# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_ip1-758 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C24 H16 Cd Co2 O8, C3 H7 N O' _chemical_formula_sum 'C27 H23 Cd Co2 N O9' _chemical_formula_weight 735.72 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M ' P-1' _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.513(2) _cell_length_b 10.585(2) _cell_length_c 13.976(3) _cell_angle_alpha 75.452(17) _cell_angle_beta 74.622(18) _cell_angle_gamma 89.947(17) _cell_volume 1447.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 215(2) _cell_measurement_reflns_used 4709 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 26.1 _exptl_crystal_description tip _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 732 _exptl_absorpt_coefficient_mu 1.911 _exptl_absorpt_correction_type none _diffrn_ambient_temperature 215(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method '\w scans' _diffrn_detector 'image plate' _diffrn_detector_type STOE _diffrn_standards_number none _diffrn_reflns_number 13977 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1113 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 26.50 _reflns_number_total 13977 _reflns_number_gt 8283 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13977 _refine_ls_number_parameters 364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0598 _refine_ls_wR_factor_ref 0.1401 _refine_ls_wR_factor_gt 0.1281 _refine_ls_goodness_of_fit_ref 0.896 _refine_ls_restrained_S_all 0.896 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6772(7) 0.7647(6) 0.3524(5) 0.0459(16) Uani 1 1 d . . . C2 C 0.8065(7) 0.8159(6) 0.2996(6) 0.0542(19) Uani 1 1 d . . . H2 H 0.8372 0.8563 0.2288 0.065 Uiso 1 1 d R . . C3 C 0.8838(8) 0.7967(7) 0.3713(7) 0.066(2) Uani 1 1 d . . . H3 H 0.9743 0.8213 0.3558 0.080 Uiso 1 1 d R . . C4 C 0.8016(9) 0.7349(8) 0.4690(7) 0.068(2) Uani 1 1 d . . . H4 H 0.8269 0.7109 0.5304 0.081 Uiso 1 1 d R . . C5 C 0.6738(7) 0.7152(7) 0.4581(6) 0.0533(18) Uani 1 1 d . . . H5 H 0.5990 0.6758 0.5115 0.064 Uiso 1 1 d R . . C6 C 0.5663(7) 0.7520(6) 0.3044(6) 0.0494(18) Uani 1 1 d . . . C7 C 0.9525(7) 0.5128(6) 0.3169(5) 0.0482(16) Uani 1 1 d . . . C8 C 0.8547(7) 0.5278(6) 0.2567(7) 0.0560(18) Uani 1 1 d . . . H8 H 0.8715 0.5665 0.1859 0.067 Uiso 1 1 d R . . C9 C 0.7334(8) 0.4742(6) 0.3240(7) 0.060(2) Uani 1 1 d . . . H9 H 0.6539 0.4690 0.3060 0.072 Uiso 1 1 d R . . C10 C 0.7497(8) 0.4284(7) 0.4254(7) 0.068(2) Uani 1 1 d . . . H10 H 0.6830 0.3875 0.4851 0.081 Uiso 1 1 d R . . C11 C 0.8826(8) 0.4553(7) 0.4202(7) 0.062(2) Uani 1 1 d . . . H11 H 0.9191 0.4376 0.4763 0.074 Uiso 1 1 d R . . C12 C 1.0926(7) 0.5675(7) 0.2768(7) 0.0535(18) Uani 1 1 d . . . C13 C 0.5093(6) 0.3268(6) 0.1800(5) 0.0408(15) Uani 1 1 d . . . C14 C 0.5751(6) 0.3261(6) 0.0794(5) 0.0496(17) Uani 1 1 d . . . H14 H 0.5974 0.3986 0.0217 0.060 Uiso 1 1 d R . . C15 C 0.6020(7) 0.1933(7) 0.0815(7) 0.060(2) Uani 1 1 d . . . H15 H 0.6458 0.1629 0.0245 0.072 Uiso 1 1 d R . . C16 C 0.5528(8) 0.1165(6) 0.1813(6) 0.059(2) Uani 1 1 d . . . H16 H 0.5568 0.0255 0.2033 0.070 Uiso 1 1 d R . . C17 C 0.4967(7) 0.1968(6) 0.2430(6) 0.0519(17) Uani 1 1 d . . . H17 H 0.4570 0.1701 0.3142 0.062 Uiso 1 1 d R . . C18 C 0.4563(7) 0.4428(6) 0.2171(5) 0.0446(16) Uani 1 1 d . . . C19 C 0.2663(7) 0.0739(6) 0.1417(5) 0.0465(16) Uani 1 1 d . . . C20 C 0.3240(7) 0.1406(6) 0.0363(5) 0.0453(16) Uani 1 1 d . . . H20 H 0.3694 0.1027 -0.0160 0.054 Uiso 1 1 d R . . C21 C 0.3000(8) 0.2747(7) 0.0250(6) 0.0568(19) Uani 1 1 d . . . H21 H 0.3265 0.3418 -0.0362 0.068 Uiso 1 1 d R . . C22 C 0.2294(7) 0.2892(6) 0.1220(6) 0.0543(18) Uani 1 1 d . . . H22 H 0.2012 0.3685 0.1362 0.065 Uiso 1 1 d R . . C23 C 0.2078(7) 0.1670(6) 0.1939(6) 0.0494(17) Uani 1 1 d . . . H23 H 0.1626 0.1498 0.2641 0.059 Uiso 1 1 d R . . C24 C 0.2773(7) -0.0714(6) 0.1904(6) 0.0477(17) Uani 1 1 d . . . C25 C 0.8999(10) 0.1284(8) 0.4613(7) 0.074(2) Uani 1 1 d . . . H25 H 0.8800 0.1052 0.5334 0.089 Uiso 1 1 calc R . . C26 C 0.6710(10) 0.0781(10) 0.4852(10) 0.118(4) Uani 1 1 d . . . H26A H 0.6743 0.0148 0.5480 0.177 Uiso 1 1 calc R . . H26B H 0.6219 0.0386 0.4490 0.177 Uiso 1 1 calc R . . H26C H 0.6274 0.1536 0.5019 0.177 Uiso 1 1 calc R . . C27 C 0.8252(12) 0.1530(9) 0.3101(7) 0.096(3) Uani 1 1 d . . . H27A H 0.7724 0.0927 0.2917 0.144 Uiso 1 1 calc R . . H27B H 0.9181 0.1481 0.2773 0.144 Uiso 1 1 calc R . . H27C H 0.8001 0.2414 0.2874 0.144 Uiso 1 1 calc R . . Cd1 Cd 0.34787(5) 0.67554(5) 0.24822(4) 0.04190(14) Uani 1 1 d . . . Co1 Co 0.80303(9) 0.62237(9) 0.36897(7) 0.0451(2) Uani 1 1 d . . . Co2 Co 0.40671(9) 0.21105(8) 0.12899(6) 0.0411(2) Uani 1 1 d . . . N1 N 0.8027(7) 0.1181(6) 0.4212(5) 0.0629(16) Uani 1 1 d . . . O1 O 0.5909(6) 0.7855(6) 0.2099(4) 0.0809(18) Uani 1 1 d . . . O2 O 0.4566(5) 0.7062(5) 0.3634(4) 0.0616(13) Uani 1 1 d . . . O3 O 1.1490(5) 0.5758(5) 0.3441(4) 0.0628(14) Uani 1 1 d . . . O4 O 1.1453(6) 0.5984(5) 0.1838(5) 0.0764(16) Uani 1 1 d . . . O5 O 0.4185(6) 0.4325(5) 0.3091(4) 0.0684(16) Uani 1 1 d . . . O6 O 0.4558(5) 0.5466(4) 0.1477(4) 0.0582(14) Uani 1 1 d . . . O7 O 0.2249(6) -0.1129(5) 0.2820(4) 0.0725(16) Uani 1 1 d . . . O8 O 0.3401(5) -0.1339(4) 0.1327(4) 0.0617(14) Uani 1 1 d . . . O9 O 1.0186(7) 0.1669(7) 0.4115(5) 0.099(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.053(4) 0.037(3) 0.048(4) -0.012(3) -0.013(3) 0.013(3) C2 0.050(4) 0.035(3) 0.067(5) -0.015(3) 0.003(4) -0.002(3) C3 0.048(5) 0.060(5) 0.101(7) -0.035(5) -0.024(5) -0.006(4) C4 0.081(6) 0.068(5) 0.081(6) -0.043(5) -0.045(5) 0.029(5) C5 0.039(4) 0.071(5) 0.061(4) -0.038(4) -0.014(3) 0.009(4) C6 0.057(5) 0.042(4) 0.061(5) -0.024(3) -0.025(4) 0.018(4) C7 0.049(4) 0.043(4) 0.056(4) -0.014(3) -0.020(3) 0.000(3) C8 0.045(4) 0.044(4) 0.081(5) -0.024(4) -0.014(4) 0.001(3) C9 0.052(5) 0.040(4) 0.093(6) -0.023(4) -0.021(4) 0.003(3) C10 0.058(5) 0.057(5) 0.083(6) -0.019(4) -0.011(4) -0.005(4) C11 0.050(5) 0.051(4) 0.088(6) -0.028(4) -0.018(4) 0.001(4) C12 0.045(4) 0.044(4) 0.073(5) -0.023(4) -0.012(4) 0.009(3) C13 0.040(4) 0.044(4) 0.041(3) -0.010(3) -0.018(3) 0.003(3) C14 0.044(4) 0.051(4) 0.055(4) -0.018(3) -0.013(3) 0.005(3) C15 0.048(4) 0.064(5) 0.084(6) -0.042(4) -0.026(4) 0.015(4) C16 0.068(5) 0.035(3) 0.082(5) -0.012(4) -0.038(4) 0.013(4) C17 0.065(5) 0.035(3) 0.053(4) -0.003(3) -0.021(4) -0.005(3) C18 0.056(4) 0.037(3) 0.048(4) -0.024(3) -0.014(3) 0.010(3) C19 0.053(4) 0.037(3) 0.050(4) -0.015(3) -0.011(3) -0.001(3) C20 0.051(4) 0.047(4) 0.041(3) -0.013(3) -0.016(3) 0.005(3) C21 0.071(5) 0.045(4) 0.061(5) -0.012(3) -0.032(4) 0.005(4) C22 0.057(4) 0.036(3) 0.078(5) -0.018(3) -0.029(4) 0.014(3) C23 0.043(4) 0.052(4) 0.055(4) -0.022(3) -0.008(3) 0.006(3) C24 0.041(4) 0.048(4) 0.051(4) -0.009(3) -0.010(3) -0.016(3) C25 0.072(6) 0.080(6) 0.073(5) -0.029(5) -0.019(5) 0.009(5) C26 0.077(7) 0.097(7) 0.160(11) -0.058(7) 0.027(7) -0.021(6) C27 0.116(8) 0.074(6) 0.116(8) -0.042(6) -0.047(8) 0.018(6) Cd1 0.0429(3) 0.0372(2) 0.0460(3) -0.0118(2) -0.0119(2) 0.0027(2) Co1 0.0391(5) 0.0432(5) 0.0558(5) -0.0158(4) -0.0148(5) 0.0018(4) Co2 0.0452(6) 0.0342(4) 0.0455(5) -0.0122(4) -0.0133(4) 0.0038(4) N1 0.054(4) 0.064(4) 0.073(4) -0.026(4) -0.016(4) 0.000(3) O1 0.092(5) 0.099(4) 0.052(3) -0.001(3) -0.038(3) 0.011(4) O2 0.044(3) 0.079(3) 0.068(3) -0.027(3) -0.017(3) -0.001(3) O3 0.039(3) 0.064(3) 0.080(4) -0.005(3) -0.021(3) -0.010(2) O4 0.060(4) 0.081(4) 0.081(4) -0.016(3) -0.013(3) -0.005(3) O5 0.098(4) 0.065(3) 0.045(3) -0.019(3) -0.020(3) 0.022(3) O6 0.073(3) 0.039(2) 0.053(3) -0.012(2) -0.001(3) 0.009(2) O7 0.086(4) 0.049(3) 0.062(4) 0.004(2) -0.004(3) -0.004(3) O8 0.083(4) 0.044(3) 0.059(3) -0.018(2) -0.017(3) 0.018(3) O9 0.075(5) 0.135(6) 0.097(5) -0.051(4) -0.023(4) -0.004(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 C1 C2 1.397(9) . ? C1 C5 1.428(9) . ? C1 C6 1.513(10) . ? C1 Co1 2.014(6) . ? C2 C3 1.427(11) . ? C2 Co1 2.030(6) . ? C3 C4 1.401(11) . ? C3 Co1 2.043(7) . ? C4 C5 1.413(10) . ? C4 Co1 2.049(7) . ? C5 Co1 2.019(6) . ? C6 O1 1.232(8) . ? C6 O2 1.241(8) . ? C7 C11 1.411(10) . ? C7 C8 1.476(10) . ? C7 C12 1.490(10) . ? C7 Co1 2.039(6) . ? C8 C9 1.389(10) . ? C8 Co1 2.023(7) . ? C9 C10 1.435(11) . ? C9 Co1 2.032(8) . ? C10 C11 1.405(11) . ? C10 Co1 2.027(8) . ? C11 Co1 2.005(7) . ? C12 O4 1.228(9) . ? C12 O3 1.257(9) . ? C13 C14 1.395(9) . ? C13 C17 1.420(8) . ? C13 C18 1.500(8) . ? C13 Co2 2.006(7) . ? C14 C15 1.428(9) . ? C14 Co2 2.007(7) . ? C15 C16 1.387(10) . ? C15 Co2 2.007(7) . ? C16 C17 1.382(9) . ? C16 Co2 2.029(7) . ? C17 Co2 2.033(7) . ? C18 O5 1.217(8) . ? C18 O6 1.270(8) . ? C19 C23 1.416(8) . ? C19 C20 1.428(9) . ? C19 C24 1.536(9) . ? C19 Co2 2.013(7) . ? C20 C21 1.418(9) . ? C20 Co2 2.019(7) . ? C21 C22 1.408(10) . ? C21 Co2 2.048(7) . ? C22 C23 1.401(9) . ? C22 Co2 2.055(6) . ? C23 Co2 2.049(7) . ? C24 O7 1.216(8) . ? C24 O8 1.229(8) . ? C24 Cd1 2.758(7) 1_545 ? C25 O9 1.267(10) . ? C25 N1 1.305(11) . ? C26 N1 1.433(11) . ? C27 N1 1.456(10) . ? Cd1 O3 2.256(5) 1_455 ? Cd1 O8 2.262(5) 1_565 ? Cd1 O6 2.288(4) . ? Cd1 O2 2.289(5) . ? Cd1 C24 2.758(7) 1_565 ? O3 Cd1 2.256(5) 1_655 ? O8 Cd1 2.262(5) 1_545 ? 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 C2 C1 C5 107.1(7) . . ? C2 C1 C6 126.0(7) . . ? C5 C1 C6 126.7(7) . . ? C2 C1 Co1 70.4(4) . . ? C5 C1 Co1 69.4(3) . . ? C6 C1 Co1 120.6(4) . . ? C1 C2 C3 108.4(7) . . ? C1 C2 Co1 69.2(4) . . ? C3 C2 Co1 70.0(4) . . ? C4 C3 C2 108.3(7) . . ? C4 C3 Co1 70.2(5) . . ? C2 C3 Co1 69.0(4) . . ? C3 C4 C5 107.4(7) . . ? C3 C4 Co1 69.7(4) . . ? C5 C4 Co1 68.5(4) . . ? C4 C5 C1 108.8(7) . . ? C4 C5 Co1 70.8(4) . . ? C1 C5 Co1 69.1(3) . . ? O1 C6 O2 124.4(8) . . ? O1 C6 C1 118.3(7) . . ? O2 C6 C1 117.3(6) . . ? C11 C7 C8 106.7(7) . . ? C11 C7 C12 127.4(7) . . ? C8 C7 C12 125.3(7) . . ? C11 C7 Co1 68.3(4) . . ? C8 C7 Co1 68.1(4) . . ? C12 C7 Co1 121.5(4) . . ? C9 C8 C7 107.5(7) . . ? C9 C8 Co1 70.3(4) . . ? C7 C8 Co1 69.3(4) . . ? C8 C9 C10 108.7(7) . . ? C8 C9 Co1 69.6(4) . . ? C10 C9 Co1 69.1(5) . . ? C11 C10 C9 108.2(7) . . ? C11 C10 Co1 68.8(4) . . ? C9 C10 Co1 69.5(4) . . ? C10 C11 C7 108.9(8) . . ? C10 C11 Co1 70.4(4) . . ? C7 C11 Co1 70.9(4) . . ? O4 C12 O3 124.8(7) . . ? O4 C12 C7 119.8(8) . . ? O3 C12 C7 115.4(7) . . ? C14 C13 C17 108.4(6) . . ? C14 C13 C18 126.8(6) . . ? C17 C13 C18 124.8(6) . . ? C14 C13 Co2 69.7(4) . . ? C17 C13 Co2 70.5(4) . . ? C18 C13 Co2 124.3(5) . . ? C13 C14 C15 106.4(6) . . ? C13 C14 Co2 69.6(4) . . ? C15 C14 Co2 69.2(4) . . ? C16 C15 C14 108.8(6) . . ? C16 C15 Co2 70.8(4) . . ? C14 C15 Co2 69.1(4) . . ? C17 C16 C15 108.3(6) . . ? C17 C16 Co2 70.3(4) . . ? C15 C16 Co2 69.1(4) . . ? C16 C17 C13 108.1(6) . . ? C16 C17 Co2 70.0(4) . . ? C13 C17 Co2 68.4(4) . . ? O5 C18 O6 124.8(6) . . ? O5 C18 C13 119.2(6) . . ? O6 C18 C13 116.0(6) . . ? C23 C19 C20 108.2(5) . . ? C23 C19 C24 126.4(6) . . ? C20 C19 C24 125.2(5) . . ? C23 C19 Co2 71.0(4) . . ? C20 C19 Co2 69.5(4) . . ? C24 C19 Co2 121.3(5) . . ? C21 C20 C19 107.2(6) . . ? C21 C20 Co2 70.7(4) . . ? C19 C20 Co2 69.0(4) . . ? C22 C21 C20 107.7(6) . . ? C22 C21 Co2 70.2(4) . . ? C20 C21 Co2 68.5(4) . . ? C23 C22 C21 109.3(5) . . ? C23 C22 Co2 69.8(4) . . ? C21 C22 Co2 69.7(4) . . ? C22 C23 C19 107.5(6) . . ? C22 C23 Co2 70.3(4) . . ? C19 C23 Co2 68.2(4) . . ? O7 C24 O8 126.4(7) . . ? O7 C24 C19 117.3(6) . . ? O8 C24 C19 116.3(6) . . ? O7 C24 Cd1 72.9(4) . 1_545 ? O8 C24 Cd1 53.8(3) . 1_545 ? C19 C24 Cd1 168.1(5) . 1_545 ? O9 C25 N1 125.7(9) . . ? O3 Cd1 O8 114.98(19) 1_455 1_565 ? O3 Cd1 O6 109.41(19) 1_455 . ? O8 Cd1 O6 103.28(16) 1_565 . ? O3 Cd1 O2 105.5(2) 1_455 . ? O8 Cd1 O2 111.2(2) 1_565 . ? O6 Cd1 O2 112.62(18) . . ? O3 Cd1 C24 99.87(19) 1_455 1_565 ? O8 Cd1 C24 26.00(18) 1_565 1_565 ? O6 Cd1 C24 129.26(19) . 1_565 ? O2 Cd1 C24 97.5(2) . 1_565 ? C11 Co1 C1 163.0(3) . . ? C11 Co1 C5 125.3(3) . . ? C1 Co1 C5 41.5(3) . . ? C11 Co1 C8 70.2(3) . . ? C1 Co1 C8 117.5(3) . . ? C5 Co1 C8 152.7(3) . . ? C11 Co1 C10 40.8(3) . . ? C1 Co1 C10 125.3(3) . . ? C5 Co1 C10 106.9(3) . . ? C8 Co1 C10 69.0(3) . . ? C11 Co1 C2 155.2(3) . . ? C1 Co1 C2 40.4(3) . . ? C5 Co1 C2 68.3(3) . . ? C8 Co1 C2 107.4(3) . . ? C10 Co1 C2 163.0(3) . . ? C11 Co1 C9 69.5(3) . . ? C1 Co1 C9 106.0(3) . . ? C5 Co1 C9 119.0(3) . . ? C8 Co1 C9 40.1(3) . . ? C10 Co1 C9 41.4(3) . . ? C2 Co1 C9 125.4(3) . . ? C11 Co1 C7 40.8(3) . . ? C1 Co1 C7 154.4(3) . . ? C5 Co1 C7 163.1(3) . . ? C8 Co1 C7 42.6(3) . . ? C10 Co1 C7 68.6(3) . . ? C2 Co1 C7 120.7(3) . . ? C9 Co1 C7 69.2(3) . . ? C11 Co1 C3 119.9(3) . . ? C1 Co1 C3 68.8(3) . . ? C5 Co1 C3 67.9(3) . . ? C8 Co1 C3 127.6(3) . . ? C10 Co1 C3 153.9(4) . . ? C2 Co1 C3 41.0(3) . . ? C9 Co1 C3 163.9(4) . . ? C7 Co1 C3 108.6(3) . . ? C11 Co1 C4 107.2(3) . . ? C1 Co1 C4 69.3(3) . . ? C5 Co1 C4 40.6(3) . . ? C8 Co1 C4 165.1(3) . . ? C10 Co1 C4 119.3(4) . . ? C2 Co1 C4 68.4(3) . . ? C9 Co1 C4 154.0(4) . . ? C7 Co1 C4 126.1(3) . . ? C3 Co1 C4 40.1(3) . . ? C13 Co2 C14 40.7(3) . . ? C13 Co2 C15 68.6(3) . . ? C14 Co2 C15 41.7(3) . . ? C13 Co2 C19 155.7(3) . . ? C14 Co2 C19 162.2(3) . . ? C15 Co2 C19 124.5(3) . . ? C13 Co2 C20 161.7(3) . . ? C14 Co2 C20 124.0(3) . . ? C15 Co2 C20 106.5(3) . . ? C19 Co2 C20 41.5(3) . . ? C13 Co2 C16 68.4(3) . . ? C14 Co2 C16 69.1(3) . . ? C15 Co2 C16 40.2(3) . . ? C19 Co2 C16 107.2(3) . . ? C20 Co2 C16 119.9(3) . . ? C13 Co2 C17 41.2(2) . . ? C14 Co2 C17 68.8(3) . . ? C15 Co2 C17 67.5(3) . . ? C19 Co2 C17 120.3(3) . . ? C20 Co2 C17 154.9(2) . . ? C16 Co2 C17 39.8(3) . . ? C13 Co2 C21 125.3(3) . . ? C14 Co2 C21 106.9(3) . . ? C15 Co2 C21 120.7(3) . . ? C19 Co2 C21 68.7(3) . . ? C20 Co2 C21 40.8(2) . . ? C16 Co2 C21 155.3(3) . . ? C17 Co2 C21 163.4(3) . . ? C13 Co2 C23 121.1(3) . . ? C14 Co2 C23 155.2(2) . . ? C15 Co2 C23 162.0(3) . . ? C19 Co2 C23 40.8(2) . . ? C20 Co2 C23 69.0(3) . . ? C16 Co2 C23 125.8(3) . . ? C17 Co2 C23 108.7(3) . . ? C21 Co2 C23 68.0(3) . . ? C13 Co2 C22 108.8(3) . . ? C14 Co2 C22 120.7(3) . . ? C15 Co2 C22 156.2(3) . . ? C19 Co2 C22 67.9(3) . . ? C20 Co2 C22 68.1(3) . . ? C16 Co2 C22 162.8(3) . . ? C17 Co2 C22 127.1(3) . . ? C21 Co2 C22 40.1(3) . . ? C23 Co2 C22 39.9(3) . . ? C25 N1 C26 120.9(9) . . ? C25 N1 C27 120.5(8) . . ? C26 N1 C27 118.6(9) . . ? C6 O2 Cd1 100.5(5) . . ? C12 O3 Cd1 102.3(5) . 1_655 ? C18 O6 Cd1 99.7(4) . . ? C24 O8 Cd1 100.2(4) . 1_545 ? _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 1.283 _refine_diff_density_min -0.704 _refine_diff_density_rms 0.153 # start Validation Reply Form _vrf_PLAT021_ip1-758 ; PROBLEM: Ratio Unique / Expected Reflections too High ... 2.324 RESPONSE: This is due to HKLF 5 refinement (twinned crystal). ; _vrf_PLAT029_ip1-758 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.952 RESPONSE: The low fraction of 95 % originates in the type of diffractometer (STOE IPDS-1) and the triclinc crystal system. ; _vrf_PLAT241_ip1-758 ; PROBLEM: Check High Ueq as Compared to Neighbors for O1 RESPONSE: O1 is a non-coordinating oxygen atom of a carboxylate group. ; _vrf_PLAT601_ip1-758 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 184 Ang3 RESPONSE: This is not unusual for coordination polymers. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 950057' ####################################################################### # # 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_ip1-761 _audit_creation_method SHELXL-97 _chemical_formula_moiety 'C24 H16 Co2 O8 Zn, 4(H2 O)' _chemical_formula_sum 'C24 H24 Co2 O12 Zn' _chemical_formula_weight 687.66 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M 'I 41/a' _symmetry_space_group_name_Hall '-I 4ad ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 10.2788(10) _cell_length_b 10.2788(10) _cell_length_c 26.373(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2786.