 calc R . . H16C H 0.4431 0.2913 0.9430 0.117 Uiso 1 1 calc R . . C17 C 0.2608(4) 0.3855(2) 0.9047(3) 0.0892(18) Uani 1 1 d . . . H17A H 0.2043 0.3608 0.9010 0.134 Uiso 1 1 calc R . . H17B H 0.2452 0.4136 0.8690 0.134 Uiso 1 1 calc R . . H17C H 0.2738 0.4017 0.9519 0.134 Uiso 1 1 calc R . . C18 C 0.6060(3) 0.31372(17) 0.8529(3) 0.0615(12) Uani 1 1 d . . . H18A H 0.5487 0.2897 0.8409 0.092 Uiso 1 1 calc R . . H18B H 0.6299 0.3133 0.9040 0.092 Uiso 1 1 calc R . . H18C H 0.6593 0.3018 0.8288 0.092 Uiso 1 1 calc R . . C19 C 0.5751(3) 0.36973(15) 0.8296(2) 0.0416(9) Uani 1 1 d . . . C20 C 0.6456(2) 0.41574(16) 0.85395(19) 0.0377(9) Uani 1 1 d . . . C21 C 0.7425(3) 0.41217(17) 0.8964(2) 0.0468(10) Uani 1 1 d . . . H21 H 0.7708 0.3783 0.9108 0.056 Uiso 1 1 calc R . . C22 C 0.7954(3) 0.45929(17) 0.9165(2) 0.0517(11) Uani 1 1 d . . . H22 H 0.8606 0.4573 0.9440 0.062 Uiso 1 1 calc R . . C23 C 0.7533(3) 0.50919(18) 0.8967(2) 0.0505(11) Uani 1 1 d . . . H23 H 0.7886 0.5412 0.9114 0.061 Uiso 1 1 calc R . . C24 C 0.6566(3) 0.51105(16) 0.8542(2) 0.0407(9) Uani 1 1 d . . . C25 C 0.5969(3) 0.56143(16) 0.8307(2) 0.0436(10) Uani 1 1 d . . . C26 C 0.6440(3) 0.61595(17) 0.8504(3) 0.0621(13) Uani 1 1 d . . . H26A H 0.6947 0.6232 0.8216 0.093 Uiso 1 1 calc R . . H26B H 0.6751 0.6160 0.9005 0.093 Uiso 1 1 calc R . . H26C H 0.5924 0.6437 0.8417 0.093 Uiso 1 1 calc R . . C27 C 0.4359(3) 0.59766(15) 0.7758(2) 0.0419(9) Uani 1 1 d . . . C28 C 0.4330(3) 0.62663(17) 0.7128(2) 0.0474(10) Uani 1 1 d . . . C29 C 0.3596(3) 0.66675(17) 0.6955(2) 0.0513(11) Uani 1 1 d . . . H29 H 0.3564 0.6863 0.6528 0.062 Uiso 1 1 calc R . . C30 C 0.2903(3) 0.67871(17) 0.7404(2) 0.0467(10) Uani 1 1 d . . . C31 C 0.2963(3) 0.64859(17) 0.8035(2) 0.0502(11) Uani 1 1 d . . . H31 H 0.2515 0.6566 0.8343 0.060 Uiso 1 1 calc R . . C32 C 0.3665(3) 0.60705(15) 0.8220(2) 0.0407(9) Uani 1 1 d . . . C33 C 0.5066(3) 0.61585(19) 0.6622(2) 0.0625(13) Uani 1 1 d . . . H33 H 0.5555 0.5883 0.6845 0.075 Uiso 1 1 calc R . . C34 C 0.4521(5) 0.5936(3) 0.5905(3) 0.106(2) Uani 1 1 d . . . H34A H 0.4172 0.5605 0.5984 0.159 Uiso 1 1 calc R . . H34B H 0.5008 0.5861 0.5602 0.159 Uiso 1 1 calc R . . H34C H 0.4039 0.6201 0.5676 0.159 Uiso 1 1 calc R . . C35 C 0.5667(4) 0.6683(3) 0.6504(4) 0.116(2) Uani 1 1 d . . . H35A H 0.5227 0.6932 0.6200 0.174 Uiso 1 1 calc R . . H35B H 0.6231 0.6589 0.6279 0.174 Uiso 1 1 calc R . . H35C H 0.5915 0.6854 0.6961 0.174 Uiso 1 1 calc R . . C36 C 0.3680(3) 0.57488(18) 0.8903(2) 0.0531(11) Uani 1 1 d . . . H36 H 0.4034 0.5404 0.8853 0.064 Uiso 1 1 calc R . . C37 C 0.2604(3) 0.5604(2) 0.9030(3) 