# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H36 N2 O15' _chemical_formula_weight 904.81 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.277(2) _cell_length_b 11.987(3) _cell_length_c 12.828(3) _cell_angle_alpha 68.347(4) _cell_angle_beta 81.383(4) _cell_angle_gamma 76.412(4) _cell_volume 1008.4(4) _cell_formula_units_Z 1 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2874 _cell_measurement_theta_min 2.9 _cell_measurement_theta_max 25.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 470 _exptl_absorpt_coefficient_mu 0.111 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9557 _exptl_absorpt_correction_T_max 0.9900 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5325 _diffrn_reflns_av_R_equivalents 0.0960 _diffrn_reflns_av_sigmaI/netI 0.0644 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3493 _reflns_number_gt 3254 _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, 1997)' _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^)+(0.1064P)^2^+0.6274P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3493 _refine_ls_number_parameters 319 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.2009 _refine_ls_wR_factor_gt 0.1964 _refine_ls_goodness_of_fit_ref 1.136 _refine_ls_restrained_S_all 1.136 _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 O5 O 0.2376(3) 0.91352(17) 0.66978(16) 0.0293(5) Uani 1 1 d . . . O1 O 0.0541(3) 0.67201(19) 1.05945(17) 0.0345(5) Uani 1 1 d . . . O4 O 0.2297(3) 1.01801(17) 0.44712(16) 0.0313(5) Uani 1 1 d . . . N1 N 0.2981(3) 0.1380(2) 0.6031(2) 0.0256(5) Uani 1 1 d . . . O2 O 0.0480(3) 0.82128(18) 0.84955(17) 0.0312(5) Uani 1 1 d . . . O6 O 0.0669(3) 0.57356(17) 0.64032(16) 0.0282(5) Uani 1 1 d . . . C20 C 0.1362(3) 0.6563(2) 0.4051(2) 0.0251(6) Uani 1 1 d . . . H008 H 0.1096 0.5763 0.4398 0.030 Uiso 1 1 calc R . . C13 C 0.1886(3) 0.7285(2) 0.6632(2) 0.0233(6) Uani 1 1 d . . . C16 C 0.1872(3) 0.8424(2) 0.4181(2) 0.0233(6) Uani 1 1 d . . . C14 C 0.1321(3) 0.6676(2) 0.5966(2) 0.0233(6) Uani 1 1 d . . . C3 C 0.2085(3) 0.6588(2) 0.7838(2) 0.0233(6) Uani 1 1 d . . . C11 C 0.2070(3) 0.9119(2) 0.4890(2) 0.0251(6) Uani 1 1 d . . . C17 C 0.2053(4) 0.8931(3) 0.3018(2) 0.0284(6) Uani 1 1 d . . . H014 H 0.2268 0.9743 0.2662 0.034 Uiso 1 1 calc R . . C5 C 0.3298(4) 0.4536(3) 0.9356(2) 0.0254(6) Uani 1 1 d . . . C10 C 0.4278(4) 0.3335(3) 0.9649(2) 0.0300(6) Uani 1 1 d . . . H016 H 0.4955 0.3035 0.9083 0.036 Uiso 1 1 calc R . . C8 C 0.3294(4) 0.3006(3) 1.1593(2) 0.0368(7) Uani 1 1 d . . . H017 H 0.3285 0.2477 1.2357 0.044 Uiso 1 1 calc R . . C15 C 0.1523(3) 0.7230(2) 0.4711(2) 0.0233(6) Uani 1 1 d . . . C1 C 0.1358(4) 0.6278(3) 0.9889(2) 0.0276(6) Uani 1 1 d . . . C21 C 0.2864(4) 0.1609(3) 0.6984(2) 0.0286(6) Uani 1 1 d . . . H020 H 0.2558 0.1015 0.7682 0.034 Uiso 1 1 calc R . . C2 C 0.1353(4) 0.7056(3) 0.8673(2) 0.0271(6) Uani 1 1 d . . . C19 C 0.1589(4) 0.7061(3) 0.2892(2) 0.0293(6) Uani 1 1 d . . . H023 H 0.1518 0.6592 0.2448 0.035 Uiso 1 1 calc R . . C6 C 0.2328(4) 0.4978(3) 1.0197(2) 0.0269(6) Uani 1 1 d . . . C24 C 0.3714(4) 0.3306(3) 0.4957(2) 0.0285(6) Uani 1 1 d . . . H025 H 0.4002 0.3889 0.4248 0.034 Uiso 1 1 calc R . . C18 C 0.1918(4) 0.8243(3) 0.2376(2) 0.0324(7) Uani 1 1 d . . . H026 H 0.2053 0.8584 0.1579 0.039 Uiso 1 1 calc R . . C12 C 0.2097(4) 0.8488(2) 0.6143(2) 0.0248(6) Uani 1 1 d . . . C23 C 0.3631(4) 0.3558(2) 0.5923(3) 0.0292(6) Uani 1 1 d . . . H028 H 0.3877 0.4316 0.5888 0.035 Uiso 1 1 calc R . . C9 C 0.4275(4) 0.2571(3) 1.0763(3) 0.0351(7) Uani 1 1 d . . . H029 H 0.4945 0.1747 1.0959 0.042 Uiso 1 1 calc R . . C25 C 0.3375(4) 0.2197(2) 0.5023(2) 0.0266(6) Uani 1 1 d . . . H030 H 0.3420 0.2013 0.4359 0.032 Uiso 1 1 calc R . . C22 C 0.3188(4) 0.2706(3) 0.6954(3) 0.0308(6) Uani 1 1 d . . . H031 H 0.3109 0.2877 0.7628 0.037 Uiso 1 1 calc R . . C7 C 0.2331(4) 0.4205(3) 1.1315(2) 0.0311(6) Uani 1 1 d . . . H033 H 0.1669 0.4501 1.1887 0.037 Uiso 1 1 calc R . . O3 O 0.4289(3) 0.49929(17) 0.74345(16) 0.0287(5) Uani 1 1 d . . . C4 C 0.3271(3) 0.5347(2) 0.8150(2) 0.0230(6) Uani 1 1 d . . . O8 O 0.8661(4) 0.9244(2) 0.0357(2) 0.0455(6) Uani 1 1 d . . . O7 O 0.4944(7) 0.9758(5) 0.0495(5) 0.0578(14) Uani 0.50 1 d P . . H100 H 0.286(5) 0.061(4) 0.608(3) 0.046(10) Uiso 1 1 d . . . H101 H 0.093(6) 0.865(4) 0.780(4) 0.059(12) Uiso 1 1 d . . . H102 H 0.903(7) 0.875(5) 0.009(4) 0.069(15) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O5 0.0342(11) 0.0250(10) 0.0323(10) -0.0126(8) 0.0043(8) -0.0122(8) O1 0.0360(11) 0.0389(12) 0.0325(11) -0.0194(9) 0.0102(9) -0.0111(9) O4 0.0322(11) 0.0246(10) 0.0350(11) -0.0072(8) 0.0040(8) -0.0108(8) N1 0.0200(11) 0.0224(12) 0.0358(13) -0.0116(10) 0.0021(9) -0.0067(9) O2 0.0323(11) 0.0266(10) 0.0333(11) -0.0132(9) 0.0097(8) -0.0062(8) O6 0.0260(10) 0.0271(10) 0.0335(10) -0.0126(8) 0.0059(8) -0.0107(8) C20 0.0174(12) 0.0262(13) 0.0316(14) -0.0116(11) 0.0005(10) -0.0029(10) C13 0.0174(12) 0.0231(13) 0.0301(14) -0.0125(11) 0.0076(10) -0.0059(10) C16 0.0134(11) 0.0237(13) 0.0301(14) -0.0095(11) 0.0033(10) -0.0016(10) C14 0.0138(12) 0.0219(13) 0.0319(14) -0.0097(11) 0.0057(10) -0.0032(10) C3 0.0184(12) 0.0276(14) 0.0276(13) -0.0127(11) 0.0055(10) -0.0107(11) C11 0.0145(12) 0.0210(13) 0.0368(15) -0.0097(11) 0.0065(10) -0.0033(10) C17 0.0205(13) 0.0294(14) 0.0318(14) -0.0081(12) 0.0024(11) -0.0054(11) C5 0.0189(12) 0.0306(14) 0.0295(14) -0.0118(12) 0.0045(10) -0.0117(11) C10 0.0227(13) 0.0310(15) 0.0376(15) -0.0129(12) 0.0014(11) -0.0083(12) C8 0.0376(16) 0.0410(17) 0.0291(15) -0.0039(13) -0.0004(12) -0.0171(14) C15 0.0102(11) 0.0266(13) 0.0324(14) -0.0125(11) 0.0045(10) -0.0024(10) C1 0.0231(13) 0.0380(16) 0.0287(14) -0.0159(12) 0.0071(11) -0.0175(12) C21 0.0234(13) 0.0284(14) 0.0331(15) -0.0107(12) 0.0031(11) -0.0065(11) C2 0.0187(12) 0.0298(14) 0.0341(15) -0.0130(12) 0.0054(10) -0.0087(11) C19 0.0214(13) 0.0358(15) 0.0337(15) -0.0175(12) -0.0003(11) -0.0033(11) C6 0.0210(13) 0.0335(15) 0.0301(14) -0.0118(12) 0.0032(10) -0.0144(11) C24 0.0213(13) 0.0251(14) 0.0362(15) -0.0088(12) 0.0068(11) -0.0075(11) C18 0.0264(14) 0.0408(17) 0.0276(14) -0.0109(12) 0.0021(11) -0.0062(12) C12 0.0168(12) 0.0254(14) 0.0324(14) -0.0126(11) 0.0063(10) -0.0051(10) C23 0.0169(12) 0.0237(13) 0.0492(17) -0.0160(12) 0.0040(11) -0.0065(11) C9 0.0309(15) 0.0307(15) 0.0396(16) -0.0067(13) -0.0036(12) -0.0066(12) C25 0.0208(13) 0.0284(14) 0.0316(14) -0.0133(11) 0.0062(10) -0.0070(11) C22 0.0260(14) 0.0319(15) 0.0389(16) -0.0185(13) 0.0012(12) -0.0059(12) C7 0.0247(14) 0.0418(17) 0.0317(15) -0.0143(13) 0.0060(11) -0.0180(12) O3 0.0271(10) 0.0279(10) 0.0314(10) -0.0134(8) 0.0080(8) -0.0069(8) C4 0.0170(12) 0.0255(13) 0.0295(14) -0.0108(11) 0.0042(10) -0.0117(10) O8 0.0453(14) 0.0407(13) 0.0498(14) -0.0230(12) 0.0015(11) 0.0016(11) O7 0.033(2) 0.060(4) 0.080(4) -0.026(3) 0.003(3) -0.009(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 O5 C12 1.295(3) . ? O1 C1 1.224(3) . ? O4 C11 1.225(3) . ? N1 C21 1.336(4) . ? N1 C25 1.341(4) . ? O2 C2 1.332(3) . ? O6 C14 1.231(3) . ? C20 C19 1.382(4) . ? C20 C15 1.394(4) . ? C13 C12 1.379(4) . ? C13 C14 1.463(4) . ? C13 C3 1.472(4) . ? C16 C17 1.386(4) . ? C16 C15 1.406(4) . ? C16 C11 1.483(4) . ? C14 C15 1.496(4) . ? C3 C2 1.371(4) . ? C3 C4 1.476(4) . ? C11 C12 1.504(4) . ? C17 C18 1.389(4) . ? C5 C10 1.386(4) . ? C5 C6 1.401(4) . ? C5 C4 1.493(4) . ? C10 C9 1.384(4) . ? C8 C7 1.381(5) . ? C8 C9 1.387(4) . ? C1 C6 1.481(4) . ? C1 C2 1.493(4) . ? C21 C22 1.375(4) . ? C19 C18 1.387(4) . ? C6 C7 1.391(4) . ? C24 C23 1.370(4) . ? C24 C25 1.378(4) . ? C23 C22 1.388(4) . ? O3 C4 1.228(3) . ? O7 O7 1.184(11) 2_675 ? 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 C21 N1 C25 122.3(2) . . ? C19 C20 C15 120.3(3) . . ? C12 C13 C14 120.1(2) . . ? C12 C13 C3 122.7(2) . . ? C14 C13 C3 117.1(2) . . ? C17 C16 C15 120.5(3) . . ? C17 C16 C11 120.9(2) . . ? C15 C16 C11 118.6(2) . . ? O6 C14 C13 122.2(2) . . ? O6 C14 C15 119.3(2) . . ? C13 C14 C15 118.5(2) . . ? C2 C3 C13 123.9(2) . . ? C2 C3 C4 118.5(2) . . ? C13 C3 C4 117.5(2) . . ? O4 C11 C16 121.3(2) . . ? O4 C11 C12 119.4(2) . . ? C16 C11 C12 119.3(2) . . ? C16 C17 C18 119.5(3) . . ? C10 C5 C6 119.5(3) . . ? C10 C5 C4 120.1(2) . . ? C6 C5 C4 120.4(2) . . ? C9 C10 C5 120.4(3) . . ? C7 C8 C9 120.2(3) . . ? C20 C15 C16 119.0(2) . . ? C20 C15 C14 120.1(2) . . ? C16 C15 C14 120.9(2) . . ? O1 C1 C6 122.1(2) . . ? O1 C1 C2 119.5(3) . . ? C6 C1 C2 118.3(2) . . ? N1 C21 C22 120.0(3) . . ? O2 C2 C3 124.4(3) . . ? O2 C2 C1 113.2(2) . . ? C3 C2 C1 122.3(3) . . ? C20 C19 C18 120.3(3) . . ? C7 C6 C5 119.8(3) . . ? C7 C6 C1 120.7(3) . . ? C5 C6 C1 119.5(2) . . ? C23 C24 C25 119.3(3) . . ? C19 C18 C17 120.4(3) . . ? O5 C12 C13 123.9(2) . . ? O5 C12 C11 115.6(2) . . ? C13 C12 C11 120.5(2) . . ? C24 C23 C22 120.0(3) . . ? C10 C9 C8 120.0(3) . . ? N1 C25 C24 119.6(3) . . ? C21 C22 C23 118.8(3) . . ? C8 C7 C6 120.1(3) . . ? O3 C4 C3 120.7(2) . . ? O3 C4 C5 119.7(2) . . ? C3 C4 C5 119.6(2) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.433 _refine_diff_density_min -0.412 _refine_diff_density_rms 0.103 _database_code_depnum_ccdc_archive 'CCDC 965089' ####################################################################### # # 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_compound_1 # start Validation Reply Form _vrf_THETM01_compound_1 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Crystals were found to be weakly diffracting and failed to provide reflections at high angles in theta. This is largely attributed to the presence of significant regions of disordered solvent molecules in the crystal. ; _vrf_PLAT051_compound_1 ; PROBLEM: Mu(calc) and Mu(CIF) Ratio Differs from 1.0 by . 13.19 % RESPONSE: The disordered solvent includes dichloromethane which could not be satisfactorily modelled. As a consequence the SQUEEZE routine within PLATON was employed. The unmodelled solvent molecules have been included in the unit cell contents but do not appear in the atom coordinate list. As a consequence there is a discrepancy between Mu(calc) and Mu(CIF). ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C108 H96 B2 Cl4 Co2 N8 O8' _chemical_formula_weight 1915.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.6851(3) _cell_length_b 20.5451(5) _cell_length_c 22.8542(7) _cell_angle_alpha 85.949(2) _cell_angle_beta 87.043(2) _cell_angle_gamma 81.098(2) _cell_volume 4477.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 10122 _cell_measurement_theta_min 2.8 _cell_measurement_theta_max 44.9 _exptl_crystal_description rod _exptl_crystal_colour red _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 4.530 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.35309 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; Crystals were found to be weakly diffracting and failed to provide reflections at high angles in theta. For this reason data was only collected to a 2theta angle of 90 degrees. ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15937 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0348 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 44.94 _reflns_number_total 6946 _reflns_number_gt 5814 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics CrystalMaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Crystals were found to be weakly diffracting and failed to provide reflections at high angles in theta. This is largely attributed to the presence of significant regions of disordered solvent molecules in the crystal. As a consequence of this disorder the SQUEEZE routine within PLATON was employed. 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^)+(0.0501P)^2^+8.7014P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6946 _refine_ls_number_parameters 1128 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0551 _refine_ls_R_factor_gt 0.0465 _refine_ls_wR_factor_ref 0.1154 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _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 C54 C 0.6846(7) 0.9181(4) 0.1353(3) 0.074(2) Uani 1 1 d . . . H54 H 0.7600 0.9051 0.1082 0.088 Uiso 1 1 calc R . . Co2 Co 0.28557(9) 0.97623(4) 0.26910(4) 0.0337(3) Uani 1 1 d . . . Co1 Co -0.08484(9) 1.37855(4) 0.23444(4) 0.0275(3) Uani 1 1 d . . . O2 O 0.0194(4) 1.28753(16) 0.23226(14) 0.0272(9) Uani 1 1 d . . . O5 O 0.2358(4) 1.07488(17) 0.26035(16) 0.0320(9) Uani 1 1 d . . . O1 O 0.1389(4) 1.38298(19) 0.27035(15) 0.0310(9) Uani 1 1 d . . . O4 O 0.1649(4) 0.9984(2) 0.18389(15) 0.0364(10) Uani 1 1 d . . . O6 O 0.1410(4) 1.2509(2) 0.11734(15) 0.0401(10) Uani 1 1 d . . . O3 O 0.4599(4) 1.1551(2) 0.23358(16) 0.0381(10) Uani 1 1 d . . . N4 N -0.0090(5) 1.4293(2) 0.16079(18) 0.0264(11) Uani 1 1 d . . . N8 N 0.4621(5) 0.9547(3) 0.2128(2) 0.0356(12) Uani 1 1 d . . . C20 C -0.0183(6) 1.1792(3) 0.0546(3) 0.0390(16) Uani 1 1 d . . . H20 H -0.0221 1.2248 0.0432 0.047 Uiso 1 1 calc R . . N5 N 0.3601(5) 0.8683(2) 0.2935(2) 0.0372(13) Uani 1 1 d . . . N7 N 0.1047(5) 0.9361(3) 0.2942(2) 0.0410(13) Uani 1 1 d . . . N6 N 0.3962(5) 0.9817(3) 0.34458(19) 0.0373(13) Uani 1 1 d . . . C7 C 0.3962(7) 1.3564(3) 0.3312(2) 0.0319(15) Uani 1 1 d . . . H7 H 0.3425 1.3984 0.3370 0.038 Uiso 1 1 calc R . . C75 C 0.7599(6) 0.6726(3) 0.3991(2) 0.0283(14) Uani 1 1 d . . . C60 C 0.7445(7) 0.4975(3) 0.5770(2) 0.0304(15) Uani 1 1 d . . . H60 H 0.7607 0.4566 0.5996 0.036 Uiso 1 1 calc R . . C262 C 0.5950(6) 0.5775(3) 0.5194(2) 0.0279(14) Uani 1 1 d . . . H262 H 0.5053 0.5907 0.5037 0.033 Uiso 1 1 calc R . . C13 C 0.1823(5) 1.1694(3) 0.1950(2) 0.0265(14) Uani 1 1 d . . . C17 C -0.0032(6) 1.0459(3) 0.0862(3) 0.0397(16) Uani 1 1 d . . . H17 H 0.0037 0.9999 0.0964 0.048 Uiso 1 1 calc R . . C40 C 0.4420(6) 0.9243(3) 0.3746(3) 0.0361(16) Uani 1 1 d . . . N1 N -0.2343(5) 1.4730(2) 0.2312(2) 0.0369(13) Uani 1 1 d . . . N3 N -0.1331(5) 1.3945(3) 0.3226(2) 0.0353(12) Uani 1 1 d . . . C28 C -0.1942(6) 1.4553(4) 0.3356(3) 0.0444(17) Uani 1 1 d . . . N2 N -0.2598(5) 1.3495(2) 0.20036(18) 0.0280(11) Uani 1 1 d . . . C12 C 0.1893(5) 1.1033(3) 0.2114(3) 0.0256(14) Uani 1 1 d . . . C3 C 0.2338(6) 1.2167(3) 0.2315(2) 0.0270(15) Uani 1 1 d . . . C22 C -0.3783(7) 1.3928(3) 0.1996(2) 0.0318(15) Uani 1 1 d . . . C27 C -0.2128(6) 1.5054(3) 0.2845(3) 0.0506(18) Uani 1 1 d . . . H27A H -0.2944 1.5395 0.2926 0.061 Uiso 1 1 calc R . . H27B H -0.1288 1.5275 0.2786 0.061 Uiso 1 1 calc R . . C5 C 0.4252(6) 1.2504(3) 0.2883(2) 0.0285(15) Uani 1 1 d . . . C77 C 0.7894(7) 0.7020(3) 0.2934(3) 0.0447(17) Uani 1 1 d . . . H77 H 0.7534 0.7265 0.2592 0.054 Uiso 1 1 calc R . . C67 C 0.2853(7) 0.7760(3) 0.4853(3) 0.0444(17) Uani 1 1 d . . . H67 H 0.2356 0.8089 0.5088 0.053 Uiso 1 1 calc R . . C15 C 0.0544(6) 1.1523(3) 0.1032(2) 0.0307(15) Uani 1 1 d . . . C26 C -0.2569(6) 1.2933(3) 0.1734(2) 0.0305(15) Uani 1 1 d . . . H26 H -0.1724 1.2628 0.1729 0.037 Uiso 1 1 calc R . . C69 C 0.7467(6) 0.7435(3) 0.4927(3) 0.0302(15) Uani 1 1 d . . . C1 C 0.2088(6) 1.3281(3) 0.2709(2) 0.0243(14) Uani 1 1 d . . . C38 C 0.1027(6) 1.4046(3) 0.1289(3) 0.0301(15) Uani 1 1 d . . . H38 H 0.1490 1.3616 0.1401 0.036 Uiso 1 1 calc R . . C33 C -0.2085(7) 1.5140(3) 0.1775(3) 0.0545(19) Uani 1 1 d . . . H33A H -0.2067 1.5597 0.1881 0.065 Uiso 1 1 calc R . . H33B H -0.2870 1.5151 0.1512 0.065 Uiso 1 1 calc R . . C8 C 0.5225(7) 1.3388(3) 0.3568(2) 0.0385(16) Uani 1 1 d . . . H8 H 0.5574 1.3692 0.3795 0.046 Uiso 1 1 calc R . . C2 C 0.1477(7) 1.2744(3) 0.2442(2) 0.0232(14) Uani 1 1 d . . . C16 C 0.0619(6) 1.0855(3) 0.1193(2) 0.0301(15) Uani 1 1 d . . . C74 C 0.7336(6) 0.7524(3) 0.5533(3) 0.0442(17) Uani 1 1 d . . . H74 H 0.6899 0.7218 0.5780 0.053 Uiso 1 1 calc R . . C56 C 0.5082(7) 0.9995(3) 0.1739(3) 0.061(2) Uani 1 1 d . . . H56 H 0.4622 1.0439 0.1730 0.073 Uiso 1 1 calc R . . C57 C 0.6983(6) 0.6176(3) 0.5064(2) 0.0259(14) Uani 1 1 d . . . C62 C 0.5092(6) 0.7100(3) 0.4558(2) 0.0286(15) Uani 1 1 d . . . C4 C 0.3773(7) 1.2034(3) 0.2491(2) 0.0295(15) Uani 1 1 d . . . C68 C 0.4289(7) 0.7582(3) 0.4890(2) 0.0367(16) Uani 1 1 d . . . H68 H 0.4756 0.7799 0.5155 0.044 Uiso 1 1 calc R . . C76 C 0.7123(6) 0.7059(3) 0.3467(3) 0.0387(16) Uani 1 1 d . . . H76 H 0.6229 0.7326 0.3474 0.046 Uiso 1 1 calc R . . C24 C -0.4920(7) 1.3226(3) 0.1464(2) 0.0406(16) Uani 1 1 d . . . H24 H -0.5718 1.3132 0.1280 0.049 Uiso 1 1 calc R . . C71 C 0.8661(7) 0.8408(3) 0.4848(3) 0.0522(18) Uani 1 1 d . . . H71 H 0.9118 0.8711 0.4605 0.063 Uiso 1 1 calc R . . C39 C 0.3777(7) 0.8656(3) 0.3571(3) 0.0469(18) Uani 1 1 d . . . H39A H 0.4388 0.8241 0.3692 0.056 Uiso 1 1 calc R . . H39B H 0.2855 0.8654 0.3778 0.056 Uiso 1 1 calc R . . C34 C -0.0744(6) 1.4899(3) 0.1450(3) 0.0351(15) Uani 1 1 d . . . C19 C -0.0858(6) 1.1398(3) 0.0225(3) 0.0459(17) Uani 1 1 d . . . H19 H -0.1372 1.1589 -0.0104 0.055 Uiso 1 1 calc R . . B1 B 0.6767(7) 0.6857(3) 0.4633(3) 0.0318(18) Uani 1 1 d . . . C79 C 0.9661(6) 0.6285(3) 0.3401(3) 0.0378(16) Uani 1 1 d . . . H79 H 1.0544 0.6009 0.3386 0.045 Uiso 1 1 calc R . . C61 C 0.6185(7) 0.5191(3) 0.5545(2) 0.0328(15) Uani 1 1 d . . . H61 H 0.5445 0.4940 0.5626 0.039 Uiso 1 1 calc R . . C9 C 0.5993(6) 1.2772(3) 0.3499(3) 0.0399(16) Uani 1 1 d . . . H9 H 0.6847 1.2648 0.3693 0.048 Uiso 1 1 calc R . . C58 C 0.8260(6) 0.5940(3) 0.5322(2) 0.0332(15) Uani 1 1 d . . . H58 H 0.8999 0.6194 0.5255 0.040 Uiso 1 1 calc R . . C23 C -0.4970(6) 1.3805(3) 0.1730(2) 0.0354(16) Uani 1 1 d . . . H23 H -0.5801 1.4119 0.1733 0.042 Uiso 1 1 calc R . . C59 C 0.8502(6) 0.5359(3) 0.5667(2) 0.0348(15) Uani 1 1 d . . . H59 H 0.9388 0.5223 0.5833 0.042 Uiso 1 1 calc R . . C47 C -0.0076(8) 0.8408(3) 0.3103(3) 0.0494(18) Uani 1 1 d . . . H47 H -0.0015 0.7941 0.3130 0.059 Uiso 1 1 calc R . . C52 C 0.5284(7) 0.8923(3) 0.2135(3) 0.0386(16) Uani 1 1 d . . . C65 C 0.2893(7) 0.6970(3) 0.4128(3) 0.0405(16) Uani 1 1 d . . . H65 H 0.2426 0.6754 0.3862 0.049 Uiso 1 1 calc R . . C41 C 0.5311(6) 0.9187(3) 0.4192(3) 0.0440(17) Uani 1 1 d . . . H41 H 0.5619 0.8771 0.4389 0.053 Uiso 1 1 calc R . . C44 C 0.4400(7) 1.0364(3) 0.3606(3) 0.0463(17) Uani 1 1 d . . . H44 H 0.4073 1.0773 0.3401 0.056 Uiso 1 1 calc R . . C78 C 0.9176(7) 0.6626(3) 0.2904(3) 0.0367(16) Uani 1 1 d . . . H78 H 0.9710 0.6593 0.2544 0.044 Uiso 1 1 calc R . . C32 C -0.1044(6) 1.3481(3) 0.3659(3) 0.0436(17) Uani 1 1 d . . . H32 H -0.0579 1.3057 0.3565 0.052 Uiso 1 1 calc R . . C64 C 0.4329(7) 0.6810(3) 0.4179(2) 0.0347(15) Uani 1 1 d . . . H64 H 0.4818 0.6481 0.3941 0.042 Uiso 1 1 calc R . . C50 C -0.0178(9) 0.9738(3) 0.3043(3) 0.0577(19) Uani 1 1 d . . . H50 H -0.0206 1.0203 0.3033 0.069 Uiso 1 1 calc R . . C80 C 0.8900(6) 0.6329(3) 0.3927(3) 0.0350(15) Uani 1 1 d . . . H80 H 0.9278 0.6078 0.4262 0.042 Uiso 1 1 calc R . . C11 C 0.1401(6) 1.0579(3) 0.1717(2) 0.0311(15) Uani 1 1 d . . . C29 C -0.2319(6) 1.4697(4) 0.3933(4) 0.062(2) Uani 1 1 d . . . H29 H -0.2757 1.5127 0.4020 0.075 Uiso 1 1 calc R . . C21 C -0.3761(6) 1.4537(3) 0.2333(3) 0.0402(16) Uani 1 1 d . . . H21A H -0.4428 1.4907 0.2162 0.048 Uiso 1 1 calc R . . H21B H -0.4067 1.4448 0.2747 0.048 Uiso 1 1 calc R . . C10 C 0.5525(7) 1.2333(3) 0.3147(3) 0.0398(16) Uani 1 1 d . . . H10 H 0.6076 1.1917 0.3088 0.048 Uiso 1 1 calc R . . C14 C 0.1281(6) 1.1947(3) 0.1380(3) 0.0318(15) Uani 1 1 d . . . C42 C 0.5755(6) 0.9755(4) 0.4349(3) 0.0554(19) Uani 1 1 d . . . H42 H 0.6374 0.9733 0.4661 0.067 Uiso 1 1 calc R . . C70 C 0.8168(6) 0.7886(3) 0.4604(3) 0.0400(16) Uani 1 1 d . . . H70 H 0.8324 0.7839 0.4194 0.048 Uiso 1 1 calc R . . C66 C 0.2152(7) 0.7444(3) 0.4464(3) 0.0469(18) Uani 1 1 d . . . H66 H 0.1169 0.7557 0.4432 0.056 Uiso 1 1 calc R . . C51 C 0.4882(7) 0.8446(3) 0.2600(3) 0.0562(19) Uani 1 1 d . . . H51A H 0.4759 0.8036 0.2418 0.067 Uiso 1 1 calc R . . H51B H 0.5656 0.8333 0.2873 0.067 Uiso 1 1 calc R . . C6 C 0.3468(6) 1.3124(3) 0.2966(2) 0.0280(15) Uani 1 1 d . . . C37 C 0.1552(6) 1.4378(3) 0.0804(3) 0.0395(16) Uani 1 1 d . . . H37 H 0.2334 1.4178 0.0578 0.047 Uiso 1 1 calc R . . C25 C -0.3695(7) 1.2776(3) 0.1465(2) 0.0363(16) Uani 1 1 d . . . H25 H -0.3638 1.2370 0.1284 0.044 Uiso 1 1 calc R . . C18 C -0.0793(6) 1.0739(3) 0.0376(3) 0.0464(17) Uani 1 1 d . . . H18 H -0.1258 1.0472 0.0153 0.056 Uiso 1 1 calc R . . C36 C 0.0911(8) 1.5007(4) 0.0657(3) 0.0474(18) Uani 1 1 d . . . H36 H 0.1273 1.5258 0.0336 0.057 Uiso 1 1 calc R . . C46 C 0.1105(7) 0.8703(3) 0.2973(2) 0.0382(16) Uani 1 1 d . . . C73 C 0.7817(7) 0.8038(3) 0.5788(3) 0.0527(18) Uani 1 1 d . . . H73 H 0.7689 0.8085 0.6199 0.063 Uiso 1 1 calc R . . C43 C 0.5300(7) 1.0361(3) 0.4052(3) 0.0514(18) Uani 1 1 d . . . H43 H 0.5600 1.0755 0.4154 0.062 Uiso 1 1 calc R . . C53 C 0.6383(7) 0.8735(3) 0.1746(3) 0.0541(19) Uani 1 1 d . . . H53 H 0.6818 0.8288 0.1755 0.065 Uiso 1 1 calc R . . C35 C -0.0246(7) 1.5268(3) 0.0973(3) 0.0429(17) Uani 1 1 d . . . H35 H -0.0711 1.5700 0.0869 0.051 Uiso 1 1 calc R . . C45 C 0.2469(7) 0.8313(3) 0.2813(3) 0.0493(18) Uani 1 1 d . . . H45A H 0.2585 0.7883 0.3043 0.059 Uiso 1 1 calc R . . H45B H 0.2508 0.8228 0.2391 0.059 Uiso 1 1 calc R . . C72 C 0.8481(7) 0.8479(3) 0.5437(4) 0.0525(18) Uani 1 1 d . . . H72 H 0.8813 0.8832 0.5606 0.063 Uiso 1 1 calc R . . C48 C -0.1326(8) 0.8799(4) 0.3193(3) 0.064(2) Uani 1 1 d . . . H48 H -0.2146 0.8603 0.3277 0.077 Uiso 1 1 calc R . . C30 C -0.2061(8) 1.4219(6) 0.4371(4) 0.075(3) Uani 1 1 d . . . H30 H -0.2331 1.4312 0.4766 0.090 Uiso 1 1 calc R . . C49 C -0.1422(8) 0.9482(4) 0.3165(3) 0.071(2) Uani 1 1 d . . . H49 H -0.2290 0.9761 0.3225 0.085 Uiso 1 1 calc R . . C31 C -0.1403(8) 1.3595(5) 0.4243(3) 0.062(2) Uani 1 1 d . . . H31 H -0.1204 1.3256 0.4545 0.075 Uiso 1 1 calc R . . C55 C 0.6204(8) 0.9829(4) 0.1351(4) 0.085(3) Uani 1 1 d . . . H55 H 0.6529 1.0156 0.1087 0.102 Uiso 1 1 calc R . . Cl1 Cl 0.3342(2) 0.05278(10) 0.02243(9) 0.0874(6) Uani 1 1 d . . . Cl2 Cl 0.4804(2) 0.14581(9) 0.07365(9) 0.0908(7) Uani 1 1 d . . . C105 C 0.4539(8) 0.1102(4) 0.0087(3) 0.087(3) Uani 1 1 d . . . H10A H 0.5442 0.0873 -0.0071 0.104 Uiso 1 1 calc R . . H10B H 0.4165 0.1451 -0.0209 0.104 Uiso 1 1 calc R . . C93 C 0.2869(6) 0.7455(3) 0.1251(2) 0.0307(15) Uani 1 1 d . . . C104 C 0.2128(6) 0.6712(3) 0.0249(3) 0.0333(15) Uani 1 1 d . . . H104 H 0.1507 0.7058 0.0419 0.040 Uiso 1 1 calc R . . C99 C 0.3403(6) 0.6490(3) 0.0508(2) 0.0289(15) Uani 1 1 d . . . C103 C 0.1724(6) 0.6446(3) -0.0250(3) 0.0341(15) Uani 1 1 d . . . H103 H 0.0843 0.6609 -0.0411 0.041 Uiso 1 1 calc R . . C92 C 0.6531(7) 0.6839(3) 0.1404(3) 0.0322(15) Uani 1 1 d . . . H92 H 0.6305 0.6672 0.1790 0.039 Uiso 1 1 calc R . . C94 C 0.1508(6) 0.7452(3) 0.1493(2) 0.0334(15) Uani 1 1 d . . . H94 H 0.1214 0.7037 0.1597 0.040 Uiso 1 1 calc R . . C100 C 0.4261(6) 0.5985(3) 0.0225(3) 0.0386(16) Uani 1 1 d . . . H100 H 0.5145 0.5817 0.0381 0.046 Uiso 1 1 calc R . . C84 C 0.2900(6) 0.5429(3) 0.2649(3) 0.0368(16) Uani 1 1 d . . . H84 H 0.2645 0.5157 0.2978 0.044 Uiso 1 1 calc R . . C87 C 0.5519(6) 0.6913(3) 0.0991(3) 0.0314(15) Uani 1 1 d . . . C102 C 0.2601(8) 0.5954(3) -0.0504(2) 0.0405(16) Uani 1 1 d . . . H102 H 0.2332 0.5771 -0.0843 0.049 Uiso 1 1 calc R . . C82 C 0.3021(6) 0.5690(3) 0.1614(3) 0.0333(15) Uani 1 1 d . . . H82 H 0.2852 0.5575 0.1231 0.040 Uiso 1 1 calc R . . C85 C 0.3566(6) 0.5958(3) 0.2726(3) 0.0372(16) Uani 1 1 d . . . H85 H 0.3784 0.6048 0.3109 0.045 Uiso 1 1 calc R . . C96 C 0.0967(7) 0.8626(3) 0.1462(2) 0.0380(16) Uani 1 1 d . . . H96 H 0.0331 0.9015 0.1537 0.046 Uiso 1 1 calc R . . C98 C 0.3217(6) 0.8090(3) 0.1126(2) 0.0355(16) Uani 1 1 d . . . H98 H 0.4127 0.8128 0.0965 0.043 Uiso 1 1 calc R . . B2 B 0.3882(7) 0.6769(3) 0.1105(3) 0.0312(18) Uani 1 1 d . . . C97 C 0.2297(7) 0.8667(3) 0.1225(2) 0.0364(16) Uani 1 1 d . . . H97 H 0.2580 0.9086 0.1131 0.044 Uiso 1 1 calc R . . C91 C 0.7867(7) 0.6998(3) 0.1284(3) 0.0368(16) Uani 1 1 d . . . H91 H 0.8521 0.6942 0.1586 0.044 Uiso 1 1 calc R . . C81 C 0.3667(5) 0.6242(3) 0.1667(2) 0.0272(14) Uani 1 1 d . . . C86 C 0.3919(6) 0.6358(3) 0.2252(3) 0.0348(15) Uani 1 1 d . . . H86 H 0.4351 0.6729 0.2320 0.042 Uiso 1 1 calc R . . C90 C 0.8245(6) 0.7236(3) 0.0734(3) 0.0370(16) Uani 1 1 d . . . H90 H 0.9156 0.7346 0.0651 0.044 Uiso 1 1 calc R . . C83 C 0.2608(6) 0.5297(3) 0.2096(3) 0.0344(15) Uani 1 1 d . . . H83 H 0.2126 0.4940 0.2039 0.041 Uiso 1 1 calc R . . C101 C 0.3883(7) 0.5720(3) -0.0269(3) 0.0420(16) Uani 1 1 d . . . H101 H 0.4501 0.5379 -0.0448 0.050 Uiso 1 1 calc R . . C95 C 0.0577(6) 0.8014(3) 0.1589(2) 0.0385(16) Uani 1 1 d . . . H95 H -0.0340 0.7980 0.1744 0.046 Uiso 1 1 calc R . . C88 C 0.5962(7) 0.7156(3) 0.0429(3) 0.0423(17) Uani 1 1 d . . . H88 H 0.5319 0.7215 0.0123 0.051 Uiso 1 1 calc R . . C89 C 0.7288(7) 0.7312(3) 0.0304(3) 0.0495(18) Uani 1 1 d . . . H89 H 0.7537 0.7473 -0.0081 0.059 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 C54 0.052(5) 0.072(6) 0.082(6) 0.010(5) 0.025(4) 0.021(5) Co2 0.0411(6) 0.0271(6) 0.0328(6) 0.0034(4) -0.0055(5) -0.0058(5) Co1 0.0342(6) 0.0220(5) 0.0266(6) -0.0007(4) 0.0000(4) -0.0063(4) O2 0.029(3) 0.025(2) 0.029(2) -0.0011(17) -0.0087(19) -0.0068(19) O5 0.040(2) 0.028(2) 0.028(3) 0.000(2) -0.007(2) -0.0051(18) O1 0.040(3) 0.019(2) 0.034(2) -0.0045(19) -0.0001(19) -0.006(2) O4 0.043(3) 0.027(3) 0.040(3) 0.000(2) -0.010(2) -0.007(2) O6 0.070(3) 0.025(3) 0.027(2) 0.004(2) -0.007(2) -0.012(2) O3 0.035(3) 0.031(3) 0.050(3) -0.005(2) -0.008(2) -0.006(2) N4 0.034(3) 0.020(3) 0.025(3) 0.007(2) -0.004(3) -0.008(3) N8 0.040(3) 0.024(3) 0.040(3) 0.008(3) -0.010(3) 0.001(3) C20 0.055(4) 0.028(4) 0.033(4) 0.006(4) -0.017(4) -0.004(3) N5 0.040(4) 0.038(3) 0.033(4) 0.005(2) -0.006(3) -0.006(3) N7 0.041(4) 0.036(4) 0.043(3) 0.000(3) 0.000(3) 0.002(3) N6 0.045(3) 0.029(3) 0.036(3) 0.008(3) -0.004(2) 0.000(3) C7 0.046(5) 0.033(4) 0.019(3) -0.003(3) 0.000(3) -0.016(3) C75 0.035(4) 0.021(3) 0.030(4) 0.002(3) -0.008(3) -0.007(3) C60 0.049(5) 0.020(3) 0.020(3) 0.004(3) -0.008(3) 0.003(4) C262 0.021(4) 0.036(4) 0.027(4) -0.005(3) -0.006(3) -0.004(3) C13 0.030(4) 0.026(4) 0.021(4) 0.003(3) 0.001(3) 0.001(3) C17 0.046(4) 0.030(4) 0.044(4) 0.001(4) -0.014(4) -0.006(3) C40 0.029(4) 0.043(5) 0.038(4) -0.003(4) -0.008(3) -0.008(3) N1 0.036(4) 0.029(3) 0.048(4) -0.006(3) 0.002(3) -0.011(2) N3 0.034(3) 0.039(4) 0.036(4) -0.012(3) -0.001(3) -0.013(3) C28 0.029(4) 0.060(6) 0.052(6) -0.033(5) 0.003(4) -0.019(4) N2 0.031(4) 0.027(3) 0.027(3) 0.000(3) 0.000(2) -0.007(3) C12 0.027(4) 0.028(4) 0.021(4) 0.000(4) -0.006(3) -0.003(3) C3 0.042(5) 0.028(4) 0.016(3) 0.002(3) -0.010(3) -0.018(4) C22 0.034(5) 0.029(4) 0.032(4) 0.002(3) 0.004(3) -0.007(4) C27 0.038(4) 0.040(4) 0.077(6) -0.024(5) 0.000(4) -0.008(3) C5 0.032(4) 0.034(5) 0.023(4) 0.001(3) -0.010(3) -0.014(4) C77 0.055(5) 0.044(4) 0.029(5) 0.005(3) 0.000(4) 0.004(4) C67 0.048(5) 0.041(4) 0.037(4) 0.012(3) 0.004(4) 0.004(4) C15 0.037(4) 0.027(5) 0.028(4) -0.003(3) -0.001(3) -0.004(3) C26 0.032(4) 0.028(4) 0.030(4) 0.001(3) -0.001(3) -0.002(3) C69 0.029(4) 0.026(4) 0.036(5) 0.009(3) -0.004(3) -0.006(3) C1 0.036(5) 0.022(4) 0.015(3) 0.002(3) 0.005(3) -0.010(4) C38 0.034(4) 0.030(4) 0.029(4) 0.000(3) -0.001(3) -0.014(3) C33 0.060(5) 0.031(4) 0.070(5) 0.008(4) -0.001(4) -0.009(4) C8 0.046(5) 0.045(5) 0.031(4) -0.007(3) 0.000(4) -0.024(4) C2 0.040(5) 0.011(4) 0.018(3) -0.002(3) -0.002(3) -0.003(4) C16 0.041(4) 0.024(4) 0.027(4) -0.005(3) -0.005(3) -0.008(3) C74 0.064(5) 0.042(4) 0.031(5) 0.001(3) -0.002(3) -0.023(4) C56 0.067(6) 0.043(5) 0.065(5) 0.023(4) 0.007(4) 0.000(4) C57 0.030(4) 0.031(4) 0.017(3) -0.004(3) -0.003(3) -0.003(4) C62 0.035(4) 0.023(4) 0.028(4) 0.007(3) -0.006(3) -0.008(3) C4 0.039(5) 0.022(4) 0.029(4) 0.002(3) -0.004(3) -0.008(4) C68 0.041(5) 0.035(4) 0.035(4) 0.002(3) -0.009(3) -0.008(3) C76 0.045(4) 0.032(4) 0.034(4) 0.007(3) -0.002(4) 0.005(3) C24 0.045(5) 0.049(5) 0.030(4) 0.003(4) -0.006(3) -0.017(4) C71 0.065(5) 0.047(5) 0.050(6) 0.011(4) -0.001(4) -0.034(4) C39 0.058(5) 0.038(4) 0.041(5) 0.006(3) -0.013(3) 0.002(4) C34 0.033(4) 0.037(5) 0.038(4) 0.008(4) -0.009(4) -0.015(4) C19 0.055(5) 0.050(5) 0.035(4) -0.003(4) -0.021(3) -0.012(4) B1 0.038(5) 0.029(4) 0.029(4) 0.000(3) -0.004(4) -0.007(4) C79 0.032(4) 0.040(4) 0.040(5) -0.002(4) -0.001(4) -0.004(3) C61 0.047(5) 0.023(4) 0.030(4) 0.003(3) -0.001(3) -0.012(3) C9 0.031(4) 0.051(5) 0.040(4) -0.001(4) -0.012(3) -0.012(4) C58 0.035(4) 0.029(4) 0.036(4) 0.013(3) -0.009(3) -0.012(3) C23 0.033(5) 0.039(5) 0.033(4) -0.002(3) 0.000(3) 0.000(3) C59 0.031(4) 0.038(4) 0.035(4) 0.005(3) -0.012(3) -0.005(4) C47 0.053(5) 0.046(4) 0.048(4) 0.006(3) 0.004(4) -0.012(5) C52 0.042(4) 0.045(5) 0.029(4) 0.005(4) 0.001(4) -0.012(4) C65 0.049(5) 0.029(4) 0.044(4) 0.006(3) -0.009(4) -0.008(3) C41 0.043(4) 0.040(5) 0.051(5) -0.006(4) -0.011(4) -0.010(4) C44 0.063(5) 0.030(5) 0.048(5) 0.003(3) -0.007(4) -0.015(4) C78 0.042(5) 0.040(4) 0.029(4) -0.001(3) 0.003(3) -0.011(4) C32 0.040(4) 0.065(5) 0.034(5) -0.006(4) -0.001(4) -0.029(3) C64 0.034(5) 0.031(4) 0.039(4) 0.002(3) -0.008(3) -0.004(3) C50 0.068(6) 0.042(5) 0.064(5) 0.007(4) 0.003(4) -0.016(5) C80 0.039(4) 0.034(4) 0.032(5) 0.003(3) -0.012(4) -0.005(4) C11 0.036(4) 0.024(4) 0.033(4) 0.004(4) -0.001(3) -0.006(3) C29 0.032(4) 0.099(7) 0.069(6) -0.062(6) 0.014(4) -0.027(4) C21 0.038(4) 0.031(4) 0.050(4) -0.009(3) -0.001(3) 0.002(3) C10 0.044(5) 0.037(4) 0.042(4) -0.009(4) -0.004(4) -0.012(4) C14 0.040(4) 0.019(4) 0.034(4) -0.003(4) 0.002(3) 0.003(3) C42 0.045(5) 0.080(6) 0.041(4) 0.004(5) -0.014(3) -0.010(4) C70 0.039(4) 0.042(4) 0.041(4) 0.000(4) -0.006(3) -0.013(4) C66 0.033(4) 0.046(5) 0.060(5) 0.019(4) -0.012(4) -0.007(4) C51 0.070(5) 0.042(4) 0.051(5) 0.007(4) 0.010(4) 0.000(4) C6 0.039(4) 0.024(4) 0.022(4) 0.004(3) 0.003(3) -0.012(4) C37 0.042(4) 0.045(5) 0.034(4) -0.002(4) 0.005(3) -0.018(4) C25 0.043(5) 0.031(4) 0.036(4) -0.004(3) -0.003(4) -0.008(4) C18 0.065(5) 0.036(5) 0.041(5) -0.010(3) -0.009(4) -0.013(4) C36 0.064(5) 0.056(6) 0.029(4) 0.009(4) -0.007(4) -0.035(4) C46 0.046(5) 0.034(5) 0.036(4) 0.005(3) -0.001(3) -0.014(4) C73 0.077(5) 0.055(5) 0.034(4) -0.011(4) -0.002(4) -0.029(4) C43 0.062(5) 0.048(5) 0.047(5) 0.002(4) -0.017(4) -0.017(4) C53 0.063(5) 0.042(4) 0.051(5) 0.008(4) 0.006(4) 0.002(4) C35 0.049(5) 0.034(4) 0.048(5) 0.015(4) -0.019(4) -0.015(4) C45 0.056(5) 0.038(4) 0.053(4) 0.007(3) -0.012(4) -0.004(4) C72 0.068(5) 0.031(4) 0.066(6) -0.007(4) -0.013(4) -0.026(4) C48 0.062(6) 0.074(6) 0.060(5) 0.010(4) 0.004(4) -0.030(5) C30 0.052(6) 0.149(9) 0.042(6) -0.045(7) 0.014(5) -0.060(6) C49 0.055(6) 0.062(6) 0.093(6) 0.016(4) 0.018(4) -0.014(5) C31 0.052(5) 0.116(8) 0.032(6) -0.012(5) 0.001(4) -0.053(5) C55 0.071(6) 0.069(6) 0.098(7) 0.027(5) 0.045(5) 0.009(5) Cl1 0.0860(15) 0.0859(14) 0.0953(15) -0.0223(12) 0.0265(12) -0.0318(12) Cl2 0.1141(17) 0.0574(12) 0.1028(17) 0.0047(11) -0.0256(13) -0.0170(12) C105 0.106(7) 0.070(5) 0.084(6) -0.009(5) 0.040(5) -0.029(5) C93 0.037(5) 0.031(4) 0.028(4) -0.006(3) -0.009(3) -0.013(3) C104 0.039(4) 0.030(4) 0.033(4) -0.002(3) -0.007(3) -0.009(3) C99 0.030(4) 0.027(4) 0.029(4) 0.003(3) -0.002(3) -0.003(3) C103 0.038(4) 0.026(4) 0.040(4) 0.007(3) -0.015(4) -0.008(3) C92 0.029(4) 0.036(4) 0.032(4) -0.001(3) -0.001(4) -0.006(3) C94 0.036(4) 0.022(4) 0.043(4) -0.003(3) -0.005(3) -0.005(3) C100 0.038(4) 0.040(4) 0.038(4) -0.002(3) -0.008(3) -0.009(4) C84 0.045(4) 0.034(4) 0.029(5) 0.007(3) 0.003(3) -0.003(3) C87 0.038(4) 0.026(4) 0.030(4) 0.000(3) -0.004(4) -0.007(3) C102 0.064(5) 0.041(4) 0.023(4) 0.000(3) -0.012(4) -0.027(4) C82 0.039(4) 0.033(4) 0.029(4) -0.002(3) -0.007(3) -0.005(3) C85 0.041(4) 0.040(4) 0.032(4) -0.006(4) -0.002(3) -0.008(3) C96 0.047(5) 0.033(5) 0.034(4) -0.008(3) -0.006(4) 0.000(3) C98 0.038(4) 0.045(5) 0.026(4) -0.006(3) 0.000(3) -0.013(4) B2 0.043(5) 0.029(4) 0.023(4) 0.001(3) -0.006(3) -0.006(4) C97 0.059(5) 0.021(4) 0.029(4) 0.001(3) -0.008(4) -0.006(4) C91 0.036(5) 0.033(4) 0.041(5) -0.002(3) -0.011(3) -0.004(3) C81 0.023(3) 0.025(4) 0.033(4) -0.003(3) -0.003(3) -0.002(3) C86 0.041(4) 0.031(4) 0.034(4) -0.003(4) 0.002(3) -0.011(3) C90 0.023(4) 0.044(4) 0.043(5) 0.005(3) 0.000(4) -0.009(3) C83 0.039(4) 0.026(4) 0.038(5) 0.003(4) -0.007(3) -0.005(3) C101 0.055(5) 0.041(4) 0.032(4) -0.009(3) -0.005(4) -0.007(4) C95 0.036(4) 0.034(4) 0.048(4) -0.009(3) -0.007(3) -0.012(4) C88 0.041(5) 0.049(4) 0.039(5) 0.009(3) -0.009(3) -0.014(3) C89 0.042(5) 0.072(5) 0.036(4) 0.012(3) -0.002(4) -0.019(4) _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 C54 C53 1.347(9) . ? C54 C55 1.379(9) . ? Co2 O5 2.008(3) . ? Co2 N7 2.086(5) . ? Co2 N8 2.096(5) . ? Co2 N6 2.096(5) . ? Co2 N5 2.264(4) . ? Co2 O4 2.305(4) . ? Co1 O2 1.986(4) . ? Co1 N4 2.079(4) . ? Co1 N3 2.083(5) . ? Co1 N2 2.086(4) . ? Co1 N1 2.233(4) . ? Co1 O1 2.373(4) . ? O2 C2 1.270(6) . ? O5 C12 1.294(6) . ? O1 C1 1.221(6) . ? O4 C11 1.223(6) . ? O6 C14 1.237(6) . ? O3 C4 1.236(6) . ? N4 C38 1.327(6) . ? N4 C34 1.340(7) . ? N8 C52 1.341(7) . ? N8 C56 1.345(7) . ? C20 C15 1.381(7) . ? C20 C19 1.384(8) . ? N5 C51 1.460(7) . ? N5 C39 1.468(7) . ? N5 C45 1.475(7) . ? N7 C50 1.332(8) . ? N7 C46 1.342(7) . ? N6 C44 1.340(7) . ? N6 C40 1.347(7) . ? C7 C8 1.370(7) . ? C7 C6 1.394(7) . ? C75 C80 1.398(7) . ? C75 C76 1.400(7) . ? C75 B1 1.655(8) . ? C60 C61 1.348(7) . ? C60 C59 1.388(7) . ? C262 C61 1.390(7) . ? C262 C57 1.399(7) . ? C13 C12 1.376(7) . ? C13 C14 1.459(8) . ? C13 C3 1.482(7) . ? C17 C16 1.387(7) . ? C17 C18 1.404(8) . ? C40 C41 1.355(8) . ? C40 C39 1.527(8) . ? N1 C27 1.468(7) . ? N1 C33 1.472(7) . ? N1 C21 1.484(7) . ? N3 C32 1.333(7) . ? N3 C28 1.344(7) . ? C28 C29 1.389(9) . ? C28 C27 1.500(9) . ? N2 C22 1.339(7) . ? N2 C26 1.343(6) . ? C12 C11 1.492(8) . ? C3 C2 1.379(7) . ? C3 C4 1.447(8) . ? C22 C23 1.391(7) . ? C22 C21 1.518(8) . ? C5 C10 1.386(7) . ? C5 C6 1.398(7) . ? C5 C4 1.501(8) . ? C77 C78 1.374(8) . ? C77 C76 1.397(7) . ? C67 C68 1.388(8) . ? C67 C66 1.397(8) . ? C15 C16 1.388(7) . ? C15 C14 1.501(8) . ? C26 C25 1.369(7) . ? C69 C70 1.381(7) . ? C69 C74 1.407(7) . ? C69 B1 1.652(8) . ? C1 C6 1.468(8) . ? C1 C2 1.509(7) . ? C38 C37 1.376(7) . ? C33 C34 1.496(8) . ? C8 C9 1.379(8) . ? C16 C11 1.481(8) . ? C74 C73 1.393(8) . ? C56 C55 1.383(9) . ? C57 C58 1.400(7) . ? C57 B1 1.646(8) . ? C62 C64 1.389(7) . ? C62 C68 1.401(7) . ? C62 B1 1.636(8) . ? C24 C23 1.368(8) . ? C24 C25 1.386(8) . ? C71 C72 1.363(8) . ? C71 C70 1.400(8) . ? C34 C35 1.393(8) . ? C19 C18 1.367(8) . ? C79 C78 1.358(7) . ? C79 C80 1.378(7) . ? C9 C10 1.391(8) . ? C58 C59 1.379(7) . ? C47 C48 1.360(9) . ? C47 C46 1.386(8) . ? C52 C53 1.377(8) . ? C52 C51 1.472(8) . ? C65 C66 1.373(8) . ? C65 C64 1.387(8) . ? C41 C42 1.380(8) . ? C44 C43 1.374(8) . ? C32 C31 1.389(9) . ? C50 C49 1.394(9) . ? C29 C30 1.358(10) . ? C42 C43 1.396(8) . ? C37 C36 1.371(8) . ? C36 C35 1.361(8) . ? C46 C45 1.477(8) . ? C73 C72 1.379(8) . ? C48 C49 1.389(9) . ? C30 C31 1.383(10) . ? Cl1 C105 1.780(7) . ? Cl2 C105 1.748(8) . ? C93 C94 1.404(7) . ? C93 C98 1.405(7) . ? C93 B2 1.632(8) . ? C104 C99 1.396(7) . ? C104 C103 1.396(7) . ? C99 C100 1.399(7) . ? C99 B2 1.631(8) . ? C103 C102 1.358(7) . ? C92 C87 1.381(7) . ? C92 C91 1.392(7) . ? C94 C95 1.374(7) . ? C100 C101 1.377(7) . ? C84 C83 1.362(7) . ? C84 C85 1.372(7) . ? C87 C88 1.415(7) . ? C87 B2 1.662(9) . ? C102 C101 1.381(8) . ? C82 C81 1.393(7) . ? C82 C83 1.398(7) . ? C85 C86 1.374(7) . ? C96 C95 1.374(7) . ? C96 C97 1.385(8) . ? C98 C97 1.394(7) . ? B2 C81 1.647(8) . ? C91 C90 1.369(7) . ? C81 C86 1.415(7) . ? C90 C89 1.369(8) . ? C88 C89 1.382(8) . ? 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 C53 C54 C55 118.7(6) . . ? O5 Co2 N7 108.56(19) . . ? O5 Co2 N8 104.56(18) . . ? N7 Co2 N8 137.8(2) . . ? O5 Co2 N6 91.55(18) . . ? N7 Co2 N6 108.24(18) . . ? N8 Co2 N6 96.06(17) . . ? O5 Co2 N5 169.88(17) . . ? N7 Co2 N5 74.7(2) . . ? N8 Co2 N5 77.23(19) . . ? N6 Co2 N5 78.34(19) . . ? O5 Co2 O4 74.32(14) . . ? N7 Co2 O4 79.76(16) . . ? N8 Co2 O4 84.89(15) . . ? N6 Co2 O4 165.55(19) . . ? N5 Co2 O4 115.80(16) . . ? O2 Co1 N4 104.65(17) . . ? O2 Co1 N3 106.29(19) . . ? N4 Co1 N3 137.78(19) . . ? O2 Co1 N2 91.23(19) . . ? N4 Co1 N2 100.18(16) . . ? N3 Co1 N2 107.11(17) . . ? O2 Co1 N1 169.59(17) . . ? N4 Co1 N1 78.12(19) . . ? N3 Co1 N1 76.6(2) . . ? N2 Co1 N1 78.37(19) . . ? O2 Co1 O1 74.09(14) . . ? N4 Co1 O1 83.51(15) . . ? N3 Co1 O1 78.18(15) . . ? N2 Co1 O1 165.31(18) . . ? N1 Co1 O1 116.31(16) . . ? C2 O2 Co1 121.6(3) . . ? C12 O5 Co2 120.1(3) . . ? C1 O1 Co1 109.6(3) . . ? C11 O4 Co2 110.9(3) . . ? C38 N4 C34 118.3(5) . . ? C38 N4 Co1 122.8(4) . . ? C34 N4 Co1 118.9(4) . . ? C52 N8 C56 118.2(5) . . ? C52 N8 Co2 118.4(4) . . ? C56 N8 Co2 123.4(4) . . ? C15 C20 C19 120.2(5) . . ? C51 N5 C39 113.6(5) . . ? C51 N5 C45 110.8(5) . . ? C39 N5 C45 109.5(5) . . ? C51 N5 Co2 110.8(3) . . ? C39 N5 Co2 104.3(3) . . ? C45 N5 Co2 107.4(3) . . ? C50 N7 C46 118.9(5) . . ? C50 N7 Co2 122.1(5) . . ? C46 N7 Co2 118.9(4) . . ? C44 N6 C40 117.6(5) . . ? C44 N6 Co2 124.8(4) . . ? C40 N6 Co2 116.9(4) . . ? C8 C7 C6 119.7(5) . . ? C80 C75 C76 113.6(5) . . ? C80 C75 B1 123.6(5) . . ? C76 C75 B1 122.5(5) . . ? C61 C60 C59 118.9(5) . . ? C61 C262 C57 122.5(5) . . ? C12 C13 C14 119.6(5) . . ? C12 C13 C3 122.9(5) . . ? C14 C13 C3 117.4(5) . . ? C16 C17 C18 119.9(5) . . ? N6 C40 C41 123.9(5) . . ? N6 C40 C39 114.3(5) . . ? C41 C40 C39 121.8(6) . . ? C27 N1 C33 112.0(5) . . ? C27 N1 C21 110.6(4) . . ? C33 N1 C21 111.6(5) . . ? C27 N1 Co1 105.7(3) . . ? C33 N1 Co1 110.8(3) . . ? C21 N1 Co1 105.8(3) . . ? C32 N3 C28 119.5(5) . . ? C32 N3 Co1 123.3(4) . . ? C28 N3 Co1 117.2(5) . . ? N3 C28 C29 120.7(7) . . ? N3 C28 C27 115.6(6) . . ? C29 C28 C27 123.7(7) . . ? C22 N2 C26 117.9(5) . . ? C22 N2 Co1 117.7(4) . . ? C26 N2 Co1 123.9(4) . . ? O5 C12 C13 125.5(5) . . ? O5 C12 C11 114.2(5) . . ? C13 C12 C11 120.3(5) . . ? C2 C3 C4 121.5(5) . . ? C2 C3 C13 119.4(5) . . ? C4 C3 C13 118.8(5) . . ? N2 C22 C23 122.1(5) . . ? N2 C22 C21 114.9(5) . . ? C23 C22 C21 122.8(6) . . ? N1 C27 C28 109.8(5) . . ? C10 C5 C6 119.2(5) . . ? C10 C5 C4 119.5(6) . . ? C6 C5 C4 121.2(6) . . ? C78 C77 C76 119.9(5) . . ? C68 C67 C66 118.7(6) . . ? C20 C15 C16 119.9(5) . . ? C20 C15 C14 120.3(6) . . ? C16 C15 C14 119.7(5) . . ? N2 C26 C25 123.3(5) . . ? C70 C69 C74 114.4(5) . . ? C70 C69 B1 123.7(5) . . ? C74 C69 B1 121.8(5) . . ? O1 C1 C6 123.3(5) . . ? O1 C1 C2 117.4(5) . . ? C6 C1 C2 119.2(6) . . ? N4 C38 C37 123.5(5) . . ? N1 C33 C34 113.4(5) . . ? C7 C8 C9 120.5(5) . . ? O2 C2 C3 124.4(5) . . ? O2 C2 C1 116.3(5) . . ? C3 C2 C1 119.2(6) . . ? C17 C16 C15 119.8(5) . . ? C17 C16 C11 121.3(6) . . ? C15 C16 C11 118.9(6) . . ? C73 C74 C69 123.2(6) . . ? N8 C56 C55 122.0(6) . . ? C262 C57 C58 114.2(5) . . ? C262 C57 B1 124.1(5) . . ? C58 C57 B1 121.7(5) . . ? C64 C62 C68 114.3(5) . . ? C64 C62 B1 121.8(5) . . ? C68 C62 B1 123.8(5) . . ? O3 C4 C3 122.6(5) . . ? O3 C4 C5 119.6(6) . . ? C3 C4 C5 117.8(6) . . ? C67 C68 C62 123.9(6) . . ? C77 C76 C75 123.4(5) . . ? C23 C24 C25 119.4(6) . . ? C72 C71 C70 119.6(6) . . ? N5 C39 C40 111.5(5) . . ? N4 C34 C35 121.1(5) . . ? N4 C34 C33 117.5(5) . . ? C35 C34 C33 121.3(6) . . ? C18 C19 C20 120.7(6) . . ? C62 B1 C57 108.9(5) . . ? C62 B1 C69 109.9(5) . . ? C57 B1 C69 109.5(5) . . ? C62 B1 C75 111.5(5) . . ? C57 B1 C75 110.0(4) . . ? C69 B1 C75 107.0(5) . . ? C78 C79 C80 121.4(5) . . ? C60 C61 C262 121.2(5) . . ? C8 C9 C10 120.4(6) . . ? C59 C58 C57 123.6(5) . . ? C24 C23 C22 118.9(5) . . ? C58 C59 C60 119.6(5) . . ? C48 C47 C46 118.8(6) . . ? N8 C52 C53 121.5(5) . . ? N8 C52 C51 118.5(6) . . ? C53 C52 C51 119.9(6) . . ? C66 C65 C64 119.7(6) . . ? C40 C41 C42 117.6(6) . . ? N6 C44 C43 123.1(6) . . ? C79 C78 C77 118.4(5) . . ? N3 C32 C31 122.2(7) . . ? C65 C64 C62 123.8(5) . . ? N7 C50 C49 123.1(6) . . ? C79 C80 C75 123.2(5) . . ? O4 C11 C16 121.8(5) . . ? O4 C11 C12 118.5(5) . . ? C16 C11 C12 119.7(6) . . ? C30 C29 C28 119.7(7) . . ? N1 C21 C22 111.6(5) . . ? C5 C10 C9 119.8(5) . . ? O6 C14 C13 121.6(5) . . ? O6 C14 C15 118.5(5) . . ? C13 C14 C15 119.9(6) . . ? C41 C42 C43 120.4(6) . . ? C69 C70 C71 123.5(6) . . ? C65 C66 C67 119.5(6) . . ? N5 C51 C52 114.1(5) . . ? C7 C6 C5 120.3(6) . . ? C7 C6 C1 121.3(6) . . ? C5 C6 C1 118.4(6) . . ? C36 C37 C38 118.0(6) . . ? C26 C25 C24 118.3(5) . . ? C19 C18 C17 119.5(6) . . ? C35 C36 C37 119.6(6) . . ? N7 C46 C47 121.6(6) . . ? N7 C46 C45 116.4(6) . . ? C47 C46 C45 121.7(6) . . ? C72 C73 C74 119.2(6) . . ? C44 C43 C42 117.3(6) . . ? C54 C53 C52 120.6(6) . . ? C36 C35 C34 119.5(6) . . ? N5 C45 C46 109.3(5) . . ? C71 C72 C73 120.0(6) . . ? C47 C48 C49 121.0(7) . . ? C29 C30 C31 119.9(7) . . ? C48 C49 C50 116.5(7) . . ? C30 C31 C32 117.9(7) . . ? C54 C55 C56 119.0(7) . . ? Cl2 C105 Cl1 110.0(4) . . ? C94 C93 C98 113.8(5) . . ? C94 C93 B2 121.3(5) . . ? C98 C93 B2 124.9(5) . . ? C99 C104 C103 122.9(5) . . ? C104 C99 C100 114.8(5) . . ? C104 C99 B2 124.1(5) . . ? C100 C99 B2 121.1(5) . . ? C102 C103 C104 119.5(5) . . ? C87 C92 C91 123.2(5) . . ? C95 C94 C93 123.8(5) . . ? C101 C100 C99 123.1(5) . . ? C83 C84 C85 119.4(5) . . ? C92 C87 C88 114.2(5) . . ? C92 C87 B2 126.3(5) . . ? C88 C87 B2 119.5(5) . . ? C103 C102 C101 120.0(5) . . ? C81 C82 C83 123.1(5) . . ? C84 C85 C86 120.5(5) . . ? C95 C96 C97 119.1(5) . . ? C97 C98 C93 123.4(5) . . ? C99 B2 C93 110.0(5) . . ? C99 B2 C81 109.6(5) . . ? C93 B2 C81 106.0(4) . . ? C99 B2 C87 107.9(4) . . ? C93 B2 C87 109.5(5) . . ? C81 B2 C87 113.8(5) . . ? C96 C97 C98 119.5(5) . . ? C90 C91 C92 120.5(5) . . ? C82 C81 C86 114.2(5) . . ? C82 C81 B2 121.8(5) . . ? C86 C81 B2 123.3(5) . . ? C85 C86 C81 122.8(5) . . ? C89 C90 C91 118.8(5) . . ? C84 C83 C82 119.9(5) . . ? C100 C101 C102 119.6(6) . . ? C94 C95 C96 120.3(6) . . ? C89 C88 C87 123.1(6) . . ? C90 C89 C88 120.2(6) . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 44.94 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 0.526 _refine_diff_density_min -0.442 _refine_diff_density_rms 0.045 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 309 101 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 965090' ####################################################################### # # 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_Compound_2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H74 Cl2 Co2 N10 O16' _chemical_formula_weight 1500.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C12/c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.0656(6) _cell_length_b 8.53010(10) _cell_length_c 25.9872(4) _cell_angle_alpha 90.00 _cell_angle_beta 105.875(2) _cell_angle_gamma 90.00 _cell_volume 7263.43(19) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 13022 _cell_measurement_theta_min 3.5335 _cell_measurement_theta_max 73.7827 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour purple _exptl_crystal_size_max 0.508 _exptl_crystal_size_mid 0.238 _exptl_crystal_size_min 0.072 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3120 _exptl_absorpt_coefficient_mu 4.871 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.262 _exptl_absorpt_correction_T_max 0.733 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.0711 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 26771 _diffrn_reflns_av_R_equivalents 0.0582 _diffrn_reflns_av_sigmaI/netI 0.0472 _diffrn_reflns_limit_h_min -40 _diffrn_reflns_limit_h_max 42 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 73.95 _reflns_number_total 7277 _reflns_number_gt 5684 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystalmaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1008P)^2^+14.4007P] 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 7277 _refine_ls_number_parameters 452 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0657 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1656 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.125821(15) 0.42968(6) 0.29208(2) 0.02228(16) Uani 1 1 d . . . Cl1 Cl 0.19054(3) 0.60575(12) 0.12457(3) 0.0361(2) Uani 1 1 d . . . O1 O 0.10711(7) 0.5081(3) 0.20986(9) 0.0253(5) Uani 1 1 d . . . O2 O 0.06835(7) 0.4933(3) 0.28480(9) 0.0232(5) Uani 1 1 d . . . O3 O -0.03740(8) 0.7861(3) 0.17097(11) 0.0374(6) Uani 1 1 d . . . O4 O 0.17334(11) 0.4546(4) 0.12850(15) 0.0594(9) Uani 1 1 d . . . O5 O 0.21035(12) 0.6668(6) 0.17648(13) 0.0754(13) Uani 1 1 d . . . O6 O 0.21902(8) 0.5954(3) 0.09285(11) 0.0373(6) Uani 1 1 d . . . O7 O 0.15832(11) 0.7121(5) 0.09897(15) 0.0627(10) Uani 1 1 d . . . O8 O 0.04516(15) 0.1428(6) 0.07463(17) 0.0830(13) Uani 1 1 d . . . N1 N 0.18978(8) 0.3928(3) 0.29927(11) 0.0235(6) Uani 1 1 d . . . N2 N 0.14297(9) 0.3521(3) 0.37139(12) 0.0271(6) Uani 1 1 d . . . N4 N 0.15165(9) 0.6533(3) 0.32258(11) 0.0261(6) Uani 1 1 d . . . N3 N 0.12636(9) 0.1963(3) 0.25970(11) 0.0254(6) Uani 1 1 d . . . N5 N 0.27399(19) 0.5625(6) 0.4626(3) 0.0885(19) Uani 1 1 d . . . C1 C 0.07152(10) 0.5550(4) 0.19747(13) 0.0233(7) Uani 1 1 d . . . C2 C 0.04912(10) 0.5578(4) 0.23990(13) 0.0209(6) Uani 1 1 d . . . C3 C 0.01122(10) 0.6259(4) 0.22926(13) 0.0233(7) Uani 1 1 d . . . C4 C -0.00703(10) 0.7028(4) 0.17867(15) 0.0280(7) Uani 1 1 d . . . C5 C 0.01250(11) 0.6801(5) 0.13384(15) 0.0348(9) Uani 1 1 d . . . C6 C 0.05074(11) 0.6074(5) 0.14333(14) 0.0310(8) Uani 1 1 d . . . C7 C 0.06862(13) 0.5828(6) 0.10134(17) 0.0466(11) Uani 1 1 d . . . H7 H 0.0946 0.5344 0.1077 0.056 Uiso 1 1 calc R . . C8 C 0.04757(15) 0.6304(8) 0.05053(19) 0.0665(17) Uani 1 1 d . . . H8 H 0.0589 0.6111 0.0215 0.080 Uiso 1 1 calc R . . C9 C 0.01043(16) 0.7053(9) 0.0412(2) 0.0704(18) Uani 1 1 d . . . H9 H -0.0032 0.7402 0.0061 0.085 Uiso 1 1 calc R . . C10 C -0.00736(13) 0.7303(7) 0.08299(18) 0.0523(13) Uani 1 1 d . . . H10 H -0.0330 0.7816 0.0764 0.063 Uiso 1 1 calc R . . C11 C 0.20820(10) 0.3121(4) 0.35095(14) 0.0280(7) Uani 1 1 d . . . H11A H 0.2346 0.3628 0.3684 0.034 Uiso 1 1 calc R . . H11B H 0.2139 0.2020 0.3434 0.034 Uiso 1 1 calc R . . C12 C 0.18220(10) 0.3125(4) 0.38978(13) 0.0253(7) Uani 1 1 d . . . C13 C 0.19890(12) 0.2643(4) 0.44225(14) 0.0315(8) Uani 1 1 d . . . H13 H 0.2270 0.2375 0.4546 0.038 Uiso 1 1 calc R . . C14 C 0.17406(14) 0.2561(5) 0.47619(16) 0.0412(9) Uani 1 1 d . . . H14 H 0.1846 0.2206 0.5120 0.049 Uiso 1 1 calc R . . C15 C 0.13344(14) 0.3005(5) 0.45726(18) 0.0443(10) Uani 1 1 d . . . H15 H 0.1159 0.2976 0.4801 0.053 Uiso 1 1 calc R . . C16 C 0.11887(13) 0.3487(5) 0.40491(17) 0.0387(9) Uani 1 1 d . . . H16 H 0.0912 0.3804 0.3921 0.046 Uiso 1 1 calc R . . C17 C 0.20911(11) 0.5481(4) 0.29749(15) 0.0306(8) Uani 1 1 d . . . H17A H 0.2043 0.5818 0.2598 0.037 Uiso 1 1 calc R . . H17B H 0.2389 0.5397 0.3135 0.037 Uiso 1 1 calc R . . C18 C 0.19183(10) 0.6675(4) 0.32751(13) 0.0270(7) Uani 1 1 d . . . C19 C 0.21497(11) 0.7884(4) 0.35633(15) 0.0325(8) Uani 1 1 d . . . H19 H 0.2433 0.7966 0.3591 0.039 Uiso 1 1 calc R . . C20 C 0.19597(13) 0.8961(4) 0.38073(16) 0.0360(9) Uani 1 1 d . . . H20 H 0.2112 0.9793 0.4011 0.043 Uiso 1 1 calc R . . C21 C 0.15474(13) 0.8827(5) 0.37542(16) 0.0358(8) Uani 1 1 d . . . H21 H 0.1412 0.9574 0.3916 0.043 Uiso 1 1 calc R . . C22 C 0.13338(11) 0.7590(5) 0.34623(15) 0.0320(8) Uani 1 1 d . . . H22 H 0.1050 0.7490 0.3429 0.038 Uiso 1 1 calc R . . C23 C 0.19165(11) 0.2940(4) 0.25335(14) 0.0290(7) Uani 1 1 d . . . H23A H 0.2194 0.2497 0.2596 0.035 Uiso 1 1 calc R . . H23B H 0.1859 0.3588 0.2205 0.035 Uiso 1 1 calc R . . C24 C 0.16103(10) 0.1632(4) 0.24580(13) 0.0268(7) Uani 1 1 d . . . C25 C 0.16703(12) 0.0213(5) 0.22413(15) 0.0338(8) Uani 1 1 d . . . H25 H 0.1916 0.0015 0.2147 0.041 Uiso 1 1 calc R . . C26 C 0.13701(14) -0.0929(5) 0.21618(17) 0.0393(9) Uani 1 1 d . . . H26 H 0.1404 -0.1913 0.2008 0.047 Uiso 1 1 calc R . . C27 C 0.10222(13) -0.0600(4) 0.23116(16) 0.0357(8) Uani 1 1 d . . . H27 H 0.0813 -0.1365 0.2263 0.043 Uiso 1 1 calc R . . C28 C 0.09751(11) 0.0843(4) 0.25324(15) 0.0303(8) Uani 1 1 d . . . C29 C 0.06051(13) 0.1198(5) 0.2713(2) 0.0451(10) Uani 1 1 d . . . H29A H 0.0625 0.2266 0.2856 0.068 Uiso 1 1 calc R . . H29B H 0.0586 0.0452 0.2992 0.068 Uiso 1 1 calc R . . H29C H 0.0361 0.1109 0.2409 0.068 Uiso 1 1 calc R . . C30 C -0.0080(2) 0.2289(11) 0.1076(3) 0.094(2) Uani 1 1 d . . . H30A H -0.0174 0.2436 0.1398 0.142 Uiso 1 1 calc R . . H30B H -0.0268 0.1585 0.0828 0.142 Uiso 1 1 calc R . . H30C H -0.0073 0.3305 0.0903 0.142 Uiso 1 1 calc R . . C31 C 0.0317(2) 0.1625(8) 0.1222(2) 0.0766(18) Uani 1 1 d . . . H31A H 0.0312 0.0598 0.1398 0.092 Uiso 1 1 calc R . . H31B H 0.0508 0.2323 0.1478 0.092 Uiso 1 1 calc R . . C32 C 0.0849(3) 0.0732(10) 0.0841(3) 0.107(3) Uani 1 1 d . . . H32A H 0.0847 -0.0333 0.0992 0.129 Uiso 1 1 calc R . . H32B H 0.1052 0.1372 0.1102 0.129 Uiso 1 1 calc R . . C33 C 0.0962(3) 0.0641(13) 0.0319(4) 0.133(4) Uani 1 1 d . . . H33A H 0.1233 0.0166 0.0382 0.200 Uiso 1 1 calc R . . H33B H 0.0966 0.1699 0.0174 0.200 Uiso 1 1 calc R . . H33C H 0.0761 0.0000 0.0064 0.200 Uiso 1 1 calc R . . C34 C 0.2916(2) 0.6751(7) 0.4771(3) 0.0737(17) Uani 1 1 d . . . C35 C 0.3136(3) 0.8196(7) 0.4969(3) 0.089(2) Uani 1 1 d . . . H35A H 0.3074 0.8988 0.4685 0.133 Uiso 1 1 calc R . . H35B H 0.3430 0.7987 0.5077 0.133 Uiso 1 1 calc R . . H35C H 0.3052 0.8582 0.5277 0.133 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 0.0195(3) 0.0217(3) 0.0241(3) 0.0028(2) 0.00342(19) 0.0013(2) Cl1 0.0307(4) 0.0510(6) 0.0280(4) 0.0029(4) 0.0103(3) -0.0055(4) O1 0.0215(11) 0.0311(13) 0.0227(11) 0.0026(10) 0.0053(9) 0.0017(9) O2 0.0209(11) 0.0256(12) 0.0225(11) 0.0010(9) 0.0052(9) 0.0019(9) O3 0.0285(13) 0.0358(15) 0.0473(16) 0.0144(12) 0.0093(12) 0.0086(11) O4 0.064(2) 0.055(2) 0.065(2) 0.0114(17) 0.0277(18) -0.0184(17) O5 0.063(2) 0.133(4) 0.0344(17) -0.018(2) 0.0196(16) -0.030(2) O6 0.0310(14) 0.0493(17) 0.0335(14) -0.0012(12) 0.0122(11) -0.0035(12) O7 0.0495(19) 0.074(3) 0.070(2) 0.0193(19) 0.0255(17) 0.0227(18) O8 0.094(3) 0.084(3) 0.059(2) 0.015(2) 0.001(2) 0.024(3) N1 0.0228(13) 0.0255(15) 0.0216(13) 0.0025(11) 0.0053(11) 0.0008(11) N2 0.0281(15) 0.0259(15) 0.0280(15) 0.0030(12) 0.0091(12) 0.0021(12) N4 0.0254(14) 0.0244(15) 0.0247(14) 0.0017(11) 0.0005(11) -0.0005(11) N3 0.0260(14) 0.0208(15) 0.0277(14) 0.0041(11) 0.0042(11) 0.0014(11) N5 0.090(4) 0.051(3) 0.104(5) 0.004(3) -0.009(3) 0.004(3) C1 0.0208(15) 0.0236(17) 0.0252(16) 0.0011(13) 0.0055(12) -0.0034(12) C2 0.0226(15) 0.0186(16) 0.0207(15) 0.0015(12) 0.0044(12) -0.0030(12) C3 0.0204(15) 0.0218(16) 0.0273(17) 0.0026(13) 0.0055(13) -0.0012(12) C4 0.0192(15) 0.0286(18) 0.0341(18) 0.0068(15) 0.0037(13) -0.0022(13) C5 0.0251(17) 0.048(2) 0.0292(18) 0.0111(16) 0.0043(14) -0.0016(16) C6 0.0224(16) 0.044(2) 0.0251(17) 0.0068(15) 0.0032(14) -0.0011(15) C7 0.030(2) 0.080(3) 0.029(2) 0.010(2) 0.0086(16) 0.003(2) C8 0.040(2) 0.130(5) 0.032(2) 0.023(3) 0.0138(19) 0.008(3) C9 0.047(3) 0.129(6) 0.035(2) 0.028(3) 0.010(2) 0.012(3) C10 0.030(2) 0.087(4) 0.038(2) 0.024(2) 0.0056(17) 0.007(2) C11 0.0212(15) 0.0334(19) 0.0275(17) 0.0078(14) 0.0033(13) 0.0049(13) C12 0.0264(16) 0.0237(17) 0.0244(16) -0.0023(13) 0.0043(13) 0.0004(13) C13 0.0372(19) 0.032(2) 0.0219(17) -0.0021(14) 0.0023(14) 0.0041(15) C14 0.059(3) 0.041(2) 0.0245(18) -0.0001(16) 0.0124(18) 0.001(2) C15 0.056(3) 0.045(3) 0.042(2) 0.0000(19) 0.031(2) 0.003(2) C16 0.036(2) 0.042(2) 0.043(2) 0.0067(18) 0.0195(17) 0.0052(17) C17 0.0261(17) 0.0306(19) 0.0366(19) 0.0047(15) 0.0112(15) -0.0075(14) C18 0.0256(16) 0.0263(18) 0.0254(16) 0.0062(13) 0.0006(13) -0.0032(13) C19 0.0295(18) 0.0267(19) 0.0364(19) 0.0057(15) 0.0010(15) -0.0060(14) C20 0.042(2) 0.0229(19) 0.037(2) 0.0008(15) 0.0000(17) -0.0059(15) C21 0.041(2) 0.0231(19) 0.039(2) -0.0008(15) 0.0043(17) 0.0033(15) C22 0.0267(17) 0.031(2) 0.0346(19) -0.0007(15) 0.0024(14) 0.0012(14) C23 0.0283(17) 0.034(2) 0.0261(17) 0.0004(14) 0.0094(14) -0.0005(15) C24 0.0277(17) 0.0276(18) 0.0241(16) 0.0058(13) 0.0054(13) 0.0041(14) C25 0.038(2) 0.031(2) 0.0336(19) 0.0002(15) 0.0123(16) 0.0030(16) C26 0.050(2) 0.029(2) 0.038(2) -0.0007(16) 0.0107(18) 0.0043(17) C27 0.041(2) 0.0228(19) 0.041(2) 0.0022(15) 0.0069(17) -0.0030(15) C28 0.0304(18) 0.0230(18) 0.0341(19) 0.0035(14) 0.0030(15) -0.0020(14) C29 0.036(2) 0.032(2) 0.070(3) -0.002(2) 0.019(2) -0.0052(17) C30 0.082(5) 0.126(7) 0.069(4) 0.026(4) 0.009(4) -0.009(4) C31 0.101(5) 0.075(4) 0.047(3) 0.013(3) 0.009(3) -0.004(4) C32 0.120(7) 0.104(6) 0.077(5) 0.009(4) -0.008(5) 0.047(5) C33 0.128(8) 0.157(10) 0.111(7) 0.022(6) 0.028(6) 0.071(7) C34 0.086(4) 0.049(3) 0.071(4) 0.022(3) -0.002(3) 0.009(3) C35 0.126(6) 0.052(4) 0.073(4) 0.016(3) 0.002(4) -0.005(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.990(2) . ? Co1 N2 2.090(3) . ? Co1 N1 2.158(3) . ? Co1 N4 2.158(3) . ? Co1 O1 2.162(2) . ? Co1 N3 2.164(3) . ? Cl1 O4 1.431(3) . ? Cl1 O5 1.431(4) . ? Cl1 O6 1.437(3) . ? Cl1 O7 1.439(3) . ? O1 C1 1.233(4) . ? O2 C2 1.294(4) . ? O3 C4 1.226(4) . ? O8 C32 1.436(9) . ? O8 C31 1.442(8) . ? N1 C23 1.477(4) . ? N1 C17 1.486(4) . ? N1 C11 1.487(4) . ? N2 C12 1.334(4) . ? N2 C16 1.351(5) . ? N4 C22 1.337(5) . ? N4 C18 1.345(4) . ? N3 C28 1.348(5) . ? N3 C24 1.356(4) . ? N5 C34 1.140(8) . ? C1 C6 1.461(5) . ? C1 C2 1.503(5) . ? C2 C3 1.373(5) . ? C3 C4 1.449(5) . ? C3 C3 1.482(6) 2 ? C4 C5 1.504(5) . ? C5 C10 1.378(5) . ? C5 C6 1.402(5) . ? C6 C7 1.404(6) . ? C7 C8 1.380(6) . ? C8 C9 1.379(7) . ? C9 C10 1.398(7) . ? C11 C12 1.514(5) . ? C12 C13 1.388(5) . ? C13 C14 1.381(6) . ? C14 C15 1.388(6) . ? C15 C16 1.377(6) . ? C17 C18 1.498(5) . ? C18 C19 1.387(5) . ? C19 C20 1.375(6) . ? C20 C21 1.378(6) . ? C21 C22 1.384(5) . ? C23 C24 1.503(5) . ? C24 C25 1.374(5) . ? C25 C26 1.386(6) . ? C26 C27 1.374(6) . ? C27 C28 1.385(5) . ? C28 C29 1.491(6) . ? C30 C31 1.421(9) . ? C32 C33 1.510(12) . ? C34 C35 1.461(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N2 100.51(10) . . ? O2 Co1 N1 172.52(10) . . ? N2 Co1 N1 82.26(11) . . ? O2 Co1 N4 94.91(10) . . ? N2 Co1 N4 86.66(11) . . ? N1 Co1 N4 78.25(11) . . ? O2 Co1 O1 78.77(9) . . ? N2 Co1 O1 179.05(11) . . ? N1 Co1 O1 98.53(10) . . ? N4 Co1 O1 94.02(10) . . ? O2 Co1 N3 109.07(10) . . ? N2 Co1 N3 93.57(11) . . ? N1 Co1 N3 77.52(11) . . ? N4 Co1 N3 155.51(11) . . ? O1 Co1 N3 86.09(10) . . ? O4 Cl1 O5 110.9(2) . . ? O4 Cl1 O6 109.8(2) . . ? O5 Cl1 O6 110.16(19) . . ? O4 Cl1 O7 109.0(2) . . ? O5 Cl1 O7 108.1(3) . . ? O6 Cl1 O7 108.82(19) . . ? C1 O1 Co1 111.2(2) . . ? C2 O2 Co1 116.3(2) . . ? C32 O8 C31 114.0(5) . . ? C23 N1 C17 111.5(3) . . ? C23 N1 C11 111.4(3) . . ? C17 N1 C11 111.1(3) . . ? C23 N1 Co1 106.2(2) . . ? C17 N1 Co1 108.3(2) . . ? C11 N1 Co1 108.2(2) . . ? C12 N2 C16 119.3(3) . . ? C12 N2 Co1 114.6(2) . . ? C16 N2 Co1 126.0(3) . . ? C22 N4 C18 119.0(3) . . ? C22 N4 Co1 124.8(2) . . ? C18 N4 Co1 114.6(2) . . ? C28 N3 C24 118.5(3) . . ? C28 N3 Co1 128.1(2) . . ? C24 N3 Co1 113.3(2) . . ? O1 C1 C6 122.2(3) . . ? O1 C1 C2 118.3(3) . . ? C6 C1 C2 119.5(3) . . ? O2 C2 C3 125.3(3) . . ? O2 C2 C1 114.9(3) . . ? C3 C2 C1 119.8(3) . . ? C2 C3 C4 121.4(3) . . ? C2 C3 C3 119.8(3) . 2 ? C4 C3 C3 118.8(3) . 2 ? O3 C4 C3 123.0(3) . . ? O3 C4 C5 118.7(3) . . ? C3 C4 C5 118.3(3) . . ? C10 C5 C6 119.7(4) . . ? C10 C5 C4 119.9(4) . . ? C6 C5 C4 120.5(3) . . ? C5 C6 C7 120.6(3) . . ? C5 C6 C1 119.1(3) . . ? C7 C6 C1 120.3(3) . . ? C8 C7 C6 118.5(4) . . ? C9 C8 C7 121.1(4) . . ? C8 C9 C10 120.4(4) . . ? C5 C10 C9 119.7(4) . . ? N1 C11 C12 114.9(3) . . ? N2 C12 C13 121.9(3) . . ? N2 C12 C11 118.2(3) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 118.9(4) . . ? C13 C14 C15 119.0(4) . . ? C16 C15 C14 119.1(4) . . ? N2 C16 C15 121.7(4) . . ? N1 C17 C18 110.4(3) . . ? N4 C18 C19 122.1(3) . . ? N4 C18 C17 115.1(3) . . ? C19 C18 C17 122.7(3) . . ? C20 C19 C18 118.4(4) . . ? C19 C20 C21 119.6(4) . . ? C20 C21 C22 119.1(4) . . ? N4 C22 C21 121.7(3) . . ? N1 C23 C24 110.3(3) . . ? N3 C24 C25 122.1(3) . . ? N3 C24 C23 115.7(3) . . ? C25 C24 C23 122.1(3) . . ? C24 C25 C26 119.6(4) . . ? C27 C26 C25 118.2(4) . . ? C26 C27 C28 120.4(4) . . ? N3 C28 C27 121.2(4) . . ? N3 C28 C29 117.8(3) . . ? C27 C28 C29 121.0(3) . . ? C30 C31 O8 108.7(5) . . ? O8 C32 C33 109.1(6) . . ? N5 C34 C35 178.4(9) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 73.95 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 1.277 _refine_diff_density_min -0.594 _refine_diff_density_rms 0.094 _database_code_depnum_ccdc_archive 'CCDC 965091' ####################################################################### # # 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_Compound_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C64 H60 Cl2 Co2 N10 O15' _chemical_formula_weight 1397.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'C 2 2 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' _cell_length_a 8.8275(4) _cell_length_b 37.7023(17) _cell_length_c 18.6602(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6210.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2142 _cell_measurement_theta_min 3.3298 _cell_measurement_theta_max 61.4222 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour purple _exptl_crystal_size_max 0.2011 _exptl_crystal_size_mid 0.0992 _exptl_crystal_size_min 0.0193 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2888 _exptl_absorpt_coefficient_mu 5.613 _exptl_absorpt_correction_type gaussian _exptl_absorpt_correction_T_min 0.498 _exptl_absorpt_correction_T_max 0.897 _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) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; Crystal were found to be weakly diffracting at high angles and as such data were only collected to a 2theta value of 123 degrees. ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean 16.0711 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8076 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0958 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -40 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.33 _diffrn_reflns_theta_max 61.51 _reflns_number_total 4579 _reflns_number_gt 3544 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystalmaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0900P)^2^+46.8527P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.019(12) _refine_ls_number_reflns 4579 _refine_ls_number_parameters 412 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.1173 _refine_ls_R_factor_gt 0.0915 _refine_ls_wR_factor_ref 0.2381 _refine_ls_wR_factor_gt 0.2195 _refine_ls_goodness_of_fit_ref 1.100 _refine_ls_restrained_S_all 1.102 _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 0.48240(17) 0.60675(4) 0.45837(8) 0.0374(4) Uani 1 1 d . . . Cl1 Cl 0.9663(7) 0.62412(12) 0.7529(4) 0.0630(16) Uiso 0.50 1 d PD . . Cl2 Cl 0.9555(7) 0.71750(13) 0.2611(3) 0.0542(17) Uani 0.50 1 d PD . . O1 O 0.4041(8) 0.58103(17) 0.3564(3) 0.0378(16) Uani 1 1 d . . . O2 O 0.4227(7) 0.55881(17) 0.4913(4) 0.0390(16) Uani 1 1 d . . . O3 O 0.1362(8) 0.4591(2) 0.4246(4) 0.0484(18) Uani 1 1 d . . . O4 O 0.9280(14) 0.6036(2) 0.6934(4) 0.104(4) Uani 1 1 d D . . O5 O 1.034(2) 0.6576(3) 0.7335(9) 0.085(6) Uiso 0.50 1 d PD . . O6 O 0.8385(19) 0.6303(5) 0.7985(9) 0.117(8) Uiso 0.50 1 d PD . . O7 O 0.927(2) 0.7468(4) 0.2137(8) 0.077(5) Uiso 0.50 1 d PD . . O8 O 0.890(2) 0.6872(4) 0.2264(9) 0.068(5) Uiso 0.50 1 d PD . . O9 O 0.887(2) 0.7197(7) 0.3305(7) 0.104(8) Uani 0.50 1 d PD . . O10 O 1.1169(14) 0.7141(7) 0.2703(16) 0.113(9) Uiso 0.50 1 d PD . . O11 O 0.991(6) 0.7584(6) 0.7682(17) 0.138(10) Uiso 0.50 1 d P . . N1 N 0.5162(10) 0.6548(2) 0.4007(4) 0.0409(19) Uani 1 1 d . . . N2 N 0.5573(10) 0.6382(2) 0.5464(5) 0.049(2) Uani 1 1 d . . . N3 N 0.7096(9) 0.5996(2) 0.4204(4) 0.0366(19) Uani 1 1 d . . . N4 N 0.2656(10) 0.6312(2) 0.4722(4) 0.042(2) Uani 1 1 d . . . N5 N 0.338(2) 0.7438(4) 0.5290(9) 0.118(5) Uiso 1 1 d . . . C1 C 0.3568(11) 0.5507(3) 0.3686(5) 0.036(2) Uani 1 1 d . . . C2 C 0.3542(11) 0.5382(3) 0.4450(5) 0.042(3) Uani 1 1 d . . . C3 C 0.2903(11) 0.5059(3) 0.4622(5) 0.038(2) Uani 1 1 d . . . C4 C 0.2141(12) 0.4849(3) 0.4082(5) 0.040(2) Uani 1 1 d . . . C5 C 0.2360(12) 0.4943(3) 0.3307(5) 0.039(2) Uani 1 1 d . . . C6 C 0.2965(11) 0.5274(2) 0.3119(5) 0.034(2) Uani 1 1 d . . . C7 C 0.3115(11) 0.5371(3) 0.2399(6) 0.040(2) Uani 1 1 d . . . H7 H 0.3530 0.5594 0.2266 0.048 Uiso 1 1 calc R . . C8 C 0.2626(15) 0.5124(3) 0.1878(6) 0.055(3) Uani 1 1 d . . . H8 H 0.2707 0.5187 0.1387 0.065 Uiso 1 1 calc R . . C9 C 0.2042(14) 0.4801(3) 0.2053(6) 0.049(3) Uani 1 1 d . . . H9 H 0.1769 0.4639 0.1685 0.059 Uiso 1 1 calc R . . C10 C 0.1840(13) 0.4705(3) 0.2781(5) 0.043(3) Uani 1 1 d . . . H10 H 0.1370 0.4487 0.2909 0.051 Uiso 1 1 calc R . . C11 C 0.5894(14) 0.6814(3) 0.4494(6) 0.052(3) Uani 1 1 d . . . H11A H 0.6943 0.6855 0.4326 0.062 Uiso 1 1 calc R . . H11B H 0.5340 0.7041 0.4450 0.062 Uiso 1 1 calc R . . C12 C 0.5950(14) 0.6713(3) 0.5271(6) 0.055(3) Uani 1 1 d . . . C13 C 0.658(2) 0.6947(4) 0.5756(8) 0.086(5) Uani 1 1 d . . . H13 H 0.6852 0.7179 0.5605 0.104 Uiso 1 1 calc R . . C14 C 0.683(2) 0.6847(5) 0.6455(9) 0.103(6) Uani 1 1 d . . . H14 H 0.7329 0.6999 0.6785 0.124 Uiso 1 1 calc R . . C15 C 0.630(3) 0.6504(5) 0.6664(9) 0.108(6) Uani 1 1 d . . . H15 H 0.6396 0.6429 0.7148 0.130 Uiso 1 1 calc R . . C16 C 0.5672(15) 0.6287(4) 0.6169(6) 0.063(4) Uani 1 1 d . . . C17 C 0.5149(17) 0.5934(3) 0.6403(6) 0.066(3) Uani 1 1 d . . . H17A H 0.4756 0.5803 0.5990 0.099 Uiso 1 1 calc R . . H17B H 0.4345 0.5962 0.6761 0.099 Uiso 1 1 calc R . . H17C H 0.5998 0.5804 0.6615 0.099 Uiso 1 1 calc R . . C18 C 0.6168(13) 0.6457(3) 0.3408(6) 0.047(3) Uani 1 1 d . . . H18A H 0.6580 0.6678 0.3195 0.056 Uiso 1 1 calc R . . H18B H 0.5581 0.6332 0.3033 0.056 Uiso 1 1 calc R . . C19 C 0.7466(12) 0.6223(3) 0.3657(5) 0.045(3) Uani 1 1 d . . . C20 C 0.8847(13) 0.6219(3) 0.3329(6) 0.048(3) Uani 1 1 d . . . H20 H 0.9056 0.6377 0.2946 0.058 Uiso 1 1 calc R . . C21 C 0.9931(13) 0.5984(3) 0.3557(5) 0.051(3) Uani 1 1 d . . . H21 H 1.0885 0.5975 0.3322 0.061 Uiso 1 1 calc R . . C22 C 0.9639(12) 0.5763(3) 0.4123(6) 0.055(3) Uani 1 1 d . . . H22 H 1.0392 0.5604 0.4292 0.066 Uiso 1 1 calc R . . C23 C 0.8215(12) 0.5777(3) 0.4449(5) 0.046(3) Uani 1 1 d . . . C24 C 0.7853(13) 0.5551(3) 0.5098(6) 0.055(3) Uani 1 1 d . . . H24A H 0.6816 0.5599 0.5258 0.083 Uiso 1 1 calc R . . H24B H 0.8563 0.5607 0.5486 0.083 Uiso 1 1 calc R . . H24C H 0.7946 0.5299 0.4971 0.083 Uiso 1 1 calc R . . C25 C 0.3670(12) 0.6655(3) 0.3745(6) 0.049(3) Uani 1 1 d . . . H25A H 0.3390 0.6507 0.3326 0.059 Uiso 1 1 calc R . . H25B H 0.3705 0.6905 0.3588 0.059 Uiso 1 1 calc R . . C26 C 0.2481(11) 0.6612(3) 0.4331(5) 0.038(2) Uani 1 1 d . . . C27 C 0.1252(12) 0.6835(3) 0.4446(7) 0.055(3) Uani 1 1 d . . . H27 H 0.1128 0.7043 0.4165 0.066 Uiso 1 1 calc R . . C28 C 0.0228(13) 0.6753(3) 0.4966(6) 0.055(3) Uani 1 1 d . . . H28 H -0.0616 0.6904 0.5048 0.066 Uiso 1 1 calc R . . C29 C 0.0414(12) 0.6448(3) 0.5378(6) 0.052(3) Uani 1 1 d . . . H29 H -0.0287 0.6388 0.5745 0.063 Uiso 1 1 calc R . . C30 C 0.1621(13) 0.6240(3) 0.5240(6) 0.053(3) Uani 1 1 d . . . H30 H 0.1755 0.6032 0.5520 0.064 Uiso 1 1 calc R . . C41 C 0.310(2) 0.7288(5) 0.5827(11) 0.097(5) Uiso 1 1 d . . . C42 C 0.271(3) 0.7107(7) 0.6504(15) 0.163(10) Uiso 1 1 d . . . H42A H 0.2850 0.6851 0.6446 0.245 Uiso 1 1 calc R . . H42B H 0.1655 0.7158 0.6627 0.245 Uiso 1 1 calc R . . H42C H 0.3375 0.7193 0.6888 0.245 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 0.0322(8) 0.0526(9) 0.0273(7) 0.0046(7) 0.0021(7) -0.0024(8) Cl2 0.077(6) 0.048(3) 0.037(4) 0.003(2) 0.003(3) 0.013(3) O1 0.047(4) 0.040(4) 0.026(4) 0.006(3) -0.003(3) -0.001(3) O2 0.036(4) 0.053(4) 0.028(4) -0.002(3) -0.001(3) -0.002(3) O3 0.050(4) 0.058(5) 0.036(4) 0.014(4) -0.006(3) -0.008(4) O4 0.174(12) 0.079(6) 0.058(6) 0.008(5) -0.005(7) -0.024(7) O9 0.104(16) 0.17(2) 0.041(10) 0.005(13) 0.014(11) 0.048(16) N1 0.034(5) 0.056(5) 0.033(4) 0.011(4) 0.005(4) -0.009(4) N2 0.044(5) 0.067(6) 0.036(5) -0.001(5) -0.008(4) 0.010(4) N3 0.032(4) 0.051(5) 0.027(4) 0.001(4) -0.003(3) -0.007(4) N4 0.043(5) 0.052(5) 0.033(5) 0.005(4) 0.004(4) -0.011(4) C1 0.038(6) 0.051(6) 0.019(5) 0.006(5) 0.003(4) 0.006(5) C2 0.032(5) 0.061(7) 0.033(6) 0.006(5) 0.003(5) 0.002(5) C3 0.044(6) 0.044(6) 0.026(5) 0.006(5) -0.005(5) 0.011(4) C4 0.041(6) 0.053(6) 0.024(5) 0.006(5) -0.004(5) 0.004(5) C5 0.049(6) 0.039(6) 0.028(5) -0.002(5) 0.004(5) 0.007(5) C6 0.041(6) 0.035(5) 0.026(5) 0.006(4) 0.002(4) 0.007(4) C7 0.044(6) 0.041(5) 0.034(6) -0.002(5) -0.001(5) 0.001(4) C8 0.089(9) 0.043(6) 0.031(6) -0.010(5) -0.002(6) 0.014(6) C9 0.064(8) 0.040(6) 0.042(7) -0.006(5) -0.006(6) -0.001(5) C10 0.053(7) 0.042(6) 0.033(6) -0.003(5) -0.006(5) 0.010(5) C11 0.058(7) 0.054(6) 0.044(7) -0.008(5) -0.003(6) -0.010(5) C12 0.062(7) 0.064(8) 0.039(7) -0.004(6) 0.000(6) -0.002(6) C13 0.125(14) 0.077(9) 0.057(9) -0.022(8) 0.007(9) -0.028(9) C14 0.151(17) 0.103(13) 0.056(10) -0.011(9) -0.023(10) 0.001(12) C15 0.171(19) 0.113(14) 0.042(8) 0.006(9) -0.007(11) -0.019(14) C16 0.070(9) 0.085(9) 0.033(7) 0.004(7) -0.004(6) -0.008(7) C17 0.079(9) 0.085(8) 0.034(6) 0.010(6) -0.007(7) 0.006(8) C18 0.055(7) 0.051(6) 0.036(6) 0.006(5) -0.002(5) -0.014(5) C19 0.037(6) 0.067(7) 0.031(6) -0.005(5) -0.004(5) 0.001(5) C20 0.050(7) 0.061(7) 0.033(6) -0.006(5) 0.001(5) -0.015(6) C21 0.036(6) 0.081(8) 0.037(6) 0.006(6) 0.004(5) 0.000(6) C22 0.028(6) 0.083(8) 0.053(7) -0.020(6) -0.011(5) 0.007(6) C23 0.044(6) 0.067(7) 0.028(6) -0.004(5) -0.004(5) -0.004(5) C24 0.040(7) 0.073(8) 0.053(7) 0.003(6) 0.003(5) 0.007(6) C25 0.040(6) 0.052(6) 0.056(7) 0.013(6) 0.004(6) -0.009(5) C26 0.024(5) 0.057(6) 0.035(6) 0.000(5) -0.003(4) -0.009(5) C27 0.035(6) 0.063(7) 0.068(9) 0.009(6) -0.006(6) -0.003(5) C28 0.038(6) 0.069(7) 0.059(7) -0.001(6) -0.002(6) 0.002(6) C29 0.039(6) 0.080(8) 0.039(6) 0.006(6) 0.009(6) 0.002(6) C30 0.055(7) 0.080(8) 0.025(6) -0.011(5) 0.000(5) -0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 1.981(7) . ? Co1 N1 2.128(8) . ? Co1 N2 2.130(9) . ? Co1 N4 2.139(9) . ? Co1 N3 2.144(8) . ? Co1 O1 2.244(7) . ? Cl1 Cl1 0.604(12) 4_756 ? Cl1 O5 1.290(11) 4_756 ? Cl1 O4 1.395(8) . ? Cl1 O6 1.432(9) . ? Cl1 O5 1.444(8) . ? Cl1 O4 1.574(12) 4_756 ? Cl1 O6 1.985(15) 4_756 ? Cl2 O10 0.88(2) 4_755 ? Cl2 Cl2 0.887(11) 4_755 ? Cl2 O9 1.432(9) . ? Cl2 O8 1.433(9) . ? Cl2 O7 1.435(9) . ? Cl2 O10 1.441(10) . ? Cl2 O7 1.583(15) 4_755 ? Cl2 O8 1.792(14) 4_755 ? O1 C1 1.237(12) . ? O2 C2 1.310(12) . ? O3 C4 1.230(12) . ? O4 Cl1 1.574(12) 4_756 ? O5 O5 0.86(3) 4_756 ? O5 Cl1 1.290(11) 4_756 ? O5 O6 1.64(3) 4_756 ? O6 O5 1.64(3) 4_756 ? O6 Cl1 1.985(15) 4_756 ? O7 O10 1.33(3) 4_755 ? O7 Cl2 1.583(15) 4_755 ? O8 O10 1.02(3) 4_755 ? O8 Cl2 1.792(14) 4_755 ? O10 Cl2 0.88(2) 4_755 ? O10 O8 1.02(3) 4_755 ? O10 O7 1.33(3) 4_755 ? O11 O11 0.70(6) 4_756 ? N1 C25 1.461(14) . ? N1 C18 1.468(14) . ? N1 C11 1.500(13) . ? N2 C12 1.343(15) . ? N2 C16 1.366(15) . ? N3 C23 1.366(13) . ? N3 C19 1.371(13) . ? N4 C26 1.356(13) . ? N4 C30 1.357(14) . ? N5 C41 1.18(2) . ? C1 C6 1.474(14) . ? C1 C2 1.502(13) . ? C2 C3 1.381(15) . ? C3 C4 1.448(14) . ? C3 C3 1.479(19) 3_566 ? C4 C5 1.501(14) . ? C5 C6 1.405(14) . ? C5 C10 1.406(15) . ? C6 C7 1.398(14) . ? C7 C8 1.412(15) . ? C8 C9 1.365(16) . ? C9 C10 1.417(15) . ? C11 C12 1.500(16) . ? C12 C13 1.381(18) . ? C13 C14 1.38(2) . ? C14 C15 1.43(2) . ? C15 C16 1.36(2) . ? C16 C17 1.472(17) . ? C18 C19 1.519(15) . ? C19 C20 1.364(15) . ? C20 C21 1.371(15) . ? C21 C22 1.369(15) . ? C22 C23 1.397(15) . ? C23 C24 1.517(15) . ? C25 C26 1.524(14) . ? C26 C27 1.389(15) . ? C27 C28 1.362(16) . ? C28 C29 1.394(15) . ? C29 C30 1.347(16) . ? C41 C42 1.48(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N1 166.2(3) . . ? O2 Co1 N2 110.5(3) . . ? N1 Co1 N2 82.7(3) . . ? O2 Co1 N4 96.7(3) . . ? N1 Co1 N4 79.7(3) . . ? N2 Co1 N4 86.9(3) . . ? O2 Co1 N3 103.7(3) . . ? N1 Co1 N3 78.9(3) . . ? N2 Co1 N3 91.9(3) . . ? N4 Co1 N3 158.5(3) . . ? O2 Co1 O1 77.7(3) . . ? N1 Co1 O1 89.0(3) . . ? N2 Co1 O1 171.6(3) . . ? N4 Co1 O1 90.7(3) . . ? N3 Co1 O1 87.4(3) . . ? Cl1 Cl1 O5 92.1(9) 4_756 4_756 ? Cl1 Cl1 O4 95.6(14) 4_756 . ? O5 Cl1 O4 134.6(11) 4_756 . ? Cl1 Cl1 O6 151.6(19) 4_756 . ? O5 Cl1 O6 73.8(12) 4_756 . ? O4 Cl1 O6 111.9(8) . . ? Cl1 Cl1 O5 63.1(8) 4_756 . ? O5 Cl1 O5 36.2(12) 4_756 . ? O4 Cl1 O5 112.8(7) . . ? O6 Cl1 O5 109.4(8) . . ? Cl1 Cl1 O4 61.9(12) 4_756 4_756 ? O5 Cl1 O4 111.0(10) 4_756 4_756 ? O4 Cl1 O4 112.1(8) . 4_756 ? O6 Cl1 O4 99.7(11) . 4_756 ? O5 Cl1 O4 110.2(10) . 4_756 ? Cl1 Cl1 O6 20.0(14) 4_756 4_756 ? O5 Cl1 O6 89.0(8) 4_756 4_756 ? O4 Cl1 O6 83.8(8) . 4_756 ? O6 Cl1 O6 162.0(11) . 4_756 ? O5 Cl1 O6 54.3(10) . 4_756 ? O4 Cl1 O6 81.4(6) 4_756 4_756 ? O10 Cl2 Cl2 110(2) 4_755 4_755 ? O10 Cl2 O9 108(2) 4_755 . ? Cl2 Cl2 O9 142.7(15) 4_755 . ? O10 Cl2 O8 44.7(19) 4_755 . ? Cl2 Cl2 O8 98.4(9) 4_755 . ? O9 Cl2 O8 106.5(13) . . ? O10 Cl2 O7 65(2) 4_755 . ? Cl2 Cl2 O7 82.3(9) 4_755 . ? O9 Cl2 O7 116.0(12) . . ? O8 Cl2 O7 105.3(11) . . ? O10 Cl2 O10 142.0(15) 4_755 . ? Cl2 Cl2 O10 34.9(13) 4_755 . ? O9 Cl2 O10 108.4(16) . . ? O8 Cl2 O10 112.4(16) . . ? O7 Cl2 O10 108.2(15) . . ? O10 Cl2 O7 141(2) 4_755 4_755 ? Cl2 Cl2 O7 63.9(8) 4_755 4_755 ? O9 Cl2 O7 88.2(13) . 4_755 ? O8 Cl2 O7 162.1(11) . 4_755 ? O7 Cl2 O7 76.1(14) . 4_755 ? O10 Cl2 O7 51.7(13) . 4_755 ? O10 Cl2 O8 123(2) 4_755 4_755 ? Cl2 Cl2 O8 52.3(7) 4_755 4_755 ? O9 Cl2 O8 103.9(11) . 4_755 ? O8 Cl2 O8 81.8(13) . 4_755 ? O7 Cl2 O8 134.5(10) . 4_755 ? O10 Cl2 O8 34.6(11) . 4_755 ? O7 Cl2 O8 84.8(9) 4_755 4_755 ? C1 O1 Co1 110.4(6) . . ? C2 O2 Co1 117.3(6) . . ? Cl1 O4 Cl1 22.5(5) . 4_756 ? O5 O5 Cl1 81.8(8) 4_756 4_756 ? O5 O5 Cl1 62.1(7) 4_756 . ? Cl1 O5 Cl1 24.7(5) 4_756 . ? O5 O5 O6 137.7(13) 4_756 4_756 ? Cl1 O5 O6 57.1(8) 4_756 4_756 ? Cl1 O5 O6 79.9(9) . 4_756 ? Cl1 O6 O5 49.1(6) . 4_756 ? Cl1 O6 Cl1 8.3(6) . 4_756 ? O5 O6 Cl1 45.8(5) 4_756 4_756 ? O10 O7 Cl2 36.7(10) 4_755 . ? O10 O7 Cl2 58.6(7) 4_755 4_755 ? Cl2 O7 Cl2 33.8(5) . 4_755 ? O10 O8 Cl2 37.2(12) 4_755 . ? O10 O8 Cl2 53.5(9) 4_755 4_755 ? Cl2 O8 Cl2 29.3(4) . 4_755 ? Cl2 O10 O8 98(2) 4_755 4_755 ? Cl2 O10 O7 78.4(18) 4_755 4_755 ? O8 O10 O7 153(3) 4_755 4_755 ? Cl2 O10 Cl2 35.5(9) 4_755 . ? O8 O10 Cl2 92.0(16) 4_755 . ? O7 O10 Cl2 69.7(11) 4_755 . ? C25 N1 C18 110.8(8) . . ? C25 N1 C11 114.0(9) . . ? C18 N1 C11 110.9(8) . . ? C25 N1 Co1 106.1(6) . . ? C18 N1 Co1 105.8(6) . . ? C11 N1 Co1 108.8(6) . . ? C12 N2 C16 119.1(10) . . ? C12 N2 Co1 112.9(7) . . ? C16 N2 Co1 128.1(8) . . ? C23 N3 C19 117.0(9) . . ? C23 N3 Co1 129.9(7) . . ? C19 N3 Co1 113.0(7) . . ? C26 N4 C30 118.2(10) . . ? C26 N4 Co1 113.4(6) . . ? C30 N4 Co1 127.1(8) . . ? O1 C1 C6 122.8(8) . . ? O1 C1 C2 118.0(9) . . ? C6 C1 C2 119.2(9) . . ? O2 C2 C3 123.9(9) . . ? O2 C2 C1 115.7(9) . . ? C3 C2 C1 120.3(9) . . ? C2 C3 C4 120.7(9) . . ? C2 C3 C3 119.2(10) . 3_566 ? C4 C3 C3 119.9(10) . 3_566 ? O3 C4 C3 121.3(9) . . ? O3 C4 C5 119.9(9) . . ? C3 C4 C5 118.8(9) . . ? C6 C5 C10 121.1(9) . . ? C6 C5 C4 120.0(9) . . ? C10 C5 C4 118.7(10) . . ? C7 C6 C5 120.6(9) . . ? C7 C6 C1 120.0(9) . . ? C5 C6 C1 119.2(9) . . ? C6 C7 C8 117.5(10) . . ? C9 C8 C7 122.7(11) . . ? C8 C9 C10 120.3(11) . . ? C5 C10 C9 117.8(10) . . ? C12 C11 N1 115.5(9) . . ? N2 C12 C13 121.3(12) . . ? N2 C12 C11 119.1(10) . . ? C13 C12 C11 119.0(12) . . ? C14 C13 C12 120.6(16) . . ? C13 C14 C15 117.2(16) . . ? C16 C15 C14 119.7(15) . . ? C15 C16 N2 121.6(13) . . ? C15 C16 C17 118.2(12) . . ? N2 C16 C17 120.2(11) . . ? N1 C18 C19 111.0(8) . . ? C20 C19 N3 122.6(10) . . ? C20 C19 C18 123.0(10) . . ? N3 C19 C18 114.3(9) . . ? C19 C20 C21 119.5(11) . . ? C22 C21 C20 120.0(10) . . ? C21 C22 C23 118.8(11) . . ? N3 C23 C22 121.9(10) . . ? N3 C23 C24 117.1(9) . . ? C22 C23 C24 121.1(10) . . ? N1 C25 C26 110.6(9) . . ? N4 C26 C27 120.7(9) . . ? N4 C26 C25 113.3(9) . . ? C27 C26 C25 125.8(10) . . ? C28 C27 C26 119.5(11) . . ? C27 C28 C29 120.1(11) . . ? C30 C29 C28 117.8(11) . . ? C29 C30 N4 123.6(11) . . ? N5 C41 C42 178(2) . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 61.51 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.761 _refine_diff_density_min -0.712 _refine_diff_density_rms 0.096 _database_code_depnum_ccdc_archive 'CCDC 965092' ####################################################################### # # 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_Compound_4 # start Validation Reply Form _vrf_CHEMW03_Compound_4 ; PROBLEM: ALERT: CHEMW03_ALERT_2_A ALERT: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.90 <> 1.10. RESPONSE: Highly disordered solvent molecules in the crystal have not been included in the atom list. The SQUEEZE routine within PLATON has been used to treat the disordered solvent. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H72 Cl2 Co2 N10 O15' _chemical_formula_weight 1482.14 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 1 21/c 1' 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 19.0266(16) _cell_length_b 18.3969(15) _cell_length_c 20.8598(19) _cell_angle_alpha 90.00 _cell_angle_beta 106.282(9) _cell_angle_gamma 90.00 _cell_volume 7008.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 11021 _cell_measurement_theta_min 3.26 _cell_measurement_theta_max 74.8 _exptl_crystal_description 'trigonal prism' _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.86 _exptl_crystal_size_mid 0.64 _exptl_crystal_size_min 0.33 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.405 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3080 _exptl_absorpt_coefficient_mu 5.017 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.03090 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.2273 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27447 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0809 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.26 _diffrn_reflns_theta_max 75.55 _reflns_number_total 14094 _reflns_number_gt 11667 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystalmaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1699P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14094 _refine_ls_number_parameters 853 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0934 _refine_ls_R_factor_gt 0.0849 _refine_ls_wR_factor_ref 0.2350 _refine_ls_wR_factor_gt 0.2233 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.027 _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 0.72920(3) 0.78820(3) 0.28448(3) 0.01746(15) Uani 1 1 d . . . Co2 Co 0.29353(3) 0.73958(3) 0.23943(3) 0.02680(17) Uani 1 1 d . A . Cl1 Cl 0.94688(5) 0.88680(6) 0.63161(5) 0.0374(2) Uani 1 1 d . . . Cl2 Cl 0.74266(7) 0.50576(9) 0.55564(5) 0.0540(3) Uani 1 1 d . . . O1 O 0.67524(13) 0.87669(12) 0.22130(12) 0.0206(5) Uani 1 1 d . . . O4 O 0.34611(15) 0.70622(16) 0.34208(13) 0.0335(6) Uani 1 1 d . . . O2 O 0.63822(12) 0.80156(12) 0.31337(11) 0.0187(4) Uani 1 1 d . . . O5 O 0.38527(13) 0.79741(12) 0.26131(12) 0.0215(5) Uani 1 1 d . . . O3 O 0.42890(14) 0.95060(12) 0.27647(13) 0.0253(5) Uani 1 1 d . . . O6 O 0.59934(13) 0.84919(13) 0.43198(12) 0.0232(5) Uani 1 1 d . . . O10 O 0.98918(18) 0.8781(2) 0.58580(19) 0.0474(8) Uani 1 1 d . . . O7 O 0.9122(5) 0.9556(4) 0.6198(4) 0.128(3) Uani 1 1 d . . . O8 O 0.8902(3) 0.8359(4) 0.6195(3) 0.111(2) Uani 1 1 d U . . O9 O 0.9916(2) 0.8811(4) 0.6977(2) 0.097(2) Uani 1 1 d . . . O11 O 0.7931(3) 0.5025(3) 0.5191(3) 0.0839(16) Uani 1 1 d . . . O12 O 0.7107(4) 0.5779(3) 0.5576(3) 0.099(2) Uani 1 1 d . . . O14 O 0.7679(5) 0.4868(4) 0.6213(3) 0.117(3) Uani 1 1 d . . . N1 N 0.80843(16) 0.79100(15) 0.23062(15) 0.0226(6) Uani 1 1 d . . . N5 N 0.21363(19) 0.6561(2) 0.2306(2) 0.0413(9) Uani 1 1 d . . . N2 N 0.78919(16) 0.69402(16) 0.33075(15) 0.0245(6) Uani 1 1 d . . . N6 N 0.22878(17) 0.7683(2) 0.14142(17) 0.0311(7) Uani 1 1 d . . . N3 N 0.68190(17) 0.70726(15) 0.20077(15) 0.0243(6) Uani 1 1 d . . . N7 N 0.34076(19) 0.64594(16) 0.19426(16) 0.0296(7) Uani 1 1 d . . . N4 N 0.80949(16) 0.86630(16) 0.34155(16) 0.0244(6) Uani 1 1 d . . . N8 N 0.21254(19) 0.7961(2) 0.28008(18) 0.0364(8) Uani 1 1 d . . . C1 C 0.61465(17) 0.89155(15) 0.22938(15) 0.0160(6) Uani 1 1 d . . . C11 C 0.40570(18) 0.73799(18) 0.36517(17) 0.0206(6) Uani 1 1 d . . . C2 C 0.59209(17) 0.85025(15) 0.28256(15) 0.0150(5) Uani 1 1 d . . . C12 C 0.43041(17) 0.78948(16) 0.31993(16) 0.0168(6) Uani 1 1 d . . . C3 C 0.52557(16) 0.86506(15) 0.29329(14) 0.0141(5) Uani 1 1 d . . . C13 C 0.49851(16) 0.82125(15) 0.34025(15) 0.0149(5) Uani 1 1 d . . . C4 C 0.47976(17) 0.92564(15) 0.25826(16) 0.0171(6) Uani 1 1 d . . . C14 C 0.54377(16) 0.81206(16) 0.40879(15) 0.0171(6) Uani 1 1 d . . . C5 C 0.49779(18) 0.95856(16) 0.19938(16) 0.0197(6) Uani 1 1 d . . . C15 C 0.51990(17) 0.75894(16) 0.45299(16) 0.0170(6) Uani 1 1 d . . . C6 C 0.56513(18) 0.94381(15) 0.18689(16) 0.0183(6) Uani 1 1 d . . . C20 C 0.45137(17) 0.72471(17) 0.43252(16) 0.0169(6) Uani 1 1 d . . . C7 C 0.5833(2) 0.97553(18) 0.13314(18) 0.0269(7) Uani 1 1 d . . . H7 H 0.6295 0.9663 0.1257 0.032 Uiso 1 1 calc R . . C19 C 0.42877(19) 0.67841(18) 0.47543(17) 0.0228(6) Uani 1 1 d . . . H19 H 0.3817 0.6565 0.4618 0.027 Uiso 1 1 calc R . . C8 C 0.5328(3) 1.0209(2) 0.0904(2) 0.0367(9) Uani 1 1 d . . . H8 H 0.5445 1.0426 0.0533 0.044 Uiso 1 1 calc R . . C18 C 0.4755(2) 0.66426(19) 0.53861(17) 0.0248(7) Uani 1 1 d . . . H18 H 0.4605 0.6329 0.5685 0.030 Uiso 1 1 calc R . . C9 C 0.4659(3) 1.0347(2) 0.1016(2) 0.0375(9) Uani 1 1 d . . . H9 H 0.4316 1.0654 0.0717 0.045 Uiso 1 1 calc R . . C17 C 0.5440(2) 0.6964(2) 0.55750(17) 0.0290(7) Uani 1 1 d . . . H17 H 0.5763 0.6857 0.6002 0.035 Uiso 1 1 calc R . . C10 C 0.4480(2) 1.00438(18) 0.1558(2) 0.0284(7) Uani 1 1 d . . . H10 H 0.4020 1.0147 0.1632 0.034 Uiso 1 1 calc R . . C16 C 0.5664(2) 0.74370(19) 0.51558(18) 0.0253(7) Uani 1 1 d . . . H16 H 0.6134 0.7656 0.5296 0.030 Uiso 1 1 calc R . . C21 C 0.86630(19) 0.73726(19) 0.26243(19) 0.0254(7) Uani 1 1 d . . . H21A H 0.9069 0.7631 0.2944 0.031 Uiso 1 1 calc R . . H21B H 0.8860 0.7158 0.2275 0.031 Uiso 1 1 calc R . . C22 C 0.8402(2) 0.6764(2) 0.29892(18) 