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 3611 _cell_measurement_theta_min 1.75 _cell_measurement_theta_max 27.1 _exptl_crystal_description tip _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.639 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.3649 _exptl_absorpt_correction_T_max 0.7264 _exptl_absorpt_process_details 'STOE X-RED' _diffrn_ambient_temperature 213(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 '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS 1' _diffrn_measurement_method '\w scans' _diffrn_detector 'image plate' _diffrn_detector_type STOE _diffrn_standards_number none _diffrn_reflns_number 3299 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0300 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 26.00 _reflns_number_total 1370 _reflns_number_gt 1040 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0539P)^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 1370 _refine_ls_number_parameters 97 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0290 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0736 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.928 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6343(2) 0.6169(2) 0.41722(9) 0.0263(5) Uani 1 1 d . . . C2 C 0.6368(3) 0.6317(3) 0.47129(9) 0.0297(5) Uani 1 1 d . . . H2 H 0.6213 0.5657 0.4952 0.036 Uiso 1 1 calc R . . C3 C 0.6667(3) 0.7634(3) 0.48235(10) 0.0334(6) Uani 1 1 d . . . H3 H 0.6753 0.7997 0.5149 0.040 Uiso 1 1 calc R . . C4 C 0.6815(3) 0.8308(3) 0.43559(10) 0.0336(6) Uani 1 1 d . . . H4 H 0.7008 0.9197 0.4319 0.040 Uiso 1 1 calc R . . C5 C 0.6624(3) 0.7418(2) 0.39579(10) 0.0302(5) Uani 1 1 d . . . H5 H 0.6673 0.7611 0.3610 0.036 Uiso 1 1 calc R . . C6 C 0.5973(2) 0.4967(2) 0.38834(9) 0.0246(5) Uani 1 1 d . . . Co1 Co 0.5000 0.7500 0.440058(16) 0.02396(16) Uani 1 2 d S . . O1 O 0.60601(19) 0.49792(18) 0.34150(7) 0.0355(4) Uani 1 1 d . . . O2 O 0.55996(17) 0.40150(16) 0.41527(6) 0.0281(4) Uani 1 1 d . . . O3 O 0.6291(4) 0.7029(4) 0.26642(14) 0.0877(10) Uani 1 1 d D . . Zn1 Zn 0.5000 0.2500 0.3750 0.02170(16) Uani 1 4 d S . . H3A H 0.616(10) 0.672(9) 0.2971(16) 0.25(5) Uiso 1 1 d D . . H3B H 0.691(7) 0.651(7) 0.253(3) 0.25(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0279(12) 0.0226(12) 0.0282(12) -0.0014(9) 0.0015(10) 0.0013(9) C2 0.0347(14) 0.0261(13) 0.0282(12) 0.0013(10) -0.0062(10) 0.0020(11) C3 0.0381(15) 0.0302(13) 0.0318(12) -0.0059(11) -0.0076(11) -0.0007(11) C4 0.0339(14) 0.0258(13) 0.0411(15) -0.0021(11) 0.0010(11) -0.0041(10) C5 0.0330(14) 0.0279(13) 0.0297(12) 0.0004(10) 0.0059(10) -0.0041(10) C6 0.0213(11) 0.0218(12) 0.0309(12) -0.0035(10) -0.0006(9) 0.0037(9) Co1 0.0322(3) 0.0176(2) 0.0220(2) 0.000 0.000 0.00035(18) O1 0.0472(11) 0.0317(10) 0.0277(9) -0.0037(8) 0.0032(8) -0.0013(8) O2 0.0342(10) 0.0199(8) 0.0301(8) -0.0012(7) -0.0024(8) -0.0026(7) O3 0.111(3) 0.073(2) 0.079(2) 0.0210(18) 0.008(2) -0.0085(19) Zn1 0.02057(19) 0.02057(19) 0.0240(3) 0.000 0.000 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.432(4) . ? C1 C2 1.434(4) . ? C1 C6 1.501(3) . ? C1 Co1 2.035(2) . ? C2 C3 1.418(4) . ? C2 Co1 2.033(3) . ? C3 C4 1.423(4) . ? C3 Co1 2.049(3) . ? C4 C5 1.406(4) . ? C4 Co1 2.046(3) . ? C5 Co1 2.039(3) . ? C6 O1 1.239(3) . ? C6 O2 1.269(3) . ? Co1 C2 2.033(3) 6_564 ? Co1 C1 2.035(2) 6_564 ? Co1 C5 2.039(3) 6_564 ? Co1 C4 2.046(3) 6_564 ? Co1 C3 2.049(3) 6_564 ? O2 Zn1 1.9831(17) . ? Zn1 O2 1.9831(17) 16_656 ? Zn1 O2 1.9831(17) 11_666 ? Zn1 O2 1.9831(17) 6_554 ? 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 C5 C1 C2 107.1(2) . . ? C5 C1 C6 126.1(2) . . ? C2 C1 C6 126.6(2) . . ? C5 C1 Co1 69.59(14) . . ? C2 C1 Co1 69.30(14) . . ? C6 C1 Co1 122.11(17) . . ? C3 C2 C1 108.0(2) . . ? C3 C2 Co1 70.29(15) . . ? C1 C2 Co1 69.41(14) . . ? C2 C3 C4 108.0(2) . . ? C2 C3 Co1 69.05(15) . . ? C4 C3 Co1 69.53(15) . . ? C5 C4 C3 108.4(2) . . ? C5 C4 Co1 69.61(15) . . ? C3 C4 Co1 69.80(16) . . ? C4 C5 C1 108.5(2) . . ? C4 C5 Co1 70.12(15) . . ? C1 C5 Co1 69.25(14) . . ? O1 C6 O2 126.0(2) . . ? O1 C6 C1 118.7(2) . . ? O2 C6 C1 115.3(2) . . ? C2 Co1 C2 132.20(15) . 6_564 ? C2 Co1 C1 172.40(10) . 6_564 ? C2 Co1 C1 41.29(10) 6_564 6_564 ? C2 Co1 C1 41.29(10) . . ? C2 Co1 C1 172.40(10) 6_564 . ? C1 Co1 C1 145.57(14) 6_564 . ? C2 Co1 C5 145.37(10) . 6_564 ? C2 Co1 C5 68.96(11) 6_564 6_564 ? C1 Co1 C5 41.16(10) 6_564 6_564 ? C1 Co1 C5 114.45(10) . 6_564 ? C2 Co1 C5 68.96(11) . . ? C2 Co1 C5 145.37(10) 6_564 . ? C1 Co1 C5 114.45(10) 6_564 . ? C1 Co1 C5 41.16(10) . . ? C5 Co1 C5 110.15(15) 6_564 . ? C2 Co1 C4 114.28(11) . 6_564 ? C2 Co1 C4 68.62(11) 6_564 6_564 ? C1 Co1 C4 68.72(10) 6_564 6_564 ? C1 Co1 C4 109.20(10) . 6_564 ? C5 Co1 C4 40.27(10) 6_564 6_564 ? C5 Co1 C4 134.20(11) . 6_564 ? C2 Co1 C4 68.62(11) . . ? C2 Co1 C4 114.28(11) 6_564 . ? C1 Co1 C4 109.20(10) 6_564 . ? C1 Co1 C4 68.72(10) . . ? C5 Co1 C4 134.20(11) 6_564 . ? C5 Co1 C4 40.27(10) . . ? C4 Co1 C4 173.40(16) 6_564 . ? C2 Co1 C3 40.65(11) . . ? C2 Co1 C3 108.52(11) 6_564 . ? C1 Co1 C3 133.12(10) 6_564 . ? C1 Co1 C3 68.82(10) . . ? C5 Co1 C3 173.51(11) 6_564 . ? C5 Co1 C3 68.26(11) . . ? C4 Co1 C3 145.21(11) 6_564 . ? C4 Co1 C3 40.67(11) . . ? C2 Co1 C3 108.52(11) . 6_564 ? C2 Co1 C3 40.65(11) 6_564 6_564 ? C1 Co1 C3 68.82(10) 6_564 6_564 ? C1 Co1 C3 133.12(10) . 6_564 ? C5 Co1 C3 68.26(11) 6_564 6_564 ? C5 Co1 C3 173.51(11) . 6_564 ? C4 Co1 C3 40.67(11) 6_564 6_564 ? C4 Co1 C3 145.21(11) . 6_564 ? C3 Co1 C3 114.05(16) . 6_564 ? C6 O2 Zn1 113.58(14) . . ? O2 Zn1 O2 115.24(10) 16_656 11_666 ? O2 Zn1 O2 106.67(5) 16_656 . ? O2 Zn1 O2 106.67(5) 11_666 . ? O2 Zn1 O2 106.67(5) 16_656 6_554 ? O2 Zn1 O2 106.67(5) 11_666 6_554 ? O2 Zn1 O2 115.24(10) . 6_554 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.651 _refine_diff_density_min -0.287 _refine_diff_density_rms 0.068 # start Validation Reply Form _vrf_PLAT415_ip1-761 ; PROBLEM: Short Inter D-H..H-X H3A .. H5 .. 1.99 Ang. RESPONSE: H3a belongs to a solvent water molecule. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 950058' ####################################################################### # # 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_t943 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H16 Co2 O8 Zn, 2(H0.50 O0.25), H0.50 O0.25 ' _chemical_formula_sum 'C24 H17.50 Co2 O8.75 Zn' _chemical_formula_weight 629.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'monoclinic, unique axis c' _symmetry_space_group_name_H-M 'I 1 1 2/b' _symmetry_space_group_name_Hall '-I 2b' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1, z+1/2' '-x, -y, -z' 'x, y-1/2, -z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y, -z+1/2' _cell_length_a 10.3301(10) _cell_length_b 10.2174(11) _cell_length_c 26.267(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 93.932(8) _cell_volume 2765.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8254 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 27.39 _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.511 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1262 _exptl_absorpt_coefficient_mu 2.090 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.5449 _exptl_absorpt_correction_T_max 0.7804 _exptl_absorpt_process_details 'STOE X-RED' _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8504 _diffrn_reflns_av_R_equivalents 0.0628 _diffrn_reflns_av_sigmaI/netI 0.0542 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 26.00 _reflns_number_total 2730 _reflns_number_gt 1794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _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^)+(0.1464P)^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 riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0023(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 2730 _refine_ls_number_parameters 164 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0947 _refine_ls_R_factor_gt 0.0687 _refine_ls_wR_factor_ref 0.2108 _refine_ls_wR_factor_gt 0.1961 _refine_ls_goodness_of_fit_ref 1.005 _refine_ls_restrained_S_all 1.005 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6346(6) 0.6269(6) 0.4176(2) 0.0440(14) Uani 1 1 d . . . C2 C 0.6366(7) 0.6421(6) 0.4716(2) 0.0473(15) Uani 1 1 d . . . H2 H 0.6214 0.5737 0.4958 0.057 Uiso 1 1 calc R . . C3 C 0.6653(7) 0.7772(6) 0.4832(2) 0.0471(15) Uani 1 1 d . . . H3 H 0.6741 0.8147 0.5162 0.056 Uiso 1 1 calc R . . C4 C 0.6785(5) 0.8462(5) 0.43551(18) 0.0508(16) Uani 1 1 d . . . H4 H 0.6948 0.9383 0.4315 0.061 Uiso 1 1 calc R . . C5 C 0.6631(5) 0.7536(5) 0.39561(18) 0.0494(15) Uani 1 1 d R . . H5 H 0.6704 0.7724 0.3603 0.059 Uiso 1 1 calc R . . C6 C 0.6026(6) 0.5028(6) 0.3886(2) 0.0457(14) Uani 1 1 d . . . C7 C 0.1456(6) 0.3810(6) 0.3319(2) 0.0435(14) Uani 1 1 d . . . C8 C 0.1285(7) 0.3866(6) 0.2777(2) 0.0456(14) Uani 1 1 d . . . H8 H 0.1922 0.3711 0.2528 0.055 Uiso 1 1 calc R . . C9 C -0.0020(7) 0.4196(6) 0.2679(2) 0.0470(15) Uani 1 1 d . . . H9 H -0.0401 0.4301 0.2354 0.056 Uiso 1 1 calc R . . C10 C -0.0634(7) 0.4336(6) 0.3153(2) 0.0491(16) Uani 1 1 d . . . H10 H -0.1506 0.4554 0.3198 0.059 Uiso 1 1 calc R . . C11 C 0.0237(7) 0.4106(7) 0.3552(2) 0.0475(15) Uani 1 1 d . . . H11 H 0.0058 0.4138 0.3906 0.057 Uiso 1 1 calc R . . C12 C 0.2610(6) 0.3404(6) 0.3604(2) 0.0433(13) Uani 1 1 d . . . Co1 Co 0.5000 0.7500 0.44006(4) 0.0422(4) Uani 1 2 d S . . Co2 Co 0.0000 0.2500 0.30991(4) 0.0416(4) Uani 1 2 d S . . O1 O 0.6201(5) 0.5032(5) 0.34169(17) 0.0584(13) Uani 1 1 d . . . O2 O 0.5589(5) 0.4061(4) 0.41555(16) 0.0476(10) Uani 1 1 d . . . O3 O 0.2574(5) 0.3386(5) 0.40745(16) 0.0549(12) Uani 1 1 d . . . O4 O 0.3545(4) 0.3077(4) 0.33236(16) 0.0478(11) Uani 1 1 d . . . Zn1 Zn 0.5000 0.2500 0.37433(4) 0.0406(3) Uani 1 2 d S . . O5 O 0.637(2) 0.714(2) 0.2664(9) 0.073(6) Uiso 0.25 1 d P . . O6 O 0.0000 0.7500 0.5110(17) 0.099(12) Uiso 0.25 2 d SP . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(4) 0.041(3) 0.039(3) -0.001(2) -0.003(3) 0.009(3) C2 0.056(4) 0.044(3) 0.043(3) 0.006(3) 0.004(3) 0.013(3) C3 0.057(4) 0.046(3) 0.039(3) -0.003(3) 0.000(3) 0.005(3) C4 0.061(4) 0.048(4) 0.044(3) -0.001(3) 0.000(3) 0.006(3) C5 0.057(4) 0.050(4) 0.041(3) 0.000(3) 0.002(3) 0.002(3) C6 0.047(4) 0.043(3) 0.048(3) -0.006(3) -0.005(3) 0.011(3) C7 0.051(4) 0.046(3) 0.034(3) -0.001(2) -0.005(3) 0.010(3) C8 0.053(4) 0.046(3) 0.038(3) 0.000(2) 0.007(3) 0.008(3) C9 0.055(4) 0.051(4) 0.036(3) 0.004(3) -0.003(3) 0.011(3) C10 0.056(4) 0.048(4) 0.045(3) -0.001(3) -0.009(3) 0.013(3) C11 0.056(4) 0.052(4) 0.036(3) -0.004(3) 0.000(3) 0.013(3) C12 0.049(4) 0.041(3) 0.041(3) 0.000(2) -0.002(3) 0.004(3) Co1 0.0553(8) 0.0380(6) 0.0341(6) 0.000 0.000 0.0080(5) Co2 0.0440(7) 0.0471(7) 0.0343(6) 0.000 0.000 0.0084(5) O1 0.085(4) 0.054(3) 0.037(2) -0.0037(19) 0.010(2) 0.002(2) O2 0.057(3) 0.043(2) 0.044(2) -0.0017(19) -0.009(2) 0.0069(19) O3 0.060(3) 0.069(3) 0.036(2) -0.004(2) -0.003(2) 0.010(2) O4 0.049(3) 0.055(3) 0.040(2) 0.0043(19) -0.0039(19) 0.008(2) Zn1 0.0456(6) 0.0407(6) 0.0360(5) 0.000 0.000 0.0071(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 C1 C2 1.427(9) . ? C1 C5 1.431(8) . ? C1 C6 1.496(8) . ? C1 Co1 2.025(6) . ? C2 C3 1.424(9) . ? C2 Co1 2.027(6) . ? C3 C4 1.439(8) . ? C3 Co1 2.052(7) . ? C4 C5 1.4131 . ? C4 Co1 2.033(5) . ? C5 Co1 2.048(5) . ? C6 O1 1.245(8) . ? C6 O2 1.273(8) . ? C7 C8 1.435(8) . ? C7 C11 1.451(9) . ? C7 C12 1.490(9) . ? C7 Co2 2.028(6) . ? C8 C9 1.435(9) . ? C8 Co2 2.042(7) . ? C9 C10 1.408(9) . ? C9 Co2 2.055(6) . ? C10 C11 1.411(9) . ? C10 Co2 2.034(6) . ? C11 Co2 2.027(6) . ? C12 O3 1.237(7) . ? C12 O4 1.278(7) . ? Co1 C1 2.025(6) 2_665 ? Co1 C2 2.027(6) 2_665 ? Co1 C4 2.033(5) 2_665 ? Co1 C5 2.048(5) 2_665 ? Co1 C3 2.052(7) 2_665 ? Co2 C11 2.027(6) 2 ? Co2 C7 2.028(7) 2 ? Co2 C10 2.034(6) 2 ? Co2 C8 2.042(7) 2 ? Co2 C9 2.055(6) 2 ? O2 Zn1 1.989(4) . ? O4 Zn1 1.985(4) . ? Zn1 O4 1.985(4) 2_655 ? Zn1 O2 1.989(4) 2_655 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 107.6(5) . . ? C2 C1 C6 126.9(6) . . ? C5 C1 C6 125.5(5) . . ? C2 C1 Co1 69.4(4) . . ? C5 C1 Co1 70.3(3) . . ? C6 C1 Co1 123.6(4) . . ? C3 C2 C1 108.6(6) . . ? C3 C2 Co1 70.5(4) . . ? C1 C2 Co1 69.3(3) . . ? C2 C3 C4 107.2(5) . . ? C2 C3 Co1 68.6(4) . . ? C4 C3 Co1 68.6(3) . . ? C5 C4 C3 108.4(3) . . ? C5 C4 Co1 70.31(13) . . ? C3 C4 Co1 70.1(3) . . ? C4 C5 C1 108.2(3) . . ? C4 C5 Co1 69.16(14) . . ? C1 C5 Co1 68.6(3) . . ? O1 C6 O2 126.6(6) . . ? O1 C6 C1 118.6(6) . . ? O2 C6 C1 114.8(5) . . ? C8 C7 C11 107.4(5) . . ? C8 C7 C12 127.8(6) . . ? C11 C7 C12 124.6(5) . . ? C8 C7 Co2 69.9(4) . . ? C11 C7 Co2 69.0(4) . . ? C12 C7 Co2 122.1(4) . . ? C7 C8 C9 107.9(5) . . ? C7 C8 Co2 68.8(4) . . ? C9 C8 Co2 70.0(4) . . ? C10 C9 C8 107.6(5) . . ? C10 C9 Co2 69.1(4) . . ? C8 C9 Co2 69.0(3) . . ? C9 C10 C11 110.0(6) . . ? C9 C10 Co2 70.7(4) . . ? C11 C10 Co2 69.4(4) . . ? C10 C11 C7 107.1(6) . . ? C10 C11 Co2 69.9(4) . . ? C7 C11 Co2 69.0(3) . . ? O3 C12 O4 126.4(6) . . ? O3 C12 C7 118.9(6) . . ? O4 C12 C7 114.6(5) . . ? C1 Co1 C1 146.2(3) 2_665 . ? C1 Co1 C2 41.2(2) 2_665 2_665 ? C1 Co1 C2 171.9(3) . 2_665 ? C1 Co1 C2 171.9(3) 2_665 . ? C1 Co1 C2 41.2(2) . . ? C2 Co1 C2 131.7(4) 2_665 . ? C1 Co1 C4 69.2(2) 2_665 2_665 ? C1 Co1 C4 108.7(2) . 2_665 ? C2 Co1 C4 69.2(2) 2_665 2_665 ? C2 Co1 C4 113.8(2) . 2_665 ? C1 Co1 C4 108.7(2) 2_665 . ? C1 Co1 C4 69.2(2) . . ? C2 Co1 C4 113.8(2) 2_665 . ? C2 Co1 C4 69.2(2) . . ? C4 Co1 C4 173.3(3) 2_665 . ? C1 Co1 C5 41.1(2) 2_665 2_665 ? C1 Co1 C5 114.9(2) . 2_665 ? C2 Co1 C5 68.9(2) 2_665 2_665 ? C2 Co1 C5 145.7(2) . 2_665 ? C4 Co1 C5 40.52(10) 2_665 2_665 ? C4 Co1 C5 133.9(2) . 2_665 ? C1 Co1 C5 114.9(2) 2_665 . ? C1 Co1 C5 41.1(2) . . ? C2 Co1 C5 145.7(2) 2_665 . ? C2 Co1 C5 68.9(2) . . ? C4 Co1 C5 133.9(2) 2_665 . ? C4 Co1 C5 40.52(10) . . ? C5 Co1 C5 110.5(3) 2_665 . ? C1 Co1 C3 69.2(2) 2_665 2_665 ? C1 Co1 C3 132.6(3) . 2_665 ? C2 Co1 C3 40.9(3) 2_665 2_665 ? C2 Co1 C3 107.7(3) . 2_665 ? C4 Co1 C3 41.2(2) 2_665 2_665 ? C4 Co1 C3 144.8(2) . 2_665 ? C5 Co1 C3 68.7(2) 2_665 2_665 ? C5 Co1 C3 173.2(2) . 2_665 ? C1 Co1 C3 132.6(3) 2_665 . ? C1 Co1 C3 69.2(2) . . ? C2 Co1 C3 107.7(3) 2_665 . ? C2 Co1 C3 40.9(3) . . ? C4 Co1 C3 144.8(2) 2_665 . ? C4 Co1 C3 41.2(2) . . ? C5 Co1 C3 173.2(2) 2_665 . ? C5 Co1 C3 68.7(2) . . ? C3 Co1 C3 113.0(4) 2_665 . ? C11 Co2 C11 108.2(4) 2 . ? C11 Co2 C7 114.2(3) 2 . ? C11 Co2 C7 41.9(3) . . ? C11 Co2 C7 41.9(3) 2 2 ? C11 Co2 C7 114.2(3) . 2 ? C7 Co2 C7 147.0(3) . 2 ? C11 Co2 C10 40.7(3) 2 2 ? C11 Co2 C10 132.6(3) . 2 ? C7 Co2 C10 108.5(3) . 2 ? C7 Co2 C10 69.1(3) 2 2 ? C11 Co2 C10 132.6(3) 2 . ? C11 Co2 C10 40.6(3) . . ? C7 Co2 C10 69.1(3) . . ? C7 Co2 C10 108.5(3) 2 . ? C10 Co2 C10 172.0(4) 2 . ? C11 Co2 C8 146.4(3) 2 . ? C11 Co2 C8 69.7(3) . . ? C7 Co2 C8 41.3(2) . . ? C7 Co2 C8 170.7(3) 2 . ? C10 Co2 C8 115.1(3) 2 . ? C10 Co2 C8 68.5(3) . . ? C11 Co2 C8 69.7(3) 2 2 ? C11 Co2 C8 146.4(3) . 2 ? C7 Co2 C8 170.7(3) . 2 ? C7 Co2 C8 41.3(2) 2 2 ? C10 Co2 C8 68.5(3) 2 2 ? C10 Co2 C8 115.1(3) . 2 ? C8 Co2 C8 131.1(4) . 2 ? C11 Co2 C9 68.9(3) 2 2 ? C11 Co2 C9 171.6(3) . 2 ? C7 Co2 C9 131.2(3) . 2 ? C7 Co2 C9 69.3(3) 2 2 ? C10 Co2 C9 40.3(3) 2 2 ? C10 Co2 C9 146.9(3) . 2 ? C8 Co2 C9 108.1(3) . 2 ? C8 Co2 C9 41.0(3) 2 2 ? C11 Co2 C9 171.6(3) 2 . ? C11 Co2 C9 68.9(3) . . ? C7 Co2 C9 69.3(3) . . ? C7 Co2 C9 131.2(3) 2 . ? C10 Co2 C9 146.9(3) 2 . ? C10 Co2 C9 40.3(3) . . ? C8 Co2 C9 41.0(3) . . ? C8 Co2 C9 108.1(3) 2 . ? C9 Co2 C9 115.1(4) 2 . ? C6 O2 Zn1 113.1(4) . . ? C12 O4 Zn1 111.1(4) . . ? O4 Zn1 O4 112.5(3) . 2_655 ? O4 Zn1 O2 110.13(19) . 2_655 ? O4 Zn1 O2 105.10(18) 2_655 2_655 ? O4 Zn1 O2 105.10(18) . . ? O4 Zn1 O2 110.13(19) 2_655 . ? O2 Zn1 O2 114.0(3) 2_655 . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.238 _refine_diff_density_min -0.618 _refine_diff_density_rms 0.224 _database_code_depnum_ccdc_archive 'CCDC 950059' ####################################################################### # # 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_ip2-948 _audit_creation_method SHELXL-97 _chemical_formula_moiety '(C24 H16 Co2 Cu O8),(C1.5 H6 O1.5)' _chemical_formula_sum 'C25.50 H22 Co2 Cu O9.50' _chemical_formula_weight 661.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 tetragonal _symmetry_space_group_name_H-M 'P 41' _symmetry_space_group_name_Hall 'P 4w ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 10.5609(6) _cell_length_b 10.5609(6) _cell_length_c 22.6410(16) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2525.