0.0740(14) Uani 1 1 d . . . H37A H 0.2311 0.5916 0.9221 0.111 Uiso 1 1 calc R . . H37B H 0.2648 0.5307 0.9367 0.111 Uiso 1 1 calc R . . H37C H 0.2186 0.5498 0.8582 0.111 Uiso 1 1 calc R . . C38 C 0.4275(4) 0.6045(2) 0.9565(2) 0.0843(16) Uani 1 1 d . . . H38A H 0.4950 0.6125 0.9487 0.126 Uiso 1 1 calc R . . H38B H 0.4314 0.5817 0.9982 0.126 Uiso 1 1 calc R . . H38C H 0.3935 0.6380 0.9638 0.126 Uiso 1 1 calc R . . C39 C 0.2142(3) 0.72307(17) 0.7214(2) 0.0499(11) Uani 1 1 d . . . C40 C 0.1890(3) 0.75832(19) 0.7729(3) 0.0614(12) Uani 1 1 d . . . H40 H 0.2189 0.7542 0.8212 0.074 Uiso 1 1 calc R . . C41 C 0.1194(4) 0.7994(2) 0.7521(3) 0.0738(14) Uani 1 1 d . . . H41 H 0.1011 0.8231 0.7861 0.089 Uiso 1 1 calc R . . C42 C 0.0773(3) 0.8048(2) 0.6802(3) 0.0639(13) Uani 1 1 d . . . H42 H 0.0315 0.8331 0.6663 0.077 Uiso 1 1 calc R . . C43 C 0.1663(3) 0.73091(17) 0.6505(2) 0.0504(11) Uani 1 1 d . . . H43 H 0.1810 0.7070 0.6156 0.060 Uiso 1 1 calc R . . N10 N 0.5692(3) 0.46593(18) 0.6822(2) 0.0744(12) Uani 1 1 d . . . C45 C 0.7063(9) 0.4191(9) 0.5980(7) 0.440(16) Uani 1 1 d D . . H45A H 0.6704 0.3897 0.5707 0.660 Uiso 1 1 calc R . . H45B H 0.7682 0.4054 0.6264 0.660 Uiso 1 1 calc R . . H45C H 0.7220 0.4468 0.5658 0.660 Uiso 1 1 calc R . . C44 C 0.6346(10) 0.4454(6) 0.6517(6) 0.285(9) Uani 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0385(3) 0.0430(3) 0.0408(3) 0.0019(3) -0.0070(2) -0.0032(3) Co2 0.0406(3) 0.0442(3) 0.0603(4) 0.0027(3) -0.0138(3) -0.0020(3) O1 0.063(2) 0.067(3) 0.125(3) 0.000(2) 0.002(2) 0.005(2) O2 0.083(2) 0.074(2) 0.085(3) -0.019(2) 0.013(2) -0.004(2) O3 0.119(3) 0.137(4) 0.115(4) -0.002(3) 0.046(3) -0.066(3) O4 0.066(2) 0.103(3) 0.088(3) -0.020(2) -0.0093(19) 0.012(2) O5 0.076(3) 0.230(6) 0.165(5) -0.041(4) 0.052(3) 0.011(3) O6 0.119(3) 0.104(3) 0.114(4) 0.005(3) -0.009(3) -0.012(3) O7 0.0584(17) 0.0457(18) 0.078(2) 0.0063(16) -0.0256(16) 0.0071(15) O8 0.0552(19) 0.073(2) 0.092(3) -0.009(2) -0.0154(18) 0.0109(18) O9 0.099(3) 0.044(2) 0.272(7) 0.015(3) -0.085(3) 0.002(2) O10 0.071(2) 0.115(3) 0.069(2) 0.008(2) -0.025(2) -0.001(2) O11 0.0484(17) 0.073(2) 0.082(2) -0.002(2) 0.0061(17) -0.0002(17) O12 0.042(2) 0.273(7) 0.206(6) -0.008(5) -0.031(3) 0.004(3) N1 0.0380(17) 0.048(2) 0.052(2) -0.0009(18) -0.0058(15) -0.0069(17) N2 0.0391(17) 0.0386(18) 0.0354(18) -0.0061(14) -0.0003(14) -0.0028(15) N3 0.0327(15) 0.0371(18) 0.0358(17) -0.0025(15) -0.0030(13) -0.0002(15) N4 0.0386(17) 0.0413(19) 0.0391(19) 0.0067(15) -0.0039(14) -0.0033(15) N5 0.051(2) 0.042(2) 0.061(2) 0.0041(18) -0.0154(18) 0.0035(18) N6 0.060(3) 0.092(4) 0.061(3) -0.005(3) 