# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_complex1a _database_code_depnum_ccdc_archive 'CCDC 918511' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H42 Cl Co N3 Si2' _chemical_formula_weight 559.20 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.0310(4) _cell_length_b 10.5956(5) _cell_length_c 16.4793(5) _cell_angle_alpha 89.090(2) _cell_angle_beta 82.464(2) _cell_angle_gamma 85.249(2) _cell_volume 1557.87(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 63353 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description prism _exptl_crystal_colour blue-green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.192 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 594 _exptl_absorpt_coefficient_mu 0.732 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8674 _exptl_absorpt_correction_T_max 0.9304 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12100 _diffrn_reflns_av_R_equivalents 0.0848 _diffrn_reflns_av_sigmaI/netI 0.0583 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5318 _reflns_number_gt 4590 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Collect (Bruker AXS BV, 1997-2004)' _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^ > 2\s(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^)+(0.1489P)^2^+3.0389P] 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 5318 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0926 _refine_ls_R_factor_gt 0.0791 _refine_ls_wR_factor_ref 0.2686 _refine_ls_wR_factor_gt 0.2537 _refine_ls_goodness_of_fit_ref 1.220 _refine_ls_restrained_S_all 1.220 _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 C01 C 0.6451(5) 0.1596(5) 0.2469(3) 0.0298(11) Uani 1 1 d . . . C02 C 0.4173(7) 0.0943(6) 0.2330(4) 0.0446(14) Uani 1 1 d . . . H02 H 0.3349 0.0736 0.2091 0.054 Uiso 1 1 calc R . . C03 C 0.4327(7) 0.0873(6) 0.3124(4) 0.0432(14) Uani 1 1 d . . . H03 H 0.3627 0.0610 0.3545 0.052 Uiso 1 1 calc R . . C04 C 0.6322(6) 0.1295(5) 0.3973(3) 0.0322(11) Uani 1 1 d . . . C05 C 0.7214(7) 0.0240(5) 0.4197(3) 0.0403(13) Uani 1 1 d . . . C06 C 0.7796(7) 0.0306(6) 0.4938(4) 0.0436(14) Uani 1 1 d . . . H06 H 0.8406 -0.0378 0.5099 0.052 Uiso 1 1 calc R . . C07 C 0.7495(7) 0.1362(6) 0.5443(3) 0.0440(14) Uani 1 1 d . . . C08 C 0.6529(7) 0.2350(6) 0.5208(3) 0.0430(13) Uani 1 1 d . . . H08 H 0.6272 0.3038 0.5556 0.052 Uiso 1 1 calc R . . C09 C 0.5938(7) 0.2349(6) 0.4477(3) 0.0397(13) Uani 1 1 d . . . C10 C 0.4897(8) 0.3433(7) 0.4224(4) 0.0565(17) Uani 1 1 d . . . H10A H 0.4719 0.4058 0.4648 0.085 Uiso 1 1 calc R . . H10B H 0.3963 0.3121 0.4135 0.085 Uiso 1 1 calc R . . H10C H 0.5347 0.3808 0.3727 0.085 Uiso 1 1 calc R . . C11 C 0.7544(9) -0.0909(6) 0.3660(4) 0.0537(16) Uani 1 1 d . . . H11A H 0.6621 -0.1193 0.3530 0.081 Uiso 1 1 calc R . . H11B H 0.8064 -0.1571 0.3942 0.081 Uiso 1 1 calc R . . H11C H 0.8158 -0.0696 0.3164 0.081 Uiso 1 1 calc R . . C12 C 0.8201(9) 0.1435(8) 0.6212(4) 0.0606(19) Uani 1 1 d . . . H12A H 0.7446 0.1691 0.6657 0.091 Uiso 1 1 calc R . . H12B H 0.8941 0.2041 0.6140 0.091 Uiso 1 1 calc R . . H12C H 0.8670 0.0618 0.6331 0.091 Uiso 1 1 calc R . . C13 C 0.5769(6) 0.1556(5) 0.1059(3) 0.0334(11) Uani 1 1 d . . . C14 C 0.5013(6) 0.2605(5) 0.0701(3) 0.0371(12) Uani 1 1 d . . . C15 C 0.5340(7) 0.2765(6) -0.0138(3) 0.0402(13) Uani 1 1 d . . . H15 H 0.4870 0.3452 -0.0388 0.048 Uiso 1 1 calc R . . C16 C 0.6350(6) 0.1929(6) -0.0619(3) 0.0390(12) Uani 1 1 d . . . C17 C 0.7018(6) 0.0902(6) -0.0245(3) 0.0393(13) Uani 1 1 d . . . H17 H 0.7689 0.0341 -0.0564 0.047 Uiso 1 1 calc R . . C18 C 0.6728(6) 0.0669(5) 0.0595(3) 0.0367(12) Uani 1 1 d . . . C19 C 0.7420(8) -0.0512(6) 0.0964(4) 0.0477(15) Uani 1 1 d . . . H19A H 0.8364 -0.0343 0.1130 0.072 Uiso 1 1 calc R . . H19B H 0.7576 -0.1177 0.0566 0.072 Uiso 1 1 calc R . . H19C H 0.6761 -0.0768 0.1432 0.072 Uiso 1 1 calc R . . C20 C 0.3901(8) 0.3521(7) 0.1202(4) 0.0540(17) Uani 1 1 d . . . H20A H 0.3710 0.4270 0.0883 0.081 Uiso 1 1 calc R . . H20B H 0.4303 0.3745 0.1686 0.081 Uiso 1 1 calc R . . H20C H 0.2982 0.3131 0.1354 0.081 Uiso 1 1 calc R . . C21 C 0.6686(8) 0.2139(7) -0.1530(4) 0.0498(15) Uani 1 1 d . . . H21A H 0.7649 0.1724 -0.1727 0.075 Uiso 1 1 calc R . . H21B H 0.6692 0.3030 -0.1643 0.075 Uiso 1 1 calc R . . H21C H 0.5930 0.1796 -0.1800 0.075 Uiso 1 1 calc R . . C22 C 0.8421(12) 0.4194(10) 0.0841(5) 0.088(3) Uani 1 1 d . . . H22A H 0.9418 0.3884 0.0619 0.132 Uiso 1 1 calc R . . H22B H 0.8006 0.4771 0.0459 0.132 Uiso 1 1 calc R . . H22C H 0.7807 0.3496 0.0942 0.132 Uiso 1 1 calc R . . C23 C 0.9783(12) 0.6310(8) 0.1601(6) 0.087(3) Uani 1 1 d . . . H23A H 0.9731 0.6835 0.2074 0.131 Uiso 1 1 calc R . . H23B H 0.9500 0.6814 0.1148 0.131 Uiso 1 1 calc R . . H23C H 1.0789 0.5935 0.1465 0.131 Uiso 1 1 calc R . . C24 C 0.6557(12) 0.5844(10) 0.2172(8) 0.101(3) Uani 1 1 d . . . H24A H 0.5823 0.5234 0.2206 0.152 Uiso 1 1 calc R . . H24B H 0.6322 0.6495 0.1787 0.152 Uiso 1 1 calc R . . H24C H 0.6551 0.6214 0.2701 0.152 Uiso 1 1 calc R . . C25 C 1.1616(8) 0.4964(7) 0.3179(4) 0.0521(16) Uani 1 1 d . . . H25A H 1.2323 0.4432 0.2824 0.078 Uiso 1 1 calc R . . H25B H 1.2008 0.5079 0.3685 0.078 Uiso 1 1 calc R . . H25C H 1.1446 0.5773 0.2921 0.078 Uiso 1 1 calc R . . C26 C 1.0256(7) 0.2662(5) 0.3907(4) 0.0417(13) Uani 1 1 d . . . H26A H 0.9349 0.2255 0.4063 0.063 Uiso 1 1 calc R . . H26B H 1.0716 0.2812 0.4386 0.063 Uiso 1 1 calc R . . H26C H 1.0931 0.2126 0.3538 0.063 Uiso 1 1 calc R . . C27 C 0.8531(9) 0.5238(7) 0.4137(4) 0.0576(17) Uani 1 1 d . . . H27A H 0.8260 0.6024 0.3876 0.086 Uiso 1 1 calc R . . H27B H 0.9034 0.5401 0.4598 0.086 Uiso 1 1 calc R . . H27C H 0.7644 0.4818 0.4319 0.086 Uiso 1 1 calc R . . N01 N 0.5480(5) 0.1387(4) 0.1930(3) 0.0338(10) Uani 1 1 d . . . N02 N 0.5722(5) 0.1264(4) 0.3202(3) 0.0322(9) Uani 1 1 d . . . N03 N 0.8996(6) 0.3941(4) 0.2533(3) 0.0397(11) Uani 1 1 d . . . Si01 Si 0.98091(17) 0.42038(14) 0.33906(9) 0.0335(4) Uani 1 1 d . . . Si02 Si 0.8480(2) 0.50342(19) 0.18228(13) 0.0577(6) Uani 1 1 d . . . Cl1 Cl 1.03883(17) 0.07974(18) 0.19510(12) 0.0634(6) Uani 1 1 d . . . Co01 Co 0.85334(7) 0.22785(6) 0.23027(4) 0.0316(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C01 0.024(2) 0.032(3) 0.032(3) -0.003(2) -0.0017(19) 0.002(2) C02 0.029(3) 0.061(4) 0.046(3) 0.000(3) -0.006(2) -0.012(3) C03 0.034(3) 0.053(4) 0.042(3) 0.005(3) -0.001(2) -0.013(3) C04 0.029(3) 0.036(3) 0.031(3) 0.001(2) -0.002(2) -0.006(2) C05 0.047(3) 0.036(3) 0.039(3) 0.004(2) -0.006(2) -0.005(2) C06 0.050(4) 0.040(3) 0.043(3) 0.014(2) -0.011(3) -0.005(3) C07 0.050(4) 0.052(4) 0.032(3) 0.011(2) -0.006(2) -0.015(3) C08 0.044(3) 0.049(3) 0.035(3) -0.004(2) 0.000(2) -0.009(3) C09 0.040(3) 0.042(3) 0.036(3) -0.002(2) 0.000(2) -0.001(2) C10 0.058(4) 0.049(4) 0.062(4) -0.010(3) -0.015(3) 0.013(3) C11 0.066(4) 0.034(3) 0.061(4) -0.002(3) -0.015(3) 0.006(3) C12 0.074(5) 0.071(5) 0.042(3) 0.009(3) -0.018(3) -0.023(4) C13 0.033(3) 0.035(3) 0.034(3) -0.003(2) -0.009(2) -0.003(2) C14 0.036(3) 0.039(3) 0.037(3) -0.005(2) -0.007(2) 0.000(2) C15 0.039(3) 0.045(3) 0.036(3) -0.001(2) -0.010(2) 0.006(2) C16 0.032(3) 0.052(3) 0.035(3) -0.004(2) -0.007(2) -0.004(2) C17 0.037(3) 0.041(3) 0.039(3) -0.011(2) -0.005(2) 0.005(2) C18 0.035(3) 0.039(3) 0.038(3) -0.002(2) -0.009(2) -0.006(2) C19 0.053(4) 0.041(3) 0.050(3) -0.006(3) -0.014(3) 0.003(3) C20 0.048(4) 0.064(4) 0.045(3) -0.008(3) -0.003(3) 0.019(3) C21 0.050(4) 0.063(4) 0.035(3) -0.002(3) -0.004(3) 0.000(3) C22 0.116(8) 0.108(7) 0.055(5) 0.027(5) -0.038(5) -0.055(6) C23 0.110(7) 0.066(5) 0.101(7) 0.046(5) -0.054(6) -0.044(5) C24 0.092(7) 0.091(7) 0.128(9) 0.021(6) -0.058(7) 0.019(6) C25 0.054(4) 0.053(4) 0.053(4) 0.006(3) -0.014(3) -0.019(3) C26 0.050(3) 0.034(3) 0.040(3) 0.004(2) -0.008(3) -0.001(2) C27 0.063(4) 0.050(4) 0.057(4) -0.010(3) -0.006(3) 0.009(3) N01 0.031(2) 0.037(2) 0.034(2) -0.0001(18) -0.0059(18) -0.0073(19) N02 0.030(2) 0.036(2) 0.031(2) 0.0000(17) -0.0021(17) -0.0040(18) N03 0.046(3) 0.036(2) 0.040(3) 0.0040(19) -0.012(2) -0.007(2) Si01 0.0356(8) 0.0295(7) 0.0358(8) -0.0002(6) -0.0066(6) -0.0012(6) Si02 0.0666(13) 0.0514(11) 0.0636(12) 0.0213(9) -0.0340(10) -0.0180(9) Cl1 0.0314(8) 0.0699(11) 0.0879(13) -0.0387(10) -0.0089(8) 0.0103(7) Co01 0.0266(4) 0.0344(4) 0.0335(4) -0.0035(3) -0.0024(3) -0.0025(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C01 N02 1.354(7) . ? C01 N01 1.359(7) . ? C01 Co01 2.054(5) . ? C02 C03 1.334(9) . ? C02 N01 1.388(7) . ? C03 N02 1.381(7) . ? C04 C09 1.395(8) . ? C04 C05 1.397(8) . ? C04 N02 1.447(7) . ? C05 C06 1.396(8) . ? C05 C11 1.503(8) . ? C06 C07 1.393(9) . ? C07 C08 1.390(9) . ? C07 C12 1.496(9) . ? C08 C09 1.380(8) . ? C09 C10 1.512(9) . ? C13 C18 1.390(8) . ? C13 C14 1.417(8) . ? C13 N01 1.436(7) . ? C14 C15 1.386(8) . ? C14 C20 1.510(8) . ? C15 C16 1.395(8) . ? C16 C17 1.376(8) . ? C16 C21 1.509(8) . ? C17 C18 1.396(8) . ? C18 C19 1.508(8) . ? C22 Si02 1.867(9) . ? C23 Si02 1.865(8) . ? C24 Si02 1.895(11) . ? C25 Si01 1.869(7) . ? C26 Si01 1.869(6) . ? C27 Si01 1.872(7) . ? N03 Si01 1.712(5) . ? N03 Si02 1.715(5) . ? N03 Co01 1.900(5) . ? Cl1 Co01 2.2234(17) . ? 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 N02 C01 N01 103.9(4) . . ? N02 C01 Co01 124.6(4) . . ? N01 C01 Co01 131.5(4) . . ? C03 C02 N01 106.8(5) . . ? C02 C03 N02 106.9(5) . . ? C09 C04 C05 122.7(5) . . ? C09 C04 N02 118.9(5) . . ? C05 C04 N02 118.3(5) . . ? C06 C05 C04 117.0(5) . . ? C06 C05 C11 121.6(5) . . ? C04 C05 C11 121.4(5) . . ? C07 C06 C05 122.2(5) . . ? C08 C07 C06 118.0(5) . . ? C08 C07 C12 121.1(6) . . ? C06 C07 C12 121.0(6) . . ? C09 C08 C07 122.5(6) . . ? C08 C09 C04 117.6(5) . . ? C08 C09 C10 122.1(5) . . ? C04 C09 C10 120.3(5) . . ? C18 C13 C14 122.4(5) . . ? C18 C13 N01 119.3(5) . . ? C14 C13 N01 118.2(5) . . ? C15 C14 C13 117.1(5) . . ? C15 C14 C20 120.7(5) . . ? C13 C14 C20 122.2(5) . . ? C14 C15 C16 122.1(5) . . ? C17 C16 C15 118.5(5) . . ? C17 C16 C21 120.9(5) . . ? C15 C16 C21 120.6(5) . . ? C16 C17 C18 122.7(5) . . ? C13 C18 C17 117.1(5) . . ? C13 C18 C19 122.5(5) . . ? C17 C18 C19 120.4(5) . . ? C01 N01 C02 111.0(5) . . ? C01 N01 C13 125.2(4) . . ? C02 N01 C13 123.8(5) . . ? C01 N02 C03 111.4(4) . . ? C01 N02 C04 124.9(4) . . ? C03 N02 C04 123.7(4) . . ? Si01 N03 Si02 127.6(3) . . ? Si01 N03 Co01 119.6(3) . . ? Si02 N03 Co01 112.7(3) . . ? N03 Si01 C25 114.0(3) . . ? N03 Si01 C26 109.7(3) . . ? C25 Si01 C26 106.0(3) . . ? N03 Si01 C27 111.4(3) . . ? C25 Si01 C27 107.2(3) . . ? C26 Si01 C27 108.3(3) . . ? N03 Si02 C23 114.3(3) . . ? N03 Si02 C22 108.4(4) . . ? C23 Si02 C22 107.4(4) . . ? N03 Si02 C24 110.8(4) . . ? C23 Si02 C24 106.9(5) . . ? C22 Si02 C24 108.8(5) . . ? N03 Co01 C01 126.7(2) . . ? N03 Co01 Cl1 119.34(17) . . ? C01 Co01 Cl1 113.59(15) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 1.433 _refine_diff_density_min -1.124 _refine_diff_density_rms 0.208 data_CoSIMesClmuCl2 _database_code_depnum_ccdc_archive 'CCDC 918512' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H52 Cl4 Co2 N4 O0' _chemical_formula_weight 872.