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 6778 _cell_measurement_theta_min 1.04 _cell_measurement_theta_max 28.54 _exptl_crystal_description tip _exptl_crystal_colour green _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.741 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 2.188 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6331 _exptl_absorpt_correction_T_max 0.7978 _exptl_absorpt_process_details 'STOE X-RED' _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_reflns_number 8663 _diffrn_reflns_av_R_equivalents 0.0307 _diffrn_reflns_av_sigmaI/netI 0.0628 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.99 _reflns_number_total 5451 _reflns_number_gt 3901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0676P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.09(2) _refine_ls_number_reflns 5451 _refine_ls_number_parameters 356 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0668 _refine_ls_R_factor_gt 0.0454 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1081 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9071(6) 0.6732(6) 0.4974(3) 0.0352(13) Uani 1 1 d . . . C2 C 0.9510(6) 0.7888(6) 0.4710(3) 0.0425(15) Uani 1 1 d . . . H2 H 0.9793 0.7990 0.4315 0.051 Uiso 1 1 calc R . . C3 C 0.9444(6) 0.8857(6) 0.5150(3) 0.0464(16) Uani 1 1 d . . . H3 H 0.9682 0.9718 0.5099 0.056 Uiso 1 1 calc R . . C4 C 0.8959(6) 0.8308(6) 0.5675(3) 0.0449(15) Uani 1 1 d . . . H4 H 0.8810 0.8746 0.6035 0.054 Uiso 1 1 calc R . . C5 C 0.8732(6) 0.6998(6) 0.5576(3) 0.0409(14) Uani 1 1 d . . . H5 H 0.8414 0.6408 0.5856 0.049 Uiso 1 1 calc R . . C6 C 0.8823(6) 0.5495(6) 0.4665(3) 0.0402(14) Uani 1 1 d . . . C7 C 0.6427(6) 0.9471(6) 0.4848(3) 0.0331(13) Uani 1 1 d . . . C8 C 0.5982(6) 0.8664(7) 0.5314(3) 0.0439(15) Uani 1 1 d . . . H8 H 0.5802 0.8913 0.5709 0.053 Uiso 1 1 calc R . . C9 C 0.5862(7) 0.7417(7) 0.5075(3) 0.0515(18) Uani 1 1 d . . . H9 H 0.5575 0.6691 0.5284 0.062 Uiso 1 1 calc R . . C10 C 0.6244(7) 0.7449(7) 0.4471(3) 0.0467(16) Uani 1 1 d . . . H10 H 0.6265 0.6744 0.4210 0.056 Uiso 1 1 calc R . . C11 C 0.6592(7) 0.8727(6) 0.4322(3) 0.0415(14) Uani 1 1 d . . . H11 H 0.6876 0.9023 0.3949 0.050 Uiso 1 1 calc R . . C12 C 0.6767(6) 1.0862(6) 0.4910(3) 0.0358(13) Uani 1 1 d . . . C13 C 0.1507(6) 0.1877(6) 0.4593(3) 0.0358(13) Uani 1 1 d . . . C14 C 0.1863(6) 0.1769(6) 0.3993(3) 0.0411(15) Uani 1 1 d . . . H14 H 0.1309 0.1821 0.3663 0.049 Uiso 1 1 calc R . . C15 C 0.3201(6) 0.1568(7) 0.3970(4) 0.0490(17) Uani 1 1 d . . . H15 H 0.3690 0.1461 0.3621 0.059 Uiso 1 1 calc R . . C16 C 0.3672(6) 0.1555(7) 0.4557(4) 0.0506(18) Uani 1 1 d . . . H16 H 0.4527 0.1427 0.4672 0.061 Uiso 1 1 calc R . . C17 C 0.2636(6) 0.1767(7) 0.4938(3) 0.0429(15) Uani 1 1 d . . . H17 H 0.2681 0.1827 0.5356 0.052 Uiso 1 1 calc R . . C18 C 0.0212(6) 0.2173(6) 0.4809(3) 0.0367(14) Uani 1 1 d . . . C19 C 0.4209(6) 0.4540(6) 0.4283(3) 0.0385(14) Uani 1 1 d . . . C20 C 0.3347(7) 0.4603(6) 0.3800(3) 0.0446(15) Uani 1 1 d . . . H20 H 0.3564 0.4486 0.3396 0.054 Uiso 1 1 calc R . . C21 C 0.2101(7) 0.4871(6) 0.4018(3) 0.0452(16) Uani 1 1 d . . . H21 H 0.1354 0.4958 0.3788 0.054 Uiso 1 1 calc R . . C22 C 0.2192(6) 0.4985(6) 0.4654(3) 0.0457(15) Uani 1 1 d . . . H22 H 0.1517 0.5176 0.4917 0.055 Uiso 1 1 calc R . . C23 C 0.3498(6) 0.4754(7) 0.4819(3) 0.0431(15) Uani 1 1 d . . . H23 H 0.3827 0.4746 0.5209 0.052 Uiso 1 1 calc R . . C24 C 0.5569(6) 0.4131(6) 0.4258(3) 0.0403(14) Uani 1 1 d . . . C25 C 0.1792(9) 0.3327(10) 0.6401(4) 0.073(3) Uani 1 1 d . . . H25A H 0.1237 0.3651 0.6713 0.110 Uiso 1 1 calc R . . H25B H 0.1618 0.3778 0.6031 0.110 Uiso 1 1 calc R . . H25C H 0.2678 0.3458 0.6514 0.110 Uiso 1 1 calc R . . C26 C 0.866(2) 0.7391(14) 0.3008(9) 0.084(7) Uani 0.50 1 d P . . H26A H 0.8402 0.7935 0.2678 0.125 Uiso 0.50 1 calc PR . . H26B H 0.9196 0.6704 0.2860 0.125 Uiso 0.50 1 calc PR . . H26C H 0.9133 0.7892 0.3297 0.125 Uiso 0.50 1 calc PR . . Co1 Co 0.76942(8) 0.80699(8) 0.50022(3) 0.0355(2) Uani 1 1 d . . . Co2 Co 0.28048(8) 0.32407(9) 0.43726(3) 0.0365(2) Uani 1 1 d . . . Cu1 Cu 0.77543(7) 0.30990(7) 0.46486(4) 0.03406(16) Uani 1 1 d . . . O1 O 0.8466(4) 0.4612(4) 0.5000(2) 0.0429(10) Uani 1 1 d . . . O2 O 0.8974(5) 0.5445(4) 0.4121(2) 0.0486(12) Uani 1 1 d . . . O3 O 0.6671(6) 1.1329(5) 0.5407(2) 0.0542(13) Uani 1 1 d . . . O4 O 0.7083(4) 1.1417(4) 0.44428(19) 0.0407(10) Uani 1 1 d . . . O5 O -0.0026(4) 0.2102(5) 0.5345(2) 0.0498(12) Uani 1 1 d . . . O6 O -0.0583(4) 0.2479(5) 0.4414(2) 0.0431(10) Uani 1 1 d . . . O7 O 0.6056(4) 0.3834(4) 0.4743(2) 0.0436(11) Uani 1 1 d . . . O8 O 0.6088(5) 0.4107(7) 0.3780(2) 0.0683(16) Uani 1 1 d . . . O9 O 0.1572(7) 0.2055(6) 0.6322(3) 0.0753(17) Uani 1 1 d . . . H9A H 0.1499 0.1899 0.5960 0.113 Uiso 1 1 calc R . . O10 O 0.7678(13) 0.6923(11) 0.3253(5) 0.069(4) Uani 0.50 1 d P . . H10A H 0.7127 0.7490 0.3294 0.104 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.035(3) 0.025(3) 0.045(3) -0.006(3) 0.000(3) -0.003(2) C2 0.035(3) 0.039(4) 0.053(4) 0.005(3) 0.008(3) 0.000(3) C3 0.038(4) 0.029(3) 0.073(5) -0.005(3) 0.000(3) -0.003(3) C4 0.041(4) 0.038(4) 0.055(4) -0.008(3) -0.004(3) 0.000(3) C5 0.043(4) 0.030(3) 0.050(3) -0.004(3) -0.005(3) 0.000(3) C6 0.029(3) 0.038(3) 0.054(4) -0.003(3) -0.001(3) 0.009(2) C7 0.029(3) 0.027(3) 0.043(3) -0.001(2) 0.000(2) 0.000(2) C8 0.034(4) 0.048(4) 0.050(3) 0.002(3) 0.003(3) -0.002(3) C9 0.044(4) 0.045(4) 0.065(4) 0.010(4) -0.006(4) -0.006(3) C10 0.042(4) 0.038(4) 0.059(4) 0.005(3) -0.007(3) -0.010(3) C11 0.045(4) 0.034(3) 0.046(3) 0.000(3) -0.008(3) 0.001(3) C12 0.032(3) 0.036(3) 0.039(3) -0.004(3) -0.007(2) 0.011(3) C13 0.029(3) 0.033(3) 0.046(3) 0.001(3) 0.003(3) 0.001(2) C14 0.033(3) 0.036(4) 0.055(4) -0.007(3) 0.004(3) -0.003(3) C15 0.031(4) 0.040(4) 0.076(5) -0.005(3) 0.020(3) 0.001(3) C16 0.027(3) 0.042(4) 0.082(5) 0.004(4) -0.003(3) 0.007(3) C17 0.031(3) 0.052(4) 0.046(3) 0.003(3) -0.006(3) 0.006(3) C18 0.029(3) 0.032(3) 0.050(4) 0.002(3) 0.003(3) -0.004(2) C19 0.026(3) 0.037(3) 0.052(4) -0.006(3) 0.001(3) -0.005(2) C20 0.041(4) 0.039(4) 0.053(4) 0.003(3) -0.005(3) -0.001(3) C21 0.036(4) 0.033(3) 0.067(4) 0.001(3) -0.011(3) 0.004(3) C22 0.033(3) 0.039(4) 0.065(4) -0.009(3) 0.002(3) 0.008(3) C23 0.030(3) 0.045(4) 0.054(4) -0.009(3) -0.005(3) 0.000(3) C24 0.035(3) 0.035(3) 0.051(4) -0.005(3) 0.010(3) -0.004(3) C25 0.057(5) 0.080(7) 0.083(6) -0.009(5) -0.005(4) -0.003(5) C26 0.126(18) 0.018(8) 0.106(14) 0.028(8) 0.058(13) -0.005(9) Co1 0.0339(5) 0.0289(5) 0.0438(5) 0.0005(4) 0.0014(4) 0.0000(4) Co2 0.0257(5) 0.0334(5) 0.0502(5) -0.0009(4) 0.0001(4) -0.0002(4) Cu1 0.0279(4) 0.0279(4) 0.0464(4) -0.0018(3) -0.0003(3) 0.0008(4) O1 0.042(3) 0.031(2) 0.055(3) 0.003(2) 0.003(2) -0.0009(19) O2 0.059(3) 0.043(3) 0.043(3) -0.007(2) -0.001(2) 0.004(2) O3 0.071(4) 0.038(3) 0.053(3) -0.007(2) -0.006(2) 0.003(2) O4 0.042(3) 0.034(2) 0.046(2) 0.0027(19) 0.003(2) -0.0014(19) O5 0.041(3) 0.060(3) 0.048(3) 0.006(2) 0.007(2) 0.001(2) O6 0.038(3) 0.045(3) 0.047(2) -0.008(2) -0.005(2) 0.005(2) O7 0.030(2) 0.042(3) 0.060(3) -0.001(2) -0.004(2) 0.0041(19) O8 0.040(3) 0.102(5) 0.063(3) 0.001(3) 0.012(2) 0.003(3) O9 0.088(5) 0.074(4) 0.064(3) 0.004(3) -0.012(3) 0.004(4) O10 0.092(9) 0.062(7) 0.054(6) -0.008(5) 0.004(6) 0.052(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 C1 C2 1.435(9) . ? C1 C5 1.438(9) . ? C1 C6 1.505(9) . ? C1 Co1 2.029(6) . ? C2 C3 1.430(9) . ? C2 Co1 2.037(6) . ? C2 H2 0.9500 . ? C3 C4 1.419(10) . ? C3 Co1 2.053(7) . ? C3 H3 0.9500 . ? C4 C5 1.422(9) . ? C4 Co1 2.042(7) . ? C4 H4 0.9500 . ? C5 Co1 2.042(6) . ? C5 H5 0.9500 . ? C6 O2 1.244(8) . ? C6 O1 1.261(8) . ? C7 C8 1.436(9) . ? C7 C11 1.437(9) . ? C7 C12 1.518(9) . ? C7 Co1 2.026(6) . ? C8 C9 1.429(11) . ? C8 Co1 2.040(7) . ? C8 H8 0.9500 . ? C9 C10 1.428(10) . ? C9 Co1 2.061(8) . ? C9 H9 0.9500 . ? C10 C11 1.439(9) . ? C10 Co1 2.055(7) . ? C10 H10 0.9500 . ? C11 Co1 2.051(6) . ? C11 H11 0.9500 . ? C12 O3 1.235(7) . ? C12 O4 1.254(7) . ? C13 C14 1.415(9) . ? C13 C17 1.429(9) . ? C13 C18 1.486(9) . ? C13 Co2 2.050(6) . ? C14 C15 1.430(9) . ? C14 Co2 2.036(7) . ? C14 H14 0.9500 . ? C15 C16 1.419(11) . ? C15 Co2 2.032(7) . ? C15 H15 0.9500 . ? C16 C17 1.412(10) . ? C16 Co2 2.045(7) . ? C16 H16 0.9500 . ? C17 Co2 2.023(7) . ? C17 H17 0.9500 . ? C18 O5 1.243(8) . ? C18 O6 1.268(7) . ? C19 C20 1.425(9) . ? C19 C23 1.445(9) . ? C19 C24 1.501(9) . ? C19 Co2 2.030(6) . ? C20 C21 1.434(10) . ? C20 Co2 2.020(7) . ? C20 H20 0.9500 . ? C21 C22 1.448(10) . ? C21 Co2 2.040(7) . ? C21 H21 0.9500 . ? C22 C23 1.449(9) . ? C22 Co2 2.054(6) . ? C22 H22 0.9500 . ? C23 Co2 2.028(7) . ? C23 H23 0.9500 . ? C24 O8 1.214(8) . ? C24 O7 1.252(8) . ? C25 O9 1.375(12) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 O10 1.28(2) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? Cu1 O1 1.937(5) . ? Cu1 O6 1.948(5) 1_655 ? Cu1 O7 1.966(4) . ? Cu1 O4 1.969(5) 1_545 ? O4 Cu1 1.969(4) 1_565 ? O6 Cu1 1.948(5) 1_455 ? O9 H9A 0.8400 . ? O10 H10A 0.8400 . ? 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 C2 C1 C5 108.0(5) . . ? C2 C1 C6 126.9(6) . . ? C5 C1 C6 124.6(6) . . ? C2 C1 Co1 69.7(4) . . ? C5 C1 Co1 69.8(4) . . ? C6 C1 Co1 119.6(4) . . ? C3 C2 C1 107.7(6) . . ? C3 C2 Co1 70.1(4) . . ? C1 C2 Co1 69.0(4) . . ? C3 C2 H2 126.2 . . ? C1 C2 H2 126.2 . . ? Co1 C2 H2 126.3 . . ? C4 C3 C2 108.0(6) . . ? C4 C3 Co1 69.3(4) . . ? C2 C3 Co1 68.9(4) . . ? C4 C3 H3 126.0 . . ? C2 C3 H3 126.0 . . ? Co1 C3 H3 127.3 . . ? C3 C4 C5 109.1(6) . . ? C3 C4 Co1 70.2(4) . . ? C5 C4 Co1 69.6(4) . . ? C3 C4 H4 125.5 . . ? C5 C4 H4 125.5 . . ? Co1 C4 H4 126.3 . . ? C4 C5 C1 107.3(6) . . ? C4 C5 Co1 69.6(4) . . ? C1 C5 Co1 68.8(4) . . ? C4 C5 H5 126.3 . . ? C1 C5 H5 126.3 . . ? Co1 C5 H5 126.8 . . ? O2 C6 O1 127.1(6) . . ? O2 C6 C1 118.4(6) . . ? O1 C6 C1 114.5(6) . . ? C8 C7 C11 108.9(5) . . ? C8 C7 C12 125.7(5) . . ? C11 C7 C12 125.2(5) . . ? C8 C7 Co1 69.9(4) . . ? C11 C7 Co1 70.3(3) . . ? C12 C7 Co1 122.3(4) . . ? C9 C8 C7 107.3(6) . . ? C9 C8 Co1 70.4(4) . . ? C7 C8 Co1 68.8(4) . . ? C9 C8 H8 126.3 . . ? C7 C8 H8 126.3 . . ? Co1 C8 H8 126.0 . . ? C10 C9 C8 108.4(6) . . ? C10 C9 Co1 69.5(4) . . ? C8 C9 Co1 68.8(4) . . ? C10 C9 H9 125.8 . . ? C8 C9 H9 125.8 . . ? Co1 C9 H9 127.5 . . ? C9 C10 C11 108.5(6) . . ? C9 C10 Co1 69.9(4) . . ? C11 C10 Co1 69.3(4) . . ? C9 C10 H10 125.7 . . ? C11 C10 H10 125.7 . . ? Co1 C10 H10 126.6 . . ? C7 C11 C10 106.8(6) . . ? C7 C11 Co1 68.4(3) . . ? C10 C11 Co1 69.7(4) . . ? C7 C11 H11 126.6 . . ? C10 C11 H11 126.6 . . ? Co1 C11 H11 126.9 . . ? O3 C12 O4 127.2(6) . . ? O3 C12 C7 116.8(6) . . ? O4 C12 C7 116.0(5) . . ? C14 C13 C17 107.2(6) . . ? C14 C13 C18 125.2(6) . . ? C17 C13 C18 127.3(6) . . ? C14 C13 Co2 69.2(4) . . ? C17 C13 Co2 68.5(4) . . ? C18 C13 Co2 123.2(4) . . ? C13 C14 C15 108.1(6) . . ? C13 C14 Co2 70.3(4) . . ? C15 C14 Co2 69.3(4) . . ? C13 C14 H14 126.0 . . ? C15 C14 H14 126.0 . . ? Co2 C14 H14 126.0 . . ? C16 C15 C14 108.2(6) . . ? C16 C15 Co2 70.1(4) . . ? C14 C15 Co2 69.5(4) . . ? C16 C15 H15 125.9 . . ? C14 C15 H15 125.9 . . ? Co2 C15 H15 126.0 . . ? C17 C16 C15 107.5(6) . . ? C17 C16 Co2 68.9(4) . . ? C15 C16 Co2 69.1(4) . . ? C17 C16 H16 126.3 . . ? C15 C16 H16 126.3 . . ? Co2 C16 H16 127.3 . . ? C16 C17 C13 109.0(6) . . ? C16 C17 Co2 70.5(4) . . ? C13 C17 Co2 70.5(4) . . ? C16 C17 H17 125.5 . . ? C13 C17 H17 125.5 . . ? Co2 C17 H17 125.1 . . ? O5 C18 O6 124.8(6) . . ? O5 C18 C13 119.6(6) . . ? O6 C18 C13 115.6(5) . . ? C20 C19 C23 107.8(5) . . ? C20 C19 C24 126.6(6) . . ? C23 C19 C24 125.1(6) . . ? C20 C19 Co2 69.0(4) . . ? C23 C19 Co2 69.0(4) . . ? C24 C19 Co2 120.6(5) . . ? C19 C20 C21 109.3(6) . . ? C19 C20 Co2 69.8(4) . . ? C21 C20 Co2 70.1(4) . . ? C19 C20 H20 125.3 . . ? C21 C20 H20 125.3 . . ? Co2 C20 H20 126.4 . . ? C20 C21 C22 107.3(6) . . ? C20 C21 Co2 68.6(4) . . ? C22 C21 Co2 69.8(4) . . ? C20 C21 H21 126.3 . . ? C22 C21 H21 126.3 . . ? Co2 C21 H21 126.9 . . ? C21 C22 C23 107.8(6) . . ? C21 C22 Co2 68.8(4) . . ? C23 C22 Co2 68.3(4) . . ? C21 C22 H22 126.1 . . ? C23 C22 H22 126.1 . . ? Co2 C22 H22 128.4 . . ? C19 C23 C22 107.8(6) . . ? C19 C23 Co2 69.2(4) . . ? C22 C23 Co2 70.2(4) . . ? C19 C23 H23 126.1 . . ? C22 C23 H23 126.1 . . ? Co2 C23 H23 126.0 . . ? O8 C24 O7 126.2(6) . . ? O8 C24 C19 118.2(6) . . ? O7 C24 C19 115.6(6) . . ? O9 C25 H25A 109.5 . . ? O9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O10 C26 H26A 109.5 . . ? O10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C7 Co1 C1 167.7(2) . . ? C7 Co1 C2 129.4(3) . . ? C1 Co1 C2 41.3(2) . . ? C7 Co1 C8 41.4(3) . . ? C1 Co1 C8 149.4(3) . . ? C2 Co1 C8 167.3(3) . . ? C7 Co1 C4 118.1(3) . . ? C1 Co1 C4 68.9(3) . . ? C2 Co1 C4 68.8(3) . . ? C8 Co1 C4 106.4(3) . . ? C7 Co1 C5 150.3(2) . . ? C1 Co1 C5 41.4(2) . . ? C2 Co1 C5 69.5(3) . . ? C8 Co1 C5 115.2(3) . . ? C4 Co1 C5 40.7(3) . . ? C7 Co1 C11 41.3(2) . . ? C1 Co1 C11 128.2(3) . . ? C2 Co1 C11 108.8(3) . . ? C8 Co1 C11 69.7(3) . . ? C4 Co1 C11 152.8(3) . . ? C5 Co1 C11 165.9(3) . . ? C7 Co1 C3 109.1(3) . . ? C1 Co1 C3 69.0(3) . . ? C2 Co1 C3 40.9(3) . . ? C8 Co1 C3 128.0(3) . . ? C4 Co1 C3 40.5(3) . . ? C5 Co1 C3 68.8(3) . . ? C11 Co1 C3 119.7(3) . . ? C7 Co1 C10 68.9(3) . . ? C1 Co1 C10 107.1(3) . . ? C2 Co1 C10 118.8(3) . . ? C8 Co1 C10 68.9(3) . . ? C4 Co1 C10 164.5(3) . . ? C5 Co1 C10 126.6(3) . . ? C11 Co1 C10 41.0(3) . . ? C3 Co1 C10 153.5(3) . . ? C7 Co1 C9 68.8(3) . . ? C1 Co1 C9 116.3(3) . . ? C2 Co1 C9 151.4(3) . . ? C8 Co1 C9 40.8(3) . . ? C4 Co1 C9 126.5(3) . . ? C5 Co1 C9 105.5(3) . . ? C11 Co1 C9 68.9(3) . . ? C3 Co1 C9 165.3(3) . . ? C10 Co1 C9 40.6(3) . . ? C20 Co2 C17 168.3(3) . . ? C20 Co2 C23 69.9(3) . . ? C17 Co2 C23 108.8(3) . . ? C20 Co2 C19 41.2(3) . . ? C17 Co2 C19 130.3(3) . . ? C23 Co2 C19 41.7(3) . . ? C20 Co2 C15 105.8(3) . . ? C17 Co2 C15 68.5(3) . . ? C23 Co2 C15 146.6(3) . . ? C19 Co2 C15 113.1(3) . . ? C20 Co2 C14 114.3(3) . . ? C17 Co2 C14 68.7(3) . . ? C23 Co2 C14 171.3(3) . . ? C19 Co2 C14 146.2(3) . . ? C15 Co2 C14 41.2(3) . . ? C20 Co2 C21 41.4(3) . . ? C17 Co2 C21 150.0(3) . . ? C23 Co2 C21 70.2(3) . . ? C19 Co2 C21 69.9(3) . . ? C15 Co2 C21 129.2(3) . . ? C14 Co2 C21 107.5(3) . . ? C20 Co2 C16 128.6(3) . . ? C17 Co2 C16 40.6(3) . . ? C23 Co2 C16 115.0(3) . . ? C19 Co2 C16 106.4(3) . . ? C15 Co2 C16 40.7(3) . . ? C14 Co2 C16 68.9(3) . . ? C21 Co2 C16 168.0(3) . . ? C20 Co2 C13 147.8(3) . . ? C17 Co2 C13 41.1(3) . . ? C23 Co2 C13 132.3(3) . . ? C19 Co2 C13 170.9(3) . . ? C15 Co2 C13 68.7(3) . . ? C14 Co2 C13 40.5(3) . . ? C21 Co2 C13 116.4(3) . . ? C16 Co2 C13 68.8(3) . . ? C20 Co2 C22 69.5(3) . . ? C17 Co2 C22 117.7(3) . . ? C23 Co2 C22 41.6(3) . . ? C19 Co2 C22 69.8(3) . . ? C15 Co2 C22 169.8(3) . . ? C14 Co2 C22 131.5(3) . . ? C21 Co2 C22 41.4(3) . . ? C16 Co2 C22 149.1(3) . . ? C13 Co2 C22 110.1(3) . . ? O1 Cu1 O6 92.3(2) . 1_655 ? O1 Cu1 O7 89.06(19) . . ? O6 Cu1 O7 170.0(2) 1_655 . ? O1 Cu1 O4 168.93(19) . 1_545 ? O6 Cu1 O4 87.5(2) 1_655 1_545 ? O7 Cu1 O4 93.1(2) . 1_545 ? C6 O1 Cu1 118.6(4) . . ? C12 O4 Cu1 108.6(4) . 1_565 ? C18 O6 Cu1 119.4(4) . 1_455 ? C24 O7 Cu1 112.3(4) . . ? C25 O9 H9A 109.5 . . ? C26 O10 H10A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.632 _refine_diff_density_min -0.561 _refine_diff_density_rms 0.088 # start Validation Reply Form _vrf_PLAT415_ip2-948 ; PROBLEM: Short Inter D-H..H-X H9A .. H17 .. 1.85 Ang. RESPONSE: H9a belongs to a solvent methanol molecule. ; _vrf_PLAT241_ip2-948 ; PROBLEM: Check High Ueq as Compared to Neighbors for O8 RESPONSE: O8 is a non-coordinating carboxylate oxygen atom. ; _vrf_PLAT420_ip2-948 ; PROBLEM: D-H Without Acceptor *O10 - *H10A ... ? Check RESPONSE: H10a belongs to a solvent methanol molecule. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 950060' ####################################################################### # # 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_ip2-953a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_formula_moiety '(C24 H16 Co2 Cu O8),(C0.5 H2 O0.5)' _chemical_formula_sum 'C24.50 H18 Co2 Cu O8.50' _chemical_formula_weight 629.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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 tetragonal _symmetry_space_group_name_H-M 'P 41' _symmetry_space_group_name_Hall 'P 4w ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+1/4' 'y, -x, z+3/4' _cell_length_a 10.5985(12) _cell_length_b 10.5985(12) _cell_length_c 20.400(3) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2291.5(5) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9772 _cell_measurement_theta_min 1.45 _cell_measurement_theta_max 27.4 _exptl_crystal_description tip _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.826 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 2.404 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.6135 _exptl_absorpt_correction_T_max 0.7512 _exptl_absorpt_process_details ' STOE X-RED' _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_probe x-ray _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device '2-circle goniometer' _diffrn_measurement_device_type 'STOE IPDS-2T' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 6.67 _diffrn_detector 'image plate (34 cm diameter / schwenk)' _diffrn_detector_type STOE _diffrn_reflns_number 6992 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0619 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4371 _reflns_number_gt 2936 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'DIAMOND 3.2' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1661P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.33(5) _refine_ls_number_reflns 4371 _refine_ls_number_parameters 337 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1071 _refine_ls_R_factor_gt 0.0765 _refine_ls_wR_factor_ref 0.2422 _refine_ls_wR_factor_gt 0.2240 _refine_ls_goodness_of_fit_ref 0.988 _refine_ls_restrained_S_all 0.988 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.9095(15) 0.7054(13) 0.4624(8) 0.070(4) Uani 1 1 d . . . C2 C 0.9441(14) 0.8151(17) 0.4234(9) 0.076(4) Uani 1 1 d . . . H2 H 0.9585 0.8176 0.3774 0.092 Uiso 1 1 calc R . . C3 C 0.9522(14) 0.9189(19) 0.4685(19) 0.138(12) Uani 1 1 d . . . H3 H 0.9802 1.0022 0.4592 0.166 Uiso 1 1 calc R . . C4 C 0.9070(19) 0.868(2) 0.5338(11) 0.098(6) Uani 1 1 d . . . H4 H 0.8935 0.9168 0.5724 0.117 Uiso 1 1 calc R . . C5 C 0.8884(19) 0.7381(17) 0.5277(8) 0.086(5) Uani 1 1 d . . . H5 H 0.8655 0.6820 0.5620 0.103 Uiso 1 1 calc R . . C6 C 0.8872(16) 0.5703(19) 0.4315(8) 0.080(5) Uani 1 1 d . . . C7 C 0.6451(13) 0.9739(13) 0.4590(7) 0.060(3) Uani 1 1 d . . . C8 C 0.6103(16) 0.8838(16) 0.5100(7) 0.071(4) Uani 1 1 d . . . H8 H 0.5975 0.9000 0.5553 0.085 Uiso 1 1 calc R . . C9 C 0.5999(14) 0.7659(15) 0.4764(8) 0.071(4) Uani 1 1 d . . . H9 H 0.5770 0.6902 0.4984 0.085 Uiso 1 1 calc R . . C10 C 0.6229(14) 0.7687(14) 0.4160(8) 0.063(3) Uani 1 1 d . . . H10 H 0.6236 0.6992 0.3866 0.076 Uiso 1 1 calc R . . C11 C 0.6488(14) 0.9031(13) 0.4001(6) 0.058(3) Uani 1 1 d . . . H11 H 0.6651 0.9360 0.3576 0.069 Uiso 1 1 calc R . . C12 C 0.6825(12) 1.1064(16) 0.4713(7) 0.061(3) Uani 1 1 d . . . C13 C 0.1567(13) 0.2087(14) 0.4712(7) 0.064(4) Uani 1 1 d . . . C14 C 0.2114(14) 0.1746(13) 0.4111(8) 0.064(4) Uani 1 1 d . . . H14 H 0.1676 0.1643 0.3708 0.076 Uiso 1 1 calc R . . C15 C 0.3418(12) 0.1583(14) 0.4203(6) 0.058(3) Uani 1 1 d . . . H15 H 0.4012 0.1361 0.3875 0.070 Uiso 1 1 calc R . . C16 C 0.3682(14) 0.1803(14) 0.4851(6) 0.062(3) Uani 1 1 d . . . H16 H 0.4504 0.1780 0.5036 0.074 Uiso 1 1 calc R . . C17 C 0.2612(17) 0.2058(12) 0.5197(7) 0.069(4) Uani 1 1 d . . . H17 H 0.2547 0.2191 0.5656 0.083 Uiso 1 1 calc R . . C18 C 0.0231(15) 0.2492(14) 0.4877(8) 0.065(4) Uani 1 1 d . . . C19 C 0.4280(12) 0.4685(10) 0.4240(5) 0.046(2) Uani 1 1 d . . . C20 C 0.3324(11) 0.4616(12) 0.3732(5) 0.049(3) Uani 1 1 d . . . H20 H 0.3467 0.4438 0.3281 0.059 Uiso 1 1 calc R . . C21 C 0.2140(12) 0.4861(12) 0.4028(6) 0.053(3) Uani 1 1 d . . . H21 H 0.1351 0.4859 0.3807 0.064 Uiso 1 1 calc R . . C22 