0.000(2) -0.010(3) N7 0.049(3) 0.111(4) 0.067(3) -0.006(3) 0.001(2) -0.013(3) N8 0.051(2) 0.051(3) 0.086(3) 0.005(2) -0.015(2) 0.000(2) N9 0.046(3) 0.106(4) 0.113(4) -0.004(3) -0.014(3) -0.001(3) C1 0.043(2) 0.044(2) 0.055(3) -0.001(2) 0.000(2) -0.008(2) C2 0.044(2) 0.053(3) 0.043(2) -0.006(2) -0.0032(19) -0.003(2) C3 0.056(3) 0.068(3) 0.048(3) 0.002(2) 0.001(2) -0.016(2) C4 0.064(3) 0.071(3) 0.065(3) 0.001(3) 0.006(2) -0.024(3) C5 0.049(2) 0.053(3) 0.074(3) -0.005(3) -0.004(2) -0.019(2) C6 0.039(2) 0.048(3) 0.047(3) -0.006(2) 0.0003(18) -0.005(2) C7 0.044(2) 0.051(3) 0.042(2) -0.013(2) -0.0022(18) -0.006(2) C8 0.044(2) 0.051(3) 0.036(2) -0.0024(19) 0.0003(18) 0.002(2) C9 0.036(2) 0.045(2) 0.035(2) -0.0051(18) 0.0023(17) -0.0034(18) C10 0.048(2) 0.045(2) 0.042(2) -0.006(2) -0.0009(19) -0.007(2) C11 0.046(2) 0.049(3) 0.045(2) -0.005(2) 0.0049(18) -0.007(2) C12 0.056(3) 0.082(4) 0.052(3) -0.019(3) 0.011(2) -0.017(3) C13 0.085(4) 0.136(6) 0.112(5) -0.027(4) 0.051(4) 0.016(4) C14 0.108(4) 0.130(5) 0.062(4) 0.010(4) 0.031(3) -0.013(4) C15 0.073(3) 0.065(3) 0.047(3) -0.022(2) 0.017(2) -0.023(3) C16 0.098(4) 0.088(4) 0.043(3) 0.000(3) -0.001(3) -0.024(3) C17 0.123(5) 0.073(4) 0.084(4) -0.024(3) 0.052(4) -0.011(4) C18 0.053(2) 0.042(3) 0.081(3) -0.004(2) -0.011(2) 0.001(2) C19 0.037(2) 0.038(2) 0.046(2) -0.0053(19) -0.0022(18) 0.0055(18) C20 0.0319(18) 0.041(2) 0.038(2) -0.0018(18) 0.0019(16) 0.0025(18) C21 0.041(2) 0.045(3) 0.049(2) 0.005(2) -0.0070(18) 0.006(2) C22 0.034(2) 0.056(3) 0.059(3) 0.000(2) -0.0093(18) 0.000(2) C23 0.038(2) 0.049(3) 0.058(3) 0.005(2) -0.0093(19) -0.008(2) C24 0.0352(19) 0.041(2) 0.043(2) -0.0006(19) 0.0013(17) -0.0052(19) C25 0.042(2) 0.039(2) 0.045(2) 0.0048(19) -0.0049(18) -0.0031(19) C26 0.056(3) 0.041(3) 0.080(3) -0.008(2) -0.012(2) -0.009(2) C27 0.039(2) 0.035(2) 0.047(2) 0.0040(19) -0.0051(18) -0.0023(18) C28 0.045(2) 0.048(3) 0.047(3) 0.007(2) 0.0041(19) 0.000(2) C29 0.050(2) 0.050(3) 0.050(3) 0.014(2) -0.001(2) 0.002(2) C30 0.045(2) 0.044(2) 0.045(2) 0.012(2) -0.0056(19) -0.001(2) C31 0.042(2) 0.053(3) 0.053(3) 0.002(2) 0.0013(19) 0.000(2) C32 0.039(2) 0.038(2) 0.040(2) 0.0082(18) -0.0041(17) -0.0044(19) C33 0.068(3) 0.065(3) 0.059(3) 0.018(2) 0.024(2) 0.014(3) C34 0.141(5) 0.126(5) 0.058(4) -0.005(4) 0.035(4) -0.001(5) C35 0.100(4) 0.098(5) 0.169(7) 0.046(5) 0.074(5) -0.001(4) C36 0.059(3) 0.055(3) 0.044(3) 0.006(2) 0.008(2) 0.005(2) C37 0.070(3) 0.088(4) 0.066(3) 0.014(3) 0.020(3) 0.002(3) C38 0.091(4) 0.115(5) 0.043(3) 0.003(3) 0.003(3) -0.008(3) C39 0.041(2) 0.043(2) 0.062(3) 0.005(2) -0.003(2) -0.004(2) C40 0.067(3) 0.058(3) 