0.0262(7) Uani 1 1 d . . . C23 C 0.8713(3) 0.6083(2) 0.3030(2) 0.0377(9) Uani 1 1 d . . . H23 H 0.9046 0.5968 0.2779 0.045 Uiso 1 1 calc R . . C42A C 0.1556(7) 0.6637(9) 0.1701(6) 0.042(3) Uani 0.607(8) 1 d PU A 1 H42A H 0.1124 0.6853 0.1806 0.050 Uiso 0.607(8) 1 calc PR A 1 H42B H 0.1414 0.6150 0.1506 0.050 Uiso 0.607(8) 1 calc PR A 1 C43A C 0.1775(6) 0.7114(7) 0.1191(7) 0.041(3) Uani 0.607(8) 1 d PU A 1 C44A C 0.1398(5) 0.7032(8) 0.0533(5) 0.077(4) Uani 0.607(8) 1 d P A 1 H44A H 0.1020 0.6680 0.0399 0.092 Uiso 0.607(8) 1 calc PR A 1 C45A C 0.1576(7) 0.7467(9) 0.0075(5) 0.092(5) Uani 0.607(8) 1 d P A 1 H45A H 0.1336 0.7405 -0.0387 0.110 Uiso 0.607(8) 1 calc PR A 1 C46A C 0.2091(6) 0.7984(8) 0.0272(5) 0.078(4) Uani 0.607(8) 1 d P A 1 H46A H 0.2227 0.8273 -0.0051 0.093 Uiso 0.607(8) 1 calc PR A 1 C47A C 0.2428(4) 0.8097(6) 0.0956(5) 0.0405(19) Uani 0.607(8) 1 d P A 1 C24 C 0.8532(3) 0.5567(2) 0.3442(3) 0.0462(11) Uani 1 1 d . . . H24 H 0.8743 0.5095 0.3482 0.055 Uiso 1 1 calc R . . C25 C 0.8043(3) 0.5748(2) 0.3791(2) 0.0419(10) Uani 1 1 d . . . H25 H 0.7924 0.5406 0.4085 0.050 Uiso 1 1 calc R . . C26 C 0.7717(2) 0.6447(2) 0.3711(2) 0.0315(8) Uani 1 1 d . . . C27 C 0.7188(3) 0.6651(3) 0.4092(2) 0.0413(10) Uani 1 1 d . . . H27A H 0.7459 0.6797 0.4546 0.062 Uiso 1 1 calc R . . H27B H 0.6876 0.6233 0.4113 0.062 Uiso 1 1 calc R . . H27C H 0.6884 0.7057 0.3868 0.062 Uiso 1 1 calc R . . C48 C 0.2999(3) 0.8745(3) 0.1228(3) 0.0451(11) Uani 1 1 d . . . H48A H 0.3170 0.8724 0.1717 0.068 Uiso 1 1 calc R A 1 H48B H 0.2757 0.9213 0.1090 0.068 Uiso 1 1 calc R A 1 H48C H 0.3417 0.8695 0.1044 0.068 Uiso 1 1 calc R A 1 C28 C 0.7719(2) 0.7721(2) 0.16051(18) 0.0268(7) Uani 1 1 d . . . H28A H 0.8092 0.7610 0.1370 0.032 Uiso 1 1 calc R . . H28B H 0.7425 0.8140 0.1379 0.032 Uiso 1 1 calc R . . C49 C 0.2534(2) 0.5857(2) 0.2405(2) 0.0365(9) Uani 1 1 d . A . H49A H 0.2805 0.5799 0.2882 0.044 Uiso 1 1 calc R . . H49B H 0.2179 0.5453 0.2278 0.044 Uiso 1 1 calc R . . C29 C 0.7229(2) 0.70723(19) 0.15750(18) 0.0267(7) Uani 1 1 d . . . C50 C 0.3055(2) 0.5827(2) 0.1992(2) 0.0334(9) Uani 1 1 d . A . C30 C 0.7190(2) 0.6523(2) 0.1114(2) 0.0378(9) Uani 1 1 d . . . H30 H 0.7491 0.6537 0.0819 0.045 Uiso 1 1 calc R . . C51 C 0.3192(3) 0.5182(2) 0.1682(2) 0.0488(13) Uani 1 1 d . . . H51 H 0.2930 0.4751 0.1715 0.059 Uiso 1 1 calc R A . C31 C 0.6705(3) 0.5948(3) 0.1087(2) 0.0485(11) Uani 1 1 d . . . H31 H 0.6663 0.5568 0.0770 0.058 Uiso 1 1 calc R . . C52 C 0.3694(3) 0.5180(2) 0.1338(2) 0.0508(13) Uani 1 1 d . A . H52 H 0.3798 0.4749 0.1131 0.061 Uiso 1 1 calc R . . C32 C 0.6296(3) 0.5945(2) 0.1521(2) 0.0457(11) Uani 1 1 d . . . H32 H 0.5966 0.5556 0.1514 0.055 Uiso 1 1 calc R . . C53 C 0.4052(3) 0.5818(2) 0.1296(3) 0.0476(11) Uani 1 1 d . . . H53 H 0.4417 0.5825 0.1064 0.057 Uiso 1 1 calc R A . C33 C 0.6355(2) 0.6511(2) 0.1983(2) 0.0342(8) Uani 1 1 d . . . C54 C 0.3889(3) 0.6456(2) 0.1587(2) 0.0372(9) Uani 1 1 d . A . C34 C 0.5924(3) 0.6492(3) 0.2480(3) 0.0542(13) Uani 1 1 d . . . H34A H 0.6229 0.6299 0.2904 0.081 Uiso 1 1 calc R . . H34B H 0.5493 0.6181 0.2312 0.081 Uiso 1 1 calc R . . H34C H 0.5765 0.6986 0.2549 0.081 Uiso 1 1 calc R . . C55 C 0.4228(4) 0.7164(3) 0.1468(3) 0.0565(15) Uani 1 1 d . . . H55A H 0.3866 0.7451 0.1138 0.085 Uiso 1 1 calc R A . H55B H 0.4650 0.7066 0.1299 0.085 Uiso 1 1 calc R . . H55C H 0.4388 0.7435 0.1888 0.085 Uiso 1 1 calc R . . C35 C 0.8386(2) 0.86580(19) 0.2359(2) 0.0274(7) Uani 1 1 d . . . H35A H 0.8033 0.8984 0.2052 0.033 Uiso 1 1 calc R . . H35B H 0.8847 0.8659 0.2226 0.033 Uiso 1 1 calc R . . C56 C 0.1770(2) 0.6694(3) 0.2825(3) 0.0534(14) Uani 1 1 d . A . H56A H 0.2088 0.6529 0.3262 0.064 Uiso 1 1 calc R . . H56B H 0.1309 0.6410 0.2725 0.064 Uiso 1 1 calc R . . C36 C 0.85328(18) 0.89292(18) 0.30610(19) 0.0241(7) Uani 1 1 d . . . C57 C 0.1602(2) 0.7480(3) 0.2862(4) 0.0573(15) Uani 1 1 d . A . C37 C 0.9085(2) 0.9432(2) 0.3323(2) 0.0361(9) Uani 1 1 d . . . H37 H 0.9383 0.9613 0.3061 0.043 Uiso 1 1 calc R . . C58 C 0.0979(4) 0.7719(5) 0.3005(6) 0.109(4) Uani 1 1 d U . . H58 H 0.0615 0.7385 0.3047 0.131 Uiso 1 1 calc R A . C38 C 0.9189(3) 0.9663(2) 0.3976(3) 0.0443(10) Uani 1 1 d . . . H38 H 0.9557 1.0012 0.4168 0.053 Uiso 1 1 calc R . . C59 C 0.0891(4) 0.8470(5) 0.3089(7) 0.121(4) Uani 1 1 d . A . H59 H 0.0467 0.8646 0.3193 0.146 Uiso 1 1 calc R . . C39 C 0.8757(2) 0.9384(3) 0.4339(2) 0.0406(9) Uani 1 1 d . . . H39 H 0.8830 0.9532 0.4789 0.049 Uiso 1 1 calc R . . C60 C 0.1419(3) 0.8947(4) 0.3020(4) 0.0710(18) Uani 1 1 d . . . H60 H 0.1364 0.9455 0.3070 0.085 Uiso 1 1 calc R A . C40 C 0.8213(2) 0.8886(2) 0.40557(19) 0.0294(7) Uani 1 1 d . . . C61 C 0.2038(3) 0.8671(3) 0.2874(2) 0.0469(11) Uani 1 1 d . A . C41 C 0.7739(2) 0.8574(3) 0.4446(2) 0.0426(10) Uani 1 1 d . . . H41A H 0.7242 0.8508 0.4152 0.064 Uiso 1 1 calc R . . H41B H 0.7727 0.8906 0.4810 0.064 Uiso 1 1 calc R . . H41C H 0.7936 0.8103 0.4632 0.064 Uiso 1 1 calc R . . C62 C 0.2626(4) 0.9182(3) 0.2812(4) 0.077(2) Uani 1 1 d . . . H62A H 0.3027 0.8905 0.2719 0.116 Uiso 1 1 calc R A . H62B H 0.2811 0.9452 0.3231 0.116 Uiso 1 1 calc R . . H62C H 0.2425 0.9523 0.2446 0.116 Uiso 1 1 calc R . . C42B C 0.1703(9) 0.6584(8) 0.1522(9) 0.030(3) Uani 0.393(8) 1 d PU A 2 H42C H 0.1967 0.6289 0.1267 0.036 Uiso 0.393(8) 1 calc PR A 2 H42D H 0.1207 0.6377 0.1449 0.036 Uiso 0.393(8) 1 calc PR A 2 C43B C 0.1648(7) 0.7367(7) 0.1278(8) 0.024(3) Uani 0.393(8) 1 d PU A 2 C44B C 0.1003(5) 0.7632(5) 0.0860(5) 0.031(2) Uani 0.393(8) 1 d P A 2 H44B H 0.0566 0.7352 0.0765 0.038 Uiso 0.393(8) 1 calc PR A 2 C45B C 0.1006(6) 0.8320(6) 0.0581(6) 0.042(3) Uani 0.393(8) 1 d P A 2 H45B H 0.0567 0.8525 0.0305 0.051 Uiso 0.393(8) 1 calc PR A 2 C46B C 0.1663(5) 0.8701(5) 0.0712(5) 0.030(2) Uani 0.393(8) 1 d P A 2 H46B H 0.1682 0.9159 0.0507 0.036 Uiso 0.393(8) 1 calc PR A 2 C47B C 0.2287(6) 0.8407(6) 0.1146(5) 0.025(2) Uani 0.393(8) 1 d P A 2 O13 O 0.6829(6) 0.4638(7) 0.5256(7) 0.240(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0141(3) 0.0164(3) 0.0239(3) 0.00598(18) 0.0087(2) 0.00165(17) Co2 0.0213(3) 0.0255(3) 0.0259(3) 0.0092(2) -0.0062(2) -0.0110(2) Cl1 0.0146(4) 0.0475(5) 0.0513(5) 0.0112(4) 0.0116(4) -0.0029(3) Cl2 0.0443(6) 0.0919(9) 0.0327(5) -0.0039(5) 0.0219(4) -0.0015(6) O1 0.0222(11) 0.0166(10) 0.0270(11) 0.0079(9) 0.0134(9) 0.0032(8) O4 0.0243(13) 0.0412(15) 0.0285(12) 0.0141(11) -0.0031(10) -0.0190(11) O2 0.0153(10) 0.0172(10) 0.0240(10) 0.0070(9) 0.0062(8) 0.0013(8) O5 0.0195(11) 0.0201(11) 0.0209(10) 0.0078(9) -0.0009(8) -0.0036(8) O3 0.0267(12) 0.0153(11) 0.0389(13) 0.0048(10) 0.0175(10) 0.0070(9) O6 0.0201(11) 0.0267(12) 0.0224(10) -0.0010(9) 0.0052(9) -0.0102(9) O10 0.0285(15) 0.060(2) 0.060(2) -0.0084(16) 0.0220(14) -0.0107(14) O7 0.184(8) 0.105(5) 0.127(5) 0.046(4) 0.094(6) 0.100(5) O8 0.058(3) 0.184(6) 0.088(3) 0.026(4) 0.016(2) -0.083(4) O9 0.032(2) 0.205(7) 0.046(2) -0.001(3) 0.0002(16) 0.002(3) O11 0.069(3) 0.129(4) 0.072(3) 0.025(3) 0.050(2) 0.010(3) O12 0.161(6) 0.059(3) 0.110(4) 0.002(3) 0.092(5) 0.007(3) O14 0.146(6) 0.167(7) 0.046(2) 0.037(3) 0.036(3) 0.045(5) N1 0.0200(13) 0.0213(14) 0.0296(14) 0.0082(11) 0.0119(11) 0.0059(10) N5 0.0203(15) 0.0352(18) 0.056(2) 0.0149(17) -0.0091(15) -0.0104(13) N2 0.0223(14) 0.0212(13) 0.0288(14) 0.0089(12) 0.0052(11) 0.0046(11) N6 0.0179(14) 0.0403(18) 0.0284(15) 0.0070(14) -0.0046(11) -0.0027(13) N3 0.0255(14) 0.0197(14) 0.0276(14) 0.0050(11) 0.0072(11) 0.0044(11) N7 0.0335(16) 0.0158(13) 0.0338(15) 0.0074(12) 0.0002(12) -0.0064(12) N4 0.0181(13) 0.0249(14) 0.0315(14) 0.0043(12) 0.0092(11) -0.0010(11) N8 0.0224(15) 0.049(2) 0.0353(17) 0.0038(15) 0.0033(13) 0.0002(14) C1 0.0186(14) 0.0103(13) 0.0218(13) -0.0001(11) 0.0099(11) -0.0020(10) C11 0.0148(14) 0.0220(15) 0.0238(15) 0.0035(12) 0.0037(12) -0.0049(11) C2 0.0198(14) 0.0080(12) 0.0183(13) 0.0010(10) 0.0068(11) -0.0017(10) C12 0.0155(14) 0.0145(14) 0.0201(13) 0.0043(11) 0.0044(11) -0.0010(10) C3 0.0131(13) 0.0094(12) 0.0201(13) 0.0031(11) 0.0051(10) -0.0007(10) C13 0.0148(13) 0.0119(13) 0.0196(13) 0.0024(11) 0.0077(11) -0.0008(10) C4 0.0194(14) 0.0064(12) 0.0250(14) 0.0009(11) 0.0052(11) 0.0000(10) C14 0.0133(13) 0.0161(14) 0.0222(14) -0.0019(11) 0.0056(11) -0.0021(10) C5 0.0238(16) 0.0095(13) 0.0272(15) 0.0023(11) 0.0095(13) 0.0033(11) C15 0.0159(14) 0.0165(14) 0.0189(14) -0.0020(11) 0.0051(11) -0.0043(11) C6 0.0262(16) 0.0063(12) 0.0252(14) 0.0016(11) 0.0119(12) 0.0029(11) C20 0.0159(14) 0.0137(13) 0.0216(14) 0.0005(12) 0.0059(11) -0.0019(11) C7 0.0373(19) 0.0173(15) 0.0323(17) 0.0076(14) 0.0198(15) 0.0045(13) C19 0.0211(15) 0.0208(15) 0.0262(15) 0.0038(13) 0.0061(13) -0.0057(12) C8 0.059(3) 0.0225(17) 0.0326(18) 0.0173(15) 0.0199(18) 0.0113(17) C18 0.0326(18) 0.0212(15) 0.0215(15) 0.0047(13) 0.0092(13) -0.0034(13) C9 0.052(3) 0.0197(17) 0.042(2) 0.0157(16) 0.0148(19) 0.0167(16) C17 0.0315(19) 0.0305(18) 0.0200(15) 0.0056(14) -0.0011(13) -0.0065(14) C10 0.0332(18) 0.0133(14) 0.0389(18) 0.0066(14) 0.0104(15) 0.0110(13) C16 0.0253(17) 0.0220(16) 0.0247(16) 0.0022(13) 0.0007(13) -0.0070(12) C21 0.0184(15) 0.0261(17) 0.0339(17) 0.0078(14) 0.0108(13) 0.0096(13) C22 0.0235(16) 0.0241(17) 0.0315(17) 0.0059(14) 0.0083(13) 0.0071(13) C23 0.043(2) 0.0277(19) 0.041(2) 0.0048(17) 0.0111(18) 0.0160(17) C42A 0.018(5) 0.057(6) 0.039(6) 0.005(5) -0.010(4) -0.015(4) C43A 0.016(4) 0.050(7) 0.049(5) 0.004(5) -0.007(3) -0.001(4) C44A 0.042(5) 0.141(11) 0.035(4) -0.002(5) -0.011(4) -0.045(6) C45A 0.070(7) 0.156(13) 0.033(4) 0.021(6) -0.011(4) -0.055(8) C46A 0.051(6) 0.124(10) 0.046(5) 0.037(6) -0.007(4) -0.026(6) C47A 0.021(3) 0.061(6) 0.036(4) 0.017(4) 0.003(3) 0.001(3) C24 0.060(3) 0.025(2) 0.052(3) 0.0092(18) 0.013(2) 0.0150(19) C25 0.054(3) 0.028(2) 0.042(2) 0.0183(18) 0.0112(19) 0.0035(18) C26 0.0314(19) 0.0261(18) 0.0346(18) 0.0136(15) 0.0053(15) -0.0010(14) C27 0.041(2) 0.041(2) 0.045(2) 0.0229(19) 0.0191(19) 0.0038(18) C48 0.035(2) 0.041(2) 0.053(3) 0.027(2) 0.0021(19) -0.0028(18) C28 0.0257(17) 0.0311(17) 0.0264(16) 0.0083(14) 0.0121(14) 0.0099(14) C49 0.0302(19) 0.0248(18) 0.045(2) 0.0184(16) -0.0046(16) -0.0129(15) C29 0.0235(17) 0.0267(18) 0.0279(16) 0.0085(14) 0.0036(13) 0.0109(13) C50 0.036(2) 0.0197(17) 0.0328(18) 0.0140(15) -0.0098(15) -0.0093(15) C30 0.040(2) 0.036(2) 0.0322(19) -0.0048(17) 0.0012(16) 0.0139(17) C51 0.071(3) 0.0164(18) 0.038(2) 0.0096(16) -0.020(2) -0.0128(18) C31 0.059(3) 0.032(2) 0.044(2) -0.0114(19) -0.002(2) 0.007(2) C52 0.078(4) 0.024(2) 0.039(2) 0.0020(18) -0.003(2) 0.005(2) C32 0.056(3) 0.0243(19) 0.046(2) 0.0029(18) -0.003(2) -0.0019(18) C53 0.066(3) 0.026(2) 0.047(2) -0.0013(18) 0.009(2) 0.006(2) C33 0.039(2) 0.0222(17) 0.039(2) 0.0069(15) 0.0059(16) -0.0036(15) C54 0.047(2) 0.0202(18) 0.042(2) 0.0042(16) 0.0094(18) -0.0003(16) C34 0.058(3) 0.053(3) 0.056(3) 0.002(2) 0.023(2) -0.032(2) C55 0.081(4) 0.029(2) 0.080(4) -0.006(2) 0.055(3) -0.006(2) C35 0.0250(16) 0.0234(17) 0.0394(19) 0.0096(14) 0.0184(14) 0.0015(13) C56 0.0164(18) 0.053(3) 0.088(4) 0.022(3) 0.010(2) -0.0086(17) C36 0.0157(14) 0.0186(15) 0.0414(19) 0.0075(14) 0.0135(13) 0.0010(11) C57 0.0145(19) 0.063(3) 0.091(4) 0.018(3) 0.008(2) 0.0012(19) C37 0.0260(18) 0.0263(18) 0.060(3) 0.0031(18) 0.0185(17) -0.0075(15) C58 0.025(3) 0.083(5) 0.221(11) 0.009(6) 0.039(5) 0.008(3) C38 0.038(2) 0.032(2) 0.062(3) -0.008(2) 0.013(2) -0.0184(18) C59 0.036(3) 0.096(6) 0.242(14) 0.013(7) 0.054(6) 0.023(4) C39 0.033(2) 0.043(2) 0.042(2) -0.0062(19) 0.0045(17) -0.0095(18) C60 0.037(3) 0.074(4) 0.097(5) 0.003(4) 0.010(3) 0.023(3) C40 0.0222(17) 0.0333(19) 0.0289(17) 0.0038(15) 0.0008(13) -0.0022(14) C61 0.034(2) 0.061(3) 0.043(2) -0.005(2) 0.0047(18) 0.004(2) C41 0.035(2) 0.066(3) 0.0248(17) 0.0024(19) 0.0048(15) -0.015(2) C62 0.090(5) 0.041(3) 0.119(6) -0.030(3) 0.060(5) -0.012(3) C42B 0.022(7) 0.017(5) 0.038(8) 0.017(5) -0.011(5) -0.010(4) C43B 0.010(5) 0.019(6) 0.031(6) 0.010(5) -0.011(4) -0.004(4) C44B 0.019(4) 0.026(5) 0.039(5) 0.016(4) -0.008(4) -0.001(3) C45B 0.020(5) 0.042(6) 0.051(6) 0.025(5) -0.011(4) -0.001(4) C46B 0.027(5) 0.019(4) 0.040(5) 0.017(4) 0.001(4) -0.005(3) C47B 0.025(5) 0.027(5) 0.017(4) 0.007(4) -0.006(4) 0.000(4) O13 0.186(9) 0.273(12) 0.334(16) -0.241(12) 0.191(11) -0.180(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 O2 2.001(2) . ? Co1 N1 2.118(3) . ? Co1 N2 2.149(3) . ? Co1 O1 2.164(2) . ? Co1 N4 2.190(3) . ? Co1 N3 2.279(3) . ? Co1 Co2 8.1257(10) . ? Co2 O5 1.985(2) . ? Co2 N5 2.132(3) . ? Co2 N6 2.136(3) . ? Co2 O4 2.182(3) . ? Co2 N8 2.215(4) . ? Co2 N7 2.267(4) . ? Cl1 O8 1.397(4) . ? Cl1 O9 1.406(4) . ? Cl1 O7 1.417(5) . ? Cl1 O10 1.421(3) . ? Cl2 O14 1.363(5) . ? Cl2 O13 1.372(7) . ? Cl2 O11 1.383(4) . ? Cl2 O12 1.465(5) . ? O1 C1 1.241(4) . ? O4 C11 1.246(4) . ? O2 C2 1.292(4) . ? O5 C12 1.290(4) . ? O3 C4 1.224(4) . ? O6 C14 1.238(4) . ? N1 C28 1.474(5) . ? N1 C35 1.483(4) . ? N1 C21 1.490(4) . ? N5 C42A 1.431(13) . ? N5 C56 1.464(7) . ? N5 C49 1.485(6) . ? N5 C42B 1.613(18) . ? N2 C26 1.342(5) . ? N2 C22 1.361(4) . ? N6 C47A 1.307(8) . ? N6 C43B 1.307(14) . ? N6 C43A 1.418(13) . ? N6 C47B 1.444(11) . ? N3 C29 1.349(5) . ? N3 C33 1.352(5) . ? N7 C54 1.330(6) . ? N7 C50 1.361(5) . ? N4 C36 1.351(4) . ? N4 C40 1.354(5) . ? N8 C61 1.330(7) . ? N8 C57 1.365(6) . ? C1 C6 1.459(4) . ? C1 C2 1.503(4) . ? C11 C20 1.450(4) . ? C11 C12 1.503(4) . ? C2 C3 1.373(4) . ? C12 C13 1.376(4) . ? C3 C13 1.469(4) . ? C3 C4 1.476(4) . ? C13 C14 1.457(4) . ? C4 C5 1.493(4) . ? C14 C15 1.499(4) . ? C5 C10 1.397(5) . ? C5 C6 1.404(4) . ? C15 C16 1.385(5) . ? C15 C20 1.403(4) . ? C6 C7 1.391(4) . ? C20 C19 1.388(4) . ? C7 C8 1.390(6) . ? C19 C18 1.392(5) . ? C8 C9 1.382(6) . ? C18 C17 1.384(5) . ? C9 C10 1.385(5) . ? C17 C16 1.383(5) . ? C21 C22 1.513(5) . ? C22 C23 1.378(5) . ? C23 C24 1.388(7) . ? C42A C43A 1.525(18) . ? C43A C44A 1.367(15) . ? C44A C45A 1.360(15) . ? C45A C46A 1.344(16) . ? C46A C47A 1.406(14) . ? C47A C48 1.606(11) . ? C24 C25 1.373(7) . ? C25 C26 1.416(6) . ? C26 C27 1.494(6) . ? C48 C47B 1.456(11) . ? C28 C29 1.505(5) . ? C49 C50 1.485(7) . ? C29 C30 1.383(6) . ? C50 C51 1.410(7) . ? C30 C31 1.395(7) . ? C51 C52 1.346(9) . ? C31 C32 1.350(8) . ? C52 C53 1.372(7) . ? C32 C33 1.401(6) . ? C53 C54 1.397(6) . ? C33 C34 1.491(6) . ? C54 C55 1.504(6) . ? C35 C36 1.498(5) . ? C56 C57 1.487(8) . ? C36 C37 1.392(5) . ? C57 C58 1.373(8) . ? C37 C38 1.388(7) . ? C58 C59 1.408(12) . ? C38 C39 1.365(6) . ? C59 C60 1.371(11) . ? C39 C40 1.385(6) . ? C60 C61 1.391(7) . ? C40 C41 1.488(5) . ? C61 C62 1.495(8) . ? C42B C43B 1.521(19) . ? C43B C44B 1.380(16) . ? C44B C45B 1.393(14) . ? C45B C46B 1.392(13) . ? C46B C47B 1.387(14) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Co1 N1 163.95(11) . . ? O2 Co1 N2 111.05(10) . . ? N1 Co1 N2 83.71(11) . . ? O2 Co1 O1 77.78(9) . . ? N1 Co1 O1 86.87(10) . . ? N2 Co1 O1 169.00(10) . . ? O2 Co1 N4 106.63(10) . . ? N1 Co1 N4 77.33(12) . . ? N2 Co1 N4 94.76(11) . . ? O1 Co1 N4 88.68(10) . . ? O2 Co1 N3 97.01(11) . . ? N1 Co1 N3 78.25(12) . . ? N2 Co1 N3 82.15(11) . . ? O1 Co1 N3 90.39(10) . . ? N4 Co1 N3 155.57(11) . . ? O2 Co1 Co2 26.86(7) . . ? N1 Co1 Co2 142.75(9) . . ? N2 Co1 Co2 111.06(8) . . ? O1 Co1 Co2 73.62(6) . . ? N4 Co1 Co2 131.96(8) . . ? N3 Co1 Co2 70.65(8) . . ? O5 Co2 N5 164.92(12) . . ? O5 Co2 N6 108.75(11) . . ? N5 Co2 N6 83.67(14) . . ? O5 Co2 O4 78.07(9) . . ? N5 Co2 O4 90.10(12) . . ? N6 Co2 O4 172.45(12) . . ? O5 Co2 N8 108.75(13) . . ? N5 Co2 N8 79.38(16) . . ? N6 Co2 N8 88.50(14) . . ? O4 Co2 N8 86.16(13) . . ? O5 Co2 N7 94.44(11) . . ? N5 Co2 N7 76.87(15) . . ? N6 Co2 N7 88.84(13) . . ? O4 Co2 N7 93.90(12) . . ? N8 Co2 N7 156.25(13) . . ? O5 Co2 Co1 27.33(7) . . ? N5 Co2 Co1 140.24(11) . . ? N6 Co2 Co1 112.29(9) . . ? O4 Co2 Co1 75.24(7) . . ? N8 Co2 Co1 134.47(10) . . ? N7 Co2 Co1 67.74(8) . . ? O8 Cl1 O9 110.6(4) . . ? O8 Cl1 O7 105.6(5) . . ? O9 Cl1 O7 111.2(5) . . ? O8 Cl1 O10 110.9(3) . . ? O9 Cl1 O10 110.5(3) . . ? O7 Cl1 O10 107.9(3) . . ? O14 Cl2 O13 109.2(8) . . ? O14 Cl2 O11 116.0(4) . . ? O13 Cl2 O11 109.8(4) . . ? O14 Cl2 O12 103.7(4) . . ? O13 Cl2 O12 103.0(7) . . ? O11 Cl2 O12 114.3(3) . . ? C1 O1 Co1 112.53(19) . . ? C11 O4 Co2 111.4(2) . . ? C2 O2 Co1 117.36(18) . . ? C12 O5 Co2 117.79(19) . . ? C28 N1 C35 110.9(3) . . ? C28 N1 C21 111.7(3) . . ? C35 N1 C21 111.1(3) . . ? C28 N1 Co1 108.2(2) . . ? C35 N1 Co1 107.6(2) . . ? C21 N1 Co1 107.12(19) . . ? C42A N5 C56 103.0(6) . . ? C42A N5 C49 116.4(7) . . ? C56 N5 C49 111.9(4) . . ? C42A N5 C42B 19.1(6) . . ? C56 N5 C42B 122.1(7) . . ? C49 N5 C42B 105.0(7) . . ? C42A N5 Co2 111.2(6) . . ? C56 N5 Co2 107.0(3) . . ? C49 N5 Co2 107.0(2) . . ? C42B N5 Co2 102.6(6) . . ? C26 N2 C22 118.8(3) . . ? C26 N2 Co1 129.3(3) . . ? C22 N2 Co1 109.6(2) . . ? C47A N6 C43B 118.0(7) . . ? C47A N6 C43A 116.9(8) . . ? C43B N6 C43A 24.0(5) . . ? C47A N6 C47B 32.6(5) . . ? C43B N6 C47B 115.3(8) . . ? C43A N6 C47B 128.9(7) . . ? C47A N6 Co2 131.5(4) . . ? C43B N6 Co2 110.5(6) . . ? C43A N6 Co2 106.9(6) . . ? C47B N6 Co2 122.5(4) . . ? C29 N3 C33 118.0(3) . . ? C29 N3 Co1 109.6(2) . . ? C33 N3 Co1 129.9(3) . . ? C54 N7 C50 118.0(4) . . ? C54 N7 Co2 130.6(3) . . ? C50 N7 Co2 110.9(3) . . ? C36 N4 C40 118.2(3) . . ? C36 N4 Co1 112.6(2) . . ? C40 N4 Co1 129.2(2) . . ? C61 N8 C57 120.5(4) . . ? C61 N8 Co2 128.9(3) . . ? C57 N8 Co2 109.6(3) . . ? O1 C1 C6 121.9(3) . . ? O1 C1 C2 117.2(3) . . ? C6 C1 C2 120.8(3) . . ? O4 C11 C20 121.9(3) . . ? O4 C11 C12 117.6(3) . . ? C20 C11 C12 120.4(3) . . ? O2 C2 C3 125.8(3) . . ? O2 C2 C1 115.0(3) . . ? C3 C2 C1 119.1(3) . . ? O5 C12 C13 124.3(3) . . ? O5 C12 C11 115.1(3) . . ? C13 C12 C11 120.5(3) . . ? C2 C3 C13 120.8(3) . . ? C2 C3 C4 120.8(3) . . ? C13 C3 C4 118.4(2) . . ? C12 C13 C14 120.0(3) . . ? C12 C13 C3 120.2(3) . . ? C14 C13 C3 119.8(3) . . ? O3 C4 C3 122.6(3) . . ? O3 C4 C5 119.2(3) . . ? C3 C4 C5 118.3(3) . . ? O6 C14 C13 121.6(3) . . ? O6 C14 C15 119.5(3) . . ? C13 C14 C15 118.8(3) . . ? C10 C5 C6 118.9(3) . . ? C10 C5 C4 120.7(3) . . ? C6 C5 C4 120.4(3) . . ? C16 C15 C20 119.3(3) . . ? C16 C15 C14 119.2(3) . . ? C20 C15 C14 121.4(3) . . ? C7 C6 C5 121.0(3) . . ? C7 C6 C1 120.1(3) . . ? C5 C6 C1 118.8(3) . . ? C19 C20 C15 120.6(3) . . ? C19 C20 C11 121.2(3) . . ? C15 C20 C11 118.2(3) . . ? C8 C7 C6 119.1(3) . . ? C20 C19 C18 119.6(3) . . ? C9 C8 C7 120.4(3) . . ? C17 C18 C19 119.4(3) . . ? C8 C9 C10 120.8(4) . . ? C16 C17 C18 121.4(3) . . ? C9 C10 C5 119.9(3) . . ? C17 C16 C15 119.6(3) . . ? N1 C21 C22 114.2(3) . . ? N2 C22 C23 122.7(4) . . ? N2 C22 C21 116.6(3) . . ? C23 C22 C21 120.5(3) . . ? C22 C23 C24 118.8(4) . . ? N5 C42A C43A 112.1(9) . . ? C44A C43A N6 122.0(11) . . ? C44A C43A C42A 117.9(11) . . ? N6 C43A C42A 119.5(10) . . ? C45A C44A C43A 118.5(10) . . ? C46A C45A C44A 120.4(9) . . ? C45A C46A C47A 120.0(9) . . ? N6 C47A C46A 121.9(9) . . ? N6 C47A C48 115.5(7) . . ? C46A C47A C48 122.7(7) . . ? C25 C24 C23 119.1(4) . . ? C24 C25 C26 119.9(4) . . ? N2 C26 C25 120.6(4) . . ? N2 C26 C27 119.1(3) . . ? C25 C26 C27 120.3(4) . . ? C47B C48 C47A 29.1(5) . . ? N1 C28 C29 110.0(3) . . ? C50 C49 N5 110.4(3) . . ? N3 C29 C30 122.5(4) . . ? N3 C29 C28 116.1(3) . . ? C30 C29 C28 121.4(4) . . ? N7 C50 C51 121.7(4) . . ? N7 C50 C49 115.8(4) . . ? C51 C50 C49 122.4(4) . . ? C29 C30 C31 119.2(4) . . ? C52 C51 C50 119.8(4) . . ? C32 C31 C30 118.4(4) . . ? C51 C52 C53 118.2(5) . . ? C31 C32 C33 120.6(4) . . ? C52 C53 C54 121.0(5) . . ? N3 C33 C32 121.3(4) . . ? N3 C33 C34 118.2(4) . . ? C32 C33 C34 120.5(4) . . ? N7 C54 C53 121.2(4) . . ? N7 C54 C55 118.9(4) . . ? C53 C54 C55 119.8(4) . . ? N1 C35 C36 110.1(3) . . ? N5 C56 C57 110.7(4) . . ? N4 C36 C37 122.7(4) . . ? N4 C36 C35 116.1(3) . . ? C37 C36 C35 121.2(3) . . ? N8 C57 C58 120.5(6) . . ? N8 C57 C56 117.0(4) . . ? C58 C57 C56 122.3(6) . . ? C38 C37 C36 118.2(4) . . ? C57 C58 C59 118.8(7) . . ? C39 C38 C37 119.2(4) . . ? C60 C59 C58 119.8(7) . . ? C38 C39 C40 120.4(4) . . ? C59 C60 C61 118.7(7) . . ? N4 C40 C39 121.2(4) . . ? N4 C40 C41 117.7(3) . . ? C39 C40 C41 121.1(4) . . ? N8 C61 C60 121.6(5) . . ? N8 C61 C62 119.1(5) . . ? C60 C61 C62 119.2(6) . . ? C43B C42B N5 109.4(12) . . ? N6 C43B C44B 126.1(11) . . ? N6 C43B C42B 112.0(12) . . ? C44B C43B C42B 120.8(12) . . ? C43B C44B C45B 118.5(9) . . ? C46B C45B C44B 119.0(9) . . ? C47B C46B C45B 119.3(8) . . ? C46B C47B N6 121.4(8) . . ? C46B C47B C48 120.6(8) . . ? N6 C47B C48 116.7(8) . . ? _diffrn_measured_fraction_theta_max 0.970 _diffrn_reflns_theta_full 75.55 _diffrn_measured_fraction_theta_full 0.970 _refine_diff_density_max 1.146 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.119 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 406 92 ' ' 2 0.500 0.000 0.500 272 77 ' ' 3 1.000 0.500 0.500 403 91 ' ' 4 0.500 0.500 0.000 269 75 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 965093' ####################################################################### # # 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_Compound_5 # start Validation Reply Form _vrf_THETM01_Compound_5 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: Crystals of this compound were found to be very weakly diffracting at high angles and as a result the data were only included to a two theta limit of 100 degrees. Despite the paucity of high angle data, the atoms of the binuclear complex are well-defined. ; # end Validation Reply Form _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C65 H62 Co2 F24 N8 O9 P4' _chemical_formula_weight 1796.