C 0.2313(14) 0.5109(14) 0.4706(7) 0.068(3) Uani 1 1 d . . . H22 H 0.1676 0.5309 0.5016 0.081 Uiso 1 1 calc R . . C23 C 0.3659(15) 0.4997(14) 0.4830(7) 0.065(3) Uani 1 1 d . . . H23 H 0.4057 0.5116 0.5243 0.078 Uiso 1 1 calc R . . C24 C 0.5610(11) 0.4382(12) 0.4156(5) 0.049(3) Uani 1 1 d . . . C25 C 0.159(2) 0.278(2) 0.7200(11) 0.050(6) Uani 0.50 1 d P . . H25A H 0.0940 0.3435 0.7168 0.074 Uiso 0.50 1 calc PR . . H25B H 0.1255 0.1983 0.7029 0.074 Uiso 0.50 1 calc PR . . H25C H 0.2329 0.3031 0.6942 0.074 Uiso 0.50 1 calc PR . . Co1 Co 0.77473(18) 0.83422(17) 0.46563(8) 0.0581(5) Uani 1 1 d . . . Co2 Co 0.29251(16) 0.33831(16) 0.44737(7) 0.0514(5) Uani 1 1 d . . . Cu1 Cu 0.78871(14) 0.33161(15) 0.45055(8) 0.0556(4) Uani 1 1 d . . . O1 O 0.8609(10) 0.4917(11) 0.4747(5) 0.074(3) Uani 1 1 d . . . O2 O 0.9096(12) 0.5612(11) 0.3749(6) 0.085(3) Uani 1 1 d . . . O3 O 0.6782(10) 1.1428(10) 0.5288(4) 0.068(2) Uani 1 1 d . . . O4 O 0.7154(9) 1.1695(9) 0.4228(5) 0.062(2) Uani 1 1 d . . . O5 O -0.0105(12) 0.2637(15) 0.5422(6) 0.102(4) Uani 1 1 d . . . O6 O -0.0451(10) 0.2618(11) 0.4347(5) 0.072(3) Uani 1 1 d . . . O7 O 0.6172(9) 0.3946(10) 0.4638(5) 0.067(2) Uani 1 1 d . . . O8 O 0.6082(9) 0.4492(12) 0.3597(4) 0.075(3) Uani 1 1 d . . . O9 O 0.193(3) 0.263(3) 0.7837(9) 0.095(8) Uani 0.50 1 d P . . H9A H 0.1304 0.2375 0.8054 0.142 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.077(9) 0.049(7) 0.085(9) -0.003(7) -0.008(8) -0.018(6) C2 0.042(7) 0.089(12) 0.099(11) -0.004(9) 0.008(7) 0.013(7) C3 0.034(8) 0.064(11) 0.32(4) -0.030(18) -0.038(15) -0.019(7) C4 0.072(11) 0.086(13) 0.135(16) -0.018(11) -0.043(11) 0.020(10) C5 0.108(14) 0.074(11) 0.076(9) -0.011(8) -0.034(9) -0.005(9) C6 0.072(10) 0.096(13) 0.073(10) -0.034(9) -0.003(8) 0.008(9) C7 0.060(7) 0.065(8) 0.057(7) -0.002(6) -0.001(6) -0.022(6) C8 0.080(11) 0.081(11) 0.050(7) 0.011(6) -0.002(6) -0.001(8) C9 0.048(8) 0.070(10) 0.094(11) 0.016(8) 0.013(7) 0.001(7) C10 0.051(8) 0.065(9) 0.074(8) 0.008(6) 0.001(6) 0.010(6) C11 0.077(9) 0.056(8) 0.041(5) 0.011(5) 0.006(5) -0.004(6) C12 0.033(6) 0.091(10) 0.059(7) -0.002(7) -0.008(5) 0.021(6) C13 0.059(8) 0.069(9) 0.064(7) 0.019(6) -0.006(6) -0.025(7) C14 0.072(9) 0.043(7) 0.076(8) -0.028(6) -0.007(7) -0.007(6) C15 0.040(7) 0.073(9) 0.060(7) 0.005(6) 0.015(5) 0.015(6) C16 0.046(7) 0.069(9) 0.070(8) -0.013(6) -0.008(6) 0.012(6) C17 0.108(12) 0.034(6) 0.066(8) 0.009(5) -0.013(8) -0.010(7) C18 0.061(9) 0.058(8) 0.075(9) 0.014(6) 0.000(7) -0.006(6) C19 0.051(7) 0.031(5) 0.055(6) 0.000(4) 0.009(5) -0.005(5) C20 0.043(6) 0.058(7) 0.045(5) 0.006(5) 0.004(4) -0.001(5) C21 0.038(6) 0.060(8) 0.062(7) -0.004(5) -0.009(5) 0.005(5) C22 0.059(8) 0.062(9) 0.082(9) -0.003(7) 0.009(7) -0.001(6) C23 0.078(10) 0.055(8) 0.061(7) 0.013(6) -0.008(6) -0.002(7) C24 0.039(6) 0.055(7) 0.053(6) -0.002(5) -0.014(5) 0.002(5) C25 0.056(14) 0.039(12) 0.053(13) -0.022(10) 0.001(10) -0.014(10) Co1 0.0617(11) 0.0515(11) 0.0612(11) -0.0008(8) -0.0046(8) 0.0009(8) Co2 0.0493(9) 0.0500(9) 0.0550(9) -0.0003(7) -0.0016(7) -0.0013(7) Cu1 0.0464(8) 0.0536(9) 0.0668(9) -0.0005(7) 0.0010(7) 0.0021(7) O1 0.066(6) 0.071(7) 0.086(7) 0.016(5) 0.002(5) -0.006(5) O2 0.092(8) 0.065(7) 0.099(8) -0.004(6) -0.007(6) 0.005(6) O3 0.076(7) 0.070(6) 0.058(5) -0.008(4) -0.008(4) 0.002(5) O4 0.059(6) 0.055(6) 0.073(6) 0.009(4) 0.007(4) 0.000(4) O5 0.076(8) 0.144(12) 0.086(7) 0.016(7) 0.036(6) 0.023(7) O6 0.055(6) 0.077(7) 0.084(7) -0.029(5) 0.015(5) -0.007(5) O7 0.063(6) 0.081(7) 0.056(5) 0.009(5) 0.002(4) 0.003(5) O8 0.053(5) 0.115(9) 0.058(5) 0.019(5) 0.001(4) 0.010(5) O9 0.114(19) 0.12(2) 0.048(10) 0.012(11) -0.005(10) 0.043(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C5 1.40(2) . ? C1 C2 1.46(2) . ? C1 C6 1.58(2) . ? C1 Co1 1.977(16) . ? C2 C3 1.44(3) . ? C2 Co1 2.002(15) . ? C2 H2 0.9500 . ? C3 C4 1.51(4) . ? C3 Co1 2.085(14) . ? C3 H3 0.9500 . ? C4 C5 1.40(3) . ? C4 Co1 2.008(17) . ? C4 H4 0.9500 . ? C5 Co1 2.023(17) . ? C5 H5 0.9500 . ? C6 O2 1.18(2) . ? C6 O1 1.24(2) . ? C7 C11 1.418(19) . ? C7 C8 1.46(2) . ? C7 C12 1.48(2) . ? C7 Co1 2.024(15) . ? C8 C9 1.43(2) . ? C8 Co1 2.033(17) . ? C8 H8 0.9500 . ? C9 C10 1.26(2) . ? C9 Co1 2.002(15) . ? C9 H9 0.9500 . ? C10 C11 1.49(2) . ? C10 Co1 2.024(16) . ? C10 H10 0.9500 . ? C11 Co1 2.026(13) . ? C11 H11 0.9500 . ? C12 O3 1.236(16) . ? C12 O4 1.244(17) . ? C13 C14 1.40(2) . ? C13 C17 1.48(2) . ? C13 C18 1.52(2) . ? C13 Co2 2.048(12) . ? C14 C15 1.405(19) . ? C14 Co2 2.073(12) . ? C14 H14 0.9500 . ? C15 C16 1.371(19) . ? C15 Co2 2.053(15) . ? C15 H15 0.9500 . ? C16 C17 1.36(2) . ? C16 Co2 2.010(15) . ? C16 H16 0.9500 . ? C17 Co2 2.063(13) . ? C17 H17 0.9500 . ? C18 O5 1.177(18) . ? C18 O6 1.307(18) . ? C19 C23 1.411(18) . ? C19 C20 1.452(16) . ? C19 C24 1.455(17) . ? C19 Co2 2.048(11) . ? C20 C21 1.417(17) . ? C20 Co2 2.044(11) . ? C20 H20 0.9500 . ? C21 C22 1.42(2) . ? C21 Co2 1.993(13) . ? C21 H21 0.9500 . ? C22 C23 1.45(2) . ? C22 Co2 1.998(15) . ? C22 H22 0.9500 . ? C23 Co2 2.015(15) . ? C23 H23 0.9500 . ? C24 O7 1.240(14) . ? C24 O8 1.250(15) . ? C25 O9 1.36(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? Cu1 O1 1.926(12) . ? Cu1 O6 1.937(10) 1_655 ? Cu1 O7 1.956(10) . ? Cu1 O4 1.969(10) 1_545 ? O4 Cu1 1.969(10) 1_565 ? O6 Cu1 1.937(10) 1_455 ? O9 H9A 0.8400 . ? 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 C5 C1 C2 111.3(14) . . ? C5 C1 C6 125.5(15) . . ? C2 C1 C6 122.9(14) . . ? C5 C1 Co1 71.4(10) . . ? C2 C1 Co1 69.4(8) . . ? C6 C1 Co1 122.1(11) . . ? C3 C2 C1 106.1(19) . . ? C3 C2 Co1 72.6(10) . . ? C1 C2 Co1 67.6(9) . . ? C3 C2 H2 127.0 . . ? C1 C2 H2 127.0 . . ? Co1 C2 H2 124.5 . . ? C2 C3 C4 105.9(17) . . ? C2 C3 Co1 66.3(8) . . ? C4 C3 Co1 65.6(9) . . ? C2 C3 H3 127.0 . . ? C4 C3 H3 127.0 . . ? Co1 C3 H3 132.5 . . ? C5 C4 C3 108.4(18) . . ? C5 C4 Co1 70.3(10) . . ? C3 C4 Co1 71.0(10) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Co1 C4 H4 124.5 . . ? C1 C5 C4 107.9(18) . . ? C1 C5 Co1 67.8(9) . . ? C4 C5 Co1 69.1(10) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Co1 C5 H5 128.6 . . ? O2 C6 O1 133.0(18) . . ? O2 C6 C1 115.6(18) . . ? O1 C6 C1 110.9(13) . . ? C11 C7 C8 105.4(11) . . ? C11 C7 C12 129.6(12) . . ? C8 C7 C12 124.5(13) . . ? C11 C7 Co1 69.6(8) . . ? C8 C7 Co1 69.2(9) . . ? C12 C7 Co1 120.0(9) . . ? C9 C8 C7 104.4(13) . . ? C9 C8 Co1 68.1(9) . . ? C7 C8 Co1 68.6(9) . . ? C9 C8 H8 127.8 . . ? C7 C8 H8 127.8 . . ? Co1 C8 H8 127.1 . . ? C10 C9 C8 115.8(15) . . ? C10 C9 Co1 72.8(10) . . ? C8 C9 Co1 70.4(9) . . ? C10 C9 H9 122.1 . . ? C8 C9 H9 122.1 . . ? Co1 C9 H9 126.4 . . ? C9 C10 C11 105.9(15) . . ? C9 C10 Co1 70.9(11) . . ? C11 C10 Co1 68.5(8) . . ? C9 C10 H10 127.1 . . ? C11 C10 H10 127.1 . . ? Co1 C10 H10 125.1 . . ? C7 C11 C10 108.4(11) . . ? C7 C11 Co1 69.4(8) . . ? C10 C11 Co1 68.4(8) . . ? C7 C11 H11 125.8 . . ? C10 C11 H11 125.8 . . ? Co1 C11 H11 128.0 . . ? O3 C12 O4 126.6(16) . . ? O3 C12 C7 116.6(14) . . ? O4 C12 C7 116.8(13) . . ? C14 C13 C17 105.6(14) . . ? C14 C13 C18 130.6(13) . . ? C17 C13 C18 123.7(15) . . ? C14 C13 Co2 71.0(8) . . ? C17 C13 Co2 69.4(7) . . ? C18 C13 Co2 121.3(11) . . ? C13 C14 C15 108.6(13) . . ? C13 C14 Co2 69.1(7) . . ? C15 C14 Co2 69.3(8) . . ? C13 C14 H14 125.7 . . ? C15 C14 H14 125.7 . . ? Co2 C14 H14 127.5 . . ? C16 C15 C14 108.0(12) . . ? C16 C15 Co2 68.6(9) . . ? C14 C15 Co2 70.9(7) . . ? C16 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Co2 C15 H15 126.1 . . ? C17 C16 C15 111.3(13) . . ? C17 C16 Co2 72.6(8) . . ? C15 C16 Co2 72.0(9) . . ? C17 C16 H16 124.4 . . ? C15 C16 H16 124.4 . . ? Co2 C16 H16 122.6 . . ? C16 C17 C13 106.3(13) . . ? C16 C17 Co2 68.4(9) . . ? C13 C17 Co2 68.3(7) . . ? C16 C17 H17 126.8 . . ? C13 C17 H17 126.8 . . ? Co2 C17 H17 128.0 . . ? O5 C18 O6 126.8(16) . . ? O5 C18 C13 121.9(14) . . ? O6 C18 C13 111.2(13) . . ? C23 C19 C20 107.2(11) . . ? C23 C19 C24 127.2(11) . . ? C20 C19 C24 125.4(10) . . ? C23 C19 Co2 68.4(8) . . ? C20 C19 Co2 69.0(6) . . ? C24 C19 Co2 123.9(8) . . ? C21 C20 C19 107.7(10) . . ? C21 C20 Co2 67.5(7) . . ? C19 C20 Co2 69.4(6) . . ? C21 C20 H20 126.2 . . ? C19 C20 H20 126.2 . . ? Co2 C20 H20 128.5 . . ? C20 C21 C22 109.6(11) . . ? C20 C21 Co2 71.4(7) . . ? C22 C21 Co2 69.4(8) . . ? C20 C21 H21 125.2 . . ? C22 C21 H21 125.2 . . ? Co2 C21 H21 125.6 . . ? C21 C22 C23 106.4(12) . . ? C21 C22 Co2 69.0(8) . . ? C23 C22 Co2 69.4(8) . . ? C21 C22 H22 126.8 . . ? C23 C22 H22 126.8 . . ? Co2 C22 H22 126.4 . . ? C19 C23 C22 109.2(12) . . ? C19 C23 Co2 70.9(8) . . ? C22 C23 Co2 68.1(8) . . ? C19 C23 H23 125.4 . . ? C22 C23 H23 125.4 . . ? Co2 C23 H23 127.1 . . ? O7 C24 O8 124.5(12) . . ? O7 C24 C19 116.9(11) . . ? O8 C24 C19 118.4(10) . . ? O9 C25 H25A 109.5 . . ? O9 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O9 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C1 Co1 C9 115.0(6) . . ? C1 Co1 C2 42.9(7) . . ? C9 Co1 C2 147.2(7) . . ? C1 Co1 C4 69.1(7) . . ? C9 Co1 C4 129.5(9) . . ? C2 Co1 C4 72.0(9) . . ? C1 Co1 C5 40.8(7) . . ? C9 Co1 C5 107.5(8) . . ? C2 Co1 C5 71.6(8) . . ? C4 Co1 C5 40.6(7) . . ? C1 Co1 C7 173.3(6) . . ? C9 Co1 C7 69.1(6) . . ? C2 Co1 C7 130.8(7) . . ? C4 Co1 C7 112.9(7) . . ? C5 Co1 C7 144.5(6) . . ? C1 Co1 C10 108.7(6) . . ? C9 Co1 C10 36.4(6) . . ? C2 Co1 C10 117.6(7) . . ? C4 Co1 C10 164.5(9) . . ? C5 Co1 C10 127.9(6) . . ? C7 Co1 C10 71.2(6) . . ? C1 Co1 C11 134.6(6) . . ? C9 Co1 C11 66.0(6) . . ? C2 Co1 C11 110.1(6) . . ? C4 Co1 C11 148.5(7) . . ? C5 Co1 C11 170.8(6) . . ? C7 Co1 C11 41.0(5) . . ? C10 Co1 C11 43.1(6) . . ? C1 Co1 C8 144.4(7) . . ? C9 Co1 C8 41.5(6) . . ? C2 Co1 C8 170.6(7) . . ? C4 Co1 C8 104.1(8) . . ? C5 Co1 C8 111.2(7) . . ? C7 Co1 C8 42.2(6) . . ? C10 Co1 C8 68.3(6) . . ? C11 Co1 C8 68.7(5) . . ? C1 Co1 C3 69.3(7) . . ? C9 Co1 C3 171.1(11) . . ? C2 Co1 C3 41.1(9) . . ? C4 Co1 C3 43.4(10) . . ? C5 Co1 C3 70.3(10) . . ? C7 Co1 C3 107.4(7) . . ? C10 Co1 C3 151.5(12) . . ? C11 Co1 C3 117.2(10) . . ? C8 Co1 C3 130.5(9) . . ? C21 Co2 C22 41.6(6) . . ? C21 Co2 C16 174.9(5) . . ? C22 Co2 C16 143.3(6) . . ? C21 Co2 C23 70.0(5) . . ? C22 Co2 C23 42.5(6) . . ? C16 Co2 C23 114.5(6) . . ? C21 Co2 C20 41.1(5) . . ? C22 Co2 C20 70.0(6) . . ? C16 Co2 C20 137.2(5) . . ? C23 Co2 C20 69.2(5) . . ? C21 Co2 C13 110.0(6) . . ? C22 Co2 C13 109.2(7) . . ? C16 Co2 C13 68.3(6) . . ? C23 Co2 C13 139.0(6) . . ? C20 Co2 C13 138.6(5) . . ? C21 Co2 C19 70.0(5) . . ? C22 Co2 C19 70.5(5) . . ? C16 Co2 C19 111.8(6) . . ? C23 Co2 C19 40.6(5) . . ? C20 Co2 C19 41.6(5) . . ? C13 Co2 C19 179.6(6) . . ? C21 Co2 C15 135.6(5) . . ? C22 Co2 C15 175.5(6) . . ? C16 Co2 C15 39.4(5) . . ? C23 Co2 C15 141.9(6) . . ? C20 Co2 C15 110.0(5) . . ? C13 Co2 C15 67.6(6) . . ? C19 Co2 C15 112.6(5) . . ? C21 Co2 C17 142.5(6) . . ? C22 Co2 C17 113.7(6) . . ? C16 Co2 C17 39.0(6) . . ? C23 Co2 C17 112.5(5) . . ? C20 Co2 C17 176.2(6) . . ? C13 Co2 C17 42.3(6) . . ? C19 Co2 C17 137.5(6) . . ? C15 Co2 C17 66.5(6) . . ? C21 Co2 C14 108.8(6) . . ? C22 Co2 C14 135.8(6) . . ? C16 Co2 C14 66.7(6) . . ? C23 Co2 C14 178.2(7) . . ? C20 Co2 C14 110.9(6) . . ? C13 Co2 C14 39.9(6) . . ? C19 Co2 C14 140.5(5) . . ? C15 Co2 C14 39.8(6) . . ? C17 Co2 C14 67.6(6) . . ? O1 Cu1 O6 91.0(5) . 1_655 ? O1 Cu1 O7 91.9(5) . . ? O6 Cu1 O7 177.0(5) 1_655 . ? O1 Cu1 O4 178.1(4) . 1_545 ? O6 Cu1 O4 88.7(4) 1_655 1_545 ? O7 Cu1 O4 88.3(5) . 1_545 ? C6 O1 Cu1 119.8(11) . . ? C12 O4 Cu1 110.6(10) . 1_565 ? C18 O6 Cu1 113.9(10) . 1_455 ? C24 O7 Cu1 117.6(9) . . ? C25 O9 H9A 109.5 . . ? _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.779 _refine_diff_density_min -0.626 _refine_diff_density_rms 0.160 # start Validation Reply Form _vrf_PLAT241_ip2-953a ; PROBLEM: Check High Ueq as Compared to Neighbors for C3 RESPONSE: ... ; _vrf_PLAT415_ip2-953a ; PROBLEM: Short Inter D-H..H-X H2 .. H9A .. 1.84 Ang. ; _vrf_PLAT213_ip2-953a ; PROBLEM: Atom C3 has ADP max/min Ratio ..... 4.3 prola ; _vrf_PLAT341_ip2-953a ; PROBLEM: Low Bond Precision on C-C Bonds ............... 0.0210 Ang. ; _vrf_PLAT369_ip2-953a ; PROBLEM: Long C(sp2)-C(sp2) Bond C1 - C6 ... 1.58 Ang. RESPONSE: These problems are due to limited crystal quality. The reason is that this crystal with low solvent content (compound 3b) was obtained by heating a crystal with higher methanol content (compound 3a). ; _vrf_PLAT420_ip2-953a ; PROBLEM: D-H Without Acceptor *O9 - *H9A ... ? Check RESPONSE: H9a belongs to a solvent methanol molecule. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 950061' ####################################################################### # # 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_ip1-1082 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Co N2 O4 Zn, F6 P' _chemical_formula_sum 'C22 H16 Co F6 N2 O4 P Zn' _chemical_formula_weight 641.64 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' Co Co 0.3494 0.9721 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8096(12) _cell_length_b 12.270(3) _cell_length_c 14.134(3) _cell_angle_alpha 84.323(16) _cell_angle_beta 78.295(15) _cell_angle_gamma 79.696(16) _cell_volume 1135.3(4) _cell_formula_units_Z 2 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 7454 _cell_measurement_theta_min 2.3 _cell_measurement_theta_max 26.6 _exptl_crystal_description tip _exptl_crystal_colour yellow _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.877 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 640 _exptl_absorpt_coefficient_mu 1.941 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.691 _exptl_absorpt_correction_T_max 0.793 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'STOE IPDS-1' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8936 _diffrn_reflns_av_R_equivalents 0.0375 _diffrn_reflns_av_sigmaI/netI 0.0681 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 25.99 _reflns_number_total 4181 _reflns_number_gt 2714 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution ? _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^)+(0.0583P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4181 _refine_ls_number_parameters 331 _refine_ls_number_restraints 8 _refine_ls_R_factor_all 0.0724 _refine_ls_R_factor_gt 0.0440 _refine_ls_wR_factor_ref 0.1055 _refine_ls_wR_factor_gt 0.0990 _refine_ls_goodness_of_fit_ref 0.873 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5796(7) 0.1825(4) 0.8367(3) 0.0491(12) Uani 1 1 d . A . C2 C 0.6723(6) 0.0910(4) 0.8998(3) 0.0444(11) Uani 1 1 d . . . C3 C 0.7274(7) -0.0250(4) 0.8828(3) 0.0525(13) Uani 1 1 d . . . H3 H 0.7224 -0.0580 0.8262 0.063 Uiso 1 1 calc R . . C4 C 0.7912(7) -0.0810(4) 0.9676(4) 0.0541(13) Uani 1 1 d . . . H4 H 0.8365 -0.1576 0.9765 0.065 Uiso 1 1 calc R . . C5 C 0.7747(7) -0.0019(5) 1.0356(4) 0.0574(14) Uani 1 1 d . . . H5 H 0.8060 -0.0166 1.0979 0.069 Uiso 1 1 calc R . . C6 C 0.7031(7) 0.1029(4) 0.9943(3) 0.0525(13) Uani 1 1 d . . . H6 H 0.6795 0.1702 1.0245 0.063 Uiso 1 1 calc R . . C7 C 0.0587(7) 0.3425(4) 0.8326(3) 0.0474(11) Uani 1 1 d . A . C8 C -0.0858(7) 0.4258(4) 0.8954(3) 0.0450(11) Uani 1 1 d . . . C9 C -0.1986(7) 0.3994(4) 0.9886(3) 0.0522(13) Uani 1 1 d . . . H9 H -0.2034 0.3274 1.0178 0.063 Uiso 1 1 calc R . . C10 C -0.3026(7) 0.4993(5) 1.0302(4) 0.0597(15) Uani 1 1 d . . . H10 H -0.3861 0.5053 1.0918 0.072 Uiso 1 1 calc R . . C11 C -0.2585(8) 0.5875(5) 0.9629(4) 0.0618(14) Uani 1 1 d . . . H11 H -0.3095 0.6630 0.9714 0.074 Uiso 1 1 calc R . . C12 C -0.1233(8) 0.5440(4) 0.8792(4) 0.0557(13) Uani 1 1 d . . . H12 H -0.0688 0.5854 0.8236 0.067 Uiso 1 1 calc R . . C13 C 0.3347(15) 0.1285(8) 0.5284(6) 0.045(2) Uiso 0.566(12) 1 d PD A 1 H13 H 0.4661 0.1429 0.5011 0.054 Uiso 0.566(12) 1 calc PR A 1 C14 C 0.2471(14) 0.0610(8) 0.4805(6) 0.041(2) Uiso 0.566(12) 1 d PD A 1 H14 H 0.3158 0.0324 0.4213 0.050 Uiso 0.566(12) 1 calc PR A 1 C16 C -0.0411(16) 0.0802(10) 0.6106(7) 0.052(3) Uiso 0.566(12) 1 d PD A 1 H16 H -0.1692 0.0642 0.6421 0.063 Uiso 0.566(12) 1 calc PR A 1 C17 C 0.0570(16) 0.1484(10) 0.6519(7) 0.054(3) Uiso 0.566(12) 1 d PD A 1 H17 H -0.0103 0.1776 0.7111 0.065 Uiso 0.566(12) 1 calc PR A 1 C13A C 0.251(2) 0.1794(12) 0.5223(8) 0.056(3) Uiso 0.434(12) 1 d PD A 2 H13A H 0.3259 0.2313 0.4849 0.068 Uiso 0.434(12) 1 calc PR A 2 C14A C 0.163(2) 0.1115(12) 0.4728(9) 0.058(3) Uiso 0.434(12) 1 d PD A 2 H14A H 0.1827 0.1179 0.4049 0.070 Uiso 0.434(12) 1 calc PR A 2 C16A C 0.0102(18) 0.0415(11) 0.6255(7) 0.039(3) Uiso 0.434(12) 1 d PD A 2 H16A H -0.0817 -0.0009 0.6644 0.047 Uiso 0.434(12) 1 calc PR A 2 C17A C 0.107(2) 0.1084(12) 0.6677(9) 0.049(3) Uiso 0.434(12) 1 d PD A 2 H17A H 0.0826 0.1083 0.7356 0.059 Uiso 0.434(12) 1 calc PR A 2 C15 C 0.0499(8) 0.0368(4) 0.5242(3) 0.0507(12) Uani 1 1 d . . . C18 C 0.7154(15) 0.3201(9) 0.5305(7) 0.050(3) Uiso 0.531(13) 1 d PD A 1 H18 H 0.6963 0.2554 0.5054 0.060 Uiso 0.531(13) 1 calc PR A 1 C19 C 0.8781(15) 0.3733(8) 0.4848(6) 0.046(2) Uiso 0.531(13) 1 d PD A 1 H19 H 0.9656 0.3449 0.4292 0.056 Uiso 0.531(13) 1 calc PR A 1 C21 C 0.7859(18) 0.4990(9) 0.6104(7) 0.046(3) Uiso 0.531(13) 1 d PD A 1 H21 H 0.8097 0.5569 0.6432 0.056 Uiso 0.531(13) 1 calc PR A 1 C22 C 0.6251(18) 0.4425(9) 0.6509(8) 0.048(3) Uiso 0.531(13) 1 d PD A 1 H22 H 0.5422 0.4646 0.7097 0.058 Uiso 0.531(13) 1 calc PR A 1 C18A C 0.6439(16) 0.3716(9) 0.5136(7) 0.041(3) Uiso 0.469(13) 1 d PD A 2 H18A H 0.5751 0.3395 0.4750 0.050 Uiso 0.469(13) 1 calc PR A 2 C19A C 0.8005(15) 0.4287(9) 0.4662(7) 0.042(3) Uiso 0.469(13) 1 d PD A 2 H19A H 0.8303 0.4380 