# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Chuan-De Wu' _publ_contact_author_email cdwu@zju.edu.cn loop_ _publ_author_name 'Chao Zou' 'Ming-Hua Xie' 'Guo-Qiang Kong' 'Chuan-De Wu' data_New1 _database_code_depnum_ccdc_archive 'CCDC 871466' #TrackingRef '- New1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H24 N4 O8 Pb2' _chemical_formula_weight 1199.09 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.3484(6) _cell_length_b 6.9216(3) _cell_length_c 27.1086(13) _cell_angle_alpha 90.00 _cell_angle_beta 99.924(4) _cell_angle_gamma 90.00 _cell_volume 2836.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 12013 _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 25.35 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 5.972 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.125 _exptl_absorpt_correction_T_max 0.550 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 12013 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_sigmaI/netI 0.0597 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.35 _reflns_number_total 5194 _reflns_number_gt 3880 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.033 0.000 279 61 ' ' 2 0.500 -0.036 0.250 284 60 ' ' 3 0.000 -0.021 0.500 279 61 ' ' 4 0.500 -0.045 0.750 284 60 ' ' _platon_squeeze_details ; ; _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^)+(0.0438P)^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 5194 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0592 _refine_ls_R_factor_gt 0.0399 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0921 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Pb1 Pb 0.059404(16) 0.86549(3) 0.239874(9) 0.04039(11) Uani 1 1 d . . . O5 O -0.0882(3) 0.9828(6) 0.25763(18) 0.0459(11) Uani 1 1 d . . . O4 O -0.0867(3) 1.8839(6) 0.69685(18) 0.0525(13) Uani 1 1 d . . . C20 C -0.5754(5) 1.3798(10) 0.6108(3) 0.056(2) Uani 1 1 d . . . H20A H -0.6118 1.4168 0.6332 0.068 Uiso 1 1 calc R . . N2 N -0.5205(4) 1.2087(7) 0.5509(2) 0.0407(13) Uani 1 1 d . . . C19 C -0.2805(4) 0.8998(10) 0.3887(3) 0.0421(16) Uani 1 1 d . . . N1 N -0.3896(3) 1.1450(7) 0.4867(2) 0.0406(13) Uani 1 1 d . . . O3 O -0.1802(4) 2.1165(7) 0.6782(3) 0.094(2) Uani 1 1 d . . . C18 C -0.3456(4) 0.9260(9) 0.4239(3) 0.0412(16) Uani 1 1 d . . . C17 C -0.3281(4) 1.5545(8) 0.5787(2) 0.0372(15) Uani 1 1 d . . . C16 C -0.3531(4) 1.3089(9) 0.5119(3) 0.0412(16) Uani 1 1 d . . . C15 C -0.3444(5) 1.7502(10) 0.5749(3) 0.064(2) Uani 1 1 d . . . H15A H -0.3927 1.7963 0.5525 0.077 Uiso 1 1 calc R . . C14 C -0.3867(4) 1.4064(9) 0.5492(3) 0.0409(16) Uani 1 1 d . . . C13 C -0.1986(5) 1.6210(9) 0.6399(3) 0.055(2) Uani 1 1 d . . . H13A H -0.1494 1.5743 0.6615 0.066 Uiso 1 1 calc R . . C12 C -0.4663(4) 1.3665(9) 0.5663(2) 