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9613(4) _cell_length_b 12.2767(3) _cell_length_c 14.9613(4) _cell_angle_alpha 90.00 _cell_angle_beta 117.21 _cell_angle_gamma 90.00 _cell_volume 2443.94(11) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 31637 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_absorpt_coefficient_mu 0.927 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8735 _exptl_absorpt_correction_T_max 0.8735 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius Roper CCD on k goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22146 _diffrn_reflns_av_R_equivalents 0.0815 _diffrn_reflns_av_sigmaI/netI 0.1142 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.51 _reflns_number_total 4888 _reflns_number_gt 3481 _reflns_threshold_expression >2\s(I) _computing_data_collection COLLECT _computing_cell_refinement 'DENZO & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics ORTEP _computing_publication_material PLATON _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^ > 2\s(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4888 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0994 _refine_ls_R_factor_gt 0.0729 _refine_ls_wR_factor_ref 0.2455 _refine_ls_wR_factor_gt 0.2243 _refine_ls_goodness_of_fit_ref 0.868 _refine_ls_restrained_S_all 0.868 _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 _platon_squeeze_void_content 1 0.500 0.000 0.500 222 35 ' ' 2 0.000 0.500 0.000 222 35 ' ' _platon_squeeze_details ; ; 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 0.57977(4) 0.56857(4) 0.07558(4) 0.0219(2) Uani 1 1 d . . . Cl2 Cl 0.74443(9) 0.52500(11) 0.15043(10) 0.0405(4) Uani 1 1 d . . . N1 N 0.5272(3) 0.7340(3) 0.1945(3) 0.0264(8) Uani 1 1 d . . . C1 C 0.4911(3) 0.6506(4) 0.2372(3) 0.0255(9) Uani 1 1 d . . . C7 C 0.5553(3) 0.7158(4) 0.1229(3) 0.0226(8) Uani 1 1 d . . . C6 C 0.3910(3) 0.6173(4) 0.1840(3) 0.0291(9) Uani 1 1 d . . . N2 N 0.5708(3) 0.8113(3) 0.0911(3) 0.0253(8) Uani 1 1 d . . . C11 C 0.5109(3) 0.8249(4) -0.0908(3) 0.0270(9) Uani 1 1 d . . . C5 C 0.3562(4) 0.5341(5) 0.2222(4) 0.0366(11) Uani 1 1 d . . . H5 H 0.2884 0.5107 0.1857 0.044 Uiso 1 1 calc R . . C9 C 0.6899(3) 0.8449(4) 0.0241(3) 0.0279(9) Uani 1 1 d . . . C8 C 0.5913(3) 0.8266(4) 0.0061(3) 0.0266(9) Uani 1 1 d . . . C2 C 0.5560(4) 0.6032(4) 0.3301(3) 0.0301(10) Uani 1 1 d . . . C3 C 0.5173(4) 0.5218(4) 0.3668(4) 0.0364(11) Uani 1 1 d . . . H3 H 0.5593 0.4908 0.4306 0.044 Uiso 1 1 calc R . . C4 C 0.4186(4) 0.4839(4) 0.3132(4) 0.0351(11) Uani 1 1 d . . . C12 C 0.7073(4) 0.8645(4) -0.0584(4) 0.0344(11) Uani 1 1 d . . . H12 H 0.7740 0.8774 -0.0479 0.041 Uiso 1 1 calc R . . C14 C 0.5324(4) 0.8436(4) -0.1706(3) 0.0298(10) Uani 1 1 d . . . H14 H 0.4792 0.8413 -0.2373 0.036 Uiso 1 1 calc R . . C13 C 0.6292(4) 0.8656(4) -0.1558(3) 0.0309(10) Uani 1 1 d . . . C16 C 0.5457(4) 0.9056(4) 0.1358(4) 0.0320(10) Uani 1 1 d . . . H16A H 0.4854 0.9439 0.0856 0.038 Uiso 1 1 calc R . . H16B H 0.6025 0.9575 0.1651 0.038 Uiso 1 1 calc R . . C17 C 0.5254(4) 0.8517(4) 0.2180(4) 0.0371(11) Uani 1 1 d . . . H17A H 0.5785 0.8697 0.2862 0.044 Uiso 1 1 calc R . . H17B H 0.4592 0.8735 0.2121 0.044 Uiso 1 1 calc R . . C18 C 0.3192(4) 0.6700(5) 0.0833(4) 0.0413(12) Uani 1 1 d . . . H18A H 0.3289 0.7492 0.0879 0.062 Uiso 1 1 calc R . . H18B H 0.2496 0.6532 0.0678 0.062 Uiso 1 1 calc R . . H18C H 0.3333 0.6414 0.0299 0.062 Uiso 1 1 calc R . . C19 C 0.6633(4) 0.6345(5) 0.3831(4) 0.0452(13) Uani 1 1 d . . . H19A H 0.6999 0.5828 0.4377 0.068 Uiso 1 1 calc R . . H19B H 0.6693 0.7079 0.4111 0.068 Uiso 1 1 calc R . . H19C H 0.6918 0.6337 0.3358 0.068 Uiso 1 1 calc R . . C20 C 0.3788(6) 0.3933(6) 0.3532(6) 0.0569(16) Uani 1 1 d . . . H20A H 0.4343 0.3609 0.4125 0.085 Uiso 1 1 calc R . . H20B H 0.3476 0.3374 0.3012 0.085 Uiso 1 1 calc R . . H20C H 0.3287 0.4227 0.3718 0.085 Uiso 1 1 calc R . . Cl3 Cl 0.4856(2) 0.4470(2) 0.0810(3) 0.1142(11) Uani 1 1 d . . . C21 C 0.6483(5) 0.8924(5) -0.2441(4) 0.0437(13) Uani 1 1 d . . . H21A H 0.5951 0.8604 -0.3053 0.066 Uiso 1 1 calc R . . H21B H 0.7135 0.8626 -0.2324 0.066 Uiso 1 1 calc R . . H21C H 0.6487 0.9717 -0.2518 0.066 Uiso 1 1 calc R . . C22 C 0.4058(4) 0.8020(4) -0.1073(4) 0.0337(10) Uani 1 1 d . . . H22A H 0.3577 0.8248 -0.1752 0.051 Uiso 1 1 calc R . . H22B H 0.3929 0.8424 -0.0579 0.051 Uiso 1 1 calc R . . H22C H 0.3982 0.7238 -0.0995 0.051 Uiso 1 1 calc R . . C25 C 0.7755(4) 0.8404(5) 0.1304(4) 0.0390(12) Uani 1 1 d . . . H25A H 0.7648 0.8955 0.1719 0.058 Uiso 1 1 calc R . . H25B H 0.8393 0.8548 0.1289 0.058 Uiso 1 1 calc R . . H25C H 0.7778 0.7680 0.1589 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0223(4) 0.0202(3) 0.0208(3) -0.0009(2) 0.0077(3) 0.0011(2) Cl2 0.0252(6) 0.0454(8) 0.0391(7) -0.0048(5) 0.0045(5) 0.0088(5) N1 0.0288(18) 0.0254(19) 0.0271(18) -0.0059(15) 0.0147(15) -0.0052(15) C1 0.025(2) 0.029(2) 0.0239(19) -0.0006(17) 0.0124(17) -0.0013(17) C7 0.0196(19) 0.023(2) 0.0213(19) 0.0021(16) 0.0057(16) 0.0029(15) C6 0.024(2) 0.033(2) 0.031(2) 0.0020(19) 0.0125(18) 0.0013(18) N2 0.031(2) 0.0168(18) 0.0283(18) -0.0012(13) 0.0132(16) -0.0010(13) C11 0.027(2) 0.022(2) 0.030(2) -0.0001(17) 0.0118(18) 0.0002(16) C5 0.031(3) 0.044(3) 0.038(3) -0.009(2) 0.019(2) -0.009(2) C9 0.025(2) 0.032(2) 0.023(2) 0.0033(17) 0.0072(17) -0.0013(17) C8 0.034(2) 0.022(2) 0.023(2) 0.0023(16) 0.0120(18) -0.0018(17) C2 0.032(2) 0.030(2) 0.028(2) -0.0018(19) 0.0141(19) -0.0010(19) C3 0.038(3) 0.032(3) 0.037(3) 0.006(2) 0.016(2) 0.002(2) C4 0.039(3) 0.036(3) 0.039(3) 0.005(2) 0.025(2) -0.003(2) C12 0.029(2) 0.038(3) 0.037(2) 0.002(2) 0.016(2) -0.006(2) C14 0.033(2) 0.027(2) 0.026(2) -0.0008(17) 0.0112(18) 0.0035(18) C13 0.038(2) 0.025(2) 0.030(2) 0.0011(18) 0.0161(19) 0.0032(19) C16 0.041(3) 0.018(2) 0.035(2) -0.0078(18) 0.016(2) -0.0028(18) C17 0.046(3) 0.030(2) 0.037(3) -0.006(2) 0.020(2) 0.000(2) C18 0.024(2) 0.056(3) 0.034(2) 0.009(2) 0.005(2) -0.004(2) C19 0.037(3) 0.050(3) 0.037(3) 0.004(2) 0.007(2) -0.004(2) C20 0.063(4) 0.050(3) 0.066(4) 0.007(3) 0.037(3) -0.012(3) Cl3 0.0871(19) 0.0875(17) 0.138(3) -0.0347(16) 0.0252(17) -0.0010(13) C21 0.048(3) 0.054(3) 0.034(3) 0.007(2) 0.023(2) 0.002(3) C22 0.031(2) 0.036(3) 0.030(2) 0.003(2) 0.0099(19) 0.0043(19) C25 0.027(2) 0.051(3) 0.029(2) 0.008(2) 0.0045(19) -0.002(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C7 2.035(4) . ? Co1 Cl3 2.080(4) . ? Co1 Cl3 2.094(4) 3_665 ? Co1 Cl2 2.2553(13) . ? Co1 Co1 2.9513(11) 3_665 ? N1 C7 1.336(6) . ? N1 C1 1.436(6) . ? N1 C17 1.489(6) . ? C1 C6 1.398(6) . ? C1 C2 1.407(7) . ? C7 N2 1.326(6) . ? C6 C5 1.383(7) . ? C6 C18 1.537(7) . ? N2 C8 1.452(6) . ? N2 C16 1.468(6) . ? C11 C14 1.391(7) . ? C11 C8 1.398(6) . ? C11 C22 1.503(7) . ? C5 C4 1.395(8) . ? C5 H5 0.9500 . ? C9 C12 1.395(7) . ? C9 C8 1.391(7) . ? C9 C25 1.519(6) . ? C2 C3 1.388(7) . ? C2 C19 1.481(7) . ? C3 C4 1.398(8) . ? C3 H3 0.9500 . ? C4 C20 1.508(8) . ? C12 C13 1.390(7) . ? C12 H12 0.9500 . ? C14 C13 1.388(7) . ? C14 H14 0.9500 . ? C13 C21 1.509(7) . ? C16 C17 1.545(7) . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Cl3 Co1 2.094(4) 3_665 ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 Co1 Cl3 113.00(15) . . ? C7 Co1 Cl3 113.83(14) . 3_665 ? Cl3 Co1 Cl3 90.01(17) . 3_665 ? C7 Co1 Cl2 111.57(12) . . ? Cl3 Co1 Cl2 114.58(10) . . ? Cl3 Co1 Cl2 112.30(10) 3_665 . ? C7 Co1 Co1 124.20(11) . 3_665 ? Cl3 Co1 Co1 45.21(10) . 3_665 ? Cl3 Co1 Co1 44.80(10) 3_665 3_665 ? Cl2 Co1 Co1 124.22(5) . 3_665 ? C7 N1 C1 123.8(4) . . ? C7 N1 C17 113.5(4) . . ? C1 N1 C17 122.4(4) . . ? C6 C1 C2 121.1(4) . . ? C6 C1 N1 118.6(4) . . ? C2 C1 N1 120.3(4) . . ? N1 C7 N2 108.1(4) . . ? N1 C7 Co1 127.0(3) . . ? N2 C7 Co1 124.9(3) . . ? C5 C6 C1 119.3(4) . . ? C5 C6 C18 119.3(4) . . ? C1 C6 C18 121.4(4) . . ? C7 N2 C8 124.8(4) . . ? C7 N2 C16 114.3(4) . . ? C8 N2 C16 119.9(4) . . ? C14 C11 C8 117.4(4) . . ? C14 C11 C22 121.7(4) . . ? C8 C11 C22 120.9(4) . . ? C4 C5 C6 121.3(5) . . ? C4 C5 H5 119.3 . . ? C6 C5 H5 119.3 . . ? C12 C9 C8 117.8(4) . . ? C12 C9 C25 121.6(4) . . ? C8 C9 C25 120.6(4) . . ? C9 C8 C11 122.6(4) . . ? C9 C8 N2 118.8(4) . . ? C11 C8 N2 118.7(4) . . ? C3 C2 C1 117.7(4) . . ? C3 C2 C19 121.4(5) . . ? C1 C2 C19 120.7(4) . . ? C4 C3 C2 122.3(5) . . ? C4 C3 H3 118.8 . . ? C2 C3 H3 118.8 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 C20 120.3(5) . . ? C3 C4 C20 121.5(5) . . ? C9 C12 C13 121.5(4) . . ? C9 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C13 C14 C11 122.0(4) . . ? C13 C14 H14 119.0 . . ? C11 C14 H14 119.0 . . ? C14 C13 C12 118.8(5) . . ? C14 C13 C21 120.3(4) . . ? C12 C13 C21 121.0(5) . . ? N2 C16 C17 102.1(4) . . ? N2 C16 H16A 111.4 . . ? C17 C16 H16A 111.4 . . ? N2 C16 H16B 111.4 . . ? C17 C16 H16B 111.4 . . ? H16A C16 H16B 109.2 . . ? N1 C17 C16 101.3(4) . . ? N1 C17 H17A 111.5 . . ? C16 C17 H17A 111.5 . . ? N1 C17 H17B 111.5 . . ? C16 C17 H17B 111.5 . . ? H17A C17 H17B 109.3 . . ? C6 C18 H18A 109.5 . . ? C6 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C6 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C2 C19 H19A 109.5 . . ? C2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C4 C20 H20A 109.5 . . ? C4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Co1 Cl3 Co1 89.99(17) . 3_665 ? C13 C21 H21A 109.5 . . ? C13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C11 C22 H22A 109.5 . . ? C11 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C11 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C9 C25 H25A 109.5 . . ? C9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.872 _refine_diff_density_max 0.804 _refine_diff_density_min -1.220 _refine_diff_density_rms 0.155 data_CoSIPrClmuCl2 _database_code_depnum_ccdc_archive 'CCDC 918513' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H76 Cl4 Co2 N4' _chemical_formula_weight 1040.85 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4957(5) _cell_length_b 13.9842(8) _cell_length_c 16.6676(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.676(3) _cell_angle_gamma 90.00 _cell_volume 2898.