0.3982 0.051 Uiso 0.469(13) 1 calc PR A 2 C21A C 0.8437(19) 0.4723(10) 0.6205(8) 0.044(3) Uiso 0.469(13) 1 d PD A 2 H21A H 0.9005 0.5118 0.6589 0.052 Uiso 0.469(13) 1 calc PR A 2 C22A C 0.688(2) 0.4128(11) 0.6618(8) 0.050(3) Uiso 0.469(13) 1 d PD A 2 H22A H 0.6493 0.4086 0.7296 0.060 Uiso 0.469(13) 1 calc PR A 2 C20 C 0.9114(7) 0.4715(4) 0.5229(3) 0.0500(12) Uani 1 1 d . . . Co1 Co 0.5000 0.0000 1.0000 0.0397(2) Uani 1 2 d S . . Co2 Co 0.0000 0.5000 1.0000 0.0411(2) Uani 1 2 d S . . F1 F 0.7072(10) 0.3485(4) 0.2579(4) 0.150(2) Uani 1 1 d . . . F2 F 0.8400(7) 0.1944(5) 0.1825(3) 0.1282(17) Uani 1 1 d . . . F3 F 0.5753(10) 0.1170(4) 0.2629(4) 0.143(2) Uani 1 1 d . . . F4 F 0.4472(8) 0.2747(4) 0.3351(3) 0.1331(19) Uani 1 1 d . . . F5 F 0.7557(10) 0.1889(4) 0.3471(3) 0.145(2) Uani 1 1 d . . . F6 F 0.5284(8) 0.2726(5) 0.1736(3) 0.1336(18) Uani 1 1 d . . . N1 N 0.2367(6) 0.1752(3) 0.6143(3) 0.0527(10) Uani 1 1 d . . . N2 N 0.5850(6) 0.3593(3) 0.6097(3) 0.0488(10) Uani 1 1 d . . . O1 O 0.5400(5) 0.1510(3) 0.7570(2) 0.0561(9) Uani 1 1 d . . . O2 O 0.5419(5) 0.2791(3) 0.8611(3) 0.0594(9) Uani 1 1 d . . . O3 O 0.1609(5) 0.3827(3) 0.7536(2) 0.0563(9) Uani 1 1 d . . . O4 O 0.0714(5) 0.2428(3) 0.8578(2) 0.0585(9) Uani 1 1 d . . . P1 P 0.6468(3) 0.23114(13) 0.25992(10) 0.0717(5) Uani 1 1 d . . . Zn1 Zn 0.37202(9) 0.26792(5) 0.69083(4) 0.04872(18) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(3) 0.058(3) 0.048(3) -0.001(2) 0.003(2) -0.020(2) C2 0.035(2) 0.050(3) 0.048(2) 0.001(2) 0.000(2) -0.018(2) C3 0.044(3) 0.060(3) 0.048(3) -0.008(2) 0.009(2) -0.012(2) C4 0.039(3) 0.054(3) 0.064(3) 0.008(2) -0.002(2) -0.009(2) C5 0.044(3) 0.077(4) 0.059(3) 0.014(3) -0.017(2) -0.031(3) C6 0.052(3) 0.060(3) 0.056(3) 0.006(2) -0.017(2) -0.033(3) C7 0.045(3) 0.055(3) 0.048(3) -0.012(2) -0.014(2) -0.012(2) C8 0.040(2) 0.054(3) 0.048(2) -0.013(2) -0.014(2) -0.013(2) C9 0.046(3) 0.061(3) 0.057(3) -0.016(2) -0.005(2) -0.029(2) C10 0.041(3) 0.086(4) 0.060(3) -0.024(3) -0.007(2) -0.022(3) C11 0.051(3) 0.059(3) 0.080(4) -0.024(3) -0.025(3) 0.002(3) C12 0.061(3) 0.062(3) 0.051(3) -0.007(2) -0.021(2) -0.014(3) C15 0.056(3) 0.060(3) 0.039(2) -0.002(2) -0.006(2) -0.022(2) C20 0.052(3) 0.060(3) 0.040(2) -0.007(2) -0.003(2) -0.018(2) Co1 0.0377(5) 0.0430(5) 0.0408(4) -0.0027(4) -0.0028(4) -0.0182(4) Co2 0.0406(5) 0.0443(5) 0.0430(4) -0.0100(4) -0.0069(4) -0.0163(4) F1 0.210(6) 0.106(3) 0.137(4) -0.028(3) 0.018(4) -0.080(4) F2 0.103(3) 0.188(5) 0.084(3) -0.050(3) 0.004(2) 0.000(3) F3 0.209(6) 0.104(3) 0.137(4) -0.021(3) -0.029(4) -0.074(4) F4 0.156(4) 0.132(4) 0.084(3) -0.005(3) 0.032(3) -0.015(3) F5 0.226(6) 0.132(4) 0.086(3) -0.028(3) -0.074(4) 0.010(4) F6 0.136(4) 0.178(5) 0.076(3) 0.003(3) -0.029(3) 0.008(4) N1 0.061(3) 0.059(2) 0.042(2) -0.0058(18) -0.0043(19) -0.022(2) N2 0.053(2) 0.058(2) 0.0380(19) -0.0035(17) -0.0025(17) -0.023(2) O1 0.056(2) 0.062(2) 0.0509(19) -0.0071(16) -0.0044(16) -0.0148(17) O2 0.065(2) 0.050(2) 0.065(2) -0.0015(17) -0.0104(18) -0.0151(18) O3 0.057(2) 0.067(2) 0.0467(18) -0.0058(16) -0.0041(16) -0.0184(18) O4 0.069(2) 0.052(2) 0.056(2) -0.0139(16) -0.0067(18) -0.0138(18) P1 0.1015(13) 0.0720(10) 0.0429(7) -0.0084(7) -0.0021(8) -0.0282(9) Zn1 0.0529(3) 0.0549(3) 0.0419(3) -0.0051(2) -0.0048(2) -0.0216(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.235(6) . ? C1 O1 1.319(6) . ? C1 C2 1.493(7) . ? C2 C6 1.419(7) . ? C2 C3 1.436(7) . ? C2 Co1 2.027(4) . ? C3 C4 1.429(7) . ? C3 Co1 2.031(4) . ? C3 H3 0.9400 . ? C4 C5 1.406(7) . ? C4 Co1 2.036(5) . ? C4 H4 0.9400 . ? C5 C6 1.405(7) . ? C5 Co1 2.029(5) . ? C5 H5 0.9400 . ? C6 Co1 2.018(4) . ? C6 H6 0.9400 . ? C7 O4 1.233(6) . ? C7 O3 1.293(5) . ? C7 C8 1.505(6) . ? C8 C9 1.422(6) . ? C8 C12 1.430(7) . ? C8 Co2 2.040(4) . ? C9 C10 1.419(7) . ? C9 Co2 2.026(4) . ? C9 H9 0.9400 . ? C10 C11 1.401(8) . ? C10 Co2 2.019(5) . ? C10 H10 0.9400 . ? C11 C12 1.428(7) . ? C11 Co2 2.028(6) . ? C11 H11 0.9400 . ? C12 Co2 2.036(5) . ? C12 H12 0.9400 . ? C13 N1 1.386(9) . ? C13 C14 1.396(10) . ? C13 H13 0.9400 . ? C14 C15 1.429(9) . ? C14 H14 0.9400 . ? C16 C15 1.364(10) . ? C16 C17 1.394(10) . ? C16 H16 0.9400 . ? C17 N1 1.316(9) . ? C17 H17 0.9400 . ? C13A N1 1.280(12) . ? C13A C14A 1.417(13) . ? C13A H13A 0.9400 . ? C14A C15 1.362(12) . ? C14A H14A 0.9400 . ? C16A C17A 1.383(12) . ? C16A C15 1.406(11) . ? C16A H16A 0.9400 . ? C17A N1 1.374(11) . ? C17A H17A 0.9400 . ? C15 C15 1.510(9) 2_556 ? C18 N2 1.351(9) . ? C18 C19 1.398(10) . ? C18 H18 0.9400 . ? C19 C20 1.440(10) . ? C19 H19 0.9400 . ? C21 C20 1.387(10) . ? C21 C22 1.395(10) . ? C21 H21 0.9400 . ? C22 N2 1.318(10) . ? C22 H22 0.9400 . ? C18A N2 1.338(10) . ? C18A C19A 1.400(10) . ? C18A H18A 0.9400 . ? C19A C20 1.401(10) . ? C19A H19A 0.9400 . ? C21A C20 1.363(11) . ? C21A C22A 1.394(11) . ? C21A H21A 0.9400 . ? C22A N2 1.389(12) . ? C22A H22A 0.9400 . ? C20 C20 1.503(8) 2_766 ? Co1 C6 2.018(4) 2_657 ? Co1 C2 2.027(4) 2_657 ? Co1 C5 2.029(5) 2_657 ? Co1 C3 2.031(4) 2_657 ? Co1 C4 2.036(5) 2_657 ? Co2 C10 2.019(5) 2_567 ? Co2 C9 2.026(4) 2_567 ? Co2 C11 2.028(6) 2_567 ? Co2 C12 2.036(5) 2_567 ? Co2 C8 2.040(4) 2_567 ? F1 P1 1.563(4) . ? F2 P1 1.560(4) . ? F3 P1 1.557(4) . ? F4 P1 1.590(5) . ? F5 P1 1.563(5) . ? F6 P1 1.590(5) . ? N1 Zn1 2.083(4) . ? N2 Zn1 2.080(3) . ? O1 Zn1 1.955(4) . ? O3 Zn1 1.961(4) . ? 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 C1 O1 124.4(5) . . ? O2 C1 C2 120.5(4) . . ? O1 C1 C2 115.0(4) . . ? C6 C2 C3 107.0(4) . . ? C6 C2 C1 124.7(4) . . ? C3 C2 C1 128.0(4) . . ? C6 C2 Co1 69.1(2) . . ? C3 C2 Co1 69.4(2) . . ? C1 C2 Co1 121.9(3) . . ? C4 C3 C2 107.4(4) . . ? C4 C3 Co1 69.6(3) . . ? C2 C3 Co1 69.1(2) . . ? C4 C3 H3 126.3 . . ? C2 C3 H3 126.3 . . ? Co1 C3 H3 126.5 . . ? C5 C4 C3 108.4(5) . . ? C5 C4 Co1 69.5(3) . . ? C3 C4 Co1 69.3(3) . . ? C5 C4 H4 125.8 . . ? C3 C4 H4 125.8 . . ? Co1 C4 H4 127.0 . . ? C6 C5 C4 108.2(5) . . ? C6 C5 Co1 69.3(3) . . ? C4 C5 Co1 70.0(3) . . ? C6 C5 H5 125.9 . . ? C4 C5 H5 125.9 . . ? Co1 C5 H5 126.3 . . ? C5 C6 C2 109.1(5) . . ? C5 C6 Co1 70.1(2) . . ? C2 C6 Co1 69.8(2) . . ? C5 C6 H6 125.4 . . ? C2 C6 H6 125.4 . . ? Co1 C6 H6 126.3 . . ? O4 C7 O3 124.5(4) . . ? O4 C7 C8 119.6(4) . . ? O3 C7 C8 116.0(4) . . ? C9 C8 C12 107.0(4) . . ? C9 C8 C7 124.5(5) . . ? C12 C8 C7 128.2(4) . . ? C9 C8 Co2 69.0(2) . . ? C12 C8 Co2 69.3(3) . . ? C7 C8 Co2 122.6(3) . . ? C10 C9 C8 108.9(5) . . ? C10 C9 Co2 69.2(2) . . ? C8 C9 Co2 70.1(2) . . ? C10 C9 H9 125.6 . . ? C8 C9 H9 125.6 . . ? Co2 C9 H9 126.8 . . ? C11 C10 C9 107.6(4) . . ? C11 C10 Co2 70.1(3) . . ? C9 C10 Co2 69.7(3) . . ? C11 C10 H10 126.2 . . ? C9 C10 H10 126.2 . . ? Co2 C10 H10 125.6 . . ? C10 C11 C12 108.9(5) . . ? C10 C11 Co2 69.4(3) . . ? C12 C11 Co2 69.8(3) . . ? C10 C11 H11 125.6 . . ? C12 C11 H11 125.6 . . ? Co2 C11 H11 126.9 . . ? C11 C12 C8 107.5(4) . . ? C11 C12 Co2 69.1(3) . . ? C8 C12 Co2 69.6(3) . . ? C11 C12 H12 126.2 . . ? C8 C12 H12 126.2 . . ? Co2 C12 H12 126.6 . . ? N1 C13 C14 123.0(7) . . ? N1 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C13 C14 C15 118.0(7) . . ? C13 C14 H14 121.0 . . ? C15 C14 H14 121.0 . . ? C15 C16 C17 119.6(8) . . ? C15 C16 H16 120.2 . . ? C17 C16 H16 120.2 . . ? N1 C17 C16 125.0(8) . . ? N1 C17 H17 117.5 . . ? C16 C17 H17 117.5 . . ? N1 C13A C14A 124.7(10) . . ? N1 C13A H13A 117.6 . . ? C14A C13A H13A 117.6 . . ? C15 C14A C13A 119.7(10) . . ? C15 C14A H14A 120.2 . . ? C13A C14A H14A 120.2 . . ? C17A C16A C15 119.8(9) . . ? C17A C16A H16A 120.1 . . ? C15 C16A H16A 120.1 . . ? N1 C17A C16A 122.6(10) . . ? N1 C17A H17A 118.7 . . ? C16A C17A H17A 118.7 . . ? C14A C15 C16A 116.1(7) . . ? C16 C15 C14 118.1(6) . . ? N2 C18 C19 121.7(8) . . ? N2 C18 H18 119.2 . . ? C19 C18 H18 119.2 . . ? C18 C19 C20 119.9(7) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C20 C21 C22 121.5(8) . . ? C20 C21 H21 119.3 . . ? C22 C21 H21 119.3 . . ? N2 C22 C21 122.5(8) . . ? N2 C22 H22 118.8 . . ? C21 C22 H22 118.8 . . ? N2 C18A C19A 124.8(8) . . ? N2 C18A H18A 117.6 . . ? C19A C18A H18A 117.6 . . ? C18A C19A C20 118.1(8) . . ? C18A C19A H19A 121.0 . . ? C20 C19A H19A 121.0 . . ? C20 C21A C22A 118.1(9) . . ? C20 C21A H21A 121.0 . . ? C22A C21A H21A 121.0 . . ? N2 C22A C21A 124.6(9) . . ? N2 C22A H22A 117.7 . . ? C21A C22A H22A 117.7 . . ? C21A C20 C19A 119.2(6) . . ? C21 C20 C19 114.8(6) . . ? C6 Co1 C6 180.0(2) . 2_657 ? C6 Co1 C2 138.94(18) . 2_657 ? C6 Co1 C2 41.06(18) 2_657 2_657 ? C6 Co1 C2 41.06(18) . . ? C6 Co1 C2 138.94(18) 2_657 . ? C2 Co1 C2 180.000(1) 2_657 . ? C6 Co1 C5 139.4(2) . 2_657 ? C6 Co1 C5 40.6(2) 2_657 2_657 ? C2 Co1 C5 69.12(19) 2_657 2_657 ? C2 Co1 C5 110.88(19) . 2_657 ? C6 Co1 C5 40.6(2) . . ? C6 Co1 C5 139.4(2) 2_657 . ? C2 Co1 C5 110.88(19) 2_657 . ? C2 Co1 C5 69.12(19) . . ? C5 Co1 C5 180.000(1) 2_657 . ? C6 Co1 C3 111.0(2) . 2_657 ? C6 Co1 C3 69.0(2) 2_657 2_657 ? C2 Co1 C3 41.46(18) 2_657 2_657 ? C2 Co1 C3 138.54(18) . 2_657 ? C5 Co1 C3 69.0(2) 2_657 2_657 ? C5 Co1 C3 111.0(2) . 2_657 ? C6 Co1 C3 69.0(2) . . ? C6 Co1 C3 111.0(2) 2_657 . ? C2 Co1 C3 138.54(18) 2_657 . ? C2 Co1 C3 41.46(18) . . ? C5 Co1 C3 111.0(2) 2_657 . ? C5 Co1 C3 69.0(2) . . ? C3 Co1 C3 180.000(1) 2_657 . ? C6 Co1 C4 68.3(2) . . ? C6 Co1 C4 111.7(2) 2_657 . ? C2 Co1 C4 110.76(19) 2_657 . ? C2 Co1 C4 69.24(19) . . ? C5 Co1 C4 139.5(2) 2_657 . ? C5 Co1 C4 40.5(2) . . ? C3 Co1 C4 138.9(2) 2_657 . ? C3 Co1 C4 41.1(2) . . ? C6 Co1 C4 111.7(2) . 2_657 ? C6 Co1 C4 68.3(2) 2_657 2_657 ? C2 Co1 C4 69.24(19) 2_657 2_657 ? C2 Co1 C4 110.76(19) . 2_657 ? C5 Co1 C4 40.5(2) 2_657 2_657 ? C5 Co1 C4 139.5(2) . 2_657 ? C3 Co1 C4 41.1(2) 2_657 2_657 ? C3 Co1 C4 138.9(2) . 2_657 ? C4 Co1 C4 180.000(1) . 2_657 ? C10 Co2 C10 180.00(6) 2_567 . ? C10 Co2 C9 41.1(2) 2_567 2_567 ? C10 Co2 C9 138.9(2) . 2_567 ? C10 Co2 C9 138.9(2) 2_567 . ? C10 Co2 C9 41.1(2) . . ? C9 Co2 C9 180.000(1) 2_567 . ? C10 Co2 C11 139.5(2) 2_567 . ? C10 Co2 C11 40.5(2) . . ? C9 Co2 C11 111.7(2) 2_567 . ? C9 Co2 C11 68.3(2) . . ? C10 Co2 C11 40.5(2) 2_567 2_567 ? C10 Co2 C11 139.5(2) . 2_567 ? C9 Co2 C11 68.3(2) 2_567 2_567 ? C9 Co2 C11 111.7(2) . 2_567 ? C11 Co2 C11 180.000(1) . 2_567 ? C10 Co2 C12 110.9(2) 2_567 . ? C10 Co2 C12 69.1(2) . . ? C9 Co2 C12 111.3(2) 2_567 . ? C9 Co2 C12 68.7(2) . . ? C11 Co2 C12 41.1(2) . . ? C11 Co2 C12 138.9(2) 2_567 . ? C10 Co2 C12 69.1(2) 2_567 2_567 ? C10 Co2 C12 110.9(2) . 2_567 ? C9 Co2 C12 68.7(2) 2_567 2_567 ? C9 Co2 C12 111.3(2) . 2_567 ? C11 Co2 C12 138.9(2) . 2_567 ? C11 Co2 C12 41.1(2) 2_567 2_567 ? C12 Co2 C12 180.000(1) . 2_567 ? C10 Co2 C8 69.43(18) 2_567 2_567 ? C10 Co2 C8 110.57(18) . 2_567 ? C9 Co2 C8 40.95(18) 2_567 2_567 ? C9 Co2 C8 139.05(18) . 2_567 ? C11 Co2 C8 111.0(2) . 2_567 ? C11 Co2 C8 69.0(2) 2_567 2_567 ? C12 Co2 C8 138.9(2) . 2_567 ? C12 Co2 C8 41.1(2) 2_567 2_567 ? C10 Co2 C8 110.57(18) 2_567 . ? C10 Co2 C8 69.43(18) . . ? C9 Co2 C8 139.05(18) 2_567 . ? C9 Co2 C8 40.95(18) . . ? C11 Co2 C8 69.0(2) . . ? C11 Co2 C8 111.0(2) 2_567 . ? C12 Co2 C8 41.1(2) . . ? C12 Co2 C8 138.9(2) 2_567 . ? C8 Co2 C8 180.000(1) 2_567 . ? C13A N1 C17A 116.2(7) . . ? C17 N1 C13 116.2(6) . . ? C17A N1 C13 110.6(6) . . ? C13A N1 Zn1 126.6(5) . . ? C17 N1 Zn1 120.1(5) . . ? C17A N1 Zn1 117.1(5) . . ? C13 N1 Zn1 123.4(4) . . ? C22 N2 C18 118.9(6) . . ? C18A N2 C22A 114.3(6) . . ? C22 N2 Zn1 117.1(4) . . ? C18A N2 Zn1 129.4(4) . . ? C18 N2 Zn1 121.8(4) . . ? C22A N2 Zn1 116.3(5) . . ? C1 O1 Zn1 113.0(3) . . ? C7 O3 Zn1 111.0(3) . . ? F3 P1 F2 91.8(3) . . ? F3 P1 F1 177.1(4) . . ? F2 P1 F1 90.6(3) . . ? F3 P1 F5 90.3(3) . . ? F2 P1 F5 93.7(3) . . ? F1 P1 F5 91.2(3) . . ? F3 P1 F4 90.2(3) . . ? F2 P1 F4 176.8(3) . . ? F1 P1 F4 87.3(3) . . ? F5 P1 F4 88.8(3) . . ? F3 P1 F6 88.3(3) . . ? F2 P1 F6 88.1(3) . . ? F1 P1 F6 90.2(3) . . ? F5 P1 F6 177.8(3) . . ? F4 P1 F6 89.5(3) . . ? O1 Zn1 O3 125.76(14) . . ? O1 Zn1 N2 102.63(16) . . ? O3 Zn1 N2 102.94(15) . . ? O1 Zn1 N1 101.41(16) . . ? O3 Zn1 N1 108.25(16) . . ? N2 Zn1 N1 116.71(14) . . ? _diffrn_measured_fraction_theta_max 0.935 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.935 _refine_diff_density_max 0.548 _refine_diff_density_min -0.435 _refine_diff_density_rms 0.087 # start Validation Reply Form _vrf_PLAT029_ip1-1082 ; PROBLEM: _diffrn_measured_fraction_theta_full Low ....... 0.935 RESPONSE: The low fraction of 93.5 % originates in the type of diffractometer (STOE IPDS-1). ; _vrf_PLAT201_ip1-1082 ; PROBLEM: Isotropic non-H Atoms in Main Residue(s) ....... 8 RESPONSE: The 4,4'-bipy ligands are disordered; the nitrogen atoms and the carbon atoms C4 and C4' belong to both parts. ; # end Validation Reply Form _database_code_depnum_ccdc_archive 'CCDC 950062' ####################################################################### # # 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_ip1-1067 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Co N2 O4 Zn, F6 P' _chemical_formula_sum 'C22 H16 Co F6 N2 O4 P Zn' _chemical_formula_weight 641.64 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zn Zn 0.2839 1.4301 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.6224(13) _cell_length_b 11.4498(8) _cell_length_c 23.447(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4462.6(7) _cell_formula_units_Z 8 _cell_measurement_temperature 213(2) _cell_measurement_reflns_used 10580 _cell_measurement_theta_min 2.1 _cell_measurement_theta_max 25.8 _exptl_crystal_description needle _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.910 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2560 _exptl_absorpt_coefficient_mu 1.976 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.904 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 213(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 'STOE IPDS-1' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19002 _diffrn_reflns_av_R_equivalents 0.0495 _diffrn_reflns_av_sigmaI/netI 0.0894 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 25.93 _reflns_number_total 8197 _reflns_number_gt 5532 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE IPDS software' _computing_cell_refinement 'STOE IPDS software' _computing_data_reduction 'STOE IPDS software, STOE X-RED' _computing_structure_solution ? _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^)+(0.0353P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.041(18) _refine_ls_number_reflns 8197 _refine_ls_number_parameters 657 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.0853 _refine_ls_wR_factor_gt 0.0802 _refine_ls_goodness_of_fit_ref 0.830 _refine_ls_restrained_S_all 0.830 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5811(5) 0.5976(7) 0.5875(3) 0.0355(17) Uani 1 1 d . . . C2 C 0.6523(6) 0.5989(7) 0.5473(3) 0.035(2) Uani 1 1 d . . . C3 C 0.7342(6) 0.5902(7) 0.5642(3) 0.0355(19) Uani 1 1 d . . . H3 H 0.7532 0.5796 0.6016 0.043 Uiso 1 1 calc R . . C4 C 0.7831(5) 0.6005(7) 0.5135(4) 0.036(2) Uani 1 1 d . . . H4 H 0.8395 0.5967 0.5119 0.043 Uiso 1 1 calc R . . C5 C 0.7315(6) 0.6171(7) 0.4672(4) 0.040(2) Uani 1 1 d . . . H5 H 0.7474 0.6278 0.4291 0.048 Uiso 1 1 calc R . . C6 C 0.6499(5) 0.6150(7) 0.4877(3) 0.0341(18) Uani 1 1 d . . . H6 H 0.6033 0.6230 0.4654 0.041 Uiso 1 1 calc R . . C7 C 0.7855(5) 0.8735(6) 0.6390(3) 0.0285(15) Uani 1 1 d . . . C8 C 0.7878(5) 0.8887(7) 0.5254(4) 0.039(2) Uani 1 1 d . . . H8 H 0.8438 0.8895 0.5199 0.047 Uiso 1 1 calc R . . C9 C 0.7468(5) 0.8803(6) 0.5789(3) 0.0253(17) Uani 1 1 d . . . C10 C 0.6618(6) 0.8831(7) 0.5683(3) 0.039(2) Uani 1 1 d . . . H10 H 0.6209 0.8781 0.5959 0.047 Uiso 1 1 calc R . . C11 C 0.6507(6) 0.8949(8) 0.5083(4) 0.047(2) Uani 1 1 d . . . H11 H 0.6014 0.9010 0.4889 0.056 Uiso 1 1 calc R . . C12 C 0.7294(7) 0.8955(8) 0.4834(4) 0.051(3) Uani 1 1 d . . . H12 H 0.7399 0.8998 0.4441 0.062 Uiso 1 1 calc R . . C13 C 0.4668(5) 0.6200(5) 0.7945(3) 0.0305(16) Uani 1 1 d . . . C14 C 0.5009(5) 0.6054(7) 0.8530(3) 0.0312(19) Uani 1 1 d . . . C15 C 0.4570(7) 0.6010(7) 0.9053(4) 0.045(2) Uani 1 1 d . . . H15 H 0.4009 0.6097 0.9085 0.055 Uiso 1 1 calc R . . C16 C 0.5099(7) 0.5817(8) 0.9515(4) 0.052(3) Uani 1 1 d . . . H16 H 0.4958 0.5728 0.9901 0.063 Uiso 1 1 calc R . . C17 C 0.5881(7) 0.5784(8) 0.9281(4) 0.051(3) Uani 1 1 d . . . H17 H 0.6359 0.5685 0.9489 0.061 Uiso 1 1 calc R . . C18 C 0.5832(6) 0.5923(7) 0.8689(4) 0.039(2) Uani 1 1 d . . . H18 H 0.6271 0.5928 0.8436 0.047 Uiso 1 1 calc R . . C19 C 0.6730(5) 0.8763(6) 0.8466(3) 0.0330(17) Uani 1 1 d . . . C20 C 0.4755(7) 0.8839(7) 0.9221(4) 0.044(2) Uani 1 1 d . . . H20 H 0.4193 0.8902 0.9245 0.053 Uiso 1 1 calc R . . C21 C 0.5286(6) 0.8630(7) 0.9694(4) 0.041(2) Uani 1 1 d . . . H21 H 0.5142 0.8543 1.0080 0.050 Uiso 1 1 calc R . . C22 C 0.6047(5) 0.8585(7) 0.9468(3) 0.0376(19) Uani 1 1 d . . . H22 H 0.6517 0.8443 0.9680 0.045 Uiso 1 1 calc R . . C23 C 0.6026(5) 0.8783(6) 0.8873(3) 0.0305(18) Uani 1 1 d . . . C24 C 0.5201(6) 0.8931(7) 0.8726(4) 0.0375(19) Uani 1 1 d . . . H24 H 0.4996 0.9068 0.8358 0.045 Uiso 1 1 calc R . . C25 C 0.2312(5) -0.1169(7) 0.7321(3) 0.0384(18) Uani 1 1 d . . . H25 H 0.1988 -0.1567 0.7056 0.046 Uiso 1 1 calc R . . C26 C 0.2305(5) 0.0047(7) 0.7319(3) 0.0443(19) Uani 1 1 d . . . H26 H 0.1965 0.0442 0.7063 0.053 Uiso 1 1 calc R . . C27 C 0.2777(5) 0.0670(6) 0.7677(4) 0.0275(16) Uani 1 1 d . . . C28 C 0.3247(5) 0.0016(8) 0.8055(4) 0.057(3) Uani 1 1 d . . . H28 H 0.3581 0.0398 0.8319 0.068 Uiso 1 1 calc R . . C29 C 0.3221(6) -0.1176(8) 0.8042(4) 0.060(3) Uani 