0.0409(16) Uani 1 1 d . . . C11 C -0.2154(4) 1.8142(9) 0.6379(3) 0.0444(17) Uani 1 1 d . . . C10 C -0.2218(5) 0.7479(9) 0.3929(3) 0.0433(16) Uani 1 1 d . . . H10A H -0.2239 0.6544 0.4173 0.052 Uiso 1 1 calc R . . C9 C -0.3357(4) 1.0912(9) 0.4535(3) 0.0412(16) Uani 1 1 d . . . C8 C -0.2632(5) 1.2298(11) 0.4582(3) 0.0511(18) Uani 1 1 d . . . H8A H -0.2173 1.2302 0.4398 0.061 Uiso 1 1 calc R . . C7 C -0.1603(5) 0.7315(10) 0.3619(3) 0.0466(17) Uani 1 1 d . . . H7A H -0.1205 0.6291 0.3660 0.056 Uiso 1 1 calc R . . C6 C -0.5884(4) 1.2123(10) 0.5775(3) 0.0432(16) Uani 1 1 d . . . C5 C -0.2540(5) 1.4936(9) 0.6103(3) 0.053(2) Uani 1 1 d . . . H5A H -0.2404 1.3625 0.6118 0.064 Uiso 1 1 calc R . . C4 C -0.2746(5) 1.3557(10) 0.4938(3) 0.0509(18) Uani 1 1 d . . . H4A H -0.2370 1.4578 0.5050 0.061 Uiso 1 1 calc R . . C3 C -0.5022(5) 1.4701(11) 0.6033(3) 0.053(2) Uani 1 1 d . . . H3A H -0.4787 1.5817 0.6195 0.064 Uiso 1 1 calc R . . C2 C -0.2774(5) 1.0345(11) 0.3506(3) 0.0516(18) Uani 1 1 d . . . H2A H -0.3168 1.1378 0.3466 0.062 Uiso 1 1 calc R . . C1 C -0.2884(5) 1.8791(10) 0.6046(3) 0.067(2) Uani 1 1 d . . . H1A H -0.3003 2.0108 0.6021 0.081 Uiso 1 1 calc R . . C22 C -0.1574(4) 0.8675(9) 0.3244(2) 0.0369(15) Uani 1 1 d . . . C23 C -0.2170(5) 1.0160(9) 0.3190(3) 0.0449(17) Uani 1 1 d . . . H23A H -0.2167 1.1059 0.2935 0.054 Uiso 1 1 calc R . . C21 C -0.1575(5) 1.9486(9) 0.6733(3) 0.0477(18) Uani 1 1 d . . . O1 O -0.0277(3) 0.7303(6) 0.30041(17) 0.0413(11) Uani 1 1 d . . . C24 C -0.0873(4) 0.8612(9) 0.2916(2) 0.0363(15) 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 Pb1 0.04678(18) 0.03189(15) 0.04450(18) -0.00104(11) 0.01354(12) 0.00041(11) O5 0.049(3) 0.042(2) 0.047(3) 0.006(2) 0.011(2) -0.007(2) O4 0.053(3) 0.044(3) 0.052(3) -0.002(2) -0.013(2) -0.005(2) C20 0.061(5) 0.059(5) 0.052(5) -0.016(4) 0.020(4) -0.011(4) N2 0.049(3) 0.039(3) 0.035(3) -0.006(2) 0.011(3) -0.013(3) C19 0.038(4) 0.049(4) 0.042(4) -0.006(3) 0.013(3) -0.006(3) N1 0.040(3) 0.043(3) 0.040(3) -0.006(3) 0.007(2) -0.006(3) O3 0.070(4) 0.041(3) 0.149(6) -0.023(3) -0.045(4) 0.004(3) C18 0.038(4) 0.045(4) 0.042(4) 0.001(3) 0.008(3) -0.007(3) C17 0.043(4) 0.034(3) 0.036(4) -0.006(3) 0.009(3) -0.007(3) C16 0.042(4) 0.040(3) 0.040(4) -0.002(3) 0.002(3) -0.005(3) C15 0.048(4) 0.043(4) 0.084(6) 0.007(4) -0.034(4) -0.017(4) C14 0.040(4) 0.036(3) 0.043(4) -0.003(3) -0.001(3) -0.012(3) C13 0.068(5) 0.040(4) 0.048(4) -0.007(3) -0.016(4) 0.006(4) C12 0.045(4) 0.039(4) 0.038(4) 0.000(3) 0.004(3) -0.008(3) C11 0.044(4) 0.045(4) 0.040(4) -0.001(3) -0.003(3) -0.008(3) C10 0.056(4) 0.039(4) 0.038(4) 0.004(3) 0.017(3) -0.001(3) C9 0.039(4) 0.045(4) 0.041(4) -0.003(3) 0.008(3) -0.009(3) C8 0.042(4) 0.061(4) 0.051(5) -0.005(4) 