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 12693 _cell_measurement_theta_min 0.998 _cell_measurement_theta_max 27.485 _exptl_crystal_description plate _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.193 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1100 _exptl_absorpt_coefficient_mu 0.792 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.93 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15312 _diffrn_reflns_av_R_equivalents 0.1392 _diffrn_reflns_av_sigmaI/netI 0.2982 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6615 _reflns_number_gt 3134 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^ > 2\s(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^)+(0.0795P)^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 6615 _refine_ls_number_parameters 297 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2580 _refine_ls_R_factor_gt 0.0969 _refine_ls_wR_factor_ref 0.2519 _refine_ls_wR_factor_gt 0.1702 _refine_ls_goodness_of_fit_ref 1.096 _refine_ls_restrained_S_all 1.096 _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 0.6026(5) 0.3623(4) 0.6463(4) 0.0192(16) Uani 1 1 d . . . C2 C 0.6105(6) 0.2599(5) 0.7582(5) 0.041(2) Uani 1 1 d . . . H2A H 0.5623 0.2090 0.7712 0.049 Uiso 1 1 calc R . . H2B H 0.6472 0.2852 0.8076 0.049 Uiso 1 1 calc R . . C3 C 0.6892(6) 0.2256(5) 0.7017(4) 0.036(2) Uani 1 1 d . . . H3A H 0.7606 0.2178 0.7295 0.044 Uiso 1 1 calc R . . H3B H 0.6662 0.1655 0.6765 0.044 Uiso 1 1 calc R . . C4 C 0.7562(5) 0.3030(5) 0.5783(4) 0.0223(16) Uani 1 1 d . . . C5 C 0.7300(6) 0.2447(5) 0.5103(4) 0.036(2) Uani 1 1 d . . . C6 C 0.8042(8) 0.2435(6) 0.4513(5) 0.054(3) Uani 1 1 d . . . H6 H 0.7906 0.2046 0.4063 0.065 Uiso 1 1 calc R . . C7 C 0.8952(7) 0.2983(7) 0.4590(6) 0.059(3) Uani 1 1 d . . . H7 H 0.9417 0.2976 0.4187 0.071 Uiso 1 1 calc R . . C8 C 0.9179(7) 0.3537(6) 0.5257(6) 0.050(2) Uani 1 1 d . . . H8 H 0.9809 0.3895 0.5307 0.060 Uiso 1 1 calc R . . C9 C 0.8496(6) 0.3582(5) 0.5863(4) 0.0305(18) Uani 1 1 d . . . C10 C 0.8780(6) 0.4215(6) 0.6606(5) 0.037(2) Uani 1 1 d . . . H10 H 0.8108 0.4397 0.6822 0.044 Uiso 1 1 calc R . . C11 C 0.9453(7) 0.3661(7) 0.7253(6) 0.067(3) Uani 1 1 d . . . H11A H 0.9025 0.3163 0.7457 0.101 Uiso 1 1 calc R . . H11B H 0.9701 0.4086 0.7685 0.101 Uiso 1 1 calc R . . H11C H 1.0060 0.3384 0.7029 0.101 Uiso 1 1 calc R . . C12 C 0.9368(7) 0.5132(6) 0.6412(6) 0.058(3) Uani 1 1 d . . . H12A H 1.0078 0.4977 0.6279 0.087 Uiso 1 1 calc R . . H12B H 0.9417 0.5548 0.6872 0.087 Uiso 1 1 calc R . . H12C H 0.8978 0.5447 0.5962 0.087 Uiso 1 1 calc R . . C13 C 0.6282(6) 0.1830(6) 0.5014(5) 0.048(2) Uani 1 1 d . . . H13 H 0.5877 0.1968 0.5475 0.057 Uiso 1 1 calc R . . C14 C 0.6565(7) 0.0760(6) 0.5046(7) 0.077(3) Uani 1 1 d . . . H14A H 0.6957 0.0600 0.4597 0.116 Uiso 1 1 calc R . . H14B H 0.5916 0.0389 0.5021 0.116 Uiso 1 1 calc R . . H14C H 0.7000 0.0622 0.5540 0.116 Uiso 1 1 calc R . . C15 C 0.5554(8) 0.2089(8) 0.4242(7) 0.099(4) Uani 1 1 d . . . H15A H 0.5949 0.2008 0.3781 0.149 Uiso 1 1 calc R . . H15B H 0.5325 0.2742 0.4272 0.149 Uiso 1 1 calc R . . H15C H 0.4936 0.1677 0.4192 0.149 Uiso 1 1 calc R . . C16 C 0.4502(5) 0.3731(5) 0.7286(4) 0.0267(18) Uani 1 1 d . . . C17 C 0.3565(6) 0.3384(5) 0.6850(4) 0.0305(18) Uani 1 1 d . . . C18 C 0.2590(6) 0.3719(6) 0.7047(5) 0.045(2) Uani 1 1 d . . . H18 H 0.1957 0.3500 0.6766 0.054 Uiso 1 1 calc R . . C19 C 0.2546(6) 0.4375(7) 0.7657(6) 0.049(2) Uani 1 1 d . . . H19 H 0.1883 0.4596 0.7786 0.059 Uiso 1 1 calc R . . C20 C 0.3471(6) 0.4707(6) 0.8076(5) 0.048(2) Uani 1 1 d . . . H20 H 0.3424 0.5156 0.8483 0.057 Uiso 1 1 calc R . . C21 C 0.4488(5) 0.4385(5) 0.7905(4) 0.0309(19) Uani 1 1 d . . . C22 C 0.5483(6) 0.4773(6) 0.8384(5) 0.041(2) Uani 1 1 d . . . H22 H 0.6097 0.4636 0.8078 0.049 Uiso 1 1 calc R . . C23 C 0.5674(7) 0.4250(7) 0.9189(5) 0.062(3) Uani 1 1 d . . . H23A H 0.5080 0.4364 0.9500 0.093 Uiso 1 1 calc R . . H23B H 0.6325 0.4481 0.9480 0.093 Uiso 1 1 calc R . . H23C H 0.5738 0.3577 0.9094 0.093 Uiso 1 1 calc R . . C24 C 0.5444(7) 0.5855(6) 0.8508(6) 0.058(3) Uani 1 1 d . . . H24A H 0.5246 0.6163 0.8000 0.087 Uiso 1 1 calc R . . H24B H 0.6139 0.6078 0.8726 0.087 Uiso 1 1 calc R . . H24C H 0.4923 0.6004 0.8875 0.087 Uiso 1 1 calc R . . C25 C 0.3595(6) 0.2644(7) 0.6182(5) 0.050(2) Uani 1 1 d . . . H25 H 0.4269 0.2729 0.5937 0.059 Uiso 1 1 calc R . . C26 C 0.3587(11) 0.1651(8) 0.6517(8) 0.120(5) Uani 1 1 d . . . H26A H 0.4130 0.1596 0.6964 0.180 Uiso 1 1 calc R . . H26B H 0.3730 0.1201 0.6107 0.180 Uiso 1 1 calc R . . H26C H 0.2895 0.1520 0.6697 0.180 Uiso 1 1 calc R . . C27 C 0.2650(8) 0.2742(7) 0.5503(5) 0.077(3) Uani 1 1 d . . . H27A H 0.2775 0.2329 0.5063 0.115 Uiso 1 1 calc R . . H27B H 0.2604 0.3392 0.5318 0.115 Uiso 1 1 calc R . . H27C H 0.1988 0.2566 0.5711 0.115 Uiso 1 1 calc R . . N1 N 0.5521(4) 0.3358(4) 0.7102(3) 0.0234(14) Uani 1 1 d . . . N2 N 0.6865(4) 0.3041(4) 0.6418(3) 0.0219(13) Uani 1 1 d . . . Cl2 Cl 0.60830(15) 0.47785(14) 0.44880(11) 0.0373(5) Uani 1 1 d . . . Cl3 Cl 0.65977(16) 0.60261(14) 0.64890(12) 0.0426(6) Uani 1 1 d . . . Co1 Co 0.57201(7) 0.48494(6) 0.58165(5) 0.0200(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.014(3) 0.017(4) 0.025(4) -0.003(3) -0.007(3) 0.002(3) C2 0.053(5) 0.028(5) 0.044(5) 0.021(4) 0.013(4) 0.010(4) C3 0.041(5) 0.027(5) 0.041(5) 0.013(4) 0.001(4) 0.003(4) C4 0.021(4) 0.015(4) 0.030(4) 0.002(3) -0.002(3) 0.009(3) C5 0.041(5) 0.032(5) 0.033(5) -0.008(4) -0.007(4) 0.009(4) C6 0.083(7) 0.046(6) 0.037(6) -0.017(4) 0.019(5) 0.017(5) C7 0.068(7) 0.057(7) 0.058(7) -0.008(5) 0.036(5) -0.003(5) C8 0.042(5) 0.047(6) 0.064(6) -0.006(5) 0.021(5) 0.000(4) C9 0.035(4) 0.021(4) 0.036(5) 0.001(4) 0.005(4) 0.006(4) C10 0.024(4) 0.041(5) 0.043(5) -0.002(4) -0.003(4) -0.001(4) C11 0.051(6) 0.075(8) 0.070(7) -0.001(6) -0.020(5) -0.008(5) C12 0.056(6) 0.034(5) 0.084(7) -0.014(5) 0.009(5) -0.010(4) C13 0.049(5) 0.037(5) 0.055(6) -0.023(5) -0.008(4) 0.006(4) C14 0.065(7) 0.033(6) 0.134(10) -0.023(6) 0.009(7) -0.006(5) C15 0.096(8) 0.071(8) 0.116(10) -0.035(7) -0.061(8) 0.017(6) C16 0.028(4) 0.028(4) 0.024(4) 0.013(4) 0.008(3) -0.004(3) C17 0.031(4) 0.032(5) 0.030(5) 0.003(4) 0.011(4) 0.000(4) C18 0.032(5) 0.050(6) 0.053(6) 0.000(5) 0.003(4) -0.015(4) C19 0.020(4) 0.059(6) 0.071(7) 0.008(5) 0.018(5) -0.001(4) C20 0.048(5) 0.042(6) 0.058(6) -0.006(5) 0.026(5) -0.005(4) C21 0.028(4) 0.037(5) 0.030(5) 0.007(4) 0.016(4) 0.000(4) C22 0.048(5) 0.040(5) 0.036(5) -0.004(4) 0.011(4) -0.006(4) C23 0.071(6) 0.075(7) 0.038(6) 0.007(5) -0.004(5) -0.024(5) C24 0.061(6) 0.044(6) 0.072(7) -0.018(5) 0.020(5) -0.018(5) C25 0.029(4) 0.062(7) 0.060(6) -0.021(5) 0.018(4) -0.019(4) C26 0.169(13) 0.045(8) 0.136(12) -0.027(8) -0.034(10) 0.011(8) C27 0.094(8) 0.087(8) 0.050(6) -0.020(6) 0.004(6) -0.039(7) N1 0.030(3) 0.018(3) 0.025(3) 0.009(3) 0.013(3) 0.003(3) N2 0.025(3) 0.015(3) 0.026(3) 0.006(3) 0.002(3) 0.001(3) Cl2 0.0403(11) 0.0401(12) 0.0310(11) 0.0035(9) 0.0004(9) 0.0082(9) Cl3 0.0530(12) 0.0315(12) 0.0394(12) -0.0090(9) -0.0142(10) -0.0048(10) Co1 0.0261(5) 0.0146(5) 0.0183(5) 0.0018(4) -0.0031(4) 0.0029(4) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 1.335(8) . ? C1 N1 1.343(8) . ? C1 Co1 2.041(6) . ? C2 N1 1.477(8) . ? C2 C3 1.506(10) . ? C3 N2 1.482(8) . ? C4 C9 1.395(9) . ? C4 C5 1.409(10) . ? C4 N2 1.435(8) . ? C5 C6 1.417(10) . ? C5 C13 1.532(10) . ? C6 C7 1.366(12) . ? C7 C8 1.361(12) . ? C8 C9 1.388(10) . ? C9 C10 1.535(10) . ? C10 C11 1.513(11) . ? C10 C12 1.528(10) . ? C13 C14 1.537(11) . ? C13 C15 1.544(11) . ? C16 C21 1.380(10) . ? C16 C17 1.403(10) . ? C16 N1 1.437(8) . ? C17 C18 1.375(10) . ? C17 C25 1.523(10) . ? C18 C19 1.374(11) . ? C19 C20 1.371(11) . ? C20 C21 1.403(10) . ? C21 C22 1.511(11) . ? C22 C24 1.529(11) . ? C22 C23 1.527(11) . ? C25 C26 1.496(13) . ? C25 C27 1.559(12) . ? Cl2 Co1 2.306(2) . ? Cl2 Co1 2.319(2) 3_666 ? Cl3 Co1 2.219(2) . ? Co1 Cl2 2.319(2) 3_666 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 108.0(6) . . ? N2 C1 Co1 126.1(5) . . ? N1 C1 Co1 124.9(5) . . ? N1 C2 C3 102.0(5) . . ? N2 C3 C2 102.3(6) . . ? C9 C4 C5 121.5(7) . . ? C9 C4 N2 119.1(6) . . ? C5 C4 N2 119.3(6) . . ? C4 C5 C6 116.7(7) . . ? C4 C5 C13 121.9(7) . . ? C6 C5 C13 121.4(7) . . ? C7 C6 C5 121.7(8) . . ? C8 C7 C6 120.0(8) . . ? C7 C8 C9 121.8(8) . . ? C8 C9 C4 118.3(7) . . ? C8 C9 C10 120.2(7) . . ? C4 C9 C10 121.4(6) . . ? C11 C10 C12 109.6(7) . . ? C11 C10 C9 110.4(7) . . ? C12 C10 C9 113.0(7) . . ? C5 C13 C14 111.0(7) . . ? C5 C13 C15 111.3(8) . . ? C14 C13 C15 111.8(7) . . ? C21 C16 C17 123.0(6) . . ? C21 C16 N1 118.5(6) . . ? C17 C16 N1 118.4(6) . . ? C18 C17 C16 118.2(7) . . ? C18 C17 C25 119.5(7) . . ? C16 C17 C25 122.3(6) . . ? C17 C18 C19 120.3(7) . . ? C20 C19 C18 120.7(8) . . ? C19 C20 C21 121.4(8) . . ? C16 C21 C20 116.4(7) . . ? C16 C21 C22 124.2(6) . . ? C20 C21 C22 119.4(7) . . ? C21 C22 C24 113.1(7) . . ? C21 C22 C23 110.0(6) . . ? C24 C22 C23 111.1(7) . . ? C26 C25 C17 110.9(8) . . ? C26 C25 C27 108.7(8) . . ? C17 C25 C27 113.5(7) . . ? C1 N1 C16 124.4(5) . . ? C1 N1 C2 112.5(5) . . ? C16 N1 C2 123.1(5) . . ? C1 N2 C4 125.8(5) . . ? C1 N2 C3 112.3(5) . . ? C4 N2 C3 120.9(5) . . ? Co1 Cl2 Co1 85.49(7) . 3_666 ? C1 Co1 Cl3 107.40(19) . . ? C1 Co1 Cl2 115.24(19) . . ? Cl3 Co1 Cl2 112.50(8) . . ? C1 Co1 Cl2 115.55(18) . 3_666 ? Cl3 Co1 Cl2 111.41(8) . 3_666 ? Cl2 Co1 Cl2 94.51(7) . 3_666 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.528 _refine_diff_density_min -0.999 _refine_diff_density_rms 0.226 data_complex2b _database_code_depnum_ccdc_archive 'CCDC 918514' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H51 Cl Co N4' _chemical_formula_weight 622.18 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 monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 16.017(3) _cell_length_b 8.3798(15) _cell_length_c 28.990(6) _cell_angle_alpha 90.00 _cell_angle_beta 97.102(4) _cell_angle_gamma 90.00 _cell_volume 3861.1(13) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.076 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1344 _exptl_absorpt_coefficient_mu 0.539 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7744 _exptl_absorpt_correction_T_max 0.9736 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21869 _diffrn_reflns_av_R_equivalents 0.0443 _diffrn_reflns_av_sigmaI/netI 0.0692 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.95 _reflns_number_total 9158 _reflns_number_gt 5957 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^ > 2\s(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^)+(0.1146P)^2^+3.6876P] 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 9158 _refine_ls_number_parameters 377 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1139 _refine_ls_R_factor_gt 0.0773 _refine_ls_wR_factor_ref 0.2184 _refine_ls_wR_factor_gt 0.2023 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.015 _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 _platon_squeeze_void_content 1 0.500 -0.020 0.000 343 49 ' ' 2 1.000 -0.011 0.500 343 49 ' ' _platon_squeeze_details ; ; 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 