0.053(3) 0.002(2) -0.006(2) 0.005(3) C41 0.086(3) 0.068(3) 0.061(3) -0.013(3) -0.002(3) 0.025(3) C42 0.057(3) 0.056(3) 0.071(3) 0.002(3) -0.006(2) 0.013(2) C43 0.048(2) 0.046(3) 0.052(3) 0.007(2) -0.0048(19) 0.004(2) N10 0.086(3) 0.090(3) 0.051(2) -0.004(2) 0.021(2) -0.019(3) C45 0.211(13) 0.92(5) 0.204(13) 0.06(2) 0.073(11) -0.22(2) C44 0.287(14) 0.42(2) 0.183(10) -0.180(12) 0.145(11) -0.259(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N3 2.044(3) . ? Co1 O10 2.053(3) . ? Co1 N10 2.065(4) . ? Co1 O11 2.158(3) . ? Co1 N2 2.172(3) . ? Co1 N4 2.183(3) . ? Co2 O7 2.050(3) . ? Co2 N1 2.112(3) . ? Co2 N5 2.159(4) 3_566 ? Co2 O4 2.184(4) . ? Co2 O2 2.227(4) . ? Co2 O1 2.233(4) . ? O1 N6 1.239(5) . ? O2 N6 1.268(5) . ? O3 N6 1.223(5) . ? O4 N7 1.222(6) . ? O5 N7 1.198(5) . ? O6 N7 1.220(5) . ? O7 N8 1.298(4) . ? O8 N8 1.211(4) . ? O9 N8 1.182(5) . ? O10 N9 1.292(6) . ? O11 N9 1.233(5) . ? O12 N9 1.202(5) . ? N1 C1 1.322(5) . ? N1 C5 1.330(5) . ? N2 C19 1.286(4) . ? N2 C9 1.456(4) . ? N3 C24 1.332(4) . ? N3 C20 1.339(4) . ? N4 C25 1.287(4) . ? N4 C27 1.452(5) . ? N5 C42 1.328(5) . ? N5 C43 1.344(5) . ? N5 Co2 2.159(4) 3_566 ? C1 C2 1.382(5) . ? C1 H1 0.9300 . ? C2 C3 1.377(6) . ? C2 C6 1.494(5) . ? C3 C4 1.388(6) . ? C3 H3 0.9300 . ? C4 C5 1.383(6) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C11 1.378(5) . ? C6 C7 1.385(5) . ? C7 C8 1.393(5) . ? C7 H7 0.9300 . ? C8 C9 1.398(5) . ? C8 C12 1.506(5) . ? C9 C10 1.386(5) . ? C10 C11 1.406(5) . ? C10 C15 1.526(5) . ? C11 H11 0.9300 . ? C12 C14 1.506(7) . ? C12 C13 1.535(7) . ? C12 H12 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C16 1.528(6) . ? C15 C17 1.533(6) . ? C15 H15 0.9800 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.475(5) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C20 1.487(5) . ? C20 C21 1.395(5) . ? C21 C22 1.369(5) . ? C21 H21 0.9300 . ? C22 C23 1.368(5) . ? C22 H22 0.9300 . ? C23 C24 1.391(5) . ? C23 H23 0.9300 . ? C24 C25 1.492(5) . ? C25 C26 1.493(5) . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.380(5) . ? C27 C32 1.404(5) . ? C28 C29 1.384(5) . ? C28 C33 1.517(6) . ? C29 C30 1.398(5) . ? C29 H29 0.9300 . ? C30 C31 1.390(5) . ? C30 C39 1.487(5) . ? C31 C32 1.385(5) . ? C31 H31 0.9300 . ? C32 C36 1.507(5) . ? C33 C34 1.514(7) . ? C33 C35 1.553(7) . ? C33 H33 0.9800 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 C38 1.535(6) . ? C36 C37 1.544(6) . ? C36 H36 0.9800 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 C43 1.385(5) . ? C39 C40 1.388(6) . ? C40 C41 1.378(6) . ? C40 H40 0.9300 . ? C41 C42 1.375(6) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? N10 