# Electronic Supplementary Material (ESI) for CrystEngComm # 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_PNC[Co-vBipy] _database_code_depnum_ccdc_archive 'CCDC 900365' #TrackingRef '900365_PNC[Co-vBipy].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C141.17 H156.92 Cl7.75 Co N10 O8.58' _chemical_formula_weight 2464.68 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.4921(9) _cell_length_b 37.4921(9) _cell_length_c 37.4921(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52701(2) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7998 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 16.68 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.932 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15616 _exptl_absorpt_coefficient_mu 0.261 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8184 _exptl_absorpt_correction_T_max 0.8591 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68840 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Station 9.8, SRS, Daresbury' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7777 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0462 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.19 _reflns_number_total 7777 _reflns_number_gt 4688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7777 _refine_ls_number_parameters 340 _refine_ls_number_restraints 14 _refine_ls_R_factor_all 0.1797 _refine_ls_R_factor_gt 0.1455 _refine_ls_wR_factor_ref 0.4358 _refine_ls_wR_factor_gt 0.4179 _refine_ls_goodness_of_fit_ref 1.581 _refine_ls_restrained_S_all 1.587 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.07761(4) 0.0607(5) Uani 1 4 d S . . O1 O 0.61106(10) 0.90381(10) 0.11068(12) 0.0782(11) Uani 1 1 d . A . O2 O 0.66872(9) 0.93957(9) 0.11137(12) 0.0752(11) Uani 1 1 d . . . N1 N 0.72207(11) 0.79271(11) 0.08185(12) 0.0634(12) Uani 1 1 d . A . N2 N 0.76818(12) 0.83771(11) 0.08522(13) 0.0689(12) Uani 1 1 d . A . C1 C 0.67454(14) 0.83186(13) 0.08883(15) 0.0650(14) Uani 1 1 d . . . C2 C 0.64151(14) 0.84825(14) 0.09550(16) 0.0681(14) Uani 1 1 d . A . H2 H 0.6200 0.8349 0.0950 0.102 Uiso 1 1 calc R . . C3 C 0.64118(14) 0.88331(15) 0.10257(16) 0.0695(15) Uani 1 1 d . . . C4 C 0.67341(14) 0.90412(13) 0.10190(15) 0.0658(14) Uani 1 1 d . A . C5 C 0.70526(15) 0.88866(14) 0.09436(17) 0.0719(15) Uani 1 1 d . . . H5 H 0.7266 0.9023 0.0931 0.108 Uiso 1 1 calc R A . C6 C 0.70541(13) 0.85135(14) 0.08850(15) 0.0661(14) Uani 1 1 d . A . C7 C 0.73472(13) 0.82683(13) 0.08384(15) 0.0606(13) Uani 1 1 d . . . C8 C 0.79500(13) 0.81487(13) 0.08469(15) 0.0629(13) Uani 1 1 d . . . C9 C 0.57864(15) 0.88628(16) 0.11366(19) 0.0744(16) Uani 1 1 d . . . C10 C 0.57046(17) 0.87216(16) 0.1467(2) 0.090(2) Uani 1 1 d . A . C11 C 0.5355(2) 0.8555(2) 0.1514(3) 0.132(4) Uani 1 1 d . . . H11 H 0.5290 0.8445 0.1732 0.198 Uiso 1 1 calc R A . C12 C 0.5129(2) 0.8564(3) 0.1235(4) 0.136(4) Uani 1 1 d . A . H12 H 0.4897 0.8467 0.1265 0.205 Uiso 1 1 calc R . . C13 C 0.5219(2) 0.8708(3) 0.0905(3) 0.129(3) Uani 1 1 d . . . H13 H 0.5053 0.8701 0.0714 0.193 Uiso 1 1 calc R A . C14 C 0.55651(18) 0.8870(2) 0.0855(2) 0.100(2) Uani 1 1 d . A . C15 C 0.59575(19) 0.87373(17) 0.1774(2) 0.092(2) Uani 1 1 d . . . H15 H 0.6199 0.8676 0.1679 0.138 Uiso 1 1 calc R A . C16 C 0.5982(2) 0.91104(19) 0.1925(2) 0.098(2) Uani 1 1 d . A . H16A H 0.5752 0.9179 0.2028 0.147 Uiso 1 1 calc R . . H16B H 0.6046 0.9277 0.1734 0.147 Uiso 1 1 calc R . . H16C H 0.6166 0.9117 0.2111 0.147 Uiso 1 1 calc R . . C17 C 0.5877(3) 0.8471(2) 0.2083(2) 0.130(3) Uani 1 1 d . A . H17A H 0.5633 0.8507 0.2167 0.195 Uiso 1 1 calc R . . H17B H 0.6044 0.8513 0.2279 0.195 Uiso 1 1 calc R . . H17C H 0.5905 0.8226 0.1995 0.195 Uiso 1 1 calc R . . C18 C 0.5668(2) 0.9058(3) 0.0515(2) 0.116(3) Uani 1 1 d . . . H18 H 0.5926 0.9003 0.0475 0.174 Uiso 1 1 calc R A . C19 C 0.5470(3) 0.8928(3) 0.0179(3) 0.166(4) Uani 1 1 d . A . H19A H 0.5514 0.9094 -0.0018 0.248 Uiso 1 1 calc R . . H19B H 0.5213 0.8917 0.0228 0.248 Uiso 1 1 calc R . . H19C H 0.5556 0.8690 0.0114 0.248 Uiso 1 1 calc R . . C20 C 0.5643(3) 0.9457(3) 0.0543(3) 0.143(4) Uani 1 1 d . A . H20A H 0.5612 0.9559 0.0304 0.214 Uiso 1 1 calc R . . H20B H 0.5862 0.9551 0.0650 0.214 Uiso 1 1 calc R . . H20C H 0.5438 0.9521 0.0692 0.214 Uiso 1 1 calc R . . C21A C 0.70050(19) 0.9600(2) 0.1139(2) 0.064(4) Uiso 0.479(13) 1 d PG A 1 C22A C 0.7097(2) 0.9806(2) 0.0846(2) 0.071(3) Uiso 0.479(13) 1 d PG A 1 C23A C 0.7401(3) 1.0020(2) 0.0857(2) 0.079(4) Uiso 0.479(13) 1 d PG A 1 H23A H 0.7464 1.0161 0.0656 0.119 Uiso 0.479(13) 1 calc PR A 1 C24A C 0.7611(2) 1.0026(2) 0.1162(3) 0.082(4) Uiso 0.479(13) 1 d PG A 1 H24A H 0.7818 1.0172 0.1170 0.123 Uiso 0.479(13) 1 calc PR A 1 C25A C 0.75188(19) 0.9819(2) 0.1455(2) 0.077(4) Uiso 0.479(13) 1 d PG A 1 H25A H 0.7663 0.9824 0.1664 0.116 Uiso 0.479(13) 1 calc PR A 1 C26A C 0.7216(2) 0.9606(2) 0.1444(2) 0.057(3) Uiso 0.479(13) 1 d PG A 1 C21B C 0.69663(18) 0.9603(2) 0.1041(2) 0.065(3) Uiso 0.521(13) 1 d PG A 2 C22B C 0.6993(2) 0.9801(2) 0.0729(2) 0.070(3) Uiso 0.521(13) 1 d PG A 2 C23B C 0.7287(2) 1.0021(2) 0.0674(2) 0.093(4) Uiso 0.521(13) 1 d PG A 2 H23B H 0.7305 1.0157 0.0460 0.139 Uiso 0.521(13) 1 calc PR A 2 C24B C 0.7553(2) 1.0043(2) 0.0931(3) 0.088(4) Uiso 0.521(13) 1 d PG A 2 H24B H 0.7754 1.0193 0.0893 0.133 Uiso 0.521(13) 1 calc PR A 2 C25B C 0.75262(19) 0.9845(2) 0.1243(3) 0.091(4) Uiso 0.521(13) 1 d PG A 2 H25B H 0.7708 0.9859 0.1418 0.137 Uiso 0.521(13) 1 calc PR A 2 C26B C 0.7233(2) 0.9625(2) 0.1298(2) 0.071(3) Uiso 0.521(13) 1 d PGD A 2 C27A C 0.6865(5) 0.9788(4) 0.0501(4) 0.080(4) Uiso 0.479(13) 1 d P A 1 H27A H 0.6804 0.9530 0.0467 0.120 Uiso 0.479(13) 1 calc PR A 1 C28A C 0.6488(5) 0.9995(6) 0.0545(6) 0.115(6) Uiso 0.479(13) 1 d P A 1 H28D H 0.6387 1.0043 0.0309 0.173 Uiso 0.479(13) 1 calc PR A 1 H28E H 0.6527 1.0221 0.0671 0.173 Uiso 0.479(13) 1 calc PR A 1 H28F H 0.6322 0.9846 0.0682 0.173 Uiso 0.479(13) 1 calc PR A 1 C29A C 0.7073(6) 0.9900(6) 0.0171(6) 0.133(7) Uiso 0.479(13) 1 d P A 1 H29A H 0.7180 0.9688 0.0059 0.200 Uiso 0.479(13) 1 calc PR A 1 H29B H 0.7262 1.0067 0.0239 0.200 Uiso 0.479(13) 1 calc PR A 1 H29C H 0.6912 1.0015 0.0001 0.200 Uiso 0.479(13) 1 calc PR A 1 C27B C 0.6685(5) 0.9766(4) 0.0464(4) 0.091(4) Uiso 0.521(13) 1 d PD A 2 H27B H 0.6501 0.9602 0.0565 0.137 Uiso 0.521(13) 1 calc PR A 2 C28B C 0.6526(5) 1.0120(5) 0.0412(6) 0.122(6) Uiso 0.521(13) 1 d P A 2 H28A H 0.6667 1.0255 0.0239 0.183 Uiso 0.521(13) 1 calc PR A 2 H28B H 0.6521 1.0248 0.0640 0.183 Uiso 0.521(13) 1 calc PR A 2 H28C H 0.6281 1.0093 0.0323 0.183 Uiso 0.521(13) 1 calc PR A 2 C29B C 0.6863(9) 0.9589(9) 0.0162(7) 0.225(14) Uiso 0.521(13) 1 d PD A 2 H29D H 0.6984 0.9374 0.0246 0.338 Uiso 0.521(13) 1 calc PR A 2 H29E H 0.7038 0.9752 0.0056 0.338 Uiso 0.521(13) 1 calc PR A 2 H29F H 0.6685 0.9524 -0.0018 0.338 Uiso 0.521(13) 1 calc PR A 2 C30 C 0.7179(2) 0.9412(2) 0.1679(3) 0.134(4) Uani 1 1 d D . . H30 H 0.7019 0.9207 0.1616 0.202 Uiso 1 1 calc R A 1 C31 C 0.7045(3) 0.9621(3) 0.2024(4) 0.161(4) Uani 1 1 d . A . H31A H 0.7019 0.9453 0.2223 0.242 Uiso 1 1 calc R . . H31B H 0.6814 0.9732 0.1974 0.242 Uiso 1 1 calc R . . H31C H 0.7219 0.9805 0.2087 0.242 Uiso 1 1 calc R . . C32A C 0.7581(6) 0.9283(7) 0.1773(6) 0.130(9) Uiso 0.48(3) 1 d P A 1 H32A H 0.7577 0.9131 0.1985 0.195 Uiso 0.48(3) 1 calc PR A 1 H32B H 0.7731 0.9492 0.1818 0.195 Uiso 0.48(3) 1 calc PR A 1 H32C H 0.7679 0.9148 0.1571 0.195 Uiso 0.48(3) 1 calc PR A 1 C32B C 0.7383(6) 0.9072(6) 0.1831(5) 0.123(8) Uiso 0.52(3) 1 d P A 2 H32D H 0.7406 0.8892 0.1643 0.185 Uiso 0.52(3) 1 calc PR A 2 H32E H 0.7249 0.8971 0.2031 0.185 Uiso 0.52(3) 1 calc PR A 2 H32F H 0.7622 0.9143 0.1912 0.185 Uiso 0.52(3) 1 calc PR A 2 Cl3S Cl 0.71055(15) 0.04613(15) 0.93148(14) 0.1371(16) Uiso 0.50 1 d P . . Cl1 Cl 0.7535(3) -0.0020(3) 0.8814(3) 0.231(4) Uiso 0.50 1 d P . . Cl2 Cl 0.6767(4) -0.0025(4) 0.8803(4) 0.311(6) Uiso 0.50 1 d P . . C7S C 0.7148(4) 0.0265(4) 0.8946(4) 0.109(5) Uiso 0.50 1 d P . . N1S N 0.7500 0.7500 0.0215(3) 0.086(3) Uani 1 4 d SD . . C1S C 0.7570(6) 0.7800(5) 0.0009(6) 0.154(7) Uiso 0.50 1 d PD . . C2S C 0.7576(6) 0.7811(11) -0.0359(7) 0.300 Uiso 0.50 1 d PD . . C3S C 0.7500 0.7500 -0.0562(17) 0.300 Uiso 1 4 d SD . . C4S C 0.7500 0.7500 -0.0968(17) 0.300 Uiso 1 4 d SD . . C5S C 0.7596(13) 0.7826(11) -0.1148(12) 0.300 Uiso 0.50 1 d PD . . C6S C 0.7615(13) 0.7841(9) -0.1527(12) 0.300 Uiso 0.50 1 d PD . . N2S N 0.7500 0.7500 -0.1655(12) 0.300 Uiso 1 4 d SD . . 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 0.0464(5) 0.0464(5) 0.0893(11) 0.000 0.000 0.000 O1 0.060(2) 0.064(2) 0.111(3) -0.005(2) 0.018(2) 0.0088(17) O2 0.061(2) 0.049(2) 0.115(3) -0.0098(19) 0.012(2) 0.0017(16) N1 0.047(2) 0.051(2) 0.092(3) 0.007(2) 0.008(2) 0.0031(17) N2 0.058(3) 0.056(3) 0.093(3) -0.002(2) 0.004(2) -0.003(2) C1 0.058(3) 0.054(3) 0.083(4) 0.009(2) 0.007(3) 0.001(2) C2 0.052(3) 0.057(3) 0.096(4) 0.010(3) 0.008(3) 0.003(2) C3 0.057(3) 0.061(3) 0.090(4) 0.001(3) 0.016(3) 0.016(2) C4 0.060(3) 0.050(3) 0.088(4) 0.000(2) 0.007(3) 0.007(2) C5 0.063(3) 0.050(3) 0.104(4) -0.001(3) 0.007(3) 0.002(2) C6 0.050(3) 0.057(3) 0.091(4) 0.006(3) 0.011(3) 0.005(2) C7 0.048(3) 0.051(3) 0.084(4) -0.002(2) 0.009(2) -0.004(2) C8 0.053(3) 0.049(3) 0.087(4) -0.003(2) 0.001(2) 0.000(2) C9 0.051(3) 0.070(3) 0.102(5) -0.015(3) 0.015(3) 0.007(3) C10 0.066(4) 0.068(4) 0.137(6) -0.031(4) 0.032(4) -0.003(3) C11 0.075(5) 0.097(5) 0.223(11) -0.055(6) 0.062(6) -0.006(4) C12 0.057(4) 0.153(8) 0.199(11) -0.098(8) 0.018(6) -0.014(5) C13 0.075(5) 0.156(8) 0.155(9) -0.065(7) 0.006(5) 0.012(5) C14 0.062(4) 0.108(5) 0.130(7) -0.039(5) 0.013(4) 0.023(4) C15 0.084(4) 0.071(4) 0.121(6) -0.002(4) 0.024(4) -0.007(3) C16 0.099(5) 0.087(5) 0.107(5) -0.011(4) 0.003(4) 0.002(4) C17 0.185(9) 0.086(5) 0.120(7) 0.011(4) 0.053(6) -0.007(5) C18 0.100(5) 0.137(7) 0.111(6) -0.032(5) -0.019(5) 0.033(5) C19 0.177(10) 0.173(10) 0.147(9) -0.012(7) -0.035(8) 0.049(8) C20 0.157(9) 0.114(7) 0.157(8) -0.015(6) 0.017(7) 0.050(6) C30 0.134(7) 0.092(5) 0.178(9) -0.038(6) -0.074(6) 0.045(5) C31 0.124(8) 0.145(9) 0.214(12) -0.033(8) -0.022(7) 0.037(7) N1S 0.078(4) 0.078(4) 0.100(8) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.920(4) . ? Co1 N1 1.920(4) 2_665 ? Co1 N1 1.920(4) 15_565 ? Co1 N1 1.920(4) 16_655 ? Co1 N1S 2.105(12) . ? O1 C9 1.386(7) . ? O1 C3 1.399(6) . ? O2 C21B 1.332(6) . ? O2 C4 1.387(6) . ? O2 C21A 1.419(7) . ? N1 C7 1.366(6) . ? N1 C8 1.392(6) 16_655 ? N2 C7 1.320(7) . ? N2 C8 1.321(7) . ? C1 C6 1.369(7) . ? C1 C2 1.405(7) . ? C1 C8 1.446(7) 16_655 ? C2 C3 1.341(8) . ? C2 H2 0.9500 . ? C3 C4 1.439(8) . ? C4 C5 1.357(7) . ? C5 C6 1.416(7) . ? C5 H5 0.9500 . ? C6 C7 1.443(7) . ? C8 N1 1.392(6) 15_565 ? C8 C1 1.446(7) 15_565 ? C9 C14 1.343(10) . ? C9 C10 1.382(10) . ? C10 C11 1.463(10) . ? C10 C15 1.493(11) . ? C11 C12 1.344(14) . ? C11 H11 0.9500 . ? C12 C13 1.392(15) . ? C12 H12 0.9500 . ? C13 C14 1.444(12) . ? C13 H13 0.9500 . ? C14 C18 1.507(13) . ? C15 C16 1.511(10) . ? C15 C17 1.555(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.503(12) . ? C18 C19 1.542(13) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.559(16) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.151(11) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.531(18) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.649(11) . ? C27A C29A 1.52(2) . ? C27A C28A 1.62(3) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C28B 1.47(2) . ? C27B C29B 1.472(18) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C32B 1.593(19) . ? C30 C31 1.595(14) . ? C30 C32A 1.62(2) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? Cl3S C7S 1.573(17) . ? Cl1 C7S 1.87(2) . ? Cl2 C7S 1.87(2) . ? N1S C1S 1.387(16) 16_655 ? N1S C1S 1.388(16) . ? N1S C1S 1.388(16) 2_665 ? N1S C1S 1.388(16) 15_565 ? C1S C2S 1.380(19) . ? C1S C1S 1.63(3) 16_655 ? C1S C1S 1.63(3) 15_565 ? C2S C3S 1.422(18) . ? C2S C2S 1.70(6) 15_565 ? C2S C2S 1.70(6) 16_655 ? C3S C2S 1.422(18) 15_565 ? C3S C2S 1.422(18) 16_655 ? C3S C2S 1.422(18) 2_665 ? C3S C4S 1.52(2) . ? C4S C5S 1.443(19) 16_655 ? C4S C5S 1.443(19) 2_665 ? C4S C5S 1.443(19) . ? C4S C5S 1.443(19) 15_565 ? C5S C6S 1.423(19) . ? C5S C5S 1.80(6) 16_655 ? C5S C5S 1.80(6) 15_565 ? C6S N2S 1.431(19) . ? C6S C6S 1.91(4) 16_655 ? C6S C6S 1.91(4) 15_565 ? N2S C6S 1.431(19) 15_565 ? N2S C6S 1.431(19) 16_655 ? N2S C6S 1.431(19) 2_665 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 170.5(3) . 2_665 ? N1 Co1 N1 89.61(2) . 15_565 ? N1 Co1 N1 89.60(2) 2_665 15_565 ? N1 Co1 N1 89.60(2) . 16_655 ? N1 Co1 N1 89.61(2) 2_665 16_655 ? N1 Co1 N1 170.5(3) 15_565 16_655 ? N1 Co1 N1S 94.76(15) . . ? N1 Co1 N1S 94.76(15) 2_665 . ? N1 Co1 N1S 94.76(15) 15_565 . ? N1 Co1 N1S 94.76(15) 16_655 . ? C9 O1 C3 117.7(4) . . ? C21B O2 C4 114.1(5) . . ? C21B O2 C21A 16.1(5) . . ? C4 O2 C21A 115.3(5) . . ? C7 N1 C8 106.5(4) . 16_655 ? C7 N1 Co1 126.6(3) . . ? C8 N1 Co1 126.9(3) 16_655 . ? C7 N2 C8 121.5(4) . . ? C6 C1 C2 120.9(5) . . ? C6 C1 C8 106.1(4) . 16_655 ? C2 C1 C8 132.8(5) . 16_655 ? C3 C2 C1 118.2(5) . . ? C3 C2 H2 120.9 . . ? C1 C2 H2 120.9 . . ? C2 C3 O1 126.1(5) . . ? C2 C3 C4 121.4(5) . . ? O1 C3 C4 112.6(5) . . ? C5 C4 O2 125.0(5) . . ? C5 C4 C3 120.7(5) . . ? O2 C4 C3 114.1(4) . . ? C4 C5 C6 117.2(5) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? C1 C6 C5 121.5(5) . . ? C1 C6 C7 107.7(4) . . ? C5 C6 C7 130.6(5) . . ? N2 C7 N1 128.4(5) . . ? N2 C7 C6 121.5(4) . . ? N1 C7 C6 109.8(4) . . ? N2 C8 N1 126.8(4) . 15_565 ? N2 C8 C1 123.2(4) . 15_565 ? N1 C8 C1 109.9(4) 15_565 15_565 ? C14 C9 C10 125.1(6) . . ? C14 C9 O1 118.0(7) . . ? C10 C9 O1 116.7(6) . . ? C9 C10 C11 118.0(8) . . ? C9 C10 C15 122.4(6) . . ? C11 C10 C15 119.6(8) . . ? C12 C11 C10 117.4(10) . . ? C12 C11 H11 121.3 . . ? C10 C11 H11 121.3 . . ? C11 C12 C13 123.2(9) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C12 C13 C14 119.7(9) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 116.4(9) . . ? C9 C14 C18 121.0(7) . . ? C13 C14 C18 122.4(9) . . ? C10 C15 C16 111.3(6) . . ? C10 C15 C17 115.2(7) . . ? C16 C15 C17 109.2(7) . . ? C10 C15 H15 106.9 . . ? C16 C15 H15 106.9 . . ? C17 C15 H15 106.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C14 113.0(7) . . ? C20 C18 C19 110.0(8) . . ? C14 C18 C19 114.8(9) . . ? C20 C18 H18 106.1 . . ? C14 C18 H18 106.1 . . ? C19 C18 H18 106.1 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 117.2(5) . . ? C26A C21A O2 122.8(5) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 119.4(7) . . ? C23A C22A C27A 120.6(7) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 116.0(7) . . ? C30 C26A C21A 123.3(7) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 122.8(5) . . ? O2 C21B C26B 117.2(5) . . ? C22B C21B C26B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B C27B 116.5(8) . . ? C23B C22B C27B 123.5(7) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 120.9(6) . . ? C21B C26B C30 118.9(6) . . ? C29A C27A C22A 112.0(14) . . ? C29A C27A C28A 113.4(14) . . ? C22A C27A C28A 112.4(12) . . ? C29A C27A H27A 106.1 . . ? C22A C27A H27A 106.1 . . ? C28A C27A H27A 106.1 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C28B C27B C29B 119.4(19) . . ? C28B C27B C22B 108.4(13) . . ? C29B C27B C22B 101.3(18) . . ? C28B C27B H27B 109.0 . . ? C29B C27B H27B 109.0 . . ? C22B C27B H27B 109.0 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C32B 136.2(12) . . ? C26A C30 C31 110.4(9) . . ? C32B C30 C31 104.7(10) . . ? C26A C30 C32A 104.0(12) . . ? C32B C30 C32A 40.2(9) . . ? C31 C30 C32A 105.2(10) . . ? C26A C30 C26B 10.3(6) . . ? C32B C30 C26B 129.7(10) . . ? C31 C30 C26B 120.2(8) . . ? C32A C30 C26B 102.6(10) . . ? C26A C30 H30 112.3 . . ? C32B C30 H30 76.0 . . ? C31 C30 H30 112.3 . . ? C32A C30 H30 112.3 . . ? C26B C30 H30 104.1 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? Cl3S C7S Cl1 125.4(11) . . ? Cl3S C7S Cl2 116.4(11) . . ? Cl1 C7S Cl2 100.6(10) . . ? C1S N1S C1S 72.0(11) 16_655 . ? C1S N1S C1S 72.0(11) 16_655 2_665 ? C1S N1S C1S 113(2) . 2_665 ? C1S N1S C1S 113(2) 16_655 15_565 ? C1S N1S C1S 72.0(11) . 15_565 ? C1S N1S C1S 72.0(11) 2_665 15_565 ? C1S N1S Co1 123.7(11) 16_655 . ? C1S N1S Co1 123.7(11) . . ? C1S N1S Co1 123.7(11) 2_665 . ? C1S N1S Co1 123.7(11) 15_565 . ? C2S C1S N1S 126(3) . . ? C2S C1S C1S 91.7(14) . 16_655 ? N1S C1S C1S 54.0(5) . 16_655 ? C2S C1S C1S 91.0(14) . 15_565 ? N1S C1S C1S 54.0(5) . 15_565 ? C1S C1S C1S 90.000(8) 16_655 15_565 ? C1S C2S C3S 120(5) . . ? C1S C2S C2S 88.9(14) . 15_565 ? C3S C2S C2S 53.3(14) . 15_565 ? C1S C2S C2S 88.3(14) . 16_655 ? C3S C2S C2S 53.3(14) . 16_655 ? C2S C2S C2S 89.993(7) 15_565 16_655 ? C2S C3S C2S 115(6) 15_565 16_655 ? C2S C3S C2S 73(3) 15_565 . ? C2S C3S C2S 73(3) 16_655 . ? C2S C3S C2S 73(3) 15_565 2_665 ? C2S C3S C2S 73(3) 16_655 2_665 ? C2S C3S C2S 115(6) . 2_665 ? C2S C3S C4S 122(3) 15_565 . ? C2S C3S C4S 122(3) 16_655 . ? C2S C3S C4S 122(3) . . ? C2S C3S C4S 122(3) 2_665 . ? C5S C4S C5S 77(3) 16_655 2_665 ? C5S C4S C5S 77(3) 16_655 . ? C5S C4S C5S 124(7) 2_665 . ? C5S C4S C5S 124(7) 16_655 15_565 ? C5S C4S C5S 77(3) 2_665 15_565 ? C5S C4S C5S 77(3) . 15_565 ? C5S C4S C3S 118(3) 16_655 . ? C5S C4S C3S 118(3) 2_665 . ? C5S C4S C3S 118(3) . . ? C5S C4S C3S 118(3) 15_565 . ? C6S C5S C4S 121(5) . . ? C6S C5S C5S 94(3) . 16_655 ? C4S C5S C5S 51.3(14) . 16_655 ? C6S C5S C5S 91(3) . 15_565 ? C4S C5S C5S 51.3(14) . 15_565 ? C5S C5S C5S 90.003(10) 16_655 15_565 ? C5S C6S N2S 107(5) . . ? C5S C6S C6S 86(2) . 16_655 ? N2S C6S C6S 48.2(9) . 16_655 ? C5S C6S C6S 89(3) . 15_565 ? N2S C6S C6S 48.2(9) . 15_565 ? C6S C6S C6S 89.998(10) 16_655 15_565 ? C6S N2S C6S 83.5(18) 15_565 . ? C6S N2S C6S 141(6) 15_565 16_655 ? C6S N2S C6S 83.5(18) . 16_655 ? C6S N2S C6S 83.5(18) 15_565 2_665 ? C6S N2S C6S 141(6) . 2_665 ? C6S N2S C6S 83.5(18) 16_655 2_665 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C7 89.6(4) 2_665 . . . ? N1 Co1 N1 C7 4.4(6) 15_565 . . . ? N1 Co1 N1 C7 174.9(4) 16_655 . . . ? N1S Co1 N1 C7 -90.4(4) . . . . ? N1 Co1 N1 C8 -88.1(4) 2_665 . . 16_655 ? N1 Co1 N1 C8 -173.3(4) 15_565 . . 16_655 ? N1 Co1 N1 C8 -2.8(6) 16_655 . . 16_655 ? N1S Co1 N1 C8 91.9(4) . . . 16_655 ? C6 C1 C2 C3 -2.0(9) . . . . ? C8 C1 C2 C3 171.4(6) 16_655 . . . ? C1 C2 C3 O1 -178.3(5) . . . . ? C1 C2 C3 C4 2.7(9) . . . . ? C9 O1 C3 C2 3.8(9) . . . . ? C9 O1 C3 C4 -177.2(5) . . . . ? C21B O2 C4 C5 16.0(9) . . . . ? C21A O2 C4 C5 -1.7(9) . . . . ? C21B O2 C4 C3 -167.5(6) . . . . ? C21A O2 C4 C3 174.8(6) . . . . ? C2 C3 C4 C5 -0.6(9) . . . . ? O1 C3 C4 C5 -179.8(5) . . . . ? C2 C3 C4 O2 -177.3(5) . . . . ? O1 C3 C4 O2 3.6(7) . . . . ? O2 C4 C5 C6 174.1(5) . . . . ? C3 C4 C5 C6 -2.1(9) . . . . ? C2 C1 C6 C5 -0.8(9) . . . . ? C8 C1 C6 C5 -175.7(5) 16_655 . . . ? C2 C1 C6 C7 175.5(5) . . . . ? C8 C1 C6 C7 0.6(6) 16_655 . . . ? C4 C5 C6 C1 2.8(9) . . . . ? C4 C5 C6 C7 -172.5(6) . . . . ? C8 N2 C7 N1 0.1(9) . . . . ? C8 N2 C7 C6 172.8(5) . . . . ? C8 N1 C7 N2 174.1(5) 16_655 . . . ? Co1 N1 C7 N2 -4.0(8) . . . . ? C8 N1 C7 C6 0.7(6) 16_655 . . . ? Co1 N1 C7 C6 -177.3(4) . . . . ? C1 C6 C7 N2 -174.8(5) . . . . ? C5 C6 C7 N2 1.1(9) . . . . ? C1 C6 C7 N1 -0.8(6) . . . . ? C5 C6 C7 N1 175.0(6) . . . . ? C7 N2 C8 N1 1.7(9) . . . 15_565 ? C7 N2 C8 C1 -175.2(5) . . . 15_565 ? C3 O1 C9 C14 -98.9(7) . . . . ? C3 O1 C9 C10 86.7(6) . . . . ? C14 C9 C10 C11 2.2(9) . . . . ? O1 C9 C10 C11 176.2(5) . . . . ? C14 C9 C10 C15 -177.1(6) . . . . ? O1 C9 C10 C15 -3.2(8) . . . . ? C9 C10 C11 C12 -2.8(9) . . . . ? C15 C10 C11 C12 176.6(7) . . . . ? C10 C11 C12 C13 2.9(12) . . . . ? C11 C12 C13 C14 -2.2(14) . . . . ? C10 C9 C14 C13 -1.5(10) . . . . ? O1 C9 C14 C13 -175.4(6) . . . . ? C10 C9 C14 C18 174.7(6) . . . . ? O1 C9 C14 C18 0.8(9) . . . . ? C12 C13 C14 C9 1.4(11) . . . . ? C12 C13 C14 C18 -174.8(8) . . . . ? C9 C10 C15 C16 73.1(8) . . . . ? C11 C10 C15 C16 -106.2(7) . . . . ? C9 C10 C15 C17 -161.9(6) . . . . ? C11 C10 C15 C17 18.7(9) . . . . ? C9 C14 C18 C20 -75.4(9) . . . . ? C13 C14 C18 C20 100.5(9) . . . . ? C9 C14 C18 C19 157.3(7) . . . . ? C13 C14 C18 C19 -26.7(11) . . . . ? C21B O2 C21A C22A 8(2) . . . . ? C4 O2 C21A C22A 97.5(6) . . . . ? C21B O2 C21A C26A -174(3) . . . . ? C4 O2 C21A C26A -84.2(7) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 178.3(8) . . . . ? C26A C21A C22A C27A 178.1(9) . . . . ? O2 C21A C22A C27A -3.6(9) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -178.1(9) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 171.3(10) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -170.6(11) . . . . ? O2 C21A C26A C30 11.2(10) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -178.2(8) . . . . ? C4 O2 C21B C22B 95.0(7) . . . . ? C21A O2 C21B C22B -167(3) . . . . ? C4 O2 C21B C26B -86.9(6) . . . . ? C21A O2 C21B C26B 11(2) . . . . ? O2 C21B C22B C23B 178.1(8) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B -0.9(10) . . . . ? C26B C21B C22B C27B -179.0(9) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B 178.9(10) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -175.2(8) . . . . ? O2 C21B C26B C25B -178.2(8) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -2.9(7) . . . . ? C22B C21B C26B C30 175.3(8) . . . . ? C21A C22A C27A C29A -156.6(11) . . . . ? C23A C22A C27A C29A 21.5(15) . . . . ? C21A C22A C27A C28A 74.3(14) . . . . ? C23A C22A C27A C28A -107.6(13) . . . . ? C21B C22B C27B C28B 119.9(13) . . . . ? C23B C22B C27B C28B -59.1(17) . . . . ? C21B C22B C27B C29B -113.6(17) . . . . ? C23B C22B C27B C29B 67.4(18) . . . . ? C25A C26A C30 C32B -65.1(17) . . . . ? C21A C26A C30 C32B 105.9(16) . . . . ? C25A C26A C30 C31 76.0(9) . . . . ? C21A C26A C30 C31 -113.0(8) . . . . ? C25A C26A C30 C32A -36.3(12) . . . . ? C21A C26A C30 C32A 134.6(10) . . . . ? C25A C26A C30 C26B -120(3) . . . . ? C21A C26A C30 C26B 51(3) . . . . ? C25B C26B C30 C26A 59(3) . . . . ? C21B C26B C30 C26A -116(3) . . . . ? C25B C26B C30 C32B -74.0(14) . . . . ? C21B C26B C30 C32B 110.8(13) . . . . ? C25B C26B C30 C31 76.0(9) . . . . ? C21B C26B C30 C31 -99.3(8) . . . . ? C25B C26B C30 C32A -40.2(11) . . . . ? C21B C26B C30 C32A 144.6(10) . . . . ? N1 Co1 N1S C1S -43.7(11) . . . 16_655 ? N1 Co1 N1S C1S 136.3(11) 2_665 . . 16_655 ? N1 Co1 N1S C1S -133.7(11) 15_565 . . 16_655 ? N1 Co1 N1S C1S 46.3(11) 16_655 . . 16_655 ? N1 Co1 N1S C1S 46.3(11) . . . . ? N1 Co1 N1S C1S -133.7(11) 2_665 . . . ? N1 Co1 N1S C1S -43.7(11) 15_565 . . . ? N1 Co1 N1S C1S 136.3(11) 16_655 . . . ? N1 Co1 N1S C1S -133.7(11) . . . 2_665 ? N1 Co1 N1S C1S 46.3(11) 2_665 . . 2_665 ? N1 Co1 N1S C1S 136.3(11) 15_565 . . 2_665 ? N1 Co1 N1S C1S -43.7(11) 16_655 . . 2_665 ? N1 Co1 N1S C1S 136.3(11) . . . 15_565 ? N1 Co1 N1S C1S -43.7(11) 2_665 . . 15_565 ? N1 Co1 N1S C1S 46.3(11) 15_565 . . 15_565 ? N1 Co1 N1S C1S -133.7(11) 16_655 . . 15_565 ? C1S N1S C1S C2S -61.5(8) 16_655 . . . ? C1S N1S C1S C2S -0.5(5) 2_665 . . . ? C1S N1S C1S C2S 60.4(8) 15_565 . . . ? Co1 N1S C1S C2S 179.5(5) . . . . ? C1S N1S C1S C1S 61.0(7) 2_665 . . 16_655 ? C1S N1S C1S C1S 121.9(14) 15_565 . . 16_655 ? Co1 N1S C1S C1S -119.0(7) . . . 16_655 ? C1S N1S C1S C1S -121.9(14) 16_655 . . 15_565 ? C1S N1S C1S C1S -61.0(7) 2_665 . . 15_565 ? Co1 N1S C1S C1S 119.0(7) . . . 15_565 ? N1S C1S C2S C3S 1.1(9) . . . . ? C1S C1S C2S C3S -44.2(7) 16_655 . . . ? C1S C1S C2S C3S 45.8(6) 15_565 . . . ? N1S C1S C2S C2S -44.2(7) . . . 15_565 ? C1S C1S C2S C2S -89.5(4) 16_655 . . 15_565 ? C1S C1S C2S C2S 0.5(4) 15_565 . . 15_565 ? N1S C1S C2S C2S 45.8(7) . . . 16_655 ? C1S C1S C2S C2S 0.5(4) 16_655 . . 16_655 ? C1S C1S C2S C2S 90.5(4) 15_565 . . 16_655 ? C1S C2S C3S C2S -62(2) . . . 15_565 ? C2S C2S C3S C2S -124(4) 16_655 . . 15_565 ? C1S C2S C3S C2S 61(2) . . . 16_655 ? C2S C2S C3S C2S 124(4) 15_565 . . 16_655 ? C1S C2S C3S C2S -0.5(4) . . . 2_665 ? C2S C2S C3S C2S 62(2) 15_565 . . 2_665 ? C2S C2S C3S C2S -62(2) 16_655 . . 2_665 ? C1S C2S C3S C4S 179.5(4) . . . . ? C2S C2S C3S C4S -118(2) 15_565 . . . ? C2S C2S C3S C4S 118(2) 16_655 . . . ? C2S C3S C4S C5S -177(2) 15_565 . . 16_655 ? C2S C3S C4S C5S 3(2) 16_655 . . 16_655 ? C2S C3S C4S C5S -87(2) . . . 16_655 ? C2S C3S C4S C5S 93(2) 2_665 . . 16_655 ? C2S C3S C4S C5S 93(2) 15_565 . . 2_665 ? C2S C3S C4S C5S -87(2) 16_655 . . 2_665 ? C2S C3S C4S C5S -177(2) . . . 2_665 ? C2S C3S C4S C5S 3(2) 2_665 . . 2_665 ? C2S C3S C4S C5S -87(2) 15_565 . . . ? C2S C3S C4S C5S 93(2) 16_655 . . . ? C2S C3S C4S C5S 3(2) . . . . ? C2S C3S C4S C5S -177(2) 2_665 . . . ? C2S C3S C4S C5S 3(2) 15_565 . . 15_565 ? C2S C3S C4S C5S -177(2) 16_655 . . 15_565 ? C2S C3S C4S C5S 93(2) . . . 15_565 ? C2S C3S C4S C5S -87(2) 2_665 . . 15_565 ? C5S C4S C5S C6S -67(4) 16_655 . . . ? C5S C4S C5S C6S -3(3) 2_665 . . . ? C5S C4S C5S C6S 62(4) 15_565 . . . ? C3S C4S C5S C6S 177(3) . . . . ? C5S C4S C5S C5S 65(2) 2_665 . . 16_655 ? C5S C4S C5S C5S 130(5) 15_565 . . 16_655 ? C3S C4S C5S C5S -115(2) . . . 16_655 ? C5S C4S C5S C5S -130(5) 16_655 . . 15_565 ? C5S C4S C5S C5S -65(2) 2_665 . . 15_565 ? C3S C4S C5S C5S 115(2) . . . 15_565 ? C4S C5S C6S N2S 4(6) . . . . ? C5S C5S C6S N2S -42(4) 16_655 . . . ? C5S C5S C6S N2S 48(4) 15_565 . . . ? C4S C5S C6S C6S 49(5) . . . 16_655 ? C5S C5S C6S C6S 2(3) 16_655 . . 16_655 ? C5S C5S C6S C6S 92(3) 15_565 . . 16_655 ? C4S C5S C6S C6S -41(5) . . . 15_565 ? C5S C5S C6S C6S -88(3) 16_655 . . 15_565 ? C5S C5S C6S C6S 2(3) 15_565 . . 15_565 ? C5S C6S N2S C6S -74(4) . . . 15_565 ? C6S C6S N2S C6S -143(5) 16_655 . . 15_565 ? C5S C6S N2S C6S 69(4) . . . 16_655 ? C6S C6S N2S C6S 143(5) 15_565 . . 16_655 ? C5S C6S N2S C6S -2(3) . . . 2_665 ? C6S C6S N2S C6S -71(2) 16_655 . . 2_665 ? C6S C6S N2S C6S 71(2) 15_565 . . 2_665 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.19 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.696 _refine_diff_density_min -1.164 _refine_diff_density_rms 0.096 data_PNC[Co-vPic)] _database_code_depnum_ccdc_archive 'CCDC 900366' #TrackingRef '900366_PNC[Co-vPic)].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C147.33 H174.33 Cl10.08 Co N9 O11.33' _chemical_formula_weight 2669.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.5208(2) _cell_length_b 37.5208(2) _cell_length_c 37.5208(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52822.2(5) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9667 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 25.46 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.60 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.007 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 16925 _exptl_absorpt_coefficient_mu 0.300 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7742 _exptl_absorpt_correction_T_max 0.8406 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69050 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 191856 _diffrn_reflns_av_R_equivalents 0.1041 _diffrn_reflns_av_sigmaI/netI 0.0350 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 31 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 24.27 _reflns_number_total 7810 _reflns_number_gt 6722 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1161P)^2^+10.5542P] 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 7810 _refine_ls_number_parameters 433 _refine_ls_number_restraints 364 _refine_ls_R_factor_all 0.0676 _refine_ls_R_factor_gt 0.0611 _refine_ls_wR_factor_ref 0.1901 _refine_ls_wR_factor_gt 0.1842 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.129 _refine_ls_shift/su_max 0.011 _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 0.7500 0.7500 0.078173(14) 0.03992(18) Uani 1 4 d S . . O1 O 0.88834(3) 0.59611(4) 0.11059(4) 0.0572(4) Uani 1 1 d . A . O2 O 0.83106(4) 0.56048(3) 0.11110(4) 0.0590(4) Uani 1 1 d . . . N1S N 0.7500 0.7500 0.02018(10) 0.0579(9) Uani 1 4 d S . . N1 N 0.77816(4) 0.70712(4) 0.08178(4) 0.0422(4) Uani 1 1 d . A . N2 N 0.73162(4) 0.66219(4) 0.08506(4) 0.0450(4) Uani 1 1 d . A . C1 C 0.82552(5) 0.66805(5) 0.08898(5) 0.0451(4) Uani 1 1 d . . . C2 C 0.85857(5) 0.65207(5) 0.09581(5) 0.0480(4) Uani 1 1 d . A . H2 H 0.8800 0.6656 0.0957 0.058 Uiso 1 1 calc R . . C3 C 0.85876(5) 0.61615(5) 0.10259(6) 0.0493(5) Uani 1 1 d . . . C4 C 0.82682(5) 0.59583(5) 0.10235(6) 0.0511(5) Uani 1 1 d . A . C5 C 0.79443(5) 0.61148(5) 0.09487(6) 0.0507(5) Uani 1 1 d . . . H5 H 0.7731 0.5979 0.0941 0.061 Uiso 1 1 calc R A . C6 C 0.79439(5) 0.64814(5) 0.08841(5) 0.0464(4) Uani 1 1 d . A . C7 C 0.76520(5) 0.67292(5) 0.08433(5) 0.0438(4) Uani 1 1 d . . . C8 C 0.70498(5) 0.68548(5) 0.08461(5) 0.0433(4) Uani 1 1 d . . . C9 C 0.92121(5) 0.61367(6) 0.11408(7) 0.0615(6) Uani 1 1 d . . . C10 C 0.92955(6) 0.62805(6) 0.14752(8) 0.0720(7) Uani 1 1 d . A . C11 C 0.96344(8) 0.64241(8) 0.15138(10) 0.0916(10) Uani 1 1 d . . . H11 H 0.9704 0.6523 0.1737 0.110 Uiso 1 1 calc R A . C12 C 0.98680(8) 0.64258(9) 0.12380(13) 0.1094(14) Uani 1 1 d . A . H12 H 1.0098 0.6526 0.1271 0.131 Uiso 1 1 calc R . . C13 C 0.97790(7) 0.62852(10) 0.09097(12) 0.1070(13) Uani 1 1 d . . . H13 H 0.9947 0.6294 0.0720 0.128 Uiso 1 1 calc R A . C14 C 0.94390(6) 0.61270(7) 0.08517(8) 0.0778(8) Uani 1 1 d . A . C15 C 0.90340(8) 0.62611(7) 0.17789(8) 0.0786(7) Uani 1 1 d . . . H15 H 0.8793 0.6318 0.1681 0.094 Uiso 1 1 calc R A . C16 C 0.90182(9) 0.58853(8) 0.19330(9) 0.0853(8) Uani 1 1 d . A . H16A H 0.8962 0.5715 0.1743 0.128 Uiso 1 1 calc R . . H16B H 0.8833 0.5874 0.2117 0.128 Uiso 1 1 calc R . . H16C H 0.9249 0.5825 0.2039 0.128 Uiso 1 1 calc R . . C17 C 0.91076(13) 0.65204(9) 0.20873(11) 0.1227(14) Uani 1 1 d . A . H17A H 0.9334 0.6458 0.2202 0.184 Uiso 1 1 calc R . . H17B H 0.8914 0.6505 0.2262 0.184 Uiso 1 1 calc R . . H17C H 0.9122 0.6764 0.1995 0.184 Uiso 1 1 calc R . . C18 C 0.93305(9) 0.59448(10) 0.05109(9) 0.0992(10) Uani 1 1 d U . . H18 H 0.9071 0.5992 0.0474 0.119 Uiso 1 1 calc R A . C19 C 0.95258(17) 0.60761(17) 0.01814(14) 0.167(2) Uani 1 1 d U A . H19A H 0.9783 0.6076 0.0227 0.250 Uiso 1 1 calc R . . H19B H 0.9447 0.6319 0.0124 0.250 Uiso 1 1 calc R . . H19C H 0.9473 0.5918 -0.0020 0.250 Uiso 1 1 calc R . . C20 C 0.93787(13) 0.55403(11) 0.05431(13) 0.1296(14) Uani 1 1 d U A . H20A H 0.9631 0.5486 0.0583 0.194 Uiso 1 1 calc R . . H20B H 0.9298 0.5425 0.0323 0.194 Uiso 1 1 calc R . . H20C H 0.9238 0.5451 0.0744 0.194 Uiso 1 1 calc R . . C21A C 0.79969(15) 0.5398(2) 0.10956(18) 0.0529(13) Uani 0.520(6) 1 d PGU A 1 C22A C 0.79037(16) 0.51870(18) 0.08059(15) 0.0703(13) Uani 0.520(6) 1 d PGU A 1 C23A C 0.76021(15) 0.49724(13) 0.08225(15) 0.0788(16) Uani 0.520(6) 1 d PGU A 1 H23A H 0.7538 0.4828 0.0624 0.095 Uiso 0.520(6) 1 calc PR A 1 C24A C 0.73938(12) 0.49691(13) 0.11288(18) 0.0886(16) Uani 0.520(6) 1 d PGU A 1 H24A H 0.7188 0.4822 0.1140 0.106 Uiso 0.520(6) 1 calc PR A 1 C25A C 0.74870(14) 0.51803(16) 0.14186(16) 0.0830(15) Uani 0.520(6) 1 d PGU A 1 H25A H 0.7345 0.5178 0.1628 0.100 Uiso 0.520(6) 1 calc PR A 1 C26A C 0.77886(16) 0.53949(19) 0.14020(16) 0.0650(11) Uani 0.520(6) 1 d PGU A 1 C21B C 0.80284(17) 0.5397(2) 0.1074(2) 0.0603(15) Uani 0.480(6) 1 d PGU A 2 C22B C 0.80116(15) 0.52140(19) 0.07524(18) 0.0630(12) Uani 0.480(6) 1 d PGU A 2 C23B C 0.77178(16) 0.50020(14) 0.06752(15) 0.0798(16) Uani 0.480(6) 1 d PGU A 2 H23B H 0.7706 0.4877 0.0455 0.096 Uiso 0.480(6) 1 calc PR A 2 C24B C 0.74408(12) 0.49733(14) 0.09194(19) 0.0853(17) Uani 0.480(6) 1 d PGU A 2 H24B H 0.7240 0.4828 0.0867 0.102 Uiso 0.480(6) 1 calc PR A 2 C25B C 0.74575(15) 0.51566(19) 0.12409(17) 0.0800(15) Uani 0.480(6) 1 d PGU A 2 H25B H 0.7268 0.5137 0.1408 0.096 Uiso 0.480(6) 1 calc PR A 2 C26B C 0.7751(2) 0.5369(2) 0.13182(17) 0.0751(14) Uani 0.480(6) 1 d PGDU A 2 C27A C 0.8152(2) 0.5211(2) 0.0478(2) 0.0763(15) Uani 0.520(6) 1 d PU A 1 H27A H 0.8224 0.5467 0.0464 0.092 Uiso 0.520(6) 1 calc PR A 1 C28A C 0.8507(2) 0.5002(2) 0.0516(2) 0.090(2) Uani 0.520(6) 1 d PU A 1 H28D H 0.8604 0.4951 0.0279 0.135 Uiso 0.520(6) 1 calc PR A 1 H28E H 0.8462 0.4777 0.0642 0.135 Uiso 0.520(6) 1 calc PR A 1 H28F H 0.8678 0.5145 0.0652 0.135 Uiso 0.520(6) 1 calc PR A 1 C29A C 0.7985(3) 0.5129(3) 0.0118(2) 0.135(3) Uani 0.520(6) 1 d PU A 1 H29A H 0.7886 0.5348 0.0016 0.202 Uiso 0.520(6) 1 calc PR A 1 H29B H 0.7795 0.4953 0.0148 0.202 Uiso 0.520(6) 1 calc PR A 1 H29C H 0.8168 0.5034 -0.0043 0.202 Uiso 0.520(6) 1 calc PR A 1 C27B C 0.8313(2) 0.5246(2) 0.0479(3) 0.0817(18) Uani 0.480(6) 1 d PU A 2 H27B H 0.8508 0.5372 0.0608 0.098 Uiso 0.480(6) 1 calc PR A 2 C28B C 0.8463(3) 0.4881(3) 0.0396(3) 0.111(3) Uani 0.480(6) 1 d PU A 2 H28A H 0.8675 0.4906 0.0245 0.167 Uiso 0.480(6) 1 calc PR A 2 H28B H 0.8283 0.4739 0.0271 0.167 Uiso 0.480(6) 1 calc PR A 2 H28C H 0.8529 0.4761 0.0619 0.167 Uiso 0.480(6) 1 calc PR A 2 C29B C 0.8230(3) 0.5472(3) 0.0180(3) 0.140(3) Uani 0.480(6) 1 d PU A 2 H29D H 0.8102 0.5683 0.0263 0.209 Uiso 0.480(6) 1 calc PR A 2 H29E H 0.8081 0.5340 0.0010 0.209 Uiso 0.480(6) 1 calc PR A 2 H29F H 0.8452 0.5545 0.0063 0.209 Uiso 0.480(6) 1 calc PR A 2 C30 C 0.78358(10) 0.55963(8) 0.16995(9) 0.0972(9) Uani 1 1 d DU . . H30 H 0.7997 0.5804 0.1657 0.117 Uiso 1 1 calc R A 1 C31 C 0.79565(12) 0.53684(11) 0.20099(12) 0.1225(13) Uani 1 1 d U A . H31A H 0.7799 0.5161 0.2032 0.184 Uiso 1 1 calc R . . H31B H 0.7948 0.5509 0.2230 0.184 Uiso 1 1 calc R . . H31C H 0.8201 0.5287 0.1968 0.184 Uiso 1 1 calc R . . C32A C 0.7422(3) 0.5720(4) 0.1800(3) 0.120(3) Uani 0.502(15) 1 d PU A 1 H32A H 0.7261 0.5516 0.1772 0.179 Uiso 0.502(15) 1 calc PR A 1 H32B H 0.7347 0.5912 0.1639 0.179 Uiso 0.502(15) 1 calc PR A 1 H32C H 0.7414 0.5805 0.2047 0.179 Uiso 0.502(15) 1 calc PR A 1 C32B C 0.7629(4) 0.5912(3) 0.1818(3) 0.113(3) Uani 0.498(15) 1 d PU A 2 H32D H 0.7635 0.6095 0.1632 0.170 Uiso 0.498(15) 1 calc PR A 2 H32E H 0.7733 0.6008 0.2038 0.170 Uiso 0.498(15) 1 calc PR A 2 H32F H 0.7381 0.5842 0.1863 0.170 Uiso 0.498(15) 1 calc PR A 2 Cl1S Cl 0.7500 0.7500 0.7500 0.097(2) Uani 0.50 24 d SP . . C1S C 0.77912(19) 0.7443(3) 0.00166(19) 0.123(2) Uani 0.50 1 d PU . . C2S C 0.7800(3) 0.7425(4) -0.0347(2) 0.156(3) Uani 0.50 1 d PU . . C3S C 0.7500 0.7500 -0.0551(2) 0.155(3) Uani 1 4 d SU . . C4S C 0.7500 0.7500 -0.0957(3) 0.222(6) Uani 1 4 d SU . . 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 0.0313(2) 0.0313(2) 0.0571(3) 0.000 0.000 0.000 O1 0.0378(7) 0.0437(7) 0.0901(11) 0.0061(7) -0.0116(7) 0.0058(5) O2 0.0429(7) 0.0349(7) 0.0994(11) 0.0070(7) -0.0105(7) 0.0033(5) N1S 0.0546(12) 0.0546(12) 0.064(2) 0.000 0.000 0.000 N1 0.0344(7) 0.0341(7) 0.0581(9) -0.0022(6) -0.0017(6) -0.0003(6) N2 0.0356(8) 0.0352(7) 0.0643(10) 0.0021(6) -0.0037(7) 0.0003(6) C1 0.0374(9) 0.0372(9) 0.0608(11) -0.0014(8) -0.0047(8) 0.0007(7) C2 0.0373(9) 0.0418(9) 0.0648(12) -0.0018(8) -0.0058(8) 0.0005(7) C3 0.0378(9) 0.0432(10) 0.0671(12) 0.0013(8) -0.0078(8) 0.0048(7) C4 0.0450(10) 0.0362(9) 0.0722(13) 0.0035(8) -0.0080(9) 0.0043(8) C5 0.0384(9) 0.0353(9) 0.0783(13) 0.0022(9) -0.0080(9) 0.0004(7) C6 0.0381(9) 0.0372(9) 0.0640(11) -0.0014(8) -0.0057(8) 0.0017(7) C7 0.0369(9) 0.0344(9) 0.0602(11) 0.0000(7) -0.0059(8) 0.0001(7) C8 0.0361(9) 0.0353(8) 0.0586(11) 0.0031(7) -0.0019(7) -0.0011(7) C9 0.0376(10) 0.0511(11) 0.0959(17) 0.0173(11) -0.0132(10) 0.0033(8) C10 0.0604(13) 0.0522(12) 0.1035(19) 0.0173(12) -0.0318(13) -0.0019(10) C11 0.0653(16) 0.0773(17) 0.132(3) 0.0338(18) -0.0419(18) -0.0146(13) C12 0.0590(17) 0.099(2) 0.170(4) 0.058(2) -0.044(2) -0.0168(15) C13 0.0488(14) 0.125(3) 0.147(3) 0.069(3) 0.0062(17) 0.0057(15) C14 0.0500(12) 0.0813(17) 0.102(2) 0.0329(15) -0.0030(13) 0.0121(11) C15 0.0835(17) 0.0661(15) 0.0863(18) 0.0002(13) -0.0221(14) 0.0063(13) C16 0.0876(19) 0.0765(17) 0.092(2) 0.0106(15) -0.0045(16) -0.0008(14) C17 0.174(4) 0.080(2) 0.114(3) -0.0149(19) -0.041(3) 0.006(2) C18 0.088(2) 0.110(2) 0.100(2) 0.0247(19) 0.0139(17) 0.0231(18) C19 0.184(5) 0.193(5) 0.124(4) 0.025(3) 0.039(3) -0.015(4) C20 0.139(3) 0.110(2) 0.140(3) -0.007(2) -0.005(3) 0.034(2) C21A 0.038(2) 0.030(3) 0.090(3) 0.004(2) -0.011(2) -0.001(2) C22A 0.062(3) 0.049(2) 0.100(3) 0.000(2) -0.018(2) -0.003(2) C23A 0.072(4) 0.050(2) 0.114(4) -0.004(3) -0.019(3) -0.016(2) C24A 0.072(3) 0.057(3) 0.136(4) 0.013(3) -0.004(3) -0.013(2) C25A 0.064(3) 0.057(3) 0.128(4) 0.018(3) 0.011(3) -0.001(2) C26A 0.047(2) 0.038(2) 0.110(3) 0.011(2) 0.007(2) 0.0040(18) C21B 0.053(3) 0.036(3) 0.092(3) -0.001(3) -0.008(2) 0.011(3) C22B 0.053(3) 0.039(2) 0.097(3) -0.001(2) -0.012(2) -0.002(2) C23B 0.076(4) 0.049(3) 0.114(4) -0.005(3) -0.013(3) -0.017(2) C24B 0.074(3) 0.059(3) 0.124(4) 0.014(3) -0.002(3) -0.022(3) C25B 0.061(3) 0.056(3) 0.122(4) 0.020(3) 0.008(3) -0.001(2) C26B 0.063(3) 0.046(3) 0.117(3) 0.007(2) 0.006(2) 0.008(2) C27A 0.078(4) 0.062(3) 0.089(3) -0.006(2) -0.015(3) 0.000(3) C28A 0.102(4) 0.081(5) 0.086(5) -0.001(3) -0.002(3) 0.019(4) C29A 0.141(6) 0.163(7) 0.099(4) -0.018(5) -0.041(4) 0.014(5) C27B 0.084(4) 0.066(3) 0.096(3) -0.006(3) 0.010(4) 0.005(4) C28B 0.141(7) 0.092(6) 0.101(7) -0.023(4) -0.005(5) 0.040(5) C29B 0.170(7) 0.122(6) 0.126(5) 0.031(5) 0.020(5) 0.038(5) C30 0.121(2) 0.0665(15) 0.1040(19) 0.0031(13) 0.0298(17) 0.0242(15) C31 0.130(3) 0.105(3) 0.133(3) 0.019(2) -0.003(2) 0.038(2) C32A 0.112(5) 0.105(7) 0.142(6) -0.020(5) 0.012(5) 0.044(5) C32B 0.134(8) 0.086(5) 0.121(5) -0.010(4) 0.013(5) 0.039(5) Cl1S 0.097(2) 0.097(2) 0.097(2) 0.000 0.000 0.000 C1S 0.088(4) 0.207(7) 0.075(3) -0.004(5) 0.023(3) 0.027(5) C2S 0.147(6) 0.234(7) 0.085(3) -0.002(5) 0.024(3) 0.028(6) C3S 0.195(5) 0.195(5) 0.074(4) 0.000 0.000 0.000 C4S 0.294(9) 0.294(9) 0.079(4) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.9297(14) 16_655 ? Co1 N1 1.9297(14) 15_565 ? Co1 N1 1.9297(14) . ? Co1 N1 1.9297(14) 2_665 ? Co1 N1S 2.176(4) . ? O1 C3 1.374(2) . ? O1 C9 1.404(2) . ? O2 C21B 1.322(4) . ? O2 C4 1.376(2) . ? O2 C21A 1.411(3) . ? N1S C1S 1.312(7) . ? N1S C1S 1.312(7) 15_565 ? N1S C1S 1.312(7) 16_655 ? N1S C1S 1.312(7) 2_665 ? N1 C8 1.371(2) 16_655 ? N1 C7 1.375(2) . ? N2 C7 1.323(2) . ? N2 C8 1.328(2) . ? C1 C6 1.387(2) . ? C1 C2 1.401(3) . ? C1 C8 1.455(2) 16_655 ? C2 C3 1.372(3) . ? C2 H2 0.9500 . ? C3 C4 1.420(3) . ? C4 C5 1.378(3) . ? C5 C6 1.397(3) . ? C5 H5 0.9500 . ? C6 C7 1.445(2) . ? C8 N1 1.371(2) 15_565 ? C8 C1 1.455(2) 15_565 ? C9 C14 1.379(4) . ? C9 C10 1.401(4) . ? C10 C11 1.389(4) . ? C10 C15 1.505(4) . ? C11 C12 1.356(5) . ? C11 H11 0.9500 . ? C12 C13 1.381(6) . ? C12 H12 0.9500 . ? C13 C14 1.424(4) . ? C13 H13 0.9500 . ? C14 C18 1.506(5) . ? C15 C16 1.525(4) . ? C15 C17 1.537(4) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.519(5) . ? C18 C20 1.533(5) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.546(9) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.360(6) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.531(8) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.696(6) . ? C27A C29A 1.521(10) . ? C27A C28A 1.551(11) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.439(13) . ? C27B C28B 1.513(12) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C32B 1.486(7) . ? C30 C31 1.514(5) . ? C30 C32A 1.664(9) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C1S C2S 1.366(11) . ? C1S C1S 1.574(10) 15_565 ? C1S C1S 1.574(10) 16_655 ? C2S C3S 1.392(10) . ? C2S C2S 1.643(14) 15_565 ? C2S C2S 1.643(14) 16_655 ? C3S C2S 1.392(10) 16_655 ? C3S C2S 1.392(10) 15_565 ? C3S C2S 1.392(10) 2_665 ? C3S C4S 1.524(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 171.96(10) 16_655 15_565 ? N1 Co1 N1 89.719(7) 16_655 . ? N1 Co1 N1 89.719(7) 15_565 . ? N1 Co1 N1 89.719(7) 16_655 2_665 ? N1 Co1 N1 89.719(7) 15_565 2_665 ? N1 Co1 N1 171.96(10) . 2_665 ? N1 Co1 N1S 94.02(5) 16_655 . ? N1 Co1 N1S 94.02(5) 15_565 . ? N1 Co1 N1S 94.02(5) . . ? N1 Co1 N1S 94.02(5) 2_665 . ? C3 O1 C9 118.24(15) . . ? C21B O2 C4 116.7(5) . . ? C21B O2 C21A 4.7(6) . . ? C4 O2 C21A 115.0(4) . . ? C1S N1S C1S 73.7(4) . 15_565 ? C1S N1S C1S 73.7(4) . 16_655 ? C1S N1S C1S 116.1(8) 15_565 16_655 ? C1S N1S C1S 116.1(8) . 2_665 ? C1S N1S C1S 73.7(4) 15_565 2_665 ? C1S N1S C1S 73.7(4) 16_655 2_665 ? C1S N1S Co1 122.0(4) . . ? C1S N1S Co1 122.0(4) 15_565 . ? C1S N1S Co1 122.0(4) 16_655 . ? C1S N1S Co1 122.0(4) 2_665 . ? C8 N1 C7 106.96(14) 16_655 . ? C8 N1 Co1 126.81(12) 16_655 . ? C7 N1 Co1 126.10(12) . . ? C7 N2 C8 121.08(15) . . ? C6 C1 C2 121.19(17) . . ? C6 C1 C8 105.81(15) . 16_655 ? C2 C1 C8 132.78(16) . 16_655 ? C3 C2 C1 117.32(17) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? C2 C3 O1 125.61(17) . . ? C2 C3 C4 121.47(17) . . ? O1 C3 C4 112.92(16) . . ? O2 C4 C5 124.16(17) . . ? O2 C4 C3 114.72(16) . . ? C5 C4 C3 121.09(17) . . ? C4 C5 C6 117.12(17) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? C1 C6 C5 121.80(17) . . ? C1 C6 C7 107.06(15) . . ? C5 C6 C7 130.77(17) . . ? N2 C7 N1 128.45(16) . . ? N2 C7 C6 121.59(16) . . ? N1 C7 C6 109.87(15) . . ? N2 C8 N1 127.74(16) . 15_565 ? N2 C8 C1 121.92(15) . 15_565 ? N1 C8 C1 110.29(15) 15_565 15_565 ? C14 C9 C10 125.2(2) . . ? C14 C9 O1 117.1(2) . . ? C10 C9 O1 117.4(2) . . ? C11 C10 C9 116.6(3) . . ? C11 C10 C15 122.5(3) . . ? C9 C10 C15 120.9(2) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 121.5(3) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 120.8(3) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 114.9(3) . . ? C9 C14 C18 120.9(2) . . ? C13 C14 C18 124.1(3) . . ? C10 C15 C16 110.9(2) . . ? C10 C15 C17 115.0(3) . . ? C16 C15 C17 107.9(3) . . ? C10 C15 H15 107.6 . . ? C16 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 114.4(4) . . ? C14 C18 C20 110.5(3) . . ? C19 C18 C20 109.2(4) . . ? C14 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 123.7(4) . . ? C26A C21A O2 116.1(4) . . ? C23A C22A C21A 120.0 . . ? C23A C22A C27A 124.1(4) . . ? C21A C22A C27A 115.9(4) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 113.0(4) . . ? C30 C26A C21A 126.9(4) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 114.8(5) . . ? O2 C21B C26B 125.1(5) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 119.3(5) . . ? C21B C22B C27B 120.7(5) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 127.8(4) . . ? C21B C26B C30 112.2(4) . . ? C29A C27A C22A 116.6(6) . . ? C29A C27A C28A 109.4(7) . . ? C22A C27A C28A 114.5(6) . . ? C29A C27A H27A 105.0 . . ? C22A C27A H27A 105.0 . . ? C28A C27A H27A 105.0 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 116.9(8) . . ? C29B C27B C22B 114.2(8) . . ? C28B C27B C22B 110.0(8) . . ? C29B C27B H27B 104.8 . . ? C28B C27B H27B 104.8 . . ? C22B C27B H27B 104.8 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C32B 128.4(6) . . ? C26A C30 C31 110.9(4) . . ? C32B C30 C31 112.2(5) . . ? C26A C30 C32A 102.7(6) . . ? C32B C30 C32A 38.9(4) . . ? C31 C30 C32A 105.2(5) . . ? C26A C30 C26B 4.6(7) . . ? C32B C30 C26B 123.8(6) . . ? C31 C30 C26B 114.9(4) . . ? C32A C30 C26B 99.0(6) . . ? C26A C30 H30 112.5 . . ? C32B C30 H30 75.0 . . ? C31 C30 H30 112.5 . . ? C32A C30 H30 112.5 . . ? C26B C30 H30 111.8 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N1S C1S C2S 123.9(8) . . ? N1S C1S C1S 53.14(18) . 15_565 ? C2S C1S C1S 89.6(8) . 15_565 ? N1S C1S C1S 53.14(18) . 16_655 ? C2S C1S C1S 93.2(7) . 16_655 ? C1S C1S C1S 90.000(2) 15_565 16_655 ? C1S C2S C3S 121.3(8) . . ? C1S C2S C2S 90.2(7) . 15_565 ? C3S C2S C2S 53.8(2) . 15_565 ? C1S C2S C2S 86.8(7) . 16_655 ? C3S C2S C2S 53.8(2) . 16_655 ? C2S C2S C2S 90.000(2) 15_565 16_655 ? C2S C3S C2S 113.2(10) 16_655 15_565 ? C2S C3S C2S 72.4(5) 16_655 . ? C2S C3S C2S 72.4(5) 15_565 . ? C2S C3S C2S 72.4(5) 16_655 2_665 ? C2S C3S C2S 72.4(5) 15_565 2_665 ? C2S C3S C2S 113.2(10) . 2_665 ? C2S C3S C4S 123.4(5) 16_655 . ? C2S C3S C4S 123.4(5) 15_565 . ? C2S C3S C4S 123.4(5) . . ? C2S C3S C4S 123.4(5) 2_665 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1S C1S 44.4(7) 16_655 . . . ? N1 Co1 N1S C1S -135.6(7) 15_565 . . . ? N1 Co1 N1S C1S -45.6(7) . . . . ? N1 Co1 N1S C1S 134.4(7) 2_665 . . . ? N1 Co1 N1S C1S 134.4(7) 16_655 . . 15_565 ? N1 Co1 N1S C1S -45.6(7) 15_565 . . 15_565 ? N1 Co1 N1S C1S 44.4(7) . . . 15_565 ? N1 Co1 N1S C1S -135.6(7) 2_665 . . 15_565 ? N1 Co1 N1S C1S -45.6(7) 16_655 . . 16_655 ? N1 Co1 N1S C1S 134.4(7) 15_565 . . 16_655 ? N1 Co1 N1S C1S -135.6(7) . . . 16_655 ? N1 Co1 N1S C1S 44.4(7) 2_665 . . 16_655 ? N1 Co1 N1S C1S -135.6(7) 16_655 . . 2_665 ? N1 Co1 N1S C1S 44.4(7) 15_565 . . 2_665 ? N1 Co1 N1S C1S 134.4(7) . . . 2_665 ? N1 Co1 N1S C1S -45.6(7) 2_665 . . 2_665 ? N1 Co1 N1 C8 -1.46(19) 16_655 . . 16_655 ? N1 Co1 N1 C8 -173.44(12) 15_565 . . 16_655 ? N1 Co1 N1 C8 -87.45(16) 2_665 . . 16_655 ? N1S Co1 N1 C8 92.55(15) . . . 16_655 ? N1 Co1 N1 C7 173.98(12) 16_655 . . . ? N1 Co1 N1 C7 1.99(19) 15_565 . . . ? N1 Co1 N1 C7 87.99(16) 2_665 . . . ? N1S Co1 N1 C7 -92.01(15) . . . . ? C6 C1 C2 C3 -1.3(3) . . . . ? C8 C1 C2 C3 172.4(2) 16_655 . . . ? C1 C2 C3 O1 -178.5(2) . . . . ? C1 C2 C3 C4 0.6(3) . . . . ? C9 O1 C3 C2 3.5(3) . . . . ? C9 O1 C3 C4 -175.6(2) . . . . ? C21B O2 C4 C5 9.2(5) . . . . ? C21A O2 C4 C5 4.3(4) . . . . ? C21B O2 C4 C3 -172.7(4) . . . . ? C21A O2 C4 C3 -177.6(3) . . . . ? C2 C3 C4 O2 -177.39(19) . . . . ? O1 C3 C4 O2 1.8(3) . . . . ? C2 C3 C4 C5 0.8(3) . . . . ? O1 C3 C4 C5 180.0(2) . . . . ? O2 C4 C5 C6 176.5(2) . . . . ? C3 C4 C5 C6 -1.5(3) . . . . ? C2 C1 C6 C5 0.5(3) . . . . ? C8 C1 C6 C5 -174.63(19) 16_655 . . . ? C2 C1 C6 C7 174.29(19) . . . . ? C8 C1 C6 C7 -0.9(2) 16_655 . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C4 C5 C6 C7 -171.3(2) . . . . ? C8 N2 C7 N1 -2.6(3) . . . . ? C8 N2 C7 C6 173.69(18) . . . . ? C8 N1 C7 N2 175.77(19) 16_655 . . . ? Co1 N1 C7 N2 -0.4(3) . . . . ? C8 N1 C7 C6 -0.9(2) 16_655 . . . ? Co1 N1 C7 C6 -177.04(13) . . . . ? C1 C6 C7 N2 -175.78(18) . . . . ? C5 C6 C7 N2 -2.8(3) . . . . ? C1 C6 C7 N1 1.1(2) . . . . ? C5 C6 C7 N1 174.1(2) . . . . ? C7 N2 C8 N1 3.2(3) . . . 15_565 ? C7 N2 C8 C1 -173.75(18) . . . 15_565 ? C3 O1 C9 C14 -99.2(2) . . . . ? C3 O1 C9 C10 86.2(2) . . . . ? C14 C9 C10 C11 0.1(3) . . . . ? O1 C9 C10 C11 174.28(19) . . . . ? C14 C9 C10 C15 -176.9(2) . . . . ? O1 C9 C10 C15 -2.8(3) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C15 C10 C11 C12 177.6(3) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C11 C12 C13 C14 -1.2(5) . . . . ? C10 C9 C14 C13 -1.3(3) . . . . ? O1 C9 C14 C13 -175.4(2) . . . . ? C10 C9 C14 C18 176.0(2) . . . . ? O1 C9 C14 C18 1.9(3) . . . . ? C12 C13 C14 C9 1.8(4) . . . . ? C12 C13 C14 C18 -175.4(3) . . . . ? C11 C10 C15 C16 -102.0(3) . . . . ? C9 C10 C15 C16 74.9(3) . . . . ? C11 C10 C15 C17 20.8(4) . . . . ? C9 C10 C15 C17 -162.4(2) . . . . ? C9 C14 C18 C19 156.5(3) . . . . ? C13 C14 C18 C19 -26.4(5) . . . . ? C9 C14 C18 C20 -79.8(3) . . . . ? C13 C14 C18 C20 97.3(4) . . . . ? C21B O2 C21A C22A -14(10) . . . . ? C4 O2 C21A C22A 97.5(5) . . . . ? C21B O2 C21A C26A 161(11) . . . . ? C4 O2 C21A C26A -86.8(4) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 175.5(7) . . . . ? C26A C21A C22A C27A 179.8(6) . . . . ? O2 C21A C22A C27A -4.7(6) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -179.8(7) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 177.4(6) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -177.0(7) . . . . ? O2 C21A C26A C30 7.2(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -175.8(7) . . . . ? C4 O2 C21B C22B 95.4(5) . . . . ? C21A O2 C21B C22B 166(11) . . . . ? C4 O2 C21B C26B -81.1(6) . . . . ? C21A O2 C21B C26B -11(10) . . . . ? O2 C21B C22B C23B -176.7(8) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 2.7(7) . . . . ? C26B C21B C22B C27B 179.4(7) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -179.4(7) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -176.6(8) . . . . ? O2 C21B C26B C25B 176.3(9) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -6.6(6) . . . . ? C22B C21B C26B C30 177.1(7) . . . . ? C23A C22A C27A C29A 26.6(10) . . . . ? C21A C22A C27A C29A -153.2(6) . . . . ? C23A C22A C27A C28A -102.9(7) . . . . ? C21A C22A C27A C28A 77.3(7) . . . . ? C23B C22B C27B C29B 75.7(9) . . . . ? C21B C22B C27B C29B -103.7(9) . . . . ? C23B C22B C27B C28B -58.2(10) . . . . ? C21B C22B C27B C28B 122.5(8) . . . . ? C25A C26A C30 C32B -72.3(9) . . . . ? C21A C26A C30 C32B 104.9(9) . . . . ? C25A C26A C30 C31 72.6(5) . . . . ? C21A C26A C30 C31 -110.3(5) . . . . ? C25A C26A C30 C32A -39.4(7) . . . . ? C21A C26A C30 C32A 137.8(6) . . . . ? C25A C26A C30 C26B -77(6) . . . . ? C21A C26A C30 C26B 100(6) . . . . ? C25B C26B C30 C26A 106(7) . . . . ? C21B C26B C30 C26A -71(6) . . . . ? C25B C26B C30 C32B -68.9(10) . . . . ? C21B C26B C30 C32B 114.3(8) . . . . ? C25B C26B C30 C31 75.2(7) . . . . ? C21B C26B C30 C31 -101.6(4) . . . . ? C25B C26B C30 C32A -36.3(8) . . . . ? C21B C26B C30 C32A 146.9(6) . . . . ? C1S N1S C1S C2S 59.0(11) 15_565 . . . ? C1S N1S C1S C2S -65.2(11) 16_655 . . . ? C1S N1S C1S C2S -3.1(11) 2_665 . . . ? Co1 N1S C1S C2S 176.9(11) . . . . ? C1S N1S C1S C1S -124.2(5) 16_655 . . 15_565 ? C1S N1S C1S C1S -62.1(2) 2_665 . . 15_565 ? Co1 N1S C1S C1S 117.9(2) . . . 15_565 ? C1S N1S C1S C1S 124.2(5) 15_565 . . 16_655 ? C1S N1S C1S C1S 62.1(2) 2_665 . . 16_655 ? Co1 N1S C1S C1S -117.9(2) . . . 16_655 ? N1S C1S C2S C3S 6(2) . . . . ? C1S C1S C2S C3S 49.5(16) 15_565 . . . ? C1S C1S C2S C3S -40.5(16) 16_655 . . . ? N1S C1S C2S C2S -40.3(17) . . . 