0.96503(3) 0.41858(6) 0.835365(17) 0.02509(16) Uani 1 1 d . . . Cl1 Cl 1.06277(7) 0.57667(13) 0.87603(4) 0.0448(3) Uani 1 1 d . . . N1 N 0.8442(2) 0.4980(4) 0.82912(11) 0.0312(7) Uani 1 1 d . . . N2 N 0.9200(2) 0.4960(4) 0.77036(11) 0.0303(7) Uani 1 1 d . . . N3 N 0.9959(2) 0.1224(4) 0.89504(11) 0.0352(8) Uani 1 1 d . . . N4 N 1.0717(2) 0.1193(4) 0.83843(12) 0.0365(8) Uani 1 1 d . . . C1 C 0.7777(2) 0.5528(4) 0.85556(13) 0.0289(8) Uani 1 1 d . . . H1 H 0.7585 0.6576 0.8436 0.035 Uiso 1 1 calc R . . C2 C 0.7022(2) 0.4396(5) 0.85068(14) 0.0347(9) Uani 1 1 d . . . H2A H 0.6794 0.4310 0.8182 0.042 Uiso 1 1 calc R . . H2B H 0.7202 0.3343 0.8616 0.042 Uiso 1 1 calc R . . C3 C 0.6345(3) 0.5004(6) 0.87853(15) 0.0393(10) Uani 1 1 d . . . H3A H 0.5883 0.4249 0.8761 0.047 Uiso 1 1 calc R . . H3B H 0.6129 0.6013 0.8657 0.047 Uiso 1 1 calc R . . C4 C 0.6690(3) 0.5234(6) 0.93004(16) 0.0461(11) Uani 1 1 d . . . H4A H 0.6258 0.5704 0.9464 0.055 Uiso 1 1 calc R . . H4B H 0.6838 0.4204 0.9440 0.055 Uiso 1 1 calc R . . C5 C 0.7455(3) 0.6299(6) 0.93498(15) 0.0455(11) Uani 1 1 d . . . H5A H 0.7686 0.6350 0.9675 0.055 Uiso 1 1 calc R . . H5B H 0.7287 0.7369 0.9250 0.055 Uiso 1 1 calc R . . C6 C 0.8133(2) 0.5719(5) 0.90668(13) 0.0356(9) Uani 1 1 d . . . H6A H 0.8351 0.4703 0.9188 0.043 Uiso 1 1 calc R . . H6B H 0.8593 0.6479 0.9093 0.043 Uiso 1 1 calc R . . C7 C 0.8507(2) 0.5470(4) 0.78589(12) 0.0270(8) Uani 1 1 d . . . C8 C 0.9437(2) 0.5456(4) 0.72534(13) 0.0278(8) Uani 1 1 d . . . H8 H 0.9196 0.6512 0.7177 0.033 Uiso 1 1 calc R . . C9 C 0.9102(2) 0.4294(5) 0.68681(13) 0.0336(8) Uani 1 1 d . . . H9A H 0.8494 0.4232 0.6849 0.040 Uiso 1 1 calc R . . H9B H 0.9329 0.3238 0.6941 0.040 Uiso 1 1 calc R . . C10 C 0.9348(3) 0.4835(6) 0.63994(14) 0.0428(10) Uani 1 1 d . . . H10A H 0.9140 0.4072 0.6161 0.051 Uiso 1 1 calc R . . H10B H 0.9091 0.5860 0.6317 0.051 Uiso 1 1 calc R . . C11 C 1.0302(3) 0.4979(6) 0.64185(16) 0.0469(11) Uani 1 1 d . . . H11A H 1.0440 0.5398 0.6125 0.056 Uiso 1 1 calc R . . H11B H 1.0554 0.3929 0.6463 0.056 Uiso 1 1 calc R . . C12 C 1.0665(3) 0.6076(6) 0.68138(17) 0.0493(12) Uani 1 1 d . . . H12A H 1.0479 0.7160 0.6744 0.059 Uiso 1 1 calc R . . H12B H 1.1274 0.6059 0.6836 0.059 Uiso 1 1 calc R . . C13 C 1.0393(2) 0.5573(5) 0.72829(14) 0.0351(9) Uani 1 1 d . . . H13A H 1.0641 0.4547 0.7374 0.042 Uiso 1 1 calc R . . H13B H 1.0598 0.6347 0.7519 0.042 Uiso 1 1 calc R . . C14 C 0.7853(3) 0.6535(6) 0.75816(14) 0.0390(10) Uani 1 1 d . . . H14A H 0.7994 0.7635 0.7642 0.059 Uiso 1 1 calc R . . H14B H 0.7307 0.6319 0.7672 0.059 Uiso 1 1 calc R . . H14C H 0.7845 0.6321 0.7256 0.059 Uiso 1 1 calc R . . C15 C 1.0112(2) 0.1987(4) 0.85692(12) 0.0265(8) Uani 1 1 d . . . C16 C 1.0454(4) -0.0265(6) 0.90418(19) 0.0623(16) Uani 1 1 d . . . H16A H 1.0092 -0.1196 0.9027 0.075 Uiso 1 1 calc R . . H16B H 1.0795 -0.0232 0.9342 0.075 Uiso 1 1 calc R . . C17 C 1.1001(4) -0.0259(6) 0.86449(19) 0.0642(16) Uani 1 1 d . . . H17A H 1.1594 -0.0196 0.8763 0.077 Uiso 1 1 calc R . . H17B H 1.0903 -0.1205 0.8453 0.077 Uiso 1 1 calc R . . C18 C 1.1076(2) 0.1563(4) 0.79669(15) 0.0317(8) Uani 1 1 d . . . C19 C 1.0691(2) 0.0978(5) 0.75437(15) 0.0338(8) Uani 1 1 d . . . C20 C 1.1085(3) 0.1249(5) 0.71502(16) 0.0421(10) Uani 1 1 d . . . H20 H 1.0835 0.0870 0.6865 0.051 Uiso 1 1 calc R . . C21 C 1.1842(3) 0.2072(6) 0.7171(2) 0.0519(13) Uani 1 1 d . . . C22 C 1.2253(4) 0.2383(8) 0.6734(3) 0.088(2) Uani 1 1 d . . . H22A H 1.1929 0.1879 0.6473 0.133 Uiso 1 1 calc R . . H22B H 1.2813 0.1954 0.6772 0.133 Uiso 1 1 calc R . . H22C H 1.2276 0.3512 0.6680 0.133 Uiso 1 1 calc R . . C23 C 1.2199(3) 0.2629(6) 0.7597(2) 0.0524(13) Uani 1 1 d . . . H23 H 1.2700 0.3197 0.7613 0.063 Uiso 1 1 calc R . . C24 C 1.1842(3) 0.2380(5) 0.80000(18) 0.0425(11) Uani 1 1 d . . . C25 C 1.2262(3) 0.2986(7) 0.8466(2) 0.0659(16) Uani 1 1 d . . . H25A H 1.2740 0.3628 0.8419 0.099 Uiso 1 1 calc R . . H25B H 1.2441 0.2096 0.8662 0.099 Uiso 1 1 calc R . . H25C H 1.1868 0.3618 0.8612 0.099 Uiso 1 1 calc R . . C26 C 0.9858(3) 0.0106(6) 0.75161(18) 0.0488(12) Uani 1 1 d . . . H26A H 0.9911 -0.0784 0.7726 0.073 Uiso 1 1 calc R . . H26B H 0.9703 -0.0271 0.7205 0.073 Uiso 1 1 calc R . . H26C H 0.9433 0.0820 0.7600 0.073 Uiso 1 1 calc R . . C27 C 0.9360(3) 0.1604(4) 0.92620(13) 0.0305(8) Uani 1 1 d . . . C28 C 0.9638(3) 0.2391(5) 0.96802(13) 0.0327(9) Uani 1 1 d . . . C29 C 0.9071(3) 0.2665(5) 0.99914(14) 0.0404(10) Uani 1 1 d . . . H29 H 0.9250 0.3209 1.0266 0.048 Uiso 1 1 calc R . . C30 C 0.8255(3) 0.2166(6) 0.99111(16) 0.0507(13) Uani 1 1 d . . . C31 C 0.7649(4) 0.2430(9) 1.0261(2) 0.087(2) Uani 1 1 d . . . H31A H 0.7952 0.2439 1.0568 0.130 Uiso 1 1 calc R . . H31B H 0.7241 0.1586 1.0237 0.130 Uiso 1 1 calc R . . H31C H 0.7369 0.3435 1.0201 0.130 Uiso 1 1 calc R . . C32 C 0.7992(3) 0.1361(6) 0.94950(17) 0.0469(11) Uani 1 1 d . . . H32 H 0.7439 0.1004 0.9438 0.056 Uiso 1 1 calc R . . C33 C 0.8532(3) 0.1082(5) 0.91661(15) 0.0383(10) Uani 1 1 d . . . C34 C 0.8246(4) 0.0252(6) 0.87131(18) 0.0614(15) Uani 1 1 d . . . H34A H 0.7671 -0.0074 0.8708 0.092 Uiso 1 1 calc R . . H34B H 0.8592 -0.0669 0.8683 0.092 Uiso 1 1 calc R . . H34C H 0.8294 0.0970 0.8460 0.092 Uiso 1 1 calc R . . C35 C 1.0542(3) 0.2908(6) 0.97976(16) 0.0498(12) Uani 1 1 d . . . H35A H 1.0586 0.3628 1.0057 0.075 Uiso 1 1 calc R . . H35B H 1.0726 0.3437 0.9534 0.075 Uiso 1 1 calc R . . H35C H 1.0888 0.1989 0.9876 0.075 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0312(3) 0.0193(2) 0.0233(2) 0.00253(19) -0.00247(18) 0.0054(2) Cl1 0.0539(6) 0.0315(5) 0.0483(6) -0.0129(5) 0.0035(5) -0.0119(5) N1 0.0325(16) 0.0386(19) 0.0227(15) 0.0058(13) 0.0039(13) 0.0084(14) N2 0.0321(16) 0.0367(19) 0.0218(15) 0.0062(13) 0.0019(13) 0.0094(14) N3 0.055(2) 0.0183(16) 0.0307(17) 0.0056(12) -0.0006(15) 0.0138(14) N4 0.0473(19) 0.0219(17) 0.0406(19) 0.0055(14) 0.0072(16) 0.0167(14) C1 0.0322(18) 0.029(2) 0.0242(17) 0.0056(14) -0.0003(15) 0.0083(15) C2 0.036(2) 0.034(2) 0.033(2) -0.0028(16) 0.0001(16) 0.0037(16) C3 0.035(2) 0.044(3) 0.040(2) 0.0071(19) 0.0059(18) -0.0005(18) C4 0.042(2) 0.061(3) 0.037(2) 0.007(2) 0.012(2) 0.006(2) C5 0.042(2) 0.065(3) 0.030(2) -0.006(2) 0.0049(18) 0.001(2) C6 0.0328(19) 0.047(2) 0.0261(19) 0.0034(17) -0.0010(15) 0.0044(18) C7 0.0291(17) 0.029(2) 0.0217(17) 0.0018(14) -0.0002(14) 0.0070(14) C8 0.0317(18) 0.0265(19) 0.0249(18) 0.0046(14) 0.0016(15) 0.0037(14) C9 0.0356(19) 0.038(2) 0.0262(18) 0.0054(16) -0.0015(15) -0.0065(17) C10 0.055(3) 0.049(3) 0.0229(19) 0.0003(18) 0.0009(19) -0.002(2) C11 0.054(3) 0.055(3) 0.035(2) 0.008(2) 0.019(2) -0.001(2) C12 0.045(2) 0.054(3) 0.052(3) 0.009(2) 0.015(2) -0.011(2) C13 0.035(2) 0.038(2) 0.032(2) -0.0022(17) 0.0022(16) -0.0006(17) C14 0.038(2) 0.050(3) 0.028(2) 0.0126(18) 0.0026(17) 0.0163(19) C15 0.0332(18) 0.0193(17) 0.0248(18) -0.0019(13) -0.0049(14) 0.0013(14) C16 0.100(4) 0.032(2) 0.059(3) 0.020(2) 0.026(3) 0.035(3) C17 0.094(4) 0.046(3) 0.058(3) 0.025(2) 0.029(3) 0.038(3) C18 0.0306(19) 0.0224(19) 0.043(2) 0.0032(16) 0.0054(17) 0.0084(15) C19 0.0333(19) 0.0236(19) 0.045(2) 0.0014(17) 0.0066(17) 0.0034(16) C20 0.047(2) 0.040(2) 0.042(2) 0.0037(19) 0.012(2) 0.0101(19) C21 0.042(2) 0.044(3) 0.076(4) 0.016(3) 0.028(2) 0.014(2) C22 0.080(4) 0.082(5) 0.117(6) 0.030(4) 0.066(4) 0.027(4) C23 0.028(2) 0.035(2) 0.095(4) 0.009(3) 0.016(2) 0.0010(18) C24 0.0297(19) 0.027(2) 0.069(3) -0.003(2) -0.002(2) 0.0051(16) C25 0.045(3) 0.053(3) 0.093(4) -0.023(3) -0.015(3) 0.005(2) C26 0.040(2) 0.049(3) 0.056(3) -0.008(2) 0.001(2) -0.012(2) C27 0.043(2) 0.0235(19) 0.0230(18) 0.0037(14) -0.0032(16) 0.0026(16) C28 0.045(2) 0.0253(19) 0.0258(18) 0.0076(15) -0.0032(16) 0.0037(16) C29 0.063(3) 0.033(2) 0.0229(19) 0.0072(16) -0.0007(19) 0.013(2) C30 0.062(3) 0.058(3) 0.034(2) 0.027(2) 0.012(2) 0.023(2) C31 0.082(4) 0.127(6) 0.056(4) 0.044(4) 0.030(3) 0.043(4) C32 0.042(2) 0.048(3) 0.049(3) 0.023(2) 0.001(2) -0.002(2) C33 0.051(2) 0.024(2) 0.037(2) 0.0062(16) -0.0058(19) -0.0022(17) C34 0.082(4) 0.049(3) 0.045(3) -0.005(2) -0.022(3) -0.020(3) C35 0.060(3) 0.048(3) 0.037(2) 0.003(2) -0.015(2) -0.008(2) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 2.033(3) . ? Co1 N2 2.039(3) . ? Co1 C15 2.054(4) . ? Co1 Cl1 2.2670(11) . ? Co1 C7 2.433(3) . ? N1 C7 1.335(5) . ? N1 C1 1.462(5) . ? N2 C7 1.320(5) . ? N2 C8 1.463(5) . ? N3 C15 1.326(5) . ? N3 C27 1.433(5) . ? N3 C16 1.484(5) . ? N4 C15 1.340(5) . ? N4 C18 1.437(5) . ? N4 C17 1.474(5) . ? C1 C2 1.529(5) . ? C1 C6 1.529(5) . ? C1 H1 0.9800 . ? C2 C3 1.517(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.539(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.508(7) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.519(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C14 1.527(5) . ? C8 C9 1.528(5) . ? C8 C13 1.527(5) . ? C8 H8 0.9800 . ? C9 C10 1.530(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.525(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.527(7) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.537(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C16 C17 1.530(7) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C19 1.393(6) . ? C18 C24 1.398(6) . ? C19 C20 1.389(6) . ? C19 C26 1.514(6) . ? C20 C21 1.391(7) . ? C20 H20 0.9300 . ? C21 C23 1.375(8) . ? C21 C22 1.521(8) . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.379(7) . ? C23 H23 0.9300 . ? C24 C25 1.521(7) . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C33 1.391(6) . ? C27 C28 1.404(5) . ? C28 C29 1.377(6) . ? C28 C35 1.508(6) . ? C29 C30 1.365(7) . ? C29 H29 0.9300 . ? C30 C32 1.401(7) . ? C30 C31 1.503(7) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 C33 1.384(7) . ? C32 H32 0.9300 . ? C33 C34 1.506(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 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 N1 Co1 N2 65.77(13) . . ? N1 Co1 C15 128.60(15) . . ? N2 Co1 C15 129.77(14) . . ? N1 Co1 Cl1 116.32(11) . . ? N2 Co1 Cl1 115.93(11) . . ? C15 Co1 Cl1 99.58(10) . . ? N1 Co1 C7 33.27(12) . . ? N2 Co1 C7 32.86(12) . . ? C15 Co1 C7 142.43(13) . . ? Cl1 Co1 C7 117.98(10) . . ? C7 N1 C1 122.8(3) . . ? C7 N1 Co1 90.1(2) . . ? C1 N1 Co1 143.5(2) . . ? C7 N2 C8 122.3(3) . . ? C7 N2 Co1 90.2(2) . . ? C8 N2 Co1 144.5(2) . . ? C15 N3 C27 128.7(3) . . ? C15 N3 C16 113.9(4) . . ? C27 N3 C16 117.3(3) . . ? C15 N4 C18 127.9(3) . . ? C15 N4 C17 113.4(4) . . ? C18 N4 C17 118.7(3) . . ? N1 C1 C2 112.1(3) . . ? N1 C1 C6 109.4(3) . . ? C2 C1 C6 110.5(3) . . ? N1 C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? C6 C1 H1 108.2 . . ? C3 C2 C1 110.6(3) . . ? C3 C2 H2A 109.5 . . ? C1 C2 H2A 109.5 . . ? C3 C2 H2B 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? C2 C3 C4 111.3(3) . . ? C2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 . . ? H3A C3 H3B 108.0 . . ? C5 C4 C3 110.9(4) . . ? C5 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.0 . . ? C4 C5 C6 112.7(4) . . ? C4 C5 H5A 109.1 . . ? C6 C5 H5A 109.1 . . ? C4 C5 H5B 109.1 . . ? C6 C5 H5B 109.1 . . ? H5A C5 H5B 107.8 . . ? C5 C6 C1 110.5(3) . . ? C5 C6 H6A 109.5 . . ? C1 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 N1 112.7(3) . . ? N2 C7 C14 124.1(3) . . ? N1 C7 C14 123.1(3) . . ? N2 C7 Co1 56.92(18) . . ? N1 C7 Co1 56.66(19) . . ? C14 C7 Co1 170.5(3) . . ? N2 C8 C9 111.4(3) . . ? N2 C8 C13 109.7(3) . . ? C9 C8 C13 109.9(3) . . ? N2 C8 H8 108.6 . . ? C9 C8 H8 108.6 . . ? C13 C8 H8 108.6 . . ? C8 C9 C10 110.8(3) . . ? C8 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 . . ? H9A C9 H9B 108.1 . . ? C11 C10 C9 111.0(3) . . ? C11 C10 H10A 109.4 . . ? C9 C10 H10A 109.4 . . ? C11 C10 H10B 109.4 . . ? C9 C10 H10B 109.4 . . ? H10A C10 H10B 108.0 . . ? C10 C11 C12 111.2(4) . . ? C10 C11 H11A 109.4 . . ? C12 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C11 C12 C13 112.1(4) . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C8 C13 C12 111.1(3) . . ? C8 C13 H13A 109.4 . . ? C12 C13 H13A 109.4 . . ? C8 C13 H13B 109.4 . . ? C12 C13 H13B 109.4 . . ? H13A C13 H13B 108.0 . . ? C7 C14 H14A 109.5 . . ? C7 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C7 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N3 C15 N4 108.1(3) . . ? N3 C15 Co1 126.1(3) . . ? N4 C15 Co1 125.1(3) . . ? N3 C16 C17 101.9(4) . . ? N3 C16 H16A 111.4 . . ? C17 C16 H16A 111.4 . . ? N3 C16 H16B 111.4 . . ? C17 C16 H16B 111.4 . . ? H16A C16 H16B 109.3 . . ? N4 C17 C16 102.7(4) . . ? N4 C17 H17A 111.2 . . ? C16 C17 H17A 111.2 . . ? N4 C17 H17B 111.2 . . ? C16 C17 H17B 111.2 . . ? H17A C17 H17B 109.1 . . ? C19 C18 C24 121.5(4) . . ? C19 C18 N4 119.0(4) . . ? C24 C18 N4 119.2(4) . . ? C20 C19 C18 118.0(4) . . ? C20 C19 C26 121.5(4) . . ? C18 C19 C26 120.6(4) . . ? C19 C20 C21 121.8(5) . . ? C19 C20 H20 119.1 . . ? C21 C20 H20 119.1 . . ? C23 C21 C20 118.1(5) . . ? C23 C21 C22 121.0(5) . . ? C20 C21 C22 120.9(6) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 C24 122.7(4) . . ? C21 C23 H23 118.7 . . ? C24 C23 H23 118.7 . . ? C23 C24 C18 117.9(4) . . ? C23 C24 C25 121.3(4) . . ? C18 C24 C25 120.8(5) . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C19 C26 H26A 109.5 . . ? C19 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C19 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C33 C27 C28 120.9(4) . . ? C33 C27 N3 120.0(4) . . ? C28 C27 N3 118.9(4) . . ? C29 C28 C27 118.6(4) . . ? C29 C28 C35 119.8(4) . . ? C27 C28 C35 121.6(4) . . ? C30 C29 C28 122.2(4) . . ? C30 C29 H29 118.9 . . ? C28 C29 H29 118.9 . . ? C29 C30 C32 118.3(4) . . ? C29 C30 C31 121.6(5) . . ? C32 C30 C31 120.1(5) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C30 121.8(4) . . ? C33 C32 H32 119.1 . . ? C30 C32 H32 119.1 . . ? C32 C33 C27 118.1(4) . . ? C32 C33 C34 122.0(4) . . ? C27 C33 C34 119.9(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 . . ? C28 C35 H35A 109.5 . . ? C28 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C28 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 27.95 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.807 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.092 data_complex3b _database_code_depnum_ccdc_archive 'CCDC 918515' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H96 Cl2 Co2 N6 O' _chemical_formula_weight 1226.29 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' 'x-1/2, y-1/2, -z-1/2' _cell_length_a 17.3027(10) _cell_length_b 23.6427(14) _cell_length_c 16.8268(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6883.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.183 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2616 _exptl_absorpt_coefficient_mu 0.604 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8786 _exptl_absorpt_correction_T_max 0.9704 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 72419 _diffrn_reflns_av_R_equivalents 0.0782 _diffrn_reflns_av_sigmaI/netI 0.0445 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 28.05 _reflns_number_total 8354 _reflns_number_gt 5251 _reflns_threshold_expression >2\s(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _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^ > 2\s(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^)+(0.0446P)^2^+9.1826P] 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 8354 _refine_ls_number_parameters 368 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1015 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1331 _refine_ls_wR_factor_gt 0.1080 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.91789(2) 0.244043(15) 0.69731(2) 0.02657(10) Uani 1 1 d . . . Cl1 Cl 1.0000 0.31338(4) 0.7500 0.0302(2) Uani 1 2 d S . . Cl2 Cl 1.0000 0.17180(4) 0.7500 0.0312(2) Uani 1 2 d S . . N1 N 0.76877(13) 0.27322(11) 0.79184(15) 0.0329(6) Uani 1 1 d . . . N2 N 0.77046(14) 0.18831(10) 0.74422(15) 0.0340(6) Uani 1 1 d . . . N3 N 0.92611(14) 0.22329(10) 0.58793(14) 0.0329(5) Uani 1 1 d . . . O2 O 1.0000 0.4447(5) 0.2500 0.200(4) Uani 1 2 d S . . C1 C 0.81102(15) 0.23633(11) 0.75003(16) 0.0274(6) Uani 1 1 d . . . C2 C 0.69547(18) 0.24890(14) 0.8220(2) 0.0493(9) Uani 1 1 d . . . H2A H 0.6516 0.2725 0.8082 0.059 Uiso 1 1 calc R . . H2B H 0.6970 0.2439 0.8792 0.059 Uiso 1 1 calc R . . C3 C 0.69231(18) 0.19264(15) 0.7793(2) 0.0487(9) Uani 1 1 d . . . H3A H 0.6825 0.1619 0.8161 0.058 Uiso 1 1 calc R . . H3B H 0.6527 0.1926 0.7385 0.058 Uiso 1 1 calc R . . C4 C 0.79110(16) 0.14158(12) 0.69408(18) 0.0325(6) Uani 1 1 d . . . C5 C 0.82425(18) 0.09356(13) 0.7281(2) 0.0397(7) Uani 1 1 d . . . C6 C 0.8388(2) 0.08939(16) 0.8161(2) 0.0578(10) Uani 1 1 d . . . H6A H 0.7905 0.0843 0.8433 0.087 Uiso 1 1 calc R . . H6B H 0.8630 0.1235 0.8344 0.087 Uiso 1 1 calc R . . H6C H 0.8720 0.0577 0.8267 0.087 Uiso 1 1 calc R . . C7 C 0.8440(2) 0.04965(14) 0.6776(3) 0.0513(9) Uani 1 1 d . . . H7 H 0.8666 0.0173 0.6989 0.062 Uiso 1 1 calc R . . C8 C 0.8310(2) 0.05224(14) 0.5966(3) 0.0519(10) Uani 1 1 d . . . C9 C 0.7964(2) 0.09978(15) 0.5651(2) 0.0468(8) Uani 1 1 d . . . H9 H 0.7868 0.1015 0.5108 0.056 Uiso 1 1 calc R . . C10 C 0.77560(17) 0.14513(13) 0.61302(19) 0.0366(7) Uani 1 1 d . . . C11 C 0.7376(2) 0.19645(15) 0.5776(2) 0.0487(9) Uani 1 1 d . . . H11A H 0.7476 0.1976 0.5216 0.073 Uiso 1 1 calc R . . H11B H 0.7580 0.2299 0.6022 0.073 Uiso 1 1 calc R . . H11C H 0.6828 0.1946 0.5866 0.073 Uiso 1 1 calc R . . C12 C 0.8548(3) 0.00380(19) 0.5422(3) 0.0896(16) Uani 1 1 d . . . H12A H 0.9004 -0.0140 0.5630 0.134 Uiso 1 1 calc R . . H12B H 0.8654 0.0183 0.4900 0.134 Uiso 1 1 calc R . . H12C H 0.8137 -0.0234 0.5394 0.134 Uiso 1 1 calc R . . C13 C 0.79432(16) 0.32684(12) 0.82207(17) 0.0314(6) Uani 1 1 d . . . C14 C 0.76262(19) 0.37612(14) 0.7905(2) 0.0430(8) Uani 1 1 d . . . C15 C 0.7843(2) 0.42726(15) 0.8242(2) 0.0569(10) Uani 1 1 d . . . H15 H 0.7640 0.4607 0.8038 0.068 Uiso 1 1 calc R . . C16 C 0.8351(2) 0.42981(16) 0.8869(3) 0.0583(11) Uani 1 1 d . . . C17 C 0.8660(2) 0.38014(15) 0.9166(2) 0.0475(9) Uani 1 1 d . . . H17 H 0.9008 0.3818 0.9586 0.057 Uiso 1 1 calc R . . C18 C 0.84611(17) 0.32778(13) 0.88502(18) 0.0341(7) Uani 1 1 d . . . C19 C 0.87958(18) 0.27414(15) 0.91875(19) 0.0421(8) Uani 1 1 d . . . H19A H 0.8388 0.2474 0.9279 0.063 Uiso 1 1 calc R . . H19B H 0.9052 0.2823 0.9681 0.063 Uiso 1 1 calc R . . H19C H 0.9161 0.2585 0.8818 0.063 Uiso 1 1 calc R . . C20 C 0.8571(3) 0.48622(19) 0.9249(3) 0.0965(18) Uani 1 1 d . . . H20A H 0.8263 0.4922 0.9716 0.145 Uiso 1 1 calc R . . H20B H 0.8480 0.5163 0.8877 0.145 Uiso 1 1 calc R . . H20C H 0.9108 0.4856 0.9392 0.145 Uiso 1 1 calc R . . C21 C 0.7057(2) 0.37448(18) 0.7224(2) 0.0626(11) Uani 1 1 d . . . H21A H 0.6546 0.3684 0.7427 0.094 Uiso 1 1 calc R . . H21B H 0.7191 0.3442 0.6869 0.094 Uiso 1 1 calc R . . H21C H 0.7073 0.4098 0.6942 0.094 Uiso 1 1 calc R . . C22 C 0.93966(15) 0.24763(12) 0.51494(16) 0.0288(6) Uani 1 1 d . . . C23 C 0.92213(17) 0.30532(13) 0.50009(17) 0.0322(6) Uani 1 1 d . . . C24 C 0.94839(19) 0.33042(15) 0.43041(19) 0.0418(8) Uani 1 1 d . . . H24 H 0.9392 0.3687 0.4223 0.050 Uiso 1 1 calc R . . C25 C 0.98768(19) 0.30034(17) 0.3730(2) 0.0485(9) Uani 1 1 d . . . H25 H 1.0072 0.3185 0.3282 0.058 Uiso 1 1 calc R . . C26 C 0.99757(18) 0.24308(16) 0.38314(18) 0.0442(8) Uani 1 1 d . . . H26 H 1.0214 0.2223 0.3431 0.053 Uiso 1 1 calc R . . C27 C 0.97302(16) 0.21539(14) 0.45153(18) 0.0361(7) Uani 1 1 d . . . C28 C 0.9839(2) 0.15213(15) 0.4608(2) 0.0447(8) Uani 1 1 d . . . H28 H 0.9425 0.1389 0.4960 0.054 Uiso 1 1 calc R . . C29 C 0.9767(3) 0.11837(18) 0.3840(2) 0.0703(13) Uani 1 1 d . . . H29A H 0.9283 0.1270 0.3589 0.105 Uiso 1 1 calc R . . H29B H 0.9788 0.0787 0.3958 0.105 Uiso 1 1 calc R . . H29C H 1.0183 0.1282 0.3489 0.105 Uiso 1 1 calc R . . C30 C 1.0600(3) 0.13815(18) 0.5022(3) 0.0755(14) Uani 1 1 d . . . H30A H 1.1024 0.1476 0.4678 0.113 Uiso 1 1 calc R . . H30B H 1.0616 0.0985 0.5144 0.113 Uiso 1 1 calc R . . H30C H 1.0640 0.1596 0.5505 0.113 Uiso 1 1 calc R . . C31 C 0.87327(18) 0.34015(13) 0.55675(19) 0.0384(7) Uani 1 1 d . . . H31 H 0.8612 0.3162 0.6026 0.046 Uiso 1 1 calc R . . C32 C 0.9140(2) 0.39271(15) 0.5878(2) 0.0536(9) Uani 1 1 d . . . H32A H 0.9615 0.3820 0.6132 0.080 Uiso 1 1 calc R . . H32B H 0.8813 0.4116 0.6255 0.080 Uiso 1 1 calc R . . H32C H 0.9250 0.4177 0.5443 0.080 Uiso 1 1 calc R . . C33 C 0.79589(19) 0.35647(16) 0.5172(2) 0.0500(9) Uani 1 1 d . . . H33A H 0.8058 0.3788 0.4707 0.075 Uiso 1 1 calc R . . H33B H 0.7653 0.3780 0.5540 0.075 Uiso 1 1 calc R . . H33C H 0.7684 0.3228 0.5024 0.075 Uiso 1 1 calc R . . C02 C 1.1125(4) 0.4502(3) 0.3349(4) 0.121(2) Uiso 1 1 d . . . H02A H 1.0908 0.4267 0.3758 0.181 Uiso 1 1 calc R . . H02B H 1.1471 0.4771 0.3583 0.181 Uiso 1 1 calc R . . H02C H 1.1403 0.4270 0.2978 0.181 Uiso 1 1 calc R . . C03 C 1.0547(5) 0.4780(3) 0.2963(5) 0.144(3) Uiso 1 1 d . . . H03A H 1.0783 0.5054 0.2609 0.173 Uiso 1 1 calc R . . H03B H 1.0256 0.4991 0.3356 0.173 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.02312(17) 0.0323(2) 0.02433(18) -0.00149(16) 0.00127(15) 0.00258(15) Cl1 0.0306(5) 0.0276(5) 0.0324(5) 0.000 0.0007(4) 0.000 Cl2 0.0288(5) 0.0275(5) 0.0373(5) 0.000 -0.0064(4) 0.000 N1 0.0234(11) 0.0395(14) 0.0359(14) -0.0077(11) 0.0053(10) 0.0000(10) N2 0.0258(12) 0.0381(13) 0.0383(14) -0.0085(12) 0.0044(11) -0.0045(10) N3 0.0382(14) 0.0347(13) 0.0259(12) -0.0012(10) 0.0032(11) 0.0037(11) O2 0.178(8) 0.255(11) 0.169(8) 0.000 -0.047(7) 0.000 C1 0.0253(13) 0.0326(14) 0.0243(13) -0.0009(12) -0.0044(11) 0.0013(11) C2 0.0301(15) 0.057(2) 