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co -2.3653 3.6143 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.9097(4) _cell_length_b 32.8461(8) _cell_length_c 13.4958(3) _cell_angle_alpha 90.00 _cell_angle_beta 100.386(2) _cell_angle_gamma 90.00 _cell_volume 7373.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 6923 _cell_measurement_theta_min 2.69 _cell_measurement_theta_max 51.27 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.619 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3640 _exptl_absorpt_coefficient_mu 5.440 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.17027 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'Enhance (Cu) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur' _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 15353 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0668 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.69 _diffrn_reflns_theta_max 49.99 _reflns_number_total 7172 _reflns_number_gt 5494 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.36 (release 02-08-2010 CrysAlis171 .NET) (compiled Aug 2 2010,13:00:58) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystalmaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Crystals of this compound were found to be very weakly diffracting at high angles and as a result the data were only included to a two theta limit of 100 degrees. Despite the paucity of high angle data, the atoms of the binuclear complex are well-defined. 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^)+(0.0425P)^2^+69.6700P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7172 _refine_ls_number_parameters 1018 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.1126 _refine_ls_R_factor_gt 0.0871 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1780 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.167 _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 C65A C 0.5292(16) 0.3413(8) 0.3211(17) 0.068(10) Uiso 0.65(4) 1 d P A 1 H65A H 0.5017 0.3456 0.3783 0.102 Uiso 0.65(4) 1 calc PR A 1 H65B H 0.5388 0.3122 0.3133 0.102 Uiso 0.65(4) 1 calc PR A 1 H65C H 0.4955 0.3518 0.2595 0.102 Uiso 0.65(4) 1 calc PR A 1 C65B C 0.578(3) 0.3224(13) 0.347(3) 0.062(17) Uiso 0.35(4) 1 d P A 2 H65D H 0.6190 0.3024 0.3381 0.093 Uiso 0.35(4) 1 calc PR A 2 H65E H 0.5305 0.3187 0.2938 0.093 Uiso 0.35(4) 1 calc PR A 2 H65F H 0.5625 0.3186 0.4128 0.093 Uiso 0.35(4) 1 calc PR A 2 O9A O 0.6138(13) 0.5111(12) 0.6744(14) 0.084(13) Uiso 0.61(9) 1 d P B 3 O9B O 0.630(3) 0.534(3) 0.682(3) 0.14(2) Uiso 0.39(9) 1 d P B 4 F12A F 0.773(5) 0.278(3) 0.330(10) 0.089(9) Uani 0.21(8) 1 d P C 5 F11A F 0.835(8) 0.262(4) 0.222(11) 0.098(9) Uani 0.21(8) 1 d P C 5 F12B F 0.7900(15) 0.2852(7) 0.384(4) 0.089(9) Uani 0.79(8) 1 d P C 6 F11B F 0.805(2) 0.2580(9) 0.233(2) 0.098(9) Uani 0.79(8) 1 d P C 6 C71 C 0.5619(11) 0.5355(6) 0.6211(12) 0.088(5) Uani 1 1 d . . . C70 C 0.4817(11) 0.5235(6) 0.6182(14) 0.117(7) Uani 1 1 d . B . H70A H 0.4803 0.5001 0.6630 0.176 Uiso 1 1 calc R . . H70B H 0.4576 0.5158 0.5491 0.176 Uiso 1 1 calc R . . H70C H 0.4513 0.5461 0.6403 0.176 Uiso 1 1 calc R . . C72 C 0.5811(12) 0.5670(5) 0.5591(15) 0.116(7) Uani 1 1 d . B . H72A H 0.5740 0.5934 0.5904 0.173 Uiso 1 1 calc R . . H72B H 0.5457 0.5655 0.4932 0.173 Uiso 1 1 calc R . . H72C H 0.6372 0.5642 0.5505 0.173 Uiso 1 1 calc R . . F20A F 0.4808(7) 0.2223(3) 0.0949(10) 0.073(5) Uiso 0.576(14) 1 d PD D 7 F19A F 0.4577(6) 0.2656(3) -0.0369(6) 0.056(4) Uiso 0.576(14) 1 d PD D 7 F21A F 0.4790(8) 0.2881(4) 0.1213(8) 0.086(5) Uiso 0.576(14) 1 d PD D 7 F24A F 0.5674(7) 0.3001(3) 0.0234(11) 0.085(5) Uiso 0.576(14) 1 d PD D 7 F22A F 0.5757(9) 0.2337(6) -0.0075(13) 0.158(9) Uiso 0.576(14) 1 d PD D 7 F23A F 0.5989(7) 0.2558(5) 0.1439(13) 0.153(9) Uiso 0.576(14) 1 d PD D 7 F19B F 0.5151(10) 0.2675(4) -0.0515(7) 0.120(9) Uiso 0.424(14) 1 d PD D 8 F22B F 0.6084(6) 0.2378(4) 0.0690(9) 0.030(5) Uiso 0.424(14) 1 d PD D 8 F23B F 0.5405(13) 0.2478(6) 0.1793(7) 0.122(10) Uiso 0.424(14) 1 d PD D 8 F21B F 0.4413(10) 0.2764(9) 0.0707(15) 0.156(12) Uiso 0.424(14) 1 d PD D 8 F24B F 0.5625(10) 0.3016(3) 0.0908(12) 0.065(6) Uiso 0.424(14) 1 d PD D 8 F20B F 0.4893(9) 0.2141(3) 0.0389(11) 0.053(5) Uiso 0.424(14) 1 d PD D 8 Co1 Co 0.77571(10) 0.63017(5) 0.92191(12) 0.0293(5) Uani 1 1 d . . . Co2 Co 0.73184(10) 0.39494(5) 0.76004(12) 0.0274(5) Uani 1 1 d . . . P1 P 0.67058(16) 0.48618(9) 0.0995(2) 0.0335(8) Uani 1 1 d . . . P2 P 0.7842(2) 0.67339(9) 0.3521(2) 0.0476(9) Uani 1 1 d . . . P4 P 0.52548(19) 0.25900(10) 0.0598(3) 0.0676(12) Uani 1 1 d D . . F3 F 0.5882(3) 0.49696(19) 0.0252(4) 0.0445(17) Uani 1 1 d . . . F1 F 0.7507(3) 0.4747(2) 0.1742(4) 0.0514(18) Uani 1 1 d . . . F2 F 0.6598(4) 0.43954(17) 0.0649(4) 0.0462(17) Uani 1 1 d . . . O1 O 0.8213(4) 0.6020(2) 1.0443(5) 0.0272(17) Uani 1 1 d . . . F4 F 0.6193(3) 0.4775(2) 0.1868(4) 0.0460(17) Uani 1 1 d . . . O4 O 0.7270(4) 0.4257(2) 0.6376(5) 0.0253(17) Uani 1 1 d . . . F6 F 0.6804(4) 0.53236(18) 0.1343(5) 0.0544(18) Uani 1 1 d . . . O5 O 0.7778(4) 0.44225(19) 0.8239(5) 0.0267(17) Uani 1 1 d . . . O3 O 0.9297(4) 0.4579(2) 0.9478(5) 0.0348(19) Uani 1 1 d . . . F5 F 0.7191(3) 0.4948(2) 0.0112(4) 0.0482(18) Uani 1 1 d . . . O2 O 0.7962(4) 0.58230(19) 0.8578(5) 0.0286(17) Uani 1 1 d . . . O6 O 0.8933(4) 0.5625(2) 0.7209(5) 0.0303(18) Uani 1 1 d . . . N1 N 0.7519(5) 0.6792(3) 0.9883(7) 0.034(2) Uani 1 1 d . . . F14 F 0.8423(5) 0.6516(2) 0.2894(5) 0.079(2) Uani 1 1 d . . . C1 C 0.8460(6) 0.5669(3) 1.0279(7) 0.024(3) Uani 1 1 d . . . N8 N 0.8318(6) 0.3718(2) 0.7418(6) 0.031(2) Uani 1 1 d . . . N6 N 0.7392(5) 0.3662(2) 0.8833(6) 0.029(2) Uani 1 1 d . . . F17 F 0.8111(5) 0.6422(2) 0.4408(5) 0.071(2) Uani 1 1 d . . . F16 F 0.7160(5) 0.6439(3) 0.3010(7) 0.105(3) Uani 1 1 d . . . N3 N 0.6702(5) 0.6132(3) 0.9360(7) 0.035(2) Uani 1 1 d . . . N2 N 0.7327(5) 0.6566(3) 0.7993(7) 0.031(2) Uani 1 1 d . . . N7 N 0.6232(5) 0.4104(2) 0.7649(6) 0.030(2) Uani 1 1 d . . . F18 F 0.8538(5) 0.7036(2) 0.4013(6) 0.091(3) Uani 1 1 d . . . N4 N 0.8787(5) 0.6547(3) 0.9216(7) 0.031(2) Uani 1 1 d . . . F13 F 0.7603(5) 0.7052(2) 0.2631(5) 0.073(2) Uani 1 1 d . . . C11 C 0.7603(6) 0.4596(3) 0.6535(8) 0.025(3) Uani 1 1 d . . . C3 C 0.8581(6) 0.5180(3) 0.8921(7) 0.022(3) Uani 1 1 d . . . C46 C 0.5665(7) 0.3873(3) 0.7062(7) 0.026(3) Uani 1 1 d . . . N5 N 0.6848(5) 0.3464(2) 0.6927(6) 0.030(2) Uani 1 1 d . . . C49 C 0.5186(7) 0.4449(3) 0.8264(8) 0.035(3) Uani 1 1 d . . . H49 H 0.5021 0.4655 0.8678 0.041 Uiso 1 1 calc R . . C44 C 0.7711(6) 0.3824(3) 0.9736(8) 0.029(3) Uani 1 1 d . . . H44 H 0.7916 0.4094 0.9779 0.035 Uiso 1 1 calc R . . C16 C 0.7646(6) 0.4887(3) 0.5740(7) 0.024(3) Uani 1 1 d . . . C43 C 0.7737(7) 0.3592(3) 1.0601(9) 0.042(3) Uani 1 1 d . . . H43 H 0.7944 0.3705 1.1244 0.051 Uiso 1 1 calc R . . C40 C 0.7130(6) 0.3281(3) 0.8752(8) 0.032(3) Uani 1 1 d . . . C52 C 0.8228(6) 0.3414(3) 0.6732(8) 0.029(3) Uani 1 1 d . . . C5 C 0.9069(5) 0.5019(3) 1.0786(7) 0.023(3) Uani 1 1 d . . . C15 C 0.8057(6) 0.5254(3) 0.5991(8) 0.029(3) Uani 1 1 d . . . C34 C 0.8933(7) 0.6876(3) 0.9838(8) 0.035(3) Uani 1 1 d . . . C12 C 0.7965(6) 0.4693(3) 0.7600(7) 0.021(2) Uani 1 1 d . . . C6 C 0.8817(6) 0.5397(3) 1.1067(7) 0.028(3) Uani 1 1 d . . . C26 C 0.7299(7) 0.6402(4) 0.7078(9) 0.042(3) Uani 1 1 d . . . H26 H 0.7526 0.6141 0.7023 0.050 Uiso 1 1 calc R . . C13 C 0.8340(6) 0.5051(3) 0.7855(7) 0.026(3) Uani 1 1 d . . . F15 F 0.7257(6) 0.6956(2) 0.4129(7) 0.099(3) Uani 1 1 d . . . C56 C 0.9046(8) 0.3811(3) 0.7900(8) 0.033(3) Uani 1 1 d . . . H56 H 0.9102 0.4024 0.8384 0.039 Uiso 1 1 calc R . . C4 C 0.9002(6) 0.4895(3) 0.9693(8) 0.027(3) Uani 1 1 d . . . C7 C 0.8894(6) 0.5505(3) 1.2071(8) 0.032(3) Uani 1 1 d . . . H7 H 0.8718 0.5766 1.2243 0.038 Uiso 1 1 calc R . . C36 C 1.0145(9) 0.6991(4) 0.9300(10) 0.057(4) Uani 1 1 d . . . H36 H 1.0620 0.7147 0.9322 0.068 Uiso 1 1 calc R . . C20 C 0.8076(6) 0.5541(3) 0.5247(8) 0.030(3) Uani 1 1 d . . . H20 H 0.8371 0.5786 0.5401 0.036 Uiso 1 1 calc R . . C2 C 0.8348(6) 0.5550(3) 0.9210(7) 0.025(3) Uani 1 1 d . . . C10 C 0.9413(6) 0.4750(3) 1.1534(8) 0.036(3) Uani 1 1 d . . . H10 H 0.9602 0.4491 1.1362 0.043 Uiso 1 1 calc R . . C23 C 0.6655(7) 0.7147(4) 0.7233(11) 0.053(4) Uani 1 1 d . . . H23 H 0.6419 0.7406 0.7303 0.063 Uiso 1 1 calc R . . C32 C 0.6273(7) 0.5831(3) 0.8857(9) 0.041(3) Uani 1 1 d . . . H32 H 0.6508 0.5663 0.8416 0.049 Uiso 1 1 calc R . . C14 C 0.8478(6) 0.5328(3) 0.7060(7) 0.026(3) Uani 1 1 d . . . C27 C 0.6954(7) 0.6674(4) 1.0553(9) 0.047(3) Uani 1 1 d . . . H27A H 0.6662 0.6916 1.0734 0.056 Uiso 1 1 calc R . . H27B H 0.7253 0.6551 1.1181 0.056 Uiso 1 1 calc R . . C41 C 0.7146(8) 0.3038(4) 0.9578(9) 0.050(3) Uani 1 1 d . . . H41 H 0.6947 0.2767 0.9512 0.060 Uiso 1 1 calc R . . C37 C 1.0016(8) 0.6663(4) 0.8658(10) 0.053(4) Uani 1 1 d . . . H37 H 1.0397 0.6588 0.8252 0.063 Uiso 1 1 calc R . . C8 C 0.9220(7) 0.5242(4) 1.2819(9) 0.043(3) Uani 1 1 d . . . H8 H 0.9268 0.5315 1.3508 0.051 Uiso 1 1 calc R . . C28 C 0.6371(7) 0.6370(4) 0.9999(9) 0.040(3) Uani 1 1 d . . . C18 C 0.7266(7) 0.5111(3) 0.4030(8) 0.042(3) Uani 1 1 d . . . H18 H 0.7005 0.5064 0.3355 0.051 Uiso 1 1 calc R . . C54 C 0.9642(8) 0.3306(3) 0.7023(9) 0.043(3) Uani 1 1 d . . . H54 H 1.0100 0.3164 0.6884 0.051 Uiso 1 1 calc R . . C35 C 0.9622(8) 0.7100(4) 0.9903(9) 0.052(4) Uani 1 1 d . . . H35 H 0.9730 0.7323 1.0355 0.063 Uiso 1 1 calc R . . C30 C 0.5146(8) 0.6010(5) 0.9601(10) 0.058(4) Uani 1 1 d . . . H30 H 0.4599 0.5972 0.9658 0.070 Uiso 1 1 calc R . . C19 C 0.7665(7) 0.5472(3) 0.4276(8) 0.040(3) Uani 1 1 d . . . H19 H 0.7660 0.5677 0.3776 0.048 Uiso 1 1 calc R . . C9 C 0.9477(6) 0.4864(4) 1.2541(8) 0.037(3) Uani 1 1 d . . . H9 H 0.9704 0.4677 1.3052 0.044 Uiso 1 1 calc R . . C17 C 0.7238(6) 0.4817(3) 0.4748(8) 0.033(3) Uani 1 1 d . . . H17 H 0.6950 0.4571 0.4579 0.040 Uiso 1 1 calc R . . C39 C 0.6807(7) 0.3137(3) 0.7701(8) 0.041(3) Uani 1 1 d . . . H39A H 0.6241 0.3051 0.7658 0.049 Uiso 1 1 calc R . . H39B H 0.7120 0.2898 0.7550 0.049 Uiso 1 1 calc R . . C31 C 0.5495(7) 0.5766(4) 0.8974(10) 0.046(3) Uani 1 1 d . . . H31 H 0.5194 0.5550 0.8619 0.055 Uiso 1 1 calc R . . C29 C 0.5603(7) 0.6312(4) 1.0151(9) 0.048(3) Uani 1 1 d . . . H29 H 0.5387 0.6475 1.0620 0.057 Uiso 1 1 calc R . . C33 C 0.8306(7) 0.6938(3) 1.0472(8) 0.040(3) Uani 1 1 d . . . H33A H 0.8270 0.7230 1.0640 0.048 Uiso 1 1 calc R . . H33B H 0.8445 0.6782 1.1108 0.048 Uiso 1 1 calc R . . C51 C 0.7382(7) 0.3342(4) 0.6217(8) 0.041(3) Uani 1 1 d . . . H51A H 0.7260 0.3506 0.5592 0.049 Uiso 1 1 calc R . . H51B H 0.7302 0.3051 0.6037 0.049 Uiso 1 1 calc R . . C42 C 0.7464(8) 0.3201(4) 1.0520(10) 0.056(4) Uani 1 1 d . . . H42 H 0.7490 0.3039 1.1107 0.067 Uiso 1 1 calc R . . C45 C 0.6028(6) 0.3584(3) 0.6408(8) 0.034(3) Uani 1 1 d . . . H45A H 0.5686 0.3339 0.6268 0.041 Uiso 1 1 calc R . . H45B H 0.6061 0.3716 0.5757 0.041 Uiso 1 1 calc R . . C38 C 0.9302(7) 0.6446(3) 0.8627(8) 0.036(3) Uani 1 1 d . . . H38 H 0.9184 0.6222 0.8177 0.043 Uiso 1 1 calc R . . C22 C 0.7038(7) 0.6936(3) 0.8078(9) 0.036(3) Uani 1 1 d . . . C50 C 0.5990(7) 0.4387(3) 0.8239(8) 0.033(3) Uani 1 1 d . . . H50 H 0.6382 0.4551 0.8652 0.040 Uiso 1 1 calc R . . C21 C 0.7171(9) 0.7104(4) 0.9122(9) 0.061(4) Uani 1 1 d . . . H21A H 0.6653 0.7202 0.9277 0.073 Uiso 1 1 calc R . . H21B H 0.7540 0.7340 0.9164 0.073 Uiso 1 1 calc R . . C48 C 0.4626(7) 0.4203(4) 0.7666(8) 0.040(3) Uani 1 1 d . . . H48 H 0.4070 0.4238 0.7675 0.048 Uiso 1 1 calc R . . C47 C 0.4866(7) 0.3911(4) 0.7068(8) 0.039(3) Uani 1 1 d . . . H47 H 0.4485 0.3740 0.6665 0.046 Uiso 1 1 calc R . . C55 C 0.9728(7) 0.3614(3) 0.7731(9) 0.039(3) Uani 1 1 d . . . H55 H 1.0243 0.3687 0.8093 0.047 Uiso 1 1 calc R . . C24 C 0.6625(8) 0.6979(4) 0.6307(11) 0.056(4) Uani 1 1 d . . . H24 H 0.6376 0.7124 0.5723 0.067 Uiso 1 1 calc R . . C25 C 0.6950(8) 0.6603(4) 0.6212(9) 0.054(4) Uani 1 1 d . . . H25 H 0.6936 0.6484 0.5568 0.065 Uiso 1 1 calc R . . C53 C 0.8881(8) 0.3207(3) 0.6519(9) 0.041(3) Uani 1 1 d . . . H53 H 0.8810 0.2997 0.6028 0.049 Uiso 1 1 calc R . . P3 P 0.8641(2) 0.27436(10) 0.3309(2) 0.0450(9) Uani 1 1 d . . . F7 F 0.8622(4) 0.31899(18) 0.2835(4) 0.0490(17) Uani 1 1 d . C . F9 F 0.8665(4) 0.2293(2) 0.3737(5) 0.067(2) Uani 1 1 d . C . F10 F 0.9207(5) 0.2894(2) 0.4297(5) 0.081(3) Uani 1 1 d . C . F8 F 0.9417(5) 0.2637(2) 0.2861(6) 0.078(2) Uani 1 1 d . C . O7 O 0.9105(6) 0.4272(3) 0.5810(8) 0.075(3) Uani 1 1 d . . . C62 C 0.9975(8) 0.3925(5) 0.4874(11) 0.074(4) Uani 1 1 d . . . H62A H 1.0384 0.3984 0.5469 0.111 Uiso 1 1 calc R . . H62B H 1.0121 0.4058 0.4283 0.111 Uiso 1 1 calc R . . H62C H 0.9941 0.3630 0.4764 0.111 Uiso 1 1 calc R . . C60 C 0.8478(9) 0.4008(4) 0.4251(12) 0.082(5) Uani 1 1 d . . . H60A H 0.7984 0.4057 0.4516 0.122 Uiso 1 1 calc R . . H60B H 0.8486 0.3724 0.4025 0.122 Uiso 1 1 calc R . . H60C H 0.8496 0.4191 0.3682 0.122 Uiso 1 1 calc R . . C61 C 0.9171(9) 0.4082(4) 0.5038(12) 0.062(4) Uani 1 1 d . . . O8 O 0.6232(6) 0.3867(3) 0.4110(7) 0.066(3) Uani 1 1 d . A . C63 C 0.6569(8) 0.3655(4) 0.2576(10) 0.064(4) Uani 1 1 d . A . H63A H 0.6786 0.3929 0.2528 0.097 Uiso 1 1 calc R . . H63B H 0.6219 0.3584 0.1939 0.097 Uiso 1 1 calc R . . H63C H 0.7013 0.3459 0.2714 0.097 Uiso 1 1 calc R . . C64 C 0.6102(8) 0.3642(4) 0.3401(11) 0.054(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 F12A 0.082(10) 0.086(10) 0.12(2) 0.045(13) 0.063(14) 0.035(8) F11A 0.12(2) 0.042(7) 0.098(11) 0.020(6) -0.066(15) -0.025(13) F12B 0.082(10) 0.086(10) 0.12(2) 0.045(13) 0.063(14) 0.035(8) F11B 0.12(2) 0.042(7) 0.098(11) 0.020(6) -0.066(15) -0.025(13) C71 0.063(12) 0.119(16) 0.075(11) 0.015(11) -0.010(9) 0.013(12) C70 0.081(14) 0.119(16) 0.140(17) 0.025(13) -0.011(12) -0.012(12) C72 0.135(18) 0.080(13) 0.140(17) -0.008(13) 0.048(14) -0.017(13) Co1 0.0331(11) 0.0175(9) 0.0343(11) 0.0016(8) -0.0021(8) -0.0012(8) Co2 0.0391(11) 0.0149(9) 0.0281(10) 0.0003(8) 0.0058(8) -0.0007(8) P1 0.0270(17) 0.0371(18) 0.0348(17) -0.0065(15) 0.0017(14) -0.0034(14) P2 0.064(2) 0.0253(18) 0.054(2) 0.0014(17) 0.0099(18) 0.0083(17) P4 0.030(2) 0.036(2) 0.128(3) -0.006(2) -0.009(2) 0.0079(17) F3 0.031(4) 0.053(4) 0.045(4) 0.001(3) -0.005(3) 0.000(3) F1 0.026(4) 0.081(5) 0.044(4) -0.006(4) -0.005(3) 0.004(3) F2 0.055(4) 0.030(4) 0.053(4) -0.003(3) 0.009(3) 0.002(3) O1 0.033(4) 0.021(4) 0.025(4) -0.002(3) -0.003(3) -0.002(4) F4 0.034(4) 0.068(5) 0.038(4) -0.008(3) 0.012(3) -0.015(3) O4 0.034(4) 0.018(4) 0.025(4) 0.003(3) 0.008(3) -0.005(4) F6 0.056(4) 0.036(4) 0.069(5) -0.017(4) 0.005(4) -0.006(3) O5 0.039(5) 0.011(4) 0.030(4) 0.002(3) 0.005(3) -0.004(3) O3 0.044(5) 0.022(4) 0.036(5) 0.001(4) 0.001(4) 0.007(4) F5 0.037(4) 0.071(5) 0.038(4) -0.005(3) 0.012(3) -0.020(3) O2 0.034(4) 0.021(4) 0.028(4) 0.007(4) -0.004(3) -0.005(4) O6 0.036(5) 0.022(4) 0.032(4) 0.002(3) 0.002(3) -0.004(4) N1 0.027(6) 0.025(5) 0.048(6) 0.004(5) 0.002(5) 0.001(4) F14 0.093(6) 0.077(6) 0.069(5) -0.007(4) 0.022(4) 0.030(5) C1 0.019(6) 0.017(7) 0.033(7) -0.013(6) -0.002(5) -0.008(5) N8 0.048(7) 0.015(5) 0.028(5) -0.008(5) 0.000(5) 0.000(5) N6 0.044(6) 0.015(5) 0.029(6) 0.010(4) 0.011(5) -0.001(4) F17 0.107(6) 0.041(4) 0.064(5) 0.017(4) 0.009(4) 0.023(4) F16 0.086(6) 0.066(6) 0.149(8) 0.021(6) -0.019(6) -0.025(5) N3 0.034(6) 0.020(5) 0.047(6) 0.015(5) -0.002(5) -0.011(5) N2 0.028(6) 0.021(6) 0.042(6) 0.006(5) -0.001(4) 0.002(4) N7 0.040(6) 0.016(5) 0.030(5) -0.004(5) 0.000(5) 0.008(5) F18 0.120(7) 0.061(5) 0.078(5) -0.005(5) -0.017(5) -0.030(5) N4 0.035(6) 0.019(5) 0.036(6) 0.002(5) 0.000(5) 0.000(5) F13 0.108(6) 0.044(4) 0.067(5) 0.013(4) 0.017(4) 0.010(4) C11 0.024(6) 0.017(7) 0.036(7) -0.001(6) 0.014(5) 0.002(5) C3 0.025(6) 0.021(6) 0.018(6) 0.006(5) 0.000(5) -0.007(5) C46 0.034(8) 0.019(6) 0.024(6) 0.004(5) 0.007(5) -0.010(6) N5 0.037(6) 0.015(5) 0.039(5) 0.002(4) 0.013(5) -0.005(4) C49 0.042(8) 0.034(7) 0.027(7) 0.002(6) 0.003(6) 0.012(6) C44 0.031(7) 0.025(6) 0.032(7) 0.000(6) 0.013(5) -0.003(5) C16 0.024(6) 0.028(7) 0.025(7) 0.007(6) 0.016(5) 0.004(5) C43 0.066(9) 0.030(8) 0.035(7) 0.009(6) 0.018(6) 0.007(7) C40 0.040(7) 0.015(7) 0.048(8) 0.008(6) 0.022(6) 0.006(6) C52 0.030(7) 0.021(6) 0.044(7) 0.008(6) 0.030(6) 0.002(6) C5 0.009(6) 0.030(7) 0.030(7) 0.007(6) 0.006(5) -0.009(5) C15 0.033(7) 0.014(6) 0.040(7) 0.007(6) 0.008(6) -0.002(5) C34 0.029(7) 0.032(7) 0.041(7) 0.005(6) -0.001(6) -0.018(6) C12 0.022(6) 0.019(6) 0.026(6) 0.003(6) 0.010(5) 0.001(5) C6 0.027(7) 0.031(7) 0.019(7) 0.000(6) -0.012(5) -0.003(6) C26 0.037(7) 0.035(7) 0.052(9) 0.005(7) 0.003(6) -0.003(6) C13 0.029(6) 0.015(6) 0.033(7) 0.012(6) -0.003(5) 0.000(5) F15 0.146(8) 0.049(5) 0.124(7) 0.032(5) 0.085(7) 0.038(5) C56 0.050(9) 0.024(7) 0.025(6) 0.007(5) 0.009(6) 0.006(7) C4 0.016(6) 0.025(7) 0.036(7) 0.004(6) -0.007(5) -0.010(5) C7 0.019(6) 0.035(7) 0.039(8) 0.002(6) 0.001(5) -0.001(5) C36 0.071(10) 0.048(9) 0.051(8) 0.001(8) 0.010(8) -0.037(8) C20 0.036(7) 0.017(6) 0.038(7) -0.002(6) 0.008(6) -0.004(5) C2 0.029(7) 0.017(6) 0.028(7) 0.002(6) 0.005(5) -0.006(5) C10 0.033(7) 0.036(7) 0.037(8) 0.013(6) 0.000(6) 0.004(6) C23 0.043(8) 0.035(8) 0.075(10) 0.022(8) -0.001(7) 0.009(6) C32 0.032(8) 0.030(7) 0.054(8) 0.017(6) -0.009(6) -0.007(6) C14 0.020(6) 0.028(7) 0.032(7) 0.003(6) 0.008(5) 0.004(6) C27 0.043(8) 0.042(8) 0.053(8) -0.006(7) 0.004(7) 0.008(7) C41 0.092(11) 0.022(7) 0.041(8) 0.000(7) 0.026(7) -0.006(7) C37 