15_565 ? C1S C1S C2S C2S 3.0(11) 15_565 . . 15_565 ? C1S C1S C2S C2S -87.0(11) 16_655 . . 15_565 ? N1S C1S C2S C2S 49.7(17) . . . 16_655 ? C1S C1S C2S C2S 93.0(10) 15_565 . . 16_655 ? C1S C1S C2S C2S 3.0(11) 16_655 . . 16_655 ? C1S C2S C3S C2S 58.3(11) . . . 16_655 ? C2S C2S C3S C2S 122.3(6) 15_565 . . 16_655 ? C1S C2S C3S C2S -64.0(11) . . . 15_565 ? C2S C2S C3S C2S -122.3(6) 16_655 . . 15_565 ? C1S C2S C3S C2S -2.9(10) . . . 2_665 ? C2S C2S C3S C2S 61.2(3) 15_565 . . 2_665 ? C2S C2S C3S C2S -61.2(3) 16_655 . . 2_665 ? C1S C2S C3S C4S 177.1(10) . . . . ? C2S C2S C3S C4S -118.8(3) 15_565 . . . ? C2S C2S C3S C4S 118.8(3) 16_655 . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.695 _refine_diff_density_min -0.631 _refine_diff_density_rms 0.046 data_copcpicsq _database_code_depnum_ccdc_archive 'CCDC 900367' #TrackingRef '900367_PNC[Co-vPic0.60Py0.40].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C136.33 H155.33 Cl0.17 Co N9 O13.33' _chemical_formula_weight 2198.20 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.1172(4) _cell_length_b 37.1172(4) _cell_length_c 37.1172(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 51135.9(10) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5226 _cell_measurement_theta_min 1.79 _cell_measurement_theta_max 23.53 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.857 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14074 _exptl_absorpt_coefficient_mu 0.150 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9634 _exptl_absorpt_correction_T_max 0.9706 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.67090 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 269869 _diffrn_reflns_av_R_equivalents 0.0843 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 23.53 _reflns_number_total 7520 _reflns_number_gt 5226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7520 _refine_ls_number_parameters 325 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.1838 _refine_ls_R_factor_gt 0.1444 _refine_ls_wR_factor_ref 0.4396 _refine_ls_wR_factor_gt 0.4132 _refine_ls_goodness_of_fit_ref 1.651 _refine_ls_restrained_S_all 1.743 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_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 0.7500 0.7500 0.07537(4) 0.0886(6) Uani 1 4 d S . . O1 O 0.88918(10) 0.59480(9) 0.10889(12) 0.1077(12) Uani 1 1 d . A . O2 O 0.83140(9) 0.55915(9) 0.10907(13) 0.1182(14) Uani 1 1 d . . . O3 O 0.7500 0.7500 0.1375(8) 0.173(8) Uiso 0.50 4 d SP . . N1S N 0.7500 0.7500 0.0186(3) 0.103(3) Uani 1 4 d SD . . N1 N 0.77845(10) 0.70646(10) 0.07903(13) 0.0891(12) Uani 1 1 d . A . N2 N 0.73114(10) 0.66119(10) 0.08161(13) 0.0931(12) Uani 1 1 d . A . C1 C 0.82592(13) 0.66702(12) 0.08594(16) 0.0926(14) Uani 1 1 d U . . C2 C 0.85926(13) 0.65064(13) 0.09349(15) 0.0943(14) Uani 1 1 d U A . H2 H 0.8810 0.6641 0.0932 0.113 Uiso 1 1 calc R . . C3 C 0.85916(13) 0.61513(14) 0.10122(16) 0.0980(15) Uani 1 1 d U . . C4 C 0.82715(14) 0.59476(13) 0.09973(17) 0.1001(16) Uani 1 1 d U A . C5 C 0.79460(14) 0.61055(13) 0.09185(17) 0.1034(16) Uani 1 1 d U . . H5 H 0.7731 0.5968 0.0907 0.124 Uiso 1 1 calc R A . C6 C 0.79438(13) 0.64740(13) 0.08560(16) 0.0956(14) Uani 1 1 d U A . C7 C 0.76528(14) 0.67245(12) 0.08140(15) 0.0897(14) Uani 1 1 d U . . C8 C 0.70463(12) 0.68512(13) 0.08112(15) 0.0907(14) Uani 1 1 d . . . C9 C 0.92220(14) 0.61214(17) 0.1114(2) 0.1113(15) Uani 1 1 d U . . C10 C 0.93082(16) 0.62676(18) 0.1452(2) 0.1248(17) Uani 1 1 d U A . C11 C 0.96513(19) 0.6414(2) 0.1494(3) 0.155(2) Uani 1 1 d U . . H11 H 0.9718 0.6520 0.1717 0.186 Uiso 1 1 calc R A . C12 C 0.9886(2) 0.6407(3) 0.1222(3) 0.182(3) Uani 1 1 d U A . H12 H 1.0121 0.6505 0.1256 0.219 Uiso 1 1 calc R . . C13 C 0.9796(2) 0.6260(3) 0.0886(3) 0.178(3) Uani 1 1 d U . . H13 H 0.9967 0.6258 0.0696 0.213 Uiso 1 1 calc R A . C14 C 0.9451(2) 0.6114(2) 0.0833(2) 0.147(2) Uani 1 1 d U A . C15 C 0.9035(2) 0.62619(17) 0.17658(19) 0.1288(18) Uani 1 1 d U . . H15 H 0.8792 0.6319 0.1665 0.155 Uiso 1 1 calc R A . C16 C 0.9020(2) 0.58902(19) 0.1922(2) 0.135(2) Uani 1 1 d U A . H16A H 0.8951 0.5718 0.1734 0.202 Uiso 1 1 calc R . . H16B H 0.8841 0.5884 0.2116 0.202 Uiso 1 1 calc R . . H16C H 0.9257 0.5826 0.2019 0.202 Uiso 1 1 calc R . . C17 C 0.9118(3) 0.6541(2) 0.2069(3) 0.191(4) Uani 1 1 d U A . H17A H 0.9295 0.6439 0.2237 0.287 Uiso 1 1 calc R . . H17B H 0.8896 0.6598 0.2200 0.287 Uiso 1 1 calc R . . H17C H 0.9216 0.6761 0.1962 0.287 Uiso 1 1 calc R . . C18 C 0.9353(3) 0.5949(3) 0.0492(3) 0.179(3) Uani 1 1 d U . . H18 H 0.9085 0.5971 0.0488 0.215 Uiso 1 1 calc R A . C19 C 0.9458(6) 0.6099(5) 0.0147(4) 0.309(9) Uani 1 1 d U A . H19A H 0.9450 0.5910 -0.0037 0.464 Uiso 1 1 calc R . . H19B H 0.9703 0.6196 0.0164 0.464 Uiso 1 1 calc R . . H19C H 0.9292 0.6293 0.0081 0.464 Uiso 1 1 calc R . . C20 C 0.9412(3) 0.5549(3) 0.0482(4) 0.239(5) Uani 1 1 d U A . H20A H 0.9647 0.5492 0.0589 0.358 Uiso 1 1 calc R . . H20B H 0.9407 0.5465 0.0232 0.358 Uiso 1 1 calc R . . H20C H 0.9221 0.5429 0.0620 0.358 Uiso 1 1 calc R . . C21A C 0.7980(2) 0.5367(2) 0.1126(2) 0.083(3) Uiso 0.461(10) 1 d PGU A 1 C22A C 0.7868(3) 0.5158(3) 0.0835(2) 0.118(4) Uiso 0.461(10) 1 d PGDU A 1 C23A C 0.7558(3) 0.4949(3) 0.0863(2) 0.119(4) Uiso 0.461(10) 1 d PGU A 1 H23A H 0.7482 0.4807 0.0665 0.143 Uiso 0.461(10) 1 calc PR A 1 C24A C 0.7361(2) 0.4949(2) 0.1182(3) 0.124(4) Uiso 0.461(10) 1 d PGU A 1 H24A H 0.7149 0.4806 0.1201 0.148 Uiso 0.461(10) 1 calc PR A 1 C25A C 0.7473(2) 0.5157(2) 0.1472(2) 0.109(4) Uiso 0.461(10) 1 d PGU A 1 H25A H 0.7338 0.5157 0.1689 0.131 Uiso 0.461(10) 1 calc PR A 1 C26A C 0.7783(2) 0.5366(2) 0.1444(2) 0.105(3) Uiso 0.461(10) 1 d PGDU A 1 C21B C 0.8043(2) 0.5412(2) 0.1037(2) 0.117(4) Uiso 0.539(10) 1 d PGU A 2 C22B C 0.8002(2) 0.5218(2) 0.0719(2) 0.107(3) Uiso 0.539(10) 1 d PGDU A 2 C23B C 0.7700(3) 0.5004(3) 0.0668(2) 0.146(4) Uiso 0.539(10) 1 d PGU A 2 H23B H 0.7672 0.4871 0.0451 0.175 Uiso 0.539(10) 1 calc PR A 2 C24B C 0.7438(2) 0.4983(3) 0.0935(3) 0.148(5) Uiso 0.539(10) 1 d PGU A 2 H24B H 0.7231 0.4836 0.0901 0.177 Uiso 0.539(10) 1 calc PR A 2 C25B C 0.7479(2) 0.5176(3) 0.1253(3) 0.134(4) Uiso 0.539(10) 1 d PGU A 2 H25B H 0.7300 0.5162 0.1436 0.161 Uiso 0.539(10) 1 calc PR A 2 C26B C 0.7782(2) 0.5391(2) 0.1304(2) 0.106(3) Uiso 0.539(10) 1 d PGDU A 2 C27A C 0.8086(4) 0.5149(5) 0.0502(3) 0.131(4) Uiso 0.461(10) 1 d PDU A 1 H27A H 0.8185 0.5393 0.0556 0.157 Uiso 0.461(10) 1 calc PR A 1 C28A C 0.8458(6) 0.4984(8) 0.0547(8) 0.196(10) Uiso 0.461(10) 1 d PDU A 1 H28D H 0.8558 0.4927 0.0309 0.294 Uiso 0.461(10) 1 calc PR A 1 H28E H 0.8439 0.4763 0.0690 0.294 Uiso 0.461(10) 1 calc PR A 1 H28F H 0.8616 0.5156 0.0670 0.294 Uiso 0.461(10) 1 calc PR A 1 C29A C 0.7991(8) 0.5267(8) 0.0127(5) 0.229(10) Uiso 0.461(10) 1 d PDU A 1 H29A H 0.7929 0.5523 0.0128 0.344 Uiso 0.461(10) 1 calc PR A 1 H29B H 0.7785 0.5126 0.0040 0.344 Uiso 0.461(10) 1 calc PR A 1 H29C H 0.8198 0.5228 -0.0033 0.344 Uiso 0.461(10) 1 calc PR A 1 C27B C 0.8276(4) 0.5255(4) 0.0425(3) 0.138(4) Uiso 0.539(10) 1 d PDU A 2 H27B H 0.8450 0.5397 0.0573 0.165 Uiso 0.539(10) 1 calc PR A 2 C28B C 0.8506(5) 0.4926(5) 0.0404(6) 0.169(7) Uiso 0.539(10) 1 d PDU A 2 H28A H 0.8747 0.4993 0.0319 0.254 Uiso 0.539(10) 1 calc PR A 2 H28B H 0.8398 0.4754 0.0237 0.254 Uiso 0.539(10) 1 calc PR A 2 H28C H 0.8525 0.4817 0.0644 0.254 Uiso 0.539(10) 1 calc PR A 2 C29B C 0.8214(9) 0.5544(7) 0.0155(7) 0.265(12) Uiso 0.539(10) 1 d PDU A 2 H29D H 0.8092 0.5748 0.0271 0.397 Uiso 0.539(10) 1 calc PR A 2 H29E H 0.8063 0.5452 -0.0041 0.397 Uiso 0.539(10) 1 calc PR A 2 H29F H 0.8445 0.5624 0.0057 0.397 Uiso 0.539(10) 1 calc PR A 2 C30 C 0.7855(2) 0.5615(2) 0.1687(2) 0.179(3) Uani 1 1 d DU . . H30 H 0.8040 0.5795 0.1612 0.215 Uiso 1 1 calc R A 1 C31 C 0.7957(3) 0.5395(3) 0.2012(3) 0.223(5) Uani 1 1 d U A . H31A H 0.7761 0.5228 0.2070 0.335 Uiso 1 1 calc R . . H31B H 0.7999 0.5556 0.2217 0.335 Uiso 1 1 calc R . . H31C H 0.8177 0.5259 0.1960 0.335 Uiso 1 1 calc R . . C32A C 0.7476(5) 0.5770(9) 0.1742(7) 0.207(9) Uiso 0.58(3) 1 d PDU A 1 H32A H 0.7297 0.5578 0.1713 0.311 Uiso 0.58(3) 1 calc PR A 1 H32B H 0.7432 0.5959 0.1564 0.311 Uiso 0.58(3) 1 calc PR A 1 H32C H 0.7457 0.5872 0.1985 0.311 Uiso 0.58(3) 1 calc PR A 1 C32B C 0.7658(9) 0.5947(6) 0.1815(6) 0.172(10) Uiso 0.42(3) 1 d PDU A 2 H32D H 0.7434 0.5876 0.1936 0.258 Uiso 0.42(3) 1 calc PR A 2 H32E H 0.7601 0.6101 0.1608 0.258 Uiso 0.42(3) 1 calc PR A 2 H32F H 0.7811 0.6081 0.1984 0.258 Uiso 0.42(3) 1 calc PR A 2 O1S O 0.7897(4) 0.9254(6) 0.0424(5) 0.253(8) Uani 0.50 1 d PU . . C1S C 0.7550(6) 0.7805(4) -0.0008(5) 0.173(6) Uiso 0.50 1 d PDU . . C2S C 0.7553(7) 0.7810(6) -0.0383(5) 0.191(7) Uiso 0.50 1 d PDU . . C3S C 0.7500 0.7500 -0.0586(9) 0.253(11) Uiso 1 4 d SDU . . C4S C 0.7500 0.7500 -0.0997(10) 0.217(15) Uiso 0.60 4 d SPDU . . Cl1S Cl 0.7500 0.7500 0.7500 0.0788(13) Uani 1 24 d S . . 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 0.0640(6) 0.0640(6) 0.1378(13) 0.000 0.000 0.000 O1 0.083(2) 0.091(2) 0.149(3) 0.015(2) -0.025(2) 0.0084(17) O2 0.079(2) 0.073(2) 0.202(4) 0.017(2) -0.022(2) 0.0030(16) N1S 0.081(3) 0.081(3) 0.147(8) 0.000 0.000 0.000 N1 0.064(2) 0.066(2) 0.137(4) -0.004(2) -0.014(2) 0.0032(16) N2 0.067(2) 0.071(2) 0.141(4) 0.007(2) -0.006(2) 0.0004(19) C1 0.076(2) 0.069(2) 0.132(4) -0.005(2) -0.016(3) -0.0014(18) C2 0.074(2) 0.085(3) 0.125(4) 0.000(3) -0.017(3) -0.003(2) C3 0.074(3) 0.085(3) 0.135(4) -0.001(3) -0.018(3) 0.013(2) C4 0.081(3) 0.073(3) 0.146(4) 0.007(3) -0.018(3) 0.0056(19) C5 0.080(3) 0.070(2) 0.161(5) 0.010(3) -0.022(3) -0.002(2) C6 0.076(2) 0.073(2) 0.138(4) 0.008(3) -0.020(3) 0.0042(19) C7 0.080(3) 0.067(3) 0.122(4) 0.000(2) -0.018(3) 0.007(2) C8 0.066(3) 0.071(3) 0.134(4) 0.008(3) -0.008(3) -0.001(2) C9 0.069(3) 0.111(4) 0.154(4) 0.042(3) -0.020(2) 0.009(3) C10 0.101(3) 0.113(4) 0.160(4) 0.047(3) -0.042(3) -0.009(3) C11 0.109(4) 0.157(5) 0.200(6) 0.078(5) -0.067(3) -0.029(4) C12 0.099(4) 0.201(7) 0.247(8) 0.122(6) -0.043(4) -0.016(4) C13 0.099(4) 0.214(8) 0.220(6) 0.114(6) 0.011(4) 0.009(4) C14 0.098(4) 0.175(6) 0.169(4) 0.067(4) -0.001(3) 0.032(4) C15 0.131(4) 0.113(4) 0.142(4) 0.020(3) -0.038(3) -0.013(4) C16 0.151(6) 0.117(4) 0.136(6) 0.018(3) 0.007(4) 0.000(4) C17 0.221(10) 0.141(5) 0.212(7) -0.037(6) -0.062(6) 0.008(6) C18 0.164(6) 0.199(6) 0.174(5) 0.032(5) 0.029(5) 0.043(6) C19 0.41(2) 0.344(15) 0.175(6) 0.066(10) -0.029(11) -0.151(15) C20 0.225(11) 0.196(7) 0.296(15) 0.008(6) -0.048(10) 0.030(9) C30 0.163(6) 0.162(6) 0.211(7) 0.037(5) 0.062(5) 0.075(5) C31 0.226(10) 0.187(9) 0.257(11) 0.064(8) 0.045(9) 0.087(8) O1S 0.147(9) 0.340(17) 0.273(15) 0.111(13) 0.054(9) 0.072(10) Cl1S 0.0788(13) 0.0788(13) 0.0788(13) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.935(3) 16_655 ? Co1 N1 1.935(3) 15_565 ? Co1 N1 1.935(3) . ? Co1 N1 1.935(3) 2_665 ? Co1 N1S 2.108(11) . ? Co1 O3 2.31(3) . ? O1 C3 1.376(6) . ? O1 C9 1.387(7) . ? O2 C21B 1.222(7) . ? O2 C4 1.376(6) . ? O2 C21A 1.500(7) . ? N1S C1S 1.355(9) 16_655 ? N1S C1S 1.355(9) 15_565 ? N1S C1S 1.355(9) 2_665 ? N1S C1S 1.355(9) . ? N1 C8 1.356(6) 16_655 ? N1 C7 1.357(6) . ? N2 C8 1.326(6) . ? N2 C7 1.334(7) . ? C1 C6 1.379(6) . ? C1 C2 1.407(7) . ? C1 C8 1.466(7) 16_655 ? C2 C3 1.349(7) . ? C2 H2 0.9500 . ? C3 C4 1.409(7) . ? C4 C5 1.374(7) . ? C5 C6 1.387(7) . ? C5 H5 0.9500 . ? C6 C7 1.434(7) . ? C8 N1 1.356(6) 15_565 ? C8 C1 1.466(7) 15_565 ? C9 C14 1.347(10) . ? C9 C10 1.404(10) . ? C10 C11 1.394(9) . ? C10 C15 1.545(10) . ? C11 C12 1.335(13) . ? C11 H11 0.9500 . ? C12 C13 1.400(15) . ? C12 H12 0.9500 . ? C13 C14 1.401(12) . ? C13 H13 0.9500 . ? C14 C18 1.452(13) . ? C15 C16 1.498(9) . ? C15 C17 1.562(11) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.449(15) . ? C18 C20 1.500(14) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.481(9) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.319(8) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.496(9) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.669(8) . ? C27A C29A 1.501(10) . ? C27A C28A 1.517(10) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.488(10) . ? C27B C28B 1.491(10) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.501(12) . ? C30 C32B 1.511(10) . ? C30 C32A 1.534(10) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C1S C2S 1.391(10) . ? C1S C1S 1.62(2) 16_655 ? C1S C1S 1.62(2) 15_565 ? C2S C3S 1.390(10) . ? C2S C2S 1.65(3) 16_655 ? C2S C2S 1.65(3) 15_565 ? C3S C2S 1.390(10) 15_565 ? C3S C2S 1.390(10) 2_665 ? C3S C2S 1.390(10) 16_655 ? C3S C4S 1.53(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 172.0(3) 16_655 15_565 ? N1 Co1 N1 89.72(2) 16_655 . ? N1 Co1 N1 89.72(2) 15_565 . ? N1 Co1 N1 89.72(2) 16_655 2_665 ? N1 Co1 N1 89.72(2) 15_565 2_665 ? N1 Co1 N1 172.0(3) . 2_665 ? N1 Co1 N1S 94.02(14) 16_655 . ? N1 Co1 N1S 94.02(14) 15_565 . ? N1 Co1 N1S 94.02(14) . . ? N1 Co1 N1S 94.02(14) 2_665 . ? N1 Co1 O3 85.98(14) 16_655 . ? N1 Co1 O3 85.98(14) 15_565 . ? N1 Co1 O3 85.98(14) . . ? N1 Co1 O3 85.98(14) 2_665 . ? N1S Co1 O3 180.000(4) . . ? C3 O1 C9 118.3(4) . . ? C21B O2 C4 112.9(6) . . ? C21B O2 C21A 14.3(6) . . ? C4 O2 C21A 117.5(5) . . ? C1S N1S C1S 115.8(19) 16_655 15_565 ? C1S N1S C1S 73.6(9) 16_655 2_665 ? C1S N1S C1S 73.6(9) 15_565 2_665 ? C1S N1S C1S 73.6(9) 16_655 . ? C1S N1S C1S 73.6(9) 15_565 . ? C1S N1S C1S 115.8(19) 2_665 . ? C1S N1S Co1 122.1(9) 16_655 . ? C1S N1S Co1 122.1(9) 15_565 . ? C1S N1S Co1 122.1(9) 2_665 . ? C1S N1S Co1 122.1(9) . . ? C8 N1 C7 108.0(4) 16_655 . ? C8 N1 Co1 126.2(3) 16_655 . ? C7 N1 Co1 125.8(3) . . ? C8 N2 C7 119.7(4) . . ? C6 C1 C2 121.3(4) . . ? C6 C1 C8 105.3(4) . 16_655 ? C2 C1 C8 133.0(4) . 16_655 ? C3 C2 C1 117.5(5) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? C2 C3 O1 125.3(5) . . ? C2 C3 C4 121.2(4) . . ? O1 C3 C4 113.4(4) . . ? C5 C4 O2 124.4(5) . . ? C5 C4 C3 121.4(5) . . ? O2 C4 C3 114.1(4) . . ? C4 C5 C6 117.5(5) . . ? C4 C5 H5 121.3 . . ? C6 C5 H5 121.3 . . ? C1 C6 C5 120.9(4) . . ? C1 C6 C7 107.3(4) . . ? C5 C6 C7 131.5(4) . . ? N2 C7 N1 129.4(4) . . ? N2 C7 C6 120.8(4) . . ? N1 C7 C6 109.8(4) . . ? N2 C8 N1 129.2(4) . 15_565 ? N2 C8 C1 121.2(4) . 15_565 ? N1 C8 C1 109.5(4) 15_565 15_565 ? C14 C9 O1 119.8(7) . . ? C14 C9 C10 123.8(7) . . ? O1 C9 C10 116.1(6) . . ? C11 C10 C9 117.3(7) . . ? C11 C10 C15 121.4(7) . . ? C9 C10 C15 121.3(5) . . ? C12 C11 C10 120.3(9) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 121.5(9) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 119.8(10) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C9 C14 C13 117.3(10) . . ? C9 C14 C18 121.7(8) . . ? C13 C14 C18 121.0(10) . . ? C16 C15 C10 109.3(6) . . ? C16 C15 C17 109.8(6) . . ? C10 C15 C17 113.9(7) . . ? C16 C15 H15 107.9 . . ? C10 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 122.8(11) . . ? C14 C18 C20 113.6(10) . . ? C19 C18 C20 108.7(13) . . ? C14 C18 H18 103.0 . . ? C19 C18 H18 103.0 . . ? C20 C18 H18 103.0 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 119.3(5) . . ? C26A C21A O2 120.7(5) . . ? C23A C22A C21A 120.0 . . ? C23A C22A C27A 120.1(9) . . ? C21A C22A C27A 119.8(9) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C30 C26A C25A 120.4(7) . . ? C30 C26A C21A 118.3(7) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 120.7(6) . . ? O2 C21B C26B 119.3(6) . . ? C22B C21B C26B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B C27B 119.9(8) . . ? C23B C22B C27B 120.1(8) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 122.1(6) . . ? C21B C26B C30 117.8(6) . . ? C22A C27A C29A 129.8(16) . . ? C22A C27A C28A 114.6(15) . . ? C29A C27A C28A 115.6(17) . . ? C22A C27A H27A 90.6 . . ? C29A C27A H27A 90.6 . . ? C28A C27A H27A 90.6 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 130.1(17) . . ? C29B C27B C22B 116.9(15) . . ? C28B C27B C22B 110.6(13) . . ? C29B C27B H27B 95.0 . . ? C28B C27B H27B 95.0 . . ? C22B C27B H27B 95.0 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 102.8(9) . . ? C26A C30 C32B 133.5(15) . . ? C31 C30 C32B 108.2(11) . . ? C26A C30 C32A 99.6(15) . . ? C31 C30 C32A 109.2(11) . . ? C32B C30 C32A 37.6(10) . . ? C26A C30 C26B 15.2(6) . . ? C31 C30 C26B 117.1(8) . . ? C32B C30 C26B 126.5(13) . . ? C32A C30 C26B 98.7(13) . . ? C26A C30 H30 114.5 . . ? C31 C30 H30 114.5 . . ? C32B C30 H30 82.7 . . ? C32A C30 H30 114.5 . . ? C26B C30 H30 101.8 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N1S C1S C2S 122.9(18) . . ? N1S C1S C1S 53.2(4) . 16_655 ? C2S C1S C1S 90.9(12) . 16_655 ? N1S C1S C1S 53.2(4) . 15_565 ? C2S C1S C1S 90.3(13) . 15_565 ? C1S C1S C1S 90.000(7) 16_655 15_565 ? C3S C2S C1S 122(3) . . ? C3S C2S C2S 53.5(8) . 16_655 ? C1S C2S C2S 89.1(12) . 16_655 ? C3S C2S C2S 53.5(8) . 15_565 ? C1S C2S C2S 89.7(13) . 15_565 ? C2S C2S C2S 90.000(7) 16_655 15_565 ? C2S C3S C2S 72.9(15) 15_565 . ? C2S C3S C2S 72.9(15) 15_565 2_665 ? C2S C3S C2S 114(3) . 2_665 ? C2S C3S C2S 114(3) 15_565 16_655 ? C2S C3S C2S 72.9(15) . 16_655 ? C2S C3S C2S 72.9(15) 2_665 16_655 ? C2S C3S C4S 122.8(16) 15_565 . ? C2S C3S C4S 122.8(16) . . ? C2S C3S C4S 122.8(16) 2_665 . ? C2S C3S C4S 122.8(16) 16_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 Co1 N1S C1S -137.6(11) 16_655 . . 16_655 ? N1 Co1 N1S C1S 42.4(11) 15_565 . . 16_655 ? N1 Co1 N1S C1S 132.4(11) . . . 16_655 ? N1 Co1 N1S C1S -47.6(11) 2_665 . . 16_655 ? O3 Co1 N1S C1S 9(100) . . . 16_655 ? N1 Co1 N1S C1S 42.4(11) 16_655 . . 15_565 ? N1 Co1 N1S C1S -137.6(11) 15_565 . . 15_565 ? N1 Co1 N1S C1S -47.6(11) . . . 15_565 ? N1 Co1 N1S C1S 132.4(11) 2_665 . . 15_565 ? O3 Co1 N1S C1S -171(100) . . . 15_565 ? N1 Co1 N1S C1S 132.4(11) 16_655 . . 2_665 ? N1 Co1 N1S C1S -47.6(11) 15_565 . . 2_665 ? N1 Co1 N1S C1S 42.4(11) . . . 2_665 ? N1 Co1 N1S C1S -137.6(11) 2_665 . . 2_665 ? O3 Co1 N1S C1S -81(100) . . . 2_665 ? N1 Co1 N1S C1S -47.6(11) 16_655 . . . ? N1 Co1 N1S C1S 132.4(11) 15_565 . . . ? N1 Co1 N1S C1S -137.6(11) . . . . ? N1 Co1 N1S C1S 42.4(11) 2_665 . . . ? O3 Co1 N1S C1S 99(100) . . . . ? N1 Co1 N1 C8 -2.9(6) 16_655 . . 16_655 ? N1 Co1 N1 C8 -174.9(4) 15_565 . . 16_655 ? N1 Co1 N1 C8 -88.9(5) 2_665 . . 16_655 ? N1S Co1 N1 C8 91.1(4) . . . 16_655 ? O3 Co1 N1 C8 -88.9(4) . . . 16_655 ? N1 Co1 N1 C7 174.3(4) 16_655 . . . ? N1 Co1 N1 C7 2.3(6) 15_565 . . . ? N1 Co1 N1 C7 88.3(4) 2_665 . . . ? N1S Co1 N1 C7 -91.7(4) . . . . ? O3 Co1 N1 C7 88.3(4) . . . . ? C6 C1 C2 C3 -1.5(8) . . . . ? C8 C1 C2 C3 170.9(6) 16_655 . . . ? C1 C2 C3 O1 179.4(5) . . . . ? C1 C2 C3 C4 3.6(9) . . . . ? C9 O1 C3 C2 4.6(9) . . . . ? C9 O1 C3 C4 -179.4(5) . . . . ? C21B O2 C4 C5 11.9(9) . . . . ? C21A O2 C4 C5 -3.1(9) . . . . ? C21B O2 C4 C3 -172.3(6) . . . . ? C21A O2 C4 C3 172.7(6) . . . . ? C2 C3 C4 C5 -2.8(10) . . . . ? O1 C3 C4 C5 -179.0(6) . . . . ? C2 C3 C4 O2 -178.7(5) . . . . ? O1 C3 C4 O2 5.0(8) . . . . ? O2 C4 C5 C6 175.2(6) . . . . ? C3 C4 C5 C6 -0.4(9) . . . . ? C2 C1 C6 C5 -1.6(9) . . . . ? C8 C1 C6 C5 -175.8(6) 16_655 . . . ? C2 C1 C6 C7 173.2(5) . . . . ? C8 C1 C6 C7 -1.0(6) 16_655 . . . ? C4 C5 C6 C1 2.5(9) . . . . ? C4 C5 C6 C7 -170.9(6) . . . . ? C8 N2 C7 N1 -3.5(9) . . . . ? C8 N2 C7 C6 173.6(5) . . . . ? C8 N1 C7 N2 178.0(5) 16_655 . . . ? Co1 N1 C7 N2 0.4(8) . . . . ? C8 N1 C7 C6 0.6(6) 16_655 . . . ? Co1 N1 C7 C6 -177.0(4) . . . . ? C1 C6 C7 N2 -177.3(5) . . . . ? C5 C6 C7 N2 -3.2(10) . . . . ? C1 C6 C7 N1 0.3(6) . . . . ? C5 C6 C7 N1 174.4(6) . . . . ? C7 N2 C8 N1 2.8(9) . . . 15_565 ? C7 N2 C8 C1 -172.1(5) . . . 15_565 ? C3 O1 C9 C14 -99.5(7) . . . . ? C3 O1 C9 C10 86.3(6) . . . . ? C14 C9 C10 C11 0.3(9) . . . . ? O1 C9 C10 C11 174.3(5) . . . . ? C14 C9 C10 C15 -179.0(6) . . . . ? O1 C9 C10 C15 -5.0(8) . . . . ? C9 C10 C11 C12 -1.1(10) . . . . ? C15 C10 C11 C12 178.2(7) . . . . ? C10 C11 C12 C13 1.0(13) . . . . ? C11 C12 C13 C14 -0.2(14) . . . . ? O1 C9 C14 C13 -173.2(6) . . . . ? C10 C9 C14 C13 0.5(10) . . . . ? O1 C9 C14 C18 4.2(10) . . . . ? C10 C9 C14 C18 177.9(7) . . . . ? C12 C13 C14 C9 -0.6(12) . . . . ? C12 C13 C14 C18 -178.1(8) . . . . ? C11 C10 C15 C16 -102.8(7) . . . . ? C9 C10 C15 C16 76.4(7) . . . . ? C11 C10 C15 C17 20.4(9) . . . . ? C9 C10 C15 C17 -160.4(6) . . . . ? C9 C14 C18 C19 141.8(13) . . . . ? C13 C14 C18 C19 -40.9(16) . . . . ? C9 C14 C18 C20 -84.0(11) . . . . ? C13 C14 C18 C20 93.3(11) . . . . ? C21B O2 C21A C22A 21(3) . . . . ? C4 O2 C21A C22A 95.9(7) . . . . ? C21B O2 C21A C26A -159(3) . . . . ? C4 O2 C21A C26A -84.0(7) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A -179.8(8) . . . . ? C26A C21A C22A C27A -177.7(10) . . . . ? O2 C21A C22A C27A 2.5(11) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A 177.7(10) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 167.1(10) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -167.4(10) . . . . ? O2 C21A C26A C30 12.5(9) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A 179.8(8) . . . . ? C4 O2 C21B C22B 95.2(7) . . . . ? C21A O2 C21B C22B -153(3) . . . . ? C4 O2 C21B C26B -87.4(7) . . . . ? C21A O2 C21B C26B 24(2) . . . . ? O2 C21B C22B C23B 177.4(10) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B -5.4(10) . . . . ? C26B C21B C22B C27B 177.1(9) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -177.1(9) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -177.2(8) . . . . ? O2 C21B C26B C25B -177.5(9) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -0.2(8) . . . . ? C22B C21B C26B C30 177.3(8) . . . . ? C23A C22A C27A C29A 65(2) . . . . ? C21A C22A C27A C29A -118(2) . . . . ? C23A C22A C27A C28A -113.1(18) . . . . ? C21A C22A C27A C28A 65(2) . . . . ? C21B C22B C27B C29B -89.3(18) . . . . ? C23B C22B C27B C29B 87.8(18) . . . . ? C21B C22B C27B C28B 106.3(13) . . . . ? C23B C22B C27B C28B -76.6(15) . . . . ? C25A C26A C30 C31 71.5(9) . . . . ? C21A C26A C30 C31 -121.2(8) . . . . ? C25A C26A C30 C32B -60(2) . . . . ? C21A C26A C30 C32B 107.6(18) . . . . ? C25A C26A C30 C32A -40.8(13) . . . . ? C21A C26A C30 C32A 126.5(12) . . . . ? C25A C26A C30 C26B -129(2) . . . . ? C21A C26A C30 C26B 38.8(18) . . . . ? C25B C26B C30 C26A 49.4(19) . . . . ? C21B C26B C30 C26A -128(2) . . . . ? C25B C26B C30 C31 71.5(9) . . . . ? C21B C26B C30 C31 -105.8(9) . . . . ? C25B C26B C30 C32B -73.2(18) . . . . ? C21B C26B C30 C32B 109.5(17) . . . . ? C25B C26B C30 C32A -45.3(14) . . . . ? C21B C26B C30 C32A 137.4(12) . . . . ? C1S N1S C1S C2S -62.6(18) 16_655 . . . ? C1S N1S C1S C2S 61.5(18) 15_565 . . . ? C1S N1S C1S C2S -0.5(17) 2_665 . . . ? Co1 N1S C1S C2S 179.5(17) . . . . ? C1S N1S C1S C1S 124.1(12) 15_565 . . 16_655 ? C1S N1S C1S C1S 62.0(6) 2_665 . . 16_655 ? Co1 N1S C1S C1S -118.0(6) . . . 16_655 ? C1S N1S C1S C1S -124.1(12) 16_655 . . 15_565 ? C1S N1S C1S C1S -62.0(6) 2_665 . . 15_565 ? Co1 N1S C1S C1S 118.0(6) . . . 15_565 ? N1S C1S C2S C3S 1(3) . . . . ? C1S C1S C2S C3S -44(3) 16_655 . . . ? C1S C1S C2S C3S 46(3) 15_565 . . . ? N1S C1S C2S C2S 46(3) . . . 16_655 ? C1S C1S C2S C2S 0.5(17) 16_655 . . 16_655 ? C1S C1S C2S C2S 90.5(17) 15_565 . . 16_655 ? N1S C1S C2S C2S -44(3) . . . 15_565 ? C1S C1S C2S C2S -89.5(17) 16_655 . . 15_565 ? C1S C1S C2S C2S 0.5(17) 15_565 . . 15_565 ? C1S C2S C3S C2S -62.1(19) . . . 15_565 ? C2S C2S C3S C2S -123(2) 16_655 . . 15_565 ? C1S C2S C3S C2S -0.5(16) . . . 2_665 ? C2S C2S C3S C2S -61.5(10) 16_655 . . 2_665 ? C2S C2S C3S C2S 61.5(10) 15_565 . . 2_665 ? C1S C2S C3S C2S 61(2) . . . 16_655 ? C2S C2S C3S C2S 123(2) 15_565 . . 16_655 ? C1S C2S C3S C4S 179.5(16) . . . . ? C2S C2S C3S C4S 118.5(10) 16_655 . . . ? C2S C2S C3S C4S -118.5(10) 15_565 . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 23.53 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.296 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.072 data_PNC[Co-vPy0.82Bupy0.18] _database_code_depnum_ccdc_archive 'CCDC 900368' #TrackingRef '900368_PNC[Co-vPy0.82Bupy0.18].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C169.08 H215.58 Co N9 O20.75' _chemical_formula_weight 2765.02 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.5512(3) _cell_length_b 37.5512(3) _cell_length_c 37.5512(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52950.7(7) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9759 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.38 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.50 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.041 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17833 _exptl_absorpt_coefficient_mu 0.157 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9115 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69050 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 187976 _diffrn_reflns_av_R_equivalents 0.1323 _diffrn_reflns_av_sigmaI/netI 0.0394 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_k_min -44 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 24.27 _reflns_number_total 7836 _reflns_number_gt 6662 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7836 _refine_ls_number_parameters 429 _refine_ls_number_restraints 342 _refine_ls_R_factor_all 0.0944 _refine_ls_R_factor_gt 0.0876 _refine_ls_wR_factor_ref 0.3008 _refine_ls_wR_factor_gt 0.2881 _refine_ls_goodness_of_fit_ref 1.338 _refine_ls_restrained_S_all 1.366 _refine_ls_shift/su_max 0.005 _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 0.7500 0.7500 0.078009(17) 0.0369(3) Uani 1 4 d S . . O1 O 0.88846(4) 0.59626(4) 0.11050(5) 0.0509(5) Uani 1 1 d . A . O2 O 0.83130(4) 0.56062(4) 0.11082(5) 0.0524(5) Uani 1 1 d . . . N1S N 0.7500 0.7500 0.01946(13) 0.0546(11) Uani 1 4 d S . . N1 N 0.77799(5) 0.70714(5) 0.08170(5) 0.0384(4) Uani 1 1 d . A . N2 N 0.73162(5) 0.66219(5) 0.08502(5) 0.0407(5) Uani 1 1 d . A . C1 C 0.82559(6) 0.66808(6) 0.08888(7) 0.0405(5) Uani 1 1 d . . . C2 C 0.85855(6) 0.65215(6) 0.09541(7) 0.0433(5) Uani 1 1 d . A . H2 H 0.8800 0.6656 0.0949 0.052 Uiso 1 1 calc R . . C3 C 0.85881(6) 0.61619(6) 0.10253(7) 0.0456(6) Uani 1 1 d . . . C4 C 0.82710(6) 0.59595(6) 0.10218(7) 0.0446(5) Uani 1 1 d . A . C5 C 0.79458(6) 0.61158(6) 0.09473(7) 0.0454(6) Uani 1 1 d . . . H5 H 0.7733 0.5979 0.0941 0.054 Uiso 1 1 calc R A . C6 C 0.79427(6) 0.64807(6) 0.08813(6) 0.0412(5) Uani 1 1 d . A . C7 C 0.76509(6) 0.67308(6) 0.08407(6) 0.0400(5) Uani 1 1 d . . . C8 C 0.70508(5) 0.68549(6) 0.08433(6) 0.0387(5) Uani 1 1 d . . . C9 C 0.92110(6) 0.61384(7) 0.11379(9) 0.0570(7) Uani 1 1 d . . . C10 C 0.92923(8) 0.62844(7) 0.14772(10) 0.0675(9) Uani 1 1 d . A . C11 C 0.96336(9) 0.64325(9) 0.15172(13) 0.0880(13) Uani 1 1 d . . . H11 H 0.9702 0.6532 0.1739 0.106 Uiso 1 1 calc R A . C12 C 0.98645(10) 0.64342(12) 0.12407(16) 0.1015(16) Uani 1 1 d . A . H12 H 1.0094 0.6536 0.1274 0.122 Uiso 1 1 calc R . . C13 C 0.97802(9) 0.62947(12) 0.09143(14) 0.0972(15) Uani 1 1 d . . . H13 H 0.9948 0.6307 0.0726 0.117 Uiso 1 1 calc R A . C14 C 0.94394(8) 0.61297(9) 0.08549(10) 0.0736(9) Uani 1 1 d . A . C15 C 0.90328(9) 0.62645(8) 0.17798(10) 0.0728(9) Uani 1 1 d . . . H15 H 0.8792 0.6320 0.1681 0.087 Uiso 1 1 calc R A . C16 C 0.90163(11) 0.58897(10) 0.19380(11) 0.0784(9) Uani 1 1 d . A . H16A H 0.8946 0.5720 0.1753 0.118 Uiso 1 1 calc R . . H16B H 0.8841 0.5885 0.2132 0.118 Uiso 1 1 calc R . . H16C H 0.9251 0.5824 0.2031 0.118 Uiso 1 1 calc R . . C17 C 0.91010(18) 0.65233(12) 0.20858(15) 0.1207(19) Uani 1 1 d . A . H17A H 0.9308 0.6443 0.2223 0.181 Uiso 1 1 calc R . . H17B H 0.8891 0.6532 0.2241 0.181 Uiso 1 1 calc R . . H17C H 0.9148 0.6761 0.1990 0.181 Uiso 1 1 calc R . . C18 C 0.93327(12) 0.59447(12) 0.05127(12) 0.0937(12) Uani 1 1 d U . . H18 H 0.9074 0.5994 0.0473 0.112 Uiso 1 1 calc R A . C19 C 0.9533(2) 0.6079(2) 0.01882(18) 0.149(2) Uani 1 1 d U A . H19A H 0.9790 0.6060 0.0231 0.224 Uiso 1 1 calc R . . H19B H 0.9471 0.6328 0.0144 0.224 Uiso 1 1 calc R . . H19C H 0.9469 0.5935 -0.0020 0.224 Uiso 1 1 calc R . . C20 C 0.93760(16) 0.55424(14) 0.05505(17) 0.1191(16) Uani 1 1 d U A . H20A H 0.9621 0.5488 0.0624 0.179 Uiso 1 1 calc R . . H20B H 0.9326 0.5428 0.0321 0.179 Uiso 1 1 calc R . . H20C H 0.9209 0.5453 0.0731 0.179 Uiso 1 1 calc R . . C21A C 0.79985(16) 0.5402(2) 0.10913(19) 0.0506(12) Uani 0.572(8) 1 d PGU A 1 C22A C 0.79096(17) 0.51879(19) 0.08025(16) 0.0657(13) Uani 0.572(8) 1 d PGU A 1 C23A C 0.76116(17) 0.49690(14) 0.08192(16) 0.0775(16) Uani 0.572(8) 1 d PGU A 1 H23A H 0.7551 0.4823 0.0622 0.093 Uiso 0.572(8) 1 calc PR A 1 C24A C 0.74026(13) 0.49638(14) 0.1125(2) 0.0822(17) Uani 0.572(8) 1 d PGU A 1 H24A H 0.7199 0.4814 0.1136 0.099 Uiso 0.572(8) 1 calc PR A 1 C25A C 0.74915(15) 0.51776(17) 0.14135(17) 0.0764(16) Uani 0.572(8) 1 d PGU A 1 H25A H 0.7349 0.5174 0.1622 0.092 Uiso 0.572(8) 1 calc PR A 1 C26A C 0.77895(17) 0.5397(2) 0.13968(17) 0.0615(12) Uani 0.572(8) 1 d PGU A 1 C21B C 0.8030(2) 0.5392(3) 0.1080(3) 0.0549(16) Uani 0.428(8) 1 d PGU A 2 C22B C 0.80109(19) 0.5212(2) 0.0758(2) 0.0581(14) Uani 0.428(8) 1 d PGU A 2 C23B C 0.7714(2) 0.50065(19) 0.0678(2) 0.0746(18) Uani 0.428(8) 1 d PGU A 2 H23B H 0.7700 0.4883 0.0458 0.090 Uiso 0.428(8) 1 calc PR A 2 C24B C 0.74361(17) 0.49806(19) 0.0922(3) 0.081(2) Uani 0.428(8) 1 d PGU A 2 H24B H 0.7233 0.4840 0.0867 0.097 Uiso 0.428(8) 1 calc PR A 2 C25B C 0.7456(2) 0.5161(2) 0.1244(2) 0.0736(17) Uani 0.428(8) 1 d PGU A 2 H25B H 0.7266 0.5143 0.1411 0.088 Uiso 0.428(8) 1 calc PR A 2 C26B C 0.7753(3) 0.5367(3) 0.1324(2) 0.0699(16) Uani 0.428(8) 1 d PGDU A 2 C27A C 0.8155(2) 0.5214(2) 0.0474(2) 0.0706(15) Uani 0.572(8) 1 d PU A 1 H27A H 0.8228 0.5470 0.0465 0.085 Uiso 0.572(8) 1 calc PR A 1 C28A C 0.8514(2) 0.5002(2) 0.0521(2) 0.086(2) Uani 0.572(8) 1 d PU A 1 H28D H 0.8615 0.4949 0.0286 0.129 Uiso 0.572(8) 1 calc PR A 1 H28E H 0.8467 0.4778 0.0647 0.129 Uiso 0.572(8) 1 calc PR A 1 H28F H 0.8683 0.5146 0.0658 0.129 Uiso 0.572(8) 1 calc PR A 1 C29A C 0.8003(3) 0.5138(3) 0.0110(2) 0.125(3) Uani 0.572(8) 1 d PU A 1 H29A H 0.7904 0.5358 0.0009 0.187 Uiso 0.572(8) 1 calc PR A 1 H29B H 0.7814 0.4959 0.0131 0.187 Uiso 0.572(8) 1 calc PR A 1 H29C H 0.8191 0.5048 -0.0046 0.187 Uiso 0.572(8) 1 calc PR A 1 C27B C 0.8307(3) 0.5243(3) 0.0481(3) 0.075(2) Uani 0.428(8) 1 d PU A 2 H27B H 0.8504 0.5362 0.0614 0.089 Uiso 0.428(8) 1 calc PR A 2 C28B C 0.8454(4) 0.4877(4) 0.0404(4) 0.102(3) Uani 0.428(8) 1 d PU A 2 H28A H 0.8714 0.4890 0.0385 0.153 Uiso 0.428(8) 1 calc PR A 2 H28B H 0.8355 0.4790 0.0179 0.153 Uiso 0.428(8) 1 calc PR A 2 H28C H 0.8388 0.4715 0.0597 0.153 Uiso 0.428(8) 1 calc PR A 2 C29B C 0.8247(4) 0.5472(4) 0.0189(4) 0.124(4) Uani 0.428(8) 1 d PU A 2 H29D H 0.8120 0.5684 0.0269 0.186 Uiso 0.428(8) 1 calc PR A 2 H29E H 0.8105 0.5347 0.0009 0.186 Uiso 0.428(8) 1 calc PR A 2 H29F H 0.8476 0.5542 0.0085 0.186 Uiso 0.428(8) 1 calc PR A 2 C30 C 0.78412(12) 0.56011(10) 0.17021(11) 0.0872(10) Uani 1 1 d DU . . H30 H 0.8004 0.5808 0.1661 0.105 Uiso 1 1 calc R A 1 C31 C 0.79573(15) 0.53712(13) 0.20077(16) 0.1152(16) Uani 1 1 d U A . H31A H 0.7795 0.5168 0.2031 0.173 Uiso 1 1 calc R . . H31B H 0.7954 0.5511 0.2228 0.173 Uiso 1 1 calc R . . H31C H 0.8199 0.5284 0.1964 0.173 Uiso 1 1 calc R . . C32A C 0.7426(4) 0.5726(5) 0.1799(4) 0.114(4) Uani 0.476(19) 1 d PU A 1 H32A H 0.7293 0.5521 0.1891 0.171 Uiso 0.476(19) 1 calc PR A 1 H32B H 0.7310 0.5816 0.1583 0.171 Uiso 0.476(19) 1 calc PR A 1 H32C H 0.7432 0.5914 0.1979 0.171 Uiso 0.476(19) 1 calc PR A 1 C32B C 0.7621(4) 0.5902(3) 0.1813(3) 0.105(4) Uani 0.524(19) 1 d PU A 2 H32D H 0.7770 0.6078 0.1935 0.158 Uiso 0.524(19) 1 calc PR A 2 H32E H 0.7435 0.5818 0.1976 0.158 Uiso 0.524(19) 1 calc PR A 2 H32F H 0.7511 0.6011 0.1603 0.158 Uiso 0.524(19) 1 calc PR A 2 C1S C 0.7790(3) 0.7459(3) 0.0016(3) 0.105(3) Uiso 0.50 1 d PU . . C2S C 0.7801(4) 0.7479(4) -0.0367(5) 0.153(4) Uiso 0.50 1 d PU . . C3S C 0.7500 0.7500 -0.0537(6) 0.170(5) Uiso 1 4 d SDU . . C4S C 0.7500 0.7500 -0.0938(8) 0.179(11) Uiso 0.18(2) 4 d SPDU . . C5S C 0.765(2) 0.7149(11) -0.1065(14) 0.193(14) Uiso 0.138(15) 1 d PDU . . O1S O 0.7114(6) 0.6817(7) 0.1781(7) 0.185(8) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0268(3) 0.0268(3) 0.0569(4) 0.000 0.000 0.000 O1 0.0337(8) 0.0372(8) 0.0818(12) 0.0036(8) -0.0106(7) 0.0044(6) O2 0.0390(9) 0.0291(8) 0.0891(13) 0.0071(7) -0.0101(8) 0.0047(6) N1S 0.0531(15) 0.0531(15) 0.058(3) 0.000 0.000 0.000 N1 0.0293(9) 0.0304(8) 0.0553(11) -0.0026(7) -0.0019(7) -0.0005(6) N2 0.0319(9) 0.0308(9) 0.0594(11) 0.0028(7) -0.0042(7) 0.0002(7) C1 0.0313(10) 0.0310(10) 0.0591(13) -0.0024(9) -0.0054(9) 0.0016(8) C2 0.0330(10) 0.0353(11) 0.0617(14) -0.0016(9) -0.0061(9) 0.0000(8) C3 0.0349(11) 0.0377(11) 0.0641(14) -0.0017(10) -0.0081(9) 0.0051(8) C4 0.0382(11) 0.0306(10) 0.0651(14) 0.0024(9) -0.0090(10) 0.0051(8) C5 0.0325(10) 0.0296(10) 0.0740(16) 0.0007(9) -0.0078(10) 0.0007(8) C6 0.0331(10) 0.0314(10) 0.0592(13) -0.0013(9) -0.0067(9) 0.0020(8) C7 0.0317(11) 0.0312(10) 0.0572(13) 0.0010(8) -0.0067(8) -0.0009(8) C8 0.0302(10) 0.0307(10) 0.0553(12) 0.0031(8) -0.0028(8) -0.0014(8) C9 0.0320(12) 0.0504(14) 0.088(2) 0.0167(12) -0.0138(11) 0.0031(10) C10 0.0562(16) 0.0477(14) 0.099(2) 0.0170(14) -0.0357(15) -0.0033(11) C11 0.0551(18) 0.0681(19) 0.141(4) 0.031(2) -0.044(2) -0.0145(14) C12 0.0478(18) 0.091(3) 0.166(5) 0.052(3) -0.039(2) -0.0158(16) C13 0.0420(16) 0.109(3) 0.141(4) 0.057(3) 0.001(2) 0.0043(17) C14 0.0426(14) 0.081(2) 0.097(2) 0.0361(18) -0.0001(14) 0.0113(13) C15 0.076(2) 0.0581(17) 0.084(2) -0.0026(15) -0.0267(17) 0.0041(14) C16 0.079(2) 0.071(2) 0.085(2) 0.0107(17) -0.0050(18) 0.0004(16) C17 0.174(5) 0.073(3) 0.115(4) -0.012(2) -0.048(3) 0.005(3) C18 0.082(2) 0.102(3) 0.097(3) 0.023(2) 0.011(2) 0.022(2) C19 0.157(5) 0.169(6) 0.121(5) 0.018(4) 0.042(4) -0.007(4) C20 0.130(4) 0.103(3) 0.124(4) -0.004(3) -0.006(3) 0.028(3) C21A 0.035(2) 0.029(3) 0.088(2) 0.004(2) -0.013(2) 0.003(2) C22A 0.057(3) 0.043(2) 0.097(3) 0.000(2) -0.019(2) -0.004(2) C23A 0.072(4) 0.044(3) 0.117(4) -0.003(3) -0.018(3) -0.017(3) C24A 0.064(3) 0.049(3) 0.134(5) 0.013(3) -0.007(3) -0.012(2) C25A 0.057(3) 0.049(3) 0.123(4) 0.013(3) 0.013(3) -0.0013(19) C26A 0.047(2) 0.030(2) 0.108(3) 0.008(2) 0.009(2) 0.0044(18) C21B 0.047(3) 0.028(3) 0.090(3) -0.002(3) -0.009(3) 0.009(3) C22B 0.050(3) 0.032(3) 0.093(3) -0.001(2) -0.018(3) -0.004(2) C23B 0.072(4) 0.041(3) 0.111(4) -0.006(3) -0.012(3) -0.019(3) C24B 0.071(4) 0.047(3) 0.124(5) 0.016(4) -0.004(4) -0.025(3) C25B 0.055(3) 0.045(3) 0.121(4) 0.021(4) 0.006(3) -0.001(2) C26B 0.058(3) 0.037(3) 0.116(3) 0.005(3) 0.006(3) 0.007(3) C27A 0.073(4) 0.054(3) 0.085(3) -0.006(2) -0.019(3) -0.003(3) C28A 0.099(4) 0.081(5) 0.079(5) -0.003(4) -0.003(3) 0.025(4) C29A 0.134(7) 0.142(7) 0.098(4) -0.029(5) -0.048(4) 0.010(5) C27B 0.077(5) 0.060(4) 0.086(4) -0.007(3) 0.000(4) 0.002(4) C28B 0.136(9) 0.084(6) 0.087(7) -0.022(5) -0.006(6) 0.034(6) C29B 0.143(8) 0.108(7) 0.121(7) 0.030(5) 0.004(6) 0.018(6) C30 0.100(2) 0.0573(17) 0.104(2) -0.0026(15) 0.0281(19) 0.0165(16) C31 0.125(4) 0.092(3) 0.129(3) 0.010(3) -0.005(3) 0.034(3) C32A 0.105(6) 0.109(9) 0.128(7) -0.013(7) 0.019(6) 0.048(6) C32B 0.130(9) 0.065(5) 0.121(6) -0.004(4) 0.030(6) 0.034(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.9272(17) 16_655 ? Co1 N1 1.9272(17) 2_665 ? Co1 N1 1.9272(17) . ? Co1 N1 1.9272(17) 15_565 ? Co1 N1S 2.199(5) . ? O1 C3 1.375(3) . ? O1 C9 1.398(3) . ? O2 C21B 1.335(5) . ? O2 C4 1.375(3) . ? O2 C21A 1.410(4) . ? N1S C1S 1.288(11) 16_655 ? N1S C1S 1.288(11) 2_665 ? N1S C1S 1.288(11) . ? N1S C1S 1.288(11) 15_565 ? N1 C7 1.371(3) . ? N1 C8 1.377(3) 16_655 ? N2 C7 1.322(3) . ? N2 C8 1.327(3) . ? C1 C6 1.396(3) . ? C1 C2 1.396(3) . ? C1 C8 1.460(3) 16_655 ? C2 C3 1.376(3) . ? C2 H2 0.9500 . ? C3 C4 1.413(3) . ? C4 C5 1.384(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C7 1.451(3) . ? C8 N1 1.377(3) 15_565 ? C8 C1 1.460(3) 15_565 ? C9 C14 1.366(5) . ? C9 C10 1.420(5) . ? C10 C11 1.405(4) . ? C10 C15 1.499(5) . ? C11 C12 1.353(7) . ? C11 H11 0.9500 . ? C12 C13 1.370(7) . ? C12 H12 0.9500 . ? C13 C14 1.439(5) . ? C13 H13 0.9500 . ? C14 C18 1.514(6) . ? C15 C17 1.526(5) . ? C15 C16 1.529(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.519(7) . ? C18 C20 1.526(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.543(10) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.394(6) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.525(12) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.704(7) . ? C27A C29A 1.509(11) . ? C27A C28A 1.576(11) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.412(17) . ? C27B C28B 1.507(15) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C32B 1.461(8) . ? C30 C31 1.501(6) . ? C30 C32A 1.667(12) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? C1S C2S 1.439(19) . ? C1S C1S 1.555(15) 16_655 ? C1S C1S 1.555(15) 15_565 ? C2S C3S 1.301(16) . ? C2S C2S 1.60(2) 16_655 ? C2S C2S 1.60(2) 15_565 ? C3S C2S 1.301(16) 16_655 ? C3S C2S 1.301(16) 2_665 ? C3S C2S 1.301(16) 15_565 ? C3S C4S 1.51(2) . ? C4S C5S 1.51(2) 2_665 ? C4S C5S 1.51(2) 16_655 ? C4S C5S 1.51(2) 15_565 ? C4S C5S 1.51(2) . ? C5S C5S 2.03(4) 16_655 ? C5S C5S 2.03(4) 15_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 89.703(9) 16_655 2_665 ? N1 Co1 N1 89.703(9) 16_655 . ? N1 Co1 N1 171.74(12) 2_665 . ? N1 Co1 N1 171.74(12) 16_655 15_565 ? N1 Co1 N1 89.703(9) 2_665 15_565 ? N1 Co1 N1 89.703(9) . 15_565 ? N1 Co1 N1S 94.13(6) 16_655 . ? N1 Co1 N1S 94.13(6) 2_665 . ? N1 Co1 N1S 94.13(6) . . ? N1 Co1 N1S 94.13(6) 15_565 . ? C3 O1 C9 118.17(18) . . ? C21B O2 C4 118.1(6) . . ? C21B O2 C21A 4.5(8) . . ? C4 O2 C21A 114.7(4) . . ? C1S N1S C1S 74.2(5) 16_655 2_665 ? C1S N1S C1S 74.2(5) 16_655 . ? C1S N1S C1S 117.2(11) 2_665 . ? C1S N1S C1S 117.2(11) 16_655 15_565 ? C1S N1S C1S 74.2(5) 2_665 15_565 ? C1S N1S C1S 74.2(5) . 15_565 ? C1S N1S Co1 121.4(6) 16_655 . ? C1S N1S Co1 121.4(6) 2_665 . ? C1S N1S Co1 121.4(6) . . ? C1S N1S Co1 121.4(6) 15_565 . ? C7 N1 C8 107.15(17) . 16_655 ? C7 N1 Co1 126.24(14) . . ? C8 N1 Co1 126.53(14) 16_655 . ? C7 N2 C8 120.65(18) . . ? C6 C1 C2 121.3(2) . . ? C6 C1 C8 105.64(18) . 16_655 ? C2 C1 C8 132.9(2) . 16_655 ? C3 C2 C1 117.4(2) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? O1 C3 C2 125.6(2) . . ? O1 C3 C4 113.1(2) . . ? C2 C3 C4 121.3(2) . . ? O2 C4 C5 123.9(2) . . ? O2 C4 C3 114.85(19) . . ? C5 C4 C3 121.2(2) . . ? C4 C5 C6 117.4(2) . . ? C4 C5 H5 121.3 . . ? C6 C5 H5 121.3 . . ? C5 C6 C1 121.27(19) . . ? C5 C6 C7 131.4(2) . . ? C1 C6 C7 106.86(18) . . ? N2 C7 N1 128.78(19) . . ? N2 C7 C6 121.00(19) . . ? N1 C7 C6 110.10(18) . . ? N2 C8 N1 128.02(18) . 15_565 ? N2 C8 C1 121.64(19) . 15_565 ? N1 C8 C1 110.22(18) 15_565 15_565 ? C14 C9 O1 118.0(3) . . ? C14 C9 C10 124.9(3) . . ? O1 C9 C10 116.8(3) . . ? C11 C10 C9 116.4(4) . . ? C11 C10 C15 122.1(3) . . ? C9 C10 C15 121.4(2) . . ? C12 C11 C10 120.3(4) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 122.5(3) . . ? C11 C12 H12 118.8 . . ? C13 C12 H12 118.8 . . ? C12 C13 C14 120.6(4) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 115.3(4) . . ? C9 C14 C18 120.3(3) . . ? C13 C14 C18 124.4(4) . . ? C10 C15 C17 115.5(4) . . ? C10 C15 C16 111.5(3) . . ? C17 C15 C16 107.5(3) . . ? C10 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C16 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 113.4(5) . . ? C14 C18 C20 110.3(4) . . ? C19 C18 C20 110.5(5) . . ? C14 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 123.4(4) . . ? C26A C21A O2 116.3(4) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 116.3(4) . . ? C23A C22A C27A 123.7(4) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A C30 113.6(4) . . ? C21A C26A C30 126.3(4) . . ? O2 C21B C22B 113.8(6) . . ? O2 C21B C26B 125.9(6) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 118.7(7) . . ? C21B C22B C27B 121.3(7) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 128.5(6) . . ? C21B C26B C30 111.5(6) . . ? C29A C27A C22A 119.0(7) . . ? C29A C27A C28A 109.2(7) . . ? C22A C27A C28A 113.0(7) . . ? C29A C27A H27A 104.7 . . ? C22A C27A H27A 104.7 . . ? C28A C27A H27A 104.7 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 117.5(11) . . ? C29B C27B C22B 117.3(10) . . ? C28B C27B C22B 109.3(10) . . ? C29B C27B H27B 103.5 . . ? C28B C27B H27B 103.5 . . ? C22B C27B H27B 103.5 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C32B 125.6(8) . . ? C26A C30 C31 110.6(5) . . ? C32B C30 C31 113.0(6) . . ? C26A C30 C32A 101.8(7) . . ? C32B C30 C32A 36.0(5) . . ? C31 C30 C32A 105.5(6) . . ? C26A C30 C26B 3.8(7) . . ? C32B C30 C26B 121.8(8) . . ? C31 C30 C26B 113.4(5) . . ? C32A C30 C26B 98.3(7) . . ? C26A C30 H30 112.7 . . ? C32B C30 H30 77.9 . . ? C31 C30 H30 112.7 . . ? C32A C30 H30 112.7 . . ? C26B C30 H30 113.1 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? N1S C1S C2S 122.6(11) . . ? N1S C1S C1S 52.9(3) . 16_655 ? C2S C1S C1S 88.6(8) . 16_655 ? N1S C1S C1S 52.9(3) . 15_565 ? C2S C1S C1S 93.1(8) . 15_565 ? C1S C1S C1S 90.000(5) 16_655 15_565 ? C3S C2S C1S 117.9(17) . . ? C3S C2S C2S 52.0(5) . 16_655 ? C1S C2S C2S 91.1(8) . 16_655 ? C3S C2S C2S 52.0(5) . 15_565 ? C1S C2S C2S 86.8(8) . 15_565 ? C2S C2S C2S 90.000(5) 16_655 15_565 ? C2S C3S C2S 76.0(11) 16_655 . ? C2S C3S C2S 76.0(11) 16_655 2_665 ? C2S C3S C2S 121(2) . 2_665 ? C2S C3S C2S 121(2) 16_655 15_565 ? C2S C3S C2S 76.0(11) . 15_565 ? C2S C3S C2S 76.0(11) 2_665 15_565 ? C2S C3S C4S 119.4(12) 16_655 . ? C2S C3S C4S 119.4(12) . . ? C2S C3S C4S 119.4(12) 2_665 . ? C2S C3S C4S 119.4(12) 15_565 . ? C3S C4S C5S 108(2) . 2_665 ? C3S C4S C5S 108(2) . 16_655 ? C5S C4S C5S 84.3(14) 2_665 16_655 ? C3S C4S C5S 108(2) . 15_565 ? C5S C4S C5S 84.3(14) 2_665 15_565 ? C5S C4S C5S 143(5) 16_655 15_565 ? C3S C4S C5S 108(2) . . ? C5S C4S C5S 143(5) 2_665 . ? C5S C4S C5S 84.3(14) 16_655 . ? C5S C4S C5S 84.3(14) 15_565 . ? C4S C5S C5S 47.9(7) . 16_655 ? C4S C5S C5S 47.9(7) . 15_565 ? C5S C5S C5S 90.000(13) 16_655 15_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1S C1S -48.8(6) 16_655 . . 16_655 ? N1 Co1 N1S C1S 41.2(6) 2_665 . . 16_655 ? N1 Co1 N1S C1S -138.8(6) . . . 16_655 ? N1 Co1 N1S C1S 131.2(6) 15_565 . . 16_655 ? N1 Co1 N1S C1S -138.8(6) 16_655 . . 2_665 ? N1 Co1 N1S C1S -48.8(6) 2_665 . . 2_665 ? N1 Co1 N1S C1S 131.2(6) . . . 2_665 ? N1 Co1 N1S C1S 41.2(6) 15_565 . . 2_665 ? N1 Co1 N1S C1S 41.2(6) 16_655 . . . ? N1 Co1 N1S C1S 131.2(6) 2_665 . . . ? N1 Co1 N1S C1S -48.8(6) . . . . ? N1 Co1 N1S C1S -138.8(6) 15_565 . . . ? N1 Co1 N1S C1S 131.2(6) 16_655 . . 15_565 ? N1 Co1 N1S C1S -138.8(6) 2_665 . . 15_565 ? N1 Co1 N1S C1S 41.2(6) . . . 15_565 ? N1 Co1 N1S C1S -48.8(6) 15_565 . . 15_565 ? N1 Co1 N1 C7 174.29(15) 16_655 . . . ? N1 Co1 N1 C7 88.41(19) 2_665 . . . ? N1 Co1 N1 C7 2.5(2) 15_565 . . . ? N1S Co1 N1 C7 -91.59(19) . . . . ? N1 Co1 N1 C8 -2.1(2) 16_655 . . 16_655 ? N1 Co1 N1 C8 -87.94(19) 2_665 . . 16_655 ? N1 Co1 N1 C8 -173.82(15) 15_565 . . 16_655 ? N1S Co1 N1 C8 92.06(18) . . . 16_655 ? C6 C1 C2 C3 -2.6(4) . . . . ? C8 C1 C2 C3 172.3(3) 16_655 . . . ? C9 O1 C3 C2 3.9(4) . . . . ? C9 O1 C3 C4 -176.1(2) . . . . ? C1 C2 C3 O1 -178.1(2) . . . . ? C1 C2 C3 C4 1.9(4) . . . . ? C21B O2 C4 C5 7.8(6) . . . . ? C21A O2 C4 C5 4.4(5) . . . . ? C21B O2 C4 C3 -174.3(5) . . . . ? C21A O2 C4 C3 -177.7(4) . . . . ? O1 C3 C4 O2 1.9(3) . . . . ? C2 C3 C4 O2 -178.1(2) . . . . ? O1 C3 C4 C5 179.9(2) . . . . ? C2 C3 C4 C5 -0.2(4) . . . . ? O2 C4 C5 C6 176.9(2) . . . . ? C3 C4 C5 C6 -0.9(4) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C4 C5 C6 C7 -171.1(3) . . . . ? C2 C1 C6 C5 1.6(4) . . . . ? C8 C1 C6 C5 -174.6(2) 16_655 . . . ? C2 C1 C6 C7 174.8(2) . . . . ? C8 C1 C6 C7 -1.4(3) 16_655 . . . ? C8 N2 C7 N1 -1.3(4) . . . . ? C8 N2 C7 C6 174.3(2) . . . . ? C8 N1 C7 N2 175.5(2) 16_655 . . . ? Co1 N1 C7 N2 -1.4(4) . . . . ? C8 N1 C7 C6 -0.4(3) 16_655 . . . ? Co1 N1 C7 C6 -177.34(16) . . . . ? C5 C6 C7 N2 -2.9(4) . . . . ? C1 C6 C7 N2 -175.2(2) . . . . ? C5 C6 C7 N1 173.4(3) . . . . ? C1 C6 C7 N1 1.2(3) . . . . ? C7 N2 C8 N1 1.9(4) . . . 15_565 ? C7 N2 C8 C1 -173.9(2) . . . 15_565 ? C3 O1 C9 C14 -99.6(3) . . . . ? C3 O1 C9 C10 86.1(3) . . . . ? C14 C9 C10 C11 0.7(4) . . . . ? O1 C9 C10 C11 174.5(2) . . . . ? C14 C9 C10 C15 -176.5(3) . . . . ? O1 C9 C10 C15 -2.7(4) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? C15 C10 C11 C12 177.7(3) . . . . ? C10 C11 C12 C13 -0.1(6) . . . . ? C11 C12 C13 C14 -1.6(6) . . . . ? O1 C9 C14 C13 -175.9(2) . . . . ? C10 C9 C14 C13 -2.2(4) . . . . ? O1 C9 C14 C18 2.1(4) . . . . ? C10 C9 C14 C18 175.8(3) . . . . ? C12 C13 C14 C9 2.6(5) . . . . ? C12 C13 C14 C18 -175.3(3) . . . . ? C11 C10 C15 C17 21.0(4) . . . . ? C9 C10 C15 C17 -162.0(3) . . . . ? C11 C10 C15 C16 -102.1(3) . . . . ? C9 C10 C15 C16 74.9(3) . . . . ? C9 C14 C18 C19 156.6(4) . . . . ? C13 C14 C18 C19 -25.5(6) . . . . ? C9 C14 C18 C20 -78.8(4) . . . . ? C13 C14 C18 C20 99.0(4) . . . . ? C21B O2 C21A C22A -40(11) . . . . ? C4 O2 C21A C22A 98.7(5) . . . . ? C21B O2 C21A C26A 135(12) . . . . ? C4 O2 C21A C26A -87.0(5) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 174.0(8) . . . . ? C26A C21A C22A C27A 179.5(6) . . . . ? O2 C21A C22A C27A -6.5(7) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -179.4(7) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C24A C25A C26A C30 178.7(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -174.5(7) . . . . ? C22A C21A C26A C30 -178.5(7) . . . . ? O2 C21A C26A C30 7.1(6) . . . . ? C4 O2 C21B C22B 94.8(6) . . . . ? C21A O2 C21B C22B 138(12) . . . . ? C4 O2 C21B C26B -78.7(8) . . . . ? C21A O2 C21B C26B -35(11) . . . . ? O2 C21B C22B C23B -174.0(10) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 4.5(9) . . . . ? C26B C21B C22B C27B 178.5(9) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -178.5(8) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -178.3(10) . . . . ? O2 C21B C26B C25B 173.2(12) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -8.2(7) . . . . ? C22B C21B C26B C30 178.6(8) . . . . ? C21A C22A C27A C29A -152.0(7) . . . . ? C23A C22A C27A C29A 27.5(10) . . . . ? C21A C22A C27A C28A 77.9(7) . . . . ? C23A C22A C27A C28A -102.7(7) . . . . ? C23B C22B C27B C29B 77.0(13) . . . . ? C21B C22B C27B C29B -101.5(12) . . . . ? C23B C22B C27B C28B -60.1(12) . . . . ? C21B C22B C27B C28B 121.4(10) . . . . ? C25A C26A C30 C32B -70.8(10) . . . . ? C21A C26A C30 C32B 107.7(9) . . . . ? C25A C26A C30 C31 70.8(6) . . . . ? C21A C26A C30 C31 -110.7(5) . . . . ? C25A C26A C30 C32A -40.9(8) . . . . ? C21A C26A C30 C32A 137.6(8) . . . . ? C25A C26A C30 C26B -66(10) . . . . ? C21A C26A C30 C26B 113(10) . . . . ? C25B C26B C30 C26A 121(10) . . . . ? C21B C26B C30 C26A -58(10) . . . . ? C25B C26B C30 C32B -64.0(12) . . . . ? C21B C26B C30 C32B 117.5(8) . . . . ? C25B C26B C30 C31 76.3(9) . . . . ? C21B C26B C30 C31 -102.2(5) . . . . ? C25B C26B C30 C32A -34.6(11) . . . . ? C21B C26B C30 C32A 146.9(8) . . . . ? C1S N1S C1S C2S -58.7(11) 16_655 . . . ? C1S N1S C1S C2S 3.8(10) 2_665 . . . ? C1S N1S C1S C2S 66.2(10) 15_565 . . . ? Co1 N1S C1S C2S -176.2(10) . . . . ? C1S N1S C1S C1S 62.5(4) 2_665 . . 16_655 ? C1S N1S C1S C1S 124.9(7) 15_565 . . 16_655 ? Co1 N1S C1S C1S -117.5(4) . . . 16_655 ? C1S N1S C1S C1S -124.9(7) 16_655 . . 15_565 ? C1S N1S C1S C1S -62.5(4) 2_665 . . 15_565 ? Co1 N1S C1S C1S 117.5(4) . . . 15_565 ? N1S C1S C2S C3S -8(2) . . . . ? C1S C1S C2S C3S -50.7(15) 16_655 . . . ? C1S C1S C2S C3S 39.3(15) 15_565 . . . ? N1S C1S C2S C2S 38.9(16) . . . 16_655 ? C1S C1S C2S C2S -4.0(10) 16_655 . . 16_655 ? C1S C1S C2S C2S 85.9(11) 15_565 . . 16_655 ? N1S C1S C2S C2S -51.0(15) . . . 15_565 ? C1S C1S C2S C2S -94.0(10) 16_655 . . 15_565 ? C1S C1S C2S C2S -4.0(11) 15_565 . . 15_565 ? C1S C2S C3S C2S 67.3(12) . . . 16_655 ? C2S C2S C3S C2S 127.7(17) 15_565 . . 16_655 ? C1S C2S C3S C2S 3.5(9) . . . 2_665 ? C2S C2S C3S C2S -63.8(9) 16_655 . . 2_665 ? C2S C2S C3S C2S 63.8(9) 15_565 . . 2_665 ? C1S C2S C3S C2S -60.4(13) . . . 15_565 ? C2S C2S C3S C2S -127.7(17) 16_655 . . 15_565 ? C1S C2S C3S C4S -176.5(9) . . . . ? C2S C2S C3S C4S 116.2(9) 16_655 . . . ? C2S C2S C3S C4S -116.2(9) 15_565 . . . ? C2S C3S C4S C5S -27(3) 16_655 . . 2_665 ? C2S C3S C4S C5S -117(3) . . . 2_665 ? C2S C3S C4S C5S 63(3) 2_665 . . 2_665 ? C2S C3S C4S C5S 153(3) 15_565 . . 2_665 ? C2S C3S C4S C5S 63(3) 16_655 . . 16_655 ? C2S C3S C4S C5S -27(3) . . . 16_655 ? C2S C3S C4S C5S 153(3) 2_665 . . 16_655 ? C2S C3S C4S C5S -117(3) 15_565 . . 16_655 ? C2S C3S C4S C5S -117(3) 16_655 . . 15_565 ? C2S C3S C4S C5S 153(3) . . . 15_565 ? C2S C3S C4S C5S -27(3) 2_665 . . 15_565 ? C2S C3S C4S C5S 63(3) 15_565 . . 15_565 ? C2S C3S C4S C5S 153(3) 16_655 . . . ? C2S C3S C4S C5S 63(3) . . . . ? C2S C3S C4S C5S -117(3) 2_665 . . . ? C2S C3S C4S C5S -27(3) 15_565 . . . ? C3S C4S C5S C5S -108(2) . . . 16_655 ? C5S C4S C5S C5S 72(2) 2_665 . . 16_655 ? C5S C4S C5S C5S 145(4) 15_565 . . 16_655 ? C3S C4S C5S C5S 108(2) . . . 15_565 ? C5S C4S C5S C5S -72(2) 2_665 . . 15_565 ? C5S C4S C5S C5S -145(4) 16_655 . . 