0.061(2) -0.0175(18) 0.0175(15) -0.0101(15) C3 0.0304(16) 0.056(2) 0.060(2) -0.0163(17) 0.0137(16) -0.0123(15) C4 0.0267(14) 0.0313(15) 0.0393(16) -0.0058(13) -0.0002(13) -0.0031(11) C5 0.0334(16) 0.0364(17) 0.049(2) 0.0048(14) -0.0014(14) -0.0067(13) C6 0.064(2) 0.056(2) 0.054(2) 0.0159(18) -0.007(2) -0.0119(19) C7 0.047(2) 0.0296(17) 0.077(3) 0.0025(17) -0.0008(19) 0.0013(14) C8 0.048(2) 0.0360(19) 0.072(3) -0.0184(18) 0.0071(19) -0.0012(15) C9 0.0460(19) 0.049(2) 0.045(2) -0.0166(16) -0.0034(16) -0.0046(16) C10 0.0322(16) 0.0365(17) 0.0412(18) -0.0058(14) -0.0068(13) -0.0003(13) C11 0.049(2) 0.051(2) 0.047(2) -0.0053(16) -0.0200(17) 0.0071(16) C12 0.099(4) 0.059(3) 0.111(4) -0.044(3) 0.012(3) 0.010(3) C13 0.0290(14) 0.0339(15) 0.0312(16) -0.0053(12) 0.0076(12) 0.0029(12) C14 0.0453(19) 0.0431(19) 0.0407(19) 0.0017(15) 0.0118(15) 0.0124(15) C15 0.075(3) 0.0343(19) 0.061(3) 0.0039(17) 0.024(2) 0.0134(18) C16 0.071(3) 0.040(2) 0.064(3) -0.0164(18) 0.027(2) -0.0111(19) C17 0.0425(19) 0.060(2) 0.0401(19) -0.0162(17) 0.0106(15) -0.0109(16) C18 0.0287(15) 0.0422(17) 0.0314(15) -0.0042(13) 0.0078(12) 0.0002(13) C19 0.0344(16) 0.060(2) 0.0321(17) 0.0003(15) 0.0032(13) 0.0094(15) C20 0.126(4) 0.054(3) 0.109(4) -0.038(3) 0.040(4) -0.027(3) C21 0.064(3) 0.078(3) 0.046(2) 0.012(2) 0.0008(19) 0.028(2) C22 0.0213(12) 0.0401(17) 0.0249(13) -0.0037(12) -0.0017(10) 0.0013(11) C23 0.0293(14) 0.0387(16) 0.0286(14) 0.0023(12) -0.0030(12) 0.0010(12) C24 0.0379(17) 0.049(2) 0.0382(18) 0.0086(15) -0.0025(14) -0.0004(15) C25 0.0358(18) 0.076(3) 0.0343(18) 0.0124(17) 0.0024(14) -0.0016(17) C26 0.0293(15) 0.077(2) 0.0262(15) -0.0081(16) 0.0029(12) 0.0062(16) C27 0.0247(14) 0.0519(19) 0.0318(16) -0.0063(14) -0.0043(12) 0.0056(13) C28 0.0443(19) 0.054(2) 0.0356(18) -0.0156(15) -0.0008(15) 0.0116(15) C29 0.081(3) 0.074(3) 0.056(3) -0.030(2) -0.012(2) 0.011(2) C30 0.081(3) 0.062(3) 0.084(3) -0.030(2) -0.039(3) 0.033(2) C31 0.0441(18) 0.0373(17) 0.0339(17) 0.0045(13) -0.0002(14) 0.0072(14) C32 0.066(2) 0.0412(19) 0.054(2) -0.0008(17) -0.0040(19) 0.0033(18) C33 0.0435(19) 0.055(2) 0.052(2) 0.0024(17) 0.0024(17) 0.0157(17) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 1.910(2) . ? Co1 C1 2.059(3) . ? Co1 Cl1 2.3435(8) . ? Co1 Cl2 2.3921(8) . ? Cl1 Co1 2.3435(8) 3_756 ? Cl2 Co1 2.3921(8) 3_756 ? N1 C1 1.338(4) . ? N1 C13 1.436(4) . ? N1 C2 1.482(4) . ? N2 C1 1.338(3) . ? N2 C4 1.435(4) . ? N2 C3 1.479(4) . ? N3 C22 1.376(4) . ? O2 C03 1.456(9) . ? O2 C03 1.456(8) 3_755 ? C2 C3 1.513(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C10 1.393(4) . ? C4 C5 1.395(4) . ? C5 C7 1.384(5) . ? C5 C6 1.506(5) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.383(5) . ? C7 H7 0.9300 . ? C8 C9 1.379(5) . ? C8 C12 1.522(5) . ? C9 C10 1.389(4) . ? C9 H9 0.9300 . ? C10 C11 1.503(4) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C18 1.387(4) . ? C13 C14 1.393(4) . ? C14 C15 1.387(5) . ? C14 C21 1.512(5) . ? C15 C16 1.374(6) . ? C15 H15 0.9300 . ? C16 C17 1.383(5) . ? C16 C20 1.527(5) . ? C17 C18 1.390(4) . ? C17 H17 0.9300 . ? C18 C19 1.505(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.419(4) . ? C22 C27 1.433(4) . ? C23 C24 1.390(4) . ? C23 C31 1.517(4) . ? C24 C25 1.379(5) . ? C24 H24 0.9300 . ? C25 C26 1.375(5) . ? C25 H25 0.9300 . ? C26 C27 1.390(4) . ? C26 H26 0.9300 . ? C27 C28 1.515(5) . ? C28 C29 1.524(5) . ? C28 C30 1.526(5) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.521(5) . ? C31 C33 1.544(4) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C02 C03 1.362(9) . ? C02 H02A 0.9600 . ? C02 H02B 0.9600 . ? C02 H02C 0.9600 . ? C03 H03A 0.9700 . ? C03 H03B 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 N3 Co1 C1 117.34(11) . . ? N3 Co1 Cl1 119.94(8) . . ? C1 Co1 Cl1 116.32(8) . . ? N3 Co1 Cl2 97.44(7) . . ? C1 Co1 Cl2 108.09(8) . . ? Cl1 Co1 Cl2 89.96(3) . . ? Co1 Cl1 Co1 91.22(4) . 3_756 ? Co1 Cl2 Co1 88.87(4) 3_756 . ? C1 N1 C13 126.4(2) . . ? C1 N1 C2 113.3(2) . . ? C13 N1 C2 119.0(2) . . ? C1 N2 C4 124.4(2) . . ? C1 N2 C3 113.0(2) . . ? C4 N2 C3 121.0(2) . . ? C22 N3 Co1 139.9(2) . . ? C03 O2 C03 114.7(10) . 3_755 ? N1 C1 N2 107.8(2) . . ? N1 C1 Co1 131.3(2) . . ? N2 C1 Co1 121.0(2) . . ? N1 C2 C3 102.1(2) . . ? N1 C2 H2A 111.4 . . ? C3 C2 H2A 111.4 . . ? N1 C2 H2B 111.4 . . ? C3 C2 H2B 111.4 . . ? H2A C2 H2B 109.2 . . ? N2 C3 C2 102.6(2) . . ? N2 C3 H3A 111.3 . . ? C2 C3 H3A 111.3 . . ? N2 C3 H3B 111.3 . . ? C2 C3 H3B 111.3 . . ? H3A C3 H3B 109.2 . . ? C10 C4 C5 122.0(3) . . ? C10 C4 N2 118.8(3) . . ? C5 C4 N2 119.2(3) . . ? C7 C5 C4 117.4(3) . . ? C7 C5 C6 120.9(3) . . ? C4 C5 C6 121.7(3) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 C8 122.1(3) . . ? C5 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C9 C8 C7 119.0(3) . . ? C9 C8 C12 120.0(4) . . ? C7 C8 C12 121.0(4) . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? C9 C10 C4 118.2(3) . . ? C9 C10 C11 120.4(3) . . ? C4 C10 C11 121.4(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C8 C12 H12A 109.5 . . ? C8 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C8 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 122.1(3) . . ? C18 C13 N1 118.9(3) . . ? C14 C13 N1 118.8(3) . . ? C15 C14 C13 117.8(3) . . ? C15 C14 C21 120.5(3) . . ? C13 C14 C21 121.6(3) . . ? C16 C15 C14 121.6(3) . . ? C16 C15 H15 119.2 . . ? C14 C15 H15 119.2 . . ? C15 C16 C17 119.1(3) . . ? C15 C16 C20 121.3(4) . . ? C17 C16 C20 119.6(4) . . ? C16 C17 C18 121.5(3) . . ? C16 C17 H17 119.2 . . ? C18 C17 H17 119.2 . . ? C13 C18 C17 117.7(3) . . ? C13 C18 C19 121.5(3) . . ? C17 C18 C19 120.7(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 . . ? C16 C20 H20A 109.5 . . ? C16 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C16 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14 C21 H21A 109.5 . . ? C14 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C14 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N3 C22 C23 121.5(3) . . ? N3 C22 C27 120.7(3) . . ? C23 C22 C27 117.8(3) . . ? C24 C23 C22 119.3(3) . . ? C24 C23 C31 118.7(3) . . ? C22 C23 C31 122.0(3) . . ? C25 C24 C23 122.1(3) . . ? C25 C24 H24 118.9 . . ? C23 C24 H24 118.9 . . ? C26 C25 C24 118.8(3) . . ? C26 C25 H25 120.6 . . ? C24 C25 H25 120.6 . . ? C25 C26 C27 121.9(3) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C26 C27 C22 119.3(3) . . ? C26 C27 C28 120.8(3) . . ? C22 C27 C28 119.9(3) . . ? C27 C28 C29 114.8(3) . . ? C27 C28 C30 111.6(3) . . ? C29 C28 C30 110.2(3) . . ? C27 C28 H28 106.6 . . ? C29 C28 H28 106.6 . . ? C30 C28 H28 106.6 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C23 C31 C32 113.6(3) . . ? C23 C31 C33 110.4(3) . . ? C32 C31 C33 110.2(3) . . ? C23 C31 H31 107.4 . . ? C32 C31 H31 107.4 . . ? C33 C31 H31 107.4 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C03 C02 H02A 109.5 . . ? C03 C02 H02B 109.5 . . ? H02A C02 H02B 109.5 . . ? C03 C02 H02C 109.5 . . ? H02A C02 H02C 109.5 . . ? H02B C02 H02C 109.5 . . ? C02 C03 O2 118.1(7) . . ? C02 C03 H03A 107.8 . . ? O2 C03 H03A 107.8 . . ? C02 C03 H03B 107.8 . . ? O2 C03 H03B 107.8 . . ? H03A C03 H03B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 28.05 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.980 _refine_diff_density_min -0.679 _refine_diff_density_rms 0.066 data_complex4 _database_code_depnum_ccdc_archive 'CCDC 918516' #TrackingRef 'CombinedCifDanopoulos.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H49 Co N2, 0.5(C4 H8 O2)' _chemical_formula_sum 'C43 H53 Co N2 O' _chemical_formula_weight 672.80 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' Co Co 0.3494 0.9721 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.8147(10) _cell_length_b 12.4360(12) _cell_length_c 15.3783(15) _cell_angle_alpha 73.166(2) _cell_angle_beta 82.284(2) _cell_angle_gamma 66.698(2) _cell_volume 1817.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5521 _cell_measurement_theta_min 2.29 _cell_measurement_theta_max 30.83 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.229 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 0.507 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8837 _exptl_absorpt_correction_T_max 0.9416 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31806 _diffrn_reflns_av_R_equivalents 0.0579 _diffrn_reflns_av_sigmaI/netI 0.0965 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 31.27 _reflns_number_total 11678 _reflns_number_gt 7000 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2\s(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^)+(0.0560P)^2^+1.4935P] 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 11678 _refine_ls_number_parameters 432 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1226 _refine_ls_R_factor_gt 0.0581 _refine_ls_wR_factor_ref 0.1535 _refine_ls_wR_factor_gt 0.1293 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.017 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.3440(2) 0.3518(2) 0.24735(17) 0.0188(5) Uani 1 1 d . . . C2 C 0.3311(3) 0.4344(2) 0.09170(17) 0.0252(5) Uani 1 1 d . . . H2 H 0.3119 0.4928 0.0346 0.030 Uiso 1 1 calc R . . C3 C 0.3897(3) 0.3142(2) 0.10547(18) 0.0266(6) Uani 1 1 d . . . H3 H 0.4200 0.2709 0.0600 0.032 Uiso 1 1 calc R . . C4 C 0.2460(2) 0.5818(2) 0.18400(17) 0.0207(5) Uani 1 1 d . . . C5 C 0.3286(3) 0.6288(2) 0.21080(18) 0.0246(5) Uani 1 1 d . . . C6 C 0.2718(3) 0.7502(3) 0.2126(2) 0.0344(7) Uani 1 1 d . . . H6 H 0.3240 0.7841 0.2327 0.041 Uiso 1 1 calc R . . C7 C 0.1412(3) 0.8226(3) 0.1857(2) 0.0391(7) Uani 1 1 d . . . H7 H 0.1048 0.9053 0.1870 0.047 Uiso 1 1 calc R . . C8 C 0.0638(3) 0.7747(3) 0.1570(2) 0.0346(7) Uani 1 1 d . . . H8 H -0.0251 0.8255 0.1374 0.041 Uiso 1 1 calc R . . C9 C 0.1133(3) 0.6528(2) 0.15608(18) 0.0253(5) Uani 1 1 d . . . C10 C 0.4769(3) 0.5533(2) 0.23197(19) 0.0279(6) Uani 1 1 d . . . H10 H 0.4847 0.4693 0.2662 0.034 Uiso 1 1 calc R . . C11 C 0.5345(3) 0.6021(3) 0.2906(3) 0.0460(8) Uani 1 1 d . . . H11A H 0.5401 0.6795 0.2552 0.069 Uiso 1 1 calc R . . H11B H 0.6246 0.5437 0.3102 0.069 Uiso 1 1 calc R . . H11C H 0.4756 0.6144 0.3441 0.069 Uiso 1 1 calc R . . C12 C 0.5604(3) 0.5456(3) 0.1440(2) 0.0443(8) Uani 1 1 d . . . H12A H 0.5236 0.5137 0.1068 0.066 Uiso 1 1 calc R . . H12B H 0.6540 0.4916 0.1584 0.066 Uiso 1 1 calc R . . H12C H 0.5573 0.6266 0.1102 0.066 Uiso 1 1 calc R . . C13 C 0.0229(3) 0.6051(3) 0.12341(19) 0.0310(6) Uani 1 1 d . . . H13 H 0.0669 0.5147 0.1381 0.037 Uiso 1 1 calc R . . C14 C 0.0056(3) 0.6535(3) 0.0200(2) 0.0446(8) Uani 1 1 d . . . H14A H -0.0339 0.7423 0.0038 0.067 Uiso 1 1 calc R . . H14B H -0.0539 0.6225 0.0009 0.067 Uiso 1 1 calc R . . H14C H 0.0937 0.6264 -0.0107 0.067 Uiso 1 1 calc R . . C15 C -0.1162(3) 0.6384(3) 0.1714(2) 0.0413(8) Uani 1 1 d . . . H15A H -0.1049 