1 1 d . . . H29 H 0.3548 -0.1589 0.8300 0.073 Uiso 1 1 calc R . . C30 C 0.2401(5) 0.3831(7) 0.7281(4) 0.049(2) Uani 1 1 d . . . H30 H 0.2085 0.4222 0.7009 0.059 Uiso 1 1 calc R . . C31 C 0.2408(7) 0.2630(7) 0.7293(5) 0.041(2) Uani 1 1 d . . . H31 H 0.2114 0.2234 0.7011 0.049 Uiso 1 1 calc R . . C32 C 0.2809(4) 0.1978(6) 0.7683(4) 0.0280(15) Uani 1 1 d . . . C33 C 0.3269(6) 0.2628(7) 0.8059(5) 0.041(3) Uani 1 1 d . . . H33 H 0.3591 0.2248 0.8331 0.049 Uiso 1 1 calc R . . C34 C 0.3257(5) 0.3840(7) 0.8035(3) 0.0428(19) Uani 1 1 d . . . H34 H 0.3562 0.4262 0.8303 0.051 Uiso 1 1 calc R . . C35 C 0.5202(5) -0.1401(7) 0.7024(3) 0.0437(19) Uani 1 1 d . . . H35 H 0.5531 -0.1805 0.7283 0.052 Uiso 1 1 calc R . . C36 C 0.5202(6) -0.0191(7) 0.7051(3) 0.045(2) Uani 1 1 d . . . H36 H 0.5507 0.0200 0.7330 0.054 Uiso 1 1 calc R . . C37 C 0.4743(6) 0.0441(6) 0.6657(4) 0.0373(19) Uani 1 1 d . . . C38 C 0.4342(5) -0.0209(7) 0.6256(3) 0.047(2) Uani 1 1 d . . . H38 H 0.4053 0.0171 0.5966 0.057 Uiso 1 1 calc R . . C39 C 0.4356(6) -0.1413(7) 0.6275(4) 0.049(2) Uani 1 1 d . . . H39 H 0.4056 -0.1824 0.6001 0.059 Uiso 1 1 calc R . . C40 C 0.4255(5) 0.3618(7) 0.6327(3) 0.0408(19) Uani 1 1 d . . . H40 H 0.3929 0.4032 0.6069 0.049 Uiso 1 1 calc R . . C41 C 0.4264(8) 0.2391(7) 0.6290(5) 0.048(3) Uani 1 1 d . . . H41 H 0.3966 0.2008 0.6005 0.057 Uiso 1 1 calc R . . C42 C 0.4714(4) 0.1756(6) 0.6675(4) 0.0321(16) Uani 1 1 d . . . C43 C 0.5192(7) 0.2398(7) 0.7071(5) 0.045(3) Uani 1 1 d . . . H43 H 0.5544 0.2018 0.7324 0.054 Uiso 1 1 calc R . . C44 C 0.5118(5) 0.3608(7) 0.7068(3) 0.047(2) Uani 1 1 d . . . H44 H 0.5402 0.4033 0.7345 0.056 Uiso 1 1 calc R . . Co1 Co 0.71443(8) 0.74555(9) 0.52595(5) 0.0307(3) Uani 1 1 d . . . Co2 Co 0.53707(8) 0.73448(9) 0.90932(5) 0.0307(3) Uani 1 1 d . . . F1 F 0.1748(9) 0.3392(14) 0.6056(6) 0.098(5) Uiso 0.505(7) 1 d P A 1 F2 F 0.2416(8) 0.1642(12) 0.5915(6) 0.082(4) Uiso 0.505(7) 1 d P A 1 F3 F 0.1361(7) 0.3434(10) 0.5208(5) 0.071(3) Uiso 0.505(7) 1 d P A 1 F4 F 0.1912(7) 0.1664(9) 0.5002(4) 0.054(3) Uiso 0.505(7) 1 d P A 1 F5 F 0.1070(7) 0.1987(11) 0.5711(5) 0.079(4) Uiso 0.505(7) 1 d P A 1 F6 F 0.2783(6) 0.3051(9) 0.5327(4) 0.065(3) Uiso 0.505(7) 1 d P A 1 F1A F 0.1130(8) 0.3417(12) 0.5595(5) 0.077(4) Uiso 0.495(7) 1 d P A 2 F2A F 0.1317(8) 0.1756(11) 0.5158(5) 0.079(4) Uiso 0.495(7) 1 d P A 2 F3A F 0.2028(8) 0.3303(12) 0.4948(5) 0.076(4) Uiso 0.495(7) 1 d P A 2 F4A F 0.2693(8) 0.1819(12) 0.5424(5) 0.076(4) Uiso 0.495(7) 1 d P A 2 F5A F 0.2401(7) 0.3458(10) 0.5899(4) 0.056(3) Uiso 0.495(7) 1 d P A 2 F6A F 0.1545(7) 0.1872(10) 0.6038(4) 0.055(3) Uiso 0.495(7) 1 d P A 2 F7 F 0.1069(6) 0.1872(8) 0.9272(4) 0.060(3) Uiso 0.608(8) 1 d P B 1 F8 F 0.0275(6) 0.3455(8) 0.9340(4) 0.061(3) Uiso 0.608(8) 1 d P B 1 F9 F 0.0073(7) 0.3504(9) 0.8397(4) 0.058(3) Uiso 0.608(8) 1 d P B 1 F10 F -0.0109(5) 0.1763(8) 0.8847(4) 0.058(3) Uiso 0.608(8) 1 d P B 1 F11 F 0.1328(6) 0.3576(10) 0.8721(4) 0.078(3) Uiso 0.608(8) 1 d P B 1 F12 F 0.0891(7) 0.1957(10) 0.8288(4) 0.075(3) Uiso 0.608(8) 1 d P B 1 F7A F 0.1423(11) 0.2065(16) 0.8930(8) 0.098(6) Uiso 0.392(8) 1 d P B 2 F8A F 0.0345(11) 0.1715(14) 0.8365(6) 0.074(5) Uiso 0.392(8) 1 d P B 2 F9A F 0.0218(13) 0.1880(19) 0.9356(8) 0.114(7) Uiso 0.392(8) 1 d P B 2 F10A F 0.0836(8) 0.3642(12) 0.9270(5) 0.053(3) Uiso 0.392(8) 1 d P B 2 F11A F 0.0534(11) 0.3437(14) 0.8308(6) 0.072(4) Uiso 0.392(8) 1 d P B 2 F12A F -0.0221(10) 0.3379(16) 0.8790(7) 0.081(6) Uiso 0.392(8) 1 d P B 2 N1 N 0.2756(3) -0.1794(5) 0.7681(3) 0.0323(14) Uani 1 1 d . . . N2 N 0.2830(4) 0.4436(5) 0.7646(3) 0.0240(12) Uani 1 1 d . . . N3 N 0.4771(4) -0.2030(5) 0.6659(3) 0.0348(14) Uani 1 1 d . . . N4 N 0.4667(4) 0.4210(5) 0.6693(4) 0.0329(15) Uani 1 1 d . . . O1 O 0.5967(3) 0.5995(5) 0.6404(2) 0.0421(14) Uani 1 1 d . . . O2 O 0.5124(3) 0.5985(6) 0.5671(2) 0.0495(15) Uani 1 1 d . . . O3 O 0.7380(3) 0.8623(4) 0.67977(18) 0.0349(12) Uani 1 1 d . . . O4 O 0.8595(3) 0.8830(5) 0.6398(2) 0.0452(14) Uani 1 1 d . . . O5 O 0.3942(3) 0.6432(5) 0.7903(2) 0.0433(14) Uani 1 1 d . . . O6 O 0.5155(3) 0.6099(4) 0.75376(18) 0.0321(11) Uani 1 1 d . . . O7 O 0.6558(3) 0.8767(5) 0.7944(2) 0.0395(13) Uani 1 1 d . . . O8 O 0.7424(3) 0.8753(5) 0.8656(2) 0.0456(15) Uani 1 1 d . . . P1 P 0.1888(2) 0.2570(2) 0.55310(14) 0.0477(7) Uani 1 1 d . . . P2 P 0.05773(19) 0.2684(2) 0.88422(12) 0.0421(7) Uani 1 1 d . . . Zn1 Zn 0.47760(5) 0.60881(7) 0.66953(4) 0.02843(19) Uani 1 1 d . . . Zn2 Zn 0.27497(5) 0.63190(7) 0.76449(4) 0.02873(19) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.044(5) 0.016(4) 0.047(4) 0.005(3) 0.010(3) -0.007(3) C2 0.049(5) 0.015(4) 0.041(5) -0.003(3) -0.001(4) -0.005(3) C3 0.042(5) 0.032(5) 0.032(4) 0.002(3) 0.007(4) 0.000(4) C4 0.033(5) 0.026(5) 0.048(5) -0.012(3) 0.012(4) 0.001(3) C5 0.049(5) 0.036(5) 0.037(4) -0.011(3) 0.009(4) -0.007(4) C6 0.044(4) 0.026(5) 0.032(4) -0.010(3) -0.008(3) -0.009(3) C7 0.043(4) 0.017(4) 0.026(3) -0.004(3) -0.001(3) 0.001(3) C8 0.030(4) 0.029(5) 0.059(6) 0.010(4) 0.012(4) -0.010(3) C9 0.032(4) 0.012(4) 0.033(4) 0.005(3) -0.003(3) 0.001(3) C10 0.057(5) 0.022(5) 0.038(4) -0.003(3) 0.000(4) 0.006(4) C11 0.050(5) 0.034(6) 0.056(6) 0.000(4) -0.014(4) 0.004(4) C12 0.086(7) 0.034(6) 0.034(5) 0.022(4) -0.002(5) -0.018(5) C13 0.037(4) 0.006(4) 0.048(4) -0.002(3) -0.008(3) -0.004(3) C14 0.044(5) 0.008(4) 0.041(4) -0.008(3) -0.002(3) -0.002(3) C15 0.084(7) 0.024(5) 0.028(4) -0.006(3) -0.001(4) -0.016(4) C16 0.091(8) 0.022(5) 0.043(5) 0.016(4) 0.012(5) -0.017(5) C17 0.078(7) 0.032(6) 0.043(5) 0.012(4) -0.022(5) 0.005(4) C18 0.041(5) 0.018(5) 0.058(5) -0.003(3) 0.001(4) 0.009(3) C19 0.051(5) 0.010(4) 0.038(4) 0.000(3) -0.004(3) -0.006(3) C20 0.049(6) 0.026(5) 0.057(6) -0.010(4) 0.001(5) 0.002(4) C21 0.053(5) 0.032(5) 0.038(4) -0.011(3) 0.013(4) -0.013(4) C22 0.050(5) 0.028(5) 0.035(4) -0.005(3) -0.004(4) -0.011(3) C23 0.033(4) 0.024(4) 0.034(4) 0.000(3) 0.001(3) -0.002(3) C24 0.029(4) 0.034(5) 0.049(5) -0.008(4) -0.003(4) 0.000(4) C25 0.041(4) 0.030(5) 0.044(4) 0.000(3) -0.025(4) 0.000(4) C26 0.054(5) 0.021(5) 0.057(4) 0.005(3) -0.012(4) 0.010(4) C27 0.029(4) 0.022(4) 0.032(4) -0.001(4) -0.002(4) 0.001(3) C28 0.065(6) 0.018(5) 0.087(6) -0.007(4) -0.038(5) -0.004(4) C29 0.076(7) 0.032(6) 0.074(6) -0.004(4) -0.054(5) -0.001(5) C30 0.055(5) 0.029(5) 0.062(5) 0.010(4) -0.023(4) 0.001(4) C31 0.051(6) 0.022(5) 0.050(6) -0.001(4) -0.014(4) -0.008(4) C32 0.030(4) 0.016(4) 0.038(4) 0.000(3) 0.001(3) 0.003(3) C33 0.034(5) 0.031(5) 0.058(7) 0.004(4) -0.035(4) -0.002(3) C34 0.056(5) 0.022(5) 0.050(4) -0.002(3) -0.016(4) -0.006(4) C35 0.055(5) 0.028(5) 0.049(4) 0.004(3) 0.002(4) 0.012(4) C36 0.067(6) 0.022(5) 0.045(4) 0.001(3) -0.018(4) -0.001(4) C37 0.045(5) 0.023(4) 0.044(5) -0.008(4) 0.004(4) 0.000(3) C38 0.068(6) 0.020(5) 0.052(5) 0.010(3) -0.023(4) 0.001(4) C39 0.068(6) 0.019(5) 0.060(5) 0.003(4) -0.022(4) -0.007(4) C40 0.046(5) 0.030(5) 0.047(4) 0.005(3) -0.025(3) -0.002(4) C41 0.084(8) 0.015(5) 0.045(6) -0.002(3) 0.003(5) 0.000(4) C42 0.033(4) 0.022(4) 0.042(4) 0.005(4) 0.003(3) -0.001(3) C43 0.059(6) 0.026(5) 0.050(6) 0.003(4) -0.034(5) 0.011(4) C44 0.055(6) 0.039(6) 0.047(4) -0.007(4) -0.017(4) 0.003(4) Co1 0.0363(8) 0.0250(6) 0.0308(7) -0.0007(4) 0.0022(6) -0.0039(4) Co2 0.0366(8) 0.0250(6) 0.0306(7) 0.0000(4) 0.0003(6) -0.0025(4) N1 0.030(3) 0.021(4) 0.046(4) 0.007(3) -0.007(3) 0.000(3) N2 0.025(3) 0.018(3) 0.029(3) 0.003(3) -0.002(3) 0.000(2) N3 0.045(4) 0.026(4) 0.034(3) -0.001(3) -0.008(3) -0.003(3) N4 0.033(4) 0.021(4) 0.045(3) -0.004(3) -0.004(4) -0.001(3) O1 0.046(3) 0.036(4) 0.044(3) -0.002(2) 0.011(2) -0.007(3) O2 0.032(3) 0.058(4) 0.058(3) 0.002(3) 0.003(3) -0.005(3) O3 0.048(3) 0.029(3) 0.028(2) -0.0038(19) -0.003(2) -0.004(2) O4 0.029(3) 0.038(4) 0.067(3) -0.008(3) -0.010(3) 0.002(2) O5 0.032(3) 0.039(4) 0.059(3) -0.004(2) -0.008(2) -0.001(2) O6 0.038(3) 0.028(3) 0.031(2) -0.0011(18) 0.006(2) 0.000(2) O7 0.039(3) 0.037(4) 0.042(3) -0.005(2) 0.012(2) -0.001(2) O8 0.035(3) 0.053(4) 0.049(3) 0.008(3) 0.002(2) -0.001(3) P1 0.0516(19) 0.0401(16) 0.0513(17) -0.0047(10) -0.0119(13) 0.0022(10) P2 0.0454(17) 0.0317(14) 0.0492(17) 0.0028(10) -0.0133(12) -0.0006(10) Zn1 0.0305(4) 0.0210(5) 0.0338(4) 0.0014(4) 0.0007(4) -0.0005(4) Zn2 0.0303(4) 0.0211(5) 0.0348(4) 0.0008(4) -0.0007(4) 0.0000(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 C1 O2 1.237(9) . ? C1 O1 1.269(9) . ? C1 C2 1.514(11) . ? C1 Zn1 2.584(7) . ? C2 C6 1.409(10) . ? C2 C3 1.421(13) . ? C2 Co1 2.033(8) . ? C3 C4 1.444(12) . ? C3 Co1 2.019(8) . ? C3 H3 0.9400 . ? C4 C5 1.395(13) . ? C4 Co1 2.036(8) . ? C4 H4 0.9400 . ? C5 C6 1.439(12) . ? C5 Co1 2.034(8) . ? C5 H5 0.9400 . ? C6 Co1 2.046(7) . ? C6 H6 0.9400 . ? C7 O4 1.235(8) . ? C7 O3 1.247(8) . ? C7 C9 1.551(10) . ? C8 C12 1.385(13) . ? C8 C9 1.429(12) . ? C8 Co1 2.042(8) . ? C8 H8 0.9400 . ? C9 C10 1.435(13) . ? C9 Co1 2.052(8) . ? C10 C11 1.425(11) . ? C10 Co1 2.057(8) . ? C10 H10 0.9400 . ? C11 C12 1.432(14) . ? C11 Co1 2.053(9) . ? C11 H11 0.9400 . ? C12 Co1 2.001(8) . ? C12 H12 0.9400 . ? C13 O5 1.239(8) . ? C13 O6 1.258(9) . ? C13 C14 1.493(11) . ? C14 C18 1.426(12) . ? C14 C15 1.428(12) . ? C14 Co2 2.071(8) . ? C15 C16 1.413(14) . ? C15 Co2 2.029(9) . ? C15 H15 0.9400 . ? C16 C17 1.412(15) . ? C16 Co2 2.060(8) . ? C16 H16 0.9400 . ? C17 C18 1.399(12) . ? C17 Co2 2.026(9) . ? C17 H17 0.9400 . ? C18 Co2 2.034(8) . ? C18 H18 0.9400 . ? C19 O8 1.237(9) . ? C19 O7 1.257(8) . ? C19 C23 1.511(11) . ? C19 Zn2 2.567(7) 4_565 ? C20 C24 1.380(13) . ? C20 C21 1.438(14) . ? C20 Co2 2.016(9) . ? C20 H20 0.9400 . ? C21 C22 1.372(12) . ? C21 Co2 2.043(8) . ? C21 H21 0.9400 . ? C22 C23 1.414(10) . ? C22 Co2 2.013(8) . ? C22 H22 0.9400 . ? C23 C24 1.424(12) . ? C23 Co2 2.040(8) . ? C24 Co2 2.030(9) . ? C24 H24 0.9400 . ? C25 N1 1.330(9) . ? C25 C26 1.392(11) . ? C25 H25 0.9400 . ? C26 C27 1.354(12) . ? C26 H26 0.9400 . ? C27 C28 1.399(12) . ? C27 C32 1.498(9) . ? C28 C29 1.365(12) . ? C28 H28 0.9400 . ? C29 N1 1.347(10) . ? C29 H29 0.9400 . ? C30 N2 1.311(11) . ? C30 C31 1.375(11) . ? C30 H30 0.9400 . ? C31 C32 1.356(12) . ? C31 H31 0.9400 . ? C32 C33 1.384(11) . ? C33 C34 1.389(11) . ? C33 H33 0.9400 . ? C34 N2 1.343(10) . ? C34 H34 0.9400 . ? C35 N3 1.326(10) . ? C35 C36 1.387(11) . ? C35 H35 0.9400 . ? C36 C37 1.400(12) . ? C36 H36 0.9400 . ? C37 C38 1.371(12) . ? C37 C42 1.507(10) . ? C38 C39 1.379(11) . ? C38 H38 0.9400 . ? C39 N3 1.338(11) . ? C39 H39 0.9400 . ? C40 N4 1.291(10) . ? C40 C41 1.408(11) . ? C40 H40 0.9400 . ? C41 C42 1.379(13) . ? C41 H41 0.9400 . ? C42 C43 1.427(12) . ? C43 C44 1.391(11) . ? C43 H43 0.9400 . ? C44 N4 1.344(11) . ? C44 H44 0.9400 . ? F1 P1 1.567(15) . ? F2 P1 1.646(14) . ? F3 P1 1.522(11) . ? F4 P1 1.617(10) . ? F5 P1 1.572(12) . ? F6 P1 1.657(11) . ? F1A P1 1.597(13) . ? F2A P1 1.591(13) . ? F3A P1 1.621(13) . ? F4A P1 1.610(14) . ? F5A P1 1.584(11) . ? F6A P1 1.541(11) . ? F7 P2 1.596(9) . ? F8 P2 1.547(9) . ? F9 P2 1.636(10) . ? F10 P2 1.554(10) . ? F11 P2 1.638(11) . ? F12 P2 1.629(11) . ? F7A P2 1.587(18) . ? F8A P2 1.622(16) . ? F9A P2 1.63(2) . ? F10A P2 1.548(13) . ? F11A P2 1.522(15) . ? F11A F12A 1.69(2) . ? F12A P2 1.553(17) . ? N1 Zn2 2.163(6) 1_545 ? N2 Zn2 2.160(6) . ? N3 Zn1 2.157(6) 1_545 ? N4 Zn1 2.159(6) . ? O1 Zn1 2.097(6) . ? O2 Zn1 2.473(5) . ? O3 Zn2 2.081(4) 4_565 ? O4 Zn1 2.085(5) 4_565 ? O5 Zn2 2.077(5) . ? O6 Zn1 2.073(4) . ? O7 Zn2 2.104(5) 4_565 ? O8 Zn2 2.434(5) 4_565 ? Zn1 O4 2.085(5) 4_465 ? Zn1 N3 2.157(6) 1_565 ? Zn2 O3 2.081(4) 4_465 ? Zn2 O7 2.104(5) 4_465 ? Zn2 N1 2.163(6) 1_565 ? Zn2 O8 2.434(5) 4_465 ? Zn2 C19 2.567(7) 4_465 ? 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 C1 O1 124.5(7) . . ? O2 C1 C2 118.8(7) . . ? O1 C1 C2 116.6(7) . . ? O2 C1 Zn1 70.9(4) . . ? O1 C1 Zn1 53.6(4) . . ? C2 C1 Zn1 169.7(6) . . ? C6 C2 C3 108.2(7) . . ? C6 C2 C1 126.6(8) . . ? C3 C2 C1 125.2(7) . . ? C6 C2 Co1 70.3(5) . . ? C3 C2 Co1 68.9(5) . . ? C1 C2 Co1 124.0(5) . . ? C2 C3 C4 107.7(7) . . ? C2 C3 Co1 70.0(5) . . ? C4 C3 Co1 69.8(4) . . ? C2 C3 H3 126.2 . . ? C4 C3 H3 126.2 . . ? Co1 C3 H3 125.6 . . ? C5 C4 C3 107.8(8) . . ? C5 C4 Co1 69.9(5) . . ? C3 C4 Co1 68.5(5) . . ? C5 C4 H4 126.1 . . ? C3 C4 H4 126.1 . . ? Co1 C4 H4 127.1 . . ? C4 C5 C6 108.5(7) . . ? C4 C5 Co1 70.0(5) . . ? C6 C5 Co1 69.8(4) . . ? C4 C5 H5 125.8 . . ? C6 C5 H5 125.8 . . ? Co1 C5 H5 126.0 . . ? C2 C6 C5 107.9(7) . . ? C2 C6 Co1 69.3(4) . . ? C5 C6 Co1 68.9(4) . . ? C2 C6 H6 126.1 . . ? C5 C6 H6 126.1 . . ? Co1 C6 H6 127.2 . . ? O4 C7 O3 128.9(6) . . ? O4 C7 C9 115.0(6) . . ? O3 C7 C9 116.1(6) . . ? C12 C8 C9 107.1(8) . . ? C12 C8 Co1 68.3(5) . . ? C9 C8 Co1 69.9(4) . . ? C12 C8 H8 126.5 . . ? C9 C8 H8 126.5 . . ? Co1 C8 H8 126.8 . . ? C8 C9 C10 108.4(7) . . ? C8 C9 C7 127.1(7) . . ? C10 C9 C7 124.5(7) . . ? C8 C9 Co1 69.2(4) . . ? C10 C9 Co1 69.8(4) . . ? C7 C9 Co1 128.4(5) . . ? C11 C10 C9 107.4(8) . . ? C11 C10 Co1 69.6(5) . . ? C9 C10 Co1 69.4(5) . . ? C11 C10 H10 126.3 . . ? C9 C10 H10 126.3 . . ? Co1 C10 H10 126.4 . . ? C10 C11 C12 106.5(8) . . ? C10 C11 Co1 69.9(5) . . ? C12 C11 Co1 67.4(5) . . ? C10 C11 H11 126.7 . . ? C12 C11 H11 126.7 . . ? Co1 C11 H11 127.6 . . ? C8 C12 C11 110.5(8) . . ? C8 C12 Co1 71.6(5) . . ? C11 C12 Co1 71.3(5) . . ? C8 C12 H12 124.8 . . ? C11 C12 H12 124.8 . . ? Co1 C12 H12 123.9 . . ? O5 C13 O6 125.9(7) . . ? O5 C13 C14 117.8(7) . . ? O6 C13 C14 116.3(6) . . ? C18 C14 C15 105.2(8) . . ? C18 C14 C13 128.0(7) . . ? C15 C14 C13 126.8(8) . . ? C18 C14 Co2 68.3(5) . . ? C15 C14 Co2 68.1(4) . . ? C13 C14 Co2 128.0(5) . . ? C16 C15 C14 110.3(10) . . ? C16 C15 Co2 71.0(5) . . ? C14 C15 Co2 71.2(5) . . ? C16 C15 H15 124.9 . . ? C14 C15 H15 124.9 . . ? Co2 C15 H15 124.5 . . ? C17 C16 C15 106.2(8) . . ? C17 C16 Co2 68.5(5) . . ? C15 C16 Co2 68.6(5) . . ? C17 C16 H16 126.9 . . ? C15 C16 H16 126.9 . . ? Co2 C16 H16 127.5 . . ? C18 C17 C16 109.2(9) . . ? C18 C17 Co2 70.2(5) . . ? C16 C17 Co2 71.1(5) . . ? C18 C17 H17 125.4 . . ? C16 C17 H17 125.4 . . ? Co2 C17 H17 125.0 . . ? C17 C18 C14 109.1(8) . . ? C17 C18 Co2 69.5(5) . . ? C14 C18 Co2 71.1(5) . . ? C17 C18 H18 125.5 . . ? C14 C18 H18 125.5 . . ? Co2 C18 H18 125.5 . . ? O8 C19 O7 124.3(7) . . ? O8 C19 C23 119.6(6) . . ? O7 C19 C23 116.0(7) . . ? O8 C19 Zn2 69.8(4) . 4_565 ? O7 C19 Zn2 54.6(4) . 4_565 ? C23 C19 Zn2 170.5(5) . 4_565 ? C24 C20 C21 109.4(9) . . ? C24 C20 Co2 70.6(5) . . ? C21 C20 Co2 70.3(5) . . ? C24 C20 H20 125.3 . . ? C21 C20 H20 125.3 . . ? Co2 C20 H20 125.4 . . ? C22 C21 C20 105.9(8) . . ? C22 C21 Co2 69.1(5) . . ? C20 C21 Co2 68.2(5) . . ? C22 C21 H21 127.1 . . ? C20 C21 H21 127.1 . . ? Co2 C21 H21 127.1 . . ? C21 C22 C23 110.6(8) . . ? C21 C22 Co2 71.4(5) . . ? C23 C22 Co2 70.6(4) . . ? C21 C22 H22 124.7 . . ? C23 C22 H22 124.7 . . ? Co2 C22 H22 124.9 . . ? C22 C23 C24 106.4(7) . . ? C22 C23 C19 127.0(7) . . ? C24 C23 C19 126.5(7) . . ? C22 C23 Co2 68.6(4) . . ? C24 C23 Co2 69.1(5) . . ? C19 C23 Co2 124.2(5) . . ? C20 C24 C23 107.7(8) . . ? C20 C24 Co2 69.5(5) . . ? C23 C24 Co2 69.9(5) . . ? C20 C24 H24 126.2 . . ? C23 C24 H24 126.2 . . ? Co2 C24 H24 126.0 . . ? N1 C25 C26 123.0(7) . . ? N1 C25 H25 118.5 . . ? C26 C25 H25 118.5 . . ? C27 C26 C25 121.3(7) . . ? C27 C26 H26 119.3 . . ? C25 C26 H26 119.3 . . ? C26 C27 C28 115.8(7) . . ? C26 C27 C32 123.6(7) . . ? C28 C27 C32 120.6(7) . . ? C29 C28 C27 120.3(7) . . ? C29 C28 H28 119.9 . . ? C27 C28 H28 119.9 . . ? N1 C29 C28 123.8(8) . . ? N1 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? N2 C30 C31 120.7(8) . . ? N2 C30 H30 119.7 . . ? C31 C30 H30 119.7 . . ? C32 C31 C30 124.7(9) . . ? C32 C31 H31 117.6 . . ? C30 C31 H31 117.6 . . ? C31 C32 C33 113.8(7) . . ? C31 C32 C27 121.8(7) . . ? C33 C32 C27 124.3(7) . . ? C32 C33 C34 120.3(7) . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? N2 C34 C33 122.8(7) . . ? N2 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? N3 C35 C36 124.9(8) . . ? N3 C35 H35 117.5 . . ? C36 C35 H35 117.5 . . ? C35 C36 C37 119.1(8) . . ? C35 C36 H36 120.5 . . ? C37 C36 H36 120.5 . . ? C38 C37 C36 115.9(7) . . ? C38 C37 C42 123.1(8) . . ? C36 C37 C42 121.0(8) . . ? C37 C38 C39 120.8(8) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? N3 C39 C38 123.9(8) . . ? N3 C39 H39 118.0 . . ? C38 C39 H39 118.0 . . ? N4 C40 C41 124.0(8) . . ? N4 C40 H40 118.0 . . ? C41 C40 H40 118.0 . . ? C42 C41 C40 119.5(9) . . ? C42 C41 H41 120.3 . . ? C40 C41 H41 120.3 . . ? C41 C42 C43 117.1(7) . . ? C41 C42 C37 121.8(8) . . ? C43 C42 C37 121.0(8) . . ? C44 C43 C42 117.4(8) . . ? C44 C43 H43 121.3 . . ? C42 C43 H43 121.3 . . ? N4 C44 C43 124.3(8) . . ? N4 C44 H44 117.9 . . ? C43 C44 H44 117.9 . . ? C12 Co1 C3 163.1(4) . . ? C12 Co1 C2 153.4(4) . . ? C3 Co1 C2 41.1(4) . . ? C12 Co1 C5 105.4(4) . . ? C3 Co1 C5 68.9(3) . . ? C2 Co1 C5 68.9(3) . . ? C12 Co1 C4 124.0(4) . . ? C3 Co1 C4 41.7(3) . . ? C2 Co1 C4 69.3(3) . . ? C5 Co1 C4 40.1(4) . . ? C12 Co1 C8 40.1(4) . . ? C3 Co1 C8 127.7(4) . . ? C2 Co1 C8 165.2(4) . . ? C5 Co1 C8 119.5(4) . . ? C4 Co1 C8 108.6(4) . . ? C12 Co1 C6 118.3(4) . . ? C3 Co1 C6 68.7(3) . . ? C2 Co1 C6 40.4(3) . . ? C5 Co1 C6 41.3(4) . . ? C4 Co1 C6 68.6(3) . . ? C8 Co1 C6 153.7(4) . . ? C12 Co1 C9 67.9(3) . . ? C3 Co1 C9 110.5(3) . . ? C2 Co1 C9 127.2(3) . . ? C5 Co1 C9 156.4(4) . . ? C4 Co1 C9 123.6(3) . . ? C8 Co1 C9 40.9(3) . . ? C6 Co1 C9 162.1(3) . . ? C12 Co1 C11 41.3(4) . . ? C3 Co1 C11 155.1(4) . . ? C2 Co1 C11 118.4(4) . . ? C5 Co1 C11 122.5(4) . . ? C4 Co1 C11 159.9(4) . . ? C8 Co1 C11 68.8(4) . . ? C6 Co1 C11 104.5(4) . . ? C9 Co1 C11 68.4(3) . . ? C12 Co1 C10 68.7(4) . . ? C3 Co1 C10 122.0(3) . . ? C2 Co1 C10 107.3(4) . . ? C5 Co1 C10 160.0(4) . . ? C4 Co1 C10 158.8(3) . . ? C8 Co1 C10 69.1(4) . . ? C6 Co1 C10 123.2(4) . . ? C9 Co1 C10 40.9(3) . . ? C11 Co1 C10 40.6(3) . . ? C22 Co2 C20 67.6(4) . . ? C22 Co2 C17 107.1(4) . . ? C20 Co2 C17 158.2(4) . . ? C22 Co2 C15 156.6(3) . . ? C20 Co2 C15 108.3(5) . . ? C17 Co2 C15 67.7(4) . . ? C22 Co2 C24 68.4(3) . . ? C20 Co2 C24 39.9(4) . . ? C17 Co2 C24 160.0(4) . . ? C15 Co2 C24 124.3(4) . . ? C22 Co2 C18 123.9(4) . . ? C20 Co2 C18 160.1(4) . . ? C17 Co2 C18 40.3(3) . . ? C15 Co2 C18 67.8(4) . . ? C24 Co2 C18 124.8(4) . . ? C22 Co2 C23 40.8(3) . . ? C20 Co2 C23 67.9(4) . . ? C17 Co2 C23 122.9(4) . . ? C15 Co2 C23 161.1(3) . . ? C24 Co2 C23 41.0(3) . . ? C18 Co2 C23 109.1(4) . . ? C22 Co2 C21 39.5(4) . . ? C20 Co2 C21 41.5(4) . . ? C17 Co2 C21 121.0(4) . . ? C15 Co2 C21 122.0(4) . . ? C24 Co2 C21 68.8(3) . . ? C18 Co2 C21 157.5(4) . . ? C23 Co2 C21 68.3(3) . . ? C22 Co2 C16 120.8(4) . . ? C20 Co2 C16 122.5(5) . . ? C17 Co2 C16 40.4(4) . . ? C15 Co2 C16 40.4(4) . . ? C24 Co2 C16 158.9(4) . . ? C18 Co2 C16 68.1(4) . . ? C23 Co2 C16 157.5(4) . . ? C21 Co2 C16 105.4(4) . . ? C22 Co2 C14 160.7(3) . . ? C20 Co2 C14 123.6(4) . . ? C17 Co2 C14 68.3(3) . . ? C15 Co2 C14 40.7(3) . . ? C24 Co2 C14 109.1(3) . . ? C18 Co2 C14 40.6(3) . . ? C23 Co2 C14 124.7(3) . . ? C21 Co2 C14 159.1(4) . . ? C16 Co2 C14 68.7(4) . . ? P2 F11A F12A 57.5(8) . . ? P2 F12A F11A 55.8(8) . . ? C25 N1 C29 115.8(7) . . ? C25 N1 Zn2 120.6(5) . 1_545 ? C29 N1 Zn2 123.5(5) . 1_545 ? C30 N2 C34 117.6(6) . . ? C30 N2 Zn2 119.6(5) . . ? C34 N2 Zn2 122.7(5) . . ? C35 N3 C39 115.2(7) . . ? C35 N3 Zn1 121.0(6) . 1_545 ? C39 N3 Zn1 123.8(5) . 1_545 ? C40 N4 C44 117.5(7) . . ? C40 N4 Zn1 124.7(6) . . ? C44 N4 Zn1 117.5(6) . . ? C1 O1 Zn1 97.2(5) . . ? C1 O2 Zn1 80.9(4) . . ? C7 O3 Zn2 122.8(4) . 4_565 ? C7 O4 Zn1 161.2(5) . 4_565 ? C13 O5 Zn2 159.9(5) . . ? C13 O6 Zn1 121.9(4) . . ? C19 O7 Zn2 96.3(5) . 4_565 ? C19 O8 Zn2 81.7(4) . 4_565 ? F3 P1 F6A 120.5(7) . . ? F3 P1 F1 85.1(7) . . ? F6A P1 F1 69.6(7) . . ? F3 P1 F5 84.9(7) . . ? F6A P1 F5 41.6(5) . . ? F1 P1 F5 85.1(7) . . ? F3 P1 F5A 99.4(6) . . ? F6A P1 F5A 96.4(6) . . ? F1 P1 F5A 42.8(6) . . ? F5 P1 F5A 126.3(6) . . ? F3 P1 F2A 76.4(7) . . ? F6A P1 F2A 84.2(6) . . ? F1 P1 F2A 134.0(8) . . ? F5 P1 F2A 52.0(6) . . ? F5A P1 F2A 175.4(7) . . ? F3 P1 F1A 36.7(5) . . ? F6A P1 F1A 87.2(7) . . ? F1 P1 F1A 56.3(7) . . ? F5 P1 F1A 63.3(7) . . ? F5A P1 F1A 89.1(6) . . ? F2A P1 F1A 86.4(7) . . ? F3 P1 F4A 138.4(7) . . ? F6A P1 F4A 98.7(7) . . ? F1 P1 F4A 124.5(8) . . ? F5 P1 F4A 122.3(7) . . ? F5A P1 F4A 88.8(7) . . ? F2A P1 F4A 95.6(7) . . ? F1A P1 F4A 174.0(8) . . ? F3 P1 F4 92.8(6) . . ? F6A P1 F4 105.5(6) . . ? F1 P1 F4 172.4(7) . . ? F5 P1 F4 87.4(6) . . ? F5A P1 F4 144.7(6) . . ? F2A P1 F4 38.5(5) . . ? F1A P1 F4 118.7(6) . . ? F4A P1 F4 61.2(6) . . ? F3 P1 F3A 47.7(6) . . ? F6A P1 F3A 166.3(7) . . ? F1 P1 F3A 111.9(7) . . ? F5 P1 F3A 124.8(7) . . ? F5A P1 F3A 92.8(6) . . ? F2A P1 F3A 85.7(7) . . ? F1A P1 F3A 82.9(7) . . ? F4A P1 F3A 91.5(7) . . ? F4 P1 F3A 71.5(6) . . ? F3 P1 F2 176.3(7) . . ? F6A P1 F2 56.0(6) . . ? F1 P1 F2 92.1(8) . . ? F5 P1 F2 92.3(7) . . ? F5A P1 F2 80.1(7) . . ? F2A P1 F2 103.9(7) . . ? F1A P1 F2 139.6(7) . . ? F4A P1 F2 45.3(6) . . ? F4 P1 F2 89.6(6) . . ? F3A P1 F2 136.0(7) . . ? F3 P1 F6 99.0(6) . . ? F6A P1 F6 136.6(6) . . ? F1 P1 F6 99.2(7) . . ? F5 P1 F6 174.3(6) . . ? F5A P1 F6 57.3(5) . . ? F2A P1 F6 124.8(6) . . ? F1A P1 F6 122.2(6) . . ? F4A P1 F6 52.2(6) . . ? F4 P1 F6 88.3(5) . . ? F3A P1 F6 57.0(6) . . ? F2 P1 F6 83.9(6) . . ? F11A P2 F8 106.4(7) . . ? F11A P2 F10A 98.3(8) . . ? F8 P2 F10A 36.6(5) . . ? F11A P2 F12A 66.7(9) . . ? F8 P2 F12A 59.3(7) . . ? F10A P2 F12A 85.7(8) . . ? F11A P2 F10 110.8(7) . . ? F8 P2 F10 98.2(5) . . ? F10A P2 F10 132.9(6) . . ? F12A P2 F10 73.8(8) . . ? F11A P2 F7A 113.7(10) . . ? F8 P2 F7A 116.4(7) . . ? F10A P2 F7A 89.2(8) . . ? F12A P2 F7A 174.9(9) . . ? F10 P2 F7A 110.2(8) . . ? F11A P2 F7 150.9(8) . . ? F8 P2 F7 91.3(5) . . ? F10A P2 F7 82.0(6) . . ? F12A P2 F7 141.8(8) . . ? F10 P2 F7 88.6(5) . . ? F7A P2 F7 37.3(7) . . ? F11A P2 F8A 79.0(8) . . ? F8 P2 F8A 146.4(8) . . ? F10A P2 F8A 176.4(8) . . ? F12A P2 F8A 95.3(9) . . ? F10 P2 F8A 50.6(7) . . ? F7A P2 F8A 89.7(9) . . ? F7 P2 F8A 99.2(7) . . ? F11A P2 F9A 155.6(11) . . ? F8 P2 F9A 69.2(8) . . ? F10A P2 F9A 91.3(9) . . ? F12A P2 F9A 92.0(10) . . ? F10 P2 F9A 48.9(8) . . ? F7A P2 F9A 88.7(10) . . ? F7 P2 F9A 52.6(8) . . ? F8A P2 F9A 92.1(9) . . ? F11A P2 F12 69.4(7) . . ? F8 P2 F12 175.8(5) . . ? F10A P2 F12 142.2(7) . . ? F12A P2 F12 118.2(7) . . ? F10 P2 F12 83.9(5) . . ? F7A P2 F12 65.9(8) . . ? F7 P2 F12 92.4(5) . . ? F8A P2 F12 34.5(6) . . ? F9A P2 F12 114.7(9) . . ? F11A P2 F9 29.0(6) . . ? F8 P2 F9 89.3(5) . . ? F10A P2 F9 98.6(6) . . ? F12A P2 F9 38.5(6) . . ? F10 P2 F9 91.0(5) . . ? F7A P2 F9 142.5(9) . . ? F7 P2 F9 179.4(5) . . ? F8A P2 F9 80.2(7) . . ? F9A P2 F9 127.4(9) . . ? F12 P2 F9 87.0(5) . . ? F11A P2 F11 62.6(7) . . ? F8 P2 F11 91.3(5) . . ? F10A P2 F11 57.2(6) . . ? F12A P2 F11 108.5(8) . . ? F10 P2 F11 169.8(5) . . ? F7A P2 F11 68.1(8) . . ? F7 P2 F11 94.7(5) . . ? F8A P2 F11 119.3(7) . . ? F9A P2 F11 139.5(8) . . ? F12 P2 F11 86.4(6) . . ? F9 P2 F11 85.5(5) . . ? O6 Zn1 O4 127.2(2) . 4_465 ? O6 Zn1 O1 91.32(19) . . ? O4 Zn1 O1 141.5(2) 4_465 . ? O6 Zn1 N3 91.9(2) . 1_565 ? O4 Zn1 N3 86.5(2) 4_465 1_565 ? O1 Zn1 N3 92.4(2) . 1_565 ? O6 Zn1 N4 91.9(3) . . ? O4 Zn1 N4 88.0(2) 4_465 . ? O1 Zn1 N4 91.6(2) . . ? N3 Zn1 N4 174.4(3) 1_565 . ? O6 Zn1 O2 148.67(18) . . ? O4 Zn1 O2 84.1(2) 4_465 . ? O1 Zn1 O2 57.36(19) . . ? N3 Zn1 O2 90.6(3) 1_565 . ? N4 Zn1 O2 88.3(3) . . ? O6 Zn1 C1 120.5(2) . . ? O4 Zn1 C1 112.3(2) 4_465 . ? O1 Zn1 C1 29.2(2) . . ? N3 Zn1 C1 91.3(3) 1_565 . ? N4 Zn1 C1 90.3(3) . . ? O2 Zn1 C1 28.2(2) . . ? O5 Zn2 O3 124.0(2) . 4_465 ? O5 Zn2 O7 143.6(2) . 4_465 ? O3 Zn2 O7 92.37(19) 4_465 4_465 ? O5 Zn2 N2 90.2(2) . . ? O3 Zn2 N2 92.9(2) 4_465 . ? O7 Zn2 N2 90.6(2) 4_465 . ? O5 Zn2 N1 85.5(2) . 1_565 ? O3 Zn2 N1 90.4(2) 4_465 1_565 ? O7 Zn2 N1 92.2(2) 4_465 1_565 ? N2 Zn2 N1 175.5(2) . 1_565 ? O5 Zn2 O8 86.0(2) . 4_465 ? O3 Zn2 O8 149.96(18) 4_465 4_465 ? O7 Zn2 O8 57.62(19) 4_465 4_465 ? N2 Zn2 O8 88.8(2) . 4_465 ? N1 Zn2 O8 89.8(3) 1_565 4_465 ? O5 Zn2 C19 114.5(2) . 4_465 ? O3 Zn2 C19 121.5(2) 4_465 4_465 ? O7 Zn2 C19 29.1(2) 4_465 4_465 ? N2 Zn2 C19 90.2(2) . 4_465 ? N1 Zn2 C19 90.6(3) 1_565 4_465 ? O8 Zn2 C19 28.5(2) 4_465 4_465 ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.93 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.637 _refine_diff_density_min -0.338 _refine_diff_density_rms 0.099 _database_code_depnum_ccdc_archive 'CCDC 950063' ####################################################################### # # 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_ip2-1438 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C22 H16 Co Cu N2 O4, (F6 P)' _chemical_formula_sum 'C22 H16 Co Cu F6 N2 O4 P' _chemical_formula_weight 639.81 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 '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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pna2(1) _symmetry_space_group_name_Hall 'P 2c -2n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 16.5410(16) _cell_length_b 11.1592(7) _cell_length_c 23.5962(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4355.5(6) _cell_formula_units_Z 8 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 10450 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.2 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.951 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2552 _exptl_absorpt_coefficient_mu 1.899 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 180(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 'STOE IPDS-2T' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14405 _diffrn_reflns_av_R_equivalents 0.0515 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7122 _reflns_number_gt 5242 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STOE X-AREA' _computing_cell_refinement 'STOE X-AREA' _computing_data_reduction 'STOE X-AREA, STOE X-RED' _computing_structure_solution ? _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^)+(0.0824P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.42(2) _refine_ls_number_reflns 7122 _refine_ls_number_parameters 658 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0748 _refine_ls_R_factor_gt 0.0523 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1232 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.5792(6) 0.5995(7) 0.5869(5) 0.040(2) Uani 1 1 d . . . C2 C 0.6520(6) 0.5970(6) 0.5484(5) 0.033(2) Uani 1 1 d . . . C3 C 0.7356(7) 0.5926(7) 0.5670(5) 0.036(2) Uani 1 1 d . . . H3 H 0.7538 0.5876 0.6051 0.043 Uiso 1 1 calc R . . C4 C 0.7848(6) 0.5969(7) 0.5185(6) 0.039(3) Uani 1 1 d . . . H4 H 0.8421 0.5907 0.5181 0.047 Uiso 1 1 calc R . . C5 C 0.7344(6) 0.6121(7) 0.4696(5) 0.036(2) Uani 1 1 d . . . H5 H 0.7525 0.6211 0.4316 0.043 Uiso 1 1 calc R . . C6 C 0.6508(6) 0.6113(7) 0.4881(4) 0.034(2) Uani 1 1 d . . . H6 H 0.6043 0.6188 0.4648 0.040 Uiso 1 1 calc R . . C7 C 0.7864(6) 0.8777(6) 0.6377(4) 0.035(2) Uani 1 1 d . . . C8 C 0.7871(6) 0.8966(7) 0.5270(5) 0.036(2) Uani 1 1 d . . . H8 H 0.8442 0.8984 0.5228 0.043 Uiso 1 1 calc R . . C9 C 0.7465(6) 0.8870(6) 0.5785(4) 0.026(2) Uani 1 1 d . . . C10 C 0.6615(7) 0.8889(7) 0.5673(5) 0.039(2) Uani 1 1 d . . . H10 H 0.6201 0.8841 0.5950 0.046 Uiso 1 1 calc R . . C11 C 0.6491(7) 0.8992(7) 0.5074(6) 0.053(3) Uani 1 1 d . . . H11 H 0.5987 0.9027 0.4881 0.063 Uiso 1 1 calc R . . C12 C 0.7308(8) 0.9032(8) 0.4815(5) 0.045(3) Uani 1 1 d . . . H12 H 0.7430 0.9091 0.4423 0.054 Uiso 1 1 calc R . . C13 C 0.4696(4) 0.6161(5) 0.7962(5) 0.029(2) Uani 1 1 d . . . C14 C 0.5040(7) 0.6037(8) 0.8534(5) 0.039(3) Uani 1 1 d . . . C15 C 0.4567(9) 0.5992(8) 0.9069(7) 0.056(4) Uani 1 1 d . . . H15 H 0.3997 0.6070 0.9101 0.068 Uiso 1 1 calc R . . C16 C 0.5109(9) 0.5815(9) 0.9515(6) 0.058(4) Uani 1 1 d . . . H16 H 0.4969 0.5722 0.9903 0.070 Uiso 1 1 calc R . . C17 C 0.5898(8) 0.5798(8) 0.9291(5) 0.051(3) Uani 1 1 d . . . H17 H 0.6380 0.5715 0.9507 0.061 Uiso 1 1 calc R . . C18 C 0.5864(7) 0.5924(8) 0.8700(5) 0.043(3) Uani 1 1 d . . . H18 H 0.6316 0.5932 0.8451 0.052 Uiso 1 1 calc R . . C19 C 0.6727(6) 0.8813(6) 0.8471(5) 0.040(2) Uani 1 1 d . . . C20 C 0.4706(7) 0.8889(7) 0.9221(6) 0.039(3) Uani 1 1 d . . . H20 H 0.4135 0.8939 0.9250 0.047 Uiso 1 1 calc R . . C21 C 0.5259(8) 0.8706(8) 0.9669(6) 0.051(3) Uani 1 1 d . . . H21 H 0.5120 0.8624 1.0058 0.061 Uiso 1 1 calc R . . C22 C 0.6035(6) 0.8665(7) 0.9451(5) 0.040(2) Uani 1 1 d . . . H22 H 0.6512 0.8538 0.9667 0.048 Uiso 1 1 calc R . . C23 C 0.6011(6) 0.8840(6) 0.8862(5) 0.031(2) Uani 1 1 d . . . C24 C 0.5190(6) 0.8985(7) 0.8702(5) 0.038(3) Uani 1 1 d . . . H24 H 0.4991 0.9118 0.8330 0.046 Uiso 1 1 calc R . . C25 C 0.2282(6) -0.1280(7) 0.7320(5) 0.045(2) Uani 1 1 d . . . H25 H 0.1945 -0.1695 0.7060 0.054 Uiso 1 1 calc R . . C26 C 0.2265(6) -0.0043(7) 0.7335(4) 0.043(2) Uani 1 1 d . . . H26 H 0.1890 0.0369 0.7100 0.051 Uiso 1 1 calc R . . C27 C 0.2766(6) 0.0604(6) 0.7674(6) 0.0280(19) Uani 1 1 d . . . C28 C 0.3249(7) -0.0074(7) 0.8038(6) 0.068(4) Uani 1 1 d . . . H28 H 0.3593 0.0327 0.8299 0.082 Uiso 1 1 calc R . . C29 C 0.3240(7) -0.1293(7) 0.8030(6) 0.062(4) Uani 1 1 d . . . H29 H 0.3575 -0.1725 0.8285 0.074 Uiso 1 1 calc R . . C30 C 0.2376(6) 0.3833(7) 0.7287(5) 0.045(2) Uani 1 1 d . . . H30 H 0.2056 0.4240 0.7013 0.054 Uiso 1 1 calc R . . C31 C 0.2377(8) 0.2579(6) 0.7297(6) 0.038(3) Uani 1 1 d . . . H31 H 0.2068 0.2160 0.7021 0.046 Uiso 1 1 calc R . . C32 C 0.2791(5) 0.1949(6) 0.7676(5) 0.0316(19) Uani 1 1 d . . . C33 C 0.3219(6) 0.2600(6) 0.8077(6) 0.035(3) Uani 1 1 d . . . H33 H 0.3513 0.2200 0.8366 0.042 Uiso 1 1 calc R . . C34 C 0.3215(6) 0.3851(7) 0.8049(4) 0.041(2) Uani 1 1 d . . . H34 H 0.3512 0.4286 0.8326 0.049 Uiso 1 1 calc R . . C35 C 0.5226(6) -0.1454(7) 0.7027(4) 0.042(2) Uani 1 1 d . . . H35 H 0.5567 -0.1878 0.7282 0.050 Uiso 1 1 calc R . . C36 C 0.5228(6) -0.0216(7) 0.7048(4) 0.043(2) Uani 1 1 d . . . H36 H 0.5550 0.0186 0.7322 0.052 Uiso 1 1 calc R . . C37 C 0.4759(6) 0.0445(6) 0.6669(6) 0.033(2) Uani 1 1 d . . . C38 C 0.4346(6) -0.0241(7) 0.6269(5) 0.051(3) Uani 1 1 d . . . H38 H 0.4063 0.0147 0.5970 0.061 Uiso 1 1 calc R . . C39 C 0.4341(7) -0.1465(8) 0.6302(6) 0.057(3) Uani 1 1 d . . . H39 H 0.4007 -0.1894 0.6044 0.068 Uiso 1 1 calc R . . C40 C 0.4292(6) 0.3679(7) 0.6301(4) 0.040(2) Uani 1 1 d . . . H40 H 0.3993 0.4101 0.6021 0.048 Uiso 1 1 calc R . . C41 C 0.4298(9) 0.2441(7) 0.6292(7) 0.048(4) Uani 1 1 d . . . H41 H 0.3991 0.2033 0.6012 0.058 Uiso 1 1 calc R . . C42 C 0.4736(5) 0.1782(5) 0.6680(6) 0.035(2) Uani 1 1 d . . . C43 C 0.5176(9) 0.2428(6) 0.7093(6) 0.043(3) Uani 1 1 d . . . H43 H 0.5497 0.2029 0.7369 0.052 Uiso 1 1 calc R . . C44 C 0.5122(6) 0.3669(7) 0.7078(4) 0.040(2) Uani 1 1 d . . . H44 H 0.5405 0.4110 0.7360 0.048 Uiso 1 1 calc R . . Co1 Co 0.71451(9) 0.74793(8) 0.52600(7) 0.0307(3) Uani 1 1 d . . . Co2 Co 0.53653(9) 0.73747(8) 0.90897(6) 0.0307(4) Uani 1 1 d . . . Cu1 Cu 0.47417(6) 0.60964(7) 0.66936(6) 0.0304(2) Uani 1 1 d . . . Cu2 Cu 0.27765(6) 0.62742(7) 0.76479(6) 0.0300(2) Uani 1 1 d . . . F1 F 0.1808(8) 0.3392(10) 0.6078(6) 0.063(3) Uiso 0.538(8) 1 d P A 1 F2 F 0.2469(7) 0.1628(9) 0.5940(6) 0.057(3) Uiso 0.538(8) 1 d P A 1 F3 F 0.1362(7) 0.3370(9) 0.5222(6) 0.055(3) Uiso 0.538(8) 1 d P A 1 F4 F 0.2015(6) 0.1622(8) 0.5033(4) 0.041(3) Uiso 0.538(8) 1 d P A 1 F5 F 0.1116(8) 0.1782(11) 0.5752(6) 0.068(3) Uiso 0.538(8) 1 d P A 1 F6 F 0.2745(6) 0.3144(10) 0.5380(6) 0.055(3) Uiso 0.538(8) 1 d P A 1 F1A F 0.1123(10) 0.3404(13) 0.5639(8) 0.071(4) Uiso 0.462(8) 1 d P A 2 F2A F 0.1361(9) 0.1686(13) 0.5139(8) 0.070(4) Uiso 0.462(8) 1 d P A 2 F3A F 0.2069(9) 0.3331(13) 0.4952(7) 0.065(4) Uiso 0.462(8) 1 d P A 2 F4A F 0.2685(8) 0.1750(11) 0.5418(7) 0.054(4) Uiso 0.462(8) 1 d P A 2 F5A F 0.2436(7) 0.3416(9) 0.5910(5) 0.038(3) Uiso 0.462(8) 1 d P A 2 F6A F 0.1657(9) 0.1765(11) 0.6035(7) 0.059(4) Uiso 0.462(8) 1 d P A 2 F7 F 0.1065(6) 0.1821(8) 0.9257(5) 0.055(3) Uiso 0.647(10) 1 d P B 1 F8 F 0.0260(7) 0.3462(9) 0.9322(5) 0.064(3) Uiso 0.647(10) 1 d P B 1 F9 F 0.0138(6) 0.3484(8) 0.8363(5) 0.050(2) Uiso 0.647(10) 1 d P B 1 F10 F -0.0148(6) 0.1771(8) 0.8849(5) 0.058(3) Uiso 0.647(10) 1 d P B 1 F11 F 0.1344(6) 0.3537(8) 0.8727(5) 0.056(3) Uiso 0.647(10) 1 d P B 1 F12 F 0.0918(6) 0.1853(7) 0.8283(4) 0.049(2) Uiso 0.647(10) 1 d P B 1 F7A F 0.1388(12) 0.1910(15) 0.8970(10) 0.064(5) Uiso 0.353(10) 1 d P B 2 F8A F 0.0351(12) 0.1658(15) 0.8327(9) 0.059(5) Uiso 0.353(10) 1 d P B 2 F9A F 0.0110(14) 0.1798(19) 0.9236(12) 0.082(6) Uiso 0.353(10) 1 d P B 2 F10A F 0.0829(10) 0.3578(12) 0.9284(7) 0.045(4) Uiso 0.353(10) 1 d P B 2 F11A F 0.111(2) 0.336(3) 0.8317(18) 0.134(12) Uiso 0.353(10) 1 d P B 2 F12A F -0.0170(10) 0.3407(14) 0.8666(9) 0.050(5) Uiso 0.353(10) 1 d P B 2 N1 N 0.2758(4) -0.1898(5) 0.7663(4) 0.0329(16) Uani 1 1 d . . . N2 N 0.2812(5) 0.4466(5) 0.7652(5) 0.0292(16) Uani 1 1 d . . . N3 N 0.4771(4) -0.2082(5) 0.6668(5) 0.0386(18) Uani 1 1 d . . . N4 N 0.4693(5) 0.4288(5) 0.6690(5) 0.0338(18) Uani 1 1 d . . . O1 O 0.5913(4) 0.6023(5) 0.6389(3) 0.0447(17) Uani 1 1 d . . . O2 O 0.5115(4) 0.5990(6) 0.5619(4) 0.0512(19) Uani 1 1 d . . . O3 O 0.7382(4) 0.8683(5) 0.6787(3) 0.0420(16) Uani 1 1 d . . . O4 O 0.8591(4) 0.8867(5) 0.6379(4) 0.052(2) Uani 1 1 d . . . O5 O 0.3946(4) 0.6352(5) 0.7922(3) 0.0490(18) Uani 1 1 d . . . O6 O 0.5179(4) 0.6104(4) 0.7555(3) 0.0338(13) Uani 1 1 d . . . O7 O 0.6583(5) 0.8799(5) 0.7955(3) 0.0487(19) Uani 1 1 d . . . O8 O 0.7420(4) 0.8785(6) 0.8685(4) 0.059(2) Uani 1 1 d . . . P1 P 0.1906(2) 0.25270(17) 0.55558(19) 0.0440(9) Uani 1 1 d . . . P2 P 0.0586(2) 0.26467(19) 0.88177(17) 0.0410(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 C1 0.047(6) 0.020(3) 0.052(7) 0.006(4) 0.008(5) -0.001(3) C2 0.034(5) 0.021(3) 0.044(7) 0.001(4) 0.003(4) -0.003(3) C3 0.050(6) 0.026(4) 0.031(6) 0.003(3) 0.009(5) 0.004(4) C4 0.028(5) 0.033(4) 0.055(8) -0.015(4) 0.019(5) 0.000(3) C5 0.038(5) 0.034(4) 0.035(6) -0.007(4) 0.014(4) -0.003(3) C6 0.040(5) 0.029(4) 0.032(6) -0.004(3) -0.008(4) -0.007(3) C7 0.053(6) 0.021(3) 0.033(6) -0.004(3) 0.007(4) -0.012(3) C8 0.042(5) 0.032(4) 0.033(6) 0.004(4) 0.015(5) -0.012(4) C9 0.031(5) 0.019(3) 0.029(5) 0.005(3) 0.006(4) 0.002(3) C10 0.050(6) 0.025(4) 0.041(7) 0.002(4) -0.003(5) 0.009(3) C11 0.054(6) 0.025(4) 0.079(10) 0.007(5) -0.019(6) 0.014(4) C12 0.069(7) 0.037(4) 0.030(6) 0.010(4) 0.001(5) -0.019(4) C13 0.022(4) 0.014(3) 0.051(6) -0.001(3) -0.007(4) 0.001(2) C14 0.047(6) 0.024(4) 0.044(7) -0.006(4) 0.007(5) 0.000(3) C15 0.089(10) 0.025(4) 0.055(9) 0.002(5) 0.007(7) -0.009(5) C16 0.091(10) 0.034(5) 0.050(8) 0.011(5) 0.012(7) -0.010(5) C17 0.075(8) 0.043(5) 0.033(7) 0.005(5) -0.024(6) 0.001(5) C18 0.050(6) 0.028(4) 0.052(8) -0.003(4) -0.008(5) 0.002(4) C19 0.046(6) 0.018(3) 0.056(7) 0.004(4) 0.016(5) -0.001(3) C20 0.040(6) 0.027(4) 0.051(8) -0.001(4) 0.000(5) 0.000(3) C21 0.066(7) 0.039(5) 0.047(7) 0.001(5) 0.009(6) -0.004(5) C22 0.041(5) 