15_565 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.27 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.741 _refine_diff_density_min -0.790 _refine_diff_density_rms 0.080 data_PNC[cBr-Co3+-vBr] _database_code_depnum_ccdc_archive 'CCDC 900369' #TrackingRef '900369_PNC[cBr-Co3+-vBr].cif' _audit_update_record ; 2012-11-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130.83 H150.25 Br2 Cl4.25 Co N8 O9.42' _chemical_formula_weight 2354.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.627(4) _cell_length_b 37.627(4) _cell_length_c 37.627(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 53272(10) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 71633 _cell_measurement_theta_min 0.9085 _cell_measurement_theta_max 25.6926 _exptl_crystal_description block _exptl_crystal_colour green _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 0.881 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14830 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_absorpt_correction_T_min 0.467 _exptl_absorpt_correction_T_max 1.000 _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator Si111 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7813 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0312 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 24.21 _reflns_number_total 7813 _reflns_number_gt 6049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2009)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2009)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2009)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7813 _refine_ls_number_parameters 305 _refine_ls_number_restraints 311 _refine_ls_R_factor_all 0.1351 _refine_ls_R_factor_gt 0.1172 _refine_ls_wR_factor_ref 0.3724 _refine_ls_wR_factor_gt 0.3544 _refine_ls_goodness_of_fit_ref 1.471 _refine_ls_restrained_S_all 1.480 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.08494(3) 0.0358(4) Uani 1 4 d SU . . O1 O 0.88777(8) 0.59573(8) 0.11127(9) 0.0497(8) Uani 1 1 d U A . O2 O 0.83064(7) 0.56003(7) 0.11149(9) 0.0511(8) Uani 1 1 d U . . N1 N 0.77824(8) 0.70696(9) 0.08524(9) 0.0362(8) Uani 1 1 d U A . N2 N 0.73118(9) 0.66255(8) 0.08789(10) 0.0428(8) Uani 1 1 d U A . C1 C 0.82495(11) 0.66782(11) 0.09148(12) 0.0420(10) Uani 1 1 d U . . C2 C 0.85816(11) 0.65166(11) 0.09767(13) 0.0436(10) Uani 1 1 d U A . H2 H 0.8796 0.6650 0.0976 0.052 Uiso 1 1 calc R . . C3 C 0.85815(11) 0.61587(11) 0.10375(12) 0.0436(10) Uani 1 1 d U . . C4 C 0.82623(11) 0.59570(10) 0.10354(12) 0.0429(9) Uani 1 1 d U A . C5 C 0.79435(11) 0.61150(10) 0.09658(13) 0.0447(10) Uani 1 1 d U . . H5 H 0.7730 0.5980 0.0956 0.054 Uiso 1 1 calc R A . C6 C 0.79421(10) 0.64817(10) 0.09091(11) 0.0412(9) Uani 1 1 d U A . C7 C 0.76535(11) 0.67286(10) 0.08754(11) 0.0395(9) Uani 1 1 d U . . C8 C 0.70450(12) 0.68564(11) 0.08750(11) 0.0412(9) Uani 1 1 d U . . C9 C 0.92085(12) 0.61282(12) 0.11452(14) 0.0536(11) Uani 1 1 d U . . C10 C 0.93020(13) 0.62717(12) 0.14684(15) 0.0618(12) Uani 1 1 d U A . C11 C 0.96404(15) 0.64092(16) 0.1499(2) 0.0807(17) Uani 1 1 d U . . H11 H 0.9714 0.6511 0.1718 0.097 Uiso 1 1 calc R A . C12 C 0.98656(16) 0.64022(18) 0.1227(2) 0.091(2) Uani 1 1 d U A . H12 H 1.0097 0.6497 0.1260 0.109 Uiso 1 1 calc R . . C13 C 0.97820(15) 0.62689(19) 0.0909(2) 0.0886(19) Uani 1 1 d U . . H13 H 0.9951 0.6277 0.0722 0.106 Uiso 1 1 calc R A . C14 C 0.94333(14) 0.61099(15) 0.08453(16) 0.0690(14) Uani 1 1 d U A . C15 C 0.90367(15) 0.62588(14) 0.17773(16) 0.0684(13) Uani 1 1 d U . . H15 H 0.8797 0.6321 0.1681 0.082 Uiso 1 1 calc R A . C16 C 0.9017(2) 0.58784(17) 0.19269(19) 0.0807(18) Uani 1 1 d U A . H16A H 0.8949 0.5714 0.1737 0.121 Uiso 1 1 calc R . . H16B H 0.8839 0.5869 0.2117 0.121 Uiso 1 1 calc R . . H16C H 0.9249 0.5810 0.2022 0.121 Uiso 1 1 calc R . . C17 C 0.9119(2) 0.65163(18) 0.2089(2) 0.101(2) Uani 1 1 d U A . H17A H 0.9293 0.6406 0.2249 0.151 Uiso 1 1 calc R . . H17B H 0.8900 0.6567 0.2220 0.151 Uiso 1 1 calc R . . H17C H 0.9217 0.6738 0.1995 0.151 Uiso 1 1 calc R . . C18 C 0.93182(19) 0.59336(18) 0.05068(18) 0.0848(17) Uani 1 1 d U . . H18 H 0.9058 0.5980 0.0478 0.102 Uiso 1 1 calc R A . C19 C 0.9505(3) 0.6074(3) 0.0170(3) 0.157(4) Uani 1 1 d U A . H19A H 0.9501 0.5891 -0.0014 0.235 Uiso 1 1 calc R . . H19B H 0.9751 0.6135 0.0227 0.235 Uiso 1 1 calc R . . H19C H 0.9380 0.6286 0.0085 0.235 Uiso 1 1 calc R . . C20 C 0.9364(2) 0.5537(2) 0.0549(3) 0.108(3) Uani 1 1 d U A . H20A H 0.9284 0.5417 0.0332 0.162 Uiso 1 1 calc R . . H20B H 0.9221 0.5454 0.0751 0.162 Uiso 1 1 calc R . . H20C H 0.9615 0.5482 0.0592 0.162 Uiso 1 1 calc R . . C21A C 0.8000(2) 0.5383(3) 0.1076(2) 0.037(6) Uiso 0.433(13) 1 d PGU A 1 C22A C 0.7899(3) 0.5164(3) 0.0796(2) 0.079(4) Uiso 0.433(13) 1 d PGDU A 1 C23A C 0.7596(3) 0.4956(2) 0.0824(2) 0.064(3) Uiso 0.433(13) 1 d PGU A 1 H23A H 0.7527 0.4806 0.0633 0.077 Uiso 0.433(13) 1 calc PR A 1 C24A C 0.7393(2) 0.4966(2) 0.1133(3) 0.069(4) Uiso 0.433(13) 1 d PGU A 1 H24A H 0.7186 0.4823 0.1153 0.082 Uiso 0.433(13) 1 calc PR A 1 C25A C 0.7495(2) 0.5185(2) 0.1413(2) 0.054(3) Uiso 0.433(13) 1 d PGU A 1 H25A H 0.7356 0.5191 0.1625 0.065 Uiso 0.433(13) 1 calc PR A 1 C26A C 0.7798(2) 0.5393(3) 0.1385(2) 0.054(4) Uiso 0.433(13) 1 d PGDU A 1 C21B C 0.8014(2) 0.5397(2) 0.1092(2) 0.056(6) Uiso 0.567(13) 1 d PGU A 2 C22B C 0.79937(19) 0.5219(2) 0.07685(17) 0.048(2) Uiso 0.567(13) 1 d PGDU A 2 C23B C 0.7702(2) 0.50058(19) 0.0693(2) 0.078(3) Uiso 0.567(13) 1 d PGU A 2 H23B H 0.7688 0.4884 0.0472 0.093 Uiso 0.567(13) 1 calc PR A 2 C24B C 0.74298(17) 0.4971(2) 0.0941(3) 0.085(4) Uiso 0.567(13) 1 d PGU A 2 H24B H 0.7230 0.4825 0.0889 0.102 Uiso 0.567(13) 1 calc PR A 2 C25B C 0.74500(18) 0.5149(2) 0.1264(2) 0.072(3) Uiso 0.567(13) 1 d PGU A 2 H25B H 0.7264 0.5124 0.1433 0.087 Uiso 0.567(13) 1 calc PR A 2 C26B C 0.7742(2) 0.5362(2) 0.13392(17) 0.062(3) Uiso 0.567(13) 1 d PGDU A 2 C27A C 0.8149(4) 0.5195(4) 0.0485(3) 0.077(4) Uiso 0.433(13) 1 d PDU A 1 H27A H 0.8227 0.5449 0.0502 0.092 Uiso 0.433(13) 1 calc PR A 1 C28A C 0.8505(4) 0.4998(5) 0.0486(5) 0.086(5) Uiso 0.433(13) 1 d PDU A 1 H28D H 0.8580 0.4954 0.0240 0.130 Uiso 0.433(13) 1 calc PR A 1 H28E H 0.8478 0.4771 0.0610 0.130 Uiso 0.433(13) 1 calc PR A 1 H28F H 0.8684 0.5142 0.0607 0.130 Uiso 0.433(13) 1 calc PR A 1 C29A C 0.7964(7) 0.5188(7) 0.0133(5) 0.147(9) Uiso 0.433(13) 1 d PDU A 1 H29A H 0.7882 0.5428 0.0073 0.221 Uiso 0.433(13) 1 calc PR A 1 H29B H 0.7759 0.5028 0.0146 0.221 Uiso 0.433(13) 1 calc PR A 1 H29C H 0.8128 0.5104 -0.0050 0.221 Uiso 0.433(13) 1 calc PR A 1 C27B C 0.8278(3) 0.5247(3) 0.0481(3) 0.070(3) Uiso 0.567(13) 1 d PDU A 2 H27B H 0.8480 0.5371 0.0600 0.084 Uiso 0.567(13) 1 calc PR A 2 C28B C 0.8422(4) 0.4881(3) 0.0395(4) 0.089(4) Uiso 0.567(13) 1 d PDU A 2 H28A H 0.8666 0.4902 0.0307 0.134 Uiso 0.567(13) 1 calc PR A 2 H28B H 0.8274 0.4770 0.0213 0.134 Uiso 0.567(13) 1 calc PR A 2 H28C H 0.8420 0.4734 0.0610 0.134 Uiso 0.567(13) 1 calc PR A 2 C29B C 0.8197(6) 0.5472(5) 0.0167(4) 0.151(7) Uiso 0.567(13) 1 d PDU A 2 H29D H 0.8074 0.5689 0.0244 0.227 Uiso 0.567(13) 1 calc PR A 2 H29E H 0.8044 0.5340 0.0002 0.227 Uiso 0.567(13) 1 calc PR A 2 H29F H 0.8418 0.5537 0.0046 0.227 Uiso 0.567(13) 1 calc PR A 2 C30 C 0.78171(19) 0.55845(17) 0.17018(16) 0.098(2) Uani 1 1 d DU . . H30 H 0.7962 0.5805 0.1665 0.117 Uiso 1 1 calc R A 1 C31 C 0.7971(2) 0.5372(2) 0.2003(3) 0.121(3) Uani 1 1 d U A . H31A H 0.7797 0.5196 0.2083 0.181 Uiso 1 1 calc R . . H31B H 0.8030 0.5532 0.2200 0.181 Uiso 1 1 calc R . . H31C H 0.8187 0.5251 0.1922 0.181 Uiso 1 1 calc R . . C32A C 0.7443(3) 0.5686(5) 0.1824(4) 0.109(6) Uiso 0.58(2) 1 d PDU A 1 H32A H 0.7282 0.5485 0.1788 0.163 Uiso 0.58(2) 1 calc PR A 1 H32B H 0.7359 0.5891 0.1686 0.163 Uiso 0.58(2) 1 calc PR A 1 H32C H 0.7448 0.5749 0.2077 0.163 Uiso 0.58(2) 1 calc PR A 1 C32B C 0.7604(5) 0.5903(4) 0.1821(5) 0.087(6) Uiso 0.42(2) 1 d PDU A 2 H32D H 0.7673 0.5967 0.2063 0.131 Uiso 0.42(2) 1 calc PR A 2 H32E H 0.7351 0.5845 0.1815 0.131 Uiso 0.42(2) 1 calc PR A 2 H32F H 0.7651 0.6103 0.1661 0.131 Uiso 0.42(2) 1 calc PR A 2 Br1 Br 0.7500 0.7500 0.14811(3) 0.0544(4) Uani 1 4 d SU . . Br2 Br 0.7500 0.7500 0.02162(5) 0.0918(6) Uani 1 4 d SU . . 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 0.0283(4) 0.0283(4) 0.0507(7) 0.000 0.000 0.000 O1 0.0300(15) 0.0397(17) 0.079(2) 0.0062(14) -0.0092(13) 0.0059(11) O2 0.0338(16) 0.0297(15) 0.090(2) 0.0081(13) -0.0057(13) 0.0024(11) N1 0.0274(17) 0.0321(17) 0.049(2) -0.0007(14) -0.0022(13) -0.0005(12) N2 0.0342(19) 0.0283(17) 0.066(2) 0.0005(14) -0.0010(15) -0.0005(13) C1 0.034(2) 0.036(2) 0.057(3) 0.0006(17) -0.0006(17) 0.0025(16) C2 0.037(2) 0.034(2) 0.059(3) 0.0000(18) -0.0037(18) 0.0008(16) C3 0.037(2) 0.039(2) 0.056(3) 0.0014(17) -0.0055(18) 0.0044(16) C4 0.039(2) 0.031(2) 0.059(3) 0.0042(17) -0.0047(18) 0.0036(15) C5 0.030(2) 0.034(2) 0.070(3) -0.0003(18) -0.0020(18) 0.0006(15) C6 0.034(2) 0.031(2) 0.058(3) -0.0011(17) -0.0026(17) 0.0008(15) C7 0.035(2) 0.031(2) 0.053(2) -0.0009(16) -0.0071(17) -0.0026(15) C8 0.040(2) 0.031(2) 0.053(3) 0.0026(16) -0.0034(18) -0.0017(16) C9 0.033(2) 0.047(3) 0.081(3) 0.020(2) -0.011(2) 0.0013(17) C10 0.055(3) 0.041(3) 0.090(3) 0.015(2) -0.028(2) -0.0009(19) C11 0.056(3) 0.065(4) 0.121(5) 0.033(3) -0.033(3) -0.017(3) C12 0.046(3) 0.089(4) 0.137(5) 0.054(4) -0.032(3) -0.011(3) C13 0.039(3) 0.104(5) 0.122(5) 0.052(4) 0.007(3) 0.005(3) C14 0.045(3) 0.073(3) 0.089(4) 0.027(3) -0.003(2) 0.008(2) C15 0.070(3) 0.056(3) 0.080(4) 0.002(2) -0.014(3) 0.000(2) C16 0.092(5) 0.070(4) 0.081(4) 0.014(3) 0.008(3) -0.001(3) C17 0.131(6) 0.073(4) 0.099(5) -0.013(3) -0.036(4) 0.007(4) C18 0.072(4) 0.090(4) 0.093(4) 0.017(3) 0.017(3) 0.020(3) C19 0.195(11) 0.179(10) 0.096(6) 0.018(6) 0.048(7) -0.021(8) C20 0.114(6) 0.086(4) 0.123(7) -0.001(4) -0.001(5) 0.019(4) C30 0.113(6) 0.078(4) 0.102(5) 0.020(4) 0.031(4) 0.044(4) C31 0.106(6) 0.116(7) 0.139(7) 0.044(5) -0.009(5) 0.011(5) Br1 0.0537(5) 0.0537(5) 0.0557(7) 0.000 0.000 0.000 Br2 0.0884(7) 0.0884(7) 0.0987(11) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.937(3) . ? Co1 N1 1.937(3) 15_565 ? Co1 N1 1.937(3) 16_655 ? Co1 N1 1.937(3) 2_665 ? Co1 Br1 2.3767(15) . ? Co1 Br2 2.383(2) . ? O1 C3 1.377(5) . ? O1 C9 1.407(5) . ? O2 C21B 1.343(6) . ? O2 C4 1.385(5) . ? O2 C21A 1.420(7) . ? N1 C8 1.365(5) 16_655 ? N1 C7 1.374(5) . ? N2 C8 1.328(6) . ? N2 C7 1.343(6) . ? C1 C6 1.373(6) . ? C1 C2 1.409(6) . ? C1 C8 1.444(6) 16_655 ? C2 C3 1.366(6) . ? C2 H2 0.9500 . ? C3 C4 1.421(6) . ? C4 C5 1.364(6) . ? C5 C6 1.396(6) . ? C5 H5 0.9500 . ? C6 C7 1.435(6) . ? C8 N1 1.365(5) 15_565 ? C8 C1 1.444(6) 15_565 ? C9 C10 1.376(7) . ? C9 C14 1.412(7) . ? C10 C11 1.379(7) . ? C10 C15 1.533(8) . ? C11 C12 1.328(10) . ? C11 H11 0.9500 . ? C12 C13 1.334(11) . ? C12 H12 0.9500 . ? C13 C14 1.462(9) . ? C13 H13 0.9500 . ? C14 C18 1.500(9) . ? C15 C16 1.540(8) . ? C15 C17 1.553(8) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.512(10) . ? C18 C19 1.541(10) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.504(9) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.396(7) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.526(8) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.626(7) . ? C27A C29A 1.498(10) . ? C27A C28A 1.530(9) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.486(9) . ? C27B C28B 1.515(9) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.502(10) . ? C30 C32B 1.508(9) . ? C30 C32A 1.531(9) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 N1 Co1 N1 90.003(2) . 15_565 ? N1 Co1 N1 89.998(2) . 16_655 ? N1 Co1 N1 179.3(2) 15_565 16_655 ? N1 Co1 N1 179.3(2) . 2_665 ? N1 Co1 N1 89.990(2) 15_565 2_665 ? N1 Co1 N1 90.001(2) 16_655 2_665 ? N1 Co1 Br1 89.66(10) . . ? N1 Co1 Br1 89.66(10) 15_565 . ? N1 Co1 Br1 89.66(10) 16_655 . ? N1 Co1 Br1 89.66(10) 2_665 . ? N1 Co1 Br2 90.34(10) . . ? N1 Co1 Br2 90.34(10) 15_565 . ? N1 Co1 Br2 90.34(10) 16_655 . ? N1 Co1 Br2 90.34(10) 2_665 . ? Br1 Co1 Br2 180.0 . . ? C3 O1 C9 118.8(3) . . ? C21B O2 C4 116.0(6) . . ? C21B O2 C21A 2.3(6) . . ? C4 O2 C21A 116.0(6) . . ? C8 N1 C7 106.5(3) 16_655 . ? C8 N1 Co1 127.1(3) 16_655 . ? C7 N1 Co1 126.0(3) . . ? C8 N2 C7 122.3(3) . . ? C6 C1 C2 121.1(4) . . ? C6 C1 C8 106.3(4) . 16_655 ? C2 C1 C8 132.4(4) . 16_655 ? C3 C2 C1 116.9(4) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C2 C3 O1 125.2(4) . . ? C2 C3 C4 121.7(4) . . ? O1 C3 C4 113.0(4) . . ? C5 C4 O2 124.7(4) . . ? C5 C4 C3 120.8(4) . . ? O2 C4 C3 114.5(3) . . ? C4 C5 C6 117.6(4) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C1 C6 C5 121.8(4) . . ? C1 C6 C7 106.9(4) . . ? C5 C6 C7 131.0(4) . . ? N2 C7 N1 127.5(4) . . ? N2 C7 C6 122.5(3) . . ? N1 C7 C6 110.1(3) . . ? N2 C8 N1 127.0(4) . 15_565 ? N2 C8 C1 122.7(4) . 15_565 ? N1 C8 C1 110.2(4) 15_565 15_565 ? C10 C9 O1 118.9(4) . . ? C10 C9 C14 124.9(5) . . ? O1 C9 C14 116.0(5) . . ? C9 C10 C11 117.1(6) . . ? C9 C10 C15 119.4(4) . . ? C11 C10 C15 123.4(5) . . ? C12 C11 C10 121.2(7) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 123.1(6) . . ? C11 C12 H12 118.4 . . ? C13 C12 H12 118.4 . . ? C12 C13 C14 120.9(6) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C9 C14 C13 112.7(6) . . ? C9 C14 C18 121.8(5) . . ? C13 C14 C18 125.5(6) . . ? C10 C15 C16 109.8(5) . . ? C10 C15 C17 115.0(5) . . ? C16 C15 C17 108.3(5) . . ? C10 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C20 108.4(6) . . ? C14 C18 C19 114.5(7) . . ? C20 C18 C19 112.0(7) . . ? C14 C18 H18 107.2 . . ? C20 C18 H18 107.2 . . ? C19 C18 H18 107.2 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 129.9(6) . . ? C26A C21A O2 110.0(6) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 111.8(8) . . ? C23A C22A C27A 128.2(8) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A C30 105.5(7) . . ? C21A C26A C30 134.5(7) . . ? O2 C21B C22B 112.1(5) . . ? O2 C21B C26B 127.9(5) . . ? C22B C21B C26B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B C27B 123.3(6) . . ? C23B C22B C27B 116.7(6) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 127.3(6) . . ? C21B C26B C30 112.7(6) . . ? C29A C27A C22A 113.2(14) . . ? C29A C27A C28A 113.6(14) . . ? C22A C27A C28A 120.6(12) . . ? C29A C27A H27A 102.0 . . ? C22A C27A H27A 102.0 . . ? C28A C27A H27A 102.0 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 115.1(12) . . ? C29B C27B C22B 117.4(11) . . ? C28B C27B C22B 109.8(9) . . ? C29B C27B H27B 104.3 . . ? C28B C27B H27B 104.3 . . ? C22B C27B H27B 104.3 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 113.0(8) . . ? C26A C30 C32B 129.5(10) . . ? C31 C30 C32B 113.8(9) . . ? C26A C30 C32A 109.8(9) . . ? C31 C30 C32A 105.2(8) . . ? C32B C30 C32A 39.1(9) . . ? C26A C30 C26B 7.1(6) . . ? C31 C30 C26B 115.2(7) . . ? C32B C30 C26B 124.5(9) . . ? C32A C30 C26B 102.8(8) . . ? C26A C30 H30 109.6 . . ? C31 C30 H30 109.6 . . ? C32B C30 H30 70.9 . . ? C32A C30 H30 109.6 . . ? C26B C30 H30 113.8 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C8 -175.5(3) 15_565 . . 16_655 ? N1 Co1 N1 C8 3.9(4) 16_655 . . 16_655 ? N1 Co1 N1 C8 -86.0(3) 2_665 . . 16_655 ? Br1 Co1 N1 C8 -85.8(3) . . . 16_655 ? Br2 Co1 N1 C8 94.2(3) . . . 16_655 ? N1 Co1 N1 C7 -3.9(4) 15_565 . . . ? N1 Co1 N1 C7 175.5(3) 16_655 . . . ? N1 Co1 N1 C7 85.6(4) 2_665 . . . ? Br1 Co1 N1 C7 85.8(3) . . . . ? Br2 Co1 N1 C7 -94.2(3) . . . . ? C6 C1 C2 C3 -1.3(7) . . . . ? C8 C1 C2 C3 173.3(5) 16_655 . . . ? C1 C2 C3 O1 -178.1(4) . . . . ? C1 C2 C3 C4 0.6(7) . . . . ? C9 O1 C3 C2 2.7(7) . . . . ? C9 O1 C3 C4 -176.0(4) . . . . ? C21B O2 C4 C5 5.6(7) . . . . ? C21A O2 C4 C5 8.2(7) . . . . ? C21B O2 C4 C3 -175.6(5) . . . . ? C21A O2 C4 C3 -173.1(5) . . . . ? C2 C3 C4 C5 1.2(7) . . . . ? O1 C3 C4 C5 180.0(4) . . . . ? C2 C3 C4 O2 -177.7(4) . . . . ? O1 C3 C4 O2 1.1(6) . . . . ? O2 C4 C5 C6 176.6(4) . . . . ? C3 C4 C5 C6 -2.1(7) . . . . ? C2 C1 C6 C5 0.3(7) . . . . ? C8 C1 C6 C5 -175.6(4) 16_655 . . . ? C2 C1 C6 C7 174.4(4) . . . . ? C8 C1 C6 C7 -1.4(5) 16_655 . . . ? C4 C5 C6 C1 1.4(7) . . . . ? C4 C5 C6 C7 -171.1(4) . . . . ? C8 N2 C7 N1 -3.0(6) . . . . ? C8 N2 C7 C6 174.7(4) . . . . ? C8 N1 C7 N2 177.3(4) 16_655 . . . ? Co1 N1 C7 N2 4.3(6) . . . . ? C8 N1 C7 C6 -0.7(5) 16_655 . . . ? Co1 N1 C7 C6 -173.7(3) . . . . ? C1 C6 C7 N2 -176.7(4) . . . . ? C5 C6 C7 N2 -3.3(7) . . . . ? C1 C6 C7 N1 1.4(5) . . . . ? C5 C6 C7 N1 174.7(4) . . . . ? C7 N2 C8 N1 2.9(7) . . . 15_565 ? C7 N2 C8 C1 -173.6(4) . . . 15_565 ? C3 O1 C9 C10 85.5(5) . . . . ? C3 O1 C9 C14 -99.9(5) . . . . ? O1 C9 C10 C11 174.4(4) . . . . ? C14 C9 C10 C11 0.4(7) . . . . ? O1 C9 C10 C15 -3.2(6) . . . . ? C14 C9 C10 C15 -177.2(5) . . . . ? C9 C10 C11 C12 -0.1(8) . . . . ? C15 C10 C11 C12 177.4(5) . . . . ? C10 C11 C12 C13 0.9(9) . . . . ? C11 C12 C13 C14 -1.9(10) . . . . ? C10 C9 C14 C13 -1.3(7) . . . . ? O1 C9 C14 C13 -175.5(4) . . . . ? C10 C9 C14 C18 177.0(5) . . . . ? O1 C9 C14 C18 2.8(7) . . . . ? C12 C13 C14 C9 2.0(8) . . . . ? C12 C13 C14 C18 -176.2(6) . . . . ? C9 C10 C15 C16 74.4(6) . . . . ? C11 C10 C15 C16 -103.1(6) . . . . ? C9 C10 C15 C17 -163.2(5) . . . . ? C11 C10 C15 C17 19.3(7) . . . . ? C9 C14 C18 C20 -80.4(7) . . . . ? C13 C14 C18 C20 97.6(7) . . . . ? C9 C14 C18 C19 153.8(7) . . . . ? C13 C14 C18 C19 -28.1(9) . . . . ? C21B O2 C21A C22A -170(26) . . . . ? C4 O2 C21A C22A 98.0(8) . . . . ? C21B O2 C21A C26A 6(25) . . . . ? C4 O2 C21A C26A -85.9(6) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 175.8(12) . . . . ? C26A C21A C22A C27A 179.2(10) . . . . ? O2 C21A C22A C27A -5.0(11) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -179.1(12) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C24A C25A C26A C30 178.3(9) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -176.6(9) . . . . ? C22A C21A C26A C30 -177.8(12) . . . . ? O2 C21A C26A C30 5.7(10) . . . . ? C4 O2 C21B C22B 97.3(6) . . . . ? C21A O2 C21B C22B 8(25) . . . . ? C4 O2 C21B C26B -80.2(7) . . . . ? C21A O2 C21B C26B -169(25) . . . . ? O2 C21B C22B C23B -177.8(9) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 1.4(8) . . . . ? C26B C21B C22B C27B 179.2(8) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -179.3(7) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -178.9(9) . . . . ? O2 C21B C26B C25B 177.4(10) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -3.6(7) . . . . ? C22B C21B C26B C30 179.0(8) . . . . ? C21A C22A C27A C29A -140.9(14) . . . . ? C23A C22A C27A C29A 38.3(19) . . . . ? C21A C22A C27A C28A 79.8(17) . . . . ? C23A C22A C27A C28A -101.0(17) . . . . ? C21B C22B C27B C29B -104.0(13) . . . . ? C23B C22B C27B C29B 75.3(14) . . . . ? C21B C22B C27B C28B 122.1(10) . . . . ? C23B C22B C27B C28B -58.6(12) . . . . ? C25A C26A C30 C31 80.5(8) . . . . ? C21A C26A C30 C31 -101.5(10) . . . . ? C25A C26A C30 C32B -76.0(14) . . . . ? C21A C26A C30 C32B 102.0(14) . . . . ? C25A C26A C30 C32A -36.5(11) . . . . ? C21A C26A C30 C32A 141.5(10) . . . . ? C25A C26A C30 C26B -29(6) . . . . ? C21A C26A C30 C26B 149(7) . . . . ? C25B C26B C30 C26A 155(7) . . . . ? C21B C26B C30 C26A -24(6) . . . . ? C25B C26B C30 C31 81.5(9) . . . . ? C21B C26B C30 C31 -97.4(7) . . . . ? C25B C26B C30 C32B -68.2(13) . . . . ? C21B C26B C30 C32B 112.9(11) . . . . ? C25B C26B C30 C32A -32.3(11) . . . . ? C21B C26B C30 C32A 148.8(8) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.869 _refine_diff_density_min -2.580 _refine_diff_density_rms 0.116 data_PNC[cBr0.51-Co3+-vBr0.36] _database_code_depnum_ccdc_archive 'CCDC 900370' #TrackingRef '900370_PNC[cBr0.51-Co3+-vBr0.36].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130.83 H155.08 Br0.88 Cl4.25 Co N8 O11.42' _chemical_formula_weight 2302.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n _symmetry_space_group_name_Hall -P4a2bc3 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.2791(3) _cell_length_b 37.2791(3) _cell_length_c 37.2791(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 51807.9(7) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 24913 _cell_measurement_theta_min 1.5883 _cell_measurement_theta_max 24.5156 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.885 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14609 _exptl_absorpt_coefficient_mu 0.412 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9817 _exptl_absorpt_correction_T_max 0.9817 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7625 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.20 _reflns_number_total 7625 _reflns_number_gt 5329 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; ? ; _computing_cell_refinement ; ? ; _computing_data_reduction ; ? ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7625 _refine_ls_number_parameters 313 _refine_ls_number_restraints 305 _refine_ls_R_factor_all 0.1228 _refine_ls_R_factor_gt 0.1025 _refine_ls_wR_factor_ref 0.3473 _refine_ls_wR_factor_gt 0.3268 _refine_ls_goodness_of_fit_ref 1.375 _refine_ls_restrained_S_all 1.452 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.08162(3) 0.0522(4) Uani 1 4 d SU . . O1 O 0.88907(7) 0.59498(7) 0.11033(8) 0.0749(8) Uani 1 1 d U A . O2 O 0.83144(7) 0.55939(6) 0.10994(9) 0.0791(9) Uani 1 1 d U . . N1 N 0.77829(7) 0.70695(7) 0.08226(8) 0.0555(7) Uani 1 1 d U A . N2 N 0.73155(7) 0.66176(7) 0.08485(8) 0.0607(8) Uani 1 1 d U A . C1 C 0.82597(9) 0.66756(9) 0.08853(11) 0.0607(9) Uani 1 1 d U . . C2 C 0.85917(10) 0.65147(10) 0.09556(11) 0.0650(10) Uani 1 1 d U A . H2 H 0.8808 0.6650 0.0958 0.078 Uiso 1 1 calc R . . C3 C 0.85901(9) 0.61529(10) 0.10209(11) 0.0669(10) Uani 1 1 d U . . C4 C 0.82733(10) 0.59501(10) 0.10134(12) 0.0702(10) Uani 1 1 d U A . C5 C 0.79460(10) 0.61076(9) 0.09411(12) 0.0697(10) Uani 1 1 d U . . H5 H 0.7731 0.5971 0.0934 0.084 Uiso 1 1 calc R A . C6 C 0.79459(9) 0.64764(9) 0.08781(11) 0.0637(9) Uani 1 1 d U A . C7 C 0.76548(9) 0.67233(9) 0.08404(10) 0.0584(8) Uani 1 1 d U . . C8 C 0.70449(9) 0.68500(9) 0.08443(10) 0.0569(8) Uani 1 1 d U . . C9 C 0.92217(11) 0.61298(12) 0.11339(15) 0.0852(12) Uani 1 1 d U . . C10 C 0.93115(12) 0.62783(12) 0.14666(16) 0.0929(13) Uani 1 1 d U A . C11 C 0.96512(15) 0.64155(16) 0.1498(2) 0.128(2) Uani 1 1 d U . . H11 H 0.9722 0.6510 0.1724 0.153 Uiso 1 1 calc R A . C12 C 0.98781(17) 0.6424(2) 0.1240(3) 0.153(3) Uani 1 1 d U A . H12 H 1.0106 0.6532 0.1276 0.184 Uiso 1 1 calc R . . C13 C 0.97925(16) 0.6275(2) 0.0906(2) 0.151(3) Uani 1 1 d U . . H13 H 0.9965 0.6277 0.0719 0.181 Uiso 1 1 calc R A . C14 C 0.94492(14) 0.61205(17) 0.08453(17) 0.1113(16) Uani 1 1 d U A . C15 C 0.90441(14) 0.62607(12) 0.17757(14) 0.0945(14) Uani 1 1 d U . . H15 H 0.8802 0.6322 0.1677 0.113 Uiso 1 1 calc R A . C16 C 0.90238(16) 0.58873(13) 0.19281(16) 0.0992(15) Uani 1 1 d U A . H16A H 0.8956 0.5719 0.1738 0.149 Uiso 1 1 calc R . . H16B H 0.8844 0.5881 0.2120 0.149 Uiso 1 1 calc R . . H16C H 0.9258 0.5820 0.2025 0.149 Uiso 1 1 calc R . . C17 C 0.9125(2) 0.65229(15) 0.2077(2) 0.144(3) Uani 1 1 d U A . H17A H 0.9300 0.6416 0.2242 0.216 Uiso 1 1 calc R . . H17B H 0.8903 0.6577 0.2207 0.216 Uiso 1 1 calc R . . H17C H 0.9223 0.6745 0.1976 0.216 Uiso 1 1 calc R . . C18 C 0.9346(2) 0.5949(2) 0.0501(2) 0.138(2) Uani 1 1 d U . . H18 H 0.9083 0.5991 0.0470 0.165 Uiso 1 1 calc R A . C19 C 0.9525(3) 0.6084(3) 0.0167(3) 0.209(5) Uani 1 1 d U A . H19A H 0.9521 0.5897 -0.0017 0.314 Uiso 1 1 calc R . . H19B H 0.9774 0.6148 0.0221 0.314 Uiso 1 1 calc R . . H19C H 0.9397 0.6296 0.0079 0.314 Uiso 1 1 calc R . . C20 C 0.9399(2) 0.5546(2) 0.0502(3) 0.176(4) Uani 1 1 d U A . H20A H 0.9203 0.5432 0.0633 0.264 Uiso 1 1 calc R . . H20B H 0.9628 0.5489 0.0618 0.264 Uiso 1 1 calc R . . H20C H 0.9403 0.5458 0.0254 0.264 Uiso 1 1 calc R . . C21A C 0.79921(13) 0.53876(15) 0.11259(16) 0.055(2) Uiso 0.497(9) 1 d PGU A 1 C22A C 0.78958(17) 0.51746(17) 0.08355(15) 0.083(3) Uiso 0.497(9) 1 d PGDU A 1 C23A C 0.75879(18) 0.49649(17) 0.08520(18) 0.091(3) Uiso 0.497(9) 1 d PGU A 1 H23A H 0.7522 0.4819 0.0654 0.109 Uiso 0.497(9) 1 calc PR A 1 C24A C 0.73763(14) 0.49684(17) 0.1159(2) 0.094(3) Uiso 0.497(9) 1 d PGU A 1 H24A H 0.7166 0.4825 0.1170 0.113 Uiso 0.497(9) 1 calc PR A 1 C25A C 0.74726(14) 0.51815(17) 0.14494(18) 0.081(3) Uiso 0.497(9) 1 d PGU A 1 H25A H 0.7328 0.5184 0.1659 0.097 Uiso 0.497(9) 1 calc PR A 1 C26A C 0.77805(14) 0.53911(15) 0.14329(15) 0.062(2) Uiso 0.497(9) 1 d PGDU A 1 C21B C 0.80326(14) 0.53983(17) 0.10319(19) 0.078(3) Uiso 0.503(9) 1 d PGU A 2 C22B C 0.79924(16) 0.52103(18) 0.07125(17) 0.079(2) Uiso 0.503(9) 1 d PGDU A 2 C23B C 0.76903(19) 0.49988(17) 0.06574(18) 0.096(3) Uiso 0.503(9) 1 d PGU A 2 H23B H 0.7663 0.4870 0.0439 0.116 Uiso 0.503(9) 1 calc PR A 2 C24B C 0.74284(16) 0.49753(18) 0.0922(2) 0.099(3) Uiso 0.503(9) 1 d PGU A 2 H24B H 0.7222 0.4831 0.0884 0.118 Uiso 0.503(9) 1 calc PR A 2 C25B C 0.74687(15) 0.51633(19) 0.1241(2) 0.092(3) Uiso 0.503(9) 1 d PGU A 2 H25B H 0.7290 0.5147 0.1422 0.110 Uiso 0.503(9) 1 calc PR A 2 C26B C 0.77708(16) 0.53748(17) 0.12963(17) 0.077(2) Uiso 0.503(9) 1 d PGDU A 2 C27A C 0.8123(3) 0.5186(3) 0.0496(2) 0.097(3) Uiso 0.497(9) 1 d PDU A 1 H27A H 0.8190 0.5446 0.0498 0.116 Uiso 0.497(9) 1 calc PR A 1 C28A C 0.8501(3) 0.5021(4) 0.0524(4) 0.128(5) Uiso 0.497(9) 1 d PDU A 1 H28D H 0.8591 0.4967 0.0283 0.191 Uiso 0.497(9) 1 calc PR A 1 H28E H 0.8489 0.4799 0.0664 0.191 Uiso 0.497(9) 1 calc PR A 1 H28F H 0.8663 0.5191 0.0642 0.191 Uiso 0.497(9) 1 calc PR A 1 C29A C 0.8004(6) 0.5154(7) 0.0108(4) 0.196(8) Uiso 0.497(9) 1 d PDU A 1 H29A H 0.7913 0.5386 0.0025 0.295 Uiso 0.497(9) 1 calc PR A 1 H29B H 0.7815 0.4973 0.0089 0.295 Uiso 0.497(9) 1 calc PR A 1 H29C H 0.8209 0.5082 -0.0041 0.295 Uiso 0.497(9) 1 calc PR A 1 C27B C 0.8279(3) 0.5258(3) 0.0432(2) 0.088(3) Uiso 0.503(9) 1 d PDU A 2 H27B H 0.8464 0.5422 0.0536 0.106 Uiso 0.503(9) 1 calc PR A 2 C28B C 0.8447(4) 0.4901(3) 0.0395(5) 0.133(5) Uiso 0.503(9) 1 d PDU A 2 H28A H 0.8696 0.4929 0.0315 0.200 Uiso 0.503(9) 1 calc PR A 2 H28B H 0.8314 0.4760 0.0218 0.200 Uiso 0.503(9) 1 calc PR A 2 H28C H 0.8443 0.4777 0.0627 0.200 Uiso 0.503(9) 1 calc PR A 2 C29B C 0.8129(7) 0.5440(7) 0.0110(5) 0.208(9) Uiso 0.503(9) 1 d PDU A 2 H29D H 0.8004 0.5659 0.0183 0.312 Uiso 0.503(9) 1 calc PR A 2 H29E H 0.7959 0.5279 -0.0010 0.312 Uiso 0.503(9) 1 calc PR A 2 H29F H 0.8324 0.5500 -0.0055 0.312 Uiso 0.503(9) 1 calc PR A 2 C30 C 0.78489(16) 0.56009(15) 0.16941(16) 0.137(3) Uani 1 1 d DU . . H30 H 0.8015 0.5803 0.1635 0.165 Uiso 1 1 calc R A 1 C31 C 0.7961(2) 0.5379(2) 0.2017(2) 0.156(3) Uani 1 1 d U A . H31A H 0.7769 0.5210 0.2078 0.235 Uiso 1 1 calc R . . H31B H 0.8005 0.5538 0.2222 0.235 Uiso 1 1 calc R . . H31C H 0.8180 0.5246 0.1960 0.235 Uiso 1 1 calc R . . C32A C 0.7463(4) 0.5717(7) 0.1784(6) 0.111(8) Uiso 0.32(2) 1 d PDU A 1 H32A H 0.7300 0.5513 0.1749 0.166 Uiso 0.32(2) 1 calc PR A 1 H32B H 0.7392 0.5914 0.1625 0.166 Uiso 0.32(2) 1 calc PR A 1 H32C H 0.7451 0.5797 0.2034 0.166 Uiso 0.32(2) 1 calc PR A 1 C32B C 0.7631(3) 0.5922(3) 0.1820(3) 0.130(4) Uiso 0.68(2) 1 d PDU A 2 H32D H 0.7763 0.6049 0.2009 0.196 Uiso 0.68(2) 1 calc PR A 2 H32E H 0.7400 0.5839 0.1915 0.196 Uiso 0.68(2) 1 calc PR A 2 H32F H 0.7590 0.6085 0.1618 0.196 Uiso 0.68(2) 1 calc PR A 2 Br1 Br 0.7500 0.7500 0.14404(5) 0.0704(8) Uani 0.507(4) 4 d SPU . . Br2 Br 0.7500 0.7500 0.02256(8) 0.0832(12) Uani 0.363(4) 4 d SPU . . O1S O 0.7500 0.6826(5) 0.2500 0.178(6) Uiso 0.50 2 d SP . . O2S O 0.7159(4) 0.5960(5) 0.0354(4) 0.120(5) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0433(4) 0.0433(4) 0.0698(7) 0.000 0.000 0.000 O1 0.0512(14) 0.0663(15) 0.107(2) 0.0100(14) -0.0130(13) 0.0105(11) O2 0.0563(15) 0.0510(14) 0.130(2) 0.0095(14) -0.0090(14) 0.0059(11) N1 0.0451(15) 0.0485(15) 0.0730(18) -0.0008(13) -0.0034(12) -0.0019(11) N2 0.0472(16) 0.0508(16) 0.084(2) 0.0045(14) -0.0018(13) 0.0012(12) C1 0.0503(18) 0.0500(18) 0.082(2) -0.0028(16) -0.0057(16) 0.0020(14) C2 0.0498(18) 0.058(2) 0.087(3) 0.0003(18) -0.0093(17) 0.0055(15) C3 0.0510(19) 0.062(2) 0.088(3) 0.0020(18) -0.0094(18) 0.0079(15) C4 0.060(2) 0.0493(19) 0.101(3) 0.0062(18) -0.0081(19) 0.0074(15) C5 0.055(2) 0.0468(18) 0.108(3) 0.0025(18) -0.0099(19) 0.0009(15) C6 0.0516(19) 0.0513(19) 0.088(3) -0.0045(17) -0.0104(17) 0.0029(14) C7 0.0493(18) 0.0499(18) 0.076(2) -0.0020(15) -0.0104(16) -0.0001(14) C8 0.0490(18) 0.0483(18) 0.074(2) 0.0028(15) 0.0001(16) -0.0026(14) C9 0.051(2) 0.080(3) 0.124(3) 0.031(2) -0.011(2) 0.0052(18) C10 0.073(3) 0.075(3) 0.131(3) 0.033(2) -0.037(2) -0.008(2) C11 0.072(3) 0.112(4) 0.198(6) 0.065(4) -0.057(3) -0.026(3) C12 0.064(3) 0.160(6) 0.236(8) 0.109(6) -0.051(4) -0.019(3) C13 0.063(3) 0.187(7) 0.204(6) 0.114(5) 0.015(4) 0.018(3) C14 0.070(3) 0.137(4) 0.127(4) 0.054(3) 0.009(3) 0.024(3) C15 0.104(3) 0.074(3) 0.105(3) 0.011(2) -0.028(3) -0.003(3) C16 0.113(4) 0.076(3) 0.108(4) 0.013(3) -0.006(3) 0.001(3) C17 0.202(7) 0.081(3) 0.149(5) -0.005(3) -0.076(5) -0.001(4) C18 0.144(5) 0.148(5) 0.121(4) 0.045(4) 0.034(4) 0.051(4) C19 0.226(11) 0.249(11) 0.154(6) 0.051(7) 0.053(7) -0.001(8) C20 0.198(9) 0.128(5) 0.202(9) 0.014(5) -0.048(6) 0.057(6) C30 0.126(5) 0.113(4) 0.174(6) 0.058(4) 0.057(4) 0.056(4) C31 0.130(5) 0.136(6) 0.203(8) 0.050(5) 0.005(5) 0.040(4) Br1 0.0665(8) 0.0665(8) 0.0783(12) 0.000 0.000 0.000 Br2 0.0737(13) 0.0737(13) 0.102(2) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.920(3) 16_655 ? Co1 N1 1.920(3) 15_565 ? Co1 N1 1.920(3) 2_665 ? Co1 N1 1.920(3) . ? Co1 Br2 2.201(3) . ? Co1 Br1 2.327(2) . ? O1 C3 1.387(4) . ? O1 C9 1.409(5) . ? O2 C21B 1.303(5) . ? O2 C4 1.374(4) . ? O2 C21A 1.430(5) . ? N1 C8 1.374(4) 16_655 ? N1 C7 1.378(4) . ? N2 C7 1.325(5) . ? N2 C8 1.330(4) . ? C1 C6 1.386(5) . ? C1 C2 1.400(5) . ? C1 C8 1.444(5) 16_655 ? C2 C3 1.371(5) . ? C2 H2 0.9500 . ? C3 C4 1.403(5) . ? C4 C5 1.381(5) . ? C5 C6 1.395(5) . ? C5 H5 0.9500 . ? C6 C7 1.430(5) . ? C8 N1 1.374(4) 15_565 ? C8 C1 1.444(5) 15_565 ? C9 C14 1.371(7) . ? C9 C10 1.399(7) . ? C10 C11 1.371(6) . ? C10 C15 1.525(7) . ? C11 C12 1.280(11) . ? C11 H11 0.9500 . ? C12 C13 1.401(12) . ? C12 H12 0.9500 . ? C13 C14 1.421(10) . ? C13 H13 0.9500 . ? C14 C18 1.485(10) . ? C15 C16 1.505(7) . ? C15 C17 1.519(8) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.500(10) . ? C18 C20 1.513(10) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.524(8) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.275(6) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.505(8) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.730(7) . ? C27A C29A 1.517(10) . ? C27A C28A 1.541(9) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C28B 1.477(9) . ? C27B C29B 1.489(10) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.520(9) . ? C30 C32B 1.521(8) . ? C30 C32A 1.539(9) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 N1 Co1 N1 178.58(19) 16_655 15_565 ? N1 Co1 N1 89.991(3) 16_655 2_665 ? N1 Co1 N1 89.991(3) 15_565 2_665 ? N1 Co1 N1 89.991(3) 16_655 . ? N1 Co1 N1 89.991(3) 15_565 . ? N1 Co1 N1 178.58(19) 2_665 . ? N1 Co1 Br2 90.71(9) 16_655 . ? N1 Co1 Br2 90.71(9) 15_565 . ? N1 Co1 Br2 90.71(9) 2_665 . ? N1 Co1 Br2 90.71(9) . . ? N1 Co1 Br1 89.29(9) 16_655 . ? N1 Co1 Br1 89.29(9) 15_565 . ? N1 Co1 Br1 89.29(9) 2_665 . ? N1 Co1 Br1 89.29(9) . . ? Br2 Co1 Br1 180.0 . . ? C3 O1 C9 117.8(3) . . ? C21B O2 C4 113.9(4) . . ? C21B O2 C21A 15.2(4) . . ? C4 O2 C21A 116.2(3) . . ? C8 N1 C7 106.2(3) 16_655 . ? C8 N1 Co1 127.1(2) 16_655 . ? C7 N1 Co1 126.4(2) . . ? C7 N2 C8 122.0(3) . . ? C6 C1 C2 121.4(3) . . ? C6 C1 C8 105.6(3) . 16_655 ? C2 C1 C8 132.7(3) . 16_655 ? C3 C2 C1 116.8(3) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 O1 125.0(3) . . ? C2 C3 C4 122.0(3) . . ? O1 C3 C4 113.0(3) . . ? O2 C4 C5 123.7(3) . . ? O2 C4 C3 115.0(3) . . ? C5 C4 C3 121.2(3) . . ? C4 C5 C6 116.9(3) . . ? C4 C5 H5 121.6 . . ? C6 C5 H5 121.6 . . ? C1 C6 C5 121.6(3) . . ? C1 C6 C7 107.3(3) . . ? C5 C6 C7 130.6(3) . . ? N2 C7 N1 127.6(3) . . ? N2 C7 C6 122.1(3) . . ? N1 C7 C6 110.2(3) . . ? N2 C8 N1 126.8(3) . 15_565 ? N2 C8 C1 122.5(3) . 15_565 ? N1 C8 C1 110.6(3) 15_565 15_565 ? C14 C9 C10 123.9(5) . . ? C14 C9 O1 117.8(5) . . ? C10 C9 O1 118.0(4) . . ? C11 C10 C9 116.4(6) . . ? C11 C10 C15 123.7(6) . . ? C9 C10 C15 119.8(4) . . ? C12 C11 C10 123.7(8) . . ? C12 C11 H11 118.1 . . ? C10 C11 H11 118.1 . . ? C11 C12 C13 120.5(7) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C12 C13 C14 120.5(7) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 C13 115.0(7) . . ? C9 C14 C18 121.9(6) . . ? C13 C14 C18 123.1(6) . . ? C16 C15 C17 109.0(5) . . ? C16 C15 C10 111.0(4) . . ? C17 C15 C10 113.7(5) . . ? C16 C15 H15 107.6 . . ? C17 C15 H15 107.6 . . ? C10 C15 H15 107.6 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 117.1(8) . . ? C14 C18 C20 113.1(6) . . ? C19 C18 C20 106.0(8) . . ? C14 C18 H18 106.7 . . ? C19 C18 H18 106.7 . . ? C20 C18 H18 106.7 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 118.1(4) . . ? C26A C21A O2 121.9(4) . . ? C23A C22A C21A 120.0 . . ? C23A C22A C27A 120.8(5) . . ? C21A C22A C27A 119.1(6) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C30 C26A C25A 118.4(5) . . ? C30 C26A C21A 121.4(5) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 122.3(4) . . ? O2 C21B C26B 117.7(4) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 122.6(5) . . ? C21B C22B C27B 117.3(5) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 122.6(4) . . ? C21B C26B C30 117.3(4) . . ? C29A C27A C22A 128.8(11) . . ? C29A C27A C28A 107.4(12) . . ? C22A C27A C28A 116.1(9) . . ? C29A C27A H27A 99.2 . . ? C22A C27A H27A 99.2 . . ? C28A C27A H27A 99.2 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C28B C27B C29B 119.6(13) . . ? C28B C27B C22B 105.1(9) . . ? C29B C27B C22B 110.3(12) . . ? C28B C27B H27B 107.1 . . ? C29B C27B H27B 107.1 . . ? C22B C27B H27B 107.1 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 109.0(6) . . ? C26A C30 C32B 127.8(7) . . ? C31 C30 C32B 109.3(6) . . ? C26A C30 C32A 98.7(11) . . ? C31 C30 C32A 103.8(9) . . ? C32B C30 C32A 38.1(8) . . ? C26A C30 C26B 9.2(4) . . ? C31 C30 C26B 117.4(6) . . ? C32B C30 C26B 124.0(6) . . ? C32A C30 C26B 99.5(10) . . ? C26A C30 H30 114.6 . . ? C31 C30 H30 114.6 . . ? C32B C30 H30 78.9 . . ? C32A C30 H30 114.6 . . ? C26B C30 H30 106.3 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C8 3.0(4) 16_655 . . 16_655 ? N1 Co1 N1 C8 -175.6(2) 15_565 . . 16_655 ? N1 Co1 N1 C8 -86.3(3) 2_665 . . 16_655 ? Br2 Co1 N1 C8 93.7(3) . . . 16_655 ? Br1 Co1 N1 C8 -86.3(3) . . . 16_655 ? N1 Co1 N1 C7 176.4(2) 16_655 . . . ? N1 Co1 N1 C7 -2.2(4) 15_565 . . . ? N1 Co1 N1 C7 87.1(3) 2_665 . . . ? Br2 Co1 N1 C7 -92.9(3) . . . . ? Br1 Co1 N1 C7 87.1(3) . . . . ? C6 C1 C2 C3 -0.7(6) . . . . ? C8 C1 C2 C3 172.2(4) 16_655 . . . ? C1 C2 C3 O1 -178.5(4) . . . . ? C1 C2 C3 C4 0.8(6) . . . . ? C9 O1 C3 C2 2.2(6) . . . . ? C9 O1 C3 C4 -177.2(4) . . . . ? C21B O2 C4 C5 14.2(7) . . . . ? C21A O2 C4 C5 -2.5(6) . . . . ? C21B O2 C4 C3 -168.8(5) . . . . ? C21A O2 C4 C3 174.5(4) . . . . ? C2 C3 C4 O2 -177.4(4) . . . . ? O1 C3 C4 O2 2.0(5) . . . . ? C2 C3 C4 C5 -0.3(7) . . . . ? O1 C3 C4 C5 179.1(4) . . . . ? O2 C4 C5 C6 176.4(4) . . . . ? C3 C4 C5 C6 -0.3(6) . . . . ? C2 C1 C6 C5 0.1(6) . . . . ? C8 C1 C6 C5 -174.5(4) 16_655 . . . ? C2 C1 C6 C7 173.6(4) . . . . ? C8 C1 C6 C7 -1.0(4) 16_655 . . . ? C4 C5 C6 C1 0.4(6) . . . . ? C4 C5 C6 C7 -171.3(4) . . . . ? C8 N2 C7 N1 -0.9(6) . . . . ? C8 N2 C7 C6 174.1(4) . . . . ? C8 N1 C7 N2 176.1(3) 16_655 . . . ? Co1 N1 C7 N2 1.6(5) . . . . ? C8 N1 C7 C6 0.7(4) 16_655 . . . ? Co1 N1 C7 C6 -173.8(3) . . . . ? C1 C6 C7 N2 -175.5(3) . . . . ? C5 C6 C7 N2 -2.8(7) . . . . ? C1 C6 C7 N1 0.3(5) . . . . ? C5 C6 C7 N1 173.0(4) . . . . ? C7 N2 C8 N1 1.8(6) . . . 15_565 ? C7 N2 C8 C1 -174.3(3) . . . 15_565 ? C3 O1 C9 C14 -99.0(5) . . . . ? C3 O1 C9 C10 86.7(5) . . . . ? C14 C9 C10 C11 -1.0(7) . . . . ? O1 C9 C10 C11 172.9(4) . . . . ? C14 C9 C10 C15 -177.4(4) . . . . ? O1 C9 C10 C15 -3.5(6) . . . . ? C9 C10 C11 C12 2.3(8) . . . . ? C15 C10 C11 C12 178.6(6) . . . . ? C10 C11 C12 C13 -2.6(10) . . . . ? C11 C12 C13 C14 1.6(10) . . . . ? C10 C9 C14 C13 0.1(7) . . . . ? O1 C9 C14 C13 -173.8(4) . . . . ? C10 C9 C14 C18 177.9(5) . . . . ? O1 C9 C14 C18 4.0(7) . . . . ? C12 C13 C14 C9 -0.3(8) . . . . ? C12 C13 C14 C18 -178.1(6) . . . . ? C11 C10 C15 C16 -101.9(5) . . . . ? C9 C10 C15 C16 74.2(5) . . . . ? C11 C10 C15 C17 21.4(7) . . . . ? C9 C10 C15 C17 -162.5(4) . . . . ? C9 C14 C18 C19 153.7(7) . . . . ? C13 C14 C18 C19 -28.7(9) . . . . ? C9 C14 C18 C20 -82.5(8) . . . . ? C13 C14 C18 C20 95.1(8) . . . . ? C21B O2 C21A C22A 14.8(18) . . . . ? C4 O2 C21A C22A 99.7(4) . . . . ? C21B O2 C21A C26A -166(2) . . . . ? C4 O2 C21A C26A -81.4(5) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 178.9(5) . . . . ? C26A C21A C22A C27A 177.5(7) . . . . ? O2 C21A C22A C27A -3.6(7) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -177.5(7) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 175.5(6) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -175.4(7) . . . . ? O2 C21A C26A C30 5.7(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -178.9(5) . . . . ? C4 O2 C21B C22B 94.3(5) . . . . ? C21A O2 C21B C22B -164(2) . . . . ? C4 O2 C21B C26B -87.1(5) . . . . ? C21A O2 C21B C26B 15.0(17) . . . . ? O2 C21B C22B C23B 178.5(7) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B -3.6(7) . . . . ? C26B C21B C22B C27B 177.9(7) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -177.7(7) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -177.1(6) . . . . ? O2 C21B C26B C25B -178.6(7) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -1.3(6) . . . . ? C22B C21B C26B C30 177.3(5) . . . . ? C23A C22A C27A C29A 32.4(17) . . . . ? C21A C22A C27A C29A -145.1(14) . . . . ? C23A C22A C27A C28A -112.9(11) . . . . ? C21A C22A C27A C28A 69.5(12) . . . . ? C23B C22B C27B C28B -66.7(11) . . . . ? C21B C22B C27B C28B 115.5(10) . . . . ? C23B C22B C27B C29B 63.5(14) . . . . ? C21B C22B C27B C29B -114.3(13) . . . . ? C25A C26A C30 C31 71.1(6) . . . . ? C21A C26A C30 C31 -113.5(6) . . . . ? C25A C26A C30 C32B -64.1(10) . . . . ? C21A C26A C30 C32B 111.4(9) . . . . ? C25A C26A C30 C32A -36.8(10) . . . . ? C21A C26A C30 C32A 138.6(9) . . . . ? C25A C26A C30 C26B -133(3) . . . . ? C21A C26A C30 C26B 43(2) . . . . ? C25B C26B C30 C26A 48(2) . . . . ? C21B C26B C30 C26A -130(3) . . . . ? C25B C26B C30 C31 73.1(7) . . . . ? C21B C26B C30 C31 -104.1(6) . . . . ? C25B C26B C30 C32B -69.8(9) . . . . ? C21B C26B C30 C32B 113.0(8) . . . . ? C25B C26B C30 C32A -37.9(10) . . . . ? C21B C26B C30 C32A 144.9(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.831 _refine_diff_density_min -0.358 _refine_diff_density_rms 0.073 data_PNC[cBr0.85-Co3+-vBr0.47] _database_code_depnum_ccdc_archive 'CCDC 900371' #TrackingRef '900371_PNC[cBr0.85-Co3+-vBr0.47].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130.17 H153.42 Br1.32 Cl3.25 Co N8 O11.08' _chemical_formula_weight 2286.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.017(4) _cell_length_b 37.017(4) _cell_length_c 37.017(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 50723(9) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 47306 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 21.3 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.898 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14489 _exptl_absorpt_coefficient_mu 0.508 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9775 _exptl_absorpt_correction_T_max 0.9775 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5287 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0449 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 21.45 _reflns_number_total 5287 _reflns_number_gt 3715 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; Rigaku CrystalClear-SM Expert 2.0 r5 ; _computing_cell_refinement ; Rigaku CrystalClear-SM Expert 2.0 r5 ; _computing_data_reduction ; Rigaku CrystalClear-SM Expert 2.0 r5 ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0013(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5287 _refine_ls_number_parameters 316 _refine_ls_number_restraints 311 _refine_ls_R_factor_all 0.1580 _refine_ls_R_factor_gt 0.1359 _refine_ls_wR_factor_ref 0.4015 _refine_ls_wR_factor_gt 0.3776 _refine_ls_goodness_of_fit_ref 1.535 _refine_ls_restrained_S_all 1.528 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.07810(5) 0.0807(8) Uani 1 4 d SU . . O1 O 0.88897(10) 0.59555(11) 0.11080(12) 0.0918(13) Uani 1 1 d U A . O2 O 0.83137(10) 0.56007(10) 0.11071(13) 0.1019(15) Uani 1 1 d U . . N1 N 0.77835(12) 0.70700(12) 0.07917(15) 0.0841(15) Uani 1 1 d U A . N2 N 0.73208(13) 0.66191(12) 0.08336(14) 0.0818(14) Uani 1 1 d U A . C1 C 0.82592(15) 0.66752(15) 0.08741(17) 0.0770(16) Uani 1 1 d U . . C2 C 0.85884(15) 0.65181(15) 0.09483(17) 0.0797(16) Uani 1 1 d U A . H2 H 0.8805 0.6656 0.0952 0.096 Uiso 1 1 calc R . . C3 C 0.85884(14) 0.61538(16) 0.10162(16) 0.0812(16) Uani 1 1 d U . . C4 C 0.82732(16) 0.59575(15) 0.10123(18) 0.0911(18) Uani 1 1 d U A . C5 C 0.79469(16) 0.61109(15) 0.0937(2) 0.0944(19) Uani 1 1 d U . . H5 H 0.7730 0.5973 0.0930 0.113 Uiso 1 1 calc R A . C6 C 0.79495(15) 0.64774(15) 0.08703(18) 0.0866(17) Uani 1 1 d U A . C7 C 0.76497(17) 0.67275(15) 0.08294(17) 0.0835(16) Uani 1 1 d U . . C8 C 0.70481(16) 0.68548(15) 0.08296(16) 0.0781(16) Uani 1 1 d U . . C9 C 0.92198(17) 0.61339(18) 0.1141(2) 0.0966(18) Uani 1 1 d U . . C10 C 0.93098(18) 0.62791(18) 0.1471(2) 0.1042(19) Uani 1 1 d U A . C11 C 0.9651(2) 0.6416(2) 0.1501(3) 0.134(3) Uani 1 1 d U . . H11 H 0.9722 0.6517 0.1726 0.160 Uiso 1 1 calc R A . C12 C 0.9885(3) 0.6417(3) 0.1236(4) 0.164(4) Uani 1 1 d U A . H12 H 1.0121 0.6511 0.1273 0.197 Uiso 1 1 calc R . . C13 C 0.9793(2) 0.6286(3) 0.0913(3) 0.150(3) Uani 1 1 d U . . H13 H 0.9962 0.6304 0.0721 0.180 Uiso 1 1 calc R A . C14 C 0.9442(2) 0.6115(2) 0.0843(2) 0.122(2) Uani 1 1 d U A . C15 C 0.9042(2) 0.62682(19) 0.1776(2) 0.110(2) Uani 1 1 d U . . H15 H 0.8799 0.6333 0.1677 0.132 Uiso 1 1 calc R A . C16 C 0.9019(2) 0.5888(2) 0.1940(3) 0.120(2) Uani 1 1 d U A . H16A H 0.8950 0.5715 0.1752 0.180 Uiso 1 1 calc R . . H16B H 0.8838 0.5886 0.2132 0.180 Uiso 1 1 calc R . . H16C H 0.9255 0.5821 0.2040 0.180 Uiso 1 1 calc R . . C17 C 0.9134(3) 0.6535(2) 0.2082(3) 0.160(4) Uani 1 1 d U A . H17A H 0.9310 0.6424 0.2245 0.240 Uiso 1 1 calc R . . H17B H 0.8914 0.6594 0.2216 0.240 Uiso 1 1 calc R . . H17C H 0.9237 0.6756 0.1978 0.240 Uiso 1 1 calc R . . C18 C 0.9334(3) 0.5943(3) 0.0501(3) 0.146(3) Uani 1 1 d U . . H18 H 0.9068 0.5986 0.0472 0.175 Uiso 1 1 calc R A . C19 C 0.9516(4) 0.6075(4) 0.0157(3) 0.255(7) Uani 1 1 d U A . H19A H 0.9508 0.5883 -0.0026 0.382 Uiso 1 1 calc R . . H19B H 0.9768 0.6137 0.0209 0.382 Uiso 1 1 calc R . . H19C H 0.9389 0.6288 0.0066 0.382 Uiso 1 1 calc R . . C20 C 0.9386(3) 0.5548(3) 0.0534(3) 0.187(5) Uani 1 1 d U A . H20A H 0.9162 0.5437 0.0621 0.281 Uiso 1 1 calc R . . H20B H 0.9582 0.5499 0.0705 0.281 Uiso 1 1 calc R . . H20C H 0.9448 0.5448 0.0297 0.281 Uiso 1 1 calc R . . C21A C 0.7985(4) 0.5376(5) 0.1042(4) 0.092(7) Uiso 0.394(15) 1 d PGU A 1 C22A C 0.7850(5) 0.5141(4) 0.0782(3) 0.171(9) Uiso 0.394(15) 1 d PGDU A 1 C23A C 0.7544(4) 0.4937(4) 0.0855(3) 0.093(6) Uiso 0.394(15) 1 d PGU A 1 H23A H 0.7451 0.4777 0.0677 0.112 Uiso 0.394(15) 1 calc PR A 1 C24A C 0.7372(3) 0.4968(3) 0.1188(4) 0.105(6) Uiso 0.394(15) 1 d PGU A 1 H24A H 0.7162 0.4828 0.1237 0.126 Uiso 0.394(15) 1 calc PR A 1 C25A C 0.7507(4) 0.5203(4) 0.1448(3) 0.099(6) Uiso 0.394(15) 1 d PGU A 1 H25A H 0.7390 0.5224 0.1675 0.119 Uiso 0.394(15) 1 calc PR A 1 C26A C 0.7814(4) 0.5407(4) 0.1375(3) 0.119(9) Uiso 0.394(15) 1 d PGDU A 1 C21B C 0.8022(2) 0.5403(3) 0.1103(2) 0.094(5) Uiso 0.606(15) 1 d PGU A 2 C22B C 0.7988(3) 0.5222(3) 0.0776(2) 0.088(3) Uiso 0.606(15) 1 d PGDU A 2 C23B C 0.7683(3) 0.5014(3) 0.0707(3) 0.162(6) Uiso 0.606(15) 1 d PGU A 2 H23B H 0.7660 0.4891 0.0483 0.194 Uiso 0.606(15) 1 calc PR A 2 C24B C 0.7412(2) 0.4988(3) 0.0965(4) 0.142(6) Uiso 0.606(15) 1 d PGU A 2 H24B H 0.7203 0.4846 0.0917 0.170 Uiso 0.606(15) 1 calc PR A 2 C25B C 0.7445(2) 0.5169(3) 0.1292(3) 0.127(5) Uiso 0.606(15) 1 d PGU A 2 H25B H 0.7260 0.5152 0.1468 0.152 Uiso 0.606(15) 1 calc PR A 2 C26B C 0.7751(3) 0.5377(3) 0.1361(2) 0.115(6) Uiso 0.606(15) 1 d PGDU A 2 C27A C 0.8121(5) 0.5190(6) 0.0489(4) 0.114(7) Uiso 0.394(15) 1 d PDU A 1 H27A H 0.8180 0.5453 0.0509 0.137 Uiso 0.394(15) 1 calc PR A 1 C28A C 0.8489(7) 0.5015(10) 0.0534(10) 0.177(13) Uiso 0.394(15) 1 d PDU A 1 H28D H 0.8589 0.4958 0.0295 0.265 Uiso 0.394(15) 1 calc PR A 1 H28E H 0.8464 0.4792 0.0675 0.265 Uiso 0.394(15) 1 calc PR A 1 H28F H 0.8651 0.5182 0.0660 0.265 Uiso 0.394(15) 1 calc PR A 1 C29A C 0.8008(8) 0.5155(9) 0.0100(6) 0.185(12) Uiso 0.394(15) 1 d PDU A 1 H29A H 0.7913 0.5387 0.0015 0.278 Uiso 0.394(15) 1 calc PR A 1 H29B H 0.7820 0.4970 0.0079 0.278 Uiso 0.394(15) 1 calc PR A 1 H29C H 0.8217 0.5086 -0.0047 0.278 Uiso 0.394(15) 1 calc PR A 1 C27B C 0.8265(4) 0.5250(4) 0.0475(4) 0.138(6) Uiso 0.606(15) 1 d PDU A 2 H27B H 0.8452 0.5408 0.0589 0.166 Uiso 0.606(15) 1 calc PR A 2 C28B C 0.8474(5) 0.4909(4) 0.0412(6) 0.145(7) Uiso 0.606(15) 1 d PDU A 2 H28A H 0.8719 0.4970 0.0332 0.218 Uiso 0.606(15) 1 calc PR A 2 H28B H 0.8354 0.4765 0.0225 0.218 Uiso 0.606(15) 1 calc PR A 2 H28C H 0.8487 0.4770 0.0636 0.218 Uiso 0.606(15) 1 calc PR A 2 C29B C 0.8173(7) 0.5458(6) 0.0145(5) 0.214(9) Uiso 0.606(15) 1 d PDU A 2 H29D H 0.8048 0.5681 0.0213 0.320 Uiso 0.606(15) 1 calc PR A 2 H29E H 0.8015 0.5312 -0.0010 0.320 Uiso 0.606(15) 1 calc PR A 2 H29F H 0.8395 0.5517 0.0014 0.320 Uiso 0.606(15) 1 calc PR A 2 C30 C 0.7841(2) 0.5597(2) 0.1709(2) 0.157(4) Uani 1 1 d DU . . H30 H 0.7998 0.5816 0.1683 0.188 Uiso 1 1 calc R A 1 C31 C 0.7952(3) 0.5384(3) 0.2019(3) 0.174(4) Uani 1 1 d U A . H31A H 0.7759 0.5213 0.2081 0.261 Uiso 1 1 calc R . . H31B H 0.7997 0.5544 0.2225 0.261 Uiso 1 1 calc R . . H31C H 0.8173 0.5250 0.1960 0.261 Uiso 1 1 calc R . . C32A C 0.7455(5) 0.5703(11) 0.1799(8) 0.172(14) Uiso 0.41(3) 1 d PDU A 1 H32A H 0.7296 0.5495 0.1762 0.259 Uiso 0.41(3) 1 calc PR A 1 H32B H 0.7379 0.5902 0.1641 0.259 Uiso 0.41(3) 1 calc PR A 1 H32C H 0.7441 0.5781 0.2052 0.259 Uiso 0.41(3) 1 calc PR A 1 C32B C 0.7633(6) 0.5926(5) 0.1829(5) 0.161(9) Uiso 0.59(3) 1 d PDU A 2 H32D H 0.7686 0.5977 0.2083 0.242 Uiso 0.59(3) 1 calc PR A 2 H32E H 0.7373 0.5881 0.1801 0.242 Uiso 0.59(3) 1 calc PR A 2 H32F H 0.7703 0.6134 0.1681 0.242 Uiso 0.59(3) 1 calc PR A 2 Br1 Br 0.7500 0.7500 0.14224(5) 0.0995(10) Uani 0.852(7) 4 d SPU . . Br2 Br 0.7500 0.7500 0.01696(12) 0.125(2) Uani 0.465(7) 4 d SPU . . O1S O 0.7143(8) 0.5887(8) 0.0326(8) 0.180(10) Uiso 0.25 1 d P . . O2S O 0.8130(8) 0.6842(8) 0.1876(9) 0.179(10) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0570(8) 0.0570(8) 0.1280(15) 0.000 0.000 0.000 O1 0.071(2) 0.084(3) 0.121(3) 0.017(2) -0.012(2) 0.012(2) O2 0.071(2) 0.067(2) 0.167(4) 0.018(2) -0.010(2) 0.0020(19) N1 0.059(3) 0.059(3) 0.134(4) -0.007(2) -0.002(3) 0.001(2) N2 0.063(3) 0.063(3) 0.119(4) -0.001(2) -0.001(3) 0.006(2) C1 0.066(3) 0.064(3) 0.101(4) 0.004(3) -0.011(3) 0.001(3) C2 0.070(3) 0.073(3) 0.096(4) -0.001(3) -0.003(3) 0.003(3) C3 0.057(3) 0.077(3) 0.110(4) 0.003(3) 0.001(3) 0.010(3) C4 0.075(3) 0.061(3) 0.137(5) 0.003(3) -0.008(3) 0.007(3) C5 0.065(3) 0.069(3) 0.149(6) 0.003(4) -0.014(4) 0.005(3) C6 0.073(3) 0.062(3) 0.125(5) -0.003(3) -0.013(3) 0.001(3) C7 0.070(3) 0.061(3) 0.119(5) -0.007(3) -0.014(3) 0.000(3) C8 0.068(3) 0.062(4) 0.105(4) 0.001(3) -0.004(3) -0.004(3) C9 0.067(3) 0.095(4) 0.127(4) 0.039(4) -0.012(3) 0.003(3) C10 0.087(4) 0.088(4) 0.137(5) 0.033(4) -0.032(3) -0.009(3) C11 0.091(5) 0.127(6) 0.183(7) 0.059(5) -0.054(4) -0.024(4) C12 0.084(5) 0.198(9) 0.212(9) 0.112(7) -0.046(5) -0.013(6) C13 0.075(4) 0.182(8) 0.193(7) 0.102(6) 0.004(5) 0.015(4) C14 0.087(4) 0.139(6) 0.139(5) 0.050(4) 0.007(4) 0.023(4) C15 0.112(5) 0.101(5) 0.118(5) 0.014(4) -0.023(4) -0.007(4) C16 0.126(6) 0.096(4) 0.138(7) 0.021(4) 0.003(5) -0.001(4) C17 0.204(10) 0.105(5) 0.170(7) -0.016(5) -0.060(7) 0.013(6) C18 0.145(7) 0.157(7) 0.136(6) 0.035(5) 0.020(5) 0.044(6) C19 0.302(17) 0.314(17) 0.148(8) 0.060(9) 0.030(10) -0.086(14) C20 0.197(10) 0.144(6) 0.221(13) 0.012(6) -0.043(9) 0.024(8) C30 0.120(6) 0.155(7) 0.195(8) 0.051(6) 0.048(6) 0.071(5) C31 0.158(8) 0.150(8) 0.214(10) 0.029(7) -0.025(7) 0.036(7) Br1 0.0882(11) 0.0882(11) 0.1219(16) 0.000 0.000 0.000 Br2 0.109(2) 0.109(2) 0.158(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.907(4) 16_655 ? Co1 N1 1.907(4) . ? Co1 N1 1.907(4) 15_565 ? Co1 N1 1.907(4) 2_665 ? Co1 Br2 2.263(5) . ? Co1 Br1 2.374(3) . ? O1 C3 1.378(6) . ? O1 C9 1.394(7) . ? O2 C21B 1.304(7) . ? O2 C4 1.375(6) . ? O2 C21A 1.492(11) . ? N1 C8 1.349(7) 16_655 ? N1 C7 1.368(7) . ? N2 C7 1.282(8) . ? N2 C8 1.334(7) . ? C1 C6 1.360(7) . ? C1 C2 1.378(8) . ? C1 C8 1.453(8) 16_655 ? C2 C3 1.372(8) . ? C2 H2 0.9500 . ? C3 C4 1.375(8) . ? C4 C5 1.364(8) . ? C5 C6 1.379(8) . ? C5 H5 0.9500 . ? C6 C7 1.453(8) . ? C8 N1 1.349(7) 15_565 ? C8 C1 1.453(8) 15_565 ? C9 C10 1.375(10) . ? C9 C14 1.378(10) . ? C10 C11 1.365(9) . ? C10 C15 1.504(10) . ? C11 C12 1.309(13) . ? C11 H11 0.9500 . ? C12 C13 1.333(15) . ? C12 H12 0.9500 . ? C13 C14 1.467(12) . ? C13 H13 0.9500 . ? C14 C18 1.472(12) . ? C15 C16 1.534(10) . ? C15 C17 1.540(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.478(13) . ? C18 C19 1.524(13) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.487(10) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.429(8) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.514(9) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.563(8) . ? C27A C29A 1.506(10) . ? C27A C28A 1.518(10) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.483(9) . ? C27B C28B 1.501(9) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.452(12) . ? C30 C32B 1.508(9) . ? C30 C32A 1.520(10) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 N1 Co1 N1 89.976(8) 16_655 . ? N1 Co1 N1 177.6(4) 16_655 15_565 ? N1 Co1 N1 89.976(8) . 