0.6093 0.2374 0.062 Uiso 1 1 calc R . . H15B H -0.1688 0.6005 0.1529 0.062 Uiso 1 1 calc R . . H15C H -0.1636 0.7267 0.1546 0.062 Uiso 1 1 calc R . . C16 C 0.4631(2) 0.1351(2) 0.23560(17) 0.0202(5) Uani 1 1 d . . . C17 C 0.6033(2) 0.0836(2) 0.22638(19) 0.0263(6) Uani 1 1 d . . . C18 C 0.6649(3) -0.0428(3) 0.2546(2) 0.0326(6) Uani 1 1 d . . . H18 H 0.7599 -0.0806 0.2486 0.039 Uiso 1 1 calc R . . C19 C 0.5898(3) -0.1131(3) 0.29079(19) 0.0318(6) Uani 1 1 d . . . H19 H 0.6329 -0.1989 0.3084 0.038 Uiso 1 1 calc R . . C20 C 0.4512(3) -0.0592(2) 0.30170(18) 0.0278(6) Uani 1 1 d . . . H20 H 0.4011 -0.1088 0.3287 0.033 Uiso 1 1 calc R . . C21 C 0.3840(2) 0.0662(2) 0.27385(17) 0.0213(5) Uani 1 1 d . . . C22 C 0.6896(3) 0.1590(3) 0.1896(2) 0.0417(8) Uani 1 1 d . . . H22 H 0.6331 0.2447 0.1903 0.050 Uiso 1 1 calc R . . C23 C 0.7364(4) 0.1575(4) 0.0910(3) 0.0620(11) Uani 1 1 d . . . H23A H 0.7899 0.0739 0.0882 0.093 Uiso 1 1 calc R . . H23B H 0.7915 0.2068 0.0694 0.093 Uiso 1 1 calc R . . H23C H 0.6577 0.1907 0.0525 0.093 Uiso 1 1 calc R . . C24 C 0.8119(3) 0.1163(4) 0.2488(3) 0.0649(12) Uani 1 1 d . . . H24A H 0.7828 0.1069 0.3128 0.097 Uiso 1 1 calc R . . H24B H 0.8541 0.1765 0.2310 0.097 Uiso 1 1 calc R . . H24C H 0.8770 0.0384 0.2404 0.097 Uiso 1 1 calc R . . C25 C 0.2324(3) 0.1250(2) 0.28602(19) 0.0261(6) Uani 1 1 d . . . H25 H 0.2139 0.1992 0.3066 0.031 Uiso 1 1 calc R . . C26 C 0.1603(3) 0.1665(3) 0.1961(2) 0.0389(7) Uani 1 1 d . . . H26A H 0.1971 0.2205 0.1508 0.058 Uiso 1 1 calc R . . H26B H 0.0638 0.2099 0.2053 0.058 Uiso 1 1 calc R . . H26C H 0.1740 0.0956 0.1746 0.058 Uiso 1 1 calc R . . C27 C 0.1714(3) 0.0451(3) 0.3581(2) 0.0427(8) Uani 1 1 d . . . H27A H 0.1731 -0.0214 0.3353 0.064 Uiso 1 1 calc R . . H27B H 0.0781 0.0937 0.3716 0.064 Uiso 1 1 calc R . . H27C H 0.2239 0.0117 0.4135 0.064 Uiso 1 1 calc R . . C28 C 0.1234(2) 0.4285(2) 0.35554(18) 0.0245(5) Uani 1 1 d . . . H28A H 0.1014 0.5036 0.3747 0.029 Uiso 1 1 calc R . . H28B H 0.1055 0.4527 0.2898 0.029 Uiso 1 1 calc R . . C29 C 0.0307(2) 0.3678(2) 0.40521(18) 0.0242(5) Uani 1 1 d . . . C30 C -0.0633(3) 0.3559(3) 0.3583(2) 0.0342(7) Uani 1 1 d . . . H30 H -0.0641 0.3831 0.2939 0.041 Uiso 1 1 calc R . . C31 C -0.1559(3) 0.3054(3) 0.4033(3) 0.0457(8) Uani 1 1 d . . . H31 H -0.2197 0.2996 0.3698 0.055 Uiso 1 1 calc R . . C32 C -0.1547(3) 0.2638(3) 0.4964(3) 0.0541(10) Uani 1 1 d . . . H32 H -0.2182 0.2300 0.5276 0.065 Uiso 1 1 calc R . . C33 C -0.0602(3) 0.2715(3) 0.5445(2) 0.0486(9) Uani 1 1 d . . . H33 H -0.0584 0.2414 0.6088 0.058 Uiso 1 1 calc R . . C34 C 0.0323(3) 0.3228(3) 0.50012(19) 0.0308(6) Uani 1 1 d . . . C35 C 0.1328(3) 0.3339(3) 0.55288(19) 0.0353(7) Uani 1 1 d . . . H35A H 0.1347 0.2831 0.6159 0.042 Uiso 1 1 calc R . . H35B H 0.1029 0.4191 0.5555 0.042 Uiso 1 1 calc R . . C36 C 0.2745(3) 0.2953(3) 0.51151(17) 0.0266(6) Uani 1 1 d . . . C37 C 0.3448(3) 0.3742(3) 0.49255(19) 0.0313(6) Uani 1 1 d . . . H37 H 0.3076 0.4471 0.5115 0.038 Uiso 1 1 calc R . . C38 C 0.4687(3) 0.3455(3) 0.4461(2) 0.0339(7) Uani 1 1 d . . . H38 H 0.5156 0.3991 0.4322 0.041 Uiso 1 1 calc R . . C39 C 0.5232(3) 0.2357(3) 0.42023(19) 0.0322(6) Uani 1 1 d . . . H39 H 0.6068 0.2162 0.3877 0.039 Uiso 1 1 calc R . . C40 C 0.4562(3) 0.1543(2) 0.44163(18) 0.0271(6) Uani 1 1 d . . . H40 H 0.4952 0.0800 0.4246 0.033 Uiso 1 1 calc R . . C41 C 0.3319(3) 0.1832(2) 0.48802(17) 0.0252(5) Uani 1 1 d . . . H41 H 0.2865 0.1284 0.5036 0.030 Uiso 1 1 calc R . . C42 C 0.4053(4) -0.0364(4) 0.0546(3) 0.0548(10) Uani 1 1 d . . . H42A H 0.4188 -0.0255 0.1134 0.066 Uiso 1 1 calc R . . H42B H 0.3298 -0.0646 0.0625 0.066 Uiso 1 1 calc R . . C43 C 0.3713(4) 0.0820(4) -0.0162(2) 0.0544(10) Uani 1 1 d . . . H43A H 0.3539 0.0717 -0.0743 0.065 Uiso 1 1 calc R . . H43B H 0.2883 0.1427 0.0027 0.065 Uiso 1 1 calc R . . N1 N 0.30356(19) 0.45794(18) 0.17651(14) 0.0189(4) Uani 1 1 d . . . N2 N 0.39806(19) 0.26462(19) 0.19878(14) 0.0200(4) Uani 1 1 d . . . Co1 Co 0.32155(3) 0.32941(3) 0.37336(2) 0.01951(10) Uani 1 1 d . . . O1 O 0.4768(3) 0.1240(2) -0.02891(17) 0.0571(7) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0113(9) 0.0126(11) 0.0309(14) -0.0046(10) -0.0024(9) -0.0029(8) C2 0.0297(13) 0.0252(14) 0.0190(13) -0.0041(10) 0.0017(10) -0.0104(11) C3 0.0325(13) 0.0249(14) 0.0214(13) -0.0084(11) 0.0046(10) -0.0098(11) C4 0.0230(11) 0.0133(11) 0.0224(13) -0.0026(9) 0.0022(9) -0.0056(9) C5 0.0286(12) 0.0206(13) 0.0242(13) -0.0045(10) 0.0021(10) -0.0106(11) C6 0.0388(15) 0.0243(15) 0.0433(18) -0.0129(13) 0.0022(13) -0.0132(13) C7 0.0403(16) 0.0165(14) 0.056(2) -0.0135(14) 0.0068(14) -0.0061(12) C8 0.0265(13) 0.0189(14) 0.0444(18) -0.0035(12) 0.0001(12) 0.0022(11) C9 0.0253(12) 0.0207(13) 0.0249(14) -0.0028(10) 0.0025(10) -0.0067(10) C10 0.0281(13) 0.0223(14) 0.0349(15) -0.0051(11) -0.0028(11) -0.0120(11) C11 0.0448(18) 0.0349(18) 0.066(2) -0.0113(16) -0.0190(16) -0.0180(15) C12 0.0313(15) 0.048(2) 0.052(2) -0.0109(16) 0.0077(14) -0.0176(15) C13 0.0245(12) 0.0280(15) 0.0334(16) 0.0003(12) -0.0062(11) -0.0067(11) C14 0.0435(18) 0.047(2) 0.0369(18) 0.0003(15) -0.0142(14) -0.0142(16) C15 0.0254(14) 0.0410(19) 0.0473(19) 0.0009(15) -0.0073(13) -0.0086(13) C16 0.0223(11) 0.0155(12) 0.0221(12) -0.0060(10) -0.0012(9) -0.0053(9) C17 0.0209(11) 0.0244(14) 0.0334(15) -0.0137(12) -0.0009(10) -0.0038(10) C18 0.0259(13) 0.0280(15) 0.0377(17) -0.0137(13) -0.0077(11) 0.0022(11) C19 0.0403(15) 0.0178(13) 0.0303(15) -0.0066(11) -0.0129(12) 0.0005(12) C20 0.0414(15) 0.0189(13) 0.0225(13) -0.0023(10) -0.0053(11) -0.0114(12) C21 0.0265(12) 0.0176(12) 0.0212(12) -0.0055(10) -0.0024(9) -0.0090(10) C22 0.0247(14) 0.0402(18) 0.067(2) -0.0270(17) 0.0086(14) -0.0129(13) C23 0.051(2) 0.066(3) 0.075(3) -0.022(2) 0.026(2) -0.033(2) C24 0.0257(15) 0.080(3) 0.110(4) -0.062(3) 0.0052(18) -0.0178(18) C25 0.0250(12) 0.0234(14) 0.0332(15) -0.0087(11) 0.0029(10) -0.0126(11) C26 0.0267(14) 0.049(2) 0.0418(18) -0.0125(15) -0.0042(12) -0.0140(14) C27 0.0417(17) 0.0405(19) 0.050(2) -0.0096(15) 0.0114(14) -0.0256(15) C28 0.0169(11) 0.0247(14) 0.0238(13) -0.0019(11) 0.0027(9) -0.0035(10) C29 0.0182(11) 0.0182(13) 0.0290(14) -0.0047(10) 0.0027(9) -0.0014(9) C30 0.0229(12) 0.0316(16) 0.0447(18) -0.0113(13) -0.0009(12) -0.0057(12) C31 0.0258(14) 0.0364(19) 0.075(3) -0.0119(17) -0.0019(14) -0.0130(14) C32 0.0318(16) 0.038(2) 0.082(3) 0.0039(18) 0.0091(16) -0.0184(15) C33 0.0325(16) 0.044(2) 0.046(2) 0.0095(16) 0.0087(14) -0.0083(14) C34 0.0231(12) 0.0259(15) 0.0307(15) -0.0014(12) 0.0049(11) -0.0022(11) C35 0.0292(14) 0.0423(18) 0.0211(14) -0.0070(12) 0.0029(11) -0.0019(13) C36 0.0271(12) 0.0277(14) 0.0189(13) -0.0043(11) -0.0023(10) -0.0048(11) C37 0.0383(15) 0.0287(15) 0.0260(14) -0.0084(12) -0.0074(11) -0.0087(12) C38 0.0312(14) 0.0376(17) 0.0341(16) -0.0041(13) -0.0104(12) -0.0146(13) C39 0.0189(12) 0.0407(17) 0.0294(15) -0.0046(13) -0.0043(10) -0.0053(12) C40 0.0287(13) 0.0201(13) 0.0241(14) -0.0034(11) -0.0068(10) -0.0002(11) C41 0.0313(13) 0.0207(13) 0.0200(13) -0.0003(10) -0.0031(10) -0.0086(11) C42 0.067(2) 0.068(3) 0.044(2) -0.0238(19) 0.0126(18) -0.039(2) C43 0.0427(19) 0.056(2) 0.043(2) -0.0200(18) -0.0095(15) 0.0117(17) N1 0.0208(9) 0.0140(10) 0.0209(11) -0.0044(8) 0.0010(8) -0.0060(8) N2 0.0204(9) 0.0185(10) 0.0208(11) -0.0057(8) 0.0019(8) -0.0073(8) Co1 0.01727(15) 0.01727(17) 0.02026(18) -0.00401(13) -0.00033(11) -0.00330(12) O1 0.091(2) 0.0297(13) 0.0442(15) -0.0103(11) 0.0039(13) -0.0176(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N2 1.388(3) . ? C1 N1 1.399(3) . ? C1 Co1 1.873(3) . ? C2 C3 1.336(4) . ? C2 N1 1.387(3) . ? C2 H2 0.9500 . ? C3 N2 1.388(3) . ? C3 H3 0.9500 . ? C4 C5 1.401(3) . ? C4 C9 1.403(3) . ? C4 N1 1.448(3) . ? C5 C6 1.394(4) . ? C5 C10 1.527(4) . ? C6 C7 1.383(4) . ? C6 H6 0.9500 . ? C7 C8 1.376(4) . ? C7 H7 0.9500 . ? C8 C9 1.397(4) . ? C8 H8 0.9500 . ? C9 C13 1.524(4) . ? C10 C12 1.528(4) . ? C10 C11 1.529(4) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.538(4) . ? C13 C15 1.539(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.399(3) . ? C16 C21 1.402(3) . ? C16 N2 1.446(3) . ? C17 C18 1.399(4) . ? C17 C22 1.520(4) . ? C18 C19 1.376(4) . ? C18 H18 0.9500 . ? C19 C20 1.388(4) . ? C19 H19 0.9500 . ? C20 C21 1.394(4) . ? C20 H20 0.9500 . ? C21 C25 1.519(3) . ? C22 C24 1.532(5) . ? C22 C23 1.536(5) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.528(4) . ? C25 C26 1.531(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.489(3) . ? C28 Co1 2.015(2) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.398(4) . ? C29 C34 1.403(4) . ? C30 C31 1.391(4) . ? C30 H30 0.9500 . ? C31 C32 1.374(5) . ? C31 H31 0.9500 . ? C32 C33 1.387(5) . ? C32 H32 0.9500 . ? C33 C34 1.394(4) . ? C33 H33 0.9500 . ? C34 C35 1.509(4) . ? C35 C36 1.522(4) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.410(4) . ? C36 C41 1.416(4) . ? C36 Co1 2.076(3) . ? C37 C38 1.394(4) . ? C37 Co1 2.135(3) . ? C37 H37 0.9500 . ? C38 C39 1.410(4) . ? C38 Co1 2.165(3) . ? C38 H38 0.9500 . ? C39 C40 1.408(4) . ? C39 Co1 2.135(3) . ? C39 H39 0.9500 . ? C40 C41 1.397(4) . ? C40 Co1 2.131(3) . ? C40 H40 0.9500 . ? C41 Co1 2.112(3) . ? C41 H41 0.9500 . ? C42 O1 1.409(5) 2_655 ? C42 C43 1.497(5) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 O1 1.402(5) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? O1 C42 1.409(5) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 C1 N1 100.8(2) . . ? N2 C1 Co1 128.54(17) . . ? N1 C1 Co1 130.48(18) . . ? C3 C2 N1 107.1(2) . . ? C3 C2 H2 126.4 . . ? N1 C2 H2 126.4 . . ? C2 C3 N2 106.9(2) . . ? C2 C3 H3 126.5 . . ? N2 C3 H3 126.5 . . ? C5 C4 C9 122.7(2) . . ? C5 C4 N1 118.7(2) . . ? C9 C4 N1 118.3(2) . . ? C6 C5 C4 117.2(2) . . ? C6 C5 C10 120.9(2) . . ? C4 C5 C10 121.8(2) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6 119.2 . . ? C5 C6 H6 119.2 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? C7 C8 C9 121.4(3) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C4 117.2(2) . . ? C8 C9 C13 119.0(2) . . ? C4 C9 C13 123.8(2) . . ? C5 C10 C12 110.3(2) . . ? C5 C10 C11 112.9(2) . . ? C12 C10 C11 109.8(2) . . ? C5 C10 H10 107.9 . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C9 C13 C14 111.1(2) . . ? C9 C13 C15 111.6(3) . . ? C14 C13 C15 109.6(2) . . ? C9 C13 H13 108.1 . . ? C14 C13 H13 108.1 . . ? C15 C13 H13 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 123.0(2) . . ? C17 C16 N2 117.6(2) . . ? C21 C16 N2 119.3(2) . . ? C16 C17 C18 117.5(2) . . ? C16 C17 C22 122.9(2) . . ? C18 C17 C22 119.6(2) . . ? C19 C18 C17 120.9(3) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 120.3(3) . . ? C18 C19 H19 119.9 . . ? C20 C19 H19 119.9 . . ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C16 116.9(2) . . ? C20 C21 C25 121.3(2) . . ? C16 C21 C25 121.8(2) . . ? C17 C22 C24 111.8(3) . . ? C17 C22 C23 111.5(3) . . ? C24 C22 C23 109.8(3) . . ? C17 C22 H22 107.9 . . ? C24 C22 H22 107.9 . . ? C23 C22 H22 107.9 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 C27 113.8(2) . . ? C21 C25 C26 111.6(2) . . ? C27 C25 C26 109.8(2) . . ? C21 C25 H25 107.1 . . ? C27 C25 H25 107.1 . . ? C26 C25 H25 107.1 . . ? 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 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 Co1 115.86(17) . . ? C29 C28 H28A 108.3 . . ? Co1 C28 H28A 108.3 . . ? C29 C28 H28B 108.3 . . ? Co1 C28 H28B 108.3 . . ? H28A C28 H28B 107.4 . . ? C30 C29 C34 117.7(2) . . ? C30 C29 C28 120.6(2) . . ? C34 C29 C28 121.7(2) . . ? C31 C30 C29 121.9(3) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 119.8(3) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C33 119.6(3) . . ? C31 C32 H32 120.2 . . ? C33 C32 H32 120.2 . . ? C32 C33 C34 121.1(3) . . ? C32 C33 H33 119.5 . . ? C34 C33 H33 119.5 . . ? C33 C34 C29 120.0(3) . . ? C33 C34 C35 120.9(3) . . ? C29 C34 C35 119.1(2) . . ? C34 C35 C36 113.0(2) . . ? C34 C35 H35A 109.0 . . ? C36 C35 H35A 109.0 . . ? C34 C35 H35B 109.0 . . ? C36 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C41 120.5(2) . . ? C37 C36 C35 119.8(3) . . ? C41 C36 C35 119.6(3) . . ? C37 C36 Co1 72.70(16) . . ? C41 C36 Co1 71.62(15) . . ? C35 C36 Co1 125.27(18) . . ? C38 C37 C36 120.3(3) . . ? C38 C37 Co1 72.24(17) . . ? C36 C37 Co1 68.20(15) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? Co1 C37 H37 132.8 . . ? C37 C38 C39 118.8(3) . . ? C37 C38 Co1 69.92(16) . . ? C39 C38 Co1 69.71(15) . . ? C37 C38 H38 120.6 . . ? C39 C38 H38 120.6 . . ? Co1 C38 H38 132.7 . . ? C40 C39 C38 121.3(3) . . ? C40 C39 Co1 70.58(14) . . ? C38 C39 Co1 72.01(15) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? Co1 C39 H39 130.9 . . ? C41 C40 C39 119.8(3) . . ? C41 C40 Co1 70.05(15) . . ? C39 C40 Co1 70.88(15) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? Co1 C40 H40 131.8 . . ? C40 C41 C36 119.2(2) . . ? C40 C41 Co1 71.50(15) . . ? C36 C41 Co1 68.87(15) . . ? C40 C41 H41 120.4 . . ? C36 C41 H41 120.4 . . ? Co1 C41 H41 132.0 . . ? O1 C42 C43 110.3(3) 2_655 . ? O1 C42 H42A 109.6 2_655 . ? C43 C42 H42A 109.6 . . ? O1 C42 H42B 109.6 2_655 . ? C43 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? O1 C43 C42 110.8(3) . . ? O1 C43 H43A 109.5 . . ? C42 C43 H43A 109.5 . . ? O1 C43 H43B 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 108.1 . . ? C2 N1 C1 112.3(2) . . ? C2 N1 C4 120.2(2) . . ? C1 N1 C4 127.4(2) . . ? C3 N2 C1 112.8(2) . . ? C3 N2 C16 120.3(2) . . ? C1 N2 C16 126.9(2) . . ? C1 Co1 C28 88.93(10) . . ? C1 Co1 C36 171.45(10) . . ? C28 Co1 C36 85.94(10) . . ? C1 Co1 C41 136.48(10) . . ? C28 Co1 C41 105.06(10) . . ? C36 Co1 C41 39.51(11) . . ? C1 Co1 C40 110.15(10) . . ? C28 Co1 C40 141.14(11) . . ? C36 Co1 C40 70.43(11) . . ? C41 Co1 C40 38.45(10) . . ? C1 Co1 C39 102.94(10) . . ? C28 Co1 C39 167.16(11) . . ? C36 Co1 C39 82.84(11) . . ? C41 Co1 C39 69.67(11) . . ? C40 Co1 C39 38.53(11) . . ? C1 Co1 C37 148.94(11) . . ? C28 Co1 C37 98.43(11) . . ? C36 Co1 C37 39.10(11) . . ? C41 Co1 C37 70.59(11) . . ? C40 Co1 C37 82.56(11) . . ? C39 Co1 C37 68.86(11) . . ? C1 Co1 C38 118.45(10) . . ? C28 Co1 C38 130.99(12) . . ? C36 Co1 C38 69.97(11) . . ? C41 Co1 C38 82.99(11) . . ? C40 Co1 C38 69.74(11) . . ? C39 Co1 C38 38.27(11) . . ? C37 Co1 C38 37.84(11) . . ? C43 O1 C42 109.0(3) . 2_655 ? 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 C2 C3 N2 -0.1(3) . . . . ? C9 C4 C5 C6 2.6(4) . . . . ? N1 C4 C5 C6 176.6(2) . . . . ? C9 C4 C5 C10 -173.9(2) . . . . ? N1 C4 C5 C10 0.1(4) . . . . ? C4 C5 C6 C7 -2.4(4) . . . . ? C10 C5 C6 C7 174.1(3) . . . . ? C5 C6 C7 C8 0.5(5) . . . . ? C6 C7 C8 C9 1.3(5) . . . . ? C7 C8 C9 C4 -1.1(4) . . . . ? C7 C8 C9 C13 -179.9(3) . . . . ? C5 C4 C9 C8 -0.9(4) . . . . ? N1 C4 C9 C8 -174.9(2) . . . . ? C5 C4 C9 C13 177.8(2) . . . . ? N1 C4 C9 C13 3.7(4) . . . . ? C6 C5 C10 C12 -99.1(3) . . . . ? C4 C5 C10 C12 77.3(3) . . . . ? C6 C5 C10 C11 24.1(4) . . . . ? C4 C5 C10 C11 -159.5(3) . . . . ? C8 C9 C13 C14 72.0(3) . . . . ? C4 C9 C13 C14 -106.7(3) . . . . ? C8 C9 C13 C15 -50.7(3) . . . . ? C4 C9 C13 C15 130.7(3) . . . . ? C21 C16 C17 C18 2.0(4) . . . . ? N2 C16 C17 C18 -174.3(2) . . . . ? C21 C16 C17 C22 -176.6(3) . . . . ? N2 C16 C17 C22 7.1(4) . . . . ? C16 C17 C18 C19 -0.7(4) . . . . ? C22 C17 C18 C19 177.9(3) . . . . ? C17 C18 C19 C20 -1.3(4) . . . . ? C18 C19 C20 C21 2.1(4) . . . . ? C19 C20 C21 C16 -0.9(4) . . . . ? C19 C20 C21 C25 -179.9(2) . . . . ? C17 C16 C21 C20 -1.2(4) . . . . ? N2 C16 C21 C20 175.0(2) . . . . ? C17 C16 C21 C25 177.8(2) . . . . ? N2 C16 C21 C25 -5.9(4) . . . . ? C16 C17 C22 C24 133.2(3) . . . . ? C18 C17 C22 C24 -45.3(4) . . . . ? C16 C17 C22 C23 -103.5(3) . . . . ? C18 C17 C22 C23 78.0(4) . . . . ? C20 C21 C25 C27 20.6(4) . . . . ? C16 C21 C25 C27 -158.3(3) . . . . ? C20 C21 C25 C26 -104.3(3) . . . . ? C16 C21 C25 C26 76.8(3) . . . . ? Co1 C28 C29 C30 -123.3(2) . . . . ? Co1 C28 C29 C34 58.0(3) . . . . ? C34 C29 C30 C31 2.2(4) . . . . ? C28 C29 C30 C31 -176.5(3) . . . . ? C29 C30 C31 C32 -1.0(5) . . . . ? C30 C31 C32 C33 -0.7(5) . . . . ? C31 C32 C33 C34 1.2(5) . . . . ? C32 C33 C34 C29 0.1(5) . . . . ? C32 C33 C34 C35 178.5(3) . . . . ? C30 C29 C34 C33 -1.7(4) . . . . ? C28 C29 C34 C33 177.0(3) . . . . ? C30 C29 C34 C35 179.9(3) . . . . ? C28 C29 C34 C35 -1.4(4) . . . . ? C33 C34 C35 C36 135.0(3) . . . . ? C29 C34 C35 C36 -46.6(4) . . . . ? C34 C35 C36 C37 127.4(3) . . . . ? C34 C35 C36 C41 -49.3(3) . . . . ? C34 C35 C36 Co1 38.3(4) . . . . ? C41 C36 C37 C38 3.4(4) . . . . ? C35 C36 C37 C38 -173.3(2) . . . . ? Co1 C36 C37 C38 -52.1(2) . . . . ? C41 C36 C37 Co1 55.5(2) . . . . ? C35 C36 C37 Co1 -121.2(2) . . . . ? C36 C37 C38 C39 -1.2(4) . . . . ? Co1 C37 C38 C39 -51.5(2) . . . . ? C36 C37 C38 Co1 50.3(2) . . . . ? C37 C38 C39 C40 -1.1(4) . . . . ? Co1 C38 C39 C40 -52.6(2) . . . . ? C37 C38 C39 Co1 51.6(2) . . . . ? C38 C39 C40 C41 1.2(4) . . . . ? Co1 C39 C40 C41 -52.1(2) . . . . ? C38 C39 C40 Co1 53.3(2) . . . . ? C39 C40 C41 C36 1.0(4) . . . . ? Co1 C40 C41 C36 -51.5(2) . . . . ? C39 C40 C41 Co1 52.5(2) . . . . ? C37 C36 C41 C40 -3.2(4) . . . . ? C35 C36 C41 C40 173.5(2) . . . . ? Co1 C36 C41 C40 52.7(2) . . . . ? C37 C36 C41 Co1 -56.0(2) . . . . ? C35 C36 C41 Co1 120.7(2) . . . . ? O1 C42 C43 O1 -59.1(4) 2_655 . . . ? C3 C2 N1 C1 -0.2(3) . . . . ? C3 C2 N1 C4 176.6(2) . . . . ? N2 C1 N1 C2 0.5(2) . . . . ? Co1 C1 N1 C2 -175.43(17) . . . . ? N2 C1 N1 C4 -176.1(2) . . . . ? Co1 C1 N1 C4 8.0(3) . . . . ? C5 C4 N1 C2 -105.9(3) . . . . ? C9 C4 N1 C2 68.4(3) . . . . ? C5 C4 N1 C1 70.5(3) . . . . ? C9 C4 N1 C1 -115.3(3) . . . . ? C2 C3 N2 C1 0.5(3) . . . . ? C2 C3 N2 C16 -177.1(2) . . . . ? N1 C1 N2 C3 -0.6(2) . . . . ? Co1 C1 N2 C3 175.47(17) . . . . ? N1 C1 N2 C16 176.8(2) . . . . ? Co1 C1 N2 C16 -7.2(3) . . . . ? C17 C16 N2 C3 71.6(3) . . . . ? C21 C16 N2 C3 -104.8(3) . . . . ? C17 C16 N2 C1 -105.5(3) . . . . ? C21 C16 N2 C1 78.0(3) . . . . ? N2 C1 Co1 C28 -123.3(2) . . . . ? N1 C1 Co1 C28 51.6(2) . . . . ? N2 C1 Co1 C41 -12.3(3) . . . . ? N1 C1 Co1 C41 162.55(18) . . . . ? N2 C1 Co1 C40 22.1(2) . . . . ? N1 C1 Co1 C40 -163.05(19) . . . . ? N2 C1 Co1 C39 61.7(2) . . . . ? N1 C1 Co1 C39 -123.5(2) . . . . ? N2 C1 Co1 C37 132.1(2) . . . . ? N1 C1 Co1 C37 -53.1(3) . . . . ? N2 C1 Co1 C38 99.3(2) . . . . ? N1 C1 Co1 C38 -85.8(2) . . . . ? C29 C28 Co1 C1 123.1(2) . . . . ? C29 C28 Co1 C36 -50.1(2) . . . . ? C29 C28 Co1 C41 -15.2(2) . . . . ? C29 C28 Co1 C40 1.4(3) . . . . ? C29 C28 Co1 C39 -79.2(6) . . . . ? C29 C28 Co1 C37 -87.2(2) . . . . ? C29 C28 Co1 C38 -109.0(2) . . . . ? C37 C36 Co1 C28 -108.70(17) . . . . ? C41 C36 Co1 C28 119.70(16) . . . . ? C35 C36 Co1 C28 5.9(3) . . . . ? C37 C36 Co1 C41 131.6(2) . . . . ? C35 C36 Co1 C41 -113.8(3) . . . . ? C37 C36 Co1 C40 102.68(18) . . . . ? C41 C36 Co1 C40 -28.92(15) . . . . ? C35 C36 Co1 C40 -142.7(3) . . . . ? C37 C36 Co1 C39 65.06(17) . . . . ? C41 C36 Co1 C39 -66.54(16) . . . . ? C35 C36 Co1 C39 179.7(3) . . . . ? C41 C36 Co1 C37 -131.6(2) . . . . ? C35 C36 Co1 C37 114.6(3) . . . . ? C37 C36 Co1 C38 27.84(17) . . . . ? C41 C36 Co1 C38 -103.76(17) . . . . ? C35 C36 Co1 C38 142.5(3) . . . . ? C40 C41 Co1 C1 58.5(2) . . . . ? C36 C41 Co1 C1 -168.58(15) . . . . ? C40 C41 Co1 C28 163.33(17) . . . . ? C36 C41 Co1 C28 -63.80(17) . . . . ? C40 C41 Co1 C36 -132.9(2) . . . . ? C36 C41 Co1 C40 132.9(2) . . . . ? C40 C41 Co1 C39 -28.97(17) . . . . ? C36 C41 Co1 C39 103.91(17) . . . . ? C40 C41 Co1 C37 -102.88(18) . . . . ? C36 C41 Co1 C37 30.00(15) . . . . ? C40 C41 Co1 C38 -66.03(17) . . . . ? C36 C41 Co1 C38 66.84(16) . . . . ? C41 C40 Co1 C1 -141.27(16) . . . . ? C39 C40 Co1 C1 85.54(18) . . . . ? C41 C40 Co1 C28 -26.2(3) . . . . ? C39 C40 Co1 C28 -159.41(18) . . . . ? C41 C40 Co1 C36 29.66(16) . . . . ? C39 C40 Co1 C36 -103.54(18) . . . . ? C39 C40 Co1 C41 -133.2(2) . . . . ? C41 C40 Co1 C39 133.2(2) . . . . ? C41 C40 Co1 C37 68.01(17) . . . . ? C39 C40 Co1 C37 -65.18(18) . . . . ? C41 C40 Co1 C38 104.81(18) . . . . ? C39 C40 Co1 C38 -28.39(17) . . . . ? C40 C39 Co1 C1 -106.19(17) . . . . ? C38 C39 Co1 C1 119.87(17) . . . . ? C40 C39 Co1 C28 96.6(5) . . . . ? C38 C39 Co1 C28 -37.3(6) . . . . ? C40 C39 Co1 C36 67.41(17) . . . . ? C38 C39 Co1 C36 -66.54(18) . . . . ? C40 C39 Co1 C41 28.91(16) . . . . ? C38 C39 Co1 C41 -105.03(19) . . . . ? C38 C39 Co1 C40 -133.9(3) . . . . ? C40 C39 Co1 C37 105.22(18) . . . . ? C38 C39 Co1 C37 -28.72(17) . . . . ? C40 C39 Co1 C38 133.9(3) . . . . ? C38 C37 Co1 C1 -50.8(3) . . . . ? C36 C37 Co1 C1 174.87(18) . . . . ? C38 C37 Co1 C28 -152.89(18) . . . . ? C36 C37 Co1 C28 72.78(17) . . . . ? C38 C37 Co1 C36 134.3(3) . . . . ? C38 C37 Co1 C41 104.04(19) . . . . ? C36 C37 Co1 C41 -30.30(16) . . . . ? C38 C37 Co1 C40 66.35(18) . . . . ? C36 C37 Co1 C40 -67.99(17) . . . . ? C38 C37 Co1 C39 29.03(17) . . . . ? C36 C37 Co1 C39 -105.30(18) . . . . ? C36 C37 Co1 C38 -134.3(3) . . . . ? C37 C38 Co1 C1 152.95(17) . . . . ? C39 C38 Co1 C1 -74.00(19) . . . . ? C37 C38 Co1 C28 36.7(2) . . . . ? C39 C38 Co1 C28 169.73(16) . . . . ? C37 C38 Co1 C36 -28.70(17) . . . . ? C39 C38 Co1 C36 104.36(18) . . . . ? C37 C38 Co1 C41 -67.21(18) . . . . ? C39 C38 Co1 C41 65.85(17) . . . . ? C37 C38 Co1 C40 -104.49(19) . . . . ? C39 C38 Co1 C40 28.57(16) . . . . ? C37 C38 Co1 C39 -133.1(3) . . . . ? C39 C38 Co1 C37 133.1(3) . . . . ? C42 C43 O1 C42 58.4(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 31.27 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.838 _refine_diff_density_min -0.725 _refine_diff_density_rms 0.081 #== END