0.047(9) 0.054(9) 0.059(9) 0.010(8) 0.015(7) -0.012(7) C8 0.038(8) 0.048(8) 0.036(7) -0.007(7) -0.009(6) 0.012(7) C28 0.038(9) 0.033(8) 0.049(8) 0.006(7) 0.008(7) 0.005(7) C18 0.074(9) 0.033(8) 0.017(6) -0.002(6) 0.000(6) -0.003(7) C54 0.042(9) 0.028(7) 0.063(9) 0.010(7) 0.026(7) 0.011(6) C35 0.067(10) 0.054(9) 0.039(8) -0.017(7) 0.018(7) -0.024(8) C30 0.045(9) 0.065(10) 0.062(9) 0.021(8) 0.001(8) 0.005(9) C19 0.064(9) 0.024(7) 0.029(7) 0.007(6) 0.001(6) 0.001(6) C9 0.019(6) 0.064(9) 0.025(7) 0.020(6) -0.001(5) 0.001(6) C17 0.046(8) 0.024(6) 0.032(7) -0.002(6) 0.013(6) 0.002(6) C39 0.062(9) 0.018(6) 0.042(8) 0.000(6) 0.008(6) -0.005(6) C31 0.028(9) 0.047(8) 0.058(9) 0.025(7) -0.008(7) -0.011(7) C29 0.030(8) 0.059(9) 0.055(8) 0.007(7) 0.013(7) 0.006(7) C33 0.048(8) 0.024(7) 0.047(7) -0.007(6) 0.003(7) -0.005(6) C51 0.050(8) 0.037(7) 0.033(7) 0.002(6) 0.003(6) -0.002(6) C42 0.094(11) 0.026(8) 0.049(9) 0.024(7) 0.015(8) 0.012(7) C45 0.039(8) 0.024(6) 0.038(7) -0.001(6) 0.005(6) -0.013(6) C38 0.041(8) 0.030(7) 0.035(7) 0.011(6) 0.005(6) -0.009(7) C22 0.036(7) 0.016(7) 0.055(8) 0.015(6) 0.010(6) -0.002(6) C50 0.040(9) 0.025(7) 0.029(7) 0.007(6) -0.009(6) 0.011(6) C21 0.090(11) 0.028(7) 0.060(9) -0.001(7) 0.004(8) 0.002(7) C48 0.035(8) 0.048(8) 0.034(7) 0.005(7) 0.002(6) -0.005(7) C47 0.037(9) 0.040(8) 0.036(7) -0.010(6) 0.001(6) -0.013(6) C55 0.042(8) 0.024(7) 0.051(8) 0.009(7) 0.007(6) -0.002(6) C24 0.055(9) 0.051(10) 0.059(10) 0.023(8) 0.002(7) 0.006(8) C25 0.065(9) 0.055(10) 0.037(8) 0.010(7) -0.005(7) 0.003(8) C53 0.060(10) 0.026(7) 0.044(7) -0.005(6) 0.028(7) -0.003(7) P3 0.052(2) 0.0370(19) 0.043(2) 0.0068(16) 0.0011(18) -0.0037(17) F7 0.067(5) 0.031(4) 0.049(4) 0.002(3) 0.011(3) -0.005(3) F9 0.071(5) 0.047(4) 0.079(5) 0.027(4) 0.004(4) -0.002(4) F10 0.117(7) 0.063(5) 0.052(5) -0.017(4) -0.011(4) 0.022(5) F8 0.108(7) 0.057(5) 0.086(6) 0.007(4) 0.060(5) 0.016(5) O7 0.075(7) 0.059(7) 0.085(8) 0.001(6) 0.001(6) 0.004(5) C62 0.050(10) 0.082(11) 0.093(11) 0.009(9) 0.019(8) 0.010(8) C60 0.069(11) 0.062(10) 0.107(13) -0.040(9) -0.003(10) 0.012(8) C61 0.078(12) 0.035(8) 0.064(10) 0.006(8) -0.007(9) -0.010(8) O8 0.091(7) 0.058(6) 0.049(6) -0.005(5) 0.009(5) -0.010(5) C63 0.060(9) 0.081(11) 0.052(9) -0.003(8) 0.010(7) 0.000(8) C64 0.063(10) 0.047(9) 0.048(9) 0.009(8) 0.001(8) -0.004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C65A C64 1.54(3) . ? C65B C64 1.49(4) . ? O9A C71 1.31(3) . ? O9B C71 1.29(5) . ? F12A P3 1.54(8) . ? F11A P3 1.52(14) . ? F12B P3 1.59(2) . ? F11B P3 1.60(3) . ? C71 C72 1.40(2) . ? C71 C70 1.41(2) . ? F20A P4 1.542(8) . ? F19A P4 1.588(7) . ? F21A P4 1.567(8) . ? F24A P4 1.641(8) . ? F22A P4 1.586(10) . ? F23A P4 1.527(9) . ? F19B P4 1.507(8) . ? F22B P4 1.551(8) . ? F23B P4 1.628(9) . ? F21B P4 1.566(9) . ? F24B P4 1.559(9) . ? F20B P4 1.602(8) . ? Co1 O2 1.857(7) . ? Co1 N2 1.894(8) . ? Co1 N3 1.911(9) . ? Co1 N4 1.919(9) . ? Co1 N1 1.922(9) . ? Co1 O1 1.929(6) . ? Co2 O5 1.876(6) . ? Co2 N6 1.896(8) . ? Co2 N8 1.909(9) . ? Co2 N7 1.918(9) . ? Co2 O4 1.926(6) . ? Co2 N5 1.935(8) . ? P1 F1 1.581(6) . ? P1 F6 1.588(7) . ? P1 F5 1.589(6) . ? P1 F2 1.602(6) . ? P1 F3 1.603(6) . ? P1 F4 1.610(6) . ? P2 F16 1.568(8) . ? P2 F15 1.573(8) . ? P2 F17 1.579(7) . ? P2 F14 1.580(8) . ? P2 F13 1.588(7) . ? P2 F18 1.590(8) . ? O1 C1 1.258(11) . ? O4 C11 1.250(11) . ? O5 C12 1.317(11) . ? O3 C4 1.207(12) . ? O2 C2 1.326(11) . ? O6 C14 1.235(12) . ? N1 C27 1.480(14) . ? N1 C21 1.494(14) . ? N1 C33 1.500(13) . ? C1 C6 1.438(14) . ? C1 C2 1.473(14) . ? N8 C56 1.321(13) . ? N8 C52 1.350(13) . ? N6 C40 1.327(13) . ? N6 C44 1.350(13) . ? N3 C32 1.336(13) . ? N3 C28 1.358(14) . ? N2 C22 1.322(13) . ? N2 C26 1.339(14) . ? N7 C50 1.337(13) . ? N7 C46 1.359(12) . ? N4 C38 1.323(13) . ? N4 C34 1.363(13) . ? C11 C16 1.448(14) . ? C11 C12 1.491(14) . ? C3 C2 1.356(13) . ? C3 C4 1.484(14) . ? C3 C13 1.485(13) . ? C46 C47 1.358(15) . ? C46 C45 1.502(14) . ? N5 C51 1.485(13) . ? N5 C45 1.489(13) . ? N5 C39 1.508(13) . ? C49 C50 1.382(15) . ? C49 C48 1.388(15) . ? C44 C43 1.388(14) . ? C16 C15 1.404(14) . ? C16 C17 1.409(14) . ? C43 C42 1.363(16) . ? C40 C41 1.366(15) . ? C40 C39 1.501(15) . ? C52 C53 1.371(15) . ? C52 C51 1.494(15) . ? C5 C6 1.385(14) . ? C5 C10 1.389(14) . ? C5 C4 1.516(14) . ? C15 C20 1.383(14) . ? C15 C14 1.508(14) . ? C34 C35 1.367(15) . ? C34 C33 1.491(15) . ? C12 C13 1.351(13) . ? C6 C7 1.385(14) . ? C26 C25 1.378(15) . ? C13 C14 1.457(14) . ? C56 C55 1.377(15) . ? C7 C8 1.369(15) . ? C36 C35 1.354(17) . ? C36 C37 1.374(17) . ? C20 C19 1.387(14) . ? C10 C9 1.395(15) . ? C23 C24 1.358(17) . ? C23 C22 1.392(15) . ? C32 C31 1.370(16) . ? C27 C28 1.505(16) . ? C41 C42 1.394(16) . ? C37 C38 1.398(16) . ? C8 C9 1.389(15) . ? C28 C29 1.364(16) . ? C18 C17 1.376(14) . ? C18 C19 1.376(15) . ? C54 C55 1.381(16) . ? C54 C53 1.382(16) . ? C30 C31 1.374(17) . ? C30 C29 1.388(17) . ? C22 C21 1.493(16) . ? C48 C47 1.360(15) . ? C24 C25 1.368(17) . ? P3 F10 1.574(8) . ? P3 F8 1.581(8) . ? P3 F9 1.586(7) . ? P3 F7 1.598(7) . ? O7 C61 1.236(16) . ? C62 C61 1.508(19) . ? C60 C61 1.454(18) . ? O8 C64 1.198(14) . ? C63 C64 1.478(18) . ? 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 O9B C71 O9A 36(3) . . ? O9B C71 C72 98(4) . . ? O9A C71 C72 125(2) . . ? O9B C71 C70 139(3) . . ? O9A C71 C70 113(2) . . ? C72 C71 C70 121.1(16) . . ? O2 Co1 N2 93.1(4) . . ? O2 Co1 N3 93.1(4) . . ? N2 Co1 N3 90.1(4) . . ? O2 Co1 N4 96.3(4) . . ? N2 Co1 N4 90.7(4) . . ? N3 Co1 N4 170.5(4) . . ? O2 Co1 N1 178.6(3) . . ? N2 Co1 N1 86.8(4) . . ? N3 Co1 N1 85.4(4) . . ? N4 Co1 N1 85.1(4) . . ? O2 Co1 O1 85.0(3) . . ? N2 Co1 O1 178.1(4) . . ? N3 Co1 O1 90.6(3) . . ? N4 Co1 O1 88.9(3) . . ? N1 Co1 O1 95.1(3) . . ? O5 Co2 N6 93.0(3) . . ? O5 Co2 N8 94.9(3) . . ? N6 Co2 N8 89.7(4) . . ? O5 Co2 N7 94.9(3) . . ? N6 Co2 N7 90.8(4) . . ? N8 Co2 N7 170.1(4) . . ? O5 Co2 O4 84.8(3) . . ? N6 Co2 O4 177.8(4) . . ? N8 Co2 O4 90.0(3) . . ? N7 Co2 O4 89.9(3) . . ? O5 Co2 N5 179.3(3) . . ? N6 Co2 N5 87.6(4) . . ? N8 Co2 N5 84.8(4) . . ? N7 Co2 N5 85.3(4) . . ? O4 Co2 N5 94.5(3) . . ? F1 P1 F6 90.4(4) . . ? F1 P1 F5 91.2(3) . . ? F6 P1 F5 90.7(4) . . ? F1 P1 F2 89.9(4) . . ? F6 P1 F2 179.3(4) . . ? F5 P1 F2 89.9(4) . . ? F1 P1 F3 178.6(4) . . ? F6 P1 F3 90.4(4) . . ? F5 P1 F3 90.0(3) . . ? F2 P1 F3 89.3(3) . . ? F1 P1 F4 90.2(3) . . ? F6 P1 F4 89.6(4) . . ? F5 P1 F4 178.5(4) . . ? F2 P1 F4 89.8(4) . . ? F3 P1 F4 88.6(3) . . ? F16 P2 F15 92.0(6) . . ? F16 P2 F17 91.1(5) . . ? F15 P2 F17 91.6(4) . . ? F16 P2 F14 87.8(5) . . ? F15 P2 F14 179.0(5) . . ? F17 P2 F14 89.4(4) . . ? F16 P2 F13 90.4(5) . . ? F15 P2 F13 89.6(4) . . ? F17 P2 F13 178.1(5) . . ? F14 P2 F13 89.4(4) . . ? F16 P2 F18 178.6(6) . . ? F15 P2 F18 88.9(5) . . ? F17 P2 F18 89.9(4) . . ? F14 P2 F18 91.3(5) . . ? F13 P2 F18 88.5(4) . . ? F19B P4 F23A 133.4(9) . . ? F19B P4 F20A 118.5(7) . . ? F23A P4 F20A 95.4(6) . . ? F19B P4 F22B 96.0(6) . . ? F23A P4 F22B 46.2(7) . . ? F20A P4 F22B 96.3(7) . . ? F19B P4 F24B 94.0(6) . . ? F23A P4 F24B 68.2(8) . . ? F20A P4 F24B 144.5(8) . . ? F22B P4 F24B 93.9(8) . . ? F19B P4 F21B 94.7(6) . . ? F23A P4 F21B 125.9(10) . . ? F20A P4 F21B 75.7(12) . . ? F22B P4 F21B 168.9(8) . . ? F24B P4 F21B 88.6(14) . . ? F19B P4 F21A 115.8(7) . . ? F23A P4 F21A 93.8(6) . . ? F20A P4 F21A 89.6(8) . . ? F22B P4 F21A 139.8(6) . . ? F24B P4 F21A 61.7(8) . . ? F21B P4 F21A 34.5(10) . . ? F19B P4 F22A 60.3(8) . . ? F23A P4 F22A 86.7(9) . . ? F20A P4 F22A 96.3(10) . . ? F22B P4 F22A 40.6(6) . . ? F24B P4 F22A 113.2(11) . . ? F21B P4 F22A 146.6(11) . . ? F21A P4 F22A 174.1(10) . . ? F19B P4 F19A 38.7(6) . . ? F23A P4 F19A 171.6(8) . . ? F20A P4 F19A 92.2(5) . . ? F22B P4 F19A 129.5(6) . . ? F24B P4 F19A 107.0(7) . . ? F21B P4 F19A 59.6(8) . . ? F21A P4 F19A 89.7(5) . . ? F22A P4 F19A 89.0(6) . . ? F19B P4 F20B 91.4(6) . . ? F23A P4 F20B 107.5(8) . . ? F20A P4 F20B 30.9(6) . . ? F22B P4 F20B 84.9(8) . . ? F24B P4 F20B 174.6(7) . . ? F21B P4 F20B 91.6(13) . . ? F21A P4 F20B 116.2(8) . . ? F22A P4 F20B 69.1(10) . . ? F19A P4 F20B 77.6(6) . . ? F19B P4 F23B 176.7(8) . . ? F23A P4 F23B 44.5(8) . . ? F20A P4 F23B 61.1(7) . . ? F22B P4 F23B 80.9(8) . . ? F24B P4 F23B 87.3(9) . . ? F21B P4 F23B 88.4(6) . . ? F21A P4 F23B 67.4(8) . . ? F22A P4 F23B 116.4(9) . . ? F19A P4 F23B 143.6(8) . . ? F20B P4 F23B 87.4(6) . . ? F19B P4 F24A 61.8(7) . . ? F23A P4 F24A 86.7(8) . . ? F20A P4 F24A 175.8(8) . . ? F22B P4 F24A 87.8(7) . . ? F24B P4 F24A 33.6(6) . . ? F21B P4 F24A 100.2(12) . . ? F21A P4 F24A 86.7(8) . . ? F22A P4 F24A 87.5(10) . . ? F19A P4 F24A 85.9(5) . . ? F20B P4 F24A 151.3(8) . . ? F23B P4 F24A 118.8(8) . . ? C1 O1 Co1 112.5(6) . . ? C11 O4 Co2 111.8(6) . . ? C12 O5 Co2 112.8(6) . . ? C2 O2 Co1 112.6(6) . . ? C27 N1 C21 112.5(9) . . ? C27 N1 C33 111.7(9) . . ? C21 N1 C33 110.3(9) . . ? C27 N1 Co1 106.0(7) . . ? C21 N1 Co1 110.1(7) . . ? C33 N1 Co1 105.9(6) . . ? O1 C1 C6 123.3(9) . . ? O1 C1 C2 115.3(9) . . ? C6 C1 C2 121.4(9) . . ? C56 N8 C52 119.2(9) . . ? C56 N8 Co2 127.7(8) . . ? C52 N8 Co2 113.0(7) . . ? C40 N6 C44 121.3(9) . . ? C40 N6 Co2 115.4(7) . . ? C44 N6 Co2 123.2(7) . . ? C32 N3 C28 120.0(10) . . ? C32 N3 Co1 126.6(9) . . ? C28 N3 Co1 113.2(7) . . ? C22 N2 C26 119.7(9) . . ? C22 N2 Co1 115.7(8) . . ? C26 N2 Co1 124.5(8) . . ? C50 N7 C46 118.5(9) . . ? C50 N7 Co2 127.0(7) . . ? C46 N7 Co2 114.3(7) . . ? C38 N4 C34 120.2(10) . . ? C38 N4 Co1 126.2(8) . . ? C34 N4 Co1 113.3(8) . . ? O4 C11 C16 122.8(9) . . ? O4 C11 C12 116.8(9) . . ? C16 C11 C12 120.5(9) . . ? C2 C3 C4 119.5(9) . . ? C2 C3 C13 119.4(9) . . ? C4 C3 C13 120.9(9) . . ? C47 C46 N7 122.8(10) . . ? C47 C46 C45 125.1(10) . . ? N7 C46 C45 112.0(9) . . ? C51 N5 C45 113.0(8) . . ? C51 N5 C39 111.4(8) . . ? C45 N5 C39 111.0(8) . . ? C51 N5 Co2 106.2(6) . . ? C45 N5 Co2 105.8(6) . . ? C39 N5 Co2 109.1(6) . . ? C50 C49 C48 118.1(11) . . ? N6 C44 C43 119.3(10) . . ? C15 C16 C17 120.4(9) . . ? C15 C16 C11 118.4(9) . . ? C17 C16 C11 121.0(9) . . ? C42 C43 C44 119.4(11) . . ? N6 C40 C41 121.8(10) . . ? N6 C40 C39 115.7(9) . . ? C41 C40 C39 122.5(10) . . ? N8 C52 C53 121.1(10) . . ? N8 C52 C51 114.6(10) . . ? C53 C52 C51 124.2(11) . . ? C6 C5 C10 118.7(10) . . ? C6 C5 C4 122.3(9) . . ? C10 C5 C4 118.9(10) . . ? C20 C15 C16 119.0(9) . . ? C20 C15 C14 121.1(9) . . ? C16 C15 C14 119.9(9) . . ? N4 C34 C35 121.6(11) . . ? N4 C34 C33 113.2(9) . . ? C35 C34 C33 125.1(11) . . ? O5 C12 C13 125.3(9) . . ? O5 C12 C11 112.4(8) . . ? C13 C12 C11 121.6(9) . . ? C7 C6 C5 121.3(9) . . ? C7 C6 C1 121.1(10) . . ? C5 C6 C1 117.7(9) . . ? N2 C26 C25 121.9(11) . . ? C12 C13 C14 119.0(9) . . ? C12 C13 C3 122.0(9) . . ? C14 C13 C3 118.9(9) . . ? N8 C56 C55 122.9(10) . . ? O3 C4 C3 122.7(10) . . ? O3 C4 C5 120.2(9) . . ? C3 C4 C5 117.0(10) . . ? C8 C7 C6 120.9(10) . . ? C35 C36 C37 122.7(12) . . ? C15 C20 C19 120.2(10) . . ? O2 C2 C3 123.8(9) . . ? O2 C2 C1 114.3(9) . . ? C3 C2 C1 121.8(9) . . ? C5 C10 C9 119.1(11) . . ? C24 C23 C22 119.1(12) . . ? N3 C32 C31 120.1(12) . . ? O6 C14 C13 123.4(9) . . ? O6 C14 C15 117.1(9) . . ? C13 C14 C15 119.5(9) . . ? N1 C27 C28 108.0(10) . . ? C40 C41 C42 117.9(11) . . ? C36 C37 C38 117.2(12) . . ? C7 C8 C9 118.1(10) . . ? N3 C28 C29 122.0(11) . . ? N3 C28 C27 112.9(10) . . ? C29 C28 C27 125.0(12) . . ? C17 C18 C19 120.9(10) . . ? C55 C54 C53 119.0(11) . . ? C36 C35 C34 117.4(12) . . ? C31 C30 C29 119.2(13) . . ? C18 C19 C20 120.6(10) . . ? C8 C9 C10 122.0(10) . . ? C18 C17 C16 118.8(10) . . ? C40 C39 N5 112.1(8) . . ? C32 C31 C30 120.5(12) . . ? C28 C29 C30 118.1(13) . . ? C34 C33 N1 107.9(9) . . ? N5 C51 C52 107.4(9) . . ? C43 C42 C41 120.3(11) . . ? N5 C45 C46 109.6(8) . . ? N4 C38 C37 120.8(11) . . ? N2 C22 C23 120.8(11) . . ? N2 C22 C21 115.4(10) . . ? C23 C22 C21 123.8(11) . . ? N7 C50 C49 121.7(10) . . ? C22 C21 N1 111.6(9) . . ? C47 C48 C49 120.7(11) . . ? C46 C47 C48 118.2(10) . . ? C56 C55 C54 118.3(11) . . ? C23 C24 C25 120.2(12) . . ? C24 C25 C26 118.1(12) . . ? C52 C53 C54 119.6(11) . . ? F11A P3 F12A 82(5) . . ? F11A P3 F10 161(6) . . ? F12A P3 F10 116(6) . . ? F11A P3 F8 74(6) . . ? F12A P3 F8 156(6) . . ? F10 P3 F8 88.5(5) . . ? F11A P3 F9 94(4) . . ? F12A P3 F9 92(3) . . ? F10 P3 F9 90.7(4) . . ? F8 P3 F9 87.9(4) . . ? F11A P3 F12B 111(5) . . ? F12A P3 F12B 28(4) . . ? F10 P3 F12B 87.5(18) . . ? F8 P3 F12B 175.9(18) . . ? F9 P3 F12B 90.9(7) . . ? F11A P3 F7 83(4) . . ? F12A P3 F7 89(3) . . ? F10 P3 F7 91.0(4) . . ? F8 P3 F7 90.5(4) . . ? F9 P3 F7 177.7(4) . . ? F12B P3 F7 90.8(7) . . ? F11A P3 F11B 21(5) . . ? F12A P3 F11B 63(5) . . ? F10 P3 F11B 177.8(15) . . ? F8 P3 F11B 92.9(16) . . ? F9 P3 F11B 87.7(11) . . ? F12B P3 F11B 91.0(12) . . ? F7 P3 F11B 90.7(11) . . ? O7 C61 C60 121.2(15) . . ? O7 C61 C62 121.2(13) . . ? C60 C61 C62 117.6(14) . . ? O8 C64 C63 122.6(12) . . ? O8 C64 C65B 122.5(19) . . ? C63 C64 C65B 109(2) . . ? O8 C64 C65A 117.5(15) . . ? C63 C64 C65A 118.0(14) . . ? C65B C64 C65A 40.1(16) . . ? _diffrn_measured_fraction_theta_max 0.946 _diffrn_reflns_theta_full 49.99 _diffrn_measured_fraction_theta_full 0.946 _refine_diff_density_max 0.880 _refine_diff_density_min -0.858 _refine_diff_density_rms 0.087 _database_code_depnum_ccdc_archive 'CCDC 965094' ####################################################################### # # 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_Compound_6 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H60 Co2 F12 N8 O12 P2' _chemical_formula_weight 1480.95 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.577(4) _cell_length_b 15.479(4) _cell_length_c 22.795(5) _cell_angle_alpha 90.00 _cell_angle_beta 97.642(6) _cell_angle_gamma 90.00 _cell_volume 6147(3) _cell_formula_units_Z 4 _cell_measurement_temperature 130(2) _cell_measurement_reflns_used 2607 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 19.8 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.600 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3032 _exptl_absorpt_coefficient_mu 0.698 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8042 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details ; SADABS - Bruker/Siemens area detector absorption and other corrections - V2.03 (Bruker, 2001). The ratio of minimum to maximum transmission is 0.8042. The \l/2 correction is 0.0015. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38443 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.1235 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.38 _diffrn_reflns_theta_max 27.55 _reflns_number_total 14015 _reflns_number_gt 7026 _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, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Crystalmaker _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14015 _refine_ls_number_parameters 825 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1515 _refine_ls_R_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.2634 _refine_ls_wR_factor_gt 0.2337 _refine_ls_goodness_of_fit_ref 0.978 _refine_ls_restrained_S_all 0.982 _refine_ls_shift/su_max 0.003 _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 P1 P 0.93270(13) 0.96854(16) 0.86963(11) 0.0724(6) Uani 1 1 d D . . F1B F 0.9139(6) 0.9272(6) 0.9260(4) 0.087(3) Uiso 0.556(10) 1 d P A 3 F3A F 0.9513(7) 0.9929(7) 0.8034(5) 0.111(4) Uiso 0.556(10) 1 d P A 3 F2A F 0.8697(7) 1.0333(8) 0.8612(6) 0.110(4) Uiso 0.556(10) 1 d P A 3 F5 F 0.9984(6) 1.0246(7) 0.8924(6) 0.097(4) Uiso 0.556(10) 1 d P A 3 F6A F 0.8731(5) 0.9008(7) 0.8342(4) 0.097(4) Uiso 0.556(10) 1 d P A 3 F1A F 0.8684(11) 0.9422(10) 0.9082(7) 0.123(6) Uiso 0.444(10) 1 d P A 4 F2B F 0.8940(8) 1.0632(8) 0.8874(6) 0.094(4) Uiso 0.444(10) 1 d PD A 4 F3B F 0.9929(8) 1.0296(9) 0.8422(7) 0.115(5) Uiso 0.444(10) 1 d P A 4 F5B F 0.9883(11) 0.9968(13) 0.9315(9) 0.155(7) Uiso 0.444(10) 1 d P A 4 F6B F 0.8771(9) 0.9793(11) 0.8163(7) 0.124(6) Uiso 0.444(10) 1 d P A 4 F4 F 0.9856(4) 0.8898(4) 0.8651(3) 0.127(2) Uani 1 1 d . A . O9 O 0.4553(3) 0.7100(4) 0.2524(2) 0.0765(15) Uiso 1 1 d . . . P2 P 0.5748(4) 0.6872(6) 0.9725(3) 0.074(3) Uiso 0.378(13) 1 d PD B 1 F11 F 0.5169(12) 0.7621(11) 0.9500(12) 0.177(10) Uiso 0.378(13) 1 d PD B 1 F7 F 0.6377(15) 0.6172(17) 1.0080(11) 0.168(9) Uiso 0.378(13) 1 d P B 1 F8 F 0.5478(14) 0.6887(18) 1.0353(11) 0.158(9) Uiso 0.378(13) 1 d P B 1 F10A F 0.5061(10) 0.6143(10) 0.9547(8) 0.115(6) Uiso 0.378(13) 1 d PD B 1 F12A F 0.6297(17) 0.771(2) 0.9719(14) 0.208(12) Uiso 0.378(13) 1 d P B 1 P2B P 0.5745(6) 0.6390(8) 0.9847(4) 0.161(3) Uiso 0.622(13) 1 d PD B 2 F11B F 0.5242(11) 0.7257(13) 0.9933(12) 0.237(9) Uiso 0.622(13) 1 d PD B 2 F7B F 0.6288(9) 0.5566(11) 0.9712(8) 0.194(7) Uiso 0.622(13) 1 d P B 2 F8B F 0.5797(10) 0.6152(13) 1.0514(7) 0.197(7) Uiso 0.622(13) 1 d P B 2 F10B F 0.5062(10) 0.5674(12) 0.9851(9) 0.232(8) Uiso 0.622(13) 1 d PD B 2 F12B F 0.6438(7) 0.7199(9) 0.9891(5) 0.132(4) Uiso 0.622(13) 1 d PD B 2 F9 F 0.5802(6) 0.6628(9) 0.9138(3) 0.241(6) Uani 1 1 d . . . Co2 Co 0.30748(4) 0.83452(4) 0.69522(3) 0.0296(2) Uani 1 1 d . . . Co1 Co 0.65143(4) 0.95255(5) 0.67365(3) 0.0386(2) Uani 1 1 d . . . O8 O 0.3571(2) 0.9524(2) 0.58523(15) 0.0327(8) Uani 1 1 d . . . O4 O 0.26070(19) 0.9185(2) 0.64401(16) 0.0311(8) Uani 1 1 d . . . O5 O 0.39244(19) 0.9074(2) 0.70880(16) 0.0311(8) Uani 1 1 d . . . N5 N 0.2183(2) 0.7618(3) 0.6831(2) 0.0331(10) Uani 1 1 d . . . C13 C 0.4155(3) 1.0563(3) 0.7018(2) 0.0284(11) Uani 1 1 d . . . O6 O 0.4275(2) 1.2034(2) 0.68361(18) 0.0419(10) Uani 1 1 d . . . N6 N 0.3554(3) 0.7477(3) 0.74722(19) 0.0313(10) Uani 1 1 d . . . O1 O 0.6797(2) 0.9929(3) 0.75242(18) 0.0488(11) Uani 1 1 d . . . N8 N 0.2578(3) 0.8844(3) 0.7570(2) 0.0328(10) Uani 1 1 d . . . C15 C 0.3156(3) 1.1396(3) 0.6363(2) 0.0266(11) Uani 1 1 d . . . C16 C 0.2763(3) 1.0648(3) 0.6176(2) 0.0278(11) Uani 1 1 d . . . C12 C 0.3771(3) 0.9826(3) 0.6842(2) 0.0273(11) Uani 1 1 d . . . O3 O 0.4277(3) 1.1354(3) 0.81596(19) 0.0562(12) Uani 1 1 d . . . N7 N 0.3408(3) 0.7707(3) 0.63151(19) 0.0330(10) Uani 1 1 d . . . N2 N 0.6172(3) 0.9149(3) 0.59339(19) 0.0352(11) Uani 1 1 d . . . O2 O 0.5503(2) 0.9648(3) 0.68900(16) 0.0401(10) Uani 1 1 d . . . C3 C 0.4838(3) 1.0544(3) 0.7473(2) 0.0287(11) Uani 1 1 d . . . C20 C 0.2825(3) 1.2181(4) 0.6212(2) 0.0338(12) Uani 1 1 d . . . H20 H 0.3093 1.2697 0.6334 0.041 Uiso 1 1 calc R . . C2 C 0.5464(3) 1.0076(4) 0.7376(2) 0.0353(13) Uani 1 1 d . . . C11 C 0.3132(3) 0.9781(3) 0.6328(2) 0.0281(11) Uani 1 1 d . . . N4 N 0.6585(3) 1.0676(4) 0.6448(2) 0.0518(14) Uani 1 1 d . . . N3 N 0.6672(3) 0.8355(3) 0.7017(2) 0.0433(12) Uani 1 1 d . . . C42 C 0.3121(3) 0.6776(4) 0.7505(2) 0.0353(13) Uani 1 1 d . . . O7 O 0.6004(3) 0.9094(3) 0.8073(2) 0.0607(13) Uani 1 1 d . . . C17 C 0.2036(3) 1.0718(4) 0.5840(2) 0.0353(13) Uani 1 1 d . . . H17 H 0.1767 1.0208 0.5705 0.042 Uiso 1 1 calc R . . C46 C 0.4263(3) 0.7487(4) 0.7736(3) 0.0382(13) Uani 1 1 d . . . H46 H 0.4559 0.7998 0.7720 0.046 Uiso 1 1 calc R . . N1 N 0.7555(3) 0.9374(4) 0.6527(3) 0.0525(14) Uani 1 1 d . . . C43 C 0.3414(4) 0.6047(4) 0.7785(3) 0.0412(14) Uani 1 1 d . . . H43 H 0.3104 0.5546 0.7795 0.049 Uiso 1 1 calc R . . C14 C 0.3913(3) 1.1346(3) 0.6747(2) 0.0285(11) Uani 1 1 d . . . C52 C 0.4121(3) 0.7659(4) 0.6182(2) 0.0385(13) Uani 1 1 d . . . H52 H 0.4505 0.8027 0.6380 0.046 Uiso 1 1 calc R . . C45 C 0.4593(4) 0.6780(4) 0.8037(3) 0.0465(15) Uani 1 1 d . . . H45 H 0.5106 0.6802 0.8230 0.056 Uiso 1 1 calc R . . C24 C 0.6723(3) 0.8863(4) 0.5629(3) 