15_565 ? N1 Co1 N1 89.975(8) 16_655 2_665 ? N1 Co1 N1 177.6(4) . 2_665 ? N1 Co1 N1 89.975(8) 15_565 2_665 ? N1 Co1 Br2 91.19(18) 16_655 . ? N1 Co1 Br2 91.19(18) . . ? N1 Co1 Br2 91.19(18) 15_565 . ? N1 Co1 Br2 91.19(18) 2_665 . ? N1 Co1 Br1 88.81(18) 16_655 . ? N1 Co1 Br1 88.81(18) . . ? N1 Co1 Br1 88.81(18) 15_565 . ? N1 Co1 Br1 88.81(18) 2_665 . ? Br2 Co1 Br1 180.0 . . ? C3 O1 C9 118.6(5) . . ? C21B O2 C4 116.4(7) . . ? C21B O2 C21A 8.6(7) . . ? C4 O2 C21A 113.9(9) . . ? C8 N1 C7 107.0(5) 16_655 . ? C8 N1 Co1 126.8(4) 16_655 . ? C7 N1 Co1 125.2(4) . . ? C7 N2 C8 120.9(5) . . ? C6 C1 C2 121.3(5) . . ? C6 C1 C8 105.4(5) . 16_655 ? C2 C1 C8 132.9(5) . 16_655 ? C3 C2 C1 116.8(5) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 C4 121.2(5) . . ? C2 C3 O1 124.7(5) . . ? C4 C3 O1 114.1(5) . . ? C5 C4 C3 122.3(5) . . ? C5 C4 O2 123.3(5) . . ? C3 C4 O2 114.4(5) . . ? C4 C5 C6 116.1(5) . . ? C4 C5 H5 121.9 . . ? C6 C5 H5 121.9 . . ? C1 C6 C5 122.3(5) . . ? C1 C6 C7 107.6(5) . . ? C5 C6 C7 129.8(5) . . ? N2 C7 N1 129.4(5) . . ? N2 C7 C6 121.6(5) . . ? N1 C7 C6 108.9(5) . . ? N2 C8 N1 127.2(5) . 15_565 ? N2 C8 C1 121.8(5) . 15_565 ? N1 C8 C1 110.9(5) 15_565 15_565 ? C10 C9 C14 125.8(7) . . ? C10 C9 O1 118.4(6) . . ? C14 C9 O1 115.5(7) . . ? C11 C10 C9 116.2(8) . . ? C11 C10 C15 124.0(8) . . ? C9 C10 C15 119.8(6) . . ? C12 C11 C10 123.5(10) . . ? C12 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? C11 C12 C13 120.1(10) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C12 C13 C14 122.8(10) . . ? C12 C13 H13 118.6 . . ? C14 C13 H13 118.6 . . ? C9 C14 C13 111.5(9) . . ? C9 C14 C18 123.0(8) . . ? C13 C14 C18 125.5(9) . . ? C10 C15 C16 111.0(6) . . ? C10 C15 C17 112.9(7) . . ? C16 C15 C17 108.0(7) . . ? C10 C15 H15 108.3 . . ? C16 C15 H15 108.3 . . ? C17 C15 H15 108.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C20 108.8(8) . . ? C14 C18 C19 117.4(11) . . ? C20 C18 C19 109.0(10) . . ? C14 C18 H18 107.1 . . ? C20 C18 H18 107.1 . . ? C19 C18 H18 107.1 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 138.9(9) . . ? C26A C21A O2 100.6(9) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 100.8(12) . . ? C23A C22A C27A 139.2(12) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C25A C26A C21A 120.0 . . ? C25A C26A C30 99.2(10) . . ? C21A C26A C30 140.8(10) . . ? O2 C21B C22B 110.8(7) . . ? O2 C21B C26B 129.0(7) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 116.9(9) . . ? C21B C22B C27B 123.1(9) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 128.0(7) . . ? C21B C26B C30 112.0(7) . . ? C22A C27A C29A 120.0(19) . . ? C22A C27A C28A 118.3(19) . . ? C29A C27A C28A 109(2) . . ? C22A C27A H27A 102.2 . . ? C29A C27A H27A 102.2 . . ? C28A C27A H27A 102.2 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 115.1(14) . . ? C29B C27B C22B 119.1(14) . . ? C28B C27B C22B 114.0(12) . . ? C29B C27B H27B 101.6 . . ? C28B C27B H27B 101.6 . . ? C22B C27B H27B 101.6 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 115.8(11) . . ? C26A C30 C32B 128.1(13) . . ? C31 C30 C32B 110.6(10) . . ? C26A C30 C32A 104.5(16) . . ? C31 C30 C32A 103.4(13) . . ? C32B C30 C32A 41.0(13) . . ? C26A C30 C26B 8.8(7) . . ? C31 C30 C26B 115.3(9) . . ? C32B C30 C26B 123.6(11) . . ? C32A C30 C26B 96.4(15) . . ? C26A C30 H30 110.9 . . ? C31 C30 H30 110.9 . . ? C32B C30 H30 70.8 . . ? C32A C30 H30 110.9 . . ? C26B C30 H30 117.8 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C8 5.4(7) 16_655 . . 16_655 ? N1 Co1 N1 C8 -172.2(4) 15_565 . . 16_655 ? N1 Co1 N1 C8 -83.4(5) 2_665 . . 16_655 ? Br2 Co1 N1 C8 96.6(5) . . . 16_655 ? Br1 Co1 N1 C8 -83.4(5) . . . 16_655 ? N1 Co1 N1 C7 172.5(4) 16_655 . . . ? N1 Co1 N1 C7 -5.1(7) 15_565 . . . ? N1 Co1 N1 C7 83.7(5) 2_665 . . . ? Br2 Co1 N1 C7 -96.3(5) . . . . ? Br1 Co1 N1 C7 83.7(5) . . . . ? C6 C1 C2 C3 0.3(9) . . . . ? C8 C1 C2 C3 172.1(7) 16_655 . . . ? C1 C2 C3 C4 -0.5(9) . . . . ? C1 C2 C3 O1 -177.5(6) . . . . ? C9 O1 C3 C2 1.0(9) . . . . ? C9 O1 C3 C4 -176.2(6) . . . . ? C2 C3 C4 C5 1.0(10) . . . . ? O1 C3 C4 C5 178.3(6) . . . . ? C2 C3 C4 O2 -176.2(6) . . . . ? O1 C3 C4 O2 1.2(8) . . . . ? C21B O2 C4 C5 3.7(10) . . . . ? C21A O2 C4 C5 12.8(10) . . . . ? C21B O2 C4 C3 -179.2(6) . . . . ? C21A O2 C4 C3 -170.1(7) . . . . ? C3 C4 C5 C6 -1.2(10) . . . . ? O2 C4 C5 C6 175.7(6) . . . . ? C2 C1 C6 C5 -0.6(11) . . . . ? C8 C1 C6 C5 -174.4(6) 16_655 . . . ? C2 C1 C6 C7 173.0(6) . . . . ? C8 C1 C6 C7 -0.8(7) 16_655 . . . ? C4 C5 C6 C1 1.0(10) . . . . ? C4 C5 C6 C7 -171.0(7) . . . . ? C8 N2 C7 N1 -5.9(10) . . . . ? C8 N2 C7 C6 173.7(6) . . . . ? C8 N1 C7 N2 175.8(6) 16_655 . . . ? Co1 N1 C7 N2 6.6(10) . . . . ? C8 N1 C7 C6 -3.8(7) 16_655 . . . ? Co1 N1 C7 C6 -173.0(4) . . . . ? C1 C6 C7 N2 -176.8(6) . . . . ? C5 C6 C7 N2 -3.8(11) . . . . ? C1 C6 C7 N1 2.9(8) . . . . ? C5 C6 C7 N1 175.8(7) . . . . ? C7 N2 C8 N1 5.8(9) . . . 15_565 ? C7 N2 C8 C1 -173.1(6) . . . 15_565 ? C3 O1 C9 C10 88.5(7) . . . . ? C3 O1 C9 C14 -97.8(7) . . . . ? C14 C9 C10 C11 0.2(10) . . . . ? O1 C9 C10 C11 173.2(5) . . . . ? C14 C9 C10 C15 -177.8(6) . . . . ? O1 C9 C10 C15 -4.8(9) . . . . ? C9 C10 C11 C12 0.5(11) . . . . ? C15 C10 C11 C12 178.3(8) . . . . ? C10 C11 C12 C13 1.5(15) . . . . ? C11 C12 C13 C14 -4.2(15) . . . . ? C10 C9 C14 C13 -2.4(10) . . . . ? O1 C9 C14 C13 -175.6(6) . . . . ? C10 C9 C14 C18 177.5(7) . . . . ? O1 C9 C14 C18 4.4(10) . . . . ? C12 C13 C14 C9 4.4(12) . . . . ? C12 C13 C14 C18 -175.5(9) . . . . ? C11 C10 C15 C16 -101.9(8) . . . . ? C9 C10 C15 C16 75.9(8) . . . . ? C11 C10 C15 C17 19.4(10) . . . . ? C9 C10 C15 C17 -162.8(6) . . . . ? C9 C14 C18 C20 -81.8(11) . . . . ? C13 C14 C18 C20 98.1(11) . . . . ? C9 C14 C18 C19 153.9(10) . . . . ? C13 C14 C18 C19 -26.2(14) . . . . ? C21B O2 C21A C22A -153(10) . . . . ? C4 O2 C21A C22A 97.6(16) . . . . ? C21B O2 C21A C26A 18(8) . . . . ? C4 O2 C21A C26A -91.5(8) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 170(2) . . . . ? C26A C21A C22A C27A -178.1(15) . . . . ? O2 C21A C22A C27A -8.4(18) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A 177(2) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C24A C25A C26A C30 179.6(14) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -173.1(14) . . . . ? C22A C21A C26A C30 -179(2) . . . . ? O2 C21A C26A C30 7.5(17) . . . . ? C4 O2 C21B C22B 95.0(8) . . . . ? C21A O2 C21B C22B 20(8) . . . . ? C4 O2 C21B C26B -80.3(9) . . . . ? C21A O2 C21B C26B -155(9) . . . . ? O2 C21B C22B C23B -175.8(10) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 1.5(11) . . . . ? C26B C21B C22B C27B 177.3(10) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -177.5(10) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -179.5(12) . . . . ? O2 C21B C26B C25B 175.0(12) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -5.5(9) . . . . ? C22B C21B C26B C30 179.6(10) . . . . ? C21A C22A C27A C29A -148(2) . . . . ? C23A C22A C27A C29A 34(3) . . . . ? C21A C22A C27A C28A 75(3) . . . . ? C23A C22A C27A C28A -102(3) . . . . ? C23B C22B C27B C29B 69.7(19) . . . . ? C21B C22B C27B C29B -107.7(18) . . . . ? C23B C22B C27B C28B -71.6(17) . . . . ? C21B C22B C27B C28B 111.0(15) . . . . ? C25A C26A C30 C31 71.0(11) . . . . ? C21A C26A C30 C31 -109.5(17) . . . . ? C25A C26A C30 C32B -80.0(17) . . . . ? C21A C26A C30 C32B 99(2) . . . . ? C25A C26A C30 C32A -42.0(17) . . . . ? C21A C26A C30 C32A 137(2) . . . . ? C25A C26A C30 C26B -18(8) . . . . ? C21A C26A C30 C26B 161(9) . . . . ? C25B C26B C30 C26A 170(9) . . . . ? C21B C26B C30 C26A -10(8) . . . . ? C25B C26B C30 C31 74.5(11) . . . . ? C21B C26B C30 C31 -105.1(8) . . . . ? C25B C26B C30 C32B -66.9(17) . . . . ? C21B C26B C30 C32B 113.6(13) . . . . ? C25B C26B C30 C32A -33.7(17) . . . . ? C21B C26B C30 C32A 146.8(15) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 21.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.236 _refine_diff_density_min -0.448 _refine_diff_density_rms 0.090 data_9cobua _database_code_depnum_ccdc_archive 'CCDC 900372' #TrackingRef '900372_PNC[cBuNH2-Co-vH2O].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H157 Co N9 O8' _chemical_formula_weight 2056.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' '-y+1/2, x, z' 'y, x, -z+1/2' 'y, -x+1/2, z' '-y+1/2, -x+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z+1/2, x' 'y, -z+1/2, -x+1/2' '-y+1/2, z, -x+1/2' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' 'z, -y+1/2, x' 'z, y, -x+1/2' 'z, x, y' '-z+1/2, x, -y+1/2' '-z+1/2, -x+1/2, y' 'z, -x+1/2, -y+1/2' '-x+1/2, -z+1/2, -y+1/2' '-x+1/2, z, y' 'x, -z+1/2, y' 'x, z, -y+1/2' '-x, -y, -z' '-x, y-1/2, z-1/2' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' 'y-1/2, -x, -z' '-y, -x, z-1/2' '-y, x-1/2, -z' 'y-1/2, x-1/2, z-1/2' '-y, -z, -x' 'y-1/2, z-1/2, -x' '-y, z-1/2, x-1/2' 'y-1/2, -z, x-1/2' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' '-z, y-1/2, -x' '-z, -y, x-1/2' '-z, -x, -y' 'z-1/2, -x, y-1/2' 'z-1/2, x-1/2, -y' '-z, x-1/2, y-1/2' 'x-1/2, z-1/2, y-1/2' 'x-1/2, -z, -y' '-x, z-1/2, -y' '-x, -z, y-1/2' _cell_length_a 37.458(5) _cell_length_b 37.458(5) _cell_length_c 37.458(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52556(12) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7516 _cell_measurement_theta_min 1.49 _cell_measurement_theta_max 25.52 _exptl_crystal_description cuboid _exptl_crystal_colour purple _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.780 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13236 _exptl_absorpt_coefficient_mu 0.138 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.9849 _exptl_absorpt_correction_T_max 0.9863 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator 'Double-crystal with Si 111' _diffrn_measurement_device_type 'Diamond, I19' _diffrn_measurement_method 'Rigaku Saturn 724 CCD detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 212805 _diffrn_reflns_av_R_equivalents 0.0885 _diffrn_reflns_av_sigmaI/netI 0.0493 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.52 _reflns_number_total 8973 _reflns_number_gt 7516 _reflns_threshold_expression >2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8973 _refine_ls_number_parameters 453 _refine_ls_number_restraints 517 _refine_ls_R_factor_all 0.1497 _refine_ls_R_factor_gt 0.1354 _refine_ls_wR_factor_ref 0.3993 _refine_ls_wR_factor_gt 0.3890 _refine_ls_goodness_of_fit_ref 1.600 _refine_ls_restrained_S_all 1.624 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.006 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 0.76525(10) 0.67300(9) 0.08652(11) 0.0504(9) Uani 1 1 d . . . C2 C 0.79459(9) 0.64799(10) 0.08986(12) 0.0560(10) Uani 1 1 d . . . C3 C 0.82600(9) 0.66792(9) 0.09025(12) 0.0523(9) Uani 1 1 d . . . C4 C 0.81505(9) 0.70506(9) 0.08652(11) 0.0513(9) Uani 1 1 d . . . C5 C 0.79489(10) 0.61137(9) 0.09566(14) 0.0617(11) Uani 1 1 d . . . H5 H 0.7735 0.5978 0.0948 0.074 Uiso 1 1 calc R . . C6 C 0.82717(10) 0.59556(9) 0.10265(13) 0.0567(10) Uani 1 1 d . A . C7 C 0.85943(10) 0.61585(10) 0.10280(12) 0.0538(9) Uani 1 1 d . . . C8 C 0.85842(8) 0.65185(8) 0.09718(10) 0.0558(10) Uani 1 1 d . . . H8 H 0.8797 0.6656 0.0980 0.067 Uiso 1 1 calc R . . C9 C 0.80179(8) 0.54169(8) 0.10356(10) 0.059(3) Uani 0.450(6) 1 d PRDU A 1 C10 C 0.77398(8) 0.53875(8) 0.12795(10) 0.069(3) Uani 0.450(6) 1 d PRDU A 1 C11 C 0.74574(8) 0.51564(8) 0.12119(10) 0.067(2) Uani 0.450(6) 1 d PRDU A 1 H11 H 0.7267 0.5136 0.1379 0.080 Uiso 0.450(6) 1 calc PR A 1 C12 C 0.74532(8) 0.49548(8) 0.09004(10) 0.070(3) Uani 0.450(6) 1 d PRDU A 1 H12 H 0.7260 0.4797 0.0854 0.084 Uiso 0.450(6) 1 calc PR A 1 C13 C 0.77313(8) 0.49842(8) 0.06565(10) 0.069(3) Uani 0.450(6) 1 d PRDU A 1 H13 H 0.7728 0.4846 0.0444 0.082 Uiso 0.450(6) 1 calc PR A 1 C14 C 0.80137(8) 0.52153(8) 0.07241(10) 0.066(3) Uani 0.450(6) 1 d PRDU A 1 C15 C 0.7775(3) 0.5560(3) 0.1662(3) 0.069(3) Uani 0.450(6) 1 d PDU A 1 H15 H 0.7930 0.5775 0.1637 0.082 Uiso 0.450(6) 1 calc PR A 1 C16 C 0.7944(6) 0.5322(5) 0.1935(4) 0.094(5) Uani 0.450(6) 1 d PDU A 1 H16A H 0.7956 0.5447 0.2165 0.141 Uiso 0.450(6) 1 calc PR A 1 H16B H 0.8185 0.5258 0.1858 0.141 Uiso 0.450(6) 1 calc PR A 1 H16C H 0.7800 0.5104 0.1962 0.141 Uiso 0.450(6) 1 calc PR A 1 C17 C 0.7406(4) 0.5689(4) 0.1794(4) 0.105(4) Uani 0.450(6) 1 d PDU A 1 H17A H 0.7294 0.5838 0.1610 0.158 Uiso 0.450(6) 1 calc PR A 1 H17B H 0.7436 0.5828 0.2013 0.158 Uiso 0.450(6) 1 calc PR A 1 H17C H 0.7253 0.5482 0.1843 0.158 Uiso 0.450(6) 1 calc PR A 1 C18 C 0.8348(3) 0.5267(3) 0.0492(3) 0.079(3) Uani 0.450(6) 1 d PDU A 1 H18 H 0.8532 0.5402 0.0631 0.095 Uiso 0.450(6) 1 calc PR A 1 C19 C 0.8498(4) 0.4907(4) 0.0386(4) 0.097(5) Uani 0.450(6) 1 d PDU A 1 H19A H 0.8709 0.4941 0.0236 0.146 Uiso 0.450(6) 1 calc PR A 1 H19B H 0.8317 0.4773 0.0253 0.146 Uiso 0.450(6) 1 calc PR A 1 H19C H 0.8565 0.4774 0.0601 0.146 Uiso 0.450(6) 1 calc PR A 1 C20 C 0.8239(4) 0.5489(4) 0.0159(3) 0.127(5) Uani 0.450(6) 1 d PDU A 1 H20A H 0.8133 0.5716 0.0235 0.191 Uiso 0.450(6) 1 calc PR A 1 H20B H 0.8064 0.5355 0.0018 0.191 Uiso 0.450(6) 1 calc PR A 1 H20C H 0.8451 0.5537 0.0012 0.191 Uiso 0.450(6) 1 calc PR A 1 C9A C 0.80021(17) 0.53735(19) 0.1111(2) 0.0455(16) Uani 0.550(6) 1 d PDU A 2 C10A C 0.77906(17) 0.53860(18) 0.14122(19) 0.0503(17) Uani 0.550(6) 1 d PDU A 2 C11A C 0.7481(2) 0.5184(2) 0.1422(2) 0.072(2) Uani 0.550(6) 1 d PDU A 2 H11A H 0.7330 0.5185 0.1626 0.087 Uiso 0.550(6) 1 calc PR A 2 C12A C 0.7397(3) 0.4981(3) 0.1122(3) 0.080(2) Uani 0.550(6) 1 d PDU A 2 H12A H 0.7194 0.4830 0.1131 0.096 Uiso 0.550(6) 1 calc PR A 2 C13A C 0.7599(3) 0.4989(3) 0.0811(3) 0.080(3) Uani 0.550(6) 1 d PDU A 2 H13A H 0.7523 0.4864 0.0605 0.097 Uiso 0.550(6) 1 calc PR A 2 C14A C 0.7918(2) 0.5186(2) 0.0806(2) 0.068(2) Uani 0.550(6) 1 d PDU A 2 C15A C 0.7897(3) 0.5622(2) 0.1741(3) 0.069(2) Uani 0.550(6) 1 d PDU A 2 H15A H 0.8124 0.5747 0.1678 0.083 Uiso 0.550(6) 1 calc PR A 2 C16A C 0.7972(4) 0.5397(3) 0.2063(3) 0.080(3) Uani 0.550(6) 1 d PDU A 2 H16D H 0.8040 0.5550 0.2263 0.120 Uiso 0.550(6) 1 calc PR A 2 H16E H 0.8167 0.5231 0.2010 0.120 Uiso 0.550(6) 1 calc PR A 2 H16F H 0.7757 0.5261 0.2126 0.120 Uiso 0.550(6) 1 calc PR A 2 C17A C 0.7616(3) 0.5911(3) 0.1815(4) 0.104(3) Uani 0.550(6) 1 d PDU A 2 H17D H 0.7577 0.6052 0.1598 0.155 Uiso 0.550(6) 1 calc PR A 2 H17E H 0.7700 0.6067 0.2006 0.155 Uiso 0.550(6) 1 calc PR A 2 H17F H 0.7391 0.5797 0.1887 0.155 Uiso 0.550(6) 1 calc PR A 2 C18A C 0.8155(3) 0.5212(3) 0.0467(2) 0.080(2) Uani 0.550(6) 1 d PDU A 2 H18A H 0.8223 0.5466 0.0421 0.096 Uiso 0.550(6) 1 calc PR A 2 C19A C 0.8487(3) 0.4986(4) 0.0521(3) 0.093(4) Uani 0.550(6) 1 d PDU A 2 H19D H 0.8638 0.5001 0.0308 0.139 Uiso 0.550(6) 1 calc PR A 2 H19E H 0.8418 0.4737 0.0562 0.139 Uiso 0.550(6) 1 calc PR A 2 H19F H 0.8620 0.5075 0.0729 0.139 Uiso 0.550(6) 1 calc PR A 2 C20A C 0.79197(5) 0.50626(6) 0.01442(7) 0.159(6) Uani 0.550(6) 1 d PDU A 2 H20D H 0.7705 0.5210 0.0117 0.238 Uiso 0.550(6) 1 calc PR A 2 H20E H 0.7850 0.4816 0.0194 0.238 Uiso 0.550(6) 1 calc PR A 2 H20F H 0.8060 0.5070 -0.0077 0.238 Uiso 0.550(6) 1 calc PR A 2 C21 C 0.92141(5) 0.61323(6) 0.11407(7) 0.0662(12) Uani 1 1 d RD . . C22 C 0.94523(5) 0.61348(6) 0.08562(7) 0.0849(17) Uani 1 1 d R . . C23 C 0.97897(5) 0.62835(6) 0.08981(7) 0.112(3) Uani 1 1 d R . . H23 H 0.9953 0.6285 0.0704 0.135 Uiso 1 1 calc R . . C24 C 0.98888(5) 0.64297(6) 0.12245(7) 0.121(3) Uani 1 1 d R . . H24 H 1.0119 0.6531 0.1253 0.145 Uiso 1 1 calc R . . C25 C 0.96506(5) 0.64272(6) 0.15090(7) 0.097(2) Uani 1 1 d R . . H25 H 0.9718 0.6527 0.1732 0.116 Uiso 1 1 calc R . . C26 C 0.93132(5) 0.62785(6) 0.14671(7) 0.0750(14) Uani 1 1 d R . . C27 C 0.93278(17) 0.59431(18) 0.0506(2) 0.100(2) Uani 1 1 d . . . H27 H 0.9067 0.5991 0.0475 0.120 Uiso 1 1 calc R . . C28 C 0.9380(2) 0.5539(2) 0.0535(3) 0.124(3) Uani 1 1 d . . . H28A H 0.9297 0.5424 0.0315 0.187 Uiso 1 1 calc R . . H28B H 0.9242 0.5447 0.0738 0.187 Uiso 1 1 calc R . . H28C H 0.9633 0.5486 0.0571 0.187 Uiso 1 1 calc R . . C29 C 0.9520(3) 0.6072(3) 0.0173(3) 0.167(4) Uani 1 1 d . . . H29A H 0.9427 0.5945 -0.0036 0.251 Uiso 1 1 calc R . . H29B H 0.9776 0.6026 0.0196 0.251 Uiso 1 1 calc R . . H29C H 0.9480 0.6329 0.0143 0.251 Uiso 1 1 calc R . . C30 C 0.90517(14) 0.62560(13) 0.17777(16) 0.0804(15) Uani 1 1 d . . . H30 H 0.8810 0.6317 0.1682 0.097 Uiso 1 1 calc R . . C31 C 0.90319(16) 0.58754(14) 0.19258(17) 0.0832(14) Uani 1 1 d . . . H31A H 0.8861 0.5868 0.2124 0.125 Uiso 1 1 calc R . . H31B H 0.9268 0.5803 0.2012 0.125 Uiso 1 1 calc R . . H31C H 0.8954 0.5712 0.1737 0.125 Uiso 1 1 calc R . . C32 C 0.9132(2) 0.65198(18) 0.2084(2) 0.117(3) Uani 1 1 d . . . H32A H 0.8953 0.6492 0.2272 0.175 Uiso 1 1 calc R . . H32B H 0.9125 0.6765 0.1992 0.175 Uiso 1 1 calc R . . H32C H 0.9370 0.6470 0.2181 0.175 Uiso 1 1 calc R . . Co1 Co 0.7500 0.7500 0.08447(3) 0.0429(3) Uani 1 4 d S . . O1 O 0.83191(7) 0.56015(7) 0.11144(10) 0.0675(9) Uani 1 1 d D . . O2 O 0.88881(7) 0.59546(7) 0.11076(9) 0.0614(8) Uani 1 1 d D . . O3 O 0.7500 0.7500 0.0326(2) 0.0699(16) Uani 1 4 d S . . O4 O 0.9188(5) 0.7153(5) 0.0321(6) 0.113(5) Uani 0.25 1 d PU . . N1 N 0.77835(7) 0.70690(7) 0.08451(9) 0.0475(7) Uani 1 1 d . . . N2 N 0.73183(8) 0.66189(8) 0.08727(10) 0.0541(8) Uani 1 1 d . . . N3 N 0.7500 0.7500 0.1383(2) 0.0637(17) Uani 1 4 d SD . . H3A H 0.7409 0.7286 0.1462 0.076 Uiso 0.25 1 calc PR . . H3B H 0.7732 0.7516 0.1462 0.076 Uiso 0.25 1 calc PR . . C33 C 0.7284(5) 0.7803(5) 0.1549(7) 0.129(10) Uani 0.25 1 d PDU . . H33A H 0.7426 0.7913 0.1743 0.155 Uiso 0.25 1 calc PR . . H33B H 0.7241 0.7988 0.1365 0.155 Uiso 0.25 1 calc PR . . C34 C 0.6931(5) 0.7681(6) 0.1697(7) 0.160(14) Uani 0.25 1 d PDU . . H34A H 0.6974 0.7512 0.1896 0.192 Uiso 0.25 1 calc PR . . H34B H 0.6797 0.7553 0.1509 0.192 Uiso 0.25 1 calc PR . . C35 C 0.6708(6) 0.7991(8) 0.1832(8) 0.135(11) Uani 0.25 1 d PDU . . H35A H 0.6591 0.8109 0.1627 0.162 Uiso 0.25 1 calc PR . . H35B H 0.6520 0.7899 0.1993 0.162 Uiso 0.25 1 calc PR . . C36 C 0.6933(9) 0.8261(8) 0.2031(12) 0.183(16) Uani 0.25 1 d PDU . . H36A H 0.6779 0.8451 0.2124 0.275 Uiso 0.25 1 calc PR . . H36B H 0.7110 0.8364 0.1868 0.275 Uiso 0.25 1 calc PR . . H36C H 0.7056 0.8143 0.2230 0.275 Uiso 0.25 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0401(17) 0.0350(16) 0.076(2) 0.0067(15) -0.0103(16) 0.0017(14) C2 0.0378(17) 0.0420(18) 0.088(3) 0.0040(18) -0.0131(17) 0.0012(14) C3 0.0387(17) 0.0347(16) 0.083(3) -0.0022(16) -0.0063(16) 0.0001(13) C4 0.0361(16) 0.0392(17) 0.079(3) 0.0014(16) -0.0075(16) 0.0008(13) C5 0.0377(17) 0.0336(17) 0.114(4) 0.0070(19) -0.0107(19) 0.0007(13) C6 0.0435(19) 0.0346(16) 0.092(3) 0.0101(17) -0.0093(18) 0.0035(14) C7 0.0407(18) 0.0455(19) 0.075(2) 0.0030(17) -0.0101(16) 0.0070(15) C8 0.0382(17) 0.0420(18) 0.087(3) 0.0034(17) -0.0138(17) -0.0023(14) C9 0.060(5) 0.032(4) 0.085(5) 0.021(4) -0.005(4) 0.006(4) C10 0.061(5) 0.054(4) 0.092(6) 0.011(4) -0.013(5) 0.011(4) C11 0.060(4) 0.055(5) 0.086(6) 0.008(5) 0.001(5) 0.004(4) C12 0.072(6) 0.050(4) 0.086(6) 0.005(5) 0.006(5) -0.013(4) C13 0.068(5) 0.050(4) 0.088(6) -0.004(4) -0.001(5) 0.001(4) C14 0.069(5) 0.044(4) 0.085(5) 0.011(4) -0.001(4) 0.004(4) C15 0.058(5) 0.060(5) 0.089(6) -0.005(5) -0.016(5) 0.009(4) C16 0.114(9) 0.088(9) 0.079(9) -0.012(7) -0.001(8) 0.011(8) C17 0.095(8) 0.103(9) 0.118(9) -0.031(8) -0.003(7) 0.032(7) C18 0.082(6) 0.066(5) 0.089(6) 0.015(5) 0.010(6) 0.006(5) C19 0.117(9) 0.094(10) 0.080(9) 0.021(8) 0.015(7) 0.041(7) C20 0.152(11) 0.105(9) 0.126(10) 0.044(8) 0.015(9) 0.033(8) C9A 0.046(3) 0.020(2) 0.071(4) 0.015(3) -0.014(3) 0.001(2) C10A 0.039(3) 0.037(3) 0.076(4) 0.019(3) -0.011(3) 0.008(2) C11A 0.058(4) 0.053(4) 0.106(6) 0.013(4) -0.005(4) -0.003(3) C12A 0.071(4) 0.055(4) 0.114(6) -0.004(5) -0.003(5) -0.007(4) C13A 0.084(6) 0.054(4) 0.104(6) -0.012(4) -0.007(5) -0.005(4) C14A 0.074(4) 0.048(4) 0.082(4) 0.008(3) -0.007(4) 0.013(3) C15A 0.062(5) 0.057(4) 0.088(5) -0.016(4) -0.005(4) 0.013(4) C16A 0.091(7) 0.064(6) 0.085(7) -0.004(5) -0.005(6) 0.025(5) C17A 0.099(7) 0.085(6) 0.126(8) -0.007(6) 0.008(6) 0.022(6) C18A 0.089(6) 0.064(4) 0.087(5) 0.011(4) -0.014(5) 0.005(5) C19A 0.111(7) 0.081(7) 0.087(8) 0.008(6) 0.007(6) 0.033(6) C20A 0.178(12) 0.176(12) 0.124(10) -0.020(9) -0.051(9) 0.038(10) C21 0.0365(18) 0.057(2) 0.106(3) 0.023(2) -0.017(2) 0.0072(16) C22 0.047(2) 0.091(4) 0.117(4) 0.042(3) -0.008(3) 0.013(2) C23 0.051(3) 0.129(5) 0.157(7) 0.076(5) 0.001(3) 0.015(3) C24 0.056(3) 0.115(5) 0.192(8) 0.078(5) -0.049(4) -0.013(3) C25 0.060(3) 0.076(3) 0.153(6) 0.040(4) -0.047(3) -0.011(2) C26 0.056(2) 0.050(2) 0.119(4) 0.016(2) -0.034(3) 0.0047(18) C27 0.086(4) 0.104(4) 0.110(5) 0.033(4) 0.011(3) 0.030(3) C28 0.112(5) 0.104(5) 0.157(7) 0.006(5) -0.004(5) 0.029(4) C29 0.167(9) 0.188(10) 0.146(8) 0.047(7) 0.046(7) 0.018(7) C30 0.073(3) 0.060(3) 0.108(4) -0.002(3) -0.032(3) 0.011(2) C31 0.081(3) 0.076(3) 0.092(4) 0.012(3) -0.005(3) -0.001(3) C32 0.140(6) 0.081(4) 0.129(6) -0.012(4) -0.043(5) 0.006(4) Co1 0.0313(4) 0.0313(4) 0.0662(6) 0.000 0.000 0.000 O1 0.0413(13) 0.0361(13) 0.125(3) 0.0170(14) -0.0112(14) 0.0040(10) O2 0.0407(13) 0.0452(14) 0.098(2) 0.0122(14) -0.0169(13) 0.0078(10) O3 0.056(2) 0.056(2) 0.098(5) 0.000 0.000 0.000 O4 0.115(9) 0.099(8) 0.125(9) -0.027(7) 0.036(7) -0.019(7) N1 0.0312(13) 0.0351(14) 0.076(2) 0.0019(13) -0.0083(13) 0.0010(10) N2 0.0349(15) 0.0348(14) 0.093(2) 0.0107(14) -0.0063(14) -0.0010(11) N3 0.061(2) 0.061(2) 0.069(4) 0.000 0.000 0.000 C33 0.18(2) 0.14(2) 0.063(12) -0.002(13) 0.015(15) -0.005(19) C34 0.18(3) 0.15(2) 0.15(2) 0.044(19) -0.07(2) 0.04(2) C35 0.15(2) 0.119(19) 0.14(2) -0.013(16) 0.019(17) 0.064(17) C36 0.12(2) 0.22(3) 0.21(3) 0.00(2) 0.07(2) -0.02(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 C1 N2 1.320(5) . ? C1 N1 1.363(4) . ? C1 C2 1.450(5) . ? C2 C5 1.389(5) . ? C2 C3 1.394(5) . ? C3 C8 1.380(5) . ? C3 C4 1.457(5) . ? C4 N2 1.324(5) 5_655 ? C4 N1 1.378(4) . ? C5 C6 1.372(5) . ? C5 H5 0.9500 . ? C6 O1 1.378(4) . ? C6 C7 1.428(5) . ? C7 C8 1.365(5) . ? C7 O2 1.372(4) . ? C8 H8 0.9500 . ? C9 O1 1.356(4) . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C10 C15 1.575(10) . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C18 1.538(10) . ? C15 C16 1.500(11) . ? C15 C17 1.545(11) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.515(8) . ? C18 C20 1.554(8) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C9A C14A 1.377(7) . ? C9A C10A 1.381(7) . ? C9A O1 1.463(6) . ? C10A C11A 1.386(7) . ? C10A C15A 1.568(10) . ? C11A C12A 1.392(8) . ? C11A H11A 0.9500 . ? C12A C13A 1.391(8) . ? C12A H12A 0.9500 . ? C13A C14A 1.404(8) . ? C13A H13A 0.9500 . ? C14A C18A 1.550(11) . ? C15A C16A 1.498(11) . ? C15A C17A 1.535(10) . ? C15A H15A 1.0000 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A C19A 1.519(10) . ? C18A C20A 1.597(9) . ? C18A H18A 1.0000 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C21 O2 1.396(3) . ? C22 C23 1.3900 . ? C22 C27 1.565(8) . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C30 1.523(7) . ? C27 C29 1.521(10) . ? C27 C28 1.531(9) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.532(7) . ? C30 C32 1.543(8) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? Co1 N1 1.932(3) 5_655 ? Co1 N1 1.932(3) . ? Co1 N1 1.932(3) 3_665 ? Co1 N1 1.932(3) 7_565 ? Co1 O3 1.945(8) . ? Co1 N3 2.017(8) . ? N2 C4 1.324(5) 7_565 ? N3 C33 1.523(10) . ? N3 H3A 0.9200 . ? N3 H3B 0.9200 . ? C33 C34 1.505(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C35 1.516(10) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C35 C36 1.513(10) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 N2 C1 N1 129.5(3) . . ? N2 C1 C2 120.9(3) . . ? N1 C1 C2 109.5(3) . . ? C5 C2 C3 121.4(3) . . ? C5 C2 C1 131.1(3) . . ? C3 C2 C1 107.1(3) . . ? C8 C3 C2 120.7(3) . . ? C8 C3 C4 133.0(3) . . ? C2 C3 C4 105.8(3) . . ? N2 C4 N1 127.9(3) 5_655 . ? N2 C4 C3 122.5(3) 5_655 . ? N1 C4 C3 109.5(3) . . ? C6 C5 C2 117.6(3) . . ? C6 C5 H5 121.2 . . ? C2 C5 H5 121.2 . . ? C5 C6 O1 125.1(3) . . ? C5 C6 C7 121.1(3) . . ? O1 C6 C7 113.7(3) . . ? C8 C7 O2 127.3(3) . . ? C8 C7 C6 120.1(3) . . ? O2 C7 C6 112.5(3) . . ? C7 C8 C3 119.0(3) . . ? C7 C8 H8 120.5 . . ? C3 C8 H8 120.5 . . ? O1 C9 C10 121.4(2) . . ? O1 C9 C14 118.0(2) . . ? C10 C9 C14 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 C15 118.9(5) . . ? C9 C10 C15 120.2(4) . . ? C12 C11 C10 120.0 . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.0 . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? C14 C13 C12 120.0 . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C13 C14 C9 120.0 . . ? C13 C14 C18 126.6(5) . . ? C9 C14 C18 113.4(5) . . ? C16 C15 C17 110.1(10) . . ? C16 C15 C10 114.4(9) . . ? C17 C15 C10 110.3(8) . . ? C16 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C10 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C14 109.7(8) . . ? C19 C18 C20 111.4(7) . . ? C14 C18 C20 107.9(8) . . ? C19 C18 H18 109.3 . . ? C14 C18 H18 109.3 . . ? C20 C18 H18 109.3 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.4 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.4 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14A C9A C10A 124.5(6) . . ? C14A C9A O1 119.4(6) . . ? C10A C9A O1 116.0(5) . . ? C9A C10A C11A 119.0(6) . . ? C9A C10A C15A 121.1(6) . . ? C11A C10A C15A 119.9(6) . . ? C10A C11A C12A 117.7(7) . . ? C10A C11A H11A 121.2 . . ? C12A C11A H11A 121.2 . . ? C13A C12A C11A 122.8(8) . . ? C13A C12A H12A 118.6 . . ? C11A C12A H12A 118.6 . . ? C12A C13A C14A 119.1(8) . . ? C12A C13A H13A 120.4 . . ? C14A C13A H13A 120.4 . . ? C9A C14A C13A 116.7(7) . . ? C9A C14A C18A 121.1(7) . . ? C13A C14A C18A 122.0(7) . . ? C16A C15A C17A 112.4(8) . . ? C16A C15A C10A 111.3(7) . . ? C17A C15A C10A 111.3(8) . . ? C16A C15A H15A 107.2 . . ? C17A C15A H15A 107.2 . . ? C10A C15A H15A 107.2 . . ? C15A C16A H16D 109.5 . . ? C15A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C15A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C15A C17A H17D 109.5 . . ? C15A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C15A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C19A C18A C14A 108.9(7) . . ? C19A C18A C20A 111.0(8) . . ? C14A C18A C20A 106.4(7) . . ? C19A C18A H18A 110.1 . . ? C14A C18A H18A 110.1 . . ? C20A C18A H18A 110.1 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18A C20A H20D 109.5 . . ? C18A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? C22 C21 C26 120.0 . . ? C22 C21 O2 119.78(18) . . ? C26 C21 O2 119.97(18) . . ? C21 C22 C23 120.0 . . ? C21 C22 C27 116.6(3) . . ? C23 C22 C27 123.3(3) . . ? C22 C23 C24 120.0 . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C24 C25 C26 120.0 . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.0 . . ? C21 C26 C30 118.6(2) . . ? C25 C26 C30 121.4(2) . . ? C29 C27 C28 108.2(7) . . ? C29 C27 C22 113.6(7) . . ? C28 C27 C22 110.9(5) . . ? C29 C27 H27 108.0 . . ? C28 C27 H27 108.0 . . ? C22 C27 H27 108.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C26 C30 C31 111.1(4) . . ? C26 C30 C32 114.0(5) . . ? C31 C30 C32 109.7(5) . . ? C26 C30 H30 107.3 . . ? C31 C30 H30 107.3 . . ? C32 C30 H30 107.3 . . ? 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 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N1 Co1 N1 90.000(1) 5_655 . ? N1 Co1 N1 90.0 5_655 3_665 ? N1 Co1 N1 179.9(2) . 3_665 ? N1 Co1 N1 179.9(2) 5_655 7_565 ? N1 Co1 N1 90.000(1) . 7_565 ? N1 Co1 N1 90.000(1) 3_665 7_565 ? N1 Co1 O3 90.05(10) 5_655 . ? N1 Co1 O3 90.05(10) . . ? N1 Co1 O3 90.05(10) 3_665 . ? N1 Co1 O3 90.05(10) 7_565 . ? N1 Co1 N3 89.95(10) 5_655 . ? N1 Co1 N3 89.95(10) . . ? N1 Co1 N3 89.95(10) 3_665 . ? N1 Co1 N3 89.95(10) 7_565 . ? O3 Co1 N3 180.000(1) . . ? C9 O1 C6 109.4(3) . . ? C9 O1 C9A 12.7(4) . . ? C6 O1 C9A 117.1(4) . . ? C7 O2 C21 117.1(3) . . ? C1 N1 C4 108.0(3) . . ? C1 N1 Co1 125.5(2) . . ? C4 N1 Co1 126.2(2) . . ? C1 N2 C4 120.8(3) . 7_565 ? C33 N3 Co1 114.0(12) . . ? C33 N3 H3A 108.7 . . ? Co1 N3 H3A 108.8 . . ? C33 N3 H3B 108.8 . . ? Co1 N3 H3B 108.8 . . ? H3A N3 H3B 107.7 . . ? C34 C33 N3 113.1(10) . . ? C34 C33 H33A 109.0 . . ? N3 C33 H33A 109.0 . . ? C34 C33 H33B 108.9 . . ? N3 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? C33 C34 C35 112.1(10) . . ? C33 C34 H34A 109.2 . . ? C35 C34 H34A 109.2 . . ? C33 C34 H34B 109.2 . . ? C35 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C36 C35 C34 111.7(10) . . ? C36 C35 H35A 109.2 . . ? C34 C35 H35A 109.3 . . ? C36 C35 H35B 109.3 . . ? C34 C35 H35B 109.3 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.4 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.52 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.829 _refine_diff_density_min -0.572 _refine_diff_density_rms 0.107 data_PNC[cCl-Co3+-vCl] _database_code_depnum_ccdc_archive 'CCDC 900373' #TrackingRef '900373_PNC[cCl-Co3+-vCl].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C128 H146 Cl2 Co N8 O10' _chemical_formula_weight 2086.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.230(4) _cell_length_b 37.230(4) _cell_length_c 37.230(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 51605(10) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 69874 _cell_measurement_theta_min 1.6 _cell_measurement_theta_max 25.5 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.806 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13332 _exptl_absorpt_coefficient_mu 0.172 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.739 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; Rigaku CrystalClear-SM Expert 2.0 r5 ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Station I19, Diamond' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 106091 _diffrn_reflns_av_R_equivalents 0.0667 _diffrn_reflns_av_sigmaI/netI 0.0270 _diffrn_reflns_limit_h_min -44 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -42 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 24.21 _reflns_number_total 7600 _reflns_number_gt 6274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7600 _refine_ls_number_parameters 316 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1885 _refine_ls_R_factor_gt 0.1749 _refine_ls_wR_factor_ref 0.4776 _refine_ls_wR_factor_gt 0.4650 _refine_ls_goodness_of_fit_ref 2.003 _refine_ls_restrained_S_all 2.016 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.07866(4) 0.0487(5) Uani 1 4 d S . . O1 O 0.61149(9) 0.90501(10) 0.10892(13) 0.0777(12) Uani 1 1 d . A . O2 O 0.66887(10) 0.94044(9) 0.10896(14) 0.0889(15) Uani 1 1 d . . . N1 N 0.72154(9) 0.79326(9) 0.07926(11) 0.0509(10) Uani 1 1 d . A . N2 N 0.76858(10) 0.83804(10) 0.08178(13) 0.0629(12) Uani 1 1 d . A . C1 C 0.67435(12) 0.83309(12) 0.08628(15) 0.0572(12) Uani 1 1 d . . . C2 C 0.64081(13) 0.84901(13) 0.09310(16) 0.0638(14) Uani 1 1 d . A . H2 H 0.6192 0.8354 0.0929 0.096 Uiso 1 1 calc R . . C3 C 0.64076(13) 0.88479(14) 0.09994(16) 0.0681(14) Uani 1 1 d . . . C4 C 0.67315(14) 0.90552(14) 0.09981(18) 0.0728(16) Uani 1 1 d . A . C5 C 0.70602(14) 0.88936(13) 0.09244(18) 0.0723(16) Uani 1 1 d . . . H5 H 0.7278 0.9027 0.0922 0.108 Uiso 1 1 calc R A . C6 C 0.70540(12) 0.85291(13) 0.08546(15) 0.0600(13) Uani 1 1 d . A . C7 C 0.73473(13) 0.82739(12) 0.08124(14) 0.0566(12) Uani 1 1 d . . . C8 C 0.79562(12) 0.81472(12) 0.08183(14) 0.0546(12) Uani 1 1 d . . . C9 C 0.57805(15) 0.88712(18) 0.1125(2) 0.089(2) Uani 1 1 d . . . C10 C 0.56933(17) 0.8721(2) 0.1446(3) 0.100(3) Uani 1 1 d . A . C11 C 0.5361(2) 0.8580(2) 0.1504(3) 0.131(4) Uani 1 1 d . . . H11 H 0.5298 0.8480 0.1730 0.197 Uiso 1 1 calc R A . C12 C 0.5130(3) 0.8585(4) 0.1234(5) 0.169(6) Uani 1 1 d . A . H12 H 0.4897 0.8488 0.1272 0.253 Uiso 1 1 calc R . . C13 C 0.5206(2) 0.8717(3) 0.0917(4) 0.152(5) Uani 1 1 d . . . H13 H 0.5034 0.8703 0.0729 0.229 Uiso 1 1 calc R A . C14 C 0.5552(2) 0.8887(2) 0.0851(3) 0.111(3) Uani 1 1 d . A . C15 C 0.5962(2) 0.87323(18) 0.1768(2) 0.101(2) Uani 1 1 d . . . H15 H 0.6205 0.8676 0.1668 0.152 Uiso 1 1 calc R A . C16 C 0.5983(2) 0.91111(19) 0.1923(2) 0.100(2) Uani 1 1 d . A . H16A H 0.5745 0.9183 0.2010 0.150 Uiso 1 1 calc R . . H16B H 0.6063 0.9278 0.1735 0.150 Uiso 1 1 calc R . . H16C H 0.6155 0.9115 0.2122 0.150 Uiso 1 1 calc R . . C17 C 0.5900(4) 0.8474(2) 0.2071(3) 0.159(5) Uani 1 1 d . A . H17A H 0.5744 0.8586 0.2251 0.239 Uiso 1 1 calc R . . H17B H 0.6130 0.8411 0.2182 0.239 Uiso 1 1 calc R . . H17C H 0.5785 0.8256 0.1978 0.239 Uiso 1 1 calc R . . C18 C 0.5667(3) 0.9072(3) 0.0503(3) 0.143(4) Uani 1 1 d . . . H18 H 0.5932 0.9032 0.0481 0.215 Uiso 1 1 calc R A . C19 C 0.5496(5) 0.8936(4) 0.0133(4) 0.210(7) Uani 1 1 d . A . H19A H 0.5431 0.9144 -0.0015 0.315 Uiso 1 1 calc R . . H19B H 0.5281 0.8793 0.0183 0.315 Uiso 1 1 calc R . . H19C H 0.5672 0.8788 0.0004 0.315 Uiso 1 1 calc R . . C20 C 0.5614(3) 0.9474(3) 0.0525(4) 0.156(4) Uani 1 1 d . A . H20A H 0.5462 0.9554 0.0326 0.234 Uiso 1 1 calc R . . H20B H 0.5848 0.9594 0.0511 0.234 Uiso 1 1 calc R . . H20C H 0.5498 0.9535 0.0754 0.234 Uiso 1 1 calc R . . C21A C 0.70061(18) 0.9609(2) 0.1147(2) 0.050(3) Uiso 0.442(13) 1 d PG A 1 C22A C 0.7093(2) 0.9826(3) 0.0856(2) 0.075(4) Uiso 0.442(13) 1 d PG A 1 C23A C 0.7396(3) 1.0044(3) 0.0869(3) 0.085(4) Uiso 0.442(13) 1 d PG A 1 H23A H 0.7456 1.0192 0.0670 0.127 Uiso 0.442(13) 1 calc PR A 1 C24A C 0.7613(2) 1.0044(2) 0.1173(3) 0.097(5) Uiso 0.442(13) 1 d PG A 1 H24A H 0.7820 1.0193 0.1182 0.146 Uiso 0.442(13) 1 calc PR A 1 C25A C 0.7526(2) 0.9827(2) 0.1464(3) 0.075(4) Uiso 0.442(13) 1 d PG A 1 H25A H 0.7674 0.9828 0.1672 0.113 Uiso 0.442(13) 1 calc PR A 1 C26A C 0.7223(2) 0.9610(2) 0.1451(2) 0.052(3) Uiso 0.442(13) 1 d PG A 1 C21B C 0.69738(17) 0.9614(2) 0.1022(2) 0.064(3) Uiso 0.558(13) 1 d PG A 2 C22B C 0.7026(2) 0.9804(2) 0.0705(2) 0.083(3) Uiso 0.558(13) 1 d PG A 2 C23B C 0.7332(2) 1.0012(2) 0.0660(3) 0.109(5) Uiso 0.558(13) 1 d PG A 2 H23B H 0.7368 1.0142 0.0443 0.163 Uiso 0.558(13) 1 calc PR A 2 C24B C 0.7587(2) 1.0030(2) 0.0932(3) 0.102(4) Uiso 0.558(13) 1 d PG A 2 H24B H 0.7797 1.0173 0.0901 0.153 Uiso 0.558(13) 1 calc PR A 2 C25B C 0.7535(2) 0.9841(3) 0.1250(3) 0.104(4) Uiso 0.558(13) 1 d PG A 2 H25B H 0.7710 0.9853 0.1436 0.157 Uiso 0.558(13) 1 calc PR A 2 C26B C 0.7229(2) 0.9633(2) 0.1295(2) 0.074(3) Uiso 0.558(13) 1 d PGD A 2 C27A C 0.6890(7) 0.9826(6) 0.0499(6) 0.116(7) Uiso 0.442(13) 1 d P A 1 H27A H 0.6807 0.9571 0.0512 0.174 Uiso 0.442(13) 1 calc PR A 1 C28A C 0.6477(6) 1.0014(7) 0.0519(7) 0.116(7) Uiso 0.442(13) 1 d P A 1 H28D H 0.6385 1.0048 0.0275 0.174 Uiso 0.442(13) 1 calc PR A 1 H28E H 0.6493 1.0248 0.0640 0.174 Uiso 0.442(13) 1 calc PR A 1 H28F H 0.6315 0.9857 0.0654 0.174 Uiso 0.442(13) 1 calc PR A 1 C29A C 0.6965(11) 0.9832(11) 0.0051(9) 0.207(14) Uiso 0.442(13) 1 d P A 1 H29A H 0.7047 0.9595 -0.0027 0.310 Uiso 0.442(13) 1 calc PR A 1 H29B H 0.7149 1.0012 -0.0004 0.310 Uiso 0.442(13) 1 calc PR A 1 H29C H 0.6741 0.9893 -0.0074 0.310 Uiso 0.442(13) 1 calc PR A 1 C27B C 0.6725(5) 0.9761(5) 0.0415(5) 0.109(5) Uiso 0.558(13) 1 d PD A 2 H27B H 0.6534 0.9636 0.0558 0.164 Uiso 0.558(13) 1 calc PR A 2 C28B C 0.6581(6) 1.0121(6) 0.0399(7) 0.147(8) Uiso 0.558(13) 1 d P A 2 H28A H 0.6603 1.0235 0.0635 0.221 Uiso 0.558(13) 1 calc PR A 2 H28B H 0.6327 1.0111 0.0330 0.221 Uiso 0.558(13) 1 calc PR A 2 H28C H 0.6715 1.0261 0.0221 0.221 Uiso 0.558(13) 1 calc PR A 2 C29B C 0.6822(9) 0.9475(9) 0.0152(8) 0.239(14) Uiso 0.558(13) 1 d PD A 2 H29D H 0.6931 0.9272 0.0279 0.359 Uiso 0.558(13) 1 calc PR A 2 H29E H 0.6994 0.9571 -0.0023 0.359 Uiso 0.558(13) 1 calc PR A 2 H29F H 0.6606 0.9394 0.0027 0.359 Uiso 0.558(13) 1 calc PR A 2 C30 C 0.7159(2) 0.9407(2) 0.1684(3) 0.129(3) Uani 1 1 d D . . H30 H 0.6991 0.9211 0.1608 0.194 Uiso 1 1 calc R A 1 C31 C 0.7025(3) 0.9613(3) 0.2004(3) 0.151(4) Uani 1 1 d . A . H31A H 0.6932 0.9444 0.2184 0.227 Uiso 1 1 calc R . . H31B H 0.6832 0.9776 0.1929 0.227 Uiso 1 1 calc R . . H31C H 0.7222 0.9752 0.2108 0.227 Uiso 1 1 calc R . . C32A C 0.7577(9) 0.9242(9) 0.1835(7) 0.173(11) Uiso 0.56(4) 1 d P A 1 H32A H 0.7752 0.9253 0.1638 0.259 Uiso 0.56(4) 1 calc PR A 1 H32B H 0.7550 0.8993 0.1914 0.259 Uiso 0.56(4) 1 calc PR A 1 H32C H 0.7662 0.9389 0.2035 0.259 Uiso 0.56(4) 1 calc PR A 1 C32B C 0.7391(7) 0.9083(6) 0.1801(5) 0.105(9) Uiso 0.44(4) 1 d P A 2 H32D H 0.7239 0.8905 0.1923 0.157 Uiso 0.44(4) 1 calc PR A 2 H32E H 0.7579 0.9164 0.1966 0.157 Uiso 0.44(4) 1 calc PR A 2 H32F H 0.7501 0.8972 0.1589 0.157 Uiso 0.44(4) 1 calc PR A 2 Cl1 Cl 0.7500 0.7500 0.13910(10) 0.0827(9) Uani 1 4 d S . . Cl2 Cl 0.7500 0.7500 0.01938(11) 0.0894(10) Uani 1 4 d S . . O1S O 0.7842(4) 0.9057(5) 0.0507(4) 0.161(5) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0394(5) 0.0394(5) 0.0674(9) 0.000 0.000 0.000 O1 0.0462(19) 0.064(2) 0.122(3) -0.018(2) 0.0130(19) 0.0096(16) O2 0.054(2) 0.0469(19) 0.165(4) -0.021(2) 0.012(2) 0.0038(16) N1 0.0400(19) 0.0383(19) 0.074(3) 0.0001(17) 0.0046(17) -0.0006(14) N2 0.038(2) 0.047(2) 0.104(3) -0.005(2) 0.003(2) -0.0005(17) C1 0.045(2) 0.046(2) 0.080(3) 0.000(2) 0.009(2) 0.0004(19) C2 0.049(3) 0.050(3) 0.092(4) -0.009(2) 0.006(2) -0.001(2) C3 0.046(3) 0.060(3) 0.098(4) -0.006(3) 0.015(3) 0.011(2) C4 0.048(3) 0.051(3) 0.119(5) -0.008(3) 0.009(3) 0.004(2) C5 0.052(3) 0.047(3) 0.117(5) -0.005(3) 0.014(3) 0.006(2) C6 0.046(3) 0.046(2) 0.088(3) -0.002(2) 0.008(2) 0.004(2) C7 0.049(3) 0.043(2) 0.078(3) -0.001(2) 0.008(2) 0.002(2) C8 0.040(2) 0.045(2) 0.079(3) -0.002(2) 0.003(2) 0.0021(18) C9 0.044(3) 0.084(4) 0.140(6) -0.046(4) 0.021(4) 0.000(3) C10 0.064(4) 0.091(5) 0.145(7) -0.049(5) 0.042(4) -0.011(3) C11 0.074(5) 0.126(7) 0.194(10) -0.087(7) 0.050(6) -0.031(5) C12 0.078(6) 0.172(10) 0.257(16) -0.117(11) 0.078(9) -0.013(6) C13 0.064(5) 0.180(10) 0.213(12) -0.111(10) 0.007(6) 0.007(5) C14 0.063(4) 0.132(7) 0.137(7) -0.056(6) 0.003(4) 0.022(4) C15 0.106(5) 0.067(4) 0.130(6) -0.006(4) 0.049(5) -0.006(4) C16 0.116(6) 0.081(4) 0.101(5) -0.022(4) 0.000(4) 0.001(4) C17 0.215(12) 0.076(5) 0.186(11) -0.003(6) 0.085(9) 0.010(6) C18 0.094(6) 0.163(9) 0.173(10) -0.068(8) -0.039(7) 0.064(6) C19 0.258(17) 0.186(13) 0.186(13) -0.073(10) -0.047(12) 0.045(11) C20 0.176(10) 0.107(7) 0.184(12) -0.018(7) 0.022(8) 0.011(7) C30 0.115(6) 0.108(6) 0.165(8) -0.039(6) -0.043(6) 0.048(5) C31 0.144(9) 0.137(8) 0.173(10) -0.040(7) -0.011(7) 0.036(7) Cl1 0.0803(12) 0.0803(12) 0.088(2) 0.000 0.000 0.000 Cl2 0.0796(13) 0.0796(13) 0.109(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.928(3) 15_565 ? Co1 N1 1.928(3) . ? Co1 N1 1.928(3) 2_665 ? Co1 N1 1.928(3) 16_655 ? Co1 Cl2 2.207(4) . ? Co1 Cl1 2.250(4) . ? O1 C3 1.366(6) . ? O1 C9 1.418(7) . ? O2 C21B 1.342(7) . ? O2 C4 1.353(6) . ? O2 C21A 1.423(7) . ? N1 C8 1.356(6) 16_655 ? N1 C7 1.365(6) . ? N2 C7 1.321(7) . ? N2 C8 1.330(6) . ? C1 C6 1.372(6) . ? C1 C2 1.405(7) . ? C1 C8 1.463(6) 16_655 ? C2 C3 1.356(7) . ? C2 H2 0.9500 . ? C3 C4 1.432(8) . ? C4 C5 1.391(7) . ? C5 C6 1.382(7) . ? C5 H5 0.9500 . ? C6 C7 1.456(7) . ? C8 N1 1.356(6) 15_565 ? C8 C1 1.462(6) 15_565 ? C9 C14 1.330(11) . ? C9 C10 1.360(11) . ? C10 C11 1.361(10) . ? C10 C15 1.562(11) . ? C11 C12 1.323(17) . ? C11 H11 0.9500 . ? C12 C13 1.31(2) . ? C12 H12 0.9500 . ? C13 C14 1.456(14) . ? C13 H13 0.9500 . ? C14 C18 1.530(15) . ? C15 C17 1.499(12) . ? C15 C16 1.525(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.513(15) . ? C18 C19 1.598(15) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.53(3) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.173(12) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.564(19) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.695(12) . ? C27A C28A 1.69(3) . ? C27A C29A 1.69(4) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C28B 1.44(3) . ? C27B C29B 1.493(18) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.503(13) . ? C30 C32B 1.55(2) . ? C30 C32A 1.77(3) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 N1 Co1 N1 89.988(3) 15_565 . ? N1 Co1 N1 90.001(4) 15_565 2_665 ? N1 Co1 N1 178.7(3) . 2_665 ? N1 Co1 N1 178.7(3) 15_565 16_655 ? N1 Co1 N1 89.994(4) . 16_655 ? N1 Co1 N1 89.986(3) 2_665 16_655 ? N1 Co1 Cl2 90.66(13) 15_565 . ? N1 Co1 Cl2 90.66(13) . . ? N1 Co1 Cl2 90.66(13) 2_665 . ? N1 Co1 Cl2 90.66(13) 16_655 . ? N1 Co1 Cl1 89.34(13) 15_565 . ? N1 Co1 Cl1 89.34(13) . . ? N1 Co1 Cl1 89.34(13) 2_665 . ? N1 Co1 Cl1 89.34(13) 16_655 . ? Cl2 Co1 Cl1 180.000(1) . . ? C3 O1 C9 117.7(4) . . ? C21B O2 C4 114.8(5) . . ? C21B O2 C21A 19.7(4) . . ? C4 O2 C21A 117.1(5) . . ? C8 N1 C7 107.1(4) 16_655 . ? C8 N1 Co1 127.0(3) 16_655 . ? C7 N1 Co1 125.5(3) . . ? C7 N2 C8 121.8(4) . . ? C6 C1 C2 121.7(4) . . ? C6 C1 C8 106.0(4) . 16_655 ? C2 C1 C8 132.1(4) . 16_655 ? C3 C2 C1 116.7(5) . . ? C3 C2 H2 121.6 . . ? C1 C2 H2 121.6 . . ? C2 C3 O1 126.0(5) . . ? C2 C3 C4 121.8(4) . . ? O1 C3 C4 112.1(5) . . ? O2 C4 C5 124.7(5) . . ? O2 C4 C3 114.7(4) . . ? C5 C4 C3 120.6(5) . . ? C6 C5 C4 116.5(5) . . ? C6 C5 H5 121.7 . . ? C4 C5 H5 121.7 . . ? C1 C6 C5 122.6(4) . . ? C1 C6 C7 106.5(4) . . ? C5 C6 C7 130.4(4) . . ? N2 C7 N1 128.6(4) . . ? N2 C7 C6 121.2(4) . . ? N1 C7 C6 110.1(4) . . ? N2 C8 N1 126.9(4) . 15_565 ? N2 C8 C1 122.7(4) . 15_565 ? N1 C8 C1 110.3(4) 15_565 15_565 ? C14 C9 C10 122.7(7) . . ? C14 C9 O1 118.0(8) . . ? C10 C9 O1 119.0(7) . . ? C9 C10 C11 120.9(9) . . ? C9 C10 C15 120.7(6) . . ? C11 C10 C15 118.2(9) . . ? C12 C11 C10 117.8(12) . . ? C12 C11 H11 121.1 . . ? C10 C11 H11 121.1 . . ? C13 C12 C11 123.3(11) . . ? C13 C12 H12 118.3 . . ? C11 C12 H12 118.3 . . ? C12 C13 C14 120.4(11) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C9 C14 C13 114.8(11) . . ? C9 C14 C18 119.3(8) . . ? C13 C14 C18 125.9(10) . . ? C17 C15 C16 108.5(7) . . ? C17 C15 C10 117.4(8) . . ? C16 C15 C10 110.2(6) . . ? C17 C15 H15 106.7 . . ? C16 C15 H15 106.7 . . ? C10 C15 H15 106.7 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C14 111.2(9) . . ? C20 C18 C19 108.0(11) . . ? C14 C18 C19 118.4(11) . . ? C20 C18 H18 106.1 . . ? C14 C18 H18 106.1 . . ? C19 C18 H18 106.1 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 112.8(6) . . ? C26A C21A O2 127.2(6) . . ? C23A C22A C21A 120.0 . . ? C23A C22A C27A 115.6(10) . . ? C21A C22A C27A 124.2(10) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 120.9(7) . . ? C30 C26A C21A 118.9(7) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 124.4(6) . . ? O2 C21B C26B 115.6(6) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 124.2(8) . . ? C21B C22B C27B 115.7(8) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C24B C25B C26B 120.0 . . ? C24B C25B H25B 120.0 . . ? C26B C25B H25B 120.0 . . ? C21B C26B C25B 120.0 . . ? C21B C26B C30 119.6(5) . . ? C25B C26B C30 120.4(5) . . ? C22A C27A C28A 114.3(16) . . ? C22A C27A C29A 141(2) . . ? C28A C27A C29A 101(2) . . ? C22A C27A H27A 96.4 . . ? C28A C27A H27A 96.4 . . ? C29A C27A H27A 96.4 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C28B C27B C29B 136(2) . . ? C28B C27B C22B 101.5(15) . . ? C29B C27B C22B 110.6(19) . . ? C28B C27B H27B 100.9 . . ? C29B C27B H27B 100.9 . . ? C22B C27B H27B 100.9 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 108.9(9) . . ? C26A C30 C32B 126.8(12) . . ? C31 C30 C32B 111.1(11) . . ? C26A C30 C26B 11.2(5) . . ? C31 C30 C26B 118.4(8) . . ? C32B C30 C26B 122.9(10) . . ? C26A C30 C32A 106.3(13) . . ? C31 C30 C32A 102.6(11) . . ? C32B C30 C32A 31.5(10) . . ? C26B C30 C32A 108.0(12) . . ? C26A C30 H30 112.8 . . ? C31 C30 H30 112.8 . . ? C32B C30 H30 81.9 . . ? C26B C30 H30 102.5 . . ? C32A C30 H30 112.8 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C8 -174.8(3) 15_565 . . 16_655 ? N1 Co1 N1 C8 -85.2(5) 2_665 . . 16_655 ? N1 Co1 N1 C8 3.9(5) 16_655 . . 16_655 ? Cl2 Co1 N1 C8 94.6(4) . . . 16_655 ? Cl1 Co1 N1 C8 -85.4(4) . . . 16_655 ? N1 Co1 N1 C7 -2.7(5) 15_565 . . . ? N1 Co1 N1 C7 86.9(4) 2_665 . . . ? N1 Co1 N1 C7 176.0(3) 16_655 . . . ? Cl2 Co1 N1 C7 -93.3(4) . . . . ? Cl1 Co1 N1 C7 86.7(4) . . . . ? C6 C1 C2 C3 -1.9(9) . . . . ? C8 C1 C2 C3 172.4(6) 16_655 . . . ? C1 C2 C3 O1 -176.6(6) . . . . ? C1 C2 C3 C4 0.7(9) . . . . ? C9 O1 C3 C2 1.8(9) . . . . ? C9 O1 C3 C4 -175.7(6) . . . . ? C21B O2 C4 C5 15.6(10) . . . . ? C21A O2 C4 C5 -6.3(10) . . . . ? C21B O2 C4 C3 -167.7(6) . . . . ? C21A O2 C4 C3 170.5(6) . . . . ? C2 C3 C4 O2 -176.7(6) . . . . ? O1 C3 C4 O2 0.9(8) . . . . ? C2 C3 C4 C5 0.2(10) . . . . ? O1 C3 C4 C5 177.9(6) . . . . ? O2 C4 C5 C6 176.6(6) . . . . ? C3 C4 C5 C6 0.0(10) . . . . ? C2 C1 C6 C5 2.3(9) . . . . ? C8 C1 C6 C5 -173.4(6) 16_655 . . . ? C2 C1 C6 C7 174.6(5) . . . . ? C8 C1 C6 C7 -1.1(6) 16_655 . . . ? C4 C5 C6 C1 -1.2(9) . . . . ? C4 C5 C6 C7 -171.5(6) . . . . ? C8 N2 C7 N1 -2.8(8) . . . . ? C8 N2 C7 C6 172.7(5) . . . . ? C8 N1 C7 N2 176.2(5) 16_655 . . . ? Co1 N1 C7 N2 2.8(8) . . . . ? C8 N1 C7 C6 0.3(6) 16_655 . . . ? Co1 N1 C7 C6 -173.2(4) . . . . ? C1 C6 C7 N2 -175.7(5) . . . . ? C5 C6 C7 N2 -4.2(9) . . . . ? C1 C6 C7 N1 0.6(6) . . . . ? C5 C6 C7 N1 172.0(6) . . . . ? C7 N2 C8 N1 4.2(8) . . . 15_565 ? C7 N2 C8 C1 -173.3(5) . . . 15_565 ? C3 O1 C9 C14 -99.5(7) . . . . ? C3 O1 C9 C10 86.6(7) . . . . ? C14 C9 C10 C11 -0.3(10) . . . . ? O1 C9 C10 C11 173.2(6) . . . . ? C14 C9 C10 C15 -175.9(6) . . . . ? O1 C9 C10 C15 -2.3(9) . . . . ? C9 C10 C11 C12 1.5(12) . . . . ? C15 C10 C11 C12 177.2(8) . . . . ? C10 C11 C12 C13 0.4(16) . . . . ? C11 C12 C13 C14 -3.3(17) . . . . ? C10 C9 C14 C13 -2.4(10) . . . . ? O1 C9 C14 C13 -176.1(6) . . . . ? C10 C9 C14 C18 177.9(7) . . . . ? O1 C9 C14 C18 4.3(10) . . . . ? C12 C13 C14 C9 4.2(13) . . . . ? C12 C13 C14 C18 -176.1(9) . . . . ? C9 C10 C15 C17 -162.2(7) . . . . ? C11 C10 C15 C17 22.1(10) . . . . ? C9 C10 C15 C16 73.0(8) . . . . ? C11 C10 C15 C16 -102.7(8) . . . . ? C9 C14 C18 C20 -83.4(10) . . . . ? C13 C14 C18 C20 97.0(11) . . . . ? C9 C14 C18 C19 150.7(8) . . . . ? C13 C14 C18 C19 -28.9(13) . . . . ? C21B O2 C21A C22A 12.8(16) . . . . ? C4 O2 C21A C22A 101.1(6) . . . . ? C21B O2 C21A C26A -167(2) . . . . ? C4 O2 C21A C26A -78.8(8) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A -179.9(7) . . . . ? C26A C21A C22A C27A 175.4(13) . . . . ? O2 C21A C22A C27A -4.6(12) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -175.8(11) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 174.6(10) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -174.7(10) . . . . ? O2 C21A C26A C30 5.2(10) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A 179.9(8) . . . . ? C4 O2 C21B C22B 91.6(7) . . . . ? C21A O2 C21B C22B -167(2) . . . . ? C4 O2 C21B C26B -87.8(7) . . . . ? C21A O2 C21B C26B 13.5(15) . . . . ? O2 C21B C22B C23B -179.4(8) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B -0.1(10) . . . . ? C26B C21B C22B C27B 179.3(10) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -179.3(10) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? O2 C21B C26B C25B 179.4(7) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -1.8(7) . . . . ? C22B C21B C26B C30 178.8(7) . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -178.8(7) . . . . ? C23A C22A C27A C28A -112.7(17) . . . . ? C21A C22A C27A C28A 72(2) . . . . ? C23A C22A C27A C29A 39(3) . . . . ? C21A C22A C27A C29A -137(3) . . . . ? C23B C22B C27B C28B -66.0(17) . . . . ? C21B C22B C27B C28B 114.7(14) . . . . ? C23B C22B C27B C29B 84(2) . . . . ? C21B C22B C27B C29B -95.2(19) . . . . ? C25A C26A C30 C31 74.2(10) . . . . ? C21A C26A C30 C31 -111.1(9) . . . . ? C25A C26A C30 C32B -62.6(17) . . . . ? C21A C26A C30 C32B 112.1(15) . . . . ? C25A C26A C30 C26B -136(3) . . . . ? C21A C26A C30 C26B 38(3) . . . . ? C25A C26A C30 C32A -35.6(14) . . . . ? C21A C26A C30 C32A 139.1(12) . . . . ? C21B C26B C30 C26A -134(3) . . . . ? C25B C26B C30 C26A 45(3) . . . . ? C21B C26B C30 C31 -100.6(9) . . . . ? C25B C26B C30 C31 78.2(9) . . . . ? C21B C26B C30 C32B 112.6(14) . . . . ? C25B C26B C30 C32B -68.6(15) . . . . ? C21B C26B C30 C32A 143.5(12) . . . . ? C25B C26B C30 C32A -37.7(13) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.21 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.191 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.145 data_PNC[cCl0.67-Co3+-vCl0.68] _database_code_depnum_ccdc_archive 'CCDC 900374' #TrackingRef '900374_PNC[cCl0.67-Co3+-vCl0.68].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130.50 H154.25 Cl3.75 Cl1.27 Co N8 O11.25' _chemical_formula_weight 2251.