C44 1.239(12) . ? C45 C44 1.649(14) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Co1 O10 178.36(15) . . ? N3 Co1 N10 86.54(14) . . ? O10 Co1 N10 92.87(17) . . ? N3 Co1 O11 119.71(13) . . ? O10 Co1 O11 60.94(15) . . ? N10 Co1 O11 153.72(15) . . ? N3 Co1 N2 75.01(11) . . ? O10 Co1 N2 106.60(14) . . ? N10 Co1 N2 97.78(15) . . ? O11 Co1 N2 88.58(12) . . ? N3 Co1 N4 74.73(12) . . ? O10 Co1 N4 103.86(14) . . ? N10 Co1 N4 98.70(14) . . ? O11 Co1 N4 90.39(12) . . ? N2 Co1 N4 144.39(11) . . ? O7 Co2 N1 93.87(12) . . ? O7 Co2 N5 89.74(13) . 3_566 ? N1 Co2 N5 175.81(14) . 3_566 ? O7 Co2 O4 84.57(15) . . ? N1 Co2 O4 91.41(13) . . ? N5 Co2 O4 86.82(14) 3_566 . ? O7 Co2 O2 147.83(14) . . ? N1 Co2 O2 93.85(13) . . ? N5 Co2 O2 84.17(13) 3_566 . ? O4 Co2 O2 126.38(16) . . ? O7 Co2 O1 91.56(14) . . ? N1 Co2 O1 96.71(13) . . ? N5 Co2 O1 85.30(14) 3_566 . ? O4 Co2 O1 171.23(15) . . ? O2 Co2 O1 56.52(13) . . ? N6 O1 Co2 94.5(3) . . ? N6 O2 Co2 94.0(3) . . ? N7 O4 Co2 104.4(3) . . ? N8 O7 Co2 124.5(3) . . ? N9 O10 Co1 93.3(3) . . ? N9 O11 Co1 90.1(3) . . ? C1 N1 C5 116.5(4) . . ? C1 N1 Co2 122.0(3) . . ? C5 N1 Co2 121.2(3) . . ? C19 N2 C9 120.5(3) . . ? C19 N2 Co1 115.8(2) . . ? C9 N2 Co1 123.7(2) . . ? C24 N3 C20 122.2(3) . . ? C24 N3 Co1 118.6(2) . . ? C20 N3 Co1 118.5(2) . . ? C25 N4 C27 120.8(3) . . ? C25 N4 Co1 115.0(3) . . ? C27 N4 Co1 123.9(2) . . ? C42 N5 C43 118.1(4) . . ? C42 N5 Co2 122.7(3) . 3_566 ? C43 N5 Co2 119.2(3) . 3_566 ? O3 N6 O1 123.4(5) . . ? O3 N6 O2 121.8(5) . . ? O1 N6 O2 114.8(5) . . ? O5 N7 O6 122.0(7) . . ? O5 N7 O4 123.3(6) . . ? O6 N7 O4 114.7(5) . . ? O9 N8 O8 122.5(4) . . ? O9 N8 O7 117.8(4) . . ? O8 N8 O7 119.7(4) . . ? O12 N9 O11 122.5(6) . . ? O12 N9 O10 121.8(6) . . ? O11 N9 O10 115.7(4) . . ? N1 C1 C2 125.0(4) . . ? N1 C1 H1 117.5 . . ? C2 C1 H1 117.5 . . ? C3 C2 C1 117.6(4) . . ? C3 C2 C6 122.9(4) . . ? C1 C2 C6 119.5(4) . . ? C2 C3 C4 118.8(4) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C5 C4 C3 118.5(4) . . ? C5 C4 H4 120.8 . . ? C3 C4 H4 120.8 . . ? N1 C5 C4 123.5(4) . . ? N1 C5 H5 118.2 . . ? C4 C5 H5 118.2 . . ? C11 C6 C7 118.8(4) . . ? C11 C6 C2 121.0(4) . . ? C7 C6 C2 120.2(4) . . ? C6 C7 C8 122.0(4) . . ? C6 C7 H7 119.0 . . ? C8 C7 H7 119.0 . . ? C7 C8 C9 117.7(4) . . ? C7 C8 C12 118.7(4) . . ? C9 C8 C12 123.4(3) . . ? C10 C9 C8 121.9(3) . . ? C10 C9 N2 118.8(3) . . ? C8 C9 N2 119.1(3) . . ? C9 C10 C11 118.0(4) . . ? C9 C10 C15 124.1(3) . . ? C11 C10 C15 117.9(4) . . ? C6 C11 C10 121.5(4) . . ? C6 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C8 C12 C14 112.3(4) . . ? C8 C12 C13 