0.0388(14) Uani 1 1 d . . . C4 C 0.4848(3) 1.1000(4) 0.8016(3) 0.0388(13) Uani 1 1 d . . . C41 C 0.2299(3) 0.6863(3) 0.7237(3) 0.0356(13) Uani 1 1 d . . . H41A H 0.2137 0.6330 0.7015 0.043 Uiso 1 1 calc R . . H41B H 0.1973 0.6931 0.7557 0.043 Uiso 1 1 calc R . . C48 C 0.2856(4) 0.7202(4) 0.6034(2) 0.0420(14) Uani 1 1 d . . . C6 C 0.6244(3) 1.0626(4) 0.8313(3) 0.0443(15) Uani 1 1 d . . . C54 C 0.1821(3) 0.8698(4) 0.7503(2) 0.0364(13) Uani 1 1 d . . . C53 C 0.1530(3) 0.8163(3) 0.6973(3) 0.0362(13) Uani 1 1 d . . . H53A H 0.1099 0.7794 0.7059 0.043 Uiso 1 1 calc R . . H53B H 0.1346 0.8541 0.6633 0.043 Uiso 1 1 calc R . . C25 C 0.6563(4) 0.8548(5) 0.5072(3) 0.0536(18) Uani 1 1 d . . . H25 H 0.6961 0.8330 0.4870 0.064 Uiso 1 1 calc R . . C10 C 0.5631(5) 1.1657(5) 0.8872(3) 0.066(2) Uani 1 1 d . . . H10 H 0.5191 1.1978 0.8940 0.080 Uiso 1 1 calc R . . C19 C 0.2116(3) 1.2228(4) 0.5892(2) 0.0387(14) Uani 1 1 d . . . H19 H 0.1896 1.2779 0.5795 0.046 Uiso 1 1 calc R . . C18 C 0.1712(3) 1.1498(4) 0.5705(2) 0.0391(14) Uani 1 1 d . . . H18 H 0.1215 1.1540 0.5485 0.047 Uiso 1 1 calc R . . C44 C 0.4160(4) 0.6045(4) 0.8052(3) 0.0490(16) Uani 1 1 d . . . H44 H 0.4374 0.5540 0.8245 0.059 Uiso 1 1 calc R . . C49 C 0.3016(4) 0.6614(4) 0.5604(3) 0.0485(16) Uani 1 1 d . . . H49 H 0.2623 0.6256 0.5408 0.058 Uiso 1 1 calc R . . C47 C 0.2091(3) 0.7349(4) 0.6199(2) 0.0386(13) Uani 1 1 d . . . H47A H 0.1783 0.6812 0.6144 0.046 Uiso 1 1 calc R . . H47B H 0.1823 0.7806 0.5947 0.046 Uiso 1 1 calc R . . C22 C 0.3105(4) 0.9252(4) 0.5330(3) 0.0426(14) Uani 1 1 d . . . H22A H 0.3432 0.9090 0.5031 0.064 Uiso 1 1 calc R . . H22B H 0.2763 0.9724 0.5178 0.064 Uiso 1 1 calc R . . H22C H 0.2797 0.8752 0.5419 0.064 Uiso 1 1 calc R . . C30 C 0.7416(4) 0.8119(4) 0.7095(3) 0.0492(16) Uani 1 1 d . . . C5 C 0.5592(4) 1.1087(4) 0.8413(3) 0.0455(15) Uani 1 1 d . . . C55 C 0.1359(4) 0.9038(4) 0.7891(3) 0.0454(15) Uani 1 1 d . . . H55 H 0.0821 0.8937 0.7834 0.054 Uiso 1 1 calc R . . C58 C 0.2901(4) 0.9304(4) 0.8027(2) 0.0398(14) Uani 1 1 d . . . H58 H 0.3440 0.9400 0.8077 0.048 Uiso 1 1 calc R . . C34 C 0.6120(4) 0.7773(5) 0.7070(3) 0.0560(18) Uani 1 1 d . . . H34 H 0.5596 0.7943 0.7007 0.067 Uiso 1 1 calc R . . C40 C 0.6020(4) 1.1256(5) 0.6340(3) 0.0586(18) Uani 1 1 d . . . H40 H 0.5521 1.1097 0.6418 0.070 Uiso 1 1 calc R . . C9 C 0.6340(5) 1.1764(5) 0.9249(3) 0.074(2) Uani 1 1 d . . . H9 H 0.6379 1.2151 0.9575 0.089 Uiso 1 1 calc R . . C28 C 0.5442(3) 0.9134(4) 0.5680(3) 0.0399(14) Uani 1 1 d . . . H28 H 0.5049 0.9338 0.5893 0.048 Uiso 1 1 calc R . . C31 C 0.7611(5) 0.7283(5) 0.7240(3) 0.062(2) Uani 1 1 d . . . H31 H 0.8137 0.7121 0.7305 0.075 Uiso 1 1 calc R . . C23 C 0.7516(3) 0.8911(4) 0.5937(3) 0.0489(16) Uani 1 1 d . . . H23A H 0.7842 0.9220 0.5683 0.059 Uiso 1 1 calc R . . H23B H 0.7722 0.8319 0.6003 0.059 Uiso 1 1 calc R . . C57 C 0.2465(4) 0.9643(4) 0.8431(3) 0.0468(16) Uani 1 1 d . . . H57 H 0.2705 0.9962 0.8762 0.056 Uiso 1 1 calc R . . C39 C 0.6119(5) 1.2040(5) 0.6130(3) 0.070(2) Uani 1 1 d . . . H39 H 0.5701 1.2433 0.6066 0.084 Uiso 1 1 calc R . . C56 C 0.1689(4) 0.9522(4) 0.8356(3) 0.0458(15) Uani 1 1 d . . . H56 H 0.1382 0.9771 0.8625 0.055 Uiso 1 1 calc R . . C51 C 0.4316(4) 0.7086(4) 0.5760(3) 0.0525(17) Uani 1 1 d . . . H51 H 0.4829 0.7056 0.5673 0.063 Uiso 1 1 calc R . . C36 C 0.7280(5) 1.0892(4) 0.6340(3) 0.0567(18) Uani 1 1 d . . . C1 C 0.6181(3) 0.9969(5) 0.7818(3) 0.0467(15) Uani 1 1 d . . . C50 C 0.3757(5) 0.6561(4) 0.5468(3) 0.0587(19) Uani 1 1 d . . . H50 H 0.3880 0.6165 0.5176 0.070 Uiso 1 1 calc R . . C29 C 0.7950(3) 0.8828(5) 0.7003(3) 0.0563(18) Uani 1 1 d . . . H29A H 0.8076 0.9168 0.7371 0.068 Uiso 1 1 calc R . . H29B H 0.8432 0.8593 0.6886 0.068 Uiso 1 1 calc R . . C33 C 0.6312(5) 0.6931(4) 0.7217(3) 0.0617(19) Uani 1 1 d . . . H33 H 0.5924 0.6520 0.7266 0.074 Uiso 1 1 calc R . . C27 C 0.5254(4) 0.8828(5) 0.5116(3) 0.0506(16) Uani 1 1 d . . . H27 H 0.4732 0.8810 0.4942 0.061 Uiso 1 1 calc R . . C7 C 0.6927(4) 1.0731(5) 0.8673(3) 0.0558(18) Uani 1 1 d . . . H7 H 0.7365 1.0411 0.8598 0.067 Uiso 1 1 calc R . . C26 C 0.5817(4) 0.8548(5) 0.4804(3) 0.068(2) Uani 1 1 d . . . H26 H 0.5694 0.8356 0.4406 0.082 Uiso 1 1 calc R . . C37 C 0.7419(5) 1.1697(5) 0.6101(3) 0.071(2) Uani 1 1 d . . . H37 H 0.7914 1.1842 0.6006 0.086 Uiso 1 1 calc R . . C21 C 0.6618(4) 0.8721(5) 0.8447(4) 0.072(2) Uani 1 1 d . . . H21A H 0.6457 0.8162 0.8590 0.108 Uiso 1 1 calc R . . H21B H 0.6770 0.9104 0.8784 0.108 Uiso 1 1 calc R . . H21C H 0.7054 0.8636 0.8226 0.108 Uiso 1 1 calc R . . C38 C 0.6823(5) 1.2272(5) 0.6009(3) 0.067(2) Uani 1 1 d . . . H38 H 0.6904 1.2833 0.5859 0.080 Uiso 1 1 calc R . . C8 C 0.6978(5) 1.1283(6) 0.9128(4) 0.079(2) Uani 1 1 d . . . H8 H 0.7455 1.1350 0.9374 0.095 Uiso 1 1 calc R . . C32 C 0.7072(5) 0.6693(5) 0.7293(3) 0.065(2) Uani 1 1 d . . . H32 H 0.7212 0.6110 0.7382 0.078 Uiso 1 1 calc R . . C35 C 0.7908(5) 1.0246(5) 0.6507(4) 0.074(2) Uani 1 1 d . . . H35A H 0.8273 1.0254 0.6211 0.088 Uiso 1 1 calc R . . H35B H 0.8193 1.0393 0.6898 0.088 Uiso 1 1 calc R . . O11 O 0.8834(6) 0.1706(7) 0.9462(5) 0.083(5) Uani 0.538(16) 1 d P C 5 O10 O 0.8946(9) 0.1274(12) 1.0043(7) 0.116(7) Uani 0.462(16) 1 d P C 6 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 P1 0.0575(12) 0.0782(16) 0.0809(15) 0.0124(13) 0.0073(11) -0.0008(12) F4 0.161(6) 0.080(4) 0.149(5) -0.013(4) 0.050(4) 0.010(4) F9 0.236(10) 0.389(17) 0.086(5) -0.014(7) -0.028(6) 0.007(10) Co2 0.0314(4) 0.0226(4) 0.0358(4) 0.0012(3) 0.0081(3) -0.0027(3) Co1 0.0343(4) 0.0431(5) 0.0394(5) -0.0017(4) 0.0082(3) 0.0101(4) O8 0.037(2) 0.030(2) 0.032(2) -0.0050(16) 0.0079(16) -0.0010(17) O4 0.0256(18) 0.0250(19) 0.042(2) 0.0037(17) 0.0028(16) -0.0035(15) O5 0.0317(19) 0.0209(18) 0.041(2) 0.0030(16) 0.0039(16) -0.0034(15) N5 0.033(2) 0.027(2) 0.040(3) 0.000(2) 0.008(2) -0.003(2) C13 0.027(3) 0.030(3) 0.029(3) -0.003(2) 0.007(2) 0.002(2) O6 0.039(2) 0.025(2) 0.057(3) -0.0001(19) -0.0091(19) -0.0033(18) N6 0.037(2) 0.022(2) 0.037(2) 0.0013(19) 0.011(2) 0.002(2) O1 0.029(2) 0.061(3) 0.056(3) 0.007(2) 0.0037(19) 0.005(2) N8 0.039(3) 0.022(2) 0.039(3) 0.005(2) 0.012(2) 0.001(2) C15 0.032(3) 0.022(3) 0.028(3) -0.002(2) 0.011(2) 0.006(2) C16 0.030(3) 0.028(3) 0.027(3) 0.001(2) 0.009(2) 0.001(2) C12 0.024(2) 0.030(3) 0.031(3) -0.003(2) 0.013(2) -0.001(2) O3 0.052(3) 0.062(3) 0.052(3) -0.020(2) -0.001(2) 0.018(2) N7 0.042(3) 0.025(2) 0.034(2) 0.003(2) 0.013(2) -0.001(2) N2 0.037(3) 0.034(3) 0.035(3) 0.003(2) 0.007(2) 0.006(2) O2 0.030(2) 0.057(3) 0.033(2) -0.0015(19) 0.0056(16) 0.0086(19) C3 0.029(3) 0.021(3) 0.035(3) -0.001(2) 0.001(2) 0.003(2) C20 0.042(3) 0.025(3) 0.036(3) -0.004(2) 0.011(3) 0.002(2) C2 0.028(3) 0.045(3) 0.034(3) 0.006(3) 0.004(2) -0.003(3) C11 0.031(3) 0.023(3) 0.031(3) 0.002(2) 0.006(2) 0.000(2) N4 0.066(4) 0.045(3) 0.046(3) -0.003(3) 0.014(3) 0.010(3) N3 0.049(3) 0.039(3) 0.045(3) 0.002(2) 0.016(2) 0.009(3) C42 0.049(3) 0.032(3) 0.028(3) -0.002(2) 0.017(3) 0.000(3) O7 0.069(3) 0.052(3) 0.059(3) -0.001(2) -0.001(2) 0.023(3) C17 0.028(3) 0.044(3) 0.034(3) 0.004(3) 0.004(2) -0.007(3) C46 0.035(3) 0.034(3) 0.046(3) 0.005(3) 0.009(3) 0.000(3) N1 0.043(3) 0.048(3) 0.066(4) -0.005(3) 0.008(3) 0.000(3) C43 0.051(4) 0.028(3) 0.049(4) 0.004(3) 0.022(3) -0.003(3) C14 0.028(3) 0.024(3) 0.034(3) -0.002(2) 0.005(2) 0.000(2) C52 0.044(3) 0.032(3) 0.041(3) 0.006(3) 0.010(3) 0.003(3) C45 0.040(3) 0.049(4) 0.052(4) 0.001(3) 0.013(3) 0.002(3) C24 0.042(3) 0.036(3) 0.040(3) 0.007(3) 0.014(3) -0.003(3) C4 0.041(3) 0.031(3) 0.042(3) -0.007(3) 0.000(3) 0.002(3) C41 0.041(3) 0.021(3) 0.047(3) 0.002(2) 0.016(3) -0.002(2) C48 0.059(4) 0.034(3) 0.034(3) 0.003(3) 0.011(3) 0.008(3) C6 0.039(3) 0.053(4) 0.038(3) 0.003(3) -0.007(3) -0.008(3) C54 0.039(3) 0.030(3) 0.043(3) 0.012(3) 0.014(3) -0.003(3) C53 0.033(3) 0.026(3) 0.051(3) 0.001(3) 0.010(3) -0.004(2) C25 0.052(4) 0.062(5) 0.052(4) -0.017(3) 0.028(3) -0.014(3) C10 0.082(5) 0.045(4) 0.066(5) -0.015(4) -0.011(4) 0.006(4) C19 0.046(3) 0.033(3) 0.038(3) 0.004(3) 0.009(3) 0.016(3) C18 0.036(3) 0.048(4) 0.033(3) 0.007(3) 0.002(2) 0.012(3) C44 0.053(4) 0.041(4) 0.053(4) 0.015(3) 0.010(3) 0.013(3) C49 0.072(5) 0.030(3) 0.045(4) -0.003(3) 0.013(3) -0.008(3) C47 0.048(3) 0.029(3) 0.038(3) -0.006(3) 0.005(3) -0.012(3) C22 0.050(4) 0.038(3) 0.039(3) 0.000(3) 0.004(3) -0.005(3) C30 0.050(4) 0.048(4) 0.047(4) -0.001(3) -0.005(3) 0.015(3) C5 0.056(4) 0.031(3) 0.047(4) -0.004(3) -0.004(3) 0.001(3) C55 0.048(3) 0.028(3) 0.064(4) 0.009(3) 0.022(3) 0.006(3) C58 0.051(4) 0.030(3) 0.039(3) 0.001(3) 0.007(3) 0.003(3) C34 0.056(4) 0.056(4) 0.061(4) 0.002(4) 0.025(3) 0.005(4) C40 0.073(5) 0.048(4) 0.053(4) 0.005(4) 0.005(4) 0.017(4) C9 0.095(6) 0.070(5) 0.051(4) -0.018(4) -0.017(4) -0.005(5) C28 0.041(3) 0.041(3) 0.039(3) 0.003(3) 0.009(3) 0.004(3) C31 0.064(5) 0.063(5) 0.058(4) 0.007(4) -0.001(4) 0.033(4) C23 0.047(4) 0.057(4) 0.045(4) -0.001(3) 0.014(3) 0.013(3) C57 0.069(4) 0.028(3) 0.044(4) -0.002(3) 0.010(3) 0.007(3) C39 0.091(6) 0.053(5) 0.062(5) -0.012(4) -0.007(4) -0.001(5) C56 0.065(4) 0.028(3) 0.050(4) 0.003(3) 0.026(3) 0.006(3) C51 0.064(4) 0.051(4) 0.050(4) 0.007(3) 0.033(3) 0.008(4) C36 0.084(5) 0.037(4) 0.046(4) -0.002(3) -0.004(4) -0.006(4) C1 0.041(3) 0.061(4) 0.039(3) 0.002(3) 0.010(3) 0.003(3) C50 0.087(5) 0.037(4) 0.057(4) -0.017(3) 0.027(4) 0.004(4) C29 0.037(3) 0.064(5) 0.064(4) -0.004(4) -0.006(3) 0.017(3) C33 0.082(5) 0.039(4) 0.067(5) 0.002(4) 0.020(4) 0.011(4) C27 0.046(4) 0.062(4) 0.047(4) -0.005(3) 0.016(3) -0.007(3) C7 0.046(4) 0.067(5) 0.052(4) -0.006(4) -0.004(3) -0.007(4) C26 0.067(5) 0.092(6) 0.053(4) -0.027(4) 0.035(4) -0.035(4) C37 0.088(6) 0.059(5) 0.064(5) -0.004(4) 0.000(4) -0.019(5) C21 0.074(5) 0.059(5) 0.079(5) 0.001(4) -0.005(4) 0.022(4) C38 0.108(7) 0.032(4) 0.053(4) -0.004(3) -0.015(4) -0.009(4) C8 0.071(5) 0.094(7) 0.067(5) -0.008(5) -0.015(4) -0.019(5) C32 0.091(6) 0.041(4) 0.063(5) 0.006(4) 0.010(4) 0.026(4) C35 0.064(5) 0.050(5) 0.105(6) 0.002(5) 0.006(5) -0.006(4) O11 0.063(7) 0.095(9) 0.092(10) -0.017(7) 0.015(6) -0.006(6) O10 0.111(12) 0.125(14) 0.105(14) -0.012(11) -0.009(9) 0.019(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 F6B 1.464(15) . ? P1 F5 1.483(11) . ? P1 F2A 1.487(12) . ? P1 F1B 1.510(10) . ? P1 F4 1.545(6) . ? P1 F1A 1.575(16) . ? P1 F3B 1.606(15) . ? P1 F6A 1.620(10) . ? P1 F3A 1.630(11) . ? P1 F5B 1.663(19) . ? P1 F2B 1.686(11) . ? P2 F9 1.405(10) . ? P2 F8 1.57(2) . ? P2 F11 1.582(15) . ? P2 F12A 1.62(3) . ? P2 F10A 1.664(19) . ? P2 F7 1.68(3) . ? P2B F8B 1.556(17) . ? P2B F11B 1.632(16) . ? P2B F10B 1.635(15) . ? P2B F7B 1.647(18) . ? P2B F9 1.672(13) . ? P2B F12B 1.740(13) . ? Co2 O4 1.863(4) . ? Co2 O5 1.865(3) . ? Co2 N6 1.912(4) . ? Co2 N7 1.912(4) . ? Co2 N8 1.915(4) . ? Co2 N5 1.921(4) . ? Co1 O2 1.867(4) . ? Co1 O1 1.903(4) . ? Co1 N4 1.909(6) . ? Co1 N3 1.929(5) . ? Co1 N2 1.938(5) . ? Co1 N1 1.965(5) . ? O8 C22 1.416(6) . ? O8 C11 1.467(6) . ? O4 C11 1.354(6) . ? O5 C12 1.303(6) . ? N5 C41 1.486(7) . ? N5 C47 1.488(7) . ? N5 C53 1.494(7) . ? C13 C12 1.359(7) . ? C13 C14 1.402(7) . ? C13 C3 1.479(7) . ? O6 C14 1.244(6) . ? N6 C46 1.311(7) . ? N6 C42 1.333(7) . ? O1 C1 1.348(7) . ? N8 C58 1.327(7) . ? N8 C54 1.338(7) . ? C15 C20 1.372(7) . ? C15 C16 1.385(7) . ? C15 C14 1.494(7) . ? C16 C17 1.404(7) . ? C16 C11 1.511(7) . ? C12 C11 1.513(7) . ? O3 C4 1.226(7) . ? N7 C52 1.330(7) . ? N7 C48 1.341(7) . ? N2 C28 1.335(7) . ? N2 C24 1.340(7) . ? O2 C2 1.301(6) . ? C3 C2 1.360(7) . ? C3 C4 1.423(7) . ? C20 C19 1.359(8) . ? C2 C1 1.513(8) . ? N4 C36 1.320(9) . ? N4 C40 1.336(8) . ? N3 C34 1.341(8) . ? N3 C30 1.347(8) . ? C42 C43 1.363(8) . ? C42 C41 1.497(8) . ? O7 C21 1.406(8) . ? O7 C1 1.522(8) . ? C17 C18 1.354(8) . ? C46 C45 1.377(8) . ? N1 C29 1.473(8) . ? N1 C35 1.490(9) . ? N1 C23 1.517(8) . ? C43 C44 1.370(8) . ? C52 C51 1.384(8) . ? C45 C44 1.373(9) . ? C24 C25 1.354(8) . ? C24 C23 1.477(8) . ? C4 C5 1.495(8) . ? C48 C49 1.393(8) . ? C48 C47 1.461(8) . ? C6 C7 1.369(8) . ? C6 C5 1.394(9) . ? C6 C1 1.513(9) . ? C54 C55 1.380(8) . ? C54 C53 1.497(8) . ? C25 C26 1.372(10) . ? C10 C5 1.363(9) . ? C10 C9 1.427(10) . ? C19 C18 1.371(8) . ? C49 C50 1.380(10) . ? C30 C31 1.369(9) . ? C30 C29 1.476(10) . ? C55 C56 1.363(9) . ? C58 C57 1.378(8) . ? C34 C33 1.377(9) . ? C40 C39 1.325(10) . ? C9 C8 1.404(12) . ? C28 C27 1.369(8) . ? C31 C32 1.333(11) . ? C57 C56 1.365(9) . ? C39 C38 1.352(11) . ? C51 C50 1.376(10) . ? C36 C37 1.393(10) . ? C36 C35 1.501(10) . ? C33 C32 1.375(10) . ? C27 C26 1.364(9) . ? C7 C8 1.338(10) . ? C37 C38 1.371(11) . ? 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 F6B P1 F5 128.9(8) . . ? F6B P1 F2A 54.0(7) . . ? F5 P1 F2A 100.6(7) . . ? F6B P1 F1B 123.8(8) . . ? F5 P1 F1B 101.4(6) . . ? F2A P1 F1B 98.7(6) . . ? F6B P1 F4 112.1(7) . . ? F5 P1 F4 92.1(5) . . ? F2A P1 F4 165.4(6) . . ? F1B P1 F4 85.7(5) . . ? F6B P1 F1A 92.5(9) . . ? F5 P1 F1A 122.7(8) . . ? F2A P1 F1A 70.6(8) . . ? F1B P1 F1A 33.0(6) . . ? F4 P1 F1A 108.4(7) . . ? F6B P1 F3B 90.7(8) . . ? F5 P1 F3B 43.1(6) . . ? F2A P1 F3B 94.1(7) . . ? F1B P1 F3B 144.2(7) . . ? F4 P1 F3B 90.3(6) . . ? F1A P1 F3B 158.2(8) . . ? F6B P1 F6A 49.0(7) . . ? F5 P1 F6A 167.3(6) . . ? F2A P1 F6A 87.2(6) . . ? F1B P1 F6A 87.1(5) . . ? F4 P1 F6A 79.1(4) . . ? F1A P1 F6A 69.3(7) . . ? F3B P1 F6A 127.0(7) . . ? F6B P1 F3A 53.1(7) . . ? F5 P1 F3A 86.9(6) . . ? F2A P1 F3A 87.8(6) . . ? F1B P1 F3A 168.2(6) . . ? F4 P1 F3A 85.7(5) . . ? F1A P1 F3A 145.4(8) . . ? F3B P1 F3A 43.9(6) . . ? F6A P1 F3A 83.3(6) . . ? F6B P1 F5B 157.8(10) . . ? F5 P1 F5B 37.5(7) . . ? F2A P1 F5B 106.0(9) . . ? F1B P1 F5B 64.0(8) . . ? F4 P1 F5B 88.4(7) . . ? F1A P1 F5B 88.8(9) . . ? F3B P1 F5B 80.3(9) . . ? F6A P1 F5B 149.4(8) . . ? F3A P1 F5B 123.8(8) . . ? F6B P1 F2B 81.6(7) . . ? F5 P1 F2B 74.2(6) . . ? F2A P1 F2B 29.4(5) . . ? F1B P1 F2B 91.3(6) . . ? F4 P1 F2B 165.2(6) . . ? F1A P1 F2B 75.5(7) . . ? F3B P1 F2B 83.7(7) . . ? F6A P1 F2B 115.3(6) . . ? F3A P1 F2B 99.1(6) . . ? F5B P1 F2B 77.2(8) . . ? F9 P2 F8 160.2(12) . . ? F9 P2 F11 90.6(11) . . ? F8 P2 F11 91.5(14) . . ? F9 P2 F12A 95.3(13) . . ? F8 P2 F12A 104.3(14) . . ? F11 P2 F12A 76.5(14) . . ? F9 P2 F10A 74.0(9) . . ? F8 P2 F10A 86.3(11) . . ? F11 P2 F10A 90.2(9) . . ? F12A P2 F10A 163.1(14) . . ? F9 P2 F7 99.3(11) . . ? F8 P2 F7 80.1(14) . . ? F11 P2 F7 169.7(14) . . ? F12A P2 F7 99.6(14) . . ? F10A P2 F7 95.1(12) . . ? F8B P2B F11B 92.3(12) . . ? F8B P2B F10B 77.4(10) . . ? F11B P2B F10B 98.4(11) . . ? F8B P2B F7B 92.1(11) . . ? F11B P2B F7B 174.7(13) . . ? F10B P2B F7B 85.4(10) . . ? F8B P2B F9 173.1(10) . . ? F11B P2B F9 92.2(11) . . ? F10B P2B F9 107.0(10) . . ? F7B P2B F9 83.1(8) . . ? F8B P2B F12B 99.4(9) . . ? F11B P2B F12B 77.8(10) . . ? F10B P2B F12B 175.0(10) . . ? F7B P2B F12B 98.6(9) . . ? F9 P2B F12B 76.5(7) . . ? P2 F9 P2B 28.3(4) . . ? O4 Co2 O5 87.64(15) . . ? O4 Co2 N6 179.50(18) . . ? O5 Co2 N6 92.63(17) . . ? O4 Co2 N7 92.23(17) . . ? O5 Co2 N7 96.86(18) . . ? N6 Co2 N7 87.32(18) . . ? O4 Co2 N8 88.44(17) . . ? O5 Co2 N8 93.89(18) . . ? N6 Co2 N8 91.96(18) . . ? N7 Co2 N8 169.25(19) . . ? O4 Co2 N5 92.01(17) . . ? O5 Co2 N5 178.03(17) . . ? N6 Co2 N5 87.73(19) . . ? N7 Co2 N5 85.10(19) . . ? N8 Co2 N5 84.16(19) . . ? O2 Co1 O1 85.73(16) . . ? O2 Co1 N4 94.4(2) . . ? O1 Co1 N4 89.9(2) . . ? O2 Co1 N3 97.6(2) . . ? O1 Co1 N3 89.3(2) . . ? N4 Co1 N3 167.9(2) . . ? O2 Co1 N2 91.35(18) . . ? O1 Co1 N2 176.77(18) . . ? N4 Co1 N2 88.9(2) . . ? N3 Co1 N2 92.5(2) . . ? O2 Co1 N1 176.6(2) . . ? O1 Co1 N1 97.7(2) . . ? N4 Co1 N1 85.6(2) . . ? N3 Co1 N1 82.6(2) . . ? N2 Co1 N1 85.3(2) . . ? C22 O8 C11 113.7(4) . . ? C11 O4 Co2 109.8(3) . . ? C12 O5 Co2 110.7(3) . . ? C41 N5 C47 111.8(4) . . ? C41 N5 C53 110.8(4) . . ? C47 N5 C53 112.4(4) . . ? C41 N5 Co2 109.2(3) . . ? C47 N5 Co2 106.5(3) . . ? C53 N5 Co2 105.8(3) . . ? C12 C13 C14 119.1(5) . . ? C12 C13 C3 121.0(5) . . ? C14 C13 C3 119.9(5) . . ? C46 N6 C42 120.0(5) . . ? C46 N6 Co2 126.1(4) . . ? C42 N6 Co2 113.5(4) . . ? C1 O1 Co1 111.0(4) . . ? C58 N8 C54 119.7(5) . . ? C58 N8 Co2 127.2(4) . . ? C54 N8 Co2 113.1(4) . . ? C20 C15 C16 119.1(5) . . ? C20 C15 C14 120.4(5) . . ? C16 C15 C14 120.4(5) . . ? C15 C16 C17 119.0(5) . . ? C15 C16 C11 119.3(4) . . ? C17 C16 C11 121.7(5) . . ? O5 C12 C13 123.8(5) . . ? O5 C12 C11 112.5(4) . . ? C13 C12 C11 123.7(5) . . ? C52 N7 C48 120.2(5) . . ? C52 N7 Co2 126.6(4) . . ? C48 N7 Co2 112.9(4) . . ? C28 N2 C24 119.3(5) . . ? C28 N2 Co1 125.0(4) . . ? C24 N2 Co1 115.7(4) . . ? C2 O2 Co1 111.7(3) . . ? C2 C3 C4 119.3(5) . . ? C2 C3 C13 119.7(5) . . ? C4 C3 C13 121.0(5) . . ? C19 C20 C15 120.6(5) . . ? O2 C2 C3 123.0(5) . . ? O2 C2 C1 112.3(5) . . ? C3 C2 C1 124.8(5) . . ? O4 C11 O8 113.1(4) . . ? O4 C11 C16 111.5(4) . . ? O8 C11 C16 108.9(4) . . ? O4 C11 C12 109.8(4) . . ? O8 C11 C12 100.2(4) . . ? C16 C11 C12 112.9(4) . . ? C36 N4 C40 118.6(6) . . ? C36 N4 Co1 113.9(5) . . ? C40 N4 Co1 127.5(5) . . ? C34 N3 C30 120.5(6) . . ? C34 N3 Co1 126.0(4) . . ? C30 N3 Co1 113.1(4) . . ? N6 C42 C43 121.1(5) . . ? N6 C42 C41 115.5(5) . . ? C43 C42 C41 123.4(5) . . ? C21 O7 C1 114.7(5) . . ? C18 C17 C16 121.1(5) . . ? N6 C46 C45 122.1(6) . . ? C29 N1 C35 112.7(6) . . ? C29 N1 C23 110.1(5) . . ? C35 N1 C23 111.7(6) . . ? C29 N1 Co1 104.6(4) . . ? C35 N1 Co1 107.7(4) . . ? C23 N1 Co1 109.7(4) . . ? C42 C43 C44 119.4(6) . . ? O6 C14 C13 123.3(5) . . ? O6 C14 C15 116.7(5) . . ? C13 C14 C15 119.8(5) . . ? N7 C52 C51 121.5(6) . . ? C44 C45 C46 118.2(6) . . ? N2 C24 C25 122.0(6) . . ? N2 C24 C23 116.0(5) . . ? C25 C24 C23 122.0(5) . . ? O3 C4 C3 122.6(5) . . ? O3 C4 C5 118.6(5) . . ? C3 C4 C5 118.7(5) . . ? N5 C41 C42 111.7(4) . . ? N7 C48 C49 121.0(6) . . ? N7 C48 C47 114.7(5) . . ? C49 C48 C47 124.2(6) . . ? C7 C6 C5 121.0(6) . . ? C7 C6 C1 119.9(6) . . ? C5 C6 C1 119.0(5) . . ? N8 C54 C55 121.5(6) . . ? N8 C54 C53 114.3(5) . . ? C55 C54 C53 124.2(5) . . ? N5 C53 C54 107.3(4) . . ? C24 C25 C26 119.1(6) . . ? C5 C10 C9 119.2(8) . . ? C20 C19 C18 121.5(5) . . ? C17 C18 C19 118.7(5) . . ? C43 C44 C45 119.2(6) . . ? C50 C49 C48 118.8(6) . . ? C48 C47 N5 108.0(5) . . ? N3 C30 C31 119.7(7) . . ? N3 C30 C29 113.9(5) . . ? C31 C30 C29 126.4(6) . . ? C10 C5 C6 119.9(6) . . ? C10 C5 C4 118.3(6) . . ? C6 C5 C4 121.8(5) . . ? C56 C55 C54 118.8(6) . . ? N8 C58 C57 120.8(6) . . ? N3 C34 C33 120.1(7) . . ? C39 C40 N4 123.5(8) . . ? C8 C9 C10 118.5(7) . . ? N2 C28 C27 120.8(5) . . ? C32 C31 C30 120.7(7) . . ? C24 C23 N1 112.0(5) . . ? C56 C57 C58 119.9(6) . . ? C40 C39 C38 119.0(8) . . ? C55 C56 C57 119.2(6) . . ? C50 C51 C52 119.1(6) . . ? N4 C36 C37 121.0(7) . . ? N4 C36 C35 116.8(6) . . ? C37 C36 C35 122.1(8) . . ? O1 C1 C6 114.7(5) . . ? O1 C1 C2 109.1(5) . . ? C6 C1 C2 113.3(5) . . ? O1 C1 O7 111.5(5) . . ? C6 C1 O7 108.1(5) . . ? C2 C1 O7 99.1(5) . . ? C51 C50 C49 119.4(6) . . ? N1 C29 C30 106.5(5) . . ? C32 C33 C34 119.1(7) . . ? C26 C27 C28 119.9(6) . . ? C8 C7 C6 120.3(7) . . ? C27 C26 C25 118.9(6) . . ? C38 C37 C36 118.0(8) . . ? C39 C38 C37 119.9(8) . . ? C7 C8 C9 121.2(7) . . ? C31 C32 C33 119.8(7) . . ? N1 C35 C36 108.5(6) . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 27.55 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.832 _refine_diff_density_min -1.151 _refine_diff_density_rms 0.115 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.500 309 101 ' ' _platon_squeeze_details ; ; _database_code_depnum_ccdc_archive 'CCDC 965095'