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.365(4) _cell_length_b 37.365(4) _cell_length_c 37.365(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52166(10) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 54797 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 21.3 _exptl_crystal_description Prism _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.860 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 14348 _exptl_absorpt_coefficient_mu 0.219 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9902 _exptl_absorpt_correction_T_max 0.9902 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5324 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 21.27 _reflns_number_total 5324 _reflns_number_gt 4044 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5324 _refine_ls_number_parameters 315 _refine_ls_number_restraints 309 _refine_ls_R_factor_all 0.1491 _refine_ls_R_factor_gt 0.1318 _refine_ls_wR_factor_ref 0.3949 _refine_ls_wR_factor_gt 0.3742 _refine_ls_goodness_of_fit_ref 1.647 _refine_ls_restrained_S_all 1.684 _refine_ls_shift/su_max 0.004 _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 0.7500 0.7500 0.08334(4) 0.0657(6) Uani 1 4 d SU . . O1 O 0.88894(10) 0.59508(10) 0.11041(11) 0.0844(12) Uani 1 1 d U A . O2 O 0.83125(9) 0.55948(9) 0.11081(12) 0.0922(13) Uani 1 1 d U . . N1 N 0.77829(10) 0.70692(10) 0.08398(12) 0.0699(12) Uani 1 1 d U A . N2 N 0.73141(11) 0.66202(11) 0.08657(13) 0.0750(12) Uani 1 1 d U A . C1 C 0.82551(13) 0.66757(13) 0.08996(15) 0.0719(14) Uani 1 1 d U . . C2 C 0.85897(14) 0.65100(14) 0.09654(16) 0.0753(15) Uani 1 1 d U A . H2 H 0.8806 0.6644 0.0969 0.090 Uiso 1 1 calc R . . C3 C 0.85894(13) 0.61506(14) 0.10232(15) 0.0759(15) Uani 1 1 d U . . C4 C 0.82716(14) 0.59497(14) 0.10239(17) 0.0832(16) Uani 1 1 d U A . C5 C 0.79444(15) 0.61074(13) 0.09497(17) 0.0823(16) Uani 1 1 d U . . H5 H 0.7730 0.5971 0.0939 0.099 Uiso 1 1 calc R A . C6 C 0.79461(13) 0.64765(13) 0.08915(14) 0.0724(14) Uani 1 1 d U A . C7 C 0.76528(15) 0.67247(13) 0.08589(15) 0.0719(14) Uani 1 1 d U . . C8 C 0.70471(13) 0.68524(13) 0.08645(14) 0.0693(14) Uani 1 1 d U . . C9 C 0.92212(14) 0.61243(16) 0.11380(19) 0.0881(16) Uani 1 1 d U . . C10 C 0.93107(16) 0.62694(16) 0.1471(2) 0.0965(17) Uani 1 1 d U A . C11 C 0.9652(2) 0.6413(2) 0.1502(3) 0.130(3) Uani 1 1 d U . . H11 H 0.9725 0.6514 0.1724 0.156 Uiso 1 1 calc R A . C12 C 0.9877(2) 0.6411(3) 0.1229(4) 0.152(3) Uani 1 1 d U A . H12 H 1.0108 0.6513 0.1257 0.182 Uiso 1 1 calc R . . C13 C 0.9782(2) 0.6261(3) 0.0895(3) 0.147(3) Uani 1 1 d U . . H13 H 0.9948 0.6264 0.0702 0.177 Uiso 1 1 calc R A . C14 C 0.94460(18) 0.6108(2) 0.0848(2) 0.112(2) Uani 1 1 d U A . C15 C 0.9042(2) 0.62540(18) 0.17782(19) 0.1061(19) Uani 1 1 d U . . H15 H 0.8800 0.6313 0.1680 0.127 Uiso 1 1 calc R A . C16 C 0.9025(2) 0.58830(19) 0.1935(2) 0.111(2) Uani 1 1 d U A . H16A H 0.8957 0.5712 0.1748 0.166 Uiso 1 1 calc R . . H16B H 0.8846 0.5877 0.2127 0.166 Uiso 1 1 calc R . . H16C H 0.9260 0.5818 0.2032 0.166 Uiso 1 1 calc R . . C17 C 0.9128(3) 0.6527(2) 0.2081(2) 0.146(3) Uani 1 1 d U A . H17A H 0.9302 0.6422 0.2246 0.219 Uiso 1 1 calc R . . H17B H 0.8908 0.6586 0.2211 0.219 Uiso 1 1 calc R . . H17C H 0.9228 0.6746 0.1975 0.219 Uiso 1 1 calc R . . C18 C 0.9332(3) 0.5938(2) 0.0499(2) 0.135(2) Uani 1 1 d U . . H18 H 0.9068 0.5977 0.0471 0.162 Uiso 1 1 calc R A . C19 C 0.9513(4) 0.6083(4) 0.0171(3) 0.228(6) Uani 1 1 d U A . H19A H 0.9511 0.5901 -0.0018 0.343 Uiso 1 1 calc R . . H19B H 0.9761 0.6147 0.0229 0.343 Uiso 1 1 calc R . . H19C H 0.9385 0.6297 0.0088 0.343 Uiso 1 1 calc R . . C20 C 0.9394(3) 0.5550(3) 0.0529(4) 0.179(4) Uani 1 1 d U A . H20A H 0.9167 0.5430 0.0585 0.269 Uiso 1 1 calc R . . H20B H 0.9566 0.5504 0.0721 0.269 Uiso 1 1 calc R . . H20C H 0.9488 0.5459 0.0303 0.269 Uiso 1 1 calc R . . C21A C 0.7987(3) 0.5371(3) 0.1102(3) 0.062(4) Uiso 0.412(12) 1 d PGU A 1 C22A C 0.7873(3) 0.5164(3) 0.0815(2) 0.107(5) Uiso 0.412(12) 1 d PGDU A 1 C23A C 0.7564(3) 0.4959(3) 0.0844(3) 0.088(5) Uiso 0.412(12) 1 d PGU A 1 H23A H 0.7487 0.4817 0.0648 0.105 Uiso 0.412(12) 1 calc PR A 1 C24A C 0.7368(2) 0.4962(3) 0.1161(3) 0.091(5) Uiso 0.412(12) 1 d PGU A 1 H24A H 0.7157 0.4822 0.1181 0.109 Uiso 0.412(12) 1 calc PR A 1 C25A C 0.7482(3) 0.5169(3) 0.1448(3) 0.087(4) Uiso 0.412(12) 1 d PGU A 1 H25A H 0.7348 0.5171 0.1664 0.104 Uiso 0.412(12) 1 calc PR A 1 C26A C 0.7791(3) 0.5374(3) 0.1419(2) 0.087(5) Uiso 0.412(12) 1 d PGDU A 1 C21B C 0.8032(2) 0.5406(3) 0.1067(2) 0.106(5) Uiso 0.588(12) 1 d PGU A 2 C22B C 0.8000(2) 0.5223(3) 0.0745(2) 0.091(3) Uiso 0.588(12) 1 d PGDU A 2 C23B C 0.7700(3) 0.5012(2) 0.0680(2) 0.120(4) Uiso 0.588(12) 1 d PGU A 2 H23B H 0.7679 0.4886 0.0459 0.144 Uiso 0.588(12) 1 calc PR A 2 C24B C 0.7433(2) 0.4983(3) 0.0937(3) 0.127(5) Uiso 0.588(12) 1 d PGU A 2 H24B H 0.7228 0.4839 0.0892 0.152 Uiso 0.588(12) 1 calc PR A 2 C25B C 0.7465(2) 0.5167(3) 0.1259(3) 0.115(4) Uiso 0.588(12) 1 d PGU A 2 H25B H 0.7282 0.5147 0.1435 0.138 Uiso 0.588(12) 1 calc PR A 2 C26B C 0.7764(2) 0.5378(3) 0.1324(2) 0.101(4) Uiso 0.588(12) 1 d PGDU A 2 C27A C 0.8112(4) 0.5184(5) 0.0495(3) 0.094(5) Uiso 0.412(12) 1 d PDU A 1 H27A H 0.8168 0.5445 0.0499 0.113 Uiso 0.412(12) 1 calc PR A 1 C28A C 0.8487(5) 0.5037(9) 0.0539(9) 0.175(12) Uiso 0.412(12) 1 d PDU A 1 H28D H 0.8587 0.4980 0.0303 0.262 Uiso 0.412(12) 1 calc PR A 1 H28E H 0.8480 0.4820 0.0685 0.262 Uiso 0.412(12) 1 calc PR A 1 H28F H 0.8638 0.5217 0.0656 0.262 Uiso 0.412(12) 1 calc PR A 1 C29A C 0.8011(8) 0.5145(9) 0.0106(5) 0.185(11) Uiso 0.412(12) 1 d PDU A 1 H29A H 0.7915 0.5372 0.0018 0.277 Uiso 0.412(12) 1 calc PR A 1 H29B H 0.7830 0.4957 0.0081 0.277 Uiso 0.412(12) 1 calc PR A 1 H29C H 0.8224 0.5080 -0.0034 0.277 Uiso 0.412(12) 1 calc PR A 1 C27B C 0.8281(4) 0.5258(3) 0.0461(3) 0.114(4) Uiso 0.588(12) 1 d PDU A 2 H27B H 0.8464 0.5409 0.0585 0.137 Uiso 0.588(12) 1 calc PR A 2 C28B C 0.8480(4) 0.4915(4) 0.0415(5) 0.127(5) Uiso 0.588(12) 1 d PDU A 2 H28A H 0.8723 0.4966 0.0332 0.190 Uiso 0.588(12) 1 calc PR A 2 H28B H 0.8356 0.4766 0.0239 0.190 Uiso 0.588(12) 1 calc PR A 2 H28C H 0.8490 0.4789 0.0645 0.190 Uiso 0.588(12) 1 calc PR A 2 C29B C 0.8191(6) 0.5485(6) 0.0149(5) 0.195(9) Uiso 0.588(12) 1 d PDU A 2 H29D H 0.8067 0.5701 0.0231 0.292 Uiso 0.588(12) 1 calc PR A 2 H29E H 0.8035 0.5352 -0.0014 0.292 Uiso 0.588(12) 1 calc PR A 2 H29F H 0.8411 0.5553 0.0023 0.292 Uiso 0.588(12) 1 calc PR A 2 C30 C 0.7837(2) 0.55962(19) 0.16990(19) 0.140(3) Uani 1 1 d DU . . H30 H 0.7997 0.5804 0.1646 0.168 Uiso 1 1 calc R A 1 C31 C 0.7961(3) 0.5375(3) 0.2008(3) 0.166(4) Uani 1 1 d U A . H31A H 0.7773 0.5204 0.2074 0.249 Uiso 1 1 calc R . . H31B H 0.8012 0.5532 0.2213 0.249 Uiso 1 1 calc R . . H31C H 0.8178 0.5245 0.1942 0.249 Uiso 1 1 calc R . . C32A C 0.7452(4) 0.5704(7) 0.1792(6) 0.163(9) Uiso 0.53(2) 1 d PDU A 1 H32A H 0.7293 0.5498 0.1756 0.245 Uiso 0.53(2) 1 calc PR A 1 H32B H 0.7377 0.5902 0.1638 0.245 Uiso 0.53(2) 1 calc PR A 1 H32C H 0.7441 0.5779 0.2043 0.245 Uiso 0.53(2) 1 calc PR A 1 C32B C 0.7642(5) 0.5926(4) 0.1833(4) 0.108(7) Uiso 0.47(2) 1 d PDU A 2 H32D H 0.7749 0.6005 0.2059 0.163 Uiso 0.47(2) 1 calc PR A 2 H32E H 0.7389 0.5868 0.1872 0.163 Uiso 0.47(2) 1 calc PR A 2 H32F H 0.7661 0.6117 0.1655 0.163 Uiso 0.47(2) 1 calc PR A 2 Cl1 Cl 0.7500 0.7500 0.14219(11) 0.0699(17) Uani 0.669(12) 4 d SPU . . Cl2 Cl 0.7500 0.7500 0.02721(15) 0.099(2) Uani 0.681(14) 4 d SPU . . O1S O 0.7137(7) 0.5898(7) 0.0343(7) 0.152(8) Uiso 0.25 1 d P . . O2S O 0.8164(6) 0.6842(6) 0.1851(7) 0.146(8) Uiso 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0545(7) 0.0545(7) 0.0881(11) 0.000 0.000 0.000 O1 0.064(2) 0.074(2) 0.115(3) 0.003(2) -0.0094(19) 0.0109(17) O2 0.061(2) 0.064(2) 0.152(4) 0.014(2) -0.011(2) -0.0009(16) N1 0.054(2) 0.058(2) 0.097(3) -0.006(2) -0.001(2) 0.0019(18) N2 0.060(2) 0.057(2) 0.108(3) 0.002(2) -0.003(2) 0.003(2) C1 0.063(3) 0.063(3) 0.090(4) 0.002(3) -0.012(3) 0.003(2) C2 0.055(3) 0.068(3) 0.102(4) 0.005(3) -0.006(3) 0.000(2) C3 0.059(3) 0.068(3) 0.101(4) -0.003(3) -0.011(3) 0.010(2) C4 0.064(3) 0.059(3) 0.127(5) -0.003(3) -0.013(3) 0.013(2) C5 0.066(3) 0.059(3) 0.122(4) 0.002(3) -0.008(3) 0.002(2) C6 0.060(3) 0.062(3) 0.096(4) 0.000(3) -0.007(3) 0.004(2) C7 0.065(3) 0.057(3) 0.094(4) 0.000(2) -0.011(3) -0.004(2) C8 0.060(3) 0.057(3) 0.091(4) -0.001(2) -0.005(3) -0.004(2) C9 0.060(3) 0.081(4) 0.123(4) 0.028(3) -0.008(3) 0.007(3) C10 0.077(3) 0.085(4) 0.128(4) 0.031(3) -0.036(3) -0.005(3) C11 0.088(4) 0.122(5) 0.180(7) 0.064(5) -0.057(4) -0.023(4) C12 0.075(5) 0.159(8) 0.221(9) 0.096(7) -0.043(5) -0.019(5) C13 0.072(4) 0.182(8) 0.188(7) 0.090(6) 0.005(4) 0.015(4) C14 0.075(4) 0.131(5) 0.130(5) 0.042(4) 0.006(3) 0.025(3) C15 0.108(4) 0.096(4) 0.115(4) 0.009(3) -0.032(4) -0.006(4) C16 0.123(5) 0.099(4) 0.111(5) 0.011(4) 0.006(4) -0.002(4) C17 0.200(9) 0.101(5) 0.137(6) -0.009(4) -0.053(6) 0.021(5) C18 0.139(6) 0.138(6) 0.128(5) 0.021(4) 0.035(5) 0.032(5) C19 0.288(16) 0.245(13) 0.153(8) 0.034(8) 0.045(10) -0.063(12) C20 0.185(10) 0.129(6) 0.225(12) 0.012(6) -0.037(8) 0.032(7) C30 0.129(6) 0.124(6) 0.167(7) 0.048(5) 0.056(5) 0.055(5) C31 0.154(8) 0.138(7) 0.205(9) 0.044(7) -0.008(7) 0.028(6) Cl1 0.063(2) 0.063(2) 0.085(3) 0.000 0.000 0.000 Cl2 0.090(3) 0.090(3) 0.116(4) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.926(4) 16_655 ? Co1 N1 1.926(4) 15_565 ? Co1 N1 1.926(4) . ? Co1 N1 1.926(4) 2_665 ? Co1 Cl2 2.098(6) . ? Co1 Cl1 2.199(4) . ? O1 C3 1.380(6) . ? O1 C9 1.405(7) . ? O2 C21B 1.274(7) . ? O2 C4 1.371(6) . ? O2 C21A 1.476(8) . ? N1 C8 1.368(6) 16_655 ? N1 C7 1.378(6) . ? N2 C8 1.322(7) . ? N2 C7 1.325(7) . ? C1 C6 1.374(7) . ? C1 C2 1.417(7) . ? C1 C8 1.451(7) 16_655 ? C2 C3 1.360(7) . ? C2 H2 0.9500 . ? C3 C4 1.405(8) . ? C4 C5 1.385(7) . ? C5 C6 1.396(7) . ? C5 H5 0.9500 . ? C6 C7 1.441(7) . ? C8 N1 1.368(6) 15_565 ? C8 C1 1.451(7) 15_565 ? C9 C14 1.371(9) . ? C9 C10 1.397(9) . ? C10 C11 1.389(9) . ? C10 C15 1.528(10) . ? C11 C12 1.323(13) . ? C11 H11 0.9500 . ? C12 C13 1.413(15) . ? C12 H12 0.9500 . ? C13 C14 1.390(12) . ? C13 H13 0.9500 . ? C14 C18 1.513(12) . ? C15 C16 1.506(9) . ? C15 C17 1.557(10) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.472(12) . ? C18 C19 1.502(12) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.495(9) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.348(7) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.501(9) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.644(8) . ? C27A C29A 1.508(10) . ? C27A C28A 1.513(10) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.481(10) . ? C27B C28B 1.489(9) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.494(11) . ? C30 C32B 1.518(9) . ? C30 C32A 1.535(9) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 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 N1 Co1 N1 178.6(3) 16_655 15_565 ? N1 Co1 N1 89.991(4) 16_655 . ? N1 Co1 N1 89.991(4) 15_565 . ? N1 Co1 N1 89.991(4) 16_655 2_665 ? N1 Co1 N1 89.991(4) 15_565 2_665 ? N1 Co1 N1 178.6(3) . 2_665 ? N1 Co1 Cl2 90.70(14) 16_655 . ? N1 Co1 Cl2 90.70(14) 15_565 . ? N1 Co1 Cl2 90.70(14) . . ? N1 Co1 Cl2 90.70(14) 2_665 . ? N1 Co1 Cl1 89.30(14) 16_655 . ? N1 Co1 Cl1 89.30(14) 15_565 . ? N1 Co1 Cl1 89.30(14) . . ? N1 Co1 Cl1 89.30(14) 2_665 . ? Cl2 Co1 Cl1 180.000(1) . . ? C3 O1 C9 119.1(4) . . ? C21B O2 C4 114.7(6) . . ? C21B O2 C21A 6.1(7) . . ? C4 O2 C21A 116.9(6) . . ? C8 N1 C7 107.0(4) 16_655 . ? C8 N1 Co1 126.7(3) 16_655 . ? C7 N1 Co1 126.0(3) . . ? C8 N2 C7 121.8(4) . . ? C6 C1 C2 120.6(5) . . ? C6 C1 C8 106.5(4) . 16_655 ? C2 C1 C8 132.7(5) . 16_655 ? C3 C2 C1 117.3(5) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? C2 C3 O1 124.6(5) . . ? C2 C3 C4 121.9(5) . . ? O1 C3 C4 113.4(5) . . ? O2 C4 C5 123.7(5) . . ? O2 C4 C3 115.0(4) . . ? C5 C4 C3 121.2(5) . . ? C4 C5 C6 116.6(5) . . ? C4 C5 H5 121.7 . . ? C6 C5 H5 121.7 . . ? C1 C6 C5 122.4(5) . . ? C1 C6 C7 107.0(4) . . ? C5 C6 C7 130.2(5) . . ? N2 C7 N1 127.8(5) . . ? N2 C7 C6 122.4(4) . . ? N1 C7 C6 109.7(4) . . ? N2 C8 N1 127.5(4) . 15_565 ? N2 C8 C1 122.7(4) . 15_565 ? N1 C8 C1 109.8(4) 15_565 15_565 ? C14 C9 C10 124.9(6) . . ? C14 C9 O1 116.7(6) . . ? C10 C9 O1 118.1(6) . . ? C11 C10 C9 116.4(7) . . ? C11 C10 C15 123.7(7) . . ? C9 C10 C15 119.8(5) . . ? C12 C11 C10 121.1(9) . . ? C12 C11 H11 119.5 . . ? C10 C11 H11 119.5 . . ? C11 C12 C13 121.6(9) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C14 C13 C12 120.0(9) . . ? C14 C13 H13 120.0 . . ? C12 C13 H13 120.0 . . ? C9 C14 C13 115.9(9) . . ? C9 C14 C18 121.7(7) . . ? C13 C14 C18 122.3(8) . . ? C16 C15 C10 110.8(6) . . ? C16 C15 C17 109.3(6) . . ? C10 C15 C17 112.6(7) . . ? C16 C15 H15 108.0 . . ? C10 C15 H15 108.0 . . ? C17 C15 H15 108.0 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 110.3(10) . . ? C20 C18 C14 107.7(8) . . ? C19 C18 C14 115.2(9) . . ? C20 C18 H18 107.8 . . ? C19 C18 H18 107.8 . . ? C14 C18 H18 107.8 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 125.3(6) . . ? C26A C21A O2 114.7(6) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 114.1(9) . . ? C23A C22A C27A 125.9(9) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 112.6(7) . . ? C30 C26A C21A 126.7(7) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 116.6(6) . . ? O2 C21B C26B 123.4(6) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 119.3(8) . . ? C21B C22B C27B 120.6(8) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 124.4(6) . . ? C21B C26B C30 115.6(6) . . ? C22A C27A C29A 128.1(16) . . ? C22A C27A C28A 116.6(16) . . ? C29A C27A C28A 107.5(18) . . ? C22A C27A H27A 99.2 . . ? C29A C27A H27A 99.2 . . ? C28A C27A H27A 99.2 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 121.1(13) . . ? C29B C27B C22B 116.6(13) . . ? C28B C27B C22B 110.8(10) . . ? C29B C27B H27B 101.4 . . ? C28B C27B H27B 101.4 . . ? C22B C27B H27B 101.4 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 107.5(9) . . ? C26A C30 C32B 134.0(10) . . ? C31 C30 C32B 110.0(9) . . ? C26A C30 C32A 102.5(12) . . ? C31 C30 C32A 104.9(10) . . ? C32B C30 C32A 42.3(9) . . ? C26A C30 C26B 8.4(9) . . ? C31 C30 C26B 115.9(8) . . ? C32B C30 C26B 127.2(9) . . ? C32A C30 C26B 99.6(11) . . ? C26A C30 H30 113.6 . . ? C31 C30 H30 113.6 . . ? C32B C30 H30 73.8 . . ? C32A C30 H30 113.6 . . ? C26B C30 H30 108.4 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C8 3.6(5) 16_655 . . 16_655 ? N1 Co1 N1 C8 -175.0(3) 15_565 . . 16_655 ? N1 Co1 N1 C8 -85.7(4) 2_665 . . 16_655 ? Cl2 Co1 N1 C8 94.3(4) . . . 16_655 ? Cl1 Co1 N1 C8 -85.7(4) . . . 16_655 ? N1 Co1 N1 C7 176.1(3) 16_655 . . . ? N1 Co1 N1 C7 -2.5(5) 15_565 . . . ? N1 Co1 N1 C7 86.8(4) 2_665 . . . ? Cl2 Co1 N1 C7 -93.2(4) . . . . ? Cl1 Co1 N1 C7 86.8(4) . . . . ? C6 C1 C2 C3 -0.7(8) . . . . ? C8 C1 C2 C3 172.7(6) 16_655 . . . ? C1 C2 C3 O1 -177.5(5) . . . . ? C1 C2 C3 C4 -1.0(9) . . . . ? C9 O1 C3 C2 1.3(8) . . . . ? C9 O1 C3 C4 -175.4(5) . . . . ? C21B O2 C4 C5 9.0(9) . . . . ? C21A O2 C4 C5 2.7(9) . . . . ? C21B O2 C4 C3 -172.1(6) . . . . ? C21A O2 C4 C3 -178.4(6) . . . . ? C2 C3 C4 O2 -176.1(6) . . . . ? O1 C3 C4 O2 0.8(8) . . . . ? C2 C3 C4 C5 2.9(10) . . . . ? O1 C3 C4 C5 179.8(5) . . . . ? O2 C4 C5 C6 176.0(6) . . . . ? C3 C4 C5 C6 -2.9(9) . . . . ? C2 C1 C6 C5 0.6(9) . . . . ? C8 C1 C6 C5 -174.4(5) 16_655 . . . ? C2 C1 C6 C7 173.8(5) . . . . ? C8 C1 C6 C7 -1.1(6) 16_655 . . . ? C4 C5 C6 C1 1.3(9) . . . . ? C4 C5 C6 C7 -170.3(6) . . . . ? C8 N2 C7 N1 -2.0(9) . . . . ? C8 N2 C7 C6 174.5(5) . . . . ? C8 N1 C7 N2 175.9(5) 16_655 . . . ? Co1 N1 C7 N2 2.2(8) . . . . ? C8 N1 C7 C6 -0.9(6) 16_655 . . . ? Co1 N1 C7 C6 -174.6(4) . . . . ? C1 C6 C7 N2 -175.8(5) . . . . ? C5 C6 C7 N2 -3.2(9) . . . . ? C1 C6 C7 N1 1.2(6) . . . . ? C5 C6 C7 N1 173.8(6) . . . . ? C7 N2 C8 N1 3.3(9) . . . 15_565 ? C7 N2 C8 C1 -175.1(5) . . . 15_565 ? C3 O1 C9 C14 -99.5(6) . . . . ? C3 O1 C9 C10 86.3(6) . . . . ? C14 C9 C10 C11 1.3(9) . . . . ? O1 C9 C10 C11 174.9(5) . . . . ? C14 C9 C10 C15 -176.9(6) . . . . ? O1 C9 C10 C15 -3.3(8) . . . . ? C9 C10 C11 C12 0.1(10) . . . . ? C15 C10 C11 C12 178.3(7) . . . . ? C10 C11 C12 C13 -0.6(13) . . . . ? C11 C12 C13 C14 -0.3(13) . . . . ? C10 C9 C14 C13 -2.2(10) . . . . ? O1 C9 C14 C13 -175.9(6) . . . . ? C10 C9 C14 C18 178.4(6) . . . . ? O1 C9 C14 C18 4.7(9) . . . . ? C12 C13 C14 C9 1.6(11) . . . . ? C12 C13 C14 C18 -179.0(7) . . . . ? C11 C10 C15 C16 -102.2(7) . . . . ? C9 C10 C15 C16 75.9(7) . . . . ? C11 C10 C15 C17 20.5(9) . . . . ? C9 C10 C15 C17 -161.4(6) . . . . ? C9 C14 C18 C20 -84.2(9) . . . . ? C13 C14 C18 C20 96.4(10) . . . . ? C9 C14 C18 C19 152.2(9) . . . . ? C13 C14 C18 C19 -27.1(12) . . . . ? C21B O2 C21A C22A 26(8) . . . . ? C4 O2 C21A C22A 95.2(9) . . . . ? C21B O2 C21A C26A -155(9) . . . . ? C4 O2 C21A C26A -85.8(8) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 178.9(11) . . . . ? C26A C21A C22A C27A -179.4(11) . . . . ? O2 C21A C22A C27A -0.4(12) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A 179.3(13) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 171.4(11) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -170.1(13) . . . . ? O2 C21A C26A C30 10.9(11) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -179.1(10) . . . . ? C4 O2 C21B C22B 95.7(7) . . . . ? C21A O2 C21B C22B -151(9) . . . . ? C4 O2 C21B C26B -84.1(8) . . . . ? C21A O2 C21B C26B 29(8) . . . . ? O2 C21B C22B C23B -179.8(10) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B -1.4(10) . . . . ? C26B C21B C22B C27B 178.4(9) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -178.4(9) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -178.0(9) . . . . ? O2 C21B C26B C25B 179.8(11) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -2.0(8) . . . . ? C22B C21B C26B C30 178.2(9) . . . . ? C21A C22A C27A C29A -149.9(19) . . . . ? C23A C22A C27A C29A 31(2) . . . . ? C21A C22A C27A C28A 65(2) . . . . ? C23A C22A C27A C28A -114.5(19) . . . . ? C23B C22B C27B C29B 74.0(16) . . . . ? C21B C22B C27B C29B -104.4(15) . . . . ? C23B C22B C27B C28B -69.8(14) . . . . ? C21B C22B C27B C28B 111.8(12) . . . . ? C25A C26A C30 C31 75.3(9) . . . . ? C21A C26A C30 C31 -114.1(10) . . . . ? C25A C26A C30 C32B -68.1(15) . . . . ? C21A C26A C30 C32B 102.6(14) . . . . ? C25A C26A C30 C32A -35.0(12) . . . . ? C21A C26A C30 C32A 135.6(12) . . . . ? C25A C26A C30 C26B -106(4) . . . . ? C21A C26A C30 C26B 65(4) . . . . ? C25B C26B C30 C26A 75(4) . . . . ? C21B C26B C30 C26A -103(4) . . . . ? C25B C26B C30 C31 76.2(10) . . . . ? C21B C26B C30 C31 -101.9(8) . . . . ? C25B C26B C30 C32B -71.3(14) . . . . ? C21B C26B C30 C32B 110.6(11) . . . . ? C25B C26B C30 C32A -35.6(13) . . . . ? C21B C26B C30 C32A 146.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 21.27 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.822 _refine_diff_density_min -0.327 _refine_diff_density_rms 0.089 data_PNC[cH2O-Co-vMeOH] _database_code_depnum_ccdc_archive 'CCDC 900375' #TrackingRef '900375_PNC[cH2O-Co-vMeOH].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C130 H157.17 Cl1.50 Co N8 O12.67' _chemical_formula_weight 2146.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.6395(3) _cell_length_b 37.6395(3) _cell_length_c 37.6395(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 53325.1(7) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Colorless _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.802 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13764 _exptl_absorpt_coefficient_mu 0.162 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.4011 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7866 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0147 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 24.20 _reflns_number_total 7866 _reflns_number_gt 7012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7866 _refine_ls_number_parameters 311 _refine_ls_number_restraints 306 _refine_ls_R_factor_all 0.1101 _refine_ls_R_factor_gt 0.1043 _refine_ls_wR_factor_ref 0.3528 _refine_ls_wR_factor_gt 0.3445 _refine_ls_goodness_of_fit_ref 1.603 _refine_ls_restrained_S_all 1.651 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.08547(2) 0.0468(4) Uani 1 4 d SU . . O1 O 0.88759(5) 0.59564(5) 0.11191(6) 0.0551(6) Uani 1 1 d U A . O2 O 0.83041(5) 0.56031(5) 0.11241(6) 0.0570(6) Uani 1 1 d U . . N1 N 0.77787(6) 0.70720(5) 0.08737(7) 0.0473(6) Uani 1 1 d U A . N2 N 0.73141(6) 0.66272(5) 0.08969(7) 0.0492(6) Uani 1 1 d U A . C1 C 0.82490(7) 0.66803(7) 0.09312(8) 0.0485(7) Uani 1 1 d U . . C2 C 0.85788(7) 0.65175(7) 0.09884(8) 0.0509(7) Uani 1 1 d U A . H2 H 0.8793 0.6651 0.0986 0.061 Uiso 1 1 calc R . . C3 C 0.85807(7) 0.61578(7) 0.10486(8) 0.0495(7) Uani 1 1 d U . . C4 C 0.82620(7) 0.59560(7) 0.10434(8) 0.0492(7) Uani 1 1 d U A . C5 C 0.79387(7) 0.61177(7) 0.09795(9) 0.0518(7) Uani 1 1 d U . . H5 H 0.7725 0.5984 0.0973 0.062 Uiso 1 1 calc R A . C6 C 0.79380(6) 0.64834(7) 0.09246(8) 0.0484(7) Uani 1 1 d U A . C7 C 0.76484(7) 0.67330(6) 0.08907(8) 0.0484(7) Uani 1 1 d U . . C8 C 0.70487(7) 0.68578(6) 0.08928(7) 0.0462(6) Uani 1 1 d U . . C9 C 0.92047(7) 0.61271(7) 0.11457(9) 0.0557(7) Uani 1 1 d U . . C10 C 0.92977(8) 0.62683(8) 0.14762(10) 0.0638(8) Uani 1 1 d U A . C11 C 0.96421(10) 0.64102(10) 0.15052(13) 0.0824(11) Uani 1 1 d U . . H11 H 0.9718 0.6509 0.1725 0.099 Uiso 1 1 calc R A . C12 C 0.98640(10) 0.64076(12) 0.12279(15) 0.0933(14) Uani 1 1 d U A . H12 H 1.0096 0.6504 0.1254 0.112 Uiso 1 1 calc R . . C13 C 0.97636(9) 0.62677(12) 0.09045(14) 0.0897(12) Uani 1 1 d U . . H13 H 0.9927 0.6274 0.0712 0.108 Uiso 1 1 calc R A . C14 C 0.94284(8) 0.61176(9) 0.08511(11) 0.0703(9) Uani 1 1 d U A . C15 C 0.90424(10) 0.62472(9) 0.17868(11) 0.0717(9) Uani 1 1 d U . . H15 H 0.8801 0.6306 0.1694 0.086 Uiso 1 1 calc R A . C16 C 0.90269(12) 0.58730(10) 0.19307(12) 0.0813(11) Uani 1 1 d U A . H16A H 0.8959 0.5709 0.1740 0.122 Uiso 1 1 calc R . . H16B H 0.8851 0.5861 0.2122 0.122 Uiso 1 1 calc R . . H16C H 0.9261 0.5806 0.2024 0.122 Uiso 1 1 calc R . . C17 C 0.91207(15) 0.65039(12) 0.20926(14) 0.0999(14) Uani 1 1 d U A . H17A H 0.9294 0.6396 0.2254 0.150 Uiso 1 1 calc R . . H17B H 0.8901 0.6554 0.2222 0.150 Uiso 1 1 calc R . . H17C H 0.9218 0.6726 0.1997 0.150 Uiso 1 1 calc R . . C18 C 0.93101(11) 0.59343(12) 0.05169(12) 0.0868(11) Uani 1 1 d U . . H18 H 0.9050 0.5978 0.0489 0.104 Uiso 1 1 calc R A . C19 C 0.9499(2) 0.6077(2) 0.01778(19) 0.161(3) Uani 1 1 d U A . H19A H 0.9496 0.5893 -0.0007 0.241 Uiso 1 1 calc R . . H19B H 0.9746 0.6138 0.0235 0.241 Uiso 1 1 calc R . . H19C H 0.9375 0.6289 0.0092 0.241 Uiso 1 1 calc R . . C20 C 0.93650(17) 0.55465(14) 0.05440(18) 0.1179(17) Uani 1 1 d U A . H20A H 0.9243 0.5456 0.0755 0.177 Uiso 1 1 calc R . . H20B H 0.9620 0.5496 0.0563 0.177 Uiso 1 1 calc R . . H20C H 0.9269 0.5430 0.0332 0.177 Uiso 1 1 calc R . . C21A C 0.79991(12) 0.53940(14) 0.11032(13) 0.039(2) Uiso 0.448(8) 1 d PGU A 1 C22A C 0.79121(15) 0.51912(15) 0.08070(12) 0.065(2) Uiso 0.448(8) 1 d PGDU A 1 C23A C 0.76096(16) 0.49794(14) 0.08107(15) 0.069(2) Uiso 0.448(8) 1 d PGU A 1 H23A H 0.7550 0.4841 0.0608 0.082 Uiso 0.448(8) 1 calc PR A 1 C24A C 0.73941(12) 0.49704(15) 0.11104(19) 0.084(3) Uiso 0.448(8) 1 d PGU A 1 H24A H 0.7187 0.4826 0.1113 0.100 Uiso 0.448(8) 1 calc PR A 1 C25A C 0.74811(13) 0.51732(15) 0.14066(16) 0.073(2) Uiso 0.448(8) 1 d PGU A 1 H25A H 0.7334 0.5167 0.1611 0.087 Uiso 0.448(8) 1 calc PR A 1 C26A C 0.77837(14) 0.53850(14) 0.14029(12) 0.0515(17) Uiso 0.448(8) 1 d PGDU A 1 C21B C 0.80200(11) 0.53924(13) 0.10661(12) 0.058(3) Uiso 0.552(8) 1 d PGU A 2 C22B C 0.80091(10) 0.52151(13) 0.07424(11) 0.0556(14) Uiso 0.552(8) 1 d PGDU A 2 C23B C 0.77223(12) 0.49971(11) 0.06610(11) 0.0686(17) Uiso 0.552(8) 1 d PGU A 2 H23B H 0.7715 0.4876 0.0440 0.082 Uiso 0.552(8) 1 calc PR A 2 C24B C 0.74465(10) 0.49565(12) 0.09032(14) 0.0719(19) Uiso 0.552(8) 1 d PGU A 2 H24B H 0.7251 0.4808 0.0847 0.086 Uiso 0.552(8) 1 calc PR A 2 C25B C 0.74575(9) 0.51339(12) 0.12269(12) 0.0609(16) Uiso 0.552(8) 1 d PGU A 2 H25B H 0.7269 0.5106 0.1392 0.073 Uiso 0.552(8) 1 calc PR A 2 C26B C 0.77442(12) 0.53519(12) 0.13084(10) 0.0594(15) Uiso 0.552(8) 1 d PGDU A 2 C27A C 0.8147(3) 0.5212(2) 0.0478(2) 0.077(2) Uiso 0.448(8) 1 d PDU A 1 H27A H 0.8225 0.5466 0.0473 0.093 Uiso 0.448(8) 1 calc PR A 1 C28A C 0.8497(3) 0.5005(5) 0.0492(5) 0.124(5) Uiso 0.448(8) 1 d PDU A 1 H28D H 0.8581 0.4961 0.0249 0.186 Uiso 0.448(8) 1 calc PR A 1 H28E H 0.8459 0.4778 0.0614 0.186 Uiso 0.448(8) 1 calc PR A 1 H28F H 0.8675 0.5144 0.0621 0.186 Uiso 0.448(8) 1 calc PR A 1 C29A C 0.7994(5) 0.5153(6) 0.0112(4) 0.173(7) Uiso 0.448(8) 1 d PDU A 1 H29A H 0.7903 0.5379 0.0018 0.259 Uiso 0.448(8) 1 calc PR A 1 H29B H 0.7799 0.4981 0.0126 0.259 Uiso 0.448(8) 1 calc PR A 1 H29C H 0.8179 0.5063 -0.0047 0.259 Uiso 0.448(8) 1 calc PR A 1 C27B C 0.8316(2) 0.52615(16) 0.04871(16) 0.0683(17) Uiso 0.552(8) 1 d PDU A 2 H27B H 0.8504 0.5403 0.0610 0.082 Uiso 0.552(8) 1 calc PR A 2 C28B C 0.8467(2) 0.4900(2) 0.0408(3) 0.091(3) Uiso 0.552(8) 1 d PDU A 2 H28A H 0.8710 0.4925 0.0320 0.136 Uiso 0.552(8) 1 calc PR A 2 H28B H 0.8321 0.4783 0.0227 0.136 Uiso 0.552(8) 1 calc PR A 2 H28C H 0.8467 0.4757 0.0626 0.136 Uiso 0.552(8) 1 calc PR A 2 C29B C 0.8194(3) 0.5468(3) 0.0171(3) 0.129(4) Uiso 0.552(8) 1 d PDU A 2 H29D H 0.8072 0.5684 0.0250 0.194 Uiso 0.552(8) 1 calc PR A 2 H29E H 0.8031 0.5322 0.0029 0.194 Uiso 0.552(8) 1 calc PR A 2 H29F H 0.8400 0.5533 0.0025 0.194 Uiso 0.552(8) 1 calc PR A 2 C30 C 0.78008(15) 0.55691(12) 0.16941(11) 0.1109(17) Uani 1 1 d DU . . H30 H 0.7948 0.5787 0.1655 0.133 Uiso 1 1 calc R A 1 C31 C 0.79603(18) 0.53457(16) 0.19906(17) 0.128(2) Uani 1 1 d U A . H31A H 0.7786 0.5169 0.2069 0.192 Uiso 1 1 calc R . . H31B H 0.8024 0.5500 0.2191 0.192 Uiso 1 1 calc R . . H31C H 0.8174 0.5225 0.1903 0.192 Uiso 1 1 calc R . . C32A C 0.7423(2) 0.5674(3) 0.1805(3) 0.115(3) Uiso 0.642(13) 1 d PDU A 1 H32A H 0.7262 0.5473 0.1767 0.173 Uiso 0.642(13) 1 calc PR A 1 H32B H 0.7343 0.5876 0.1661 0.173 Uiso 0.642(13) 1 calc PR A 1 H32C H 0.7421 0.5741 0.2056 0.173 Uiso 0.642(13) 1 calc PR A 1 C32B C 0.7631(4) 0.5909(3) 0.1819(4) 0.108(6) Uiso 0.358(13) 1 d PDU A 2 H32D H 0.7431 0.5969 0.1664 0.162 Uiso 0.358(13) 1 calc PR A 2 H32E H 0.7806 0.6102 0.1812 0.162 Uiso 0.358(13) 1 calc PR A 2 H32F H 0.7545 0.5879 0.2063 0.162 Uiso 0.358(13) 1 calc PR A 2 O1S O 0.7500 0.7500 0.02529(13) 0.0678(12) Uiso 1 4 d SU . . O2S O 0.7500 0.7500 0.1507(2) 0.106(2) Uiso 1 4 d SU . . O3S O 0.9178(5) 0.7154(5) 0.0396(5) 0.241(7) Uiso 0.50 1 d P . . C1S C 0.7545(7) 0.7805(6) 0.0058(7) 0.120(7) Uiso 0.25 1 d PU . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0299(4) 0.0299(4) 0.0805(6) 0.000 0.000 0.000 O1 0.0350(9) 0.0397(10) 0.0905(15) 0.0041(9) -0.0063(9) 0.0034(7) O2 0.0394(10) 0.0338(9) 0.0978(16) 0.0050(9) -0.0074(9) 0.0031(7) N1 0.0329(10) 0.0334(10) 0.0755(15) -0.0003(9) -0.0045(9) -0.0005(8) N2 0.0341(11) 0.0332(11) 0.0802(16) 0.0014(10) -0.0036(10) 0.0012(8) C1 0.0364(13) 0.0349(12) 0.0742(18) -0.0011(11) -0.0032(11) 0.0006(10) C2 0.0356(13) 0.0396(13) 0.0774(19) 0.0002(12) -0.0052(12) 0.0021(10) C3 0.0364(13) 0.0435(13) 0.0686(17) -0.0012(12) -0.0049(11) 0.0035(10) C4 0.0403(13) 0.0346(12) 0.0726(17) 0.0009(11) -0.0036(12) 0.0034(10) C5 0.0348(13) 0.0352(12) 0.0855(19) -0.0007(12) -0.0043(12) 0.0000(9) C6 0.0342(12) 0.0356(12) 0.0755(18) -0.0004(11) -0.0041(11) 0.0017(10) C7 0.0374(13) 0.0325(12) 0.0755(18) 0.0023(11) -0.0016(11) 0.0008(10) C8 0.0351(12) 0.0319(12) 0.0716(17) 0.0007(11) -0.0036(11) -0.0012(9) C9 0.0332(13) 0.0442(14) 0.090(2) 0.0138(13) -0.0082(13) 0.0048(10) C10 0.0511(16) 0.0443(15) 0.096(2) 0.0124(14) -0.0195(15) 0.0019(12) C11 0.0550(19) 0.068(2) 0.124(3) 0.027(2) -0.0279(19) -0.0101(16) C12 0.0468(18) 0.093(3) 0.140(4) 0.046(3) -0.027(2) -0.0132(17) C13 0.0439(17) 0.105(3) 0.120(3) 0.049(2) 0.0051(18) 0.0040(17) C14 0.0467(16) 0.071(2) 0.093(2) 0.0257(17) -0.0015(15) 0.0113(14) C15 0.0664(19) 0.0624(19) 0.086(2) 0.0021(16) -0.0097(16) 0.0044(15) C16 0.086(2) 0.070(2) 0.088(3) 0.0132(18) 0.000(2) -0.0019(18) C17 0.123(4) 0.079(3) 0.098(3) -0.005(2) -0.020(3) 0.005(2) C18 0.072(2) 0.099(3) 0.089(3) 0.012(2) 0.0077(19) 0.018(2) C19 0.172(7) 0.198(7) 0.113(4) 0.020(4) 0.044(4) -0.007(6) C20 0.127(4) 0.097(3) 0.130(4) -0.009(3) -0.011(3) 0.020(3) C30 0.143(4) 0.090(3) 0.099(3) 0.024(2) 0.042(3) 0.054(3) C31 0.132(5) 0.120(4) 0.132(4) 0.030(4) 0.012(4) 0.044(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.924(2) 2_665 ? Co1 N1 1.924(2) 16_655 ? Co1 N1 1.924(2) . ? Co1 N1 1.924(2) 15_565 ? Co1 O1S 2.265(5) . ? Co1 O2S 2.454(8) . ? O1 C3 1.371(3) . ? O1 C9 1.398(3) . ? O2 C21B 1.349(3) . ? O2 C4 1.372(3) . ? O2 C21A 1.394(4) . ? N1 C7 1.368(3) . ? N1 C8 1.373(3) 16_655 ? N2 C7 1.320(4) . ? N2 C8 1.323(3) . ? C1 C6 1.385(4) . ? C1 C2 1.401(4) . ? C1 C8 1.451(4) 16_655 ? C2 C3 1.373(4) . ? C2 H2 0.9500 . ? C3 C4 1.420(4) . ? C4 C5 1.382(4) . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? C6 C7 1.445(4) . ? C8 N1 1.373(3) 15_565 ? C8 C1 1.451(4) 15_565 ? C9 C14 1.393(5) . ? C9 C10 1.397(5) . ? C10 C11 1.406(5) . ? C10 C15 1.515(5) . ? C11 C12 1.337(6) . ? C11 H11 0.9500 . ? C12 C13 1.379(7) . ? C12 H12 0.9500 . ? C13 C14 1.397(5) . ? C13 H13 0.9500 . ? C14 C18 1.502(6) . ? C15 C16 1.510(5) . ? C15 C17 1.531(6) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.478(7) . ? C18 C19 1.557(8) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.523(7) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.298(5) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.513(6) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.680(5) . ? C27A C29A 1.512(9) . ? C27A C28A 1.530(9) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.495(8) . ? C27B C28B 1.503(8) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C32B 1.507(9) . ? C30 C31 1.521(7) . ? C30 C32A 1.535(7) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? O1S C1S 1.37(3) 2_665 ? O1S C1S 1.37(3) 15_565 ? O1S C1S 1.37(3) . ? O1S C1S 1.37(3) 16_655 ? C1S C1S 1.64(3) 15_565 ? C1S C1S 1.64(3) 16_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 N1 Co1 N1 89.919(6) 2_665 16_655 ? N1 Co1 N1 175.72(15) 2_665 . ? N1 Co1 N1 89.921(7) 16_655 . ? N1 Co1 N1 89.918(6) 2_665 15_565 ? N1 Co1 N1 175.72(15) 16_655 15_565 ? N1 Co1 N1 89.922(6) . 15_565 ? N1 Co1 O1S 92.14(8) 2_665 . ? N1 Co1 O1S 92.14(8) 16_655 . ? N1 Co1 O1S 92.14(8) . . ? N1 Co1 O1S 92.14(8) 15_565 . ? N1 Co1 O2S 87.86(8) 2_665 . ? N1 Co1 O2S 87.86(8) 16_655 . ? N1 Co1 O2S 87.86(8) . . ? N1 Co1 O2S 87.86(8) 15_565 . ? O1S Co1 O2S 180.000(1) . . ? C3 O1 C9 118.5(2) . . ? C21B O2 C4 116.2(3) . . ? C21B O2 C21A 6.4(3) . . ? C4 O2 C21A 116.1(3) . . ? C7 N1 C8 107.2(2) . 16_655 ? C7 N1 Co1 125.95(17) . . ? C8 N1 Co1 126.79(17) 16_655 . ? C7 N2 C8 121.4(2) . . ? C6 C1 C2 121.2(2) . . ? C6 C1 C8 106.0(2) . 16_655 ? C2 C1 C8 132.8(2) . 16_655 ? C3 C2 C1 117.5(2) . . ? C3 C2 H2 121.3 . . ? C1 C2 H2 121.3 . . ? O1 C3 C2 125.6(2) . . ? O1 C3 C4 113.1(2) . . ? C2 C3 C4 121.4(2) . . ? O2 C4 C5 124.5(2) . . ? O2 C4 C3 114.7(2) . . ? C5 C4 C3 120.7(2) . . ? C4 C5 C6 117.6(2) . . ? C4 C5 H5 121.2 . . ? C6 C5 H5 121.2 . . ? C1 C6 C5 121.6(2) . . ? C1 C6 C7 106.9(2) . . ? C5 C6 C7 131.1(2) . . ? N2 C7 N1 128.6(2) . . ? N2 C7 C6 121.4(2) . . ? N1 C7 C6 109.9(2) . . ? N2 C8 N1 127.3(2) . 15_565 ? N2 C8 C1 122.6(2) . 15_565 ? N1 C8 C1 110.0(2) 15_565 15_565 ? C14 C9 C10 124.5(3) . . ? C14 C9 O1 117.8(3) . . ? C10 C9 O1 117.4(3) . . ? C9 C10 C11 116.4(4) . . ? C9 C10 C15 120.5(3) . . ? C11 C10 C15 123.0(4) . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 121.9(4) . . ? C12 C13 H13 119.0 . . ? C14 C13 H13 119.0 . . ? C9 C14 C13 114.9(4) . . ? C9 C14 C18 120.0(3) . . ? C13 C14 C18 125.0(4) . . ? C16 C15 C10 110.5(3) . . ? C16 C15 C17 109.0(4) . . ? C10 C15 C17 115.1(3) . . ? C16 C15 H15 107.3 . . ? C10 C15 H15 107.3 . . ? C17 C15 H15 107.3 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C14 110.8(4) . . ? C20 C18 C19 109.5(5) . . ? C14 C18 C19 113.1(5) . . ? C20 C18 H18 107.8 . . ? C14 C18 H18 107.8 . . ? C19 C18 H18 107.8 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 123.3(3) . . ? C26A C21A O2 116.6(3) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 119.1(5) . . ? C23A C22A C27A 120.9(5) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C23A C24A C25A 120.0 . . ? C23A C24A H24A 120.0 . . ? C25A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 109.8(4) . . ? C30 C26A C21A 130.0(4) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 116.6(3) . . ? O2 C21B C26B 123.4(3) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 121.4(4) . . ? C21B C22B C27B 118.6(4) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 125.2(3) . . ? C21B C26B C30 114.8(3) . . ? C29A C27A C22A 120.8(10) . . ? C29A C27A C28A 106.6(11) . . ? C22A C27A C28A 116.5(9) . . ? C29A C27A H27A 103.6 . . ? C22A C27A H27A 103.6 . . ? C28A C27A H27A 103.6 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 115.4(7) . . ? C29B C27B C22B 109.4(7) . . ? C28B C27B C22B 108.0(6) . . ? C29B C27B H27B 107.9 . . ? C28B C27B H27B 107.9 . . ? C22B C27B H27B 107.9 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C32B 134.1(8) . . ? C26A C30 C31 110.1(5) . . ? C32B C30 C31 114.1(7) . . ? C26A C30 C32A 108.7(6) . . ? C32B C30 C32A 45.8(6) . . ? C31 C30 C32A 108.0(5) . . ? C26A C30 C26B 5.3(4) . . ? C32B C30 C26B 129.0(7) . . ? C31 C30 C26B 114.5(4) . . ? C32A C30 C26B 104.0(5) . . ? C26A C30 H30 110.0 . . ? C32B C30 H30 65.4 . . ? C31 C30 H30 110.0 . . ? C32A C30 H30 110.0 . . ? C26B C30 H30 110.1 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? H32A C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? H32A C32A H32C 109.5 . . ? H32B C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C1S O1S C1S 73.4(10) 2_665 15_565 ? C1S O1S C1S 115(2) 2_665 . ? C1S O1S C1S 73.4(10) 15_565 . ? C1S O1S C1S 73.4(11) 2_665 16_655 ? C1S O1S C1S 115(2) 15_565 16_655 ? C1S O1S C1S 73.4(11) . 16_655 ? C1S O1S Co1 122.3(11) 2_665 . ? C1S O1S Co1 122.3(11) 15_565 . ? C1S O1S Co1 122.3(11) . . ? C1S O1S Co1 122.3(11) 16_655 . ? O1S C1S C1S 53.3(5) . 15_565 ? O1S C1S C1S 53.3(5) . 16_655 ? C1S C1S C1S 90.002(7) 15_565 16_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 Co1 N1 C7 88.3(2) 2_665 . . . ? N1 Co1 N1 C7 176.12(19) 16_655 . . . ? N1 Co1 N1 C7 0.4(3) 15_565 . . . ? O1S Co1 N1 C7 -91.7(2) . . . . ? O2S Co1 N1 C7 88.3(2) . . . . ? N1 Co1 N1 C8 -87.9(2) 2_665 . . 16_655 ? N1 Co1 N1 C8 0.0(3) 16_655 . . 16_655 ? N1 Co1 N1 C8 -175.73(19) 15_565 . . 16_655 ? O1S Co1 N1 C8 92.1(2) . . . 16_655 ? O2S Co1 N1 C8 -87.9(2) . . . 16_655 ? C6 C1 C2 C3 -2.0(5) . . . . ? C8 C1 C2 C3 173.5(3) 16_655 . . . ? C9 O1 C3 C2 2.4(5) . . . . ? C9 O1 C3 C4 -177.4(3) . . . . ? C1 C2 C3 O1 -178.1(3) . . . . ? C1 C2 C3 C4 1.8(5) . . . . ? C21B O2 C4 C5 13.8(5) . . . . ? C21A O2 C4 C5 6.6(5) . . . . ? C21B O2 C4 C3 -169.6(3) . . . . ? C21A O2 C4 C3 -176.8(3) . . . . ? O1 C3 C4 O2 2.7(4) . . . . ? C2 C3 C4 O2 -177.2(3) . . . . ? O1 C3 C4 C5 179.4(3) . . . . ? C2 C3 C4 C5 -0.5(5) . . . . ? O2 C4 C5 C6 175.7(3) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? C2 C1 C6 C5 1.0(5) . . . . ? C8 C1 C6 C5 -175.6(3) 16_655 . . . ? C2 C1 C6 C7 175.3(3) . . . . ? C8 C1 C6 C7 -1.3(3) 16_655 . . . ? C4 C5 C6 C1 0.4(5) . . . . ? C4 C5 C6 C7 -172.4(3) . . . . ? C8 N2 C7 N1 -1.2(5) . . . . ? C8 N2 C7 C6 174.8(3) . . . . ? C8 N1 C7 N2 176.9(3) 16_655 . . . ? Co1 N1 C7 N2 0.1(5) . . . . ? C8 N1 C7 C6 0.5(3) 16_655 . . . ? Co1 N1 C7 C6 -176.3(2) . . . . ? C1 C6 C7 N2 -176.2(3) . . . . ? C5 C6 C7 N2 -2.6(5) . . . . ? C1 C6 C7 N1 0.5(3) . . . . ? C5 C6 C7 N1 174.1(3) . . . . ? C7 N2 C8 N1 1.6(5) . . . 15_565 ? C7 N2 C8 C1 -174.4(3) . . . 15_565 ? C3 O1 C9 C14 -99.5(3) . . . . ? C3 O1 C9 C10 86.0(3) . . . . ? C14 C9 C10 C11 0.3(4) . . . . ? O1 C9 C10 C11 174.5(2) . . . . ? C14 C9 C10 C15 -176.5(3) . . . . ? O1 C9 C10 C15 -2.3(4) . . . . ? C9 C10 C11 C12 0.1(5) . . . . ? C15 C10 C11 C12 176.7(3) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C11 C12 C13 C14 -0.9(6) . . . . ? C10 C9 C14 C13 -0.9(4) . . . . ? O1 C9 C14 C13 -175.0(3) . . . . ? C10 C9 C14 C18 175.4(3) . . . . ? O1 C9 C14 C18 1.2(4) . . . . ? C12 C13 C14 C9 1.2(5) . . . . ? C12 C13 C14 C18 -174.8(4) . . . . ? C9 C10 C15 C16 74.0(4) . . . . ? C11 C10 C15 C16 -102.6(4) . . . . ? C9 C10 C15 C17 -162.0(3) . . . . ? C11 C10 C15 C17 21.5(5) . . . . ? C9 C14 C18 C20 -81.3(5) . . . . ? C13 C14 C18 C20 94.5(5) . . . . ? C9 C14 C18 C19 155.3(5) . . . . ? C13 C14 C18 C19 -28.8(6) . . . . ? C21B O2 C21A C22A 3(4) . . . . ? C4 O2 C21A C22A 96.5(4) . . . . ? C21B O2 C21A C26A -179(100) . . . . ? C4 O2 C21A C26A -85.6(4) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 177.7(5) . . . . ? C26A C21A C22A C27A 178.5(6) . . . . ? O2 C21A C22A C27A -3.8(6) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -178.5(6) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 175.6(5) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -174.5(6) . . . . ? O2 C21A C26A C30 7.6(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -177.9(5) . . . . ? C4 O2 C21B C22B 95.0(3) . . . . ? C21A O2 C21B C22B -175(4) . . . . ? C4 O2 C21B C26B -84.0(4) . . . . ? C21A O2 C21B C26B 6(4) . . . . ? O2 C21B C22B C23B -179.1(5) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 1.7(4) . . . . ? C26B C21B C22B C27B -179.2(5) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B 179.2(5) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -177.5(4) . . . . ? O2 C21B C26B C25B 179.0(5) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -3.3(4) . . . . ? C22B C21B C26B C30 177.7(4) . . . . ? C21A C22A C27A C29A -150.5(11) . . . . ? C23A C22A C27A C29A 28.0(13) . . . . ? C21A C22A C27A C28A 77.6(12) . . . . ? C23A C22A C27A C28A -103.9(11) . . . . ? C23B C22B C27B C29B 69.6(8) . . . . ? C21B C22B C27B C29B -111.2(7) . . . . ? C23B C22B C27B C28B -56.7(8) . . . . ? C21B C22B C27B C28B 122.5(6) . . . . ? C25A C26A C30 C32B -81.6(11) . . . . ? C21A C26A C30 C32B 93.4(11) . . . . ? C25A C26A C30 C31 82.4(5) . . . . ? C21A C26A C30 C31 -102.7(6) . . . . ? C25A C26A C30 C32A -35.8(6) . . . . ? C21A C26A C30 C32A 139.2(6) . . . . ? C25A C26A C30 C26B -65(3) . . . . ? C21A C26A C30 C26B 110(4) . . . . ? C25B C26B C30 C26A 117(4) . . . . ? C21B C26B C30 C26A -61(4) . . . . ? C25B C26B C30 C32B -78.9(10) . . . . ? C21B C26B C30 C32B 103.5(9) . . . . ? C25B C26B C30 C31 82.5(6) . . . . ? C21B C26B C30 C31 -95.1(5) . . . . ? C25B C26B C30 C32A -35.2(6) . . . . ? C21B C26B C30 C32A 147.2(5) . . . . ? N1 Co1 O1S C1S -138.6(12) 2_665 . . 2_665 ? N1 Co1 O1S C1S 131.4(12) 16_655 . . 2_665 ? N1 Co1 O1S C1S 41.4(12) . . . 2_665 ? N1 Co1 O1S C1S -48.6(12) 15_565 . . 2_665 ? O2S Co1 O1S C1S -172(100) . . . 2_665 ? N1 Co1 O1S C1S 131.4(12) 2_665 . . 15_565 ? N1 Co1 O1S C1S 41.4(12) 16_655 . . 15_565 ? N1 Co1 O1S C1S -48.6(12) . . . 15_565 ? N1 Co1 O1S C1S -138.6(12) 15_565 . . 15_565 ? O2S Co1 O1S C1S 98(100) . . . 15_565 ? N1 Co1 O1S C1S 41.4(12) 2_665 . . . ? N1 Co1 O1S C1S -48.6(12) 16_655 . . . ? N1 Co1 O1S C1S -138.6(12) . . . . ? N1 Co1 O1S C1S 131.4(12) 15_565 . . . ? O2S Co1 O1S C1S 8(100) . . . . ? N1 Co1 O1S C1S -48.6(12) 2_665 . . 16_655 ? N1 Co1 O1S C1S -138.6(12) 16_655 . . 16_655 ? N1 Co1 O1S C1S 131.4(12) . . . 16_655 ? N1 Co1 O1S C1S 41.4(12) 15_565 . . 16_655 ? O2S Co1 O1S C1S -82(100) . . . 16_655 ? C1S O1S C1S C1S -61.9(7) 2_665 . . 15_565 ? C1S O1S C1S C1S -123.8(15) 16_655 . . 15_565 ? Co1 O1S C1S C1S 118.1(7) . . . 15_565 ? C1S O1S C1S C1S 61.9(7) 2_665 . . 16_655 ? C1S O1S C1S C1S 123.8(15) 15_565 . . 16_655 ? Co1 O1S C1S C1S -118.1(7) . . . 16_655 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.900 _refine_diff_density_min -0.406 _refine_diff_density_rms 0.085 data_PNC[cIm-Co-vIm] _database_code_depnum_ccdc_archive 'CCDC 900376' #TrackingRef '900376_PNC[cIm-Co-vIm].cif' _audit_update_record ; 2012-11-21 # Formatted by publCIF ; _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C135.50 H157.17 Co N12 O8.75' _chemical_formula_weight 2152.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.5719(16) _cell_length_b 37.5719(16) _cell_length_c 37.5719(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 53038(4) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9989 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 21.43 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.809 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13814 _exptl_absorpt_coefficient_mu 0.140 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6191 _exptl_absorpt_correction_T_max 0.7453 _exptl_absorpt_process_details SADABS _exptl_special_details ? _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.69390 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Station 9.8, SRS, Daresbury' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7811 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0281 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 2 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 24.39 _reflns_number_total 7811 _reflns_number_gt 5594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7811 _refine_ls_number_parameters 332 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1037 _refine_ls_R_factor_gt 0.0835 _refine_ls_wR_factor_ref 0.2950 _refine_ls_wR_factor_gt 0.2717 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.190 _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 0.7500 0.7500 0.08672(2) 0.0413(3) Uani 1 4 d S . . O1 O 0.61215(5) 0.90437(5) 0.11152(6) 0.0529(5) Uani 1 1 d . A . O2 O 0.66936(5) 0.93958(5) 0.11202(6) 0.0594(6) Uani 1 1 d . . . N1 N 0.72204(5) 0.79296(5) 0.08716(6) 0.0451(5) Uani 1 1 d . A . N2 N 0.76847(6) 0.83733(6) 0.08973(6) 0.0484(6) Uani 1 1 d . A . C1 C 0.67471(7) 0.83186(7) 0.09292(8) 0.0466(6) Uani 1 1 d . . . C2 C 0.64191(7) 0.84795(7) 0.09847(8) 0.0481(7) Uani 1 1 d . A . H2 H 0.6204 0.8346 0.0981 0.072 Uiso 1 1 calc R . . C3 C 0.64182(7) 0.88429(7) 0.10456(8) 0.0485(7) Uani 1 1 d . . . C4 C 0.67356(7) 0.90417(7) 0.10402(8) 0.0505(7) Uani 1 1 d . A . C5 C 0.70587(7) 0.88805(6) 0.09754(9) 0.0509(7) Uani 1 1 d . . . H5 H 0.7273 0.9015 0.0966 0.076 Uiso 1 1 calc R A . C6 C 0.70592(7) 0.85174(7) 0.09244(8) 0.0472(6) Uani 1 1 d . A . C7 C 0.73521(7) 0.82679(7) 0.08907(7) 0.0453(6) Uani 1 1 d . . . C8 C 0.79498(7) 0.81433(7) 0.08910(7) 0.0444(6) Uani 1 1 d . . . C9 C 0.57918(7) 0.88728(8) 0.11423(9) 0.0581(8) Uani 1 1 d . . . C10 C 0.56986(9) 0.87324(8) 0.14762(11) 0.0689(10) Uani 1 1 d . A . C11 C 0.53567(10) 0.85946(10) 0.15009(14) 0.0904(14) Uani 1 1 d . . . H11 H 0.5279 0.8497 0.1721 0.136 Uiso 1 1 calc R A . C12 C 0.51312(11) 0.85961(13) 0.12185(18) 0.1043(17) Uani 1 1 d . A . H12 H 0.4899 0.8500 0.1246 0.156 Uiso 1 1 calc R . . C13 C 0.52298(10) 0.87314(13) 0.08968(16) 0.0998(16) Uani 1 1 d . . . H13 H 0.5067 0.8725 0.0703 0.150 Uiso 1 1 calc R A . C14 C 0.55737(9) 0.88822(10) 0.08470(11) 0.0740(10) Uani 1 1 d . A . C15 C 0.59528(10) 0.87520(9) 0.17837(11) 0.0754(10) Uani 1 1 d . . . H15 H 0.6195 0.8690 0.1693 0.113 Uiso 1 1 calc R A . C16 C 0.59678(12) 0.91323(10) 0.19307(12) 0.0846(11) Uani 1 1 d . A . H16A H 0.6035 0.9297 0.1740 0.127 Uiso 1 1 calc R . . H16B H 0.6144 0.9144 0.2123 0.127 Uiso 1 1 calc R . . H16C H 0.5733 0.9199 0.2024 0.127 Uiso 1 1 calc R . . C17 C 0.58672(16) 0.84990(13) 0.20916(14) 0.1142(18) Uani 1 1 d . A . H17A H 0.5623 0.8542 0.2174 0.171 Uiso 1 1 calc R . . H17B H 0.6034 0.8541 0.2288 0.171 Uiso 1 1 calc R . . H17C H 0.5890 0.8252 0.2010 0.171 Uiso 1 1 calc R . . C18 C 0.56960(12) 0.90566(12) 0.05065(12) 0.0910(12) Uani 1 1 d . . . H18 H 0.5958 0.9016 0.0481 0.137 Uiso 1 1 calc R A . C19 C 0.5512(2) 0.8913(2) 0.01747(19) 0.171(3) Uani 1 1 d . A . H19A H 0.5599 0.8673 0.0124 0.257 Uiso 1 1 calc R . . H19B H 0.5565 0.9069 -0.0028 0.257 Uiso 1 1 calc R . . H19C H 0.5255 0.8907 0.0214 0.257 Uiso 1 1 calc R . . C20 C 0.56330(17) 0.94535(15) 0.05398(18) 0.131(2) Uani 1 1 d . A . H20A H 0.5377 0.9500 0.0553 0.196 Uiso 1 1 calc R . . H20B H 0.5733 0.9575 0.0332 0.196 Uiso 1 1 calc R . . H20C H 0.5749 0.9542 0.0756 0.196 Uiso 1 1 calc R . . C21A C 0.70001(11) 0.96031(14) 0.11124(14) 0.041(2) Uiso 0.440(7) 1 d PG A 1 C22A C 0.70871(14) 0.98030(15) 0.08135(13) 0.066(2) Uiso 0.440(7) 1 d PG A 1 C23A C 0.73939(16) 1.00097(14) 0.08120(15) 0.065(2) Uiso 0.440(7) 1 d PG A 1 H23A H 0.7453 1.0146 0.0608 0.097 Uiso 0.440(7) 1 calc PR A 1 C24A C 0.76137(12) 1.00166(14) 0.11095(18) 0.072(2) Uiso 0.440(7) 1 d PG A 1 H24A H 0.7823 1.0158 0.1109 0.108 Uiso 0.440(7) 1 calc PR A 1 C25A C 0.75267(12) 0.98168(14) 0.14085(16) 0.065(2) Uiso 0.440(7) 1 d PG A 1 H25A H 0.7677 0.9821 0.1612 0.098 Uiso 0.440(7) 1 calc PR A 1 C26A C 0.72199(12) 0.96100(13) 0.14099(13) 0.0446(16) Uiso 0.440(7) 1 d PG A 1 C21B C 0.69776(10) 0.96024(12) 0.10563(11) 0.049(2) Uiso 0.560(7) 1 d PG A 2 C22B C 0.69932(10) 0.97816(12) 0.07330(10) 0.0541(14) Uiso 0.560(7) 1 d PG A 2 C23B C 0.72817(12) 1.00001(11) 0.06564(11) 0.0728(18) Uiso 0.560(7) 1 d PG A 2 H23B H 0.7292 1.0123 0.0435 0.109 Uiso 0.560(7) 1 calc PR A 2 C24B C 0.75546(10) 1.00394(11) 0.09030(15) 0.073(2) Uiso 0.560(7) 1 d PG A 2 H24B H 0.7752 1.0189 0.0851 0.109 Uiso 0.560(7) 1 calc PR A 2 C25B C 0.75390(9) 0.98602(12) 0.12263(13) 0.0634(16) Uiso 0.560(7) 1 d PG A 2 H25B H 0.7726 0.9887 0.1395 0.095 Uiso 0.560(7) 1 calc PR A 2 C26B C 0.72505(11) 0.96416(11) 0.13029(11) 0.0566(15) Uiso 0.560(7) 1 d PGD A 2 C27A C 0.6859(3) 0.9782(2) 0.0471(2) 0.071(2) Uiso 0.440(7) 1 d P A 1 H27A H 0.6779 0.9529 0.0457 0.107 Uiso 0.440(7) 1 calc PR A 1 C28A C 0.6480(4) 1.0021(4) 0.0475(4) 0.099(4) Uiso 0.440(7) 1 d P A 1 H28D H 0.6397 1.0057 0.0231 0.149 Uiso 0.440(7) 1 calc PR A 1 H28E H 0.6525 1.0253 0.0587 0.149 Uiso 0.440(7) 1 calc PR A 1 H28F H 0.6298 0.9893 0.0612 0.149 Uiso 0.440(7) 1 calc PR A 1 C29A C 0.7007(5) 0.9862(5) 0.0113(5) 0.164(6) Uiso 0.440(7) 1 d P A 1 H29A H 0.7108 0.9644 0.0011 0.246 Uiso 0.440(7) 1 calc PR A 1 H29B H 0.7193 1.0043 0.0135 0.246 Uiso 0.440(7) 1 calc PR A 1 H29C H 0.6816 0.9950 -0.0042 0.246 Uiso 0.440(7) 1 calc PR A 1 C27B C 0.6677(2) 0.97379(18) 0.04842(18) 0.0710(18) Uiso 0.560(7) 1 d P A 2 H27B H 0.6483 0.9608 0.0613 0.107 Uiso 0.560(7) 1 calc PR A 2 C28B C 0.6546(3) 1.0100(3) 0.0385(3) 0.107(4) Uiso 0.560(7) 1 d P A 2 H28A H 0.6305 1.0082 0.0288 0.161 Uiso 0.560(7) 1 calc PR A 2 H28B H 0.6705 1.0204 0.0206 0.161 Uiso 0.560(7) 1 calc PR A 2 H28C H 0.6544 1.0252 0.0597 0.161 Uiso 0.560(7) 1 calc PR A 2 C29B C 0.6784(3) 0.9530(3) 0.0177(3) 0.143(4) Uiso 0.560(7) 1 d P A 2 H29D H 0.6913 0.9317 0.0256 0.215 Uiso 0.560(7) 1 calc PR A 2 H29E H 0.6940 0.9674 0.0024 0.215 Uiso 0.560(7) 1 calc PR A 2 H29F H 0.6573 0.9458 0.0042 0.215 Uiso 0.560(7) 1 calc PR A 2 C30 C 0.71919(15) 0.94286(13) 0.16888(12) 0.1078(17) Uani 1 1 d D . . H30 H 0.7041 0.9213 0.1650 0.162 Uiso 1 1 calc R A 1 C31 C 0.70525(16) 0.96532(15) 0.19924(15) 0.1229(19) Uani 1 1 d . A . H31A H 0.7218 0.9849 0.2039 0.184 Uiso 1 1 calc R . . H31B H 0.7030 0.9506 0.2206 0.184 Uiso 1 1 calc R . . H31C H 0.6819 0.9750 0.1929 0.184 Uiso 1 1 calc R . . C32A C 0.7592(3) 0.9323(3) 0.1808(3) 0.118(4) Uiso 0.632(13) 1 d P A 1 H32A H 0.7737 0.9539 0.1825 0.178 Uiso 0.632(13) 1 calc PR A 1 H32B H 0.7696 0.9162 0.1632 0.178 Uiso 0.632(13) 1 calc PR A 1 H32C H 0.7584 0.9205 0.2041 0.178 Uiso 0.632(13) 1 calc PR A 1 C32B C 0.7375(4) 0.9090(4) 0.1811(4) 0.105(5) Uiso 0.368(13) 1 d P A 2 H32D H 0.7195 0.8911 0.1869 0.157 Uiso 0.368(13) 1 calc PR A 2 H32E H 0.7519 0.9141 0.2022 0.157 Uiso 0.368(13) 1 calc PR A 2 H32F H 0.7528 0.9001 0.1620 0.157 Uiso 0.368(13) 1 calc PR A 2 N1S N 0.7500 0.7500 0.03524(14) 0.0520(11) Uani 1 4 d S . . C1S C 0.7773(2) 0.7440(2) 0.0138(2) 0.084(2) Uiso 0.50 1 d P . . C2S C 0.76830(17) 0.7481(3) -0.0216(2) 0.090(2) Uiso 0.25 1 d P . . N2S N 0.76830(17) 0.7481(3) -0.0216(2) 0.090(2) Uiso 0.25 1 d P . . N3S N 0.7500 0.7500 0.13887(13) 0.0468(10) Uani 1 4 d S . . C3S C 0.7762(2) 0.7391(2) 0.1602(2) 0.0737(18) Uiso 0.50 1 d P . . C4S C 0.76725(18) 0.7441(3) 0.19499(18) 0.083(2) Uiso 0.25 1 d P . . N4S N 0.76725(18) 0.7441(3) 0.19499(18) 0.083(2) Uiso 0.25 1 d P . . O1S O 0.5725(3) 0.7894(3) 0.0424(3) 0.158(3) Uiso 0.50 1 d P . . O2S O 0.7500 0.7500 0.7500 0.086(7) Uiso 0.50 24 d SP . . 