0.034(4) 0.044(7) -0.005(4) 0.013(5) -0.009(4) C23 0.033(5) 0.026(4) 0.036(6) -0.001(4) 0.005(4) 0.002(3) C24 0.033(5) 0.025(4) 0.057(8) 0.001(4) -0.015(5) -0.002(3) C25 0.044(5) 0.031(4) 0.059(7) -0.007(4) -0.018(6) 0.000(4) C26 0.050(5) 0.025(4) 0.053(6) -0.005(4) -0.008(5) 0.001(4) C27 0.035(4) 0.016(3) 0.033(5) -0.003(4) -0.002(5) -0.002(3) C28 0.072(7) 0.022(4) 0.110(11) -0.007(5) -0.049(7) 0.005(4) C29 0.082(8) 0.023(4) 0.079(9) -0.005(5) -0.056(7) 0.006(4) C30 0.058(6) 0.022(4) 0.054(7) 0.004(4) -0.017(5) 0.004(4) C31 0.049(6) 0.020(4) 0.044(8) -0.002(4) -0.015(6) -0.009(3) C32 0.039(4) 0.018(3) 0.038(6) -0.001(4) 0.001(4) -0.001(3) C33 0.028(5) 0.022(3) 0.055(9) -0.003(4) -0.025(5) 0.001(3) C34 0.056(6) 0.028(4) 0.038(6) -0.001(4) -0.004(4) -0.005(4) C35 0.059(6) 0.024(3) 0.042(6) -0.004(4) -0.008(5) -0.003(4) C36 0.060(6) 0.027(4) 0.044(6) 0.001(4) -0.017(5) 0.001(4) C37 0.030(4) 0.020(3) 0.050(7) -0.003(4) 0.001(5) -0.001(3) C38 0.064(7) 0.021(4) 0.067(8) 0.008(4) -0.027(6) -0.002(4) C39 0.067(7) 0.022(4) 0.082(10) 0.009(5) -0.018(6) -0.001(4) C40 0.049(5) 0.024(4) 0.046(6) 0.006(4) -0.014(5) 0.002(3) C41 0.071(9) 0.023(4) 0.051(9) -0.004(4) 0.002(7) -0.008(4) C42 0.037(4) 0.014(3) 0.054(6) 0.001(5) 0.001(4) 0.005(3) C43 0.067(8) 0.024(4) 0.038(8) -0.002(4) -0.029(6) 0.005(4) C44 0.048(6) 0.033(4) 0.039(6) 0.004(4) -0.009(4) 0.003(4) Co1 0.0357(8) 0.0239(5) 0.0324(9) -0.0004(4) 0.0021(8) -0.0028(4) Co2 0.0355(8) 0.0237(5) 0.0329(10) -0.0008(5) 0.0031(7) -0.0020(4) Cu1 0.0339(5) 0.0179(4) 0.0393(7) 0.0008(5) 0.0028(5) -0.0001(3) Cu2 0.0343(5) 0.0179(4) 0.0377(6) -0.0002(5) 0.0011(5) -0.0005(3) N1 0.020(3) 0.041(3) 0.037(5) 0.002(4) 0.002(3) -0.001(3) N2 0.036(4) 0.022(3) 0.029(4) -0.001(3) 0.001(4) 0.004(3) N3 0.055(4) 0.011(2) 0.050(5) -0.001(3) -0.005(4) -0.003(3) N4 0.037(4) 0.018(2) 0.046(5) 0.002(4) 0.002(4) 0.005(3) O1 0.057(4) 0.032(3) 0.046(5) -0.004(3) 0.015(4) -0.008(3) O2 0.030(4) 0.060(4) 0.064(6) -0.002(3) 0.003(3) -0.001(3) O3 0.055(4) 0.029(2) 0.041(4) -0.001(3) -0.003(3) -0.001(2) O4 0.032(4) 0.041(3) 0.084(6) -0.009(3) -0.014(4) -0.001(3) O5 0.038(3) 0.041(3) 0.068(5) -0.007(3) 0.004(3) 0.003(3) O6 0.042(3) 0.031(2) 0.028(4) -0.001(2) 0.007(3) 0.004(2) O7 0.069(5) 0.038(3) 0.040(5) -0.007(3) 0.015(4) -0.004(3) O8 0.039(5) 0.059(4) 0.080(7) 0.013(4) 0.012(4) 0.001(3) P1 0.0435(17) 0.0269(10) 0.062(2) -0.0057(10) -0.0077(16) 0.0005(8) P2 0.0480(18) 0.0274(10) 0.048(2) 0.0017(11) -0.0113(16) -0.0019(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.244(13) . ? C1 O2 1.266(12) . ? C1 C2 1.508(14) . ? C2 C6 1.431(15) . ? C2 C3 1.452(15) . ? C2 Co1 2.045(8) . ? C3 C4 1.406(16) . ? C3 Co1 2.016(9) . ? C3 H3 0.9500 . ? C4 C5 1.434(18) . ? C4 Co1 2.056(9) . ? C4 H4 0.9500 . ? C5 C6 1.450(14) . ? C5 Co1 2.044(9) . ? C5 H5 0.9500 . ? C6 Co1 2.058(8) . ? C6 H6 0.9500 . ? C7 O4 1.207(11) . ? C7 O3 1.259(12) . ? C7 C9 1.549(14) . ? C8 C9 1.392(16) . ? C8 C12 1.423(17) . ? C8 Co1 2.048(8) . ? C8 H8 0.9500 . ? C9 C10 1.430(15) . ? C9 Co1 2.054(9) . ? C10 C11 1.432(17) . ? C10 Co1 2.047(10) . ? C10 H10 0.9500 . ? C11 C12 1.483(18) . ? C11 Co1 2.052(9) . ? C11 H11 0.9500 . ? C12 Co1 2.044(9) . ? C12 H12 0.9500 . ? C13 O6 1.252(11) . ? C13 O5 1.262(9) . ? C13 C14 1.470(16) . ? C14 C18 1.424(16) . ? C14 C15 1.49(2) . ? C14 Co2 2.059(10) . ? C15 C16 1.40(2) . ? C15 Co2 2.031(11) . ? C15 H15 0.9500 . ? C16 C17 1.409(19) . ? C16 Co2 2.054(10) . ? C16 H16 0.9500 . ? C17 C18 1.403(16) . ? C17 Co2 2.024(10) . ? C17 H17 0.9500 . ? C18 Co2 2.037(11) . ? C18 H18 0.9500 . ? C19 O7 1.240(14) . ? C19 O8 1.252(13) . ? C19 C23 1.502(14) . ? C20 C21 1.413(19) . ? C20 C24 1.466(18) . ? C20 Co2 2.034(9) . ? C20 H20 0.9500 . ? C21 C22 1.383(16) . ? C21 Co2 2.027(11) . ? C21 H21 0.9500 . ? C22 C23 1.406(15) . ? C22 Co2 2.007(10) . ? C22 H22 0.9500 . ? C23 C24 1.418(14) . ? C23 Co2 2.026(9) . ? C24 Co2 2.037(9) . ? C24 H24 0.9500 . ? C25 N1 1.323(12) . ? C25 C26 1.381(11) . ? C25 H25 0.9500 . ? C26 C27 1.361(14) . ? C26 H26 0.9500 . ? C27 C28 1.396(15) . ? C27 C32 1.501(8) . ? C28 C29 1.360(12) . ? C28 H28 0.9500 . ? C29 N1 1.357(12) . ? C29 H29 0.9500 . ? C30 N2 1.328(13) . ? C30 C31 1.400(10) . ? C30 H30 0.9500 . ? C31 C32 1.328(16) . ? C31 H31 0.9500 . ? C32 C33 1.387(14) . ? C33 C34 1.397(10) . ? C33 H33 0.9500 . ? C34 N2 1.339(13) . ? C34 H34 0.9500 . ? C35 N3 1.333(13) . ? C35 C36 1.382(10) . ? C35 H35 0.9500 . ? C36 C37 1.397(15) . ? C36 H36 0.9500 . ? C37 C38 1.393(15) . ? C37 C42 1.492(8) . ? C38 C39 1.369(11) . ? C38 H38 0.9500 . ? C39 N3 1.315(14) . ? C39 H39 0.9500 . ? C40 N4 1.322(14) . ? C40 C41 1.381(10) . ? C40 H40 0.9500 . ? C41 C42 1.380(18) . ? C41 H41 0.9500 . ? C42 C43 1.414(16) . ? C43 C44 1.388(10) . ? C43 H43 0.9500 . ? C44 N4 1.349(13) . ? C44 H44 0.9500 . ? Cu1 N4 2.019(6) . ? Cu1 N3 2.034(5) 1_565 ? Cu1 O4 2.043(7) 4_465 ? Cu1 O1 2.068(7) . ? Cu1 O6 2.157(7) . ? Cu2 N2 2.019(6) . ? Cu2 N1 2.040(6) 1_565 ? Cu2 O5 2.041(7) . ? Cu2 O7 2.104(8) 4_465 ? Cu2 O3 2.133(7) 4_465 ? F1 P1 1.574(13) . ? F2 P1 1.641(13) . ? F3 P1 1.522(12) . ? F4 P1 1.604(11) . ? F5 P1 1.618(13) . ? F6 P1 1.603(11) . ? F1A P1 1.636(16) . ? F2A P1 1.631(17) . ? F3A P1 1.704(17) . ? F4A P1 1.585(13) . ? F5A P1 1.565(12) . ? F6A P1 1.473(16) . ? F7 P2 1.597(11) . ? F8 P2 1.592(12) . ? F9 P2 1.604(10) . ? F10 P2 1.560(11) . ? F11 P2 1.613(10) . ? F12 P2 1.636(11) . ? F7A P2 1.602(18) . ? F8A P2 1.646(19) . ? F9A P2 1.58(2) . ? F10A P2 1.567(16) . ? F11A P2 1.66(4) . ? F12A P2 1.552(17) . ? N1 Cu2 2.040(6) 1_545 ? N3 Cu1 2.034(5) 1_545 ? O3 Cu2 2.133(7) 4_565 ? O4 Cu1 2.043(7) 4_565 ? O7 Cu2 2.104(8) 4_565 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 126.9(10) . . ? O1 C1 C2 117.9(9) . . ? O2 C1 C2 115.2(10) . . ? C6 C2 C3 108.5(9) . . ? C6 C2 C1 125.8(9) . . ? C3 C2 C1 125.4(10) . . ? C6 C2 Co1 70.0(5) . . ? C3 C2 Co1 68.0(5) . . ? C1 C2 Co1 123.0(5) . . ? C4 C3 C2 107.8(10) . . ? C4 C3 Co1 71.3(6) . . ? C2 C3 Co1 70.2(5) . . ? C4 C3 H3 126.1 . . ? C2 C3 H3 126.1 . . ? Co1 C3 H3 124.0 . . ? C3 C4 C5 108.8(9) . . ? C3 C4 Co1 68.3(5) . . ? C5 C4 Co1 69.1(5) . . ? C3 C4 H4 125.6 . . ? C5 C4 H4 125.6 . . ? Co1 C4 H4 128.6 . . ? C4 C5 C6 108.1(9) . . ? C4 C5 Co1 70.0(6) . . ? C6 C5 Co1 69.8(5) . . ? C4 C5 H5 125.9 . . ? C6 C5 H5 125.9 . . ? Co1 C5 H5 125.9 . . ? C2 C6 C5 106.7(9) . . ? C2 C6 Co1 69.1(5) . . ? C5 C6 Co1 68.8(5) . . ? C2 C6 H6 126.6 . . ? C5 C6 H6 126.6 . . ? Co1 C6 H6 127.0 . . ? O4 C7 O3 129.5(10) . . ? O4 C7 C9 115.0(9) . . ? O3 C7 C9 115.4(8) . . ? C9 C8 C12 110.3(10) . . ? C9 C8 Co1 70.4(5) . . ? C12 C8 Co1 69.5(5) . . ? C9 C8 H8 124.9 . . ? C12 C8 H8 124.9 . . ? Co1 C8 H8 126.8 . . ? C8 C9 C10 108.2(10) . . ? C8 C9 C7 125.9(9) . . ? C10 C9 C7 125.9(9) . . ? C8 C9 Co1 69.9(5) . . ? C10 C9 Co1 69.3(5) . . ? C7 C9 Co1 127.1(5) . . ? C9 C10 C11 108.9(10) . . ? C9 C10 Co1 69.8(5) . . ? C11 C10 Co1 69.7(6) . . ? C9 C10 H10 125.5 . . ? C11 C10 H10 125.5 . . ? Co1 C10 H10 126.5 . . ? C10 C11 C12 106.2(10) . . ? C10 C11 Co1 69.4(5) . . ? C12 C11 Co1 68.5(5) . . ? C10 C11 H11 126.9 . . ? C12 C11 H11 126.9 . . ? Co1 C11 H11 126.8 . . ? C8 C12 C11 106.5(10) . . ? C8 C12 Co1 69.8(5) . . ? C11 C12 Co1 69.1(5) . . ? C8 C12 H12 126.7 . . ? C11 C12 H12 126.7 . . ? Co1 C12 H12 125.9 . . ? O6 C13 O5 125.3(9) . . ? O6 C13 C14 116.9(7) . . ? O5 C13 C14 117.8(9) . . ? C18 C14 C13 129.2(10) . . ? C18 C14 C15 105.5(11) . . ? C13 C14 C15 125.3(10) . . ? C18 C14 Co2 68.8(6) . . ? C13 C14 Co2 128.1(6) . . ? C15 C14 Co2 67.7(6) . . ? C16 C15 C14 108.0(13) . . ? C16 C15 Co2 70.9(7) . . ? C14 C15 Co2 69.7(6) . . ? C16 C15 H15 126.0 . . ? C14 C15 H15 126.0 . . ? Co2 C15 H15 125.0 . . ? C15 C16 C17 108.2(12) . . ? C15 C16 Co2 69.1(6) . . ? C17 C16 Co2 68.7(6) . . ? C15 C16 H16 125.9 . . ? C17 C16 H16 125.9 . . ? Co2 C16 H16 127.9 . . ? C18 C17 C16 109.5(11) . . ? C18 C17 Co2 70.3(6) . . ? C16 C17 Co2 70.9(6) . . ? C18 C17 H17 125.2 . . ? C16 C17 H17 125.2 . . ? Co2 C17 H17 125.2 . . ? C17 C18 C14 108.7(11) . . ? C17 C18 Co2 69.3(7) . . ? C14 C18 Co2 70.5(6) . . ? C17 C18 H18 125.6 . . ? C14 C18 H18 125.6 . . ? Co2 C18 H18 126.1 . . ? O7 C19 O8 124.8(10) . . ? O7 C19 C23 116.8(10) . . ? O8 C19 C23 118.4(10) . . ? C21 C20 C24 106.4(10) . . ? C21 C20 Co2 69.4(6) . . ? C24 C20 Co2 69.0(5) . . ? C21 C20 H20 126.8 . . ? C24 C20 H20 126.8 . . ? Co2 C20 H20 126.4 . . ? C22 C21 C20 109.1(12) . . ? C22 C21 Co2 69.2(6) . . ? C20 C21 Co2 69.9(7) . . ? C22 C21 H21 125.5 . . ? C20 C21 H21 125.5 . . ? Co2 C21 H21 127.0 . . ? C21 C22 C23 109.7(10) . . ? C21 C22 Co2 70.7(6) . . ? C23 C22 Co2 70.3(6) . . ? C21 C22 H22 125.2 . . ? C23 C22 H22 125.2 . . ? Co2 C22 H22 125.4 . . ? C22 C23 C24 107.8(9) . . ? C22 C23 C19 125.6(10) . . ? C24 C23 C19 126.5(10) . . ? C22 C23 Co2 68.9(5) . . ? C24 C23 Co2 70.0(5) . . ? C19 C23 Co2 124.2(5) . . ? C23 C24 C20 107.0(10) . . ? C23 C24 Co2 69.2(5) . . ? C20 C24 Co2 68.8(5) . . ? C23 C24 H24 126.5 . . ? C20 C24 H24 126.5 . . ? Co2 C24 H24 127.1 . . ? N1 C25 C26 121.2(9) . . ? N1 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C27 C26 C25 122.2(9) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 115.0(7) . . ? C26 C27 C32 123.3(9) . . ? C28 C27 C32 121.7(9) . . ? C29 C28 C27 121.9(9) . . ? C29 C28 H28 119.1 . . ? C27 C28 H28 119.1 . . ? N1 C29 C28 120.8(9) . . ? N1 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? N2 C30 C31 121.3(10) . . ? N2 C30 H30 119.3 . . ? C31 C30 H30 119.3 . . ? C32 C31 C30 122.7(10) . . ? C32 C31 H31 118.6 . . ? C30 C31 H31 118.6 . . ? C31 C32 C33 116.5(7) . . ? C31 C32 C27 120.9(9) . . ? C33 C32 C27 122.6(9) . . ? C32 C33 C34 119.2(9) . . ? C32 C33 H33 120.4 . . ? C34 C33 H33 120.4 . . ? N2 C34 C33 123.2(9) . . ? N2 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? N3 C35 C36 123.4(9) . . ? N3 C35 H35 118.3 . . ? C36 C35 H35 118.3 . . ? C35 C36 C37 120.3(9) . . ? C35 C36 H36 119.9 . . ? C37 C36 H36 119.9 . . ? C38 C37 C36 114.6(6) . . ? C38 C37 C42 123.3(10) . . ? C36 C37 C42 122.1(9) . . ? C39 C38 C37 120.9(10) . . ? C39 C38 H38 119.5 . . ? C37 C38 H38 119.5 . . ? N3 C39 C38 123.8(10) . . ? N3 C39 H39 118.1 . . ? C38 C39 H39 118.1 . . ? N4 C40 C41 121.4(10) . . ? N4 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 121.8(12) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C43 117.1(7) . . ? C41 C42 C37 122.3(10) . . ? C43 C42 C37 120.6(9) . . ? C44 C43 C42 117.2(10) . . ? C44 C43 H43 121.4 . . ? C42 C43 H43 121.4 . . ? N4 C44 C43 124.2(10) . . ? N4 C44 H44 117.9 . . ? C43 C44 H44 117.9 . . ? C3 Co1 C12 162.4(5) . . ? C3 Co1 C5 69.3(4) . . ? C12 Co1 C5 105.9(5) . . ? C3 Co1 C2 41.9(4) . . ? C12 Co1 C2 153.8(5) . . ? C5 Co1 C2 68.9(4) . . ? C3 Co1 C10 120.5(4) . . ? C12 Co1 C10 69.5(5) . . ? C5 Co1 C10 161.5(5) . . ? C2 Co1 C10 107.0(5) . . ? C3 Co1 C8 126.1(5) . . ? C12 Co1 C8 40.7(5) . . ? C5 Co1 C8 120.9(4) . . ? C2 Co1 C8 163.8(5) . . ? C10 Co1 C8 67.9(4) . . ? C3 Co1 C11 154.3(5) . . ? C12 Co1 C11 42.4(5) . . ? C5 Co1 C11 123.7(5) . . ? C2 Co1 C11 117.8(4) . . ? C10 Co1 C11 40.9(5) . . ? C8 Co1 C11 69.2(4) . . ? C3 Co1 C9 108.4(4) . . ? C12 Co1 C9 68.6(4) . . ? C5 Co1 C9 155.7(4) . . ? C2 Co1 C9 126.6(4) . . ? C10 Co1 C9 40.8(4) . . ? C8 Co1 C9 39.7(4) . . ? C11 Co1 C9 69.1(4) . . ? C3 Co1 C4 40.4(4) . . ? C12 Co1 C4 125.2(5) . . ? C5 Co1 C4 40.9(5) . . ? C2 Co1 C4 68.5(4) . . ? C10 Co1 C4 156.0(5) . . ? C8 Co1 C4 109.5(4) . . ? C11 Co1 C4 162.6(6) . . ? C9 Co1 C4 121.7(4) . . ? C3 Co1 C6 70.1(4) . . ? C12 Co1 C6 118.2(4) . . ? C5 Co1 C6 41.4(4) . . ? C2 Co1 C6 40.8(4) . . ? C10 Co1 C6 123.8(4) . . ? C8 Co1 C6 154.9(5) . . ? C11 Co1 C6 104.3(4) . . ? C9 Co1 C6 162.4(4) . . ? C4 Co1 C6 69.2(4) . . ? C22 Co2 C17 106.5(4) . . ? C22 Co2 C23 40.8(4) . . ? C17 Co2 C23 122.3(5) . . ? C22 Co2 C21 40.1(5) . . ? C17 Co2 C21 121.1(5) . . ? C23 Co2 C21 68.5(4) . . ? C22 Co2 C15 156.1(6) . . ? C17 Co2 C15 68.2(5) . . ? C23 Co2 C15 161.7(6) . . ? C21 Co2 C15 121.1(6) . . ? C22 Co2 C20 68.6(4) . . ? C17 Co2 C20 156.9(5) . . ? C23 Co2 C20 69.6(4) . . ? C21 Co2 C20 40.7(5) . . ? C15 Co2 C20 106.7(5) . . ? C22 Co2 C24 68.7(4) . . ? C17 Co2 C24 159.1(5) . . ? C23 Co2 C24 40.8(4) . . ? C21 Co2 C24 69.1(5) . . ? C15 Co2 C24 124.5(5) . . ? C20 Co2 C24 42.2(5) . . ? C22 Co2 C18 122.6(4) . . ? C17 Co2 C18 40.4(4) . . ? C23 Co2 C18 108.0(5) . . ? C21 Co2 C18 157.3(5) . . ? C15 Co2 C18 69.4(5) . . ? C20 Co2 C18 161.1(5) . . ? C24 Co2 C18 123.8(5) . . ? C22 Co2 C16 120.9(5) . . ? C17 Co2 C16 40.4(5) . . ? C23 Co2 C16 157.4(5) . . ? C21 Co2 C16 105.9(5) . . ? C15 Co2 C16 40.0(6) . . ? C20 Co2 C16 121.3(5) . . ? C24 Co2 C16 159.7(5) . . ? C18 Co2 C16 68.3(5) . . ? C22 Co2 C14 159.3(4) . . ? C17 Co2 C14 68.5(4) . . ? C23 Co2 C14 123.6(4) . . ? C21 Co2 C14 159.8(5) . . ? C15 Co2 C14 42.6(5) . . ? C20 Co2 C14 124.0(5) . . ? C24 Co2 C14 108.4(5) . . ? C18 Co2 C14 40.7(4) . . ? C16 Co2 C14 69.1(5) . . ? N4 Cu1 N3 177.9(5) . 1_565 ? N4 Cu1 O4 88.9(3) . 4_465 ? N3 Cu1 O4 89.5(3) 1_565 4_465 ? N4 Cu1 O1 89.8(3) . . ? N3 Cu1 O1 90.4(3) 1_565 . ? O4 Cu1 O1 138.3(4) 4_465 . ? N4 Cu1 O6 91.2(4) . . ? N3 Cu1 O6 90.9(3) 1_565 . ? O4 Cu1 O6 130.9(3) 4_465 . ? O1 Cu1 O6 90.7(3) . . ? N2 Cu2 N1 178.5(4) . 1_565 ? N2 Cu2 O5 90.8(3) . . ? N1 Cu2 O5 88.1(3) 1_565 . ? N2 Cu2 O7 89.2(3) . 4_465 ? N1 Cu2 O7 91.1(3) 1_565 4_465 ? O5 Cu2 O7 141.4(3) . 4_465 ? N2 Cu2 O3 92.1(3) . 4_465 ? N1 Cu2 O3 89.4(3) 1_565 4_465 ? O5 Cu2 O3 126.2(3) . 4_465 ? O7 Cu2 O3 92.4(3) 4_465 4_465 ? C25 N1 C29 118.7(7) . . ? C25 N1 Cu2 121.3(6) . 1_545 ? C29 N1 Cu2 120.0(6) . 1_545 ? C30 N2 C34 116.9(6) . . ? C30 N2 Cu2 120.8(6) . . ? C34 N2 Cu2 122.0(7) . . ? C39 N3 C35 116.6(7) . . ? C39 N3 Cu1 122.0(7) . 1_545 ? C35 N3 Cu1 121.4(7) . 1_545 ? C40 N4 C44 118.2(6) . . ? C40 N4 Cu1 122.4(7) . . ? C44 N4 Cu1 119.2(7) . . ? C1 O1 Cu1 101.2(7) . . ? C7 O3 Cu2 122.4(6) . 4_565 ? C7 O4 Cu1 158.6(8) . 4_565 ? C13 O5 Cu2 161.5(7) . . ? C13 O6 Cu1 120.6(5) . . ? C19 O7 Cu2 99.1(7) . 4_565 ? F6A P1 F3 126.0(8) . . ? F6A P1 F5A 96.5(8) . . ? F3 P1 F5A 102.5(6) . . ? F6A P1 F1 74.0(8) . . ? F3 P1 F1 88.0(7) . . ? F5A P1 F1 41.5(6) . . ? F6A P1 F4A 94.0(8) . . ? F3 P1 F4A 135.4(8) . . ? F5A P1 F4A 90.1(7) . . ? F1 P1 F4A 125.4(7) . . ? F6A P1 F6 133.5(8) . . ? F3 P1 F6 96.5(6) . . ? F5A P1 F6 51.8(6) . . ? F1 P1 F6 91.6(7) . . ? F4A P1 F6 58.7(6) . . ? F6A P1 F4 104.9(7) . . ? F3 P1 F4 93.3(6) . . ? F5A P1 F4 138.4(6) . . ? F1 P1 F4 178.7(6) . . ? F4A P1 F4 53.7(6) . . ? F6 P1 F4 88.6(6) . . ? F6A P1 F5 42.0(7) . . ? F3 P1 F5 89.3(7) . . ? F5A P1 F5 128.7(7) . . ? F1 P1 F5 90.4(7) . . ? F4A P1 F5 115.7(7) . . ? F6 P1 F5 173.9(6) . . ? F4 P1 F5 89.2(6) . . ? F6A P1 F2A 88.6(9) . . ? F3 P1 F2A 73.5(7) . . ? F5A P1 F2A 174.9(8) . . ? F1 P1 F2A 140.1(8) . . ? F4A P1 F2A 90.6(8) . . ? F6 P1 F2A 124.8(8) . . ? F4 P1 F2A 40.2(6) . . ? F5 P1 F2A 55.2(7) . . ? F6A P1 F1A 91.8(9) . . ? F3 P1 F1A 39.0(7) . . ? F5A P1 F1A 90.0(7) . . ? F1 P1 F1A 57.1(8) . . ? F4A P1 F1A 174.2(9) . . ? F6 P1 F1A 117.4(7) . . ? F4 P1 F1A 123.8(8) . . ? F5 P1 F1A 68.4(7) . . ? F2A P1 F1A 88.7(8) . . ? F6A P1 F2 51.9(7) . . ? F3 P1 F2 177.6(8) . . ? F5A P1 F2 77.0(6) . . ? F1 P1 F2 90.1(7) . . ? F4A P1 F2 47.0(7) . . ? F6 P1 F2 85.1(6) . . ? F4 P1 F2 88.6(6) . . ? F5 P1 F2 89.2(7) . . ? F2A P1 F2 107.1(7) . . ? F1A P1 F2 138.5(9) . . ? F6A P1 F3A 171.4(8) . . ? F3 P1 F3A 48.4(7) . . ? F5A P1 F3A 91.4(7) . . ? F1 P1 F3A 110.3(7) . . ? F4A P1 F3A 89.4(8) . . ? F6 P1 F3A 54.7(7) . . ? F4 P1 F3A 70.8(7) . . ? F5 P1 F3A 129.6(8) . . ? F2A P1 F3A 83.5(8) . . ? F1A P1 F3A 84.9(8) . . ? F2 P1 F3A 133.9(7) . . ? F12A P2 F10 74.1(8) . . ? F12A P2 F10A 90.3(9) . . ? F10 P2 F10A 125.6(8) . . ? F12A P2 F9A 94.1(11) . . ? F10 P2 F9A 37.5(9) . . ? F10A P2 F9A 95.0(11) . . ? F12A P2 F8 65.6(8) . . ? F10 P2 F8 93.4(6) . . ? F10A P2 F8 35.2(6) . . ? F9A P2 F8 72.9(9) . . ? F12A P2 F7 149.8(9) . . ? F10 P2 F7 89.7(6) . . ? F10A P2 F7 78.4(7) . . ? F9A P2 F7 59.7(10) . . ? F8 P2 F7 90.7(6) . . ? F12A P2 F7A 177.6(9) . . ? F10 P2 F7A 108.2(8) . . ? F10A P2 F7A 88.3(9) . . ? F9A P2 F7A 88.0(11) . . ? F8 P2 F7A 113.9(9) . . ? F7 P2 F7A 31.5(8) . . ? F12A P2 F9 32.4(7) . . ? F10 P2 F9 92.1(6) . . ? F10A P2 F9 101.6(7) . . ? F9A P2 F9 122.5(10) . . ? F8 P2 F9 90.6(6) . . ? F7 P2 F9 177.7(6) . . ? F7A P2 F9 146.3(9) . . ? F12A P2 F11 105.0(7) . . ? F10 P2 F11 175.1(7) . . ? F10A P2 F11 59.0(7) . . ? F9A P2 F11 147.1(11) . . ? F8 P2 F11 90.6(6) . . ? F7 P2 F11 93.2(5) . . ? F7A P2 F11 72.7(8) . . ? F9 P2 F11 84.9(5) . . ? F12A P2 F12 112.9(8) . . ? F10 P2 F12 87.7(5) . . ? F10A P2 F12 144.5(7) . . ? F9A P2 F12 108.9(9) . . ? F8 P2 F12 177.8(5) . . ? F7 P2 F12 91.2(5) . . ? F7A P2 F12 67.5(9) . . ? F9 P2 F12 87.5(5) . . ? F11 P2 F12 88.3(5) . . ? F12A P2 F8A 90.8(9) . . ? F10 P2 F8A 55.3(8) . . ? F10A P2 F8A 178.7(9) . . ? F9A P2 F8A 85.4(11) . . ? F8 P2 F8A 146.0(8) . . ? F7 P2 F8A 100.8(7) . . ? F7A P2 F8A 90.6(10) . . ? F9 P2 F8A 79.1(8) . . ? F11 P2 F8A 120.2(8) . . ? F12 P2 F8A 34.3(7) . . ? F12A P2 F11A 89.5(14) . . ? F10 P2 F11A 137.3(14) . . ? F10A P2 F11A 92.8(15) . . ? F9A P2 F11A 171.4(15) . . ? F8 P2 F11A 115.7(13) . . ? F7 P2 F11A 118.7(13) . . ? F7A P2 F11A 88.7(14) . . ? F9 P2 F11A 59.0(12) . . ? F11 P2 F11A 37.8(13) . . ? F12 P2 F11A 62.5(13) . . ? F8A P2 F11A 86.7(15) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.459 _refine_diff_density_min -0.592 _refine_diff_density_rms 0.106 _database_code_depnum_ccdc_archive 'CCDC 950064'