111.1(4) . . ? C14 C12 C13 109.9(4) . . ? C8 C12 H12 107.8 . . ? C14 C12 H12 107.8 . . ? C13 C12 H12 107.8 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C10 C15 C16 110.2(4) . . ? C10 C15 C17 111.6(4) . . ? C16 C15 C17 110.4(4) . . ? C10 C15 H15 108.2 . . ? C16 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 H18A 109.5 . . ? C19 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C19 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C18 126.0(4) . . ? N2 C19 C20 114.9(3) . . ? C18 C19 C20 119.1(3) . . ? N3 C20 C21 119.4(3) . . ? N3 C20 C19 113.7(3) . . ? C21 C20 C19 126.8(4) . . ? C22 C21 C20 118.9(4) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 120.8(3) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? C22 C23 C24 118.6(4) . . ? C22 C23 H23 120.7 . . ? C24 C23 H23 120.7 . . ? N3 C24 C23 120.1(4) . . ? N3 C24 C25 113.7(3) . . ? C23 C24 C25 126.0(4) . . ? N4 C25 C24 114.8(3) . . ? N4 C25 C26 126.0(4) . . ? C24 C25 C26 119.2(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 122.3(4) . . ? C28 C27 N4 121.0(4) . . ? C32 C27 N4 116.6(3) . . ? C27 C28 C29 118.3(4) . . ? C27 C28 C33 122.4(4) . . ? C29 C28 C33 119.3(4) . . ? C28 C29 C30 121.7(4) . . ? C28 C29 H29 119.1 . . ? C30 C29 H29 119.1 . . ? C31 C30 C29 117.9(4) . . ? C31 C30 C39 121.5(4) . . ? C29 C30 C39 120.6(4) . . ? C32 C31 C30 122.3(4) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C31 C32 C27 117.3(4) . . ? C31 C32 C36 120.1(4) . . ? C27 C32 C36 122.6(3) . . ? C34 C33 C28 111.3(4) . . ? C34 C33 C35 110.3(5) . . ? C28 C33 C35 111.1(4) . . ? C34 C33 H33 108.0 . . ? C28 C33 H33 108.0 . . ? C35 C33 H33 108.0 . . ? 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 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C32 C36 C38 111.8(4) . . ? C32 C36 C37 112.8(3) . . ? C38 C36 C37 109.9(4) . . ? C32 C36 H36 107.3 . . ? C38 C36 H36 107.3 . . ? C37 C36 H36 107.3 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C43 C39 C40 117.5(4) . . ? C43 C39 C30 120.6(4) . . ? C40 C39 C30 122.0(4) . . ? C41 C40 C39 119.6(4) . . ? C41 C40 H40 120.2 . . ? C39 C40 H40 120.2 . . ? C42 C41 C40 118.9(4) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? N5 C42 C41 122.9(4) . . ? N5 C42 H42 118.6 . . ? C41 C42 H42 118.6 . . ? N5 C43 C39 123.1(4) . . ? N5 C43 H43 118.4 . . ? C39 C43 H43 118.4 . . ? C44 N10 Co1 154.7(8) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N10 C44 C45 169.8(12) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.49 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.569 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.059 #########END