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 0.0313(3) 0.0313(3) 0.0611(5) 0.000 0.000 0.000 O1 0.0358(10) 0.0392(10) 0.0837(14) -0.0036(9) 0.0046(9) 0.0047(7) O2 0.0391(10) 0.0346(10) 0.1044(17) -0.0049(9) 0.0062(10) 0.0033(7) N1 0.0338(11) 0.0339(11) 0.0675(15) 0.0015(10) 0.0036(9) 0.0008(8) N2 0.0353(12) 0.0368(11) 0.0730(16) 0.0013(10) 0.0023(10) 0.0005(9) C1 0.0361(13) 0.0373(13) 0.0664(17) 0.0055(11) 0.0019(12) 0.0012(10) C2 0.0370(13) 0.0385(14) 0.0688(18) 0.0003(12) 0.0039(12) 0.0004(10) C3 0.0361(13) 0.0432(14) 0.0661(17) 0.0011(12) 0.0037(12) 0.0042(11) C4 0.0424(15) 0.0335(13) 0.0755(19) 0.0004(12) 0.0006(13) 0.0017(11) C5 0.0350(13) 0.0332(13) 0.085(2) 0.0005(12) 0.0026(13) -0.0016(10) C6 0.0353(13) 0.0381(13) 0.0682(17) 0.0018(12) 0.0013(12) 0.0006(10) C7 0.0355(13) 0.0353(13) 0.0650(17) -0.0015(11) 0.0016(11) -0.0005(10) C8 0.0363(13) 0.0325(12) 0.0644(17) 0.0000(11) 0.0010(11) 0.0020(10) C9 0.0361(14) 0.0453(16) 0.093(2) -0.0178(15) 0.0063(14) 0.0028(11) C10 0.0526(18) 0.0467(17) 0.107(3) -0.0136(16) 0.0256(18) -0.0004(13) C11 0.061(2) 0.072(2) 0.139(4) -0.030(2) 0.034(2) -0.0128(18) C12 0.050(2) 0.100(3) 0.163(5) -0.056(3) 0.033(3) -0.018(2) C13 0.047(2) 0.107(3) 0.146(4) -0.060(3) -0.010(2) 0.003(2) C14 0.0475(18) 0.075(2) 0.099(3) -0.031(2) -0.0051(17) 0.0077(15) C15 0.074(2) 0.064(2) 0.088(3) 0.0047(18) 0.0176(19) 0.0089(17) C16 0.095(3) 0.069(2) 0.089(3) -0.0123(19) -0.001(2) 0.002(2) C17 0.148(5) 0.085(3) 0.109(4) 0.018(3) 0.041(3) 0.012(3) C18 0.080(3) 0.104(3) 0.089(3) -0.015(2) -0.016(2) 0.017(2) C19 0.191(8) 0.200(8) 0.123(5) -0.017(5) -0.021(5) -0.034(6) C20 0.137(5) 0.104(4) 0.151(5) 0.004(3) -0.011(4) 0.016(3) C30 0.132(4) 0.091(3) 0.100(3) -0.023(2) -0.036(3) 0.056(3) C31 0.125(4) 0.126(4) 0.118(4) -0.030(3) -0.007(3) 0.040(3) N1S 0.0441(15) 0.0441(15) 0.068(3) 0.000 0.000 0.000 N3S 0.0429(14) 0.0429(14) 0.055(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.926(2) 15_565 ? Co1 N1 1.926(2) 2_665 ? Co1 N1 1.926(2) 16_655 ? Co1 N1 1.926(2) . ? Co1 N1S 1.934(5) . ? Co1 N3S 1.959(5) . ? O1 C3 1.371(3) . ? O1 C9 1.399(3) . ? O2 C21B 1.341(3) . ? O2 C4 1.373(3) . ? O2 C21A 1.391(4) . ? N1 C7 1.366(3) . ? N1 C8 1.371(3) 16_655 ? N2 C7 1.311(3) . ? N2 C8 1.319(3) . ? C1 C2 1.388(4) . ? C1 C6 1.390(3) . ? C1 C8 1.453(3) 16_655 ? C2 C3 1.385(4) . ? C2 H2 0.9500 . ? C3 C4 1.407(4) . ? C4 C5 1.378(4) . ? C5 C6 1.378(4) . ? C5 H5 0.9500 . ? C6 C7 1.451(4) . ? C8 N1 1.371(3) 15_565 ? C8 C1 1.453(3) 15_565 ? C9 C14 1.380(5) . ? C9 C10 1.405(5) . ? C10 C11 1.388(5) . ? C10 C15 1.501(5) . ? C11 C12 1.358(7) . ? C11 H11 0.9500 . ? C12 C13 1.363(7) . ? C12 H12 0.9500 . ? C13 C14 1.423(6) . ? C13 H13 0.9500 . ? C14 C18 1.509(6) . ? C15 C17 1.531(6) . ? C15 C16 1.533(5) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.515(7) . ? C18 C19 1.523(8) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.549(10) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.254(7) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.522(8) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.670(6) . ? C27A C29A 1.483(19) . ? C27A C28A 1.682(16) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.453(13) . ? C27B C28B 1.494(13) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.512(6) . ? C30 C32B 1.516(14) . ? C30 C32A 1.617(10) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? N1S C1S 1.324(9) 2_665 ? N1S C1S 1.324(9) 15_565 ? N1S C1S 1.324(9) . ? N1S C1S 1.324(9) 16_655 ? C1S C2S 1.380(11) . ? C1S C1S 1.485(12) 15_565 ? C1S C1S 1.485(12) 16_655 ? C1S N2S 1.785(12) 15_565 ? C1S C2S 1.785(12) 15_565 ? C1S N2S 1.873(12) 16_655 ? C1S C2S 1.873(12) 16_655 ? C2S N2S 0.977(9) 16_655 ? C2S C2S 0.977(9) 16_655 ? C2S N2S 0.978(9) 15_565 ? C2S C2S 0.978(9) 15_565 ? C2S C2S 1.382(12) 2_665 ? C2S N2S 1.382(12) 2_665 ? C2S C1S 1.785(12) 16_655 ? C2S C1S 1.873(12) 15_565 ? N3S C3S 1.334(8) 16_655 ? N3S C3S 1.334(8) 2_665 ? N3S C3S 1.334(8) 15_565 ? N3S C3S 1.334(8) . ? C3S C4S 1.362(10) . ? C3S C3S 1.507(11) 16_655 ? C3S C3S 1.507(11) 15_565 ? C3S N4S 1.793(11) 15_565 ? C3S C4S 1.793(11) 15_565 ? C3S N4S 1.845(11) 16_655 ? C3S C4S 1.845(11) 16_655 ? C4S N4S 0.968(8) 15_565 ? C4S C4S 0.968(8) 15_565 ? C4S N4S 0.968(8) 16_655 ? C4S C4S 0.968(8) 16_655 ? C4S N4S 1.369(12) 2_665 ? C4S C4S 1.369(12) 2_665 ? C4S C3S 1.793(11) 16_655 ? C4S C3S 1.845(11) 15_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 89.996(2) 15_565 2_665 ? N1 Co1 N1 179.04(14) 15_565 16_655 ? N1 Co1 N1 89.993(1) 2_665 16_655 ? N1 Co1 N1 89.996(2) 15_565 . ? N1 Co1 N1 179.03(14) 2_665 . ? N1 Co1 N1 89.998(2) 16_655 . ? N1 Co1 N1S 90.48(7) 15_565 . ? N1 Co1 N1S 90.48(7) 2_665 . ? N1 Co1 N1S 90.48(7) 16_655 . ? N1 Co1 N1S 90.49(7) . . ? N1 Co1 N3S 89.52(7) 15_565 . ? N1 Co1 N3S 89.52(7) 2_665 . ? N1 Co1 N3S 89.52(7) 16_655 . ? N1 Co1 N3S 89.51(7) . . ? N1S Co1 N3S 180.000(1) . . ? C3 O1 C9 118.7(2) . . ? C21B O2 C4 115.5(3) . . ? C21B O2 C21A 9.3(3) . . ? C4 O2 C21A 116.3(3) . . ? C7 N1 C8 107.9(2) . 16_655 ? C7 N1 Co1 125.64(17) . . ? C8 N1 Co1 126.22(17) 16_655 . ? C7 N2 C8 121.5(2) . . ? C2 C1 C6 121.1(2) . . ? C2 C1 C8 133.0(2) . 16_655 ? C6 C1 C8 105.8(2) . 16_655 ? C3 C2 C1 117.2(2) . . ? C3 C2 H2 121.4 . . ? C1 C2 H2 121.4 . . ? O1 C3 C2 125.2(2) . . ? O1 C3 C4 113.6(2) . . ? C2 C3 C4 121.2(2) . . ? O2 C4 C5 124.4(2) . . ? O2 C4 C3 114.4(2) . . ? C5 C4 C3 121.1(2) . . ? C6 C5 C4 117.4(2) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? C5 C6 C1 121.9(2) . . ? C5 C6 C7 130.8(2) . . ? C1 C6 C7 107.1(2) . . ? N2 C7 N1 128.9(2) . . ? N2 C7 C6 121.7(2) . . ? N1 C7 C6 109.3(2) . . ? N2 C8 N1 127.7(2) . 15_565 ? N2 C8 C1 122.2(2) . 15_565 ? N1 C8 C1 109.9(2) 15_565 15_565 ? C14 C9 O1 117.1(3) . . ? C14 C9 C10 125.4(3) . . ? O1 C9 C10 117.3(3) . . ? C11 C10 C9 115.5(4) . . ? C11 C10 C15 123.7(4) . . ? C9 C10 C15 120.7(3) . . ? C12 C11 C10 121.6(5) . . ? C12 C11 H11 119.2 . . ? C10 C11 H11 119.2 . . ? C11 C12 C13 121.7(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 120.8(4) . . ? C12 C13 H13 119.6 . . ? C14 C13 H13 119.6 . . ? C9 C14 C13 115.0(4) . . ? C9 C14 C18 120.8(3) . . ? C13 C14 C18 124.1(4) . . ? C10 C15 C17 114.7(4) . . ? C10 C15 C16 110.3(3) . . ? C17 C15 C16 108.3(4) . . ? C10 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C20 108.1(4) . . ? C14 C18 C19 113.8(5) . . ? C20 C18 C19 110.1(5) . . ? C14 C18 H18 108.2 . . ? C20 C18 H18 108.2 . . ? C19 C18 H18 108.2 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 121.0(3) . . ? C26A C21A O2 119.0(3) . . ? C23A C22A C21A 120.0 . . ? C23A C22A C27A 118.9(5) . . ? C21A C22A C27A 121.0(5) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C30 C26A C25A 112.1(4) . . ? C30 C26A C21A 127.7(4) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 118.1(3) . . ? O2 C21B C26B 121.9(3) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 123.1(4) . . ? C21B C22B C27B 116.9(4) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 124.4(3) . . ? C21B C26B C30 115.5(3) . . ? C29A C27A C22A 122.4(10) . . ? C29A C27A C28A 102.6(10) . . ? C22A C27A C28A 115.6(7) . . ? C29A C27A H27A 104.9 . . ? C22A C27A H27A 104.9 . . ? C28A C27A H27A 104.9 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 112.6(8) . . ? C29B C27B C22B 109.2(7) . . ? C28B C27B C22B 108.1(7) . . ? C29B C27B H27B 109.0 . . ? C28B C27B H27B 109.0 . . ? C22B C27B H27B 109.0 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 110.8(5) . . ? C26A C30 C32B 132.1(7) . . ? C31 C30 C32B 113.4(7) . . ? C26A C30 C32A 106.7(6) . . ? C31 C30 C32A 104.4(5) . . ? C32B C30 C32A 44.8(6) . . ? C26A C30 C26B 5.0(4) . . ? C31 C30 C26B 115.6(4) . . ? C32B C30 C26B 127.2(7) . . ? C32A C30 C26B 103.7(5) . . ? C26A C30 H30 111.5 . . ? C31 C30 H30 111.5 . . ? C32B C30 H30 67.6 . . ? C32A C30 H30 111.5 . . ? C26B C30 H30 109.7 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C1S N1S C1S 68.2(4) 2_665 15_565 ? C1S N1S C1S 105.0(8) 2_665 . ? C1S N1S C1S 68.2(4) 15_565 . ? C1S N1S C1S 68.2(4) 2_665 16_655 ? C1S N1S C1S 105.0(8) 15_565 16_655 ? C1S N1S C1S 68.2(4) . 16_655 ? C1S N1S Co1 127.5(4) 2_665 . ? C1S N1S Co1 127.5(4) 15_565 . ? C1S N1S Co1 127.5(4) . . ? C1S N1S Co1 127.5(4) 16_655 . ? N1S C1S C2S 112.2(7) . . ? N1S C1S C1S 55.9(2) . 15_565 ? C2S C1S C1S 81.6(5) . 15_565 ? N1S C1S C1S 55.9(2) . 16_655 ? C2S C1S C1S 77.0(5) . 16_655 ? C1S C1S C1S 90.002(3) 15_565 16_655 ? N1S C1S N2S 91.2(6) . 15_565 ? C2S C1S N2S 32.9(4) . 15_565 ? C1S C1S N2S 48.9(4) 15_565 15_565 ? C1S C1S N2S 83.5(3) 16_655 15_565 ? N1S C1S C2S 91.2(6) . 15_565 ? C2S C1S C2S 32.9(4) . 15_565 ? C1S C1S C2S 48.9(4) 15_565 15_565 ? C1S C1S C2S 83.5(3) 16_655 15_565 ? N2S C1S C2S 0.0(7) 15_565 15_565 ? N1S C1S N2S 87.4(6) . 16_655 ? C2S C1S N2S 30.4(4) . 16_655 ? C1S C1S N2S 80.4(4) 15_565 16_655 ? C1S C1S N2S 46.8(3) 16_655 16_655 ? N2S C1S N2S 44.3(4) 15_565 16_655 ? C2S C1S N2S 44.3(4) 15_565 16_655 ? N1S C1S C2S 87.4(6) . 16_655 ? C2S C1S C2S 30.4(4) . 16_655 ? C1S C1S C2S 80.4(4) 15_565 16_655 ? C1S C1S C2S 46.8(3) 16_655 16_655 ? N2S C1S C2S 44.3(4) 15_565 16_655 ? C2S C1S C2S 44.3(4) 15_565 16_655 ? N2S C1S C2S 0.0(8) 16_655 16_655 ? N2S C2S C2S 0.0(15) 16_655 16_655 ? N2S C2S N2S 89.996(8) 16_655 15_565 ? C2S C2S N2S 89.996(8) 16_655 15_565 ? N2S C2S C2S 89.996(8) 16_655 15_565 ? C2S C2S C2S 89.996(8) 16_655 15_565 ? N2S C2S C2S 0.0(14) 15_565 15_565 ? N2S C2S C1S 103.9(6) 16_655 . ? C2S C2S C1S 103.9(6) 16_655 . ? N2S C2S C1S 97.0(7) 15_565 . ? C2S C2S C1S 97.0(7) 15_565 . ? N2S C2S C2S 44.998(4) 16_655 2_665 ? C2S C2S C2S 44.998(4) 16_655 2_665 ? N2S C2S C2S 44.998(8) 15_565 2_665 ? C2S C2S C2S 44.998(8) 15_565 2_665 ? C1S C2S C2S 104.8(5) . 2_665 ? N2S C2S N2S 44.998(4) 16_655 2_665 ? C2S C2S N2S 44.998(4) 16_655 2_665 ? N2S C2S N2S 44.998(8) 15_565 2_665 ? C2S C2S N2S 44.998(8) 15_565 2_665 ? C1S C2S N2S 104.8(5) . 2_665 ? C2S C2S N2S 0.0(12) 2_665 2_665 ? N2S C2S C1S 50.1(5) 16_655 16_655 ? C2S C2S C1S 50.1(5) 16_655 16_655 ? N2S C2S C1S 100.7(5) 15_565 16_655 ? C2S C2S C1S 100.7(5) 15_565 16_655 ? C1S C2S C1S 54.1(5) . 16_655 ? C2S C2S C1S 71.2(6) 2_665 16_655 ? N2S C2S C1S 71.2(6) 2_665 16_655 ? N2S C2S C1S 95.1(6) 16_655 15_565 ? C2S C2S C1S 95.1(6) 16_655 15_565 ? N2S C2S C1S 45.7(4) 15_565 15_565 ? C2S C2S C1S 45.7(4) 15_565 15_565 ? C1S C2S C1S 51.7(5) . 15_565 ? C2S C2S C1S 64.5(6) 2_665 15_565 ? N2S C2S C1S 64.5(6) 2_665 15_565 ? C1S C2S C1S 70.0(6) 16_655 15_565 ? C3S N3S C3S 68.8(4) 16_655 2_665 ? C3S N3S C3S 106.0(7) 16_655 15_565 ? C3S N3S C3S 68.8(4) 2_665 15_565 ? C3S N3S C3S 68.8(4) 16_655 . ? C3S N3S C3S 106.0(7) 2_665 . ? C3S N3S C3S 68.8(4) 15_565 . ? C3S N3S Co1 127.0(4) 16_655 . ? C3S N3S Co1 127.0(4) 2_665 . ? C3S N3S Co1 127.0(4) 15_565 . ? C3S N3S Co1 127.0(4) . . ? N3S C3S C4S 110.7(6) . . ? N3S C3S C3S 55.60(19) . 16_655 ? C4S C3S C3S 77.2(5) . 16_655 ? N3S C3S C3S 55.61(19) . 15_565 ? C4S C3S C3S 79.9(5) . 15_565 ? C3S C3S C3S 89.998(3) 16_655 15_565 ? N3S C3S N4S 89.1(5) . 15_565 ? C4S C3S N4S 32.2(4) . 15_565 ? C3S C3S N4S 82.3(3) 16_655 15_565 ? C3S C3S N4S 47.8(3) 15_565 15_565 ? N3S C3S C4S 89.1(5) . 15_565 ? C4S C3S C4S 32.2(4) . 15_565 ? C3S C3S C4S 82.3(3) 16_655 15_565 ? C3S C3S C4S 47.8(3) 15_565 15_565 ? N4S C3S C4S 0.0(6) 15_565 15_565 ? N3S C3S N4S 86.9(5) . 16_655 ? C4S C3S N4S 30.7(4) . 16_655 ? C3S C3S N4S 46.6(3) 16_655 16_655 ? C3S C3S N4S 80.6(3) 15_565 16_655 ? N4S C3S N4S 44.2(4) 15_565 16_655 ? C4S C3S N4S 44.2(4) 15_565 16_655 ? N3S C3S C4S 86.9(5) . 16_655 ? C4S C3S C4S 30.7(4) . 16_655 ? C3S C3S C4S 46.6(3) 16_655 16_655 ? C3S C3S C4S 80.6(3) 15_565 16_655 ? N4S C3S C4S 44.2(4) 15_565 16_655 ? C4S C3S C4S 44.2(4) 15_565 16_655 ? N4S C3S C4S 0.0(9) 16_655 16_655 ? N4S C4S C4S 0.0(11) 15_565 15_565 ? N4S C4S N4S 90.000(4) 15_565 16_655 ? C4S C4S N4S 90.000(4) 15_565 16_655 ? N4S C4S C4S 90.000(4) 15_565 16_655 ? C4S C4S C4S 90.000(4) 15_565 16_655 ? N4S C4S C4S 0.0(15) 16_655 16_655 ? N4S C4S C3S 99.2(7) 15_565 . ? C4S C4S C3S 99.2(7) 15_565 . ? N4S C4S C3S 103.4(6) 16_655 . ? C4S C4S C3S 103.4(6) 16_655 . ? N4S C4S N4S 45.012(7) 15_565 2_665 ? C4S C4S N4S 45.012(7) 15_565 2_665 ? N4S C4S N4S 44.989(4) 16_655 2_665 ? C4S C4S N4S 44.989(4) 16_655 2_665 ? C3S C4S N4S 106.1(4) . 2_665 ? N4S C4S C4S 45.012(7) 15_565 2_665 ? C4S C4S C4S 45.012(7) 15_565 2_665 ? N4S C4S C4S 44.989(4) 16_655 2_665 ? C4S C4S C4S 44.989(4) 16_655 2_665 ? C3S C4S C4S 106.1(4) . 2_665 ? N4S C4S C4S 0.0(10) 2_665 2_665 ? N4S C4S C3S 100.2(5) 15_565 16_655 ? C4S C4S C3S 100.2(5) 15_565 16_655 ? N4S C4S C3S 48.6(5) 16_655 16_655 ? C4S C4S C3S 48.6(5) 16_655 16_655 ? C3S C4S C3S 55.0(5) . 16_655 ? N4S C4S C3S 69.9(6) 2_665 16_655 ? C4S C4S C3S 69.9(6) 2_665 16_655 ? N4S C4S C3S 45.9(4) 15_565 15_565 ? C4S C4S C3S 45.9(4) 15_565 15_565 ? N4S C4S C3S 96.8(5) 16_655 15_565 ? C4S C4S C3S 96.8(5) 16_655 15_565 ? C3S C4S C3S 53.5(5) . 15_565 ? N4S C4S C3S 65.9(6) 2_665 15_565 ? C4S C4S C3S 65.9(6) 2_665 15_565 ? C3S C4S C3S 71.7(5) 16_655 15_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C7 -2.9(3) 15_565 . . . ? N1 Co1 N1 C7 86.7(2) 2_665 . . . ? N1 Co1 N1 C7 176.16(17) 16_655 . . . ? N1S Co1 N1 C7 -93.4(2) . . . . ? N3S Co1 N1 C7 86.6(2) . . . . ? N1 Co1 N1 C8 -176.09(18) 15_565 . . 16_655 ? N1 Co1 N1 C8 -86.5(2) 2_665 . . 16_655 ? N1 Co1 N1 C8 2.9(3) 16_655 . . 16_655 ? N1S Co1 N1 C8 93.4(2) . . . 16_655 ? N3S Co1 N1 C8 -86.6(2) . . . 16_655 ? C6 C1 C2 C3 -1.9(4) . . . . ? C8 C1 C2 C3 173.4(3) 16_655 . . . ? C9 O1 C3 C2 2.7(4) . . . . ? C9 O1 C3 C4 -177.3(3) . . . . ? C1 C2 C3 O1 -178.1(3) . . . . ? C1 C2 C3 C4 2.0(4) . . . . ? C21B O2 C4 C5 14.3(5) . . . . ? C21A O2 C4 C5 4.0(5) . . . . ? C21B O2 C4 C3 -168.7(3) . . . . ? C21A O2 C4 C3 -179.0(3) . . . . ? O1 C3 C4 O2 2.7(4) . . . . ? C2 C3 C4 O2 -177.4(3) . . . . ? O1 C3 C4 C5 179.8(3) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? O2 C4 C5 C6 175.3(3) . . . . ? C3 C4 C5 C6 -1.4(5) . . . . ? C4 C5 C6 C1 1.5(5) . . . . ? C4 C5 C6 C7 -172.4(3) . . . . ? C2 C1 C6 C5 0.2(5) . . . . ? C8 C1 C6 C5 -176.2(3) 16_655 . . . ? C2 C1 C6 C7 175.4(3) . . . . ? C8 C1 C6 C7 -1.1(3) 16_655 . . . ? C8 N2 C7 N1 -1.1(5) . . . . ? C8 N2 C7 C6 175.3(3) . . . . ? C8 N1 C7 N2 176.9(3) 16_655 . . . ? Co1 N1 C7 N2 2.6(4) . . . . ? C8 N1 C7 C6 0.1(3) 16_655 . . . ? Co1 N1 C7 C6 -174.19(19) . . . . ? C5 C6 C7 N2 -1.9(5) . . . . ? C1 C6 C7 N2 -176.4(3) . . . . ? C5 C6 C7 N1 175.2(3) . . . . ? C1 C6 C7 N1 0.7(3) . . . . ? C7 N2 C8 N1 1.2(5) . . . 15_565 ? C7 N2 C8 C1 -174.5(3) . . . 15_565 ? C3 O1 C9 C14 -99.2(3) . . . . ? C3 O1 C9 C10 86.0(3) . . . . ? C14 C9 C10 C11 -0.1(5) . . . . ? O1 C9 C10 C11 174.2(3) . . . . ? C14 C9 C10 C15 -177.1(3) . . . . ? O1 C9 C10 C15 -2.8(4) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C15 C10 C11 C12 177.2(3) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C11 C12 C13 C14 -1.0(7) . . . . ? O1 C9 C14 C13 -174.9(3) . . . . ? C10 C9 C14 C13 -0.6(5) . . . . ? O1 C9 C14 C18 2.6(4) . . . . ? C10 C9 C14 C18 176.9(3) . . . . ? C12 C13 C14 C9 1.1(5) . . . . ? C12 C13 C14 C18 -176.3(4) . . . . ? C11 C10 C15 C17 20.4(5) . . . . ? C9 C10 C15 C17 -162.8(3) . . . . ? C11 C10 C15 C16 -102.2(4) . . . . ? C9 C10 C15 C16 74.6(4) . . . . ? C9 C14 C18 C20 -82.5(5) . . . . ? C13 C14 C18 C20 94.8(5) . . . . ? C9 C14 C18 C19 154.9(5) . . . . ? C13 C14 C18 C19 -27.8(6) . . . . ? C21B O2 C21A C22A 10(2) . . . . ? C4 O2 C21A C22A 96.8(4) . . . . ? C21B O2 C21A C26A -171(3) . . . . ? C4 O2 C21A C26A -83.5(4) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 179.7(5) . . . . ? C26A C21A C22A C27A 176.3(6) . . . . ? O2 C21A C22A C27A -4.0(6) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -176.4(6) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 175.6(5) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -174.9(6) . . . . ? O2 C21A C26A C30 5.5(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -179.7(5) . . . . ? C4 O2 C21B C22B 95.1(3) . . . . ? C21A O2 C21B C22B -168(3) . . . . ? C4 O2 C21B C26B -85.3(4) . . . . ? C21A O2 C21B C26B 12(2) . . . . ? O2 C21B C22B C23B 179.6(4) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 2.3(5) . . . . ? C26B C21B C22B C27B -177.4(5) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B 177.2(5) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -176.9(4) . . . . ? O2 C21B C26B C25B -179.6(5) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -2.5(4) . . . . ? C22B C21B C26B C30 177.2(4) . . . . ? C23A C22A C27A C29A 22.0(12) . . . . ? C21A C22A C27A C29A -154.3(10) . . . . ? C23A C22A C27A C28A -104.3(9) . . . . ? C21A C22A C27A C28A 79.4(9) . . . . ? C23B C22B C27B C29B 72.1(8) . . . . ? C21B C22B C27B C29B -110.7(7) . . . . ? C23B C22B C27B C28B -50.8(8) . . . . ? C21B C22B C27B C28B 126.5(7) . . . . ? C25A C26A C30 C31 79.6(5) . . . . ? C21A C26A C30 C31 -105.2(5) . . . . ? C25A C26A C30 C32B -76.7(10) . . . . ? C21A C26A C30 C32B 98.5(10) . . . . ? C25A C26A C30 C32A -33.4(6) . . . . ? C21A C26A C30 C32A 141.8(5) . . . . ? C25A C26A C30 C26B -86(3) . . . . ? C21A C26A C30 C26B 89(3) . . . . ? C25B C26B C30 C26A 93(3) . . . . ? C21B C26B C30 C26A -84(3) . . . . ? C25B C26B C30 C31 78.5(5) . . . . ? C21B C26B C30 C31 -98.5(5) . . . . ? C25B C26B C30 C32B -78.0(9) . . . . ? C21B C26B C30 C32B 105.0(9) . . . . ? C25B C26B C30 C32A -35.1(5) . . . . ? C21B C26B C30 C32A 147.9(4) . . . . ? N1 Co1 N1S C1S -134.6(5) 15_565 . . 2_665 ? N1 Co1 N1S C1S 135.4(5) 2_665 . . 2_665 ? N1 Co1 N1S C1S 45.4(5) 16_655 . . 2_665 ? N1 Co1 N1S C1S -44.6(5) . . . 2_665 ? N3S Co1 N1S C1S 0(100) . . . 2_665 ? N1 Co1 N1S C1S 135.4(5) 15_565 . . 15_565 ? N1 Co1 N1S C1S 45.4(5) 2_665 . . 15_565 ? N1 Co1 N1S C1S -44.6(5) 16_655 . . 15_565 ? N1 Co1 N1S C1S -134.6(5) . . . 15_565 ? N3S Co1 N1S C1S 0(100) . . . 15_565 ? N1 Co1 N1S C1S 45.4(5) 15_565 . . . ? N1 Co1 N1S C1S -44.6(5) 2_665 . . . ? N1 Co1 N1S C1S -134.6(5) 16_655 . . . ? N1 Co1 N1S C1S 135.4(5) . . . . ? N3S Co1 N1S C1S 0(98) . . . . ? N1 Co1 N1S C1S -44.6(5) 15_565 . . 16_655 ? N1 Co1 N1S C1S -134.6(5) 2_665 . . 16_655 ? N1 Co1 N1S C1S 135.4(5) 16_655 . . 16_655 ? N1 Co1 N1S C1S 45.4(5) . . . 16_655 ? N3S Co1 N1S C1S 0(71) . . . 16_655 ? C1S N1S C1S C2S 3.4(6) 2_665 . . . ? C1S N1S C1S C2S 62.1(6) 15_565 . . . ? C1S N1S C1S C2S -55.2(7) 16_655 . . . ? Co1 N1S C1S C2S -176.6(6) . . . . ? C1S N1S C1S C1S -58.7(2) 2_665 . . 15_565 ? C1S N1S C1S C1S -117.3(5) 16_655 . . 15_565 ? Co1 N1S C1S C1S 121.3(2) . . . 15_565 ? C1S N1S C1S C1S 58.7(2) 2_665 . . 16_655 ? C1S N1S C1S C1S 117.3(5) 15_565 . . 16_655 ? Co1 N1S C1S C1S -121.3(2) . . . 16_655 ? C1S N1S C1S N2S -22.6(2) 2_665 . . 15_565 ? C1S N1S C1S N2S 36.0(4) 15_565 . . 15_565 ? C1S N1S C1S N2S -81.3(3) 16_655 . . 15_565 ? Co1 N1S C1S N2S 157.4(2) . . . 15_565 ? C1S N1S C1S C2S -22.6(2) 2_665 . . 15_565 ? C1S N1S C1S C2S 36.0(4) 15_565 . . 15_565 ? C1S N1S C1S C2S -81.3(3) 16_655 . . 15_565 ? Co1 N1S C1S C2S 157.4(2) . . . 15_565 ? C1S N1S C1S N2S 21.5(2) 2_665 . . 16_655 ? C1S N1S C1S N2S 80.2(3) 15_565 . . 16_655 ? C1S N1S C1S N2S -37.1(4) 16_655 . . 16_655 ? Co1 N1S C1S N2S -158.5(2) . . . 16_655 ? C1S N1S C1S C2S 21.5(2) 2_665 . . 16_655 ? C1S N1S C1S C2S 80.2(3) 15_565 . . 16_655 ? C1S N1S C1S C2S -37.1(4) 16_655 . . 16_655 ? Co1 N1S C1S C2S -158.5(2) . . . 16_655 ? N1S C1S C2S N2S 37.8(15) . . . 16_655 ? C1S C1S C2S N2S 85.5(12) 15_565 . . 16_655 ? C1S C1S C2S N2S -6.5(12) 16_655 . . 16_655 ? N2S C1S C2S N2S 91.73(15) 15_565 . . 16_655 ? C2S C1S C2S N2S 91.73(15) 15_565 . . 16_655 ? C2S C1S C2S N2S 0.000(2) 16_655 . . 16_655 ? N1S C1S C2S C2S 37.8(15) . . . 16_655 ? C1S C1S C2S C2S 85.5(12) 15_565 . . 16_655 ? C1S C1S C2S C2S -6.5(12) 16_655 . . 16_655 ? N2S C1S C2S C2S 91.73(15) 15_565 . . 16_655 ? C2S C1S C2S C2S 91.73(15) 15_565 . . 16_655 ? N2S C1S C2S C2S 0.000(2) 16_655 . . 16_655 ? N1S C1S C2S N2S -53.9(14) . . . 15_565 ? C1S C1S C2S N2S -6.2(11) 15_565 . . 15_565 ? C1S C1S C2S N2S -98.2(11) 16_655 . . 15_565 ? C2S C1S C2S N2S 0.000(2) 15_565 . . 15_565 ? N2S C1S C2S N2S -91.73(15) 16_655 . . 15_565 ? C2S C1S C2S N2S -91.73(15) 16_655 . . 15_565 ? N1S C1S C2S C2S -53.9(14) . . . 15_565 ? C1S C1S C2S C2S -6.2(11) 15_565 . . 15_565 ? C1S C1S C2S C2S -98.2(11) 16_655 . . 15_565 ? N2S C1S C2S C2S 0.000(2) 15_565 . . 15_565 ? N2S C1S C2S C2S -91.73(15) 16_655 . . 15_565 ? C2S C1S C2S C2S -91.73(15) 16_655 . . 15_565 ? N1S C1S C2S C2S -8.7(15) . . . 2_665 ? C1S C1S C2S C2S 39.0(12) 15_565 . . 2_665 ? C1S C1S C2S C2S -53.0(12) 16_655 . . 2_665 ? N2S C1S C2S C2S 45.20(17) 15_565 . . 2_665 ? C2S C1S C2S C2S 45.20(17) 15_565 . . 2_665 ? N2S C1S C2S C2S -46.52(10) 16_655 . . 2_665 ? C2S C1S C2S C2S -46.52(10) 16_655 . . 2_665 ? N1S C1S C2S N2S -8.7(15) . . . 2_665 ? C1S C1S C2S N2S 39.0(12) 15_565 . . 2_665 ? C1S C1S C2S N2S -53.0(12) 16_655 . . 2_665 ? N2S C1S C2S N2S 45.20(17) 15_565 . . 2_665 ? C2S C1S C2S N2S 45.20(17) 15_565 . . 2_665 ? N2S C1S C2S N2S -46.52(10) 16_655 . . 2_665 ? C2S C1S C2S N2S -46.52(10) 16_655 . . 2_665 ? N1S C1S C2S C1S 44.3(3) . . . 16_655 ? C1S C1S C2S C1S 91.97(12) 15_565 . . 16_655 ? N2S C1S C2S C1S 98.2(11) 15_565 . . 16_655 ? C2S C1S C2S C1S 98.2(11) 15_565 . . 16_655 ? N2S C1S C2S C1S 6.5(12) 16_655 . . 16_655 ? C2S C1S C2S C1S 6.5(12) 16_655 . . 16_655 ? N1S C1S C2S C1S -47.7(3) . . . 15_565 ? C1S C1S C2S C1S -91.97(12) 16_655 . . 15_565 ? N2S C1S C2S C1S 6.2(11) 15_565 . . 15_565 ? C2S C1S C2S C1S 6.2(11) 15_565 . . 15_565 ? N2S C1S C2S C1S -85.5(12) 16_655 . . 15_565 ? C2S C1S C2S C1S -85.5(12) 16_655 . . 15_565 ? N1 Co1 N3S C3S 34.4(4) 15_565 . . 16_655 ? N1 Co1 N3S C3S 124.4(4) 2_665 . . 16_655 ? N1 Co1 N3S C3S -145.6(4) 16_655 . . 16_655 ? N1 Co1 N3S C3S -55.6(4) . . . 16_655 ? N1S Co1 N3S C3S 0(46) . . . 16_655 ? N1 Co1 N3S C3S 124.4(4) 15_565 . . 2_665 ? N1 Co1 N3S C3S -145.6(4) 2_665 . . 2_665 ? N1 Co1 N3S C3S -55.6(4) 16_655 . . 2_665 ? N1 Co1 N3S C3S 34.4(4) . . . 2_665 ? N1S Co1 N3S C3S 0(100) . . . 2_665 ? N1 Co1 N3S C3S -145.6(4) 15_565 . . 15_565 ? N1 Co1 N3S C3S -55.6(4) 2_665 . . 15_565 ? N1 Co1 N3S C3S 34.4(4) 16_655 . . 15_565 ? N1 Co1 N3S C3S 124.4(4) . . . 15_565 ? N1S Co1 N3S C3S 0(100) . . . 15_565 ? N1 Co1 N3S C3S -55.6(4) 15_565 . . . ? N1 Co1 N3S C3S 34.4(4) 2_665 . . . ? N1 Co1 N3S C3S 124.4(4) 16_655 . . . ? N1 Co1 N3S C3S -145.6(4) . . . . ? N1S Co1 N3S C3S 0(100) . . . . ? C3S N3S C3S C4S 57.0(6) 16_655 . . . ? C3S N3S C3S C4S -2.0(5) 2_665 . . . ? C3S N3S C3S C4S -61.0(6) 15_565 . . . ? Co1 N3S C3S C4S 178.0(5) . . . . ? C3S N3S C3S C3S -59.0(2) 2_665 . . 16_655 ? C3S N3S C3S C3S -117.9(4) 15_565 . . 16_655 ? Co1 N3S C3S C3S 121.0(2) . . . 16_655 ? C3S N3S C3S C3S 117.9(4) 16_655 . . 15_565 ? C3S N3S C3S C3S 59.0(2) 2_665 . . 15_565 ? Co1 N3S C3S C3S -121.0(2) . . . 15_565 ? C3S N3S C3S N4S 81.4(3) 16_655 . . 15_565 ? C3S N3S C3S N4S 22.4(2) 2_665 . . 15_565 ? C3S N3S C3S N4S -36.6(4) 15_565 . . 15_565 ? Co1 N3S C3S N4S -157.6(2) . . . 15_565 ? C3S N3S C3S C4S 81.4(3) 16_655 . . 15_565 ? C3S N3S C3S C4S 22.4(2) 2_665 . . 15_565 ? C3S N3S C3S C4S -36.6(4) 15_565 . . 15_565 ? Co1 N3S C3S C4S -157.6(2) . . . 15_565 ? C3S N3S C3S N4S 37.2(4) 16_655 . . 16_655 ? C3S N3S C3S N4S -21.8(2) 2_665 . . 16_655 ? C3S N3S C3S N4S -80.7(3) 15_565 . . 16_655 ? Co1 N3S C3S N4S 158.2(2) . . . 16_655 ? C3S N3S C3S C4S 37.2(4) 16_655 . . 16_655 ? C3S N3S C3S C4S -21.8(2) 2_665 . . 16_655 ? C3S N3S C3S C4S -80.7(3) 15_565 . . 16_655 ? Co1 N3S C3S C4S 158.2(2) . . . 16_655 ? N3S C3S C4S N4S 50.8(13) . . . 15_565 ? C3S C3S C4S N4S 96.0(10) 16_655 . . 15_565 ? C3S C3S C4S N4S 3.7(10) 15_565 . . 15_565 ? C4S C3S C4S N4S 0.000(1) 15_565 . . 15_565 ? N4S C3S C4S N4S 92.23(13) 16_655 . . 15_565 ? C4S C3S C4S N4S 92.23(13) 16_655 . . 15_565 ? N3S C3S C4S C4S 50.8(13) . . . 15_565 ? C3S C3S C4S C4S 96.0(10) 16_655 . . 15_565 ? C3S C3S C4S C4S 3.7(10) 15_565 . . 15_565 ? N4S C3S C4S C4S 0.000(1) 15_565 . . 15_565 ? N4S C3S C4S C4S 92.23(13) 16_655 . . 15_565 ? C4S C3S C4S C4S 92.23(13) 16_655 . . 15_565 ? N3S C3S C4S N4S -41.4(13) . . . 16_655 ? C3S C3S C4S N4S 3.8(11) 16_655 . . 16_655 ? C3S C3S C4S N4S -88.5(11) 15_565 . . 16_655 ? N4S C3S C4S N4S -92.23(13) 15_565 . . 16_655 ? C4S C3S C4S N4S -92.23(13) 15_565 . . 16_655 ? C4S C3S C4S N4S 0.000(5) 16_655 . . 16_655 ? N3S C3S C4S C4S -41.4(13) . . . 16_655 ? C3S C3S C4S C4S 3.8(11) 16_655 . . 16_655 ? C3S C3S C4S C4S -88.5(11) 15_565 . . 16_655 ? N4S C3S C4S C4S -92.23(13) 15_565 . . 16_655 ? C4S C3S C4S C4S -92.23(13) 15_565 . . 16_655 ? N4S C3S C4S C4S 0.000(5) 16_655 . . 16_655 ? N3S C3S C4S N4S 5.1(14) . . . 2_665 ? C3S C3S C4S N4S 50.3(11) 16_655 . . 2_665 ? C3S C3S C4S N4S -42.0(11) 15_565 . . 2_665 ? N4S C3S C4S N4S -45.69(15) 15_565 . . 2_665 ? C4S C3S C4S N4S -45.69(15) 15_565 . . 2_665 ? N4S C3S C4S N4S 46.54(12) 16_655 . . 2_665 ? C4S C3S C4S N4S 46.54(12) 16_655 . . 2_665 ? N3S C3S C4S C4S 5.1(14) . . . 2_665 ? C3S C3S C4S C4S 50.3(11) 16_655 . . 2_665 ? C3S C3S C4S C4S -42.0(11) 15_565 . . 2_665 ? N4S C3S C4S C4S -45.69(15) 15_565 . . 2_665 ? C4S C3S C4S C4S -45.69(15) 15_565 . . 2_665 ? N4S C3S C4S C4S 46.54(12) 16_655 . . 2_665 ? C4S C3S C4S C4S 46.54(12) 16_655 . . 2_665 ? N3S C3S C4S C3S -45.2(3) . . . 16_655 ? C3S C3S C4S C3S -92.32(12) 15_565 . . 16_655 ? N4S C3S C4S C3S -96.0(10) 15_565 . . 16_655 ? C4S C3S C4S C3S -96.0(10) 15_565 . . 16_655 ? N4S C3S C4S C3S -3.8(11) 16_655 . . 16_655 ? C4S C3S C4S C3S -3.8(11) 16_655 . . 16_655 ? N3S C3S C4S C3S 47.1(3) . . . 15_565 ? C3S C3S C4S C3S 92.32(12) 16_655 . . 15_565 ? N4S C3S C4S C3S -3.7(10) 15_565 . . 15_565 ? C4S C3S C4S C3S -3.7(10) 15_565 . . 15_565 ? N4S C3S C4S C3S 88.5(11) 16_655 . . 15_565 ? C4S C3S C4S C3S 88.5(11) 16_655 . . 15_565 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 24.39 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.680 _refine_diff_density_min -0.432 _refine_diff_density_rms 0.064 data_PNC[cIm-Co-vIm]2 _database_code_depnum_ccdc_archive 'CCDC 900377' #TrackingRef '900377_PNC[cIm-Co-vIm]2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C144.50 H184.25 Cl9.75 Co N12 O15.25' _chemical_formula_weight 2737.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.603(3) _cell_length_b 37.603(3) _cell_length_c 37.603(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 53170(8) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 91092 _cell_measurement_theta_min 0.9 _cell_measurement_theta_max 25.6 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.07 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.026 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 17400 _exptl_absorpt_coefficient_mu 0.296 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9796 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7645 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min 1 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 0.74 _diffrn_reflns_theta_max 24.20 _reflns_number_total 7645 _reflns_number_gt 6962 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7645 _refine_ls_number_parameters 343 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.1223 _refine_ls_R_factor_gt 0.1171 _refine_ls_wR_factor_ref 0.4004 _refine_ls_wR_factor_gt 0.3932 _refine_ls_goodness_of_fit_ref 1.865 _refine_ls_restrained_S_all 1.874 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Co1 Co 0.7500 0.7500 0.08430(2) 0.0325(4) Uani 1 4 d S . . O1 O 0.61142(6) 0.90483(6) 0.11125(7) 0.0439(6) Uani 1 1 d . A . O2 O 0.66931(6) 0.94011(6) 0.11190(8) 0.0609(8) Uani 1 1 d . . . N1 N 0.72167(6) 0.79327(6) 0.08457(7) 0.0347(6) Uani 1 1 d . A . N2 N 0.76843(7) 0.83769(6) 0.08773(7) 0.0407(7) Uani 1 1 d . A . C1 C 0.67439(8) 0.83207(7) 0.09112(9) 0.0366(7) Uani 1 1 d . . . C2 C 0.64107(8) 0.84842(8) 0.09746(9) 0.0388(7) Uani 1 1 d . A . H2 H 0.6196 0.8351 0.0975 0.058 Uiso 1 1 calc R . . C3 C 0.64122(7) 0.88463(8) 0.10360(9) 0.0374(7) Uani 1 1 d . . . C4 C 0.67312(8) 0.90487(8) 0.10345(10) 0.0469(8) Uani 1 1 d . A . C5 C 0.70566(8) 0.88886(7) 0.09632(11) 0.0475(9) Uani 1 1 d . . . H5 H 0.7270 0.9023 0.0953 0.071 Uiso 1 1 calc R A . C6 C 0.70567(8) 0.85213(8) 0.09074(9) 0.0416(8) Uani 1 1 d . A . C7 C 0.73505(8) 0.82714(7) 0.08660(8) 0.0364(7) Uani 1 1 d . . . C8 C 0.79510(8) 0.81474(7) 0.08697(8) 0.0361(7) Uani 1 1 d . . . C9 C 0.57837(8) 0.88722(8) 0.11405(10) 0.0458(8) Uani 1 1 d . . . C10 C 0.56934(9) 0.87290(9) 0.14696(12) 0.0581(10) Uani 1 1 d . A . C11 C 0.53501(12) 0.85827(11) 0.15041(16) 0.0802(16) Uani 1 1 d . . . H11 H 0.5276 0.8480 0.1723 0.120 Uiso 1 1 calc R A . C12 C 0.51220(12) 0.85912(15) 0.1215(2) 0.097(2) Uani 1 1 d . A . H12 H 0.4889 0.8496 0.1239 0.146 Uiso 1 1 calc R . . C13 C 0.52257(12) 0.87349(15) 0.08906(18) 0.0911(19) Uani 1 1 d . . . H13 H 0.5064 0.8730 0.0697 0.137 Uiso 1 1 calc R A . C14 C 0.55610(10) 0.88860(11) 0.08422(12) 0.0636(11) Uani 1 1 d . A . C15 C 0.59492(12) 0.87465(11) 0.17838(12) 0.0676(11) Uani 1 1 d . . . H15 H 0.6191 0.8685 0.1691 0.101 Uiso 1 1 calc R A . C16 C 0.59682(13) 0.91316(12) 0.19280(14) 0.0722(12) Uani 1 1 d . A . H16A H 0.6038 0.9293 0.1736 0.108 Uiso 1 1 calc R . . H16B H 0.6144 0.9144 0.2120 0.108 Uiso 1 1 calc R . . H16C H 0.5735 0.9201 0.2020 0.108 Uiso 1 1 calc R . . C17 C 0.5875(2) 0.84995(15) 0.20954(17) 0.108(2) Uani 1 1 d . A . H17A H 0.5670 0.8589 0.2230 0.161 Uiso 1 1 calc R . . H17B H 0.6084 0.8490 0.2251 0.161 Uiso 1 1 calc R . . H17C H 0.5822 0.8260 0.2006 0.161 Uiso 1 1 calc R . . C18 C 0.56850(13) 0.90621(13) 0.05030(14) 0.0779(14) Uani 1 1 d . . . H18 H 0.5945 0.9014 0.0478 0.117 Uiso 1 1 calc R A . C19 C 0.5504(3) 0.8926(2) 0.0169(2) 0.135(3) Uani 1 1 d . A . H19A H 0.5559 0.8674 0.0136 0.203 Uiso 1 1 calc R . . H19B H 0.5588 0.9062 -0.0037 0.203 Uiso 1 1 calc R . . H19C H 0.5246 0.8956 0.0192 0.203 Uiso 1 1 calc R . . C20 C 0.56382(19) 0.94685(15) 0.0543(2) 0.1024(19) Uani 1 1 d . A . H20A H 0.5400 0.9520 0.0636 0.154 Uiso 1 1 calc R . . H20B H 0.5667 0.9583 0.0310 0.154 Uiso 1 1 calc R . . H20C H 0.5818 0.9561 0.0708 0.154 Uiso 1 1 calc R . . C21A C 0.70008(12) 0.96077(15) 0.11044(14) 0.034(3) Uiso 0.467(9) 1 d PG A 1 C22A C 0.70931(15) 0.98098(17) 0.08090(12) 0.065(2) Uiso 0.467(9) 1 d PG A 1 C23A C 0.74004(16) 1.00152(15) 0.08143(15) 0.057(2) Uiso 0.467(9) 1 d PG A 1 H23A H 0.7464 1.0153 0.0612 0.086 Uiso 0.467(9) 1 calc PR A 1 C24A C 0.76153(12) 1.00186(14) 0.11151(18) 0.060(2) Uiso 0.467(9) 1 d PG A 1 H24A H 0.7825 1.0159 0.1119 0.090 Uiso 0.467(9) 1 calc PR A 1 C25A C 0.75229(12) 0.98165(14) 0.14105(15) 0.052(2) Uiso 0.467(9) 1 d PG A 1 H25A H 0.7670 0.9819 0.1616 0.077 Uiso 0.467(9) 1 calc PR A 1 C26A C 0.72157(13) 0.96111(13) 0.14052(13) 0.0350(16) Uiso 0.467(9) 1 d PG A 1 C21B C 0.69761(12) 0.96091(15) 0.10664(14) 0.049(3) Uiso 0.533(9) 1 d PG A 2 C22B C 0.69929(12) 0.97882(14) 0.07435(12) 0.0446(16) Uiso 0.533(9) 1 d PG A 2 C23B C 0.72855(13) 0.99999(12) 0.06646(12) 0.0565(19) Uiso 0.533(9) 1 d PG A 2 H23B H 0.7297 1.0122 0.0444 0.085 Uiso 0.533(9) 1 calc PR A 2 C24B C 0.75613(11) 1.00324(13) 0.09086(16) 0.061(2) Uiso 0.533(9) 1 d PG A 2 H24B H 0.7761 1.0177 0.0855 0.091 Uiso 0.533(9) 1 calc PR A 2 C25B C 0.75445(11) 0.98532(14) 0.12315(14) 0.0523(18) Uiso 0.533(9) 1 d PG A 2 H25B H 0.7733 0.9875 0.1398 0.078 Uiso 0.533(9) 1 calc PR A 2 C26B C 0.72519(14) 0.96416(15) 0.13104(12) 0.057(2) Uiso 0.533(9) 1 d PGD A 2 C27A C 0.6873(3) 0.9800(3) 0.0458(3) 0.066(2) Uiso 0.467(9) 1 d P A 1 H27A H 0.6798 0.9546 0.0432 0.099 Uiso 0.467(9) 1 calc PR A 1 C28A C 0.6492(3) 1.0029(4) 0.0480(4) 0.073(3) Uiso 0.467(9) 1 d P A 1 H28D H 0.6401 1.0070 0.0239 0.109 Uiso 0.467(9) 1 calc PR A 1 H28E H 0.6535 1.0258 0.0597 0.109 Uiso 0.467(9) 1 calc PR A 1 H28F H 0.6317 0.9893 0.0617 0.109 Uiso 0.467(9) 1 calc PR A 1 C29A C 0.7037(5) 0.9893(5) 0.0105(5) 0.134(6) Uiso 0.467(9) 1 d P A 1 H29A H 0.7140 0.9679 -0.0002 0.202 Uiso 0.467(9) 1 calc PR A 1 H29B H 0.7224 1.0071 0.0140 0.202 Uiso 0.467(9) 1 calc PR A 1 H29C H 0.6854 0.9990 -0.0054 0.202 Uiso 0.467(9) 1 calc PR A 1 C27B C 0.6687(2) 0.9739(2) 0.0484(2) 0.0573(19) Uiso 0.533(9) 1 d P A 2 H27B H 0.6493 0.9613 0.0615 0.086 Uiso 0.533(9) 1 calc PR A 2 C28B C 0.6551(3) 1.0105(3) 0.0392(4) 0.085(3) Uiso 0.533(9) 1 d P A 2 H28A H 0.6298 1.0091 0.0331 0.127 Uiso 0.533(9) 1 calc PR A 2 H28B H 0.6685 1.0199 0.0189 0.127 Uiso 0.533(9) 1 calc PR A 2 H28C H 0.6583 1.0263 0.0597 0.127 Uiso 0.533(9) 1 calc PR A 2 C29B C 0.6779(4) 0.9523(4) 0.0180(4) 0.111(4) Uiso 0.533(9) 1 d P A 2 H29D H 0.6907 0.9310 0.0259 0.166 Uiso 0.533(9) 1 calc PR A 2 H29E H 0.6930 0.9660 0.0018 0.166 Uiso 0.533(9) 1 calc PR A 2 H29F H 0.6561 0.9451 0.0055 0.166 Uiso 0.533(9) 1 calc PR A 2 C30 C 0.7187(2) 0.94244(16) 0.16960(14) 0.102(2) Uani 1 1 d D . . H30 H 0.7037 0.9209 0.1653 0.152 Uiso 1 1 calc R A 1 C31 C 0.70416(18) 0.96370(18) 0.20019(18) 0.105(2) Uani 1 1 d . A . H31A H 0.7196 0.9842 0.2046 0.158 Uiso 1 1 calc R . . H31B H 0.7032 0.9487 0.2215 0.158 Uiso 1 1 calc R . . H31C H 0.6802 0.9720 0.1943 0.158 Uiso 1 1 calc R . . C32A C 0.7587(3) 0.9306(3) 0.1834(3) 0.084(3) Uiso 0.544(15) 1 d P A 1 H32A H 0.7722 0.9519 0.1902 0.126 Uiso 0.544(15) 1 calc PR A 1 H32B H 0.7712 0.9182 0.1642 0.126 Uiso 0.544(15) 1 calc PR A 1 H32C H 0.7564 0.9148 0.2040 0.126 Uiso 0.544(15) 1 calc PR A 1 C32B C 0.7367(4) 0.9077(4) 0.1784(3) 0.092(4) Uiso 0.456(15) 1 d P A 2 H32D H 0.7221 0.8879 0.1699 0.138 Uiso 0.456(15) 1 calc PR A 2 H32E H 0.7398 0.9058 0.2042 0.138 Uiso 0.456(15) 1 calc PR A 2 H32F H 0.7601 0.9069 0.1668 0.138 Uiso 0.456(15) 1 calc PR A 2 N1S N 0.7500 0.7500 0.03228(16) 0.0434(12) Uani 1 4 d SD . . C1S C 0.7787(2) 0.7449(3) 0.0103(2) 0.071(2) Uiso 0.50 1 d PD . . C2S C 0.7678(2) 0.7476(3) -0.0244(2) 0.080(3) Uiso 0.25 1 d PD . . N2S N 0.7678(2) 0.7476(3) -0.0244(2) 0.080(3) Uiso 0.25 1 d PD . . N3S N 0.7500 0.7500 0.13696(16) 0.0416(12) Uani 1 4 d SD . . C3S C 0.7765(2) 0.7381(2) 0.1585(2) 0.0601(18) Uiso 0.50 1 d PD . . C4S C 0.7677(2) 0.7427(3) 0.19363(19) 0.0637(18) Uiso 0.25 1 d PD . . N4S N 0.7677(2) 0.7427(3) 0.19363(19) 0.0637(18) Uiso 0.25 1 d PD . . O1S O 0.8184(3) 0.6822(3) 0.2180(3) 0.110(3) Uiso 0.50 1 d PD . . C5T C 0.8100(3) 0.6502(3) 0.1985(3) 0.080(2) Uiso 0.50 1 d PD . . O2S O 0.5784(5) 0.7900(4) 0.0382(5) 0.187(6) Uiso 0.50 1 d PD . . C6S C 0.5819(5) 0.7962(5) 0.0007(5) 0.138(5) Uiso 0.50 1 d PD . . 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 0.0244(4) 0.0244(4) 0.0486(6) 0.000 0.000 0.000 O1 0.0306(11) 0.0348(11) 0.0664(15) -0.0049(10) 0.0058(9) 0.0053(8) O2 0.0315(11) 0.0308(11) 0.120(2) -0.0129(12) 0.0066(12) 0.0044(9) N1 0.0281(11) 0.0277(11) 0.0484(14) 0.0017(10) 0.0002(10) 0.0011(9) N2 0.0313(13) 0.0302(12) 0.0606(17) -0.0030(11) 0.0039(11) -0.0018(10) C1 0.0300(14) 0.0282(13) 0.0515(17) 0.0056(12) 0.0017(12) 0.0003(11) C2 0.0280(14) 0.0330(14) 0.0555(18) -0.0009(13) 0.0009(12) -0.0009(11) C3 0.0282(14) 0.0326(14) 0.0515(17) -0.0003(12) 0.0019(12) 0.0045(11) C4 0.0357(16) 0.0297(14) 0.075(2) -0.0009(14) 0.0016(15) 0.0051(12) C5 0.0291(14) 0.0270(14) 0.086(2) -0.0017(14) 0.0078(15) 0.0004(11) C6 0.0294(14) 0.0321(14) 0.0633(19) -0.0039(13) 0.0042(13) 0.0023(11) C7 0.0294(15) 0.0287(14) 0.0512(17) -0.0030(11) 0.0030(12) 0.0025(11) C8 0.0330(14) 0.0295(13) 0.0456(16) -0.0016(11) -0.0006(11) -0.0006(11) C9 0.0294(15) 0.0362(15) 0.072(2) -0.0173(14) 0.0030(14) 0.0029(12) C10 0.0464(19) 0.0358(16) 0.092(3) -0.0091(16) 0.0249(19) 0.0034(14) C11 0.057(2) 0.050(2) 0.133(4) -0.029(2) 0.045(3) -0.0079(18) C12 0.040(2) 0.088(3) 0.164(6) -0.066(4) 0.027(3) -0.014(2) C13 0.042(2) 0.100(4) 0.131(5) -0.062(4) -0.013(3) 0.008(2) C14 0.0397(18) 0.067(2) 0.084(3) -0.030(2) -0.0042(17) 0.0152(16) C15 0.074(3) 0.061(2) 0.068(2) 0.0044(19) 0.018(2) 0.019(2) C16 0.069(3) 0.074(3) 0.073(3) -0.015(2) -0.003(2) 0.012(2) C17 0.147(6) 0.082(3) 0.094(4) 0.016(3) 0.050(4) 0.038(4) C18 0.069(3) 0.081(3) 0.083(3) -0.020(2) -0.020(2) 0.024(2) C19 0.169(8) 0.133(6) 0.103(5) -0.029(4) -0.039(5) -0.013(5) C20 0.113(4) 0.074(3) 0.120(5) -0.002(3) -0.018(4) 0.022(3) C30 0.145(5) 0.083(3) 0.077(3) -0.017(3) -0.027(3) 0.057(4) C31 0.104(4) 0.106(4) 0.106(4) -0.039(3) -0.007(3) 0.038(3) N1S 0.0383(17) 0.0383(17) 0.054(3) 0.000 0.000 0.000 N3S 0.0338(16) 0.0338(16) 0.057(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.945(2) 2_665 ? Co1 N1 1.945(2) . ? Co1 N1 1.945(2) 16_655 ? Co1 N1 1.945(2) 15_565 ? Co1 N1S 1.956(6) . ? Co1 N3S 1.980(6) . ? O1 C3 1.384(3) . ? O1 C9 1.412(4) . ? O2 C21B 1.335(4) . ? O2 C4 1.370(4) . ? O2 C21A 1.395(4) . ? N1 C7 1.371(4) . ? N1 C8 1.374(4) 16_655 ? N2 C7 1.317(4) . ? N2 C8 1.323(4) . ? C1 C6 1.397(4) . ? C1 C2 1.416(4) . ? C1 C8 1.457(4) 16_655 ? C2 C3 1.381(4) . ? C2 H2 0.9500 . ? C3 C4 1.420(4) . ? C4 C5 1.390(4) . ? C5 C6 1.397(4) . ? C5 H5 0.9500 . ? C6 C7 1.459(4) . ? C8 N1 1.374(4) 15_565 ? C8 C1 1.457(4) 15_565 ? C9 C10 1.392(6) . ? C9 C14 1.401(6) . ? C10 C11 1.409(5) . ? C10 C15 1.525(6) . ? C11 C12 1.386(9) . ? C11 H11 0.9500 . ? C12 C13 1.389(10) . ? C12 H12 0.9500 . ? C13 C14 1.395(7) . ? C13 H13 0.9500 . ? C14 C18 1.511(7) . ? C15 C17 1.521(7) . ? C15 C16 1.548(6) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.517(8) . ? C18 C20 1.546(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.559(11) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.304(7) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.518(9) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.682(7) . ? C27A C29A 1.51(2) . ? C27A C28A 1.672(16) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C29B 1.446(15) . ? C27B C28B 1.510(15) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.504(7) . ? C30 C32B 1.507(14) . ? C30 C32A 1.652(12) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? N1S C1S 1.373(10) 15_565 ? N1S C1S 1.373(10) 16_655 ? N1S C1S 1.373(10) . ? N1S C1S 1.373(10) 2_665 ? C1S C2S 1.372(11) . ? C1S C1S 1.550(13) 15_565 ? C1S C1S 1.550(13) 16_655 ? C1S N2S 1.816(13) 15_565 ? C1S C2S 1.816(13) 15_565 ? C1S N2S 1.850(13) 16_655 ? C1S C2S 1.850(13) 16_655 ? C2S N2S 0.954(11) 16_655 ? C2S C2S 0.954(11) 16_655 ? C2S N2S 0.954(11) 15_565 ? C2S C2S 0.954(11) 15_565 ? C2S N2S 1.349(16) 2_665 ? C2S C2S 1.349(16) 2_665 ? C2S C1S 1.816(13) 16_655 ? C2S C1S 1.850(13) 15_565 ? N3S C3S 1.360(9) . ? N3S C3S 1.360(9) 16_655 ? N3S C3S 1.360(9) 2_665 ? N3S C3S 1.360(9) 15_565 ? C3S C4S 1.372(10) . ? C3S C3S 1.543(11) 16_655 ? C3S C3S 1.543(11) 15_565 ? C3S N4S 1.845(11) 15_565 ? C3S C4S 1.845(11) 15_565 ? C3S N4S 1.870(11) 16_655 ? C3S C4S 1.870(11) 16_655 ? C4S N4S 1.017(10) 16_655 ? C4S C4S 1.017(10) 16_655 ? C4S N4S 1.017(10) 15_565 ? C4S C4S 1.017(10) 15_565 ? C4S C4S 1.438(15) 2_665 ? C4S N4S 1.438(15) 2_665 ? C4S C3S 1.845(11) 16_655 ? C4S C3S 1.870(11) 15_565 ? O1S C5T 1.444(13) . ? O2S C6S 1.435(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 N1 Co1 N1 179.40(16) 2_665 . ? N1 Co1 N1 89.998(1) 2_665 16_655 ? N1 Co1 N1 89.998(1) . 16_655 ? N1 Co1 N1 89.998(1) 2_665 15_565 ? N1 Co1 N1 89.998(1) . 15_565 ? N1 Co1 N1 179.40(16) 16_655 15_565 ? N1 Co1 N1S 90.30(8) 2_665 . ? N1 Co1 N1S 90.30(8) . . ? N1 Co1 N1S 90.30(8) 16_655 . ? N1 Co1 N1S 90.30(8) 15_565 . ? N1 Co1 N3S 89.70(8) 2_665 . ? N1 Co1 N3S 89.70(8) . . ? N1 Co1 N3S 89.70(8) 16_655 . ? N1 Co1 N3S 89.70(8) 15_565 . ? N1S Co1 N3S 180.000(1) . . ? C3 O1 C9 118.1(2) . . ? C21B O2 C4 116.7(4) . . ? C21B O2 C21A 6.7(4) . . ? C4 O2 C21A 116.3(3) . . ? C7 N1 C8 108.4(2) . 16_655 ? C7 N1 Co1 125.18(19) . . ? C8 N1 Co1 126.02(19) 16_655 . ? C7 N2 C8 121.7(3) . . ? C6 C1 C2 120.8(3) . . ? C6 C1 C8 106.1(2) . 16_655 ? C2 C1 C8 132.9(3) . 16_655 ? C3 C2 C1 116.9(3) . . ? C3 C2 H2 121.5 . . ? C1 C2 H2 121.5 . . ? C2 C3 O1 124.9(3) . . ? C2 C3 C4 122.1(3) . . ? O1 C3 C4 113.0(2) . . ? O2 C4 C5 123.7(3) . . ? O2 C4 C3 115.4(3) . . ? C5 C4 C3 120.8(3) . . ? C4 C5 C6 117.2(3) . . ? C4 C5 H5 121.4 . . ? C6 C5 H5 121.4 . . ? C1 C6 C5 122.1(3) . . ? C1 C6 C7 106.9(2) . . ? C5 C6 C7 130.8(3) . . ? N2 C7 N1 129.1(3) . . ? N2 C7 C6 121.6(3) . . ? N1 C7 C6 109.0(2) . . ? N2 C8 N1 127.8(3) . 15_565 ? N2 C8 C1 122.5(2) . 15_565 ? N1 C8 C1 109.5(2) 15_565 15_565 ? C10 C9 C14 125.5(3) . . ? C10 C9 O1 117.5(3) . . ? C14 C9 O1 116.7(3) . . ? C9 C10 C11 117.2(4) . . ? C9 C10 C15 121.2(3) . . ? C11 C10 C15 121.6(4) . . ? C12 C11 C10 119.1(5) . . ? C12 C11 H11 120.5 . . ? C10 C11 H11 120.5 . . ? C11 C12 C13 121.6(4) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C14 121.8(5) . . ? C12 C13 H13 119.1 . . ? C14 C13 H13 119.1 . . ? C13 C14 C9 114.9(5) . . ? C13 C14 C18 124.6(5) . . ? C9 C14 C18 120.5(4) . . ? C17 C15 C10 117.0(5) . . ? C17 C15 C16 108.0(4) . . ? C10 C15 C16 109.9(3) . . ? C17 C15 H15 107.1 . . ? C10 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C14 C18 C19 114.4(5) . . ? C14 C18 C20 108.4(4) . . ? C19 C18 C20 111.2(5) . . ? C14 C18 H18 107.5 . . ? C19 C18 H18 107.5 . . ? C20 C18 H18 107.5 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22A C21A C26A 120.0 . . ? C22A C21A O2 122.9(4) . . ? C26A C21A O2 117.1(4) . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 122.0(5) . . ? C23A C22A C27A 117.9(5) . . ? C24A C23A C22A 120.0 . . ? C24A C23A H23A 120.0 . . ? C22A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C24A C25A C26A 120.0 . . ? C24A C25A H25A 120.0 . . ? C26A C25A H25A 120.0 . . ? C30 C26A C25A 110.8(5) . . ? C30 C26A C21A 129.0(5) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 116.7(3) . . ? O2 C21B C26B 123.2(3) . . ? C22B C21B C26B 120.0 . . ? C23B C22B C21B 120.0 . . ? C23B C22B C27B 122.2(4) . . ? C21B C22B C27B 117.8(4) . . ? C22B C23B C24B 120.0 . . ? C22B C23B H23B 120.0 . . ? C24B C23B H23B 120.0 . . ? C25B C24B C23B 120.0 . . ? C25B C24B H24B 120.0 . . ? C23B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 125.2(4) . . ? C21B C26B C30 114.7(4) . . ? C29A C27A C22A 121.5(11) . . ? C29A C27A C28A 106.0(10) . . ? C22A C27A C28A 113.5(8) . . ? C29A C27A H27A 104.7 . . ? C22A C27A H27A 104.7 . . ? C28A C27A H27A 104.7 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C29B C27B C28B 114.3(9) . . ? C29B C27B C22B 113.5(8) . . ? C28B C27B C22B 106.9(7) . . ? C29B C27B H27B 107.3 . . ? C28B C27B H27B 107.3 . . ? C22B C27B H27B 107.3 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 112.7(5) . . ? C26A C30 C32B 127.8(7) . . ? C31 C30 C32B 117.1(7) . . ? C26A C30 C32A 109.5(7) . . ? C31 C30 C32A 103.5(5) . . ? C32B C30 C32A 44.7(6) . . ? C26A C30 C26B 4.9(4) . . ? C31 C30 C26B 117.0(5) . . ? C32B C30 C26B 123.0(7) . . ? C32A C30 C26B 105.7(6) . . ? C26A C30 H30 110.3 . . ? C31 C30 H30 110.3 . . ? C32B C30 H30 65.7 . . ? C32A C30 H30 110.3 . . ? C26B C30 H30 109.7 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C1S N1S C1S 105.9(9) 15_565 16_655 ? C1S N1S C1S 68.7(5) 15_565 . ? C1S N1S C1S 68.7(5) 16_655 . ? C1S N1S C1S 68.7(5) 15_565 2_665 ? C1S N1S C1S 68.7(5) 16_655 2_665 ? C1S N1S C1S 105.9(9) . 2_665 ? C1S N1S Co1 127.1(4) 15_565 . ? C1S N1S Co1 127.1(4) 16_655 . ? C1S N1S Co1 127.1(4) . . ? C1S N1S Co1 127.1(4) 2_665 . ? C2S C1S N1S 109.2(7) . . ? C2S C1S C1S 78.3(6) . 15_565 ? N1S C1S C1S 55.7(2) . 15_565 ? C2S C1S C1S 76.6(6) . 16_655 ? N1S C1S C1S 55.7(2) . 16_655 ? C1S C1S C1S 90.000(2) 15_565 16_655 ? C2S C1S N2S 31.0(5) . 15_565 ? N1S C1S N2S 88.0(6) . 15_565 ? C1S C1S N2S 47.3(4) 15_565 15_565 ? C1S C1S N2S 81.2(4) 16_655 15_565 ? C2S C1S C2S 31.0(5) . 15_565 ? N1S C1S C2S 88.0(6) . 15_565 ? C1S C1S C2S 47.3(4) 15_565 15_565 ? C1S C1S C2S 81.2(4) 16_655 15_565 ? N2S C1S C2S 0.0(8) 15_565 15_565 ? C2S C1S N2S 30.0(5) . 16_655 ? N1S C1S N2S 86.6(6) . 16_655 ? C1S C1S N2S 80.1(4) 15_565 16_655 ? C1S C1S N2S 46.6(3) 16_655 16_655 ? N2S C1S N2S 43.2(5) 15_565 16_655 ? C2S C1S N2S 43.2(5) 15_565 16_655 ? C2S C1S C2S 30.0(5) . 16_655 ? N1S C1S C2S 86.6(6) . 16_655 ? C1S C1S C2S 80.1(4) 15_565 16_655 ? C1S C1S C2S 46.6(3) 16_655 16_655 ? N2S C1S C2S 43.2(5) 15_565 16_655 ? C2S C1S C2S 43.2(5) 15_565 16_655 ? N2S C1S C2S 0.0(9) 16_655 16_655 ? N2S C2S C2S 0.0(18) 16_655 16_655 ? N2S C2S N2S 90.000(9) 16_655 15_565 ? C2S C2S N2S 90.000(9) 16_655 15_565 ? N2S C2S C2S 90.000(9) 16_655 15_565 ? C2S C2S C2S 90.000(9) 16_655 15_565 ? N2S C2S C2S 0.0(15) 15_565 15_565 ? N2S C2S N2S 45.000(4) 16_655 2_665 ? C2S C2S N2S 45.000(4) 16_655 2_665 ? N2S C2S N2S 45.000(8) 15_565 2_665 ? C2S C2S N2S 45.000(8) 15_565 2_665 ? N2S C2S C2S 45.000(4) 16_655 2_665 ? C2S C2S C2S 45.000(4) 16_655 2_665 ? N2S C2S C2S 45.000(8) 15_565 2_665 ? C2S C2S C2S 45.000(8) 15_565 2_665 ? N2S C2S C2S 0.0(13) 2_665 2_665 ? N2S C2S C1S 103.9(8) 16_655 . ? C2S C2S C1S 103.9(8) 16_655 . ? N2S C2S C1S 101.1(8) 15_565 . ? C2S C2S C1S 101.1(8) 15_565 . ? N2S C2S C1S 107.8(5) 2_665 . ? C2S C2S C1S 107.8(5) 2_665 . ? N2S C2S C1S 47.9(6) 16_655 16_655 ? C2S C2S C1S 47.9(6) 16_655 16_655 ? N2S C2S C1S 100.5(6) 15_565 16_655 ? C2S C2S C1S 100.5(6) 15_565 16_655 ? N2S C2S C1S 69.8(7) 2_665 16_655 ? C2S C2S C1S 69.8(7) 2_665 16_655 ? C1S C2S C1S 56.1(6) . 16_655 ? N2S C2S C1S 98.2(6) 16_655 15_565 ? C2S C2S C1S 98.2(6) 16_655 15_565 ? N2S C2S C1S 46.0(5) 15_565 15_565 ? C2S C2S C1S 46.0(5) 15_565 15_565 ? N2S C2S C1S 67.1(7) 2_665 15_565 ? C2S C2S C1S 67.1(7) 2_665 15_565 ? C1S C2S C1S 55.1(6) . 15_565 ? C1S C2S C1S 73.4(6) 16_655 15_565 ? C3S N3S C3S 69.1(4) . 16_655 ? C3S N3S C3S 106.7(8) . 2_665 ? C3S N3S C3S 69.1(4) 16_655 2_665 ? C3S N3S C3S 69.1(4) . 15_565 ? C3S N3S C3S 106.7(8) 16_655 15_565 ? C3S N3S C3S 69.1(4) 2_665 15_565 ? C3S N3S Co1 126.6(4) . . ? C3S N3S Co1 126.6(4) 16_655 . ? C3S N3S Co1 126.6(4) 2_665 . ? C3S N3S Co1 126.6(4) 15_565 . ? N3S C3S C4S 110.9(7) . . ? N3S C3S C3S 55.4(2) . 16_655 ? C4S C3S C3S 78.3(5) . 16_655 ? N3S C3S C3S 55.4(2) . 15_565 ? C4S C3S C3S 79.6(5) . 15_565 ? C3S C3S C3S 90.000(2) 16_655 15_565 ? N3S C3S N4S 87.8(5) . 15_565 ? C4S C3S N4S 32.9(4) . 15_565 ? C3S C3S N4S 82.3(3) 16_655 15_565 ? C3S C3S N4S 46.7(3) 15_565 15_565 ? N3S C3S C4S 87.8(5) . 15_565 ? C4S C3S C4S 32.9(4) . 15_565 ? C3S C3S C4S 82.3(3) 16_655 15_565 ? C3S C3S C4S 46.7(3) 15_565 15_565 ? N4S C3S C4S 0.0(7) 15_565 15_565 ? N3S C3S N4S 86.8(5) . 16_655 ? C4S C3S N4S 32.1(4) . 16_655 ? C3S C3S N4S 46.2(3) 16_655 16_655 ? C3S C3S N4S 81.4(3) 15_565 16_655 ? N4S C3S N4S 45.5(5) 15_565 16_655 ? C4S C3S N4S 45.5(5) 15_565 16_655 ? N3S C3S C4S 86.8(5) . 16_655 ? C4S C3S C4S 32.1(4) . 16_655 ? C3S C3S C4S 46.2(3) 16_655 16_655 ? C3S C3S C4S 81.4(3) 15_565 16_655 ? N4S C3S C4S 45.5(5) 15_565 16_655 ? C4S C3S C4S 45.5(5) 15_565 16_655 ? N4S C3S C4S 0.0(8) 16_655 16_655 ? N4S C4S C4S 0.0(13) 16_655 16_655 ? N4S C4S N4S 90.000(6) 16_655 15_565 ? C4S C4S N4S 90.000(6) 16_655 15_565 ? N4S C4S C4S 90.000(6) 16_655 15_565 ? C4S C4S C4S 90.000(6) 16_655 15_565 ? N4S C4S C4S 0.0(12) 15_565 15_565 ? N4S C4S C3S 102.1(6) 16_655 . ? C4S C4S C3S 102.1(6) 16_655 . ? N4S C4S C3S 100.1(6) 15_565 . ? C4S C4S C3S 100.1(6) 15_565 . ? N4S C4S C4S 45.000(3) 16_655 2_665 ? C4S C4S C4S 45.000(3) 16_655 2_665 ? N4S C4S C4S 45.000(6) 15_565 2_665 ? C4S C4S C4S 45.000(6) 15_565 2_665 ? C3S C4S C4S 105.7(4) . 2_665 ? N4S C4S N4S 45.000(3) 16_655 2_665 ? C4S C4S N4S 45.000(3) 16_655 2_665 ? N4S C4S N4S 45.000(6) 15_565 2_665 ? C4S C4S N4S 45.000(6) 15_565 2_665 ? C3S C4S N4S 105.7(4) . 2_665 ? C4S C4S N4S 0.0(9) 2_665 2_665 ? N4S C4S C3S 47.1(4) 16_655 16_655 ? C4S C4S C3S 47.1(4) 16_655 16_655 ? N4S C4S C3S 98.9(5) 15_565 16_655 ? C4S C4S C3S 98.9(5) 15_565 16_655 ? C3S C4S C3S 55.0(5) . 16_655 ? C4S C4S C3S 68.2(5) 2_665 16_655 ? N4S C4S C3S 68.2(5) 2_665 16_655 ? N4S C4S C3S 97.4(5) 16_655 15_565 ? C4S C4S C3S 97.4(5) 16_655 15_565 ? N4S C4S C3S 45.8(4) 15_565 15_565 ? C4S C4S C3S 45.8(4) 15_565 15_565 ? C3S C4S C3S 54.3(5) . 15_565 ? C4S C4S C3S 66.3(5) 2_665 15_565 ? N4S C4S C3S 66.3(5) 2_665 15_565 ? C3S C4S C3S 72.0(5) 16_655 15_565 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C7 86.3(3) 2_665 . . . ? N1 Co1 N1 C7 176.01(19) 16_655 . . . ? N1 Co1 N1 C7 -3.4(3) 15_565 . . . ? N1S Co1 N1 C7 -93.7(2) . . . . ? N3S Co1 N1 C7 86.3(2) . . . . ? N1 Co1 N1 C8 -85.6(3) 2_665 . . 16_655 ? N1 Co1 N1 C8 4.1(3) 16_655 . . 16_655 ? N1 Co1 N1 C8 -175.27(19) 15_565 . . 16_655 ? N1S Co1 N1 C8 94.4(2) . . . 16_655 ? N3S Co1 N1 C8 -85.6(2) . . . 16_655 ? C6 C1 C2 C3 -0.8(5) . . . . ? C8 C1 C2 C3 173.5(3) 16_655 . . . ? C1 C2 C3 O1 -178.1(3) . . . . ? C1 C2 C3 C4 0.3(5) . . . . ? C9 O1 C3 C2 1.9(5) . . . . ? C9 O1 C3 C4 -176.6(3) . . . . ? C21B O2 C4 C5 12.3(6) . . . . ? C21A O2 C4 C5 4.8(6) . . . . ? C21B O2 C4 C3 -169.9(4) . . . . ? C21A O2 C4 C3 -177.4(4) . . . . ? C2 C3 C4 O2 -176.5(3) . . . . ? O1 C3 C4 O2 2.0(5) . . . . ? C2 C3 C4 C5 1.3(6) . . . . ? O1 C3 C4 C5 179.9(3) . . . . ? O2 C4 C5 C6 175.3(4) . . . . ? C3 C4 C5 C6 -2.4(6) . . . . ? C2 C1 C6 C5 -0.4(5) . . . . ? C8 C1 C6 C5 -176.0(3) 16_655 . . . ? C2 C1 C6 C7 175.3(3) . . . . ? C8 C1 C6 C7 -0.3(4) 16_655 . . . ? C4 C5 C6 C1 2.0(6) . . . . ? C4 C5 C6 C7 -172.5(4) . . . . ? C8 N2 C7 N1 0.0(5) . . . . ? C8 N2 C7 C6 174.2(3) . . . . ? C8 N1 C7 N2 175.2(3) 16_655 . . . ? Co1 N1 C7 N2 2.1(5) . . . . ? C8 N1 C7 C6 0.4(3) 16_655 . . . ? Co1 N1 C7 C6 -172.7(2) . . . . ? C1 C6 C7 N2 -175.3(3) . . . . ? C5 C6 C7 N2 -0.1(6) . . . . ? C1 C6 C7 N1 0.0(4) . . . . ? C5 C6 C7 N1 175.1(4) . . . . ? C7 N2 C8 N1 0.9(5) . . . 15_565 ? C7 N2 C8 C1 -174.8(3) . . . 15_565 ? C3 O1 C9 C10 86.5(4) . . . . ? C3 O1 C9 C14 -99.2(3) . . . . ? C14 C9 C10 C11 0.6(5) . . . . ? O1 C9 C10 C11 174.3(3) . . . . ? C14 C9 C10 C15 -176.5(3) . . . . ? O1 C9 C10 C15 -2.8(4) . . . . ? C9 C10 C11 C12 -0.6(5) . . . . ? C15 C10 C11 C12 176.5(4) . . . . ? C10 C11 C12 C13 1.1(7) . . . . ? C11 C12 C13 C14 -1.6(7) . . . . ? C12 C13 C14 C9 1.6(6) . . . . ? C12 C13 C14 C18 -177.0(4) . . . . ? C10 C9 C14 C13 -1.1(5) . . . . ? O1 C9 C14 C13 -174.9(3) . . . . ? C10 C9 C14 C18 177.5(3) . . . . ? O1 C9 C14 C18 3.8(5) . . . . ? C9 C10 C15 C17 -163.5(4) . . . . ? C11 C10 C15 C17 19.5(5) . . . . ? C9 C10 C15 C16 72.8(4) . . . . ? C11 C10 C15 C16 -104.2(4) . . . . ? C13 C14 C18 C19 -26.8(7) . . . . ? C9 C14 C18 C19 154.7(5) . . . . ? C13 C14 C18 C20 97.9(5) . . . . ? C9 C14 C18 C20 -80.6(5) . . . . ? C21B O2 C21A C22A 1(4) . . . . ? C4 O2 C21A C22A 95.9(4) . . . . ? C21B O2 C21A C26A 180(100) . . . . ? C4 O2 C21A C26A -85.3(5) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C23A 178.8(6) . . . . ? C26A C21A C22A C27A 176.6(7) . . . . ? O2 C21A C22A C27A -4.6(6) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -176.7(7) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 175.9(5) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? C22A C21A C26A C30 -175.1(6) . . . . ? O2 C21A C26A C30 6.1(6) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? O2 C21A C26A C25A -178.9(5) . . . . ? C4 O2 C21B C22B 94.3(4) . . . . ? C21A O2 C21B C22B -177(100) . . . . ? C4 O2 C21B C26B -83.4(5) . . . . ? C21A O2 C21B C26B 5(4) . . . . ? O2 C21B C22B C23B -177.8(6) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 1.3(5) . . . . ? C26B C21B C22B C27B 179.0(5) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B -179.0(6) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -177.2(5) . . . . ? O2 C21B C26B C25B 177.6(6) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -4.9(5) . . . . ? C22B C21B C26B C30 177.5(5) . . . . ? C21A C22A C27A C29A -155.4(10) . . . . ? C23A C22A C27A C29A 21.2(13) . . . . ? C21A C22A C27A C28A 76.3(9) . . . . ? C23A C22A C27A C28A -107.0(9) . . . . ? C23B C22B C27B C29B 71.4(9) . . . . ? C21B C22B C27B C29B -107.6(8) . . . . ? C23B C22B C27B C28B -55.5(9) . . . . ? C21B C22B C27B C28B 125.5(7) . . . . ? C25A C26A C30 C31 80.6(6) . . . . ? C21A C26A C30 C31 -104.0(6) . . . . ? C25A C26A C30 C32B -81.1(10) . . . . ? C21A C26A C30 C32B 94.3(10) . . . . ? C25A C26A C30 C32A -34.0(6) . . . . ? C21A C26A C30 C32A 141.5(6) . . . . ? C25A C26A C30 C26B -73(4) . . . . ? C21A C26A C30 C26B 103(4) . . . . ? C25B C26B C30 C26A 109(4) . . . . ? C21B C26B C30 C26A -69(4) . . . . ? C25B C26B C30 C31 80.9(7) . . . . ? C21B C26B C30 C31 -96.4(6) . . . . ? C25B C26B C30 C32B -79.3(9) . . . . ? C21B C26B C30 C32B 103.4(8) . . . . ? C25B C26B C30 C32A -33.6(7) . . . . ? C21B C26B C30 C32A 149.1(5) . . . . ? N1 Co1 N1S C1S 43.2(5) 2_665 . . 15_565 ? N1 Co1 N1S C1S -136.8(5) . . . 15_565 ? N1 Co1 N1S C1S -46.8(5) 16_655 . . 15_565 ? N1 Co1 N1S C1S 133.2(5) 15_565 . . 15_565 ? N3S Co1 N1S C1S 0(100) . . . 15_565 ? N1 Co1 N1S C1S -136.8(5) 2_665 . . 16_655 ? N1 Co1 N1S C1S 43.2(5) . . . 16_655 ? N1 Co1 N1S C1S 133.2(5) 16_655 . . 16_655 ? N1 Co1 N1S C1S -46.8(5) 15_565 . . 16_655 ? N3S Co1 N1S C1S 0(49) . . . 16_655 ? N1 Co1 N1S C1S -46.8(5) 2_665 . . . ? N1 Co1 N1S C1S 133.2(5) . . . . ? N1 Co1 N1S C1S -136.8(5) 16_655 . . . ? N1 Co1 N1S C1S 43.2(5) 15_565 . . . ? N3S Co1 N1S C1S 0(100) . . . . ? N1 Co1 N1S C1S 133.2(5) 2_665 . . 2_665 ? N1 Co1 N1S C1S -46.8(5) . . . 2_665 ? N1 Co1 N1S C1S 43.2(5) 16_655 . . 2_665 ? N1 Co1 N1S C1S -136.8(5) 15_565 . . 2_665 ? N3S Co1 N1S C1S 0(100) . . . 2_665 ? C1S N1S C1S C2S 60.2(7) 15_565 . . . ? C1S N1S C1S C2S -57.7(7) 16_655 . . . ? C1S N1S C1S C2S 1.3(6) 2_665 . . . ? Co1 N1S C1S C2S -178.7(6) . . . . ? C1S N1S C1S C1S -117.8(5) 16_655 . . 15_565 ? C1S N1S C1S C1S -58.9(3) 2_665 . . 15_565 ? Co1 N1S C1S C1S 121.1(3) . . . 15_565 ? C1S N1S C1S C1S 117.8(5) 15_565 . . 16_655 ? C1S N1S C1S C1S 58.9(3) 2_665 . . 16_655 ? Co1 N1S C1S C1S -121.1(3) . . . 16_655 ? C1S N1S C1S N2S 37.1(4) 15_565 . . 15_565 ? C1S N1S C1S N2S -80.7(3) 16_655 . . 15_565 ? C1S N1S C1S N2S -21.8(3) 2_665 . . 15_565 ? Co1 N1S C1S N2S 158.2(3) . . . 15_565 ? C1S N1S C1S C2S 37.1(4) 15_565 . . 15_565 ? C1S N1S C1S C2S -80.7(3) 16_655 . . 15_565 ? C1S N1S C1S C2S -21.8(3) 2_665 . . 15_565 ? Co1 N1S C1S C2S 158.2(3) . . . 15_565 ? C1S N1S C1S N2S 80.3(3) 15_565 . . 16_655 ? C1S N1S C1S N2S -37.5(4) 16_655 . . 16_655 ? C1S N1S C1S N2S 21.4(3) 2_665 . . 16_655 ? Co1 N1S C1S N2S -158.6(3) . . . 16_655 ? C1S N1S C1S C2S 80.3(3) 15_565 . . 16_655 ? C1S N1S C1S C2S -37.5(4) 16_655 . . 16_655 ? C1S N1S C1S C2S 21.4(3) 2_665 . . 16_655 ? Co1 N1S C1S C2S -158.6(3) . . . 16_655 ? N1S C1S C2S N2S 43.4(16) . . . 16_655 ? C1S C1S C2S N2S 90.4(13) 15_565 . . 16_655 ? C1S C1S C2S N2S -2.5(13) 16_655 . . 16_655 ? N2S C1S C2S N2S 92.79(17) 15_565 . . 16_655 ? C2S C1S C2S N2S 92.79(17) 15_565 . . 16_655 ? C2S C1S C2S N2S 0.000(3) 16_655 . . 16_655 ? N1S C1S C2S C2S 43.4(16) . . . 16_655 ? C1S C1S C2S C2S 90.4(13) 15_565 . . 16_655 ? C1S C1S C2S C2S -2.5(13) 16_655 . . 16_655 ? N2S C1S C2S C2S 92.79(17) 15_565 . . 16_655 ? C2S C1S C2S C2S 92.79(17) 15_565 . . 16_655 ? N2S C1S C2S C2S 0.000(3) 16_655 . . 16_655 ? N1S C1S C2S N2S -49.4(15) . . . 15_565 ? C1S C1S C2S N2S -2.4(12) 15_565 . . 15_565 ? C1S C1S C2S N2S -95.2(12) 16_655 . . 15_565 ? C2S C1S C2S N2S 0.000(3) 15_565 . . 15_565 ? N2S C1S C2S N2S -92.79(17) 16_655 . . 15_565 ? C2S C1S C2S N2S -92.79(17) 16_655 . . 15_565 ? N1S C1S C2S C2S -49.4(15) . . . 15_565 ? C1S C1S C2S C2S -2.4(12) 15_565 . . 15_565 ? C1S C1S C2S C2S -95.2(12) 16_655 . . 15_565 ? N2S C1S C2S C2S 0.000(3) 15_565 . . 15_565 ? N2S C1S C2S C2S -92.79(17) 16_655 . . 15_565 ? C2S C1S C2S C2S -92.79(17) 16_655 . . 15_565 ? N1S C1S C2S N2S -3.4(17) . . . 2_665 ? C1S C1S C2S N2S 43.7(14) 15_565 . . 2_665 ? C1S C1S C2S N2S -49.2(14) 16_655 . . 2_665 ? N2S C1S C2S N2S 46.1(2) 15_565 . . 2_665 ? C2S C1S C2S N2S 46.1(2) 15_565 . . 2_665 ? N2S C1S C2S N2S -46.72(17) 16_655 . . 2_665 ? C2S C1S C2S N2S -46.72(17) 16_655 . . 2_665 ? N1S C1S C2S C2S -3.4(17) . . . 2_665 ? C1S C1S C2S C2S 43.7(14) 15_565 . . 2_665 ? C1S C1S C2S C2S -49.2(14) 16_655 . . 2_665 ? N2S C1S C2S C2S 46.1(2) 15_565 . . 2_665 ? C2S C1S C2S C2S 46.1(2) 15_565 . . 2_665 ? N2S C1S C2S C2S -46.72(17) 16_655 . . 2_665 ? C2S C1S C2S C2S -46.72(17) 16_655 . . 2_665 ? N1S C1S C2S C1S 45.8(3) . . . 16_655 ? C1S C1S C2S C1S 92.83(16) 15_565 . . 16_655 ? N2S C1S C2S C1S 95.2(12) 15_565 . . 16_655 ? C2S C1S C2S C1S 95.2(12) 15_565 . . 16_655 ? N2S C1S C2S C1S 2.5(13) 16_655 . . 16_655 ? C2S C1S C2S C1S 2.5(13) 16_655 . . 16_655 ? N1S C1S C2S C1S -47.0(3) . . . 15_565 ? C1S C1S C2S C1S -92.83(16) 16_655 . . 15_565 ? N2S C1S C2S C1S 2.4(12) 15_565 . . 15_565 ? C2S C1S C2S C1S 2.4(12) 15_565 . . 15_565 ? N2S C1S C2S C1S -90.4(13) 16_655 . . 15_565 ? C2S C1S C2S C1S -90.4(13) 16_655 . . 15_565 ? N1 Co1 N3S C3S 32.6(5) 2_665 . . . ? N1 Co1 N3S C3S -147.4(5) . . . . ? N1 Co1 N3S C3S 122.6(5) 16_655 . . . ? N1 Co1 N3S C3S -57.4(5) 15_565 . . . ? N1S Co1 N3S C3S 0(100) . . . . ? N1 Co1 N3S C3S 122.6(5) 2_665 . . 16_655 ? N1 Co1 N3S C3S -57.4(5) . . . 16_655 ? N1 Co1 N3S C3S -147.4(5) 16_655 . . 16_655 ? N1 Co1 N3S C3S 32.6(5) 15_565 . . 16_655 ? N1S Co1 N3S C3S 0(52) . . . 16_655 ? N1 Co1 N3S C3S -147.4(5) 2_665 . . 2_665 ? N1 Co1 N3S C3S 32.6(5) . . . 2_665 ? N1 Co1 N3S C3S -57.4(5) 16_655 . . 2_665 ? N1 Co1 N3S C3S 122.6(5) 15_565 . . 2_665 ? N1S Co1 N3S C3S 0(100) . . . 2_665 ? N1 Co1 N3S C3S -57.4(5) 2_665 . . 15_565 ? N1 Co1 N3S C3S 122.6(5) . . . 15_565 ? N1 Co1 N3S C3S 32.6(5) 16_655 . . 15_565 ? N1 Co1 N3S C3S -147.4(5) 15_565 . . 15_565 ? N1S Co1 N3S C3S 0(100) . . . 15_565 ? C3S N3S C3S C4S 58.2(6) 16_655 . . . ? C3S N3S C3S C4S -1.0(5) 2_665 . . . ? C3S N3S C3S C4S -60.2(6) 15_565 . . . ? Co1 N3S C3S C4S 179.0(5) . . . . ? C3S N3S C3S C3S -59.2(2) 2_665 . . 16_655 ? C3S N3S C3S C3S -118.4(5) 15_565 . . 16_655 ? Co1 N3S C3S C3S 120.8(2) . . . 16_655 ? C3S N3S C3S C3S 118.4(5) 16_655 . . 15_565 ? C3S N3S C3S C3S 59.2(2) 2_665 . . 15_565 ? Co1 N3S C3S C3S -120.8(2) . . . 15_565 ? C3S N3S C3S N4S 82.1(3) 16_655 . . 15_565 ? C3S N3S C3S N4S 22.9(2) 2_665 . . 15_565 ? C3S N3S C3S N4S -36.2(4) 15_565 . . 15_565 ? Co1 N3S C3S N4S -157.1(2) . . . 15_565 ? C3S N3S C3S C4S 82.1(3) 16_655 . . 15_565 ? C3S N3S C3S C4S 22.9(2) 2_665 . . 15_565 ? C3S N3S C3S C4S -36.2(4) 15_565 . . 15_565 ? Co1 N3S C3S C4S -157.1(2) . . . 15_565 ? C3S N3S C3S N4S 36.5(4) 16_655 . . 16_655 ? C3S N3S C3S N4S -22.6(2) 2_665 . . 16_655 ? C3S N3S C3S N4S -81.8(3) 15_565 . . 16_655 ? Co1 N3S C3S N4S 157.4(2) . . . 16_655 ? C3S N3S C3S C4S 36.5(4) 16_655 . . 16_655 ? C3S N3S C3S C4S -22.6(2) 2_665 . . 16_655 ? C3S N3S C3S C4S -81.8(3) 15_565 . . 16_655 ? Co1 N3S C3S C4S 157.4(2) . . . 16_655 ? N3S C3S C4S N4S -43.9(12) . . . 16_655 ? C3S C3S C4S N4S 1.7(9) 16_655 . . 16_655 ? C3S C3S C4S N4S -90.4(9) 15_565 . . 16_655 ? N4S C3S C4S N4S -92.17(13) 15_565 . . 16_655 ? C4S C3S C4S N4S -92.17(13) 15_565 . . 16_655 ? C4S C3S C4S N4S 0.000(4) 16_655 . . 16_655 ? N3S C3S C4S C4S -43.9(12) . . . 16_655 ? C3S C3S C4S C4S 1.7(9) 16_655 . . 16_655 ? C3S C3S C4S C4S -90.4(9) 15_565 . . 16_655 ? N4S C3S C4S C4S -92.17(13) 15_565 . . 16_655 ? C4S C3S C4S C4S -92.17(13) 15_565 . . 16_655 ? N4S C3S C4S C4S 0.000(4) 16_655 . . 16_655 ? N3S C3S C4S N4S 48.3(11) . . . 15_565 ? C3S C3S C4S N4S 93.9(9) 16_655 . . 15_565 ? C3S C3S C4S N4S 1.7(9) 15_565 . . 15_565 ? C4S C3S C4S N4S 0.0 15_565 . . 15_565 ? N4S C3S C4S N4S 92.17(13) 16_655 . . 15_565 ? C4S C3S C4S N4S 92.17(13) 16_655 . . 15_565 ? N3S C3S C4S C4S 48.3(11) . . . 15_565 ? C3S C3S C4S C4S 93.9(9) 16_655 . . 15_565 ? C3S C3S C4S C4S 1.7(9) 15_565 . . 15_565 ? N4S C3S C4S C4S 0.0 15_565 . . 15_565 ? N4S C3S C4S C4S 92.17(13) 16_655 . . 15_565 ? C4S C3S C4S C4S 92.17(13) 16_655 . . 15_565 ? N3S C3S C4S C4S 2.4(13) . . . 2_665 ? C3S C3S C4S C4S 48.0(10) 16_655 . . 2_665 ? C3S C3S C4S C4S -44.2(10) 15_565 . . 2_665 ? N4S C3S C4S C4S -45.88(13) 15_565 . . 2_665 ? C4S C3S C4S C4S -45.88(13) 15_565 . . 2_665 ? N4S C3S C4S C4S 46.29(12) 16_655 . . 2_665 ? C4S C3S C4S C4S 46.29(12) 16_655 . . 2_665 ? N3S C3S C4S N4S 2.4(13) . . . 2_665 ? C3S C3S C4S N4S 48.0(10) 16_655 . . 2_665 ? C3S C3S C4S N4S -44.2(10) 15_565 . . 2_665 ? N4S C3S C4S N4S -45.88(13) 15_565 . . 2_665 ? C4S C3S C4S N4S -45.88(13) 15_565 . . 2_665 ? N4S C3S C4S N4S 46.29(12) 16_655 . . 2_665 ? C4S C3S C4S N4S 46.29(12) 16_655 . . 2_665 ? N3S C3S C4S C3S -45.6(3) . . . 16_655 ? C3S C3S C4S C3S -92.19(13) 15_565 . . 16_655 ? N4S C3S C4S C3S -93.9(9) 15_565 . . 16_655 ? C4S C3S C4S C3S -93.9(9) 15_565 . . 16_655 ? N4S C3S C4S C3S -1.7(9) 16_655 . . 16_655 ? C4S C3S C4S C3S -1.7(9) 16_655 . . 16_655 ? N3S C3S C4S C3S 46.6(3) . . . 15_565 ? C3S C3S C4S C3S 92.19(12) 16_655 . . 15_565 ? N4S C3S C4S C3S -1.7(9) 15_565 . . 15_565 ? C4S C3S C4S C3S -1.7(9) 15_565 . . 15_565 ? N4S C3S C4S C3S 90.4(9) 16_655 . . 15_565 ? C4S C3S C4S C3S 90.4(9) 16_655 . . 15_565 ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 24.20 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 1.105 _refine_diff_density_min -0.533 _refine_diff_density_rms 0.089 data_10colu _database_code_depnum_ccdc_archive 'CCDC 900378' #TrackingRef '900378_PNC[cLu0.5-Co-vLu].cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C152.50 H176.50 Co N11.50 O8.50' _chemical_formula_sum 'C152.50 H176.50 Co N11.50 O8.50' _chemical_formula_weight 2365.48 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M 'P n -3 n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, -z+1/2' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' '-y+1/2, x, z' 'y, x, -z+1/2' 'y, -x+1/2, z' '-y+1/2, -x+1/2, -z+1/2' 'y, z, x' '-y+1/2, -z+1/2, x' 'y, -z+1/2, -x+1/2' '-y+1/2, z, -x+1/2' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' 'z, -y+1/2, x' 'z, y, -x+1/2' 'z, x, y' '-z+1/2, x, -y+1/2' '-z+1/2, -x+1/2, y' 'z, -x+1/2, -y+1/2' '-x+1/2, -z+1/2, -y+1/2' '-x+1/2, z, y' 'x, -z+1/2, y' 'x, z, -y+1/2' '-x, -y, -z' '-x, y-1/2, z-1/2' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' 'y-1/2, -x, -z' '-y, -x, z-1/2' '-y, x-1/2, -z' 'y-1/2, x-1/2, z-1/2' '-y, -z, -x' 'y-1/2, z-1/2, -x' '-y, z-1/2, x-1/2' 'y-1/2, -z, x-1/2' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' '-z, y-1/2, -x' '-z, -y, x-1/2' '-z, -x, -y' 'z-1/2, -x, y-1/2' 'z-1/2, x-1/2, -y' '-z, x-1/2, y-1/2' 'x-1/2, z-1/2, y-1/2' 'x-1/2, -z, -y' '-x, z-1/2, -y' '-x, -z, y-1/2' _cell_length_a 37.3922(2) _cell_length_b 37.3922(2) _cell_length_c 37.3922(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52280.9(5) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8109 _cell_measurement_theta_min 0.75 _cell_measurement_theta_max 25.59 _exptl_crystal_description cube _exptl_crystal_colour purple _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.902 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 15204 _exptl_absorpt_coefficient_mu 0.146 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9870 _exptl_absorpt_correction_T_max 0.9870 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type Synchrotron _diffrn_radiation_source Synchrotron _diffrn_radiation_monochromator 'Double-crystal with Si 111' _diffrn_measurement_device_type 'Diamond, I19' _diffrn_measurement_method 'Rigaku Saturn 724 CCD detector' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 204441 _diffrn_reflns_av_R_equivalents 0.1189 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 46 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 0.75 _diffrn_reflns_theta_max 25.59 _reflns_number_total 8991 _reflns_number_gt 8109 _reflns_threshold_expression >2\s(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0081(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8991 _refine_ls_number_parameters 655 _refine_ls_number_restraints 1064 _refine_ls_R_factor_all 0.1611 _refine_ls_R_factor_gt 0.1508 _refine_ls_wR_factor_ref 0.4565 _refine_ls_wR_factor_gt 0.4504 _refine_ls_goodness_of_fit_ref 2.143 _refine_ls_restrained_S_all 2.088 _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 0.91482(10) 0.31474(9) 0.29519(9) 0.0326(7) Uani 1 1 d . . . C2 C 0.91026(10) 0.32583(9) 0.33228(9) 0.0336(8) Uani 1 1 d . . . C3 C 0.91082(10) 0.29471(9) 0.35216(9) 0.0341(8) Uani 1 1 d . . . C4 C 0.91494(10) 0.26514(9) 0.32725(8) 0.0313(7) Uani 1 1 d . . . C5 C 0.90298(11) 0.35900(9) 0.34821(9) 0.0354(8) Uani 1 1 d . . . H5 H 0.9024 0.3805 0.3346 0.043 Uiso 1 1 calc R . . C6 C 0.89663(10) 0.35890(9) 0.38459(9) 0.0344(8) Uani 1 1 d . A . C7 C 0.89653(11) 0.32690(9) 0.40480(9) 0.0370(8) Uani 1 1 d . A . C8 C 0.90381(9) 0.29401(6) 0.38823(7) 0.0381(8) Uani 1 1 d . . . H8 H 0.9039 0.2723 0.4014 0.046 Uiso 1 1 calc R . . C9 C 0.88434(9) 0.42012(6) 0.38734(7) 0.0431(17) Uani 0.731(9) 1 d PRDU A 1 C10 C 0.91311(9) 0.44366(6) 0.38708(7) 0.0562(18) Uani 0.731(9) 1 d PRDU A 1 C11 C 0.90930(9) 0.47751(6) 0.37222(7) 0.065(2) Uani 0.731(9) 1 d PRDU A 1 H11 H 0.9290 0.4936 0.3720 0.078 Uiso 0.731(9) 1 calc PR A 1 C12 C 0.87670(9) 0.48784(6) 0.35762(7) 0.070(2) Uani 0.731(9) 1 d PRDU A 1 H12 H 0.8741 0.5110 0.3475 0.084 Uiso 0.731(9) 1 calc PR A 1 C13 C 0.84793(9) 0.46431(6) 0.35788(7) 0.060(2) Uani 0.731(9) 1 d PRDU A 1 H13 H 0.8257 0.4714 0.3479 0.072 Uiso 0.731(9) 1 calc PR A 1 C14 C 0.85175(9) 0.43045(6) 0.37275(7) 0.0465(16) Uani 0.731(9) 1 d PRDU A 1 C15 C 0.9479(3) 0.4333(3) 0.4043(3) 0.073(2) Uani 0.731(9) 1 d PDU A 1 H15 H 0.9523 0.4074 0.3993 0.088 Uiso 0.731(9) 1 calc PR A 1 C16 C 0.9443(4) 0.4380(3) 0.4451(3) 0.084(3) Uani 0.731(9) 1 d PDU A 1 H16A H 0.9667 0.4311 0.4567 0.127 Uiso 0.731(9) 1 calc PR A 1 H16B H 0.9248 0.4228 0.4539 0.127 Uiso 0.731(9) 1 calc PR A 1 H16C H 0.9390 0.4631 0.4505 0.127 Uiso 0.731(9) 1 calc PR A 1 C17 C 0.9804(3) 0.4549(4) 0.3905(4) 0.103(4) Uani 0.731(9) 1 d PDU A 1 H17A H 1.0022 0.4466 0.4025 0.154 Uiso 0.731(9) 1 calc PR A 1 H17B H 0.9768 0.4803 0.3956 0.154 Uiso 0.731(9) 1 calc PR A 1 H17C H 0.9828 0.4514 0.3647 0.154 Uiso 0.731(9) 1 calc PR A 1 C18 C 0.8201(2) 0.4029(2) 0.37604(19) 0.0540(18) Uani 0.731(9) 1 d PDU A 1 H18 H 0.8302 0.3789 0.3703 0.065 Uiso 0.731(9) 1 calc PR A 1 C19 C 0.7874(3) 0.4080(4) 0.3513(3) 0.082(3) Uani 0.731(9) 1 d PDU A 1 H19A H 0.7698 0.3891 0.3560 0.123 Uiso 0.731(9) 1 calc PR A 1 H19B H 0.7950 0.4068 0.3263 0.123 Uiso 0.731(9) 1 calc PR A 1 H19C H 0.7764 0.4314 0.3560 0.123 Uiso 0.731(9) 1 calc PR A 1 C20 C 0.8058(3) 0.4006(3) 0.4145(2) 0.060(2) Uani 0.731(9) 1 d PDU A 1 H20A H 0.8259 0.3974 0.4310 0.090 Uiso 0.731(9) 1 calc PR A 1 H20B H 0.7894 0.3803 0.4165 0.090 Uiso 0.731(9) 1 calc PR A 1 H20C H 0.7930 0.4227 0.4204 0.090 Uiso 0.731(9) 1 calc PR A 1 C9A C 0.8907(3) 0.4245(4) 0.3884(5) 0.037(3) Uani 0.269(9) 1 d PDU A 2 C10A C 0.9225(4) 0.4426(4) 0.3937(6) 0.056(4) Uani 0.269(9) 1 d PDU A 2 C11A C 0.9234(4) 0.4786(4) 0.3844(6) 0.055(4) Uani 0.269(9) 1 d PDU A 2 H11A H 0.9439 0.4928 0.3893 0.066 Uiso 0.269(9) 1 calc PR A 2 C12A C 0.8938(4) 0.4932(4) 0.3678(5) 0.054(4) Uani 0.269(9) 1 d PDU A 2 H12A H 0.8954 0.5172 0.3596 0.065 Uiso 0.269(9) 1 calc PR A 2 C13A C 0.8621(4) 0.4752(3) 0.3625(4) 0.043(3) Uani 0.269(9) 1 d PDU A 2 H13A H 0.8424 0.4862 0.3507 0.052 Uiso 0.269(9) 1 calc PR A 2 C14A C 0.8601(3) 0.4400(4) 0.3752(6) 0.057(4) Uani 0.269(9) 1 d PDU A 2 C15A C 0.9543(4) 0.4257(6) 0.4115(6) 0.074(6) Uani 0.269(9) 1 d PDU A 2 H15A H 0.9494 0.4000 0.4167 0.088 Uiso 0.269(9) 1 calc PR A 2 C16A C 0.9614(9) 0.4461(11) 0.4467(6) 0.095(8) Uani 0.269(9) 1 d PDU A 2 H16D H 0.9817 0.4353 0.4592 0.142 Uiso 0.269(9) 1 calc PR A 2 H16E H 0.9401 0.4449 0.4619 0.142 Uiso 0.269(9) 1 calc PR A 2 H16F H 0.9668 0.4712 0.4413 0.142 Uiso 0.269(9) 1 calc PR A 2 C17A C 0.9883(5) 0.4292(9) 0.3878(7) 0.087(6) Uani 0.269(9) 1 d PDU A 2 H17D H 1.0087 0.4185 0.4002 0.131 Uiso 0.269(9) 1 calc PR A 2 H17E H 0.9931 0.4545 0.3831 0.131 Uiso 0.269(9) 1 calc PR A 2 H17F H 0.9843 0.4167 0.3651 0.131 Uiso 0.269(9) 1 calc PR A 2 C18A C 0.8258(4) 0.4160(5) 0.3731(3) 0.056(4) Uani 0.269(9) 1 d PDU A 2 H18A H 0.8344 0.3920 0.3651 0.067 Uiso 0.269(9) 1 calc PR A 2 C19A C 0.7963(4) 0.4265(6) 0.3462(4) 0.048(4) Uani 0.269(9) 1 d PDU A 2 H19D H 0.7765 0.4095 0.3479 0.072 Uiso 0.269(9) 1 calc PR A 2 H19E H 0.8061 0.4261 0.3219 0.072 Uiso 0.269(9) 1 calc PR A 2 H19F H 0.7876 0.4506 0.3518 0.072 Uiso 0.269(9) 1 calc PR A 2 C20A C 0.80738(16) 0.40956(11) 0.40923(12) 0.048(6) Uani 0.269(9) 1 d PDU A 2 H20D H 0.7861 0.3947 0.4057 0.071 Uiso 0.269(9) 1 calc PR A 2 H20E H 0.8003 0.4325 0.4197 0.071 Uiso 0.269(9) 1 calc PR A 2 H20F H 0.8240 0.3973 0.4254 0.071 Uiso 0.269(9) 1 calc PR A 2 C21 C 0.88853(16) 0.30082(11) 0.45979(12) 0.040(2) Uani 0.592(9) 1 d PRDU B 1 C22 C 0.86014(16) 0.27688(11) 0.46150(12) 0.0362(17) Uani 0.592(9) 1 d PRDU B 1 C23 C 0.86268(16) 0.24652(11) 0.48280(12) 0.057(2) Uani 0.592(9) 1 d PRDU B 1 H23 H 0.8433 0.2302 0.4840 0.069 Uiso 0.592(9) 1 calc PR B 1 C24 C 0.89362(16) 0.24010(11) 0.50238(12) 0.066(3) Uani 0.592(9) 1 d PRDU B 1 H24 H 0.8954 0.2193 0.5169 0.079 Uiso 0.592(9) 1 calc PR B 1 C25 C 0.92201(16) 0.26403(11) 0.50067(12) 0.065(3) Uani 0.592(9) 1 d PRDU B 1 H25 H 0.9432 0.2596 0.5141 0.078 Uiso 0.592(9) 1 calc PR B 1 C26 C 0.91946(16) 0.29439(11) 0.47937(12) 0.053(2) Uani 0.592(9) 1 d PRDU B 1 C27 C 0.8260(3) 0.2876(3) 0.4391(2) 0.052(2) Uani 0.592(9) 1 d PDU B 1 H27 H 0.8316 0.3106 0.4267 0.063 Uiso 0.592(9) 1 calc PR B 1 C28 C 0.8178(4) 0.2603(4) 0.4104(3) 0.088(4) Uani 0.592(9) 1 d PDU B 1 H28A H 0.8392 0.2564 0.3958 0.132 Uiso 0.592(9) 1 calc PR B 1 H28B H 0.7984 0.2693 0.3953 0.132 Uiso 0.592(9) 1 calc PR B 1 H28C H 0.8105 0.2378 0.4216 0.132 Uiso 0.592(9) 1 calc PR B 1 C29 C 0.7939(4) 0.2941(4) 0.4621(4) 0.067(3) Uani 0.592(9) 1 d PDU B 1 H29A H 0.7997 0.3121 0.4803 0.100 Uiso 0.592(9) 1 calc PR B 1 H29B H 0.7869 0.2718 0.4738 0.100 Uiso 0.592(9) 1 calc PR B 1 H29C H 0.7742 0.3028 0.4472 0.100 Uiso 0.592(9) 1 calc PR B 1 C30 C 0.9536(2) 0.3160(3) 0.4767(2) 0.057(2) Uani 0.592(9) 1 d PDU B 1 H30 H 0.9553 0.3247 0.4515 0.068 Uiso 0.592(9) 1 calc PR B 1 C31 C 0.9506(3) 0.3490(3) 0.5006(4) 0.071(3) Uani 0.592(9) 1 d PDU B 1 H31A H 0.9281 0.3615 0.4956 0.107 Uiso 0.592(9) 1 calc PR B 1 H31B H 0.9707 0.3651 0.4958 0.107 Uiso 0.592(9) 1 calc PR B 1 H31C H 0.9511 0.3417 0.5258 0.107 Uiso 0.592(9) 1 calc PR B 1 C32 C 0.9876(3) 0.2957(4) 0.4844(5) 0.092(4) Uani 0.592(9) 1 d PDU B 1 H32A H 1.0081 0.3119 0.4820 0.138 Uiso 0.592(9) 1 calc PR B 1 H32B H 0.9900 0.2760 0.4673 0.138 Uiso 0.592(9) 1 calc PR B 1 H32C H 0.9868 0.2862 0.5088 0.138 Uiso 0.592(9) 1 calc PR B 1 C21A C 0.8941(3) 0.3000(3) 0.4624(3) 0.031(2) Uani 0.408(9) 1 d PDU B 2 C22A C 0.8714(3) 0.2713(3) 0.4640(4) 0.054(3) Uani 0.408(9) 1 d PDU B 2 C23A C 0.8817(3) 0.2434(3) 0.4866(4) 0.045(2) Uani 0.408(9) 1 d PDU B 2 H23A H 0.8657 0.2243 0.4914 0.054 Uiso 0.408(9) 1 calc PR B 2 C24A C 0.9152(3) 0.2436(3) 0.5017(4) 0.058(3) Uani 0.408(9) 1 d PDU B 2 H24A H 0.9226 0.2232 0.5150 0.070 Uiso 0.408(9) 1 calc PR B 2 C25A C 0.9386(3) 0.2722(3) 0.4986(4) 0.059(3) Uani 0.408(9) 1 d PDU B 2 H25A H 0.9615 0.2718 0.5097 0.071 Uiso 0.408(9) 1 calc PR B 2 C26A C 0.9275(3) 0.3011(3) 0.4789(3) 0.052(3) Uani 0.408(9) 1 d PDU B 2 C27A C 0.8340(3) 0.2746(4) 0.4448(4) 0.050(3) Uani 0.408(9) 1 d PDU B 2 H27A H 0.8378 0.2894 0.4228 0.060 Uiso 0.408(9) 1 calc PR B 2 C28A C 0.8188(4) 0.2395(4) 0.4328(5) 0.072(4) Uani 0.408(9) 1 d PDU B 2 H28D H 0.8364 0.2269 0.4181 0.108 Uiso 0.408(9) 1 calc PR B 2 H28E H 0.7971 0.2437 0.4187 0.108 Uiso 0.408(9) 1 calc PR B 2 H28F H 0.8128 0.2249 0.4537 0.108 Uiso 0.408(9) 1 calc PR B 2 C29A C 0.8073(5) 0.2942(6) 0.4675(5) 0.064(5) Uani 0.408(9) 1 d PDU B 2 H29D H 0.8175 0.3172 0.4751 0.097 Uiso 0.408(9) 1 calc PR B 2 H29E H 0.8016 0.2798 0.4886 0.097 Uiso 0.408(9) 1 calc PR B 2 H29F H 0.7855 0.2985 0.4536 0.097 Uiso 0.408(9) 1 calc PR B 2 C30A C 0.9511(3) 0.3338(4) 0.4744(3) 0.050(3) Uani 0.408(9) 1 d PDU B 2 H30A H 0.9361 0.3531 0.4635 0.060 Uiso 0.408(9) 1 calc PR B 2 C31A C 0.9635(5) 0.3473(5) 0.5107(4) 0.069(4) Uani 0.408(9) 1 d PDU B 2 H31D H 0.9426 0.3519 0.5259 0.103 Uiso 0.408(9) 1 calc PR B 2 H31E H 0.9771 0.3695 0.5077 0.103 Uiso 0.408(9) 1 calc PR B 2 H31F H 0.9786 0.3292 0.5221 0.103 Uiso 0.408(9) 1 calc PR B 2 C32A C 0.9814(4) 0.3262(4) 0.4486(4) 0.076(4) Uani 0.408(9) 1 d PDU B 2 H32D H 0.9715 0.3175 0.4259 0.115 Uiso 0.408(9) 1 calc PR B 2 H32E H 0.9971 0.3079 0.4588 0.115 Uiso 0.408(9) 1 calc PR B 2 H32F H 0.9950 0.3482 0.4444 0.115 Uiso 0.408(9) 1 calc PR B 2 C33 C 0.9969(3) 0.2216(3) 0.2391(4) 0.061(3) Uani 0.50 1 d P . . H33 H 0.9837 0.2012 0.2317 0.074 Uiso 0.50 1 calc PR . . C34 C 1.0342(4) 0.2200(4) 0.2379(6) 0.086(4) Uani 0.50 1 d P . . C35 C 1.0543(5) 0.1865(5) 0.2262(7) 0.111(6) Uani 0.50 1 d PU . . H35A H 1.0399 0.1732 0.2088 0.166 Uiso 0.50 1 calc PR . . H35B H 1.0589 0.1713 0.2471 0.166 Uiso 0.50 1 calc PR . . H35C H 1.0771 0.1933 0.2152 0.166 Uiso 0.50 1 calc PR . . C36 C 1.0535(4) 0.2500 0.2500 0.079(4) Uani 1 4 d S . . H36 H 1.0789 0.2500 0.2500 0.095 Uiso 1 4 calc SR . . N1 N 0.91759(8) 0.27827(8) 0.29302(7) 0.0316(7) Uani 1 1 d . . . N2 N 0.91434(9) 0.33814(8) 0.26858(8) 0.0346(7) Uani 1 1 d . . . N3 N 0.9790(2) 0.2500 0.2500 0.0446(16) Uani 1 4 d S . . O1 O 0.88830(9) 0.38877(7) 0.40460(7) 0.0405(7) Uani 1 1 d . . . O2 O 0.88775(10) 0.33091(7) 0.44014(7) 0.0461(8) Uani 1 1 d . . . Co1 Co 0.92015(3) 0.2500 0.2500 0.0328(4) Uani 1 4 d S . . N4 N 1.0675(4) 0.3981(5) 0.3258(5) 0.113(5) Uani 0.50 1 d PD . . C37 C 1.0436(4) 0.4105(5) 0.3002(6) 0.110(6) Uani 0.50 1 d PD . . H37 H 1.0519 0.4249 0.2810 0.132 Uiso 0.50 1 calc PR . . C38 C 1.0075(3) 0.4018(3) 0.3026(3) 0.076(3) Uani 0.50 1 d PD . . C39 C 0.9954(3) 0.3807(4) 0.3307(4) 0.090(5) Uani 0.50 1 d PD . . H39 H 0.9707 0.3747 0.3324 0.108 Uiso 0.50 1 calc PR . . C40 C 1.0192(3) 0.3683(5) 0.3563(5) 0.100(5) Uani 0.50 1 d PD . . C41 C 1.0553(4) 0.3770(5) 0.3539(5) 0.103(5) Uani 0.50 1 d PD . . H41 H 1.0716 0.3686 0.3714 0.124 Uiso 0.50 1 calc PR . . C42 C 0.9821(7) 0.4147(7) 0.2782(7) 0.129(9) Uani 0.50 1 d P . . H42A H 0.9942 0.4284 0.2594 0.193 Uiso 0.50 1 calc PR . . H42B H 0.9650 0.4302 0.2907 0.193 Uiso 0.50 1 calc PR . . H42C H 0.9693 0.3945 0.2674 0.193 Uiso 0.50 1 calc PR . . C43 C 1.0098(8) 0.3467(9) 0.3893(8) 0.148(9) Uani 0.50 1 d PU . . H43A H 1.0318 0.3391 0.4014 0.222 Uiso 0.50 1 calc PR . . H43B H 0.9960 0.3256 0.3823 0.222 Uiso 0.50 1 calc PR . . H43C H 0.9956 0.3615 0.4057 0.222 Uiso 0.50 1 calc PR . . C44 C 0.8340(6) 0.2580(7) 0.2226(7) 0.088(5) Uani 0.25 1 d PDU . 1 H44 H 0.8454 0.2643 0.2008 0.105 Uiso 0.25 1 calc PR . 1 C45 C 0.7966(5) 0.2588(7) 0.2201(6) 0.095(6) Uani 0.25 1 d PDU . 1 C46 C 0.7760(8) 0.2500 0.2500 0.088(7) Uani 0.50 4 d SPDU . 1 H46 H 0.7506 0.2500 0.2500 0.105 Uiso 1 8 calc SR . 1 C47 C 0.7764(11) 0.2701(11) 0.1873(8) 0.111(10) Uani 0.25 1 d PDU . 1 H47A H 0.7933 0.2771 0.1686 0.166 Uiso 0.25 1 calc PR . 1 H47B H 0.7609 0.2905 0.1931 0.166 Uiso 0.25 1 calc PR . 1 H47C H 0.7617 0.2501 0.1788 0.166 Uiso 0.25 1 calc PR . 1 N5 N 0.8585(8) 0.2500 0.2500 0.085(6) Uani 0.50 4 d SPDU . 1 O3 O 0.8460(9) 0.2500 0.2500 0.099(6) Uani 0.50 4 d SPU C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0425(17) 0.0301(16) 0.0253(15) -0.0022(12) -0.0014(12) 0.0020(12) C2 0.0459(18) 0.0274(15) 0.0276(15) -0.0009(12) 0.0003(13) -0.0001(13) C3 0.0447(18) 0.0280(15) 0.0297(16) -0.0023(12) 0.0024(13) 0.0037(13) C4 0.0470(18) 0.0261(16) 0.0208(14) -0.0015(12) 0.0028(12) 0.0013(12) C5 0.052(2) 0.0283(15) 0.0258(15) 0.0004(12) 0.0016(13) 0.0049(13) C6 0.0480(19) 0.0252(15) 0.0302(16) -0.0034(12) 0.0041(13) 0.0038(13) C7 0.056(2) 0.0300(16) 0.0250(15) 0.0001(12) 0.0069(14) 0.0029(14) C8 0.062(2) 0.0261(15) 0.0265(15) -0.0002(12) 0.0026(14) 0.0066(14) C9 0.067(4) 0.024(3) 0.038(3) -0.003(2) 0.022(3) 0.002(3) C10 0.076(4) 0.037(3) 0.056(4) -0.012(3) 0.028(3) -0.005(3) C11 0.091(6) 0.034(3) 0.070(4) -0.008(3) 0.032(4) -0.009(3) C12 0.107(7) 0.029(3) 0.073(4) 0.004(3) 0.037(5) 0.002(4) C13 0.097(5) 0.039(3) 0.044(3) 0.004(3) 0.018(3) 0.028(3) C14 0.077(4) 0.028(3) 0.034(2) 0.002(2) 0.013(3) 0.019(3) C15 0.079(5) 0.063(4) 0.078(5) -0.016(4) 0.016(4) -0.020(4) C16 0.088(6) 0.087(6) 0.078(5) -0.031(5) 0.009(5) -0.023(5) C17 0.106(7) 0.093(7) 0.109(7) -0.018(6) 0.033(6) -0.037(6) C18 0.063(4) 0.049(4) 0.050(3) -0.006(3) 0.001(3) 0.018(3) C19 0.083(6) 0.090(7) 0.073(5) 0.004(5) 0.014(4) 0.010(5) C20 0.072(5) 0.052(4) 0.055(4) 0.003(4) 0.010(3) 0.013(3) C9A 0.063(6) 0.006(4) 0.042(6) -0.003(5) 0.017(5) -0.004(5) C10A 0.066(7) 0.038(6) 0.064(6) -0.004(5) 0.014(6) -0.008(5) C11A 0.052(7) 0.048(6) 0.066(8) 0.001(6) -0.010(6) -0.023(6) C12A 0.052(7) 0.052(7) 0.058(7) 0.004(6) 0.002(6) -0.024(6) C13A 0.046(6) 0.034(6) 0.050(5) -0.026(5) -0.011(5) -0.013(4) C14A 0.075(7) 0.040(6) 0.056(6) 0.000(6) 0.008(6) 0.007(6) C15A 0.069(9) 0.068(9) 0.083(10) -0.007(8) 0.005(8) -0.008(8) C16A 0.086(14) 0.106(15) 0.091(13) -0.018(12) -0.014(12) 0.000(12) C17A 0.056(9) 0.096(12) 0.110(13) 0.013(11) 0.029(9) 0.026(9) C18A 0.077(8) 0.044(8) 0.047(7) 0.006(6) 0.002(7) 0.015(7) C19A 0.043(7) 0.059(9) 0.042(7) 0.007(7) 0.002(6) 0.014(7) C20A 0.045(8) 0.043(10) 0.055(10) 0.014(7) 0.005(7) 0.007(7) C21 0.058(4) 0.040(4) 0.023(4) -0.005(3) -0.002(3) 0.004(4) C22 0.058(4) 0.031(3) 0.019(2) -0.002(2) 0.002(3) -0.005(3) C23 0.097(6) 0.040(3) 0.035(3) 0.001(3) 0.000(4) -0.022(4) C24 0.103(7) 0.051(4) 0.044(4) 0.011(3) -0.020(5) 0.010(5) C25 0.079(6) 0.072(6) 0.044(4) 0.004(4) -0.016(4) 0.029(5) C26 0.062(5) 0.062(4) 0.036(4) -0.009(3) 0.000(4) 0.009(4) C27 0.064(5) 0.060(5) 0.033(4) -0.001(3) -0.013(3) -0.007(4) C28 0.091(7) 0.099(8) 0.073(6) -0.035(6) -0.008(6) -0.005(6) C29 0.071(7) 0.063(6) 0.066(6) -0.013(5) 0.001(6) -0.002(6) C30 0.066(5) 0.058(5) 0.047(4) -0.009(4) -0.001(3) 0.015(4) C31 0.052(6) 0.082(6) 0.080(7) -0.017(6) 0.005(5) 0.008(5) C32 0.071(6) 0.089(8) 0.117(9) -0.003(7) 0.006(6) 0.011(6) C21A 0.051(5) 0.029(5) 0.015(4) 0.007(4) 0.006(4) 0.012(4) C22A 0.058(6) 0.059(5) 0.044(5) 0.000(4) 0.000(4) -0.004(5) C23A 0.032(4) 0.041(4) 0.063(6) -0.005(4) -0.002(5) 0.001(4) C24A 0.056(6) 0.072(6) 0.045(5) 0.012(5) 0.001(5) 0.010(6) C25A 0.055(6) 0.074(6) 0.048(5) 0.006(5) 0.004(5) 0.007(5) C26A 0.049(5) 0.069(6) 0.037(5) -0.002(4) -0.004(4) 0.013(5) C27A 0.060(6) 0.052(6) 0.040(5) -0.002(5) 0.004(5) 0.000(5) C28A 0.083(8) 0.058(7) 0.075(8) -0.030(6) -0.011(7) -0.012(6) C29A 0.064(9) 0.068(8) 0.061(8) -0.019(6) -0.001(7) -0.005(8) C30A 0.052(5) 0.049(6) 0.049(5) -0.012(5) -0.001(4) 0.002(5) C31A 0.060(9) 0.092(9) 0.055(7) -0.014(6) -0.018(6) 0.008(7) C32A 0.084(8) 0.076(8) 0.069(7) -0.018(6) 0.036(7) -0.004(7) C33 0.053(5) 0.048(5) 0.083(7) -0.018(5) 0.005(5) 0.003(4) C34 0.066(7) 0.067(7) 0.125(12) -0.033(8) 0.000(8) -0.006(6) C35 0.084(9) 0.096(10) 0.151(14) -0.040(10) -0.002(9) 0.004(8) C36 0.053(6) 0.092(6) 0.092(6) 0.000 0.000 0.000 N1 0.0438(15) 0.0283(14) 0.0227(13) 0.0015(10) -0.0015(10) 0.0009(11) N2 0.0492(17) 0.0264(13) 0.0283(14) -0.0016(10) -0.0026(11) 0.0031(11) N3 0.057(4) 0.038(2) 0.038(2) 0.000 0.000 0.000 O1 0.0642(17) 0.0268(12) 0.0307(12) -0.0047(9) 0.0065(11) 0.0074(11) O2 0.085(2) 0.0288(12) 0.0246(12) -0.0015(9) 0.0067(12) 0.0065(12) Co1 0.0556(7) 0.0214(4) 0.0214(4) 0.000 0.000 0.000 N4 0.068(7) 0.105(10) 0.165(17) -0.001(11) 0.002(9) -0.019(7) C37 0.101(12) 0.077(9) 0.154(18) 0.008(10) 0.017(12) -0.022(9) C38 0.081(8) 0.066(7) 0.081(8) -0.008(6) 0.006(6) -0.005(6) C39 0.059(6) 0.060(7) 0.149(15) 0.023(8) 0.008(8) -0.002(5) C40 0.085(10) 0.095(11) 0.119(14) 0.031(10) 0.013(9) 0.019(8) C41 0.073(9) 0.114(13) 0.124(14) 0.018(11) -0.016(9) 0.002(9) C42 0.140(18) 0.120(15) 0.126(16) 0.035(13) -0.069(15) -0.031(13) C43 0.135(15) 0.160(16) 0.149(16) 0.049(13) -0.003(13) 0.027(13) C44 0.074(10) 0.101(10) 0.088(9) -0.006(9) -0.002(8) 0.002(9) C45 0.082(10) 0.113(11) 0.091(11) -0.007(10) 0.000(9) 0.008(10) C46 0.061(10) 0.101(9) 0.101(9) 0.000 0.000 0.000 C47 0.104(16) 0.129(17) 0.100(15) -0.017(14) 0.000(13) 0.014(14) N5 0.083(12) 0.086(7) 0.086(7) 0.000 0.000 0.000 O3 0.106(13) 0.096(7) 0.096(7) 0.000 0.000 0.000 _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 1.325(5) . ? C1 N1 1.370(4) . ? C1 C2 1.458(4) . ? C2 C3 1.381(5) . ? C2 C5 1.403(5) . ? C3 C8 1.374(4) . ? C3 C4 1.454(4) . ? C4 N2 1.325(5) 23 ? C4 N1 1.375(4) . ? C5 C6 1.381(5) . ? C5 H5 0.9500 . ? C6 O1 1.380(4) . ? C6 C7 1.415(5) . ? C7 O2 1.370(4) . ? C7 C8 1.404(4) . ? C8 H8 0.9500 . ? C9 O1 1.346(4) . ? C9 C10 1.3900 . ? C9 C14 1.3900 . ? C10 C11 1.3900 . ? C10 C15 1.503(13) . ? C11 C12 1.3900 . ? C11 H11 0.9500 . ? C12 C13 1.3900 . ? C12 H12 0.9500 . ? C13 C14 1.3900 . ? C13 H13 0.9500 . ? C14 C18 1.574(10) . ? C15 C16 1.539(13) . ? C15 C17 1.547(12) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C20 1.535(10) . ? C18 C19 1.544(11) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C9A C14A 1.376(9) . ? C9A C10A 1.380(9) . ? C9A O1 1.470(14) . ? C10A C11A 1.392(9) . ? C10A C15A 1.504(15) . ? C11A C12A 1.383(9) . ? C11A H11A 0.9500 . ? C12A C13A 1.379(9) . ? C12A H12A 0.9500 . ? C13A C14A 1.402(9) . ? C13A H13A 0.9500 . ? C14A C18A 1.566(13) . ? C15A C16A 1.543(16) . ? C15A C17A 1.554(14) . ? C15A H15A 1.0000 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? C17A H17D 0.9800 . ? C17A H17E 0.9800 . ? C17A H17F 0.9800 . ? C18A C20A 1.536(12) . ? C18A C19A 1.540(13) . ? C18A H18A 1.0000 . ? C19A H19D 0.9800 . ? C19A H19E 0.9800 . ? C19A H19F 0.9800 . ? C20A H20D 0.9800 . ? C20A H20E 0.9800 . ? C20A H20F 0.9800 . ? C21 O2 1.344(5) . ? C21 C22 1.3900 . ? C21 C26 1.3900 . ? C22 C23 1.3900 . ? C22 C27 1.577(11) . ? C23 C24 1.3900 . ? C23 H23 0.9500 . ? C24 C25 1.3900 . ? C24 H24 0.9500 . ? C25 C26 1.3900 . ? C25 H25 0.9500 . ? C26 C30 1.512(11) . ? C27 C29 1.495(13) . ? C27 C28 1.511(11) . ? C27 H27 1.0000 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C32 1.508(13) . ? C30 C31 1.530(12) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C21A C22A 1.371(8) . ? C21A C26A 1.394(8) . ? C21A O2 1.444(10) . ? C22A C23A 1.397(8) . ? C22A C27A 1.575(13) . ? C23A C24A 1.375(8) . ? C23A H23A 0.9500 . ? C24A C25A 1.388(9) . ? C24A H24A 0.9500 . ? C25A C26A 1.372(8) . ? C25A H25A 0.9500 . ? C26A C30A 1.518(12) . ? C27A C29A 1.500(14) . ? C27A C28A 1.501(12) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29D 0.9800 . ? C29A H29E 0.9800 . ? C29A H29F 0.9800 . ? C30A C32A 1.512(13) . ? C30A C31A 1.522(13) . ? C30A H30A 1.0000 . ? C31A H31D 0.9800 . ? C31A H31E 0.9800 . ? C31A H31F 0.9800 . ? C32A H32D 0.9800 . ? C32A H32E 0.9800 . ? C32A H32F 0.9800 . ? C33 N3 1.319(10) . ? C33 C34 1.400(18) . ? C33 H33 0.9500 . ? C34 C36 1.409(14) . ? C34 C35 1.52(2) . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C34 1.409(14) 2 ? C36 H36 0.9500 . ? N1 Co1 1.927(3) . ? N2 C4 1.325(5) 24 ? N3 C33 1.319(10) 24 ? N3 C33 1.319(10) 23 ? N3 C33 1.319(10) 2 ? N3 Co1 2.200(9) . ? Co1 N1 1.927(3) 23 ? Co1 N1 1.927(3) 2 ? Co1 N1 1.927(3) 24 ? Co1 N5 2.31(3) . ? N4 C41 1.390(9) . ? N4 C37 1.390(9) . ? C37 C38 1.390(9) . ? C37 H37 0.9500 . ? C38 C39 1.390(9) . ? C38 C42 1.40(2) . ? C39 C40 1.390(9) . ? C39 H39 0.9500 . ? C40 C41 1.390(9) . ? C40 C43 1.52(3) . ? C41 H41 0.9500 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 C45 1.404(10) . ? C44 N5 1.405(10) . ? C44 H44 0.9500 . ? C45 C46 1.397(10) . ? C45 C47 1.501(10) . ? C46 C45 1.397(10) 2 ? C46 C46 1.94(6) 3_655 ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? N5 C44 1.405(10) 24 ? N5 C44 1.405(10) 23 ? N5 C44 1.405(10) 2 ? 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 127.9(3) . . ? N2 C1 C2 121.7(3) . . ? N1 C1 C2 110.4(3) . . ? C3 C2 C5 121.3(3) . . ? C3 C2 C1 105.7(3) . . ? C5 C2 C1 132.7(3) . . ? C8 C3 C2 122.8(3) . . ? C8 C3 C4 129.4(3) . . ? C2 C3 C4 107.3(3) . . ? N2 C4 N1 128.8(3) 23 . ? N2 C4 C3 121.7(3) 23 . ? N1 C4 C3 109.4(3) . . ? C6 C5 C2 116.7(3) . . ? C6 C5 H5 121.7 . . ? C2 C5 H5 121.7 . . ? O1 C6 C5 124.8(3) . . ? O1 C6 C7 113.2(3) . . ? C5 C6 C7 121.9(3) . . ? O2 C7 C8 124.6(3) . . ? O2 C7 C6 115.0(3) . . ? C8 C7 C6 120.3(3) . . ? C3 C8 C7 117.0(3) . . ? C3 C8 H8 121.5 . . ? C7 C8 H8 121.5 . . ? O1 C9 C10 118.0(2) . . ? O1 C9 C14 121.8(2) . . ? C10 C9 C14 120.0 . . ? C11 C10 C9 120.0 . . ? C11 C10 C15 119.7(4) . . ? C9 C10 C15 120.2(4) . . ? C10 C11 C12 120.0 . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.0 . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 120.0 . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C9 C14 C13 120.0 . . ? C9 C14 C18 116.6(3) . . ? C13 C14 C18 123.3(3) . . ? C10 C15 C16 108.6(8) . . ? C10 C15 C17 113.7(10) . . ? C16 C15 C17 109.8(9) . . ? C10 C15 H15 108.2 . . ? C16 C15 H15 108.2 . . ? C17 C15 H15 108.2 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C20 C18 C19 107.0(7) . . ? C20 C18 C14 111.8(6) . . ? C19 C18 C14 118.0(8) . . ? C20 C18 H18 106.5 . . ? C19 C18 H18 106.5 . . ? C14 C18 H18 106.5 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C14A C9A C10A 124.2(10) . . ? C14A C9A O1 118.6(10) . . ? C10A C9A O1 116.0(9) . . ? C9A C10A C11A 117.4(9) . . ? C9A C10A C15A 122.7(11) . . ? C11A C10A C15A 119.7(10) . . ? C12A C11A C10A 118.3(9) . . ? C12A C11A H11A 120.9 . . ? C10A C11A H11A 120.9 . . ? C13A C12A C11A 124.1(10) . . ? C13A C12A H12A 117.9 . . ? C11A C12A H12A 117.9 . . ? C12A C13A C14A 117.2(10) . . ? C12A C13A H13A 121.4 . . ? C14A C13A H13A 121.4 . . ? C9A C14A C13A 118.2(9) . . ? C9A C14A C18A 117.4(10) . . ? C13A C14A C18A 124.3(9) . . ? C10A C15A C16A 107.8(13) . . ? C10A C15A C17A 111.0(14) . . ? C16A C15A C17A 107.9(14) . . ? C10A C15A H15A 110.0 . . ? C16A C15A H15A 110.0 . . ? C17A C15A H15A 110.0 . . ? C15A C16A H16D 109.5 . . ? C15A C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? C15A C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? C15A C17A H17D 109.5 . . ? C15A C17A H17E 109.5 . . ? H17D C17A H17E 109.5 . . ? C15A C17A H17F 109.5 . . ? H17D C17A H17F 109.5 . . ? H17E C17A H17F 109.5 . . ? C20A C18A C19A 107.1(10) . . ? C20A C18A C14A 114.3(11) . . ? C19A C18A C14A 118.2(13) . . ? C20A C18A H18A 105.3 . . ? C19A C18A H18A 105.3 . . ? C14A C18A H18A 105.3 . . ? C18A C19A H19D 109.5 . . ? C18A C19A H19E 109.5 . . ? H19D C19A H19E 109.5 . . ? C18A C19A H19F 109.5 . . ? H19D C19A H19F 109.5 . . ? H19E C19A H19F 109.5 . . ? C18A C20A H20D 109.5 . . ? C18A C20A H20E 109.5 . . ? H20D C20A H20E 109.5 . . ? C18A C20A H20F 109.5 . . ? H20D C20A H20F 109.5 . . ? H20E C20A H20F 109.5 . . ? O2 C21 C22 123.2(3) . . ? O2 C21 C26 116.8(3) . . ? C22 C21 C26 120.0 . . ? C21 C22 C23 120.0 . . ? C21 C22 C27 115.5(4) . . ? C23 C22 C27 124.5(4) . . ? C24 C23 C22 120.0 . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.0 . . ? C23 C24 H24 120.0 . . ? C25 C24 H24 120.0 . . ? C26 C25 C24 120.0 . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C21 120.0 . . ? C25 C26 C30 114.5(5) . . ? C21 C26 C30 125.1(4) . . ? C29 C27 C28 110.8(9) . . ? C29 C27 C22 112.7(8) . . ? C28 C27 C22 111.8(9) . . ? C29 C27 H27 107.1 . . ? C28 C27 H27 107.1 . . ? C22 C27 H27 107.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C32 C30 C26 115.6(10) . . ? C32 C30 C31 110.9(9) . . ? C26 C30 C31 109.4(7) . . ? C32 C30 H30 106.8 . . ? C26 C30 H30 106.8 . . ? C31 C30 H30 106.8 . . ? 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 . . ? C30 C32 H32A 109.5 . . ? C30 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C30 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C22A C21A C26A 124.1(8) . . ? C22A C21A O2 123.3(8) . . ? C26A C21A O2 112.3(7) . . ? C21A C22A C23A 116.0(7) . . ? C21A C22A C27A 118.0(9) . . ? C23A C22A C27A 125.4(8) . . ? C24A C23A C22A 119.9(8) . . ? C24A C23A H23A 120.1 . . ? C22A C23A H23A 120.1 . . ? C23A C24A C25A 122.9(9) . . ? C23A C24A H24A 118.5 . . ? C25A C24A H24A 118.5 . . ? C26A C25A C24A 117.5(9) . . ? C26A C25A H25A 121.2 . . ? C24A C25A H25A 121.2 . . ? C25A C26A C21A 119.0(8) . . ? C25A C26A C30A 121.3(9) . . ? C21A C26A C30A 119.7(8) . . ? C29A C27A C28A 110.2(11) . . ? C29A C27A C22A 111.8(10) . . ? C28A C27A C22A 113.8(12) . . ? C29A C27A H27A 106.9 . . ? C28A C27A H27A 106.9 . . ? C22A C27A H27A 106.9 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29D 109.5 . . ? C27A C29A H29E 109.5 . . ? H29D C29A H29E 109.5 . . ? C27A C29A H29F 109.5 . . ? H29D C29A H29F 109.5 . . ? H29E C29A H29F 109.5 . . ? C32A C30A C26A 110.7(11) . . ? C32A C30A C31A 113.9(11) . . ? C26A C30A C31A 110.0(10) . . ? C32A C30A H30A 107.3 . . ? C26A C30A H30A 107.3 . . ? C31A C30A H30A 107.3 . . ? C30A C31A H31D 109.5 . . ? C30A C31A H31E 109.5 . . ? H31D C31A H31E 109.5 . . ? C30A C31A H31F 109.5 . . ? H31D C31A H31F 109.5 . . ? H31E C31A H31F 109.5 . . ? C30A C32A H32D 109.5 . . ? C30A C32A H32E 109.5 . . ? H32D C32A H32E 109.5 . . ? C30A C32A H32F 109.5 . . ? H32D C32A H32F 109.5 . . ? H32E C32A H32F 109.5 . . ? N3 C33 C34 123.5(10) . . ? N3 C33 H33 118.2 . . ? C34 C33 H33 118.2 . . ? C33 C34 C36 117.7(11) . . ? C33 C34 C35 122.5(12) . . ? C36 C34 C35 119.7(13) . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 C34 118.6(15) . 2 ? C34 C36 H36 120.7 . . ? C34 C36 H36 120.7 2 . ? C1 N1 C4 107.1(3) . . ? C1 N1 Co1 126.8(2) . . ? C4 N1 Co1 125.8(2) . . ? C1 N2 C4 120.7(3) . 24 ? C33 N3 C33 75.1(5) 24 . ? C33 N3 C33 119.0(11) 24 23 ? C33 N3 C33 75.1(5) . 23 ? C33 N3 C33 75.1(5) 24 2 ? C33 N3 C33 119.0(11) . 2 ? C33 N3 C33 75.1(5) 23 2 ? C33 N3 Co1 120.5(6) 24 . ? C33 N3 Co1 120.5(6) . . ? C33 N3 Co1 120.5(6) 23 . ? C33 N3 Co1 120.5(6) 2 . ? C9 O1 C6 118.0(3) . . ? C9 O1 C9A 10.8(5) . . ? C6 O1 C9A 120.0(7) . . ? C21 O2 C7 115.5(3) . . ? C21 O2 C21A 8.7(5) . . ? C7 O2 C21A 115.4(5) . . ? N1 Co1 N1 89.859(10) 23 2 ? N1 Co1 N1 89.859(10) 23 . ? N1 Co1 N1 174.3(2) 2 . ? N1 Co1 N1 174.3(2) 23 24 ? N1 Co1 N1 89.859(10) 2 24 ? N1 Co1 N1 89.859(10) . 24 ? N1 Co1 N3 92.84(10) 23 . ? N1 Co1 N3 92.84(10) 2 . ? N1 Co1 N3 92.84(10) . . ? N1 Co1 N3 92.84(10) 24 . ? N1 Co1 N5 87.16(10) 23 . ? N1 Co1 N5 87.16(10) 2 . ? N1 Co1 N5 87.16(10) . . ? N1 Co1 N5 87.16(10) 24 . ? N3 Co1 N5 180.000(1) . . ? C41 N4 C37 120.0(14) . . ? C38 C37 N4 120.0(15) . . ? C38 C37 H37 120.0 . . ? N4 C37 H37 120.0 . . ? C37 C38 C39 120.0(13) . . ? C37 C38 C42 122.2(15) . . ? C39 C38 C42 117.7(15) . . ? C40 C39 C38 120.0(12) . . ? C40 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C39 C40 C41 120.0(14) . . ? C39 C40 C43 126.1(16) . . ? C41 C40 C43 113.8(16) . . ? N4 C41 C40 120.0(14) . . ? N4 C41 H41 120.0 . . ? C40 C41 H41 120.0 . . ? C38 C42 H42A 109.5 . . ? C38 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C38 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C45 C44 N5 135(3) . . ? C45 C44 H44 112.7 . . ? N5 C44 H44 112.7 . . ? C46 C45 C44 119(3) . . ? C46 C45 C47 116(2) . . ? C44 C45 C47 124(2) . . ? C45 C46 C45 113(3) . 2 ? C45 C46 C46 123.4(14) . 3_655 ? C45 C46 C46 123.4(14) 2 3_655 ? C45 C46 H46 123.4 . . ? C45 C46 H46 123.4 2 . ? C46 C46 H46 0.0 3_655 . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C44 N5 C44 65.0(19) 24 . ? C44 N5 C44 99(3) 24 23 ? C44 N5 C44 65.0(19) . 23 ? C44 N5 C44 65.0(19) 24 2 ? C44 N5 C44 99(3) . 2 ? C44 N5 C44 65.0(19) 23 2 ? C44 N5 Co1 130.6(17) 24 . ? C44 N5 Co1 130.6(17) . . ? C44 N5 Co1 130.6(17) 23 . ? C44 N5 Co1 130.6(17) 2 . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.59 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.247 _refine_diff_density_min -0.622 _refine_diff_density_rms 0.227 data_pcco16daa _database_code_depnum_ccdc_archive 'CCDC 900379' #TrackingRef '900379_PNC[vH2O-Co-cDAH-Co-vH2O.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C132 H155 Cl3 Co N9 O9' _chemical_formula_weight 2176.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Cubic _symmetry_space_group_name_H-M Pn-3n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' 'z, x, y' 'z, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y' '-z+1/2, x, -y+1/2' 'y, z, x' '-y+1/2, z, -x+1/2' 'y, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x' 'y, x, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y, -x+1/2, z' '-y+1/2, x, z' 'x, z, -y+1/2' '-x+1/2, z, y' '-x+1/2, -z+1/2, -y+1/2' 'x, -z+1/2, y' 'z, y, -x+1/2' 'z, -y+1/2, x' '-z+1/2, y, x' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, y-1/2, z-1/2' '-z, -x, -y' '-z, x-1/2, y-1/2' 'z-1/2, x-1/2, -y' 'z-1/2, -x, y-1/2' '-y, -z, -x' 'y-1/2, -z, x-1/2' '-y, z-1/2, x-1/2' 'y-1/2, z-1/2, -x' '-y, -x, z-1/2' 'y-1/2, x-1/2, z-1/2' '-y, x-1/2, -z' 'y-1/2, -x, -z' '-x, -z, y-1/2' 'x-1/2, -z, -y' 'x-1/2, z-1/2, y-1/2' '-x, z-1/2, -y' '-z, -y, x-1/2' '-z, y-1/2, -x' 'z-1/2, -y, -x' 'z-1/2, y-1/2, x-1/2' _cell_length_a 37.4908(2) _cell_length_b 37.4908(2) _cell_length_c 37.4908(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 52695.6(5) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9339 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.69 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.70 _exptl_crystal_size_mid 0.45 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.823 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 13920 _exptl_absorpt_coefficient_mu 0.185 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8814 _exptl_absorpt_correction_T_max 0.9296 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.67100 _diffrn_radiation_type synchrotron _diffrn_radiation_source synchrotron _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 226206 _diffrn_reflns_av_R_equivalents 0.0968 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_k_min -36 _diffrn_reflns_limit_k_max 43 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 0.73 _diffrn_reflns_theta_max 23.18 _reflns_number_total 7453 _reflns_number_gt 5513 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 CONSTR _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7453 _refine_ls_number_parameters 354 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1843 _refine_ls_R_factor_gt 0.1458 _refine_ls_wR_factor_ref 0.4590 _refine_ls_wR_factor_gt 0.4153 _refine_ls_goodness_of_fit_ref 2.041 _refine_ls_restrained_S_all 2.057 _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 0.7500 0.7500 0.09308(4) 0.0436(5) Uani 1 4 d S . . O1 O 0.88918(8) 0.59542(8) 0.11164(10) 0.0508(9) Uani 1 1 d . A . O2 O 0.83156(8) 0.55953(8) 0.11143(10) 0.0540(9) Uani 1 1 d . . . O3 O 0.7500 0.7500 0.0410(2) 0.064(2) Uani 1 4 d S . . N1 N 0.77826(9) 0.70707(9) 0.09280(11) 0.0470(10) Uani 1 1 d . A . N2 N 0.73151(10) 0.66204(10) 0.09422(11) 0.0505(10) Uani 1 1 d . A . C1 C 0.82583(12) 0.66811(12) 0.09611(14) 0.0483(12) Uani 1 1 d . . . C2 C 0.85877(11) 0.65189(12) 0.10040(13) 0.0475(11) Uani 1 1 d . A . H2 H 0.8802 0.6654 0.1000 0.071 Uiso 1 1 calc R . . C3 C 0.85935(11) 0.61533(12) 0.10528(13) 0.0472(11) Uani 1 1 d . . . C4 C 0.82745(12) 0.59531(11) 0.10488(14) 0.0487(11) Uani 1 1 d . A . C5 C 0.79471(12) 0.61134(11) 0.09921(14) 0.0506(12) Uani 1 1 d . . . H5 H 0.7734 0.5977 0.0981 0.076 Uiso 1 1 calc R A . C6 C 0.79441(11) 0.64827(12) 0.09525(13) 0.0489(11) Uani 1 1 d . A . C7 C 0.76535(12) 0.67305(11) 0.09369(13) 0.0473(11) Uani 1 1 d . . . C8 C 0.70486(11) 0.68525(11) 0.09387(13) 0.0461(11) Uani 1 1 d . . . C9 C 0.92206(12) 0.61319(13) 0.11502(16) 0.0576(13) Uani 1 1 d . . . C10 C 0.93105(14) 0.62707(13) 0.14772(17) 0.0659(16) Uani 1 1 d . A . C11 C 0.96466(16) 0.64168(16) 0.1512(2) 0.086(2) Uani 1 1 d . . . H11 H 0.9718 0.6514 0.1735 0.129 Uiso 1 1 calc R A . C12 C 0.98756(17) 0.6425(2) 0.1236(3) 0.103(3) Uani 1 1 d . A . H12 H 1.0105 0.6528 0.1266 0.154 Uiso 1 1 calc R . . C13 C 0.97785(16) 0.6282(2) 0.0909(3) 0.098(3) Uani 1 1 d . . . H13 H 0.9943 0.6290 0.0717 0.147 Uiso 1 1 calc R A . C14 C 0.94426(14) 0.61280(17) 0.08583(19) 0.0772(19) Uani 1 1 d . A . C15 C 0.90525(16) 0.62493(14) 0.17896(16) 0.0679(15) Uani 1 1 d . . . H15 H 0.8810 0.6309 0.1697 0.102 Uiso 1 1 calc R A . C16 C 0.90378(17) 0.58715(15) 0.19346(18) 0.0721(16) Uani 1 1 d . A . H16A H 0.8957 0.5709 0.1747 0.108 Uiso 1 1 calc R . . H16B H 0.8871 0.5862 0.2136 0.108 Uiso 1 1 calc R . . H16C H 0.9276 0.5800 0.2015 0.108 Uiso 1 1 calc R . . C17 C 0.9133(2) 0.65080(18) 0.2099(2) 0.105(3) Uani 1 1 d . A . H17A H 0.9390 0.6512 0.2144 0.158 Uiso 1 1 calc R . . H17B H 0.9008 0.6428 0.2314 0.158 Uiso 1 1 calc R . . H17C H 0.9052 0.6748 0.2035 0.158 Uiso 1 1 calc R . . C18 C 0.9330(2) 0.59431(19) 0.0512(2) 0.087(2) Uani 1 1 d . . . H18 H 0.9071 0.5994 0.0474 0.130 Uiso 1 1 calc R A . C19 C 0.9526(3) 0.6072(3) 0.0189(3) 0.142(4) Uani 1 1 d . A . H19A H 0.9779 0.6011 0.0211 0.214 Uiso 1 1 calc R . . H19B H 0.9500 0.6331 0.0169 0.214 Uiso 1 1 calc R . . H19C H 0.9427 0.5957 -0.0024 0.214 Uiso 1 1 calc R . . C20 C 0.9370(2) 0.5549(2) 0.0556(3) 0.108(3) Uani 1 1 d . A . H20A H 0.9624 0.5486 0.0551 0.163 Uiso 1 1 calc R . . H20B H 0.9246 0.5426 0.0362 0.163 Uiso 1 1 calc R . . H20C H 0.9267 0.5476 0.0785 0.163 Uiso 1 1 calc R . . C21A C 0.80055(15) 0.53931(18) 0.11274(19) 0.043(3) Uiso 0.524(11) 1 d PG A 1 C22A C 0.79139(18) 0.5195(2) 0.08277(17) 0.062(3) Uiso 0.524(11) 1 d PG A 1 C23A C 0.76047(19) 0.49904(18) 0.08281(19) 0.056(3) Uiso 0.524(11) 1 d PG A 1 H23A H 0.7542 0.4855 0.0623 0.084 Uiso 0.524(11) 1 calc PR A 1 C24A C 0.73869(15) 0.49842(18) 0.1128(2) 0.067(3) Uiso 0.524(11) 1 d PG A 1 H24A H 0.7176 0.4844 0.1128 0.100 Uiso 0.524(11) 1 calc PR A 1 C25A C 0.74785(15) 0.51824(18) 0.1428(2) 0.058(3) Uiso 0.524(11) 1 d PG A 1 H25A H 0.7330 0.5178 0.1633 0.087 Uiso 0.524(11) 1 calc PR A 1 C26A C 0.77878(16) 0.53868(17) 0.14274(17) 0.046(2) Uiso 0.524(11) 1 d PG A 1 C21B C 0.80270(16) 0.5397(2) 0.1051(2) 0.044(3) Uiso 0.476(11) 1 d PG A 2 C22B C 0.79959(18) 0.5214(2) 0.07303(19) 0.050(3) Uiso 0.476(11) 1 d PG A 2 C23B C 0.7697(2) 0.5005(2) 0.0664(2) 0.068(3) Uiso 0.476(11) 1 d PG A 2 H23B H 0.7676 0.4880 0.0445 0.101 Uiso 0.476(11) 1 calc PR A 2 C24B C 0.74291(17) 0.4979(2) 0.0919(2) 0.063(3) Uiso 0.476(11) 1 d PG A 2 H24B H 0.7225 0.4836 0.0874 0.095 Uiso 0.476(11) 1 calc PR A 2 C25B C 0.74603(16) 0.5162(2) 0.1240(2) 0.054(3) Uiso 0.476(11) 1 d PG A 2 H25B H 0.7277 0.5144 0.1415 0.081 Uiso 0.476(11) 1 calc PR A 2 C26B C 0.77592(19) 0.5371(2) 0.13064(19) 0.052(3) Uiso 0.476(11) 1 d PGD A 2 C27A C 0.8136(4) 0.5213(3) 0.0480(3) 0.064(3) Uiso 0.524(11) 1 d P A 1 H27A H 0.8199 0.5471 0.0451 0.095 Uiso 0.524(11) 1 calc PR A 1 C28A C 0.8518(4) 0.5008(5) 0.0527(5) 0.090(5) Uiso 0.524(11) 1 d P A 1 H28D H 0.8618 0.4956 0.0292 0.134 Uiso 0.524(11) 1 calc PR A 1 H28E H 0.8481 0.4784 0.0657 0.134 Uiso 0.524(11) 1 calc PR A 1 H28F H 0.8683 0.5160 0.0661 0.134 Uiso 0.524(11) 1 calc PR A 1 C29A C 0.7981(4) 0.5109(4) 0.0138(4) 0.105(5) Uiso 0.524(11) 1 d P A 1 H29A H 0.7876 0.5318 0.0022 0.158 Uiso 0.524(11) 1 calc PR A 1 H29B H 0.7795 0.4929 0.0178 0.158 Uiso 0.524(11) 1 calc PR A 1 H29C H 0.8167 0.5008 -0.0015 0.158 Uiso 0.524(11) 1 calc PR A 1 C27B C 0.8296(5) 0.5254(4) 0.0474(4) 0.069(4) Uiso 0.476(11) 1 d P A 2 H27B H 0.8478 0.5373 0.0627 0.104 Uiso 0.476(11) 1 calc PR A 2 C28B C 0.8466(4) 0.4915(5) 0.0406(5) 0.085(5) Uiso 0.476(11) 1 d P A 2 H28A H 0.8678 0.4952 0.0258 0.127 Uiso 0.476(11) 1 calc PR A 2 H28B H 0.8300 0.4757 0.0282 0.127 Uiso 0.476(11) 1 calc PR A 2 H28C H 0.8537 0.4807 0.0633 0.127 Uiso 0.476(11) 1 calc PR A 2 C29B C 0.8242(8) 0.5527(8) 0.0195(8) 0.178(12) Uiso 0.476(11) 1 d P A 2 H29D H 0.8116 0.5732 0.0298 0.267 Uiso 0.476(11) 1 calc PR A 2 H29E H 0.8100 0.5426 0.0000 0.267 Uiso 0.476(11) 1 calc PR A 2 H29F H 0.8474 0.5604 0.0103 0.267 Uiso 0.476(11) 1 calc PR A 2 C30 C 0.7838(2) 0.55796(19) 0.1705(2) 0.102(3) Uani 1 1 d D . . H30 H 0.7995 0.5790 0.1659 0.154 Uiso 1 1 calc R A 1 C31 C 0.7955(2) 0.5359(2) 0.2029(3) 0.108(3) Uani 1 1 d . A . H31A H 0.7765 0.5191 0.2094 0.162 Uiso 1 1 calc R . . H31B H 0.8002 0.5519 0.2231 0.162 Uiso 1 1 calc R . . H31C H 0.8173 0.5227 0.1971 0.162 Uiso 1 1 calc R . . C32A C 0.7400(6) 0.5699(6) 0.1808(5) 0.101(7) Uiso 0.44(2) 1 d P A 1 H32A H 0.7299 0.5839 0.1611 0.151 Uiso 0.44(2) 1 calc PR A 1 H32B H 0.7398 0.5842 0.2026 0.151 Uiso 0.44(2) 1 calc PR A 1 H32C H 0.7257 0.5483 0.1844 0.151 Uiso 0.44(2) 1 calc PR A 1 C32B C 0.7606(4) 0.5897(4) 0.1845(3) 0.084(5) Uiso 0.56(2) 1 d P A 2 H32D H 0.7484 0.6011 0.1645 0.126 Uiso 0.56(2) 1 calc PR A 2 H32E H 0.7760 0.6071 0.1965 0.126 Uiso 0.56(2) 1 calc PR A 2 H32F H 0.7429 0.5806 0.2015 0.126 Uiso 0.56(2) 1 calc PR A 2 N1S N 0.7500 0.7500 0.1471(2) 0.0531(19) Uiso 1 4 d S . . C1S C 0.7690(11) 0.7708(11) 0.1688(12) 0.125(13) Uiso 0.25 1 d P . . C2S C 0.7724(7) 0.7690(7) 0.2089(7) 0.071(6) Uiso 0.25 1 d P . . C3S C 0.7925(12) 0.7942(12) 0.2275(12) 0.139(15) Uiso 0.25 1 d P . . C4S C 0.8917(5) 0.7123(5) 0.0222(5) 0.053(4) Uiso 0.25 1 d P . . H4S H 0.8717 0.7130 0.0398 0.4(4) Uiso 0.25 1 calc PR . . Cl1S Cl 0.92925(12) 0.70951(13) 0.05079(16) 0.0624(14) Uani 0.25 1 d P . . Cl2S Cl 0.8887(7) 0.7518(3) 0.0042(4) 0.245(11) Uani 0.25 1 d P . . Cl3S Cl 0.8837(3) 0.6750(2) 0.0017(3) 0.140(4) Uani 0.25 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0312(5) 0.0312(5) 0.0685(9) 0.000 0.000 0.000 O1 0.0352(16) 0.0390(16) 0.078(2) 0.0036(14) -0.0102(15) 0.0050(12) O2 0.0361(16) 0.0319(15) 0.094(2) 0.0039(15) -0.0070(15) 0.0053(12) O3 0.054(2) 0.054(2) 0.086(5) 0.000 0.000 0.000 N1 0.0349(19) 0.0337(18) 0.072(3) 0.0021(16) -0.0044(16) -0.0022(14) N2 0.036(2) 0.0355(19) 0.080(3) 0.0046(17) -0.0062(17) -0.0002(16) C1 0.040(2) 0.037(2) 0.068(3) -0.004(2) -0.002(2) -0.0039(18) C2 0.032(2) 0.039(2) 0.072(3) 0.004(2) -0.0053(19) -0.0004(17) C3 0.035(2) 0.041(2) 0.066(3) -0.003(2) -0.0067(19) 0.0075(18) C4 0.039(2) 0.033(2) 0.073(3) -0.001(2) -0.006(2) 0.0024(17) C5 0.036(2) 0.033(2) 0.082(3) 0.003(2) -0.009(2) 0.0028(17) C6 0.036(2) 0.037(2) 0.074(3) -0.004(2) -0.0062(19) -0.0019(17) C7 0.036(2) 0.034(2) 0.071(3) -0.0012(19) -0.006(2) -0.0032(17) C8 0.035(2) 0.035(2) 0.069(3) 0.0028(19) 0.0022(19) -0.0012(17) C9 0.036(2) 0.049(3) 0.089(4) 0.019(2) -0.010(2) 0.003(2) C10 0.052(3) 0.043(3) 0.102(4) 0.015(3) -0.030(3) -0.004(2) C11 0.055(3) 0.072(4) 0.132(6) 0.038(4) -0.037(4) -0.011(3) C12 0.046(3) 0.101(5) 0.161(8) 0.059(5) -0.034(5) -0.011(3) C13 0.043(3) 0.099(5) 0.151(8) 0.067(5) 0.005(4) 0.005(3) C14 0.045(3) 0.084(4) 0.102(5) 0.039(4) 0.005(3) 0.018(3) C15 0.075(4) 0.052(3) 0.076(4) -0.002(3) -0.018(3) 0.003(3) C16 0.083(4) 0.055(3) 0.078(4) 0.002(3) 0.000(3) -0.001(3) C17 0.141(7) 0.066(4) 0.108(6) -0.008(4) -0.036(5) 0.001(4) C18 0.081(4) 0.092(5) 0.088(5) 0.022(4) 0.014(4) 0.022(4) C19 0.152(9) 0.153(9) 0.123(8) 0.036(7) 0.036(7) 0.024(7) C20 0.115(6) 0.091(5) 0.118(7) 0.006(4) 0.001(5) 0.031(5) C30 0.125(6) 0.076(4) 0.106(5) 0.019(4) 0.045(5) 0.048(4) C31 0.091(5) 0.086(5) 0.149(7) 0.019(5) 0.016(5) 0.028(4) Cl1S 0.043(2) 0.055(3) 0.090(4) -0.021(2) 0.019(2) -0.013(2) Cl2S 0.49(3) 0.111(9) 0.138(10) 0.054(7) -0.113(15) -0.002(12) Cl3S 0.188(10) 0.069(4) 0.164(9) -0.018(5) -0.092(8) -0.001(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N1 1.927(3) 16_655 ? Co1 N1 1.927(3) 2_665 ? Co1 N1 1.927(3) . ? Co1 N1 1.927(3) 15_565 ? Co1 O3 1.953(9) . ? Co1 N1S 2.024(9) . ? O1 C3 1.366(5) . ? O1 C9 1.407(6) . ? O2 C21B 1.334(5) . ? O2 C4 1.373(5) . ? O2 C21A 1.389(5) . ? N1 C7 1.365(5) . ? N1 C8 1.371(6) 16_655 ? N2 C8 1.325(6) . ? N2 C7 1.334(6) . ? C1 C2 1.386(6) . ? C1 C6 1.393(6) . ? C1 C8 1.442(6) 16_655 ? C2 C3 1.383(6) . ? C2 H2 0.9500 . ? C3 C4 1.412(6) . ? C4 C5 1.383(6) . ? C5 C6 1.393(6) . ? C5 H5 0.9500 . ? C6 C7 1.433(6) . ? C8 N1 1.371(6) 15_565 ? C8 C1 1.442(6) 15_565 ? C9 C10 1.374(8) . ? C9 C14 1.375(8) . ? C10 C11 1.380(8) . ? C10 C15 1.521(9) . ? C11 C12 1.344(11) . ? C11 H11 0.9500 . ? C12 C13 1.385(13) . ? C12 H12 0.9500 . ? C13 C14 1.399(10) . ? C13 H13 0.9500 . ? C14 C18 1.532(10) . ? C15 C16 1.518(8) . ? C15 C17 1.541(9) . ? C15 H15 1.0000 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 C19 1.495(11) . ? C18 C20 1.496(10) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21A C22A 1.3900 . ? C21A C26A 1.3900 . ? C22A C23A 1.3900 . ? C22A C27A 1.549(13) . ? C23A C24A 1.3900 . ? C23A H23A 0.9500 . ? C24A C25A 1.3900 . ? C24A H24A 0.9500 . ? C25A C26A 1.3900 . ? C25A H25A 0.9500 . ? C26A C30 1.281(9) . ? C21B C22B 1.3900 . ? C21B C26B 1.3900 . ? C22B C23B 1.3900 . ? C22B C27B 1.487(16) . ? C23B C24B 1.3900 . ? C23B H23B 0.9500 . ? C24B C25B 1.3900 . ? C24B H24B 0.9500 . ? C25B C26B 1.3900 . ? C25B H25B 0.9500 . ? C26B C30 1.712(10) . ? C27A C29A 1.461(19) . ? C27A C28A 1.63(2) . ? C27A H27A 1.0000 . ? C28A H28D 0.9800 . ? C28A H28E 0.9800 . ? C28A H28F 0.9800 . ? C29A H29A 0.9800 . ? C29A H29B 0.9800 . ? C29A H29C 0.9800 . ? C27B C28B 1.44(2) . ? C27B C29B 1.48(3) . ? C27B H27B 1.0000 . ? C28B H28A 0.9800 . ? C28B H28B 0.9800 . ? C28B H28C 0.9800 . ? C29B H29D 0.9800 . ? C29B H29E 0.9800 . ? C29B H29F 0.9800 . ? C30 C31 1.536(11) . ? C30 C32B 1.563(14) . ? C30 C32A 1.74(2) . ? C30 H30 1.0000 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32A H32A 0.9800 . ? C32A H32B 0.9800 . ? C32A H32C 0.9800 . ? C32B H32D 0.9800 . ? C32B H32E 0.9800 . ? C32B H32F 0.9800 . ? N1S C1S 1.33(4) 16_655 ? N1S C1S 1.33(4) 15_565 ? N1S C1S 1.33(4) . ? N1S C1S 1.33(4) 2_665 ? C1S C1S 1.49(6) 16_655 ? C1S C1S 1.49(6) 15_565 ? C1S C2S 1.51(5) . ? C2S C3S 1.39(5) . ? C2S C2S 1.56(4) 16_655 ? C2S C2S 1.56(4) 15_565 ? C3S C3S 1.69(9) 13 ? C4S Cl3S 1.62(2) . ? C4S Cl2S 1.63(2) . ? C4S Cl1S 1.77(2) . ? C4S H4S 1.0000 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Co1 N1 89.998(2) 16_655 2_665 ? N1 Co1 N1 89.998(2) 16_655 . ? N1 Co1 N1 179.4(3) 2_665 . ? N1 Co1 N1 179.4(3) 16_655 15_565 ? N1 Co1 N1 89.998(2) 2_665 15_565 ? N1 Co1 N1 89.998(2) . 15_565 ? N1 Co1 O3 89.69(13) 16_655 . ? N1 Co1 O3 89.69(13) 2_665 . ? N1 Co1 O3 89.69(13) . . ? N1 Co1 O3 89.69(13) 15_565 . ? N1 Co1 N1S 90.31(13) 16_655 . ? N1 Co1 N1S 90.31(13) 2_665 . ? N1 Co1 N1S 90.31(13) . . ? N1 Co1 N1S 90.31(13) 15_565 . ? O3 Co1 N1S 180.000(2) . . ? C3 O1 C9 118.3(3) . . ? C21B O2 C4 114.9(5) . . ? C21B O2 C21A 12.3(5) . . ? C4 O2 C21A 116.5(4) . . ? C7 N1 C8 107.3(3) . 16_655 ? C7 N1 Co1 125.8(3) . . ? C8 N1 Co1 126.8(3) 16_655 . ? C8 N2 C7 120.9(4) . . ? C2 C1 C6 121.5(4) . . ? C2 C1 C8 133.1(4) . 16_655 ? C6 C1 C8 105.4(4) . 16_655 ? C3 C2 C1 117.7(4) . . ? C3 C2 H2 121.2 . . ? C1 C2 H2 121.2 . . ? O1 C3 C2 125.3(4) . . ? O1 C3 C4 113.9(4) . . ? C2 C3 C4 120.8(4) . . ? O2 C4 C5 123.5(4) . . ? O2 C4 C3 115.0(4) . . ? C5 C4 C3 121.5(4) . . ? C4 C5 C6 117.1(4) . . ? C4 C5 H5 121.5 . . ? C6 C5 H5 121.5 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 C7 130.9(4) . . ? C1 C6 C7 107.3(4) . . ? N2 C7 N1 128.8(4) . . ? N2 C7 C6 121.5(4) . . ? N1 C7 C6 109.7(4) . . ? N2 C8 N1 127.6(4) . 15_565 ? N2 C8 C1 122.1(4) . 15_565 ? N1 C8 C1 110.3(4) 15_565 15_565 ? C10 C9 C14 124.5(5) . . ? C10 C9 O1 118.3(5) . . ? C14 C9 O1 117.0(5) . . ? C9 C10 C11 117.3(6) . . ? C9 C10 C15 120.7(4) . . ? C11 C10 C15 121.9(6) . . ? C12 C11 C10 121.3(7) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 120.3(6) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C13 C14 121.2(7) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C9 C14 C13 115.5(7) . . ? C9 C14 C18 120.9(5) . . ? C13 C14 C18 123.5(7) . . ? C16 C15 C10 110.4(5) . . ? C16 C15 C17 109.0(5) . . ? C10 C15 C17 114.9(6) . . ? C16 C15 H15 107.4 . . ? C10 C15 H15 107.4 . . ? C17 C15 H15 107.4 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C20 111.0(7) . . ? C19 C18 C14 113.9(8) . . ? C20 C18 C14 109.0(6) . . ? C19 C18 H18 107.6 . . ? C20 C18 H18 107.6 . . ? C14 C18 H18 107.6 . . ? 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 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O2 C21A C22A 118.0(4) . . ? O2 C21A C26A 122.0(4) . . ? C22A C21A C26A 120.0 . . ? C21A C22A C23A 120.0 . . ? C21A C22A C27A 121.6(6) . . ? C23A C22A C27A 118.3(6) . . ? C22A C23A C24A 120.0 . . ? C22A C23A H23A 120.0 . . ? C24A C23A H23A 120.0 . . ? C25A C24A C23A 120.0 . . ? C25A C24A H24A 120.0 . . ? C23A C24A H24A 120.0 . . ? C26A C25A C24A 120.0 . . ? C26A C25A H25A 120.0 . . ? C24A C25A H25A 120.0 . . ? C30 C26A C25A 115.6(6) . . ? C30 C26A C21A 124.2(6) . . ? C25A C26A C21A 120.0 . . ? O2 C21B C22B 119.7(5) . . ? O2 C21B C26B 120.3(5) . . ? C22B C21B C26B 120.0 . . ? C21B C22B C23B 120.0 . . ? C21B C22B C27B 116.6(7) . . ? C23B C22B C27B 123.4(7) . . ? C24B C23B C22B 120.0 . . ? C24B C23B H23B 120.0 . . ? C22B C23B H23B 120.0 . . ? C23B C24B C25B 120.0 . . ? C23B C24B H24B 120.0 . . ? C25B C24B H24B 120.0 . . ? C26B C25B C24B 120.0 . . ? C26B C25B H25B 120.0 . . ? C24B C25B H25B 120.0 . . ? C25B C26B C21B 120.0 . . ? C25B C26B C30 123.5(5) . . ? C21B C26B C30 116.3(5) . . ? C29A C27A C22A 120.8(12) . . ? C29A C27A C28A 108.5(11) . . ? C22A C27A C28A 111.0(9) . . ? C29A C27A H27A 105.1 . . ? C22A C27A H27A 105.1 . . ? C28A C27A H27A 105.1 . . ? C27A C28A H28D 109.5 . . ? C27A C28A H28E 109.5 . . ? H28D C28A H28E 109.5 . . ? C27A C28A H28F 109.5 . . ? H28D C28A H28F 109.5 . . ? H28E C28A H28F 109.5 . . ? C27A C29A H29A 109.5 . . ? C27A C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27A C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C28B C27B C29B 123.2(17) . . ? C28B C27B C22B 111.1(12) . . ? C29B C27B C22B 115.1(16) . . ? C28B C27B H27B 100.9 . . ? C29B C27B H27B 100.9 . . ? C22B C27B H27B 100.9 . . ? C27B C28B H28A 109.5 . . ? C27B C28B H28B 109.5 . . ? H28A C28B H28B 109.5 . . ? C27B C28B H28C 109.5 . . ? H28A C28B H28C 109.5 . . ? H28B C28B H28C 109.5 . . ? C27B C29B H29D 109.5 . . ? C27B C29B H29E 109.5 . . ? H29D C29B H29E 109.5 . . ? C27B C29B H29F 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? C26A C30 C31 112.4(7) . . ? C26A C30 C32B 128.4(9) . . ? C31 C30 C32B 107.5(7) . . ? C26A C30 C26B 7.2(5) . . ? C31 C30 C26B 119.6(6) . . ? C32B C30 C26B 123.1(8) . . ? C26A C30 C32A 100.8(9) . . ? C31 C30 C32A 103.4(8) . . ? C32B C30 C32A 37.6(7) . . ? C26B C30 C32A 98.6(8) . . ? C26A C30 H30 113.1 . . ? C31 C30 H30 113.1 . . ? C32B C30 H30 77.7 . . ? C26B C30 H30 108.2 . . ? C32A C30 H30 113.1 . . ? 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 . . ? C30 C32A H32A 109.5 . . ? C30 C32A H32B 109.5 . . ? C30 C32A H32C 109.5 . . ? C30 C32B H32D 109.5 . . ? C30 C32B H32E 109.5 . . ? H32D C32B H32E 109.5 . . ? C30 C32B H32F 109.5 . . ? H32D C32B H32F 109.5 . . ? H32E C32B H32F 109.5 . . ? C1S N1S C1S 105(4) 16_655 15_565 ? C1S N1S C1S 68(2) 16_655 . ? C1S N1S C1S 68(2) 15_565 . ? C1S N1S C1S 68(2) 16_655 2_665 ? C1S N1S C1S 68(2) 15_565 2_665 ? C1S N1S C1S 105(4) . 2_665 ? C1S N1S Co1 127.6(19) 16_655 . ? C1S N1S Co1 127.6(19) 15_565 . ? C1S N1S Co1 127.6(19) . . ? C1S N1S Co1 127.6(19) 2_665 . ? N1S C1S C1S 55.9(10) . 16_655 ? N1S C1S C1S 55.9(10) . 15_565 ? C1S C1S C1S 90.000(9) 16_655 15_565 ? N1S C1S C2S 129(3) . . ? C1S C1S C2S 94.7(18) 16_655 . ? C1S C1S C2S 87(2) 15_565 . ? C3S C2S C1S 121(3) . . ? C3S C2S C2S 119(3) . 16_655 ? C1S C2S C2S 85.0(19) . 16_655 ? C3S C2S C2S 136(3) . 15_565 ? C1S C2S C2S 92.1(18) . 15_565 ? C2S C2S C2S 90.000(4) 16_655 15_565 ? C2S C3S C3S 120(2) . 13 ? Cl3S C4S Cl2S 125.1(14) . . ? Cl3S C4S Cl1S 112.6(12) . . ? Cl2S C4S Cl1S 111.0(13) . . ? Cl3S C4S H4S 101.3 . . ? Cl2S C4S H4S 101.3 . . ? Cl1S C4S H4S 101.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Co1 N1 C7 178.4(3) 16_655 . . . ? N1 Co1 N1 C7 -92.0(4) 2_665 . . . ? N1 Co1 N1 C7 -2.3(5) 15_565 . . . ? O3 Co1 N1 C7 -92.0(4) . . . . ? N1S Co1 N1 C7 88.0(4) . . . . ? N1 Co1 N1 C8 2.6(5) 16_655 . . 16_655 ? N1 Co1 N1 C8 92.3(4) 2_665 . . 16_655 ? N1 Co1 N1 C8 -178.0(3) 15_565 . . 16_655 ? O3 Co1 N1 C8 92.3(4) . . . 16_655 ? N1S Co1 N1 C8 -87.7(4) . . . 16_655 ? C6 C1 C2 C3 -2.6(8) . . . . ? C8 C1 C2 C3 173.2(5) 16_655 . . . ? C9 O1 C3 C2 2.7(7) . . . . ? C9 O1 C3 C4 -175.7(4) . . . . ? C1 C2 C3 O1 -176.6(5) . . . . ? C1 C2 C3 C4 1.7(7) . . . . ? C21B O2 C4 C5 12.6(8) . . . . ? C21A O2 C4 C5 -0.9(7) . . . . ? C21B O2 C4 C3 -169.1(5) . . . . ? C21A O2 C4 C3 177.3(5) . . . . ? O1 C3 C4 O2 1.0(6) . . . . ? C2 C3 C4 O2 -177.5(4) . . . . ? O1 C3 C4 C5 179.3(5) . . . . ? C2 C3 C4 C5 0.8(8) . . . . ? O2 C4 C5 C6 175.8(5) . . . . ? C3 C4 C5 C6 -2.4(8) . . . . ? C4 C5 C6 C1 1.5(8) . . . . ? C4 C5 C6 C7 -171.0(5) . . . . ? C2 C1 C6 C5 1.0(8) . . . . ? C8 C1 C6 C5 -175.8(5) 16_655 . . . ? C2 C1 C6 C7 175.0(5) . . . . ? C8 C1 C6 C7 -1.8(5) 16_655 . . . ? C8 N2 C7 N1 0.1(8) . . . . ? C8 N2 C7 C6 177.9(5) . . . . ? C8 N1 C7 N2 177.8(5) 16_655 . . . ? Co1 N1 C7 N2 1.4(7) . . . . ? C8 N1 C7 C6 -0.2(5) 16_655 . . . ? Co1 N1 C7 C6 -176.6(3) . . . . ? C5 C6 C7 N2 -3.6(8) . . . . ? C1 C6 C7 N2 -176.9(5) . . . . ? C5 C6 C7 N1 174.6(5) . . . . ? C1 C6 C7 N1 1.3(6) . . . . ? C7 N2 C8 N1 0.4(8) . . . 15_565 ? C7 N2 C8 C1 -177.0(5) . . . 15_565 ? C3 O1 C9 C10 84.4(5) . . . . ? C3 O1 C9 C14 -100.8(5) . . . . ? C14 C9 C10 C11 0.2(7) . . . . ? O1 C9 C10 C11 174.6(4) . . . . ? C14 C9 C10 C15 -177.4(5) . . . . ? O1 C9 C10 C15 -3.1(7) . . . . ? C9 C10 C11 C12 0.4(8) . . . . ? C15 C10 C11 C12 178.0(5) . . . . ? C10 C11 C12 C13 -0.5(10) . . . . ? C11 C12 C13 C14 0.0(10) . . . . ? C10 C9 C14 C13 -0.7(8) . . . . ? O1 C9 C14 C13 -175.1(5) . . . . ? C10 C9 C14 C18 175.5(5) . . . . ? O1 C9 C14 C18 1.1(7) . . . . ? C12 C13 C14 C9 0.6(9) . . . . ? C12 C13 C14 C18 -175.5(6) . . . . ? C9 C10 C15 C16 74.1(6) . . . . ? C11 C10 C15 C16 -103.5(6) . . . . ? C9 C10 C15 C17 -162.2(5) . . . . ? C11 C10 C15 C17 20.2(7) . . . . ? C9 C14 C18 C19 158.5(6) . . . . ? C13 C14 C18 C19 -25.6(9) . . . . ? C9 C14 C18 C20 -77.0(7) . . . . ? C13 C14 C18 C20 99.0(7) . . . . ? C21B O2 C21A C22A 14(3) . . . . ? C4 O2 C21A C22A 100.2(5) . . . . ? C21B O2 C21A C26A -165(3) . . . . ? C4 O2 C21A C26A -79.3(6) . . . . ? O2 C21A C22A C23A -179.6(7) . . . . ? C26A C21A C22A C23A 0.0 . . . . ? O2 C21A C22A C27A -3.5(8) . . . . ? C26A C21A C22A C27A 176.1(8) . . . . ? C21A C22A C23A C24A 0.0 . . . . ? C27A C22A C23A C24A -176.2(8) . . . . ? C22A C23A C24A C25A 0.0 . . . . ? C23A C24A C25A C26A 0.0 . . . . ? C24A C25A C26A C30 175.3(7) . . . . ? C24A C25A C26A C21A 0.0 . . . . ? O2 C21A C26A C30 4.7(8) . . . . ? C22A C21A C26A C30 -174.9(8) . . . . ? O2 C21A C26A C25A 179.6(7) . . . . ? C22A C21A C26A C25A 0.0 . . . . ? C4 O2 C21B C22B 97.9(6) . . . . ? C21A O2 C21B C22B -162(3) . . . . ? C4 O2 C21B C26B -82.6(6) . . . . ? C21A O2 C21B C26B 17(3) . . . . ? O2 C21B C22B C23B 179.5(7) . . . . ? C26B C21B C22B C23B 0.0 . . . . ? O2 C21B C22B C27B 0.1(9) . . . . ? C26B C21B C22B C27B -179.4(9) . . . . ? C21B C22B C23B C24B 0.0 . . . . ? C27B C22B C23B C24B 179.4(9) . . . . ? C22B C23B C24B C25B 0.0 . . . . ? C23B C24B C25B C26B 0.0 . . . . ? C24B C25B C26B C21B 0.0 . . . . ? C24B C25B C26B C30 -175.1(7) . . . . ? O2 C21B C26B C25B -179.5(7) . . . . ? C22B C21B C26B C25B 0.0 . . . . ? O2 C21B C26B C30 -4.1(7) . . . . ? C22B C21B C26B C30 175.4(6) . . . . ? C21A C22A C27A C29A -158.9(10) . . . . ? C23A C22A C27A C29A 17.2(13) . . . . ? C21A C22A C27A C28A 72.5(11) . . . . ? C23A C22A C27A C28A -111.4(11) . . . . ? C21B C22B C27B C28B 117.6(12) . . . . ? C23B C22B C27B C28B -61.8(15) . . . . ? C21B C22B C27B C29B -96.4(17) . . . . ? C23B C22B C27B C29B 84.2(17) . . . . ? C25A C26A C30 C31 74.4(8) . . . . ? C21A C26A C30 C31 -110.5(7) . . . . ? C25A C26A C30 C32B -63.6(11) . . . . ? C21A C26A C30 C32B 111.5(10) . . . . ? C25A C26A C30 C26B -108(3) . . . . ? C21A C26A C30 C26B 67(3) . . . . ? C25A C26A C30 C32A -35.1(9) . . . . ? C21A C26A C30 C32A 140.0(8) . . . . ? C25B C26B C30 C26A 71(3) . . . . ? C21B C26B C30 C26A -104(3) . . . . ? C25B C26B C30 C31 73.6(8) . . . . ? C21B C26B C30 C31 -101.7(7) . . . . ? C25B C26B C30 C32B -68.1(10) . . . . ? C21B C26B C30 C32B 116.7(9) . . . . ? C25B C26B C30 C32A -37.2(9) . . . . ? C21B C26B C30 C32A 147.5(8) . . . . ? N1 Co1 N1S C1S 104(2) 16_655 . . 16_655 ? N1 Co1 N1S C1S 14(2) 2_665 . . 16_655 ? N1 Co1 N1S C1S -166(2) . . . 16_655 ? N1 Co1 N1S C1S -76(2) 15_565 . . 16_655 ? O3 Co1 N1S C1S 48(100) . . . 16_655 ? N1 Co1 N1S C1S -76(2) 16_655 . . 15_565 ? N1 Co1 N1S C1S -166(2) 2_665 . . 15_565 ? N1 Co1 N1S C1S 14(2) . . . 15_565 ? N1 Co1 N1S C1S 104(2) 15_565 . . 15_565 ? O3 Co1 N1S C1S -132(100) . . . 15_565 ? N1 Co1 N1S C1S 14(2) 16_655 . . . ? N1 Co1 N1S C1S -76(2) 2_665 . . . ? N1 Co1 N1S C1S 104(2) . . . . ? N1 Co1 N1S C1S -166(2) 15_565 . . . ? O3 Co1 N1S C1S -42(100) . . . . ? N1 Co1 N1S C1S -166(2) 16_655 . . 2_665 ? N1 Co1 N1S C1S 104(2) 2_665 . . 2_665 ? N1 Co1 N1S C1S -76(2) . . . 2_665 ? N1 Co1 N1S C1S 14(2) 15_565 . . 2_665 ? O3 Co1 N1S C1S 138(100) . . . 2_665 ? C1S N1S C1S C1S -117(2) 15_565 . . 16_655 ? C1S N1S C1S C1S -58.6(11) 2_665 . . 16_655 ? Co1 N1S C1S C1S 121.4(11) . . . 16_655 ? C1S N1S C1S C1S 117(2) 16_655 . . 15_565 ? C1S N1S C1S C1S 58.6(11) 2_665 . . 15_565 ? Co1 N1S C1S C1S -121.4(11) . . . 15_565 ? C1S N1S C1S C2S 65(3) 16_655 . . . ? C1S N1S C1S C2S -52(3) 15_565 . . . ? C1S N1S C1S C2S 7(3) 2_665 . . . ? Co1 N1S C1S C2S -173(3) . . . . ? N1S C1S C2S C3S -177(4) . . . . ? C1S C1S C2S C3S -128(3) 16_655 . . . ? C1S C1S C2S C3S 142(3) 15_565 . . . ? N1S C1S C2S C2S -56(4) . . . 16_655 ? C1S C1S C2S C2S -7(3) 16_655 . . 16_655 ? C1S C1S C2S C2S -97(3) 15_565 . . 16_655 ? N1S C1S C2S C2S 34(4) . . . 15_565 ? C1S C1S C2S C2S 83(3) 16_655 . . 15_565 ? C1S C1S C2S C2S -7(3) 15_565 . . 15_565 ? C1S C2S C3S C3S 177(4) . . . 13 ? C2S C2S C3S C3S 75(5) 16_655 . . 13 ? C2S C2S C3S C3S -50(6) 15_565 . . 13 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.18 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.772 _refine_diff_density_min -1.434 _refine_diff_density_rms 0.226 data_copo21 _database_code_depnum_ccdc_archive 'CCDC 900380' #TrackingRef '900380_PCCo.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C128 H144 Co N8 O8, 2(C H Cl3)' _chemical_formula_sum 'C130 H146 Cl6 Co N8 O8' _chemical_formula_weight 2220.18 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 21.336(8) _cell_length_b 16.819(6) _cell_length_c 18.474(7) _cell_angle_alpha 90.00 _cell_angle_beta 114.455(5) _cell_angle_gamma 90.00 _cell_volume 6035(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9624 _cell_measurement_theta_min 1.8799 _cell_measurement_theta_max 25.6062 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2350 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.807 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details 'Jacobson, R. (1998) Private communication' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.68890 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Station I19, Diamond' _diffrn_radiation_monochromator silicon _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean 28.5714 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27489 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.0631 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 22.50 _reflns_number_total 8610 _reflns_number_gt 7766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1069P)^2^+6.5640P] 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 8610 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0732 _refine_ls_R_factor_gt 0.0684 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1882 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.026 _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 1.0000 1.0000 0.5000 0.0253(2) Uani 1 2 d S . . O1 O 1.27414(11) 0.77500(14) 0.39710(14) 0.0445(6) Uani 1 1 d . . . O2 O 1.16400(12) 0.71063(15) 0.29637(15) 0.0521(7) Uani 1 1 d . . . O3 O 0.72216(11) 0.70465(13) 0.22306(13) 0.0415(6) Uani 1 1 d . . . O4 O 0.64095(10) 0.80218(13) 0.25188(13) 0.0406(5) Uani 1 1 d . . . N1 N 1.17009(12) 0.98684(14) 0.54571(14) 0.0283(5) Uani 1 1 d . . . N2 N 1.05636(12) 0.93305(14) 0.46833(13) 0.0266(5) Uani 1 1 d . . . N3 N 0.96994(12) 0.84730(14) 0.37400(14) 0.0311(6) Uani 1 1 d . . . N4 N 0.91922(11) 0.94490(14) 0.43021(13) 0.0270(5) Uani 1 1 d . . . C1 C 1.12673(14) 0.93715(17) 0.49300(16) 0.0271(6) Uani 1 1 d . . . C2 C 1.14879(15) 0.87950(17) 0.45027(17) 0.0303(6) Uani 1 1 d . . . C3 C 1.21297(15) 0.85917(19) 0.45329(18) 0.0337(7) Uani 1 1 d . . . H3 H 1.2530 0.8835 0.4890 0.040 Uiso 1 1 calc R . . C4 C 1.21504(16) 0.8016(2) 0.40130(19) 0.0376(7) Uani 1 1 d . . . C5 C 1.15467(16) 0.7654(2) 0.3462(2) 0.0396(8) Uani 1 1 d . . . C6 C 1.09113(16) 0.7844(2) 0.34424(19) 0.0387(8) Uani 1 1 d . . . H6 H 1.0511 0.7601 0.3086 0.046 Uiso 1 1 calc R . . C7 C 1.08966(15) 0.84144(18) 0.39787(17) 0.0314(7) Uani 1 1 d . . . C8 C 1.03309(15) 0.87446(17) 0.41154(16) 0.0292(6) Uani 1 1 d . . . C9 C 0.91821(14) 0.87991(17) 0.38477(17) 0.0290(6) Uani 1 1 d . . . C10 C 0.84885(15) 0.84965(18) 0.34528(17) 0.0319(7) Uani 1 1 d . . . C11 C 0.82356(16) 0.78275(19) 0.29805(19) 0.0363(7) Uani 1 1 d . . . H11 H 0.8525 0.7487 0.2863 0.044 Uiso 1 1 calc R . . C12 C 0.75393(15) 0.76907(19) 0.26940(18) 0.0351(7) Uani 1 1 d . . . C13 C 0.71026(15) 0.82234(19) 0.28519(18) 0.0349(7) Uani 1 1 d . . . C14 C 0.73594(15) 0.88766(18) 0.33357(17) 0.0326(7) Uani 1 1 d . . . H14 H 0.7071 0.9220 0.3451 0.039 Uiso 1 1 calc R . . C15 C 0.80679(15) 0.90017(17) 0.36445(17) 0.0304(7) Uani 1 1 d . . . C16 C 0.85206(14) 0.95862(17) 0.41919(16) 0.0283(6) Uani 1 1 d . . . C17 C 1.33800(16) 0.7931(2) 0.4605(2) 0.0407(8) Uani 1 1 d . . . C18 C 1.37308(17) 0.8592(2) 0.4516(2) 0.0437(8) Uani 1 1 d . . . C19 C 1.43920(18) 0.8708(2) 0.5111(2) 0.0521(9) Uani 1 1 d . . . H19 H 1.4650 0.9143 0.5082 0.063 Uiso 1 1 calc R . . C20 C 1.46664(19) 0.8186(3) 0.5741(2) 0.0623(11) Uani 1 1 d . . . H20 H 1.5113 0.8260 0.6122 0.075 Uiso 1 1 calc R . . C21 C 1.4282(2) 0.7556(3) 0.5809(2) 0.0607(10) Uani 1 1 d . . . H21 H 1.4471 0.7217 0.6244 0.073 Uiso 1 1 calc R . . C22 C 1.36245(19) 0.7417(2) 0.5246(2) 0.0514(9) Uani 1 1 d . . . C23 C 1.34055(19) 0.9138(2) 0.3810(2) 0.0511(9) Uani 1 1 d . . . H23 H 1.2928 0.9220 0.3735 0.061 Uiso 1 1 calc R . . C24 C 1.3376(2) 0.8768(3) 0.3049(2) 0.0609(10) Uani 1 1 d . . . H24A H 1.3835 0.8675 0.3096 0.091 Uiso 1 1 calc R . . H24B H 1.3142 0.9122 0.2612 0.091 Uiso 1 1 calc R . . H24C H 1.3131 0.8273 0.2956 0.091 Uiso 1 1 calc R . . C25 C 1.3739(2) 0.9959(2) 0.3938(3) 0.0656(12) Uani 1 1 d . . . H25A H 1.3774 1.0172 0.4435 0.098 Uiso 1 1 calc R . . H25B H 1.3463 1.0306 0.3513 0.098 Uiso 1 1 calc R . . H25C H 1.4191 0.9915 0.3947 0.098 Uiso 1 1 calc R . . C26 C 1.3170(2) 0.6749(3) 0.5311(3) 0.0660(11) Uani 1 1 d . . . H26 H 1.2693 0.6922 0.5016 0.079 Uiso 1 1 calc R . . C27 C 1.3264(4) 0.6603(4) 0.6160(4) 0.108(2) Uani 1 1 d . . . H27A H 1.2918 0.6239 0.6161 0.163 Uiso 1 1 calc R . . H27B H 1.3222 0.7097 0.6397 0.163 Uiso 1 1 calc R . . H27C H 1.3712 0.6380 0.6460 0.163 Uiso 1 1 calc R . . C28 C 1.3254(4) 0.6021(3) 0.4932(4) 0.102(2) Uani 1 1 d . . . H28A H 1.3707 0.5811 0.5225 0.154 Uiso 1 1 calc R . . H28B H 1.3191 0.6137 0.4397 0.154 Uiso 1 1 calc R . . H28C H 1.2918 0.5638 0.4923 0.154 Uiso 1 1 calc R . . C29 C 1.10481(17) 0.6762(2) 0.2382(2) 0.0445(8) Uani 1 1 d . . . C30 C 1.0817(2) 0.6043(2) 0.2563(2) 0.0521(9) Uani 1 1 d . . . C31 C 1.0221(2) 0.5715(2) 0.1966(2) 0.0553(10) Uani 1 1 d . . . H31 H 1.0047 0.5239 0.2062 0.066 Uiso 1 1 calc R . . C32 C 0.9896(2) 0.6084(2) 0.1249(2) 0.0524(9) Uani 1 1 d . . . H32 H 0.9501 0.5857 0.0863 0.063 Uiso 1 1 calc R . . C33 C 1.0140(2) 0.6778(2) 0.1090(2) 0.0522(9) Uani 1 1 d . . . H33 H 0.9911 0.7013 0.0594 0.063 Uiso 1 1 calc R . . C34 C 1.0725(2) 0.7149(2) 0.1654(2) 0.0501(9) Uani 1 1 d . . . C35 C 1.1174(3) 0.5635(3) 0.3355(3) 0.0744(13) Uani 1 1 d . . . H35 H 1.1606 0.5917 0.3656 0.089 Uiso 1 1 calc R . . C36 C 1.1349(3) 0.4774(3) 0.3260(3) 0.0921(17) Uani 1 1 d . . . H36A H 1.0933 0.4486 0.2962 0.138 Uiso 1 1 calc R . . H36B H 1.1582 0.4536 0.3775 0.138 Uiso 1 1 calc R . . H36C H 1.1642 0.4759 0.2982 0.138 Uiso 1 1 calc R . . C37 C 1.0737(4) 0.5681(4) 0.3826(3) 0.114(2) Uani 1 1 d . . . H37A H 1.0584 0.6218 0.3823 0.171 Uiso 1 1 calc R . . H37B H 1.1006 0.5516 0.4365 0.171 Uiso 1 1 calc R . . H37C H 1.0345 0.5337 0.3589 0.171 Uiso 1 1 calc R . . C38 C 1.0986(2) 0.7921(3) 0.1469(3) 0.0663(11) Uani 1 1 d . . . H38 H 1.1348 0.8115 0.1966 0.080 Uiso 1 1 calc R . . C39 C 1.1310(4) 0.7788(4) 0.0893(4) 0.116(2) Uani 1 1 d . . . H39A H 1.1658 0.7385 0.1098 0.173 Uiso 1 1 calc R . . H39B H 1.1514 0.8274 0.0825 0.173 Uiso 1 1 calc R . . H39C H 1.0963 0.7620 0.0390 0.173 Uiso 1 1 calc R . . C40 C 1.0420(4) 0.8540(3) 0.1193(6) 0.142(3) Uani 1 1 d . . . H40A H 1.0617 0.9056 0.1207 0.212 Uiso 1 1 calc R . . H40B H 1.0185 0.8535 0.1539 0.212 Uiso 1 1 calc R . . H40C H 1.0099 0.8421 0.0660 0.212 Uiso 1 1 calc R . . C41 C 0.76395(16) 0.6397(2) 0.2252(2) 0.0413(8) Uani 1 1 d . . . C42 C 0.7787(2) 0.5850(2) 0.2866(2) 0.0537(9) Uani 1 1 d . . . C43 C 0.8153(2) 0.5179(3) 0.2826(3) 0.0683(12) Uani 1 1 d . . . H43 H 0.8257 0.4792 0.3218 0.082 Uiso 1 1 calc R . . C44 C 0.8365(2) 0.5071(2) 0.2225(3) 0.0682(13) Uani 1 1 d . . . H44 H 0.8609 0.4616 0.2214 0.082 Uiso 1 1 calc R . . C45 C 0.8218(2) 0.5638(2) 0.1637(3) 0.0564(10) Uani 1 1 d . . . H45 H 0.8363 0.5558 0.1232 0.068 Uiso 1 1 calc R . . C46 C 0.78570(18) 0.6324(2) 0.1639(2) 0.0464(8) Uani 1 1 d . . . C47 C 0.7545(3) 0.6001(3) 0.3521(3) 0.0701(12) Uani 1 1 d . . . H47 H 0.7619 0.6568 0.3653 0.084 Uiso 1 1 calc R . . C48 C 0.7943(4) 0.5554(4) 0.4273(4) 0.111(2) Uani 1 1 d . . . H48A H 0.7848 0.4996 0.4184 0.166 Uiso 1 1 calc R . . H48B H 0.7810 0.5734 0.4682 0.166 Uiso 1 1 calc R . . H48C H 0.8427 0.5646 0.4435 0.166 Uiso 1 1 calc R . . C49 C 0.6767(3) 0.5847(3) 0.3239(3) 0.0825(14) Uani 1 1 d . . . H49A H 0.6515 0.6162 0.2777 0.124 Uiso 1 1 calc R . . H49B H 0.6628 0.5987 0.3655 0.124 Uiso 1 1 calc R . . H49C H 0.6672 0.5294 0.3111 0.124 Uiso 1 1 calc R . . C50 C 0.7707(2) 0.6961(3) 0.1012(2) 0.0589(10) Uani 1 1 d . . . H50 H 0.7510 0.7414 0.1179 0.071 Uiso 1 1 calc R . . C51 C 0.8334(4) 0.7254(5) 0.0939(6) 0.160(4) Uani 1 1 d . . . H51A H 0.8641 0.6817 0.0999 0.240 Uiso 1 1 calc R . . H51B H 0.8560 0.7642 0.1346 0.240 Uiso 1 1 calc R . . H51C H 0.8208 0.7493 0.0426 0.240 Uiso 1 1 calc R . . C52 C 0.7198(6) 0.6710(6) 0.0242(4) 0.186(5) Uani 1 1 d . . . H52A H 0.7041 0.7164 -0.0103 0.279 Uiso 1 1 calc R . . H52B H 0.6816 0.6470 0.0304 0.279 Uiso 1 1 calc R . . H52C H 0.7402 0.6332 0.0014 0.279 Uiso 1 1 calc R . . C53 C 0.59470(16) 0.8653(2) 0.2208(2) 0.0435(8) Uani 1 1 d . . . C54 C 0.58457(19) 0.8944(2) 0.1464(2) 0.0543(10) Uani 1 1 d . . . C55 C 0.5368(2) 0.9565(3) 0.1174(3) 0.0735(13) Uani 1 1 d . . . H55 H 0.5289 0.9790 0.0684 0.088 Uiso 1 1 calc R . . C56 C 0.5012(2) 0.9850(3) 0.1593(4) 0.0806(15) Uani 1 1 d . . . H56 H 0.4701 1.0265 0.1387 0.097 Uiso 1 1 calc R . . C57 C 0.5114(2) 0.9524(3) 0.2311(3) 0.0698(13) Uani 1 1 d . . . H57 H 0.4868 0.9719 0.2587 0.084 Uiso 1 1 calc R . . C58 C 0.55833(17) 0.8901(2) 0.2636(2) 0.0505(9) Uani 1 1 d . . . C59 C 0.6223(2) 0.8617(3) 0.0997(2) 0.0612(10) Uani 1 1 d . . . H59 H 0.6418 0.8103 0.1233 0.073 Uiso 1 1 calc R . . C60 C 0.6816(3) 0.9146(3) 0.1076(3) 0.0861(15) Uani 1 1 d . . . H60A H 0.7054 0.8922 0.0784 0.129 Uiso 1 1 calc R . . H60B H 0.7126 0.9191 0.1627 0.129 Uiso 1 1 calc R . . H60C H 0.6645 0.9663 0.0869 0.129 Uiso 1 1 calc R . . C61 C 0.5752(3) 0.8467(4) 0.0143(3) 0.1006(18) Uani 1 1 d . . . H61A H 0.5378 0.8133 0.0116 0.151 Uiso 1 1 calc R . . H61B H 0.6003 0.8208 -0.0118 0.151 Uiso 1 1 calc R . . H61C H 0.5573 0.8963 -0.0117 0.151 Uiso 1 1 calc R . . C62 C 0.5672(2) 0.8478(3) 0.3385(2) 0.0670(12) Uani 1 1 d . . . H62 H 0.6156 0.8320 0.3652 0.080 Uiso 1 1 calc R . . C63 C 0.5249(3) 0.7727(4) 0.3185(3) 0.0902(17) Uani 1 1 d . . . H63A H 0.4778 0.7852 0.2850 0.135 Uiso 1 1 calc R . . H63B H 0.5273 0.7482 0.3666 0.135 Uiso 1 1 calc R . . H63C H 0.5425 0.7366 0.2912 0.135 Uiso 1 1 calc R . . C64 C 0.5514(3) 0.9000(5) 0.3966(3) 0.114(2) Uani 1 1 d . . . H64A H 0.5035 0.9139 0.3736 0.172 Uiso 1 1 calc R . . H64B H 0.5787 0.9476 0.4073 0.172 Uiso 1 1 calc R . . H64C H 0.5622 0.8715 0.4453 0.172 Uiso 1 1 calc R . . Cl1 Cl 0.74570(7) 0.09874(9) 0.26559(9) 0.0882(4) Uani 1 1 d . . . Cl2 Cl 0.64219(9) 0.11288(11) 0.32621(9) 0.1051(5) Uani 1 1 d . . . Cl3 Cl 0.61134(8) 0.15418(8) 0.16329(9) 0.0914(4) Uani 1 1 d . . . C1S C 0.6586(2) 0.0918(3) 0.2434(3) 0.0663(11) Uani 1 1 d . . . H1S H 0.6441 0.0369 0.2272 0.080 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 0.0158(3) 0.0306(3) 0.0239(3) -0.0037(2) 0.0026(2) 0.0004(2) O1 0.0242(12) 0.0595(15) 0.0485(13) -0.0178(11) 0.0139(11) 0.0022(10) O2 0.0303(13) 0.0655(16) 0.0587(15) -0.0335(13) 0.0167(12) -0.0041(11) O3 0.0267(12) 0.0417(13) 0.0471(13) -0.0175(10) 0.0063(10) -0.0069(9) O4 0.0182(11) 0.0483(13) 0.0443(13) -0.0082(10) 0.0020(10) -0.0046(9) N1 0.0182(12) 0.0344(13) 0.0272(12) -0.0028(10) 0.0043(11) 0.0002(10) N2 0.0187(12) 0.0304(13) 0.0260(12) -0.0007(10) 0.0047(10) 0.0006(10) N3 0.0203(13) 0.0355(14) 0.0322(13) -0.0080(11) 0.0055(11) -0.0031(10) N4 0.0193(12) 0.0316(13) 0.0256(12) -0.0020(10) 0.0046(10) 0.0012(10) C1 0.0201(14) 0.0310(15) 0.0263(14) 0.0008(12) 0.0056(12) 0.0007(12) C2 0.0240(15) 0.0344(16) 0.0288(15) -0.0031(12) 0.0073(13) -0.0007(12) C3 0.0199(15) 0.0429(18) 0.0334(16) -0.0077(13) 0.0060(13) -0.0037(13) C4 0.0250(16) 0.0458(19) 0.0412(18) -0.0097(15) 0.0131(14) 0.0027(14) C5 0.0305(17) 0.0466(19) 0.0420(18) -0.0171(15) 0.0152(15) -0.0021(14) C6 0.0248(16) 0.0479(19) 0.0383(17) -0.0147(15) 0.0081(14) -0.0041(14) C7 0.0241(15) 0.0366(16) 0.0304(15) -0.0067(13) 0.0083(13) -0.0010(12) C8 0.0225(16) 0.0334(16) 0.0263(14) -0.0022(12) 0.0048(12) -0.0014(12) C9 0.0205(15) 0.0334(16) 0.0270(14) -0.0033(12) 0.0037(12) -0.0011(12) C10 0.0208(15) 0.0359(17) 0.0316(15) -0.0048(13) 0.0035(13) -0.0017(12) C11 0.0247(16) 0.0396(18) 0.0395(17) -0.0085(14) 0.0082(14) -0.0009(13) C12 0.0227(16) 0.0398(18) 0.0329(16) -0.0078(13) 0.0017(13) -0.0057(13) C13 0.0196(15) 0.0430(18) 0.0335(16) -0.0027(14) 0.0024(13) -0.0038(13) C14 0.0207(15) 0.0385(17) 0.0331(16) -0.0051(13) 0.0056(13) 0.0004(12) C15 0.0223(15) 0.0354(16) 0.0270(15) -0.0028(12) 0.0037(12) -0.0013(12) C16 0.0221(15) 0.0327(16) 0.0262(14) 0.0007(12) 0.0061(12) 0.0016(12) C17 0.0225(16) 0.055(2) 0.0412(18) -0.0120(16) 0.0098(14) 0.0020(14) C18 0.0283(17) 0.057(2) 0.0455(19) -0.0099(16) 0.0147(15) 0.0024(15) C19 0.0309(19) 0.070(2) 0.053(2) -0.0098(19) 0.0154(18) -0.0060(17) C20 0.030(2) 0.095(3) 0.050(2) -0.007(2) 0.0051(18) 0.005(2) C21 0.044(2) 0.077(3) 0.053(2) 0.006(2) 0.0116(19) 0.014(2) C22 0.040(2) 0.058(2) 0.051(2) -0.0013(18) 0.0147(18) 0.0087(17) C23 0.037(2) 0.063(2) 0.049(2) -0.0035(18) 0.0138(17) 0.0043(17) C24 0.055(2) 0.072(3) 0.054(2) 0.002(2) 0.021(2) 0.005(2) C25 0.059(3) 0.058(3) 0.075(3) 0.002(2) 0.022(2) 0.0087(19) C26 0.055(3) 0.061(3) 0.069(3) 0.007(2) 0.013(2) 0.000(2) C27 0.153(6) 0.098(4) 0.113(5) -0.024(4) 0.094(5) -0.036(4) C28 0.134(6) 0.082(4) 0.119(5) -0.020(3) 0.080(5) -0.021(3) C29 0.0339(18) 0.050(2) 0.050(2) -0.0254(17) 0.0180(16) -0.0046(15) C30 0.049(2) 0.059(2) 0.043(2) -0.0139(17) 0.0139(18) 0.0008(18) C31 0.055(2) 0.056(2) 0.054(2) -0.0191(18) 0.021(2) -0.0153(19) C32 0.046(2) 0.055(2) 0.047(2) -0.0192(18) 0.0105(18) -0.0098(18) C33 0.053(2) 0.055(2) 0.043(2) -0.0173(17) 0.0147(18) -0.0018(18) C34 0.050(2) 0.053(2) 0.048(2) -0.0180(17) 0.0209(18) -0.0038(17) C35 0.079(3) 0.072(3) 0.054(2) -0.006(2) 0.009(2) -0.003(2) C36 0.096(4) 0.090(4) 0.074(3) 0.010(3) 0.019(3) 0.029(3) C37 0.185(7) 0.102(4) 0.069(3) 0.017(3) 0.068(4) 0.034(4) C38 0.075(3) 0.059(3) 0.060(2) -0.014(2) 0.023(2) -0.018(2) C39 0.178(7) 0.084(4) 0.132(5) -0.010(4) 0.111(6) -0.030(4) C40 0.114(5) 0.052(3) 0.235(9) 0.013(4) 0.049(6) 0.002(3) C41 0.0279(17) 0.0399(18) 0.0480(19) -0.0150(15) 0.0076(15) -0.0075(14) C42 0.048(2) 0.047(2) 0.059(2) -0.0056(18) 0.0148(19) -0.0054(17) C43 0.071(3) 0.050(2) 0.077(3) 0.002(2) 0.024(3) 0.001(2) C44 0.061(3) 0.045(2) 0.097(4) -0.015(2) 0.031(3) 0.0015(18) C45 0.043(2) 0.054(2) 0.071(3) -0.018(2) 0.023(2) -0.0037(18) C46 0.0333(18) 0.049(2) 0.051(2) -0.0166(16) 0.0117(16) -0.0074(15) C47 0.084(3) 0.066(3) 0.064(3) -0.001(2) 0.033(3) -0.004(2) C48 0.133(6) 0.119(5) 0.084(4) 0.025(4) 0.049(4) 0.009(4) C49 0.084(4) 0.084(3) 0.099(4) -0.007(3) 0.058(3) -0.011(3) C50 0.051(2) 0.074(3) 0.051(2) -0.0038(19) 0.0203(19) 0.012(2) C51 0.108(6) 0.142(7) 0.241(10) 0.112(7) 0.084(6) 0.014(5) C52 0.244(11) 0.180(8) 0.059(4) 0.018(4) -0.014(5) -0.117(8) C53 0.0197(16) 0.054(2) 0.0419(19) -0.0094(16) -0.0023(14) -0.0027(14) C54 0.034(2) 0.063(2) 0.049(2) 0.0022(18) 0.0015(17) -0.0007(17) C55 0.055(3) 0.075(3) 0.069(3) 0.015(2) 0.003(2) 0.010(2) C56 0.044(3) 0.075(3) 0.100(4) 0.004(3) 0.008(3) 0.020(2) C57 0.033(2) 0.087(3) 0.081(3) -0.019(3) 0.015(2) 0.009(2) C58 0.0217(17) 0.069(2) 0.049(2) -0.0145(18) 0.0019(15) -0.0001(16) C59 0.063(3) 0.069(3) 0.045(2) 0.0043(19) 0.016(2) -0.001(2) C60 0.095(4) 0.087(4) 0.086(3) 0.005(3) 0.047(3) -0.011(3) C61 0.100(4) 0.123(5) 0.060(3) -0.005(3) 0.015(3) 0.005(4) C62 0.0286(19) 0.116(4) 0.050(2) -0.012(2) 0.0096(17) -0.001(2) C63 0.057(3) 0.129(5) 0.074(3) 0.022(3) 0.016(3) -0.011(3) C64 0.057(3) 0.212(8) 0.074(3) -0.034(4) 0.027(3) 0.015(4) Cl1 0.0659(8) 0.1025(10) 0.0966(9) 0.0218(7) 0.0339(7) -0.0062(7) Cl2 0.1113(12) 0.1334(13) 0.0892(9) -0.0400(9) 0.0601(9) -0.0278(10) Cl3 0.0888(9) 0.0745(8) 0.0996(10) 0.0209(7) 0.0274(8) 0.0180(7) C1S 0.071(3) 0.060(3) 0.072(3) -0.001(2) 0.033(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 N2 1.908(2) . ? Co1 N2 1.908(2) 3_776 ? Co1 N4 1.911(2) . ? Co1 N4 1.911(2) 3_776 ? O1 C4 1.370(4) . ? O1 C17 1.414(4) . ? O2 C5 1.373(4) . ? O2 C29 1.401(4) . ? O3 C12 1.373(4) . ? O3 C41 1.400(4) . ? O4 C13 1.388(4) . ? O4 C53 1.401(4) . ? N1 C16 1.319(4) 3_776 ? N1 C1 1.325(4) . ? N2 C8 1.374(4) . ? N2 C1 1.378(4) . ? N3 C8 1.316(4) . ? N3 C9 1.319(4) . ? N4 C9 1.373(4) . ? N4 C16 1.381(4) . ? C1 C2 1.447(4) . ? C2 C7 1.388(4) . ? C2 C3 1.390(4) . ? C3 C4 1.377(4) . ? C3 H3 0.9300 . ? C4 C5 1.408(5) . ? C5 C6 1.379(4) . ? C6 C7 1.389(4) . ? C6 H6 0.9300 . ? C7 C8 1.443(4) . ? C9 C10 1.445(4) . ? C10 C15 1.384(4) . ? C10 C11 1.389(4) . ? C11 C12 1.375(4) . ? C11 H11 0.9300 . ? C12 C13 1.408(5) . ? C13 C14 1.379(4) . ? C14 C15 1.393(4) . ? C14 H14 0.9300 . ? C15 C16 1.454(4) . ? C16 N1 1.319(4) 3_776 ? C17 C22 1.382(5) . ? C17 C18 1.388(5) . ? C18 C19 1.397(5) . ? C18 C23 1.509(5) . ? C19 C20 1.380(6) . ? C19 H19 0.9300 . ? C20 C21 1.377(6) . ? C20 H20 0.9300 . ? C21 C22 1.378(6) . ? C21 H21 0.9300 . ? C22 C26 1.521(6) . ? C23 C24 1.514(5) . ? C23 C25 1.526(6) . ? C23 H23 0.9800 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 C28 1.457(7) . ? C26 C27 1.516(7) . ? C26 H26 0.9800 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 C34 1.393(5) . ? C29 C30 1.397(5) . ? C30 C31 1.405(5) . ? C30 C35 1.507(6) . ? C31 C32 1.365(6) . ? C31 H31 0.9300 . ? C32 C33 1.358(6) . ? C32 H32 0.9300 . ? C33 C34 1.399(5) . ? C33 H33 0.9300 . ? C34 C38 1.506(6) . ? C35 C37 1.517(8) . ? C35 C36 1.523(7) . ? C35 H35 0.9800 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 C39 1.505(7) . ? C38 C40 1.514(8) . ? C38 H38 0.9800 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.392(5) . ? C41 C46 1.396(5) . ? C42 C43 1.391(6) . ? C42 C47 1.522(6) . ? C43 C44 1.374(7) . ? C43 H43 0.9300 . ? C44 C45 1.380(6) . ? C44 H44 0.9300 . ? C45 C46 1.389(5) . ? C45 H45 0.9300 . ? C46 C50 1.512(6) . ? C47 C48 1.496(7) . ? C47 C49 1.543(7) . ? C47 H47 0.9800 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? C49 H49A 0.9600 . ? C49 H49B 0.9600 . ? C49 H49C 0.9600 . ? C50 C52 1.449(7) . ? C50 C51 1.484(7) . ? C50 H50 0.9800 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C53 C58 1.381(5) . ? C53 C54 1.389(5) . ? C54 C55 1.402(6) . ? C54 C59 1.507(6) . ? C55 C56 1.375(7) . ? C55 H55 0.9300 . ? C56 C57 1.366(7) . ? C56 H56 0.9300 . ? C57 C58 1.401(6) . ? C57 H57 0.9300 . ? C58 C62 1.497(6) . ? C59 C61 1.501(6) . ? C59 C60 1.502(7) . ? C59 H59 0.9800 . ? C60 H60A 0.9600 . ? C60 H60B 0.9600 . ? C60 H60C 0.9600 . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 C63 1.508(7) . ? C62 C64 1.527(7) . ? C62 H62 0.9800 . ? C63 H63A 0.9600 . ? C63 H63B 0.9600 . ? C63 H63C 0.9600 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? Cl1 C1S 1.734(5) . ? Cl2 C1S 1.740(5) . ? Cl3 C1S 1.753(5) . ? C1S H1S 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 N2 Co1 N2 179.999(1) . 3_776 ? N2 Co1 N4 90.79(10) . . ? N2 Co1 N4 89.21(10) 3_776 . ? N2 Co1 N4 89.21(10) . 3_776 ? N2 Co1 N4 90.79(10) 3_776 3_776 ? N4 Co1 N4 179.999(1) . 3_776 ? C4 O1 C17 118.4(2) . . ? C5 O2 C29 117.2(2) . . ? C12 O3 C41 117.0(2) . . ? C13 O4 C53 115.9(2) . . ? C16 N1 C1 121.1(3) 3_776 . ? C8 N2 C1 106.8(2) . . ? C8 N2 Co1 125.68(19) . . ? C1 N2 Co1 127.42(19) . . ? C8 N3 C9 120.9(3) . . ? C9 N4 C16 106.9(2) . . ? C9 N4 Co1 125.46(19) . . ? C16 N4 Co1 127.56(19) . . ? N1 C1 N2 127.4(3) . . ? N1 C1 C2 122.5(3) . . ? N2 C1 C2 110.0(2) . . ? C7 C2 C3 120.7(3) . . ? C7 C2 C1 106.4(3) . . ? C3 C2 C1 132.9(3) . . ? C4 C3 C2 117.4(3) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? O1 C4 C3 124.4(3) . . ? O1 C4 C5 113.9(3) . . ? C3 C4 C5 121.7(3) . . ? O2 C5 C6 123.5(3) . . ? O2 C5 C4 115.6(3) . . ? C6 C5 C4 120.9(3) . . ? C5 C6 C7 117.0(3) . . ? C5 C6 H6 121.5 . . ? C7 C6 H6 121.5 . . ? C2 C7 C6 122.2(3) . . ? C2 C7 C8 106.6(2) . . ? C6 C7 C8 131.2(3) . . ? N3 C8 N2 128.3(3) . . ? N3 C8 C7 121.5(3) . . ? N2 C8 C7 110.2(2) . . ? N3 C9 N4 128.4(3) . . ? N3 C9 C10 121.6(3) . . ? N4 C9 C10 110.0(2) . . ? C15 C10 C11 122.3(3) . . ? C15 C10 C9 107.0(3) . . ? C11 C10 C9 130.8(3) . . ? C12 C11 C10 117.0(3) . . ? C12 C11 H11 121.5 . . ? C10 C11 H11 121.5 . . ? O3 C12 C11 123.2(3) . . ? O3 C12 C13 115.7(3) . . ? C11 C12 C13 121.1(3) . . ? C14 C13 O4 123.1(3) . . ? C14 C13 C12 121.5(3) . . ? O4 C13 C12 115.3(3) . . ? C13 C14 C15 117.3(3) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? C10 C15 C14 120.7(3) . . ? C10 C15 C16 106.2(3) . . ? C14 C15 C16 133.1(3) . . ? N1 C16 N4 127.2(3) 3_776 . ? N1 C16 C15 122.8(3) 3_776 . ? N4 C16 C15 109.9(2) . . ? C22 C17 C18 124.9(3) . . ? C22 C17 O1 117.9(3) . . ? C18 C17 O1 117.1(3) . . ? C17 C18 C19 115.9(3) . . ? C17 C18 C23 120.8(3) . . ? C19 C18 C23 123.3(3) . . ? C20 C19 C18 120.8(4) . . ? C20 C19 H19 119.6 . . ? C18 C19 H19 119.6 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 121.4(4) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? C21 C22 C17 116.5(4) . . ? C21 C22 C26 123.3(4) . . ? C17 C22 C26 120.2(3) . . ? C18 C23 C24 112.4(3) . . ? C18 C23 C25 113.4(3) . . ? C24 C23 C25 110.7(3) . . ? C18 C23 H23 106.6 . . ? C24 C23 H23 106.6 . . ? C25 C23 H23 106.6 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C28 C26 C27 111.8(4) . . ? C28 C26 C22 111.9(4) . . ? C27 C26 C22 112.7(4) . . ? C28 C26 H26 106.6 . . ? C27 C26 H26 106.6 . . ? C22 C26 H26 106.6 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C34 C29 C30 123.6(3) . . ? C34 C29 O2 118.4(3) . . ? C30 C29 O2 118.0(3) . . ? C29 C30 C31 116.5(4) . . ? C29 C30 C35 122.7(4) . . ? C31 C30 C35 120.8(4) . . ? C32 C31 C30 121.0(4) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C33 C32 C31 120.9(4) . . ? C33 C32 H32 119.6 . . ? C31 C32 H32 119.6 . . ? C32 C33 C34 121.8(4) . . ? C32 C33 H33 119.1 . . ? C34 C33 H33 119.1 . . ? C29 C34 C33 116.2(4) . . ? C29 C34 C38 122.7(3) . . ? C33 C34 C38 121.0(4) . . ? C30 C35 C37 110.5(4) . . ? C30 C35 C36 111.7(4) . . ? C37 C35 C36 110.7(5) . . ? C30 C35 H35 107.9 . . ? C37 C35 H35 107.9 . . ? C36 C35 H35 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C35 C37 H37A 109.5 . . ? C35 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C35 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C39 C38 C34 110.6(4) . . ? C39 C38 C40 113.6(6) . . ? C34 C38 C40 110.5(4) . . ? C39 C38 H38 107.3 . . ? C34 C38 H38 107.3 . . ? C40 C38 H38 107.3 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 124.3(3) . . ? C42 C41 O3 117.7(3) . . ? C46 C41 O3 117.9(3) . . ? C43 C42 C41 115.9(4) . . ? C43 C42 C47 124.1(4) . . ? C41 C42 C47 120.0(3) . . ? C44 C43 C42 121.9(4) . . ? C44 C43 H43 119.0 . . ? C42 C43 H43 119.0 . . ? C43 C44 C45 120.1(4) . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 121.2(4) . . ? C44 C45 H45 119.4 . . ? C46 C45 H45 119.4 . . ? C45 C46 C41 116.5(4) . . ? C45 C46 C50 122.0(3) . . ? C41 C46 C50 121.5(3) . . ? C48 C47 C42 113.9(4) . . ? C48 C47 C49 110.3(5) . . ? C42 C47 C49 112.1(4) . . ? C48 C47 H47 106.7 . . ? C42 C47 H47 106.7 . . ? C49 C47 H47 106.7 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C47 C49 H49A 109.5 . . ? C47 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C47 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C52 C50 C51 110.2(6) . . ? C52 C50 C46 112.4(4) . . ? C51 C50 C46 113.0(4) . . ? C52 C50 H50 107.0 . . ? C51 C50 H50 107.0 . . ? C46 C50 H50 107.0 . . ? C50 C51 H51A 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C50 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50 C52 H52A 109.5 . . ? C50 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C50 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C58 C53 C54 124.5(3) . . ? C58 C53 O4 117.5(3) . . ? C54 C53 O4 117.8(3) . . ? C53 C54 C55 115.5(4) . . ? C53 C54 C59 122.5(3) . . ? C55 C54 C59 122.0(4) . . ? C56 C55 C54 121.9(5) . . ? C56 C55 H55 119.1 . . ? C54 C55 H55 119.1 . . ? C57 C56 C55 120.2(4) . . ? C57 C56 H56 119.9 . . ? C55 C56 H56 119.9 . . ? C56 C57 C58 121.0(4) . . ? C56 C57 H57 119.5 . . ? C58 C57 H57 119.5 . . ? C53 C58 C57 116.8(4) . . ? C53 C58 C62 120.0(3) . . ? C57 C58 C62 123.1(4) . . ? C61 C59 C60 111.9(4) . . ? C61 C59 C54 112.3(4) . . ? C60 C59 C54 110.8(4) . . ? C61 C59 H59 107.2 . . ? C60 C59 H59 107.2 . . ? C54 C59 H59 107.2 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C59 C61 H61A 109.5 . . ? C59 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C59 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C58 C62 C63 109.8(4) . . ? C58 C62 C64 113.3(5) . . ? C63 C62 C64 111.8(4) . . ? C58 C62 H62 107.2 . . ? C63 C62 H62 107.2 . . ? C64 C62 H62 107.2 . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Cl1 C1S Cl2 111.4(3) . . ? Cl1 C1S Cl3 110.1(2) . . ? Cl2 C1S Cl3 111.5(3) . . ? Cl1 C1S H1S 107.9 . . ? Cl2 C1S H1S 107.9 . . ? Cl3 C1S H1S 107.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Co1 N2 C8 170(26) 3_776 . . . ? N4 Co1 N2 C8 3.0(2) . . . . ? N4 Co1 N2 C8 -177.0(2) 3_776 . . . ? N2 Co1 N2 C1 -15(26) 3_776 . . . ? N4 Co1 N2 C1 178.0(2) . . . . ? N4 Co1 N2 C1 -2.0(2) 3_776 . . . ? N2 Co1 N4 C9 3.2(2) . . . . ? N2 Co1 N4 C9 -176.8(2) 3_776 . . . ? N4 Co1 N4 C9 -175(8) 3_776 . . . ? N2 Co1 N4 C16 178.8(2) . . . . ? N2 Co1 N4 C16 -1.2(2) 3_776 . . . ? N4 Co1 N4 C16 1(8) 3_776 . . . ? C16 N1 C1 N2 -1.1(5) 3_776 . . . ? C16 N1 C1 C2 176.6(3) 3_776 . . . ? C8 N2 C1 N1 178.1(3) . . . . ? Co1 N2 C1 N1 2.3(4) . . . . ? C8 N2 C1 C2 0.2(3) . . . . ? Co1 N2 C1 C2 -175.59(19) . . . . ? N1 C1 C2 C7 -176.9(3) . . . . ? N2 C1 C2 C7 1.2(3) . . . . ? N1 C1 C2 C3 2.8(5) . . . . ? N2 C1 C2 C3 -179.1(3) . . . . ? C7 C2 C3 C4 1.5(5) . . . . ? C1 C2 C3 C4 -178.2(3) . . . . ? C17 O1 C4 C3 15.2(5) . . . . ? C17 O1 C4 C5 -165.6(3) . . . . ? C2 C3 C4 O1 -179.8(3) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C29 O2 C5 C6 3.6(5) . . . . ? C29 O2 C5 C4 -177.0(3) . . . . ? O1 C4 C5 O2 -1.1(5) . . . . ? C3 C4 C5 O2 178.2(3) . . . . ? O1 C4 C5 C6 178.4(3) . . . . ? C3 C4 C5 C6 -2.4(5) . . . . ? O2 C5 C6 C7 -179.5(3) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? C3 C2 C7 C6 -2.8(5) . . . . ? C1 C2 C7 C6 177.0(3) . . . . ? C3 C2 C7 C8 178.3(3) . . . . ? C1 C2 C7 C8 -2.0(3) . . . . ? C5 C6 C7 C2 1.4(5) . . . . ? C5 C6 C7 C8 -179.9(3) . . . . ? C9 N3 C8 N2 4.6(5) . . . . ? C9 N3 C8 C7 -177.5(3) . . . . ? C1 N2 C8 N3 176.6(3) . . . . ? Co1 N2 C8 N3 -7.5(4) . . . . ? C1 N2 C8 C7 -1.5(3) . . . . ? Co1 N2 C8 C7 174.40(19) . . . . ? C2 C7 C8 N3 -176.0(3) . . . . ? C6 C7 C8 N3 5.1(5) . . . . ? C2 C7 C8 N2 2.2(3) . . . . ? C6 C7 C8 N2 -176.6(3) . . . . ? C8 N3 C9 N4 3.0(5) . . . . ? C8 N3 C9 C10 -178.6(3) . . . . ? C16 N4 C9 N3 176.8(3) . . . . ? Co1 N4 C9 N3 -6.9(4) . . . . ? C16 N4 C9 C10 -1.7(3) . . . . ? Co1 N4 C9 C10 174.66(19) . . . . ? N3 C9 C10 C15 -175.6(3) . . . . ? N4 C9 C10 C15 3.0(3) . . . . ? N3 C9 C10 C11 6.1(5) . . . . ? N4 C9 C10 C11 -175.3(3) . . . . ? C15 C10 C11 C12 1.1(5) . . . . ? C9 C10 C11 C12 179.2(3) . . . . ? C41 O3 C12 C11 19.4(5) . . . . ? C41 O3 C12 C13 -161.7(3) . . . . ? C10 C11 C12 O3 -179.0(3) . . . . ? C10 C11 C12 C13 2.2(5) . . . . ? C53 O4 C13 C14 42.7(4) . . . . ? C53 O4 C13 C12 -140.3(3) . . . . ? O3 C12 C13 C14 177.3(3) . . . . ? C11 C12 C13 C14 -3.8(5) . . . . ? O3 C12 C13 O4 0.2(4) . . . . ? C11 C12 C13 O4 179.1(3) . . . . ? O4 C13 C14 C15 178.7(3) . . . . ? C12 C13 C14 C15 1.8(5) . . . . ? C11 C10 C15 C14 -3.0(5) . . . . ? C9 C10 C15 C14 178.5(3) . . . . ? C11 C10 C15 C16 175.5(3) . . . . ? C9 C10 C15 C16 -2.9(3) . . . . ? C13 C14 C15 C10 1.5(4) . . . . ? C13 C14 C15 C16 -176.6(3) . . . . ? C9 N4 C16 N1 176.8(3) . . . 3_776 ? Co1 N4 C16 N1 0.6(4) . . . 3_776 ? C9 N4 C16 C15 -0.2(3) . . . . ? Co1 N4 C16 C15 -176.43(19) . . . . ? C10 C15 C16 N1 -175.1(3) . . . 3_776 ? C14 C15 C16 N1 3.2(5) . . . 3_776 ? C10 C15 C16 N4 2.0(3) . . . . ? C14 C15 C16 N4 -179.7(3) . . . . ? C4 O1 C17 C22 87.3(4) . . . . ? C4 O1 C17 C18 -96.0(4) . . . . ? C22 C17 C18 C19 3.1(5) . . . . ? O1 C17 C18 C19 -173.3(3) . . . . ? C22 C17 C18 C23 -177.4(3) . . . . ? O1 C17 C18 C23 6.2(4) . . . . ? C17 C18 C19 C20 0.1(5) . . . . ? C23 C18 C19 C20 -179.4(3) . . . . ? C18 C19 C20 C21 -2.3(6) . . . . ? C19 C20 C21 C22 1.6(6) . . . . ? C20 C21 C22 C17 1.4(6) . . . . ? C20 C21 C22 C26 -177.5(4) . . . . ? C18 C17 C22 C21 -3.8(5) . . . . ? O1 C17 C22 C21 172.6(3) . . . . ? C18 C17 C22 C26 175.1(3) . . . . ? O1 C17 C22 C26 -8.5(5) . . . . ? C17 C18 C23 C24 -73.0(4) . . . . ? C19 C18 C23 C24 106.5(4) . . . . ? C17 C18 C23 C25 160.4(3) . . . . ? C19 C18 C23 C25 -20.0(5) . . . . ? C21 C22 C26 C28 -90.9(5) . . . . ? C17 C22 C26 C28 90.3(5) . . . . ? C21 C22 C26 C27 36.1(6) . . . . ? C17 C22 C26 C27 -142.7(4) . . . . ? C5 O2 C29 C34 87.4(4) . . . . ? C5 O2 C29 C30 -93.0(4) . . . . ? C34 C29 C30 C31 -0.6(5) . . . . ? O2 C29 C30 C31 179.9(3) . . . . ? C34 C29 C30 C35 -179.9(4) . . . . ? O2 C29 C30 C35 0.5(5) . . . . ? C29 C30 C31 C32 0.4(5) . . . . ? C35 C30 C31 C32 179.8(4) . . . . ? C30 C31 C32 C33 0.3(6) . . . . ? C31 C32 C33 C34 -0.9(6) . . . . ? C30 C29 C34 C33 0.0(5) . . . . ? O2 C29 C34 C33 179.5(3) . . . . ? C30 C29 C34 C38 -179.6(4) . . . . ? O2 C29 C34 C38 -0.1(5) . . . . ? C32 C33 C34 C29 0.8(5) . . . . ? C32 C33 C34 C38 -179.6(4) . . . . ? C29 C30 C35 C37 109.7(5) . . . . ? C31 C30 C35 C37 -69.6(6) . . . . ? C29 C30 C35 C36 -126.6(5) . . . . ? C31 C30 C35 C36 54.1(6) . . . . ? C29 C34 C38 C39 107.3(5) . . . . ? C33 C34 C38 C39 -72.3(6) . . . . ? C29 C34 C38 C40 -126.0(5) . . . . ? C33 C34 C38 C40 54.4(6) . . . . ? C12 O3 C41 C42 83.9(4) . . . . ? C12 O3 C41 C46 -98.7(3) . . . . ? C46 C41 C42 C43 -2.6(5) . . . . ? O3 C41 C42 C43 174.6(3) . . . . ? C46 C41 C42 C47 177.9(3) . . . . ? O3 C41 C42 C47 -4.9(5) . . . . ? C41 C42 C43 C44 1.1(6) . . . . ? C47 C42 C43 C44 -179.5(4) . . . . ? C42 C43 C44 C45 0.1(7) . . . . ? C43 C44 C45 C46 0.2(7) . . . . ? C44 C45 C46 C41 -1.6(5) . . . . ? C44 C45 C46 C50 178.4(4) . . . . ? C42 C41 C46 C45 2.9(5) . . . . ? O3 C41 C46 C45 -174.3(3) . . . . ? C42 C41 C46 C50 -177.1(3) . . . . ? O3 C41 C46 C50 5.7(5) . . . . ? C43 C42 C47 C48 22.2(7) . . . . ? C41 C42 C47 C48 -158.4(5) . . . . ? C43 C42 C47 C49 -103.8(5) . . . . ? C41 C42 C47 C49 75.6(5) . . . . ? C45 C46 C50 C52 71.0(7) . . . . ? C41 C46 C50 C52 -109.1(7) . . . . ? C45 C46 C50 C51 -54.5(7) . . . . ? C41 C46 C50 C51 125.4(6) . . . . ? C13 O4 C53 C58 -105.9(3) . . . . ? C13 O4 C53 C54 79.1(4) . . . . ? C58 C53 C54 C55 4.1(6) . . . . ? O4 C53 C54 C55 178.7(3) . . . . ? C58 C53 C54 C59 -175.9(4) . . . . ? O4 C53 C54 C59 -1.3(5) . . . . ? C53 C54 C55 C56 -1.6(6) . . . . ? C59 C54 C55 C56 178.4(4) . . . . ? C54 C55 C56 C57 -0.5(8) . . . . ? C55 C56 C57 C58 0.4(7) . . . . ? C54 C53 C58 C57 -4.3(5) . . . . ? O4 C53 C58 C57 -178.9(3) . . . . ? C54 C53 C58 C62 172.4(4) . . . . ? O4 C53 C58 C62 -2.3(5) . . . . ? C56 C57 C58 C53 1.8(6) . . . . ? C56 C57 C58 C62 -174.7(4) . . . . ? C53 C54 C59 C61 133.7(4) . . . . ? C55 C54 C59 C61 -46.3(6) . . . . ? C53 C54 C59 C60 -100.3(5) . . . . ? C55 C54 C59 C60 79.6(5) . . . . ? C53 C58 C62 C63 -80.0(5) . . . . ? C57 C58 C62 C63 96.4(5) . . . . ? C53 C58 C62 C64 154.2(4) . . . . ? C57 C58 C62 C64 -29.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.849 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.068