0.011(3) -0.021(4) C7 0.051(4) 0.041(4) 0.049(5) -0.002(3) 0.013(4) 0.001(3) C6 0.041(4) 0.051(4) 0.039(4) -0.004(3) 0.012(3) -0.005(3) C5 0.061(5) 0.032(3) 0.058(5) -0.005(3) -0.013(4) -0.005(3) C4 0.050(4) 0.047(4) 0.057(5) -0.010(4) 0.014(4) -0.024(4) C3 0.054(5) 0.052(4) 0.056(5) -0.021(4) 0.018(4) -0.014(4) C2 0.053(4) 0.052(4) 0.052(5) 0.007(4) 0.016(4) 0.005(4) C1 0.064(5) 0.040(4) 0.085(6) -0.002(4) -0.025(5) 0.005(4) C22 0.039(4) 0.036(3) 0.039(4) -0.008(3) 0.015(3) -0.007(3) C23 0.056(4) 0.043(4) 0.039(4) 0.006(3) 0.017(3) -0.001(3) C21 0.048(4) 0.033(4) 0.055(5) -0.003(3) -0.011(4) -0.009(3) O1 0.048(3) 0.034(2) 0.044(3) 0.000(2) 0.013(2) -0.003(2) C24 0.039(4) 0.037(3) 0.033(4) -0.007(3) 0.006(3) 0.002(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 Pb1 O4 2.424(4) 3_586 ? Pb1 O1 2.472(4) . ? Pb1 O5 2.530(5) . ? Pb1 O3 2.640(6) 3_586 ? Pb1 O5 2.684(4) 2_545 ? Pb1 C24 2.850(6) . ? O5 C24 1.246(7) . ? O5 Pb1 2.684(4) 2 ? O4 C21 1.244(8) . ? O4 Pb1 2.424(4) 3_586 ? C20 C3 1.331(10) . ? C20 C6 1.461(9) . ? N2 C6 1.367(8) . ? N2 C12 1.394(8) . ? C19 C10 1.376(9) . ? C19 C2 1.399(9) . ? C19 C18 1.506(9) . ? N1 C9 1.373(9) . ? N1 C16 1.391(8) . ? O3 C21 1.227(8) . ? O3 Pb1 2.640(6) 3_586 ? C18 C6 1.390(9) 3_476 ? C18 C9 1.391(9) . ? C17 C5 1.367(9) . ? C17 C15 1.378(9) . ? C17 C14 1.501(8) . ? C16 C14 1.387(10) . ? C16 C4 1.413(10) . ? C15 C1 1.395(9) . ? C14 C12 1.408(9) . ? C13 C11 1.361(9) . ? C13 C5 1.382(9) . ? C12 C3 1.419(10) . ? C11 C1 1.387(9) . ? C11 C21 1.511(9) . ? C10 C7 1.373(10) . ? C9 C8 1.458(9) . ? C8 C4 1.334(10) . ? C7 C22 1.394(9) . ? C6 C18 1.390(9) 3_476 ? C2 C23 1.373(10) . ? C22 C23 1.368(9) . ? C22 C24 1.510(9) . ? O1 C24 1.280(7) . ? 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 O4 Pb1 O1 81.28(16) 3_586 . ? O4 Pb1 O5 71.77(15) 3_586 . ? O1 Pb1 O5 52.45(15) . . ? O4 Pb1 O3 50.22(16) 3_586 3_586 ? O1 Pb1 O3 80.9(2) . 3_586 ? O5 Pb1 O3 110.3(2) . 3_586 ? O4 Pb1 O5 132.87(15) 3_586 2_545 ? O1 Pb1 O5 73.48(14) . 2_545 ? O5 Pb1 O5 117.46(13) . 2_545 ? O3 Pb1 O5 86.36(14) 3_586 2_545 ? O4 Pb1 C24 73.41(17) 3_586 . ? O1 Pb1 C24 26.63(15) . . ? O5 Pb1 C24 25.91(15) . . ? O3 Pb1 C24 95.0(2) 3_586 . ? O5 Pb1 C24 96.78(16) 2_545 . ? C24 O5 Pb1 91.5(4) . . ? C24 O5 Pb1 131.9(4) . 2 ? Pb1 O5 Pb1 99.92(15) . 2 ? C21 O4 Pb1 97.7(4) . 3_586 ? C3 C20 C6 107.9(6) . . ? C6 N2 C12 107.2(5) . . ? C10 C19 C2 117.7(6) . . ? C10 C19 C18 122.4(6) . . ? C2 C19 C18 119.9(6) . . ? C9 N1 C16 107.8(5) . . ? C21 O3 Pb1 87.9(4) . 3_586 ? C6 C18 C9 126.1(6) 3_476 . ? C6 C18 C19 117.4(6) 3_476 . ? C9 C18 C19 116.5(6) . . ? C5 C17 C15 118.1(6) . . ? C5 C17 C14 118.7(6) . . ? C15 C17 C14 123.2(6) . . ? C14 C16 N1 125.9(6) . . ? C14 C16 C4 125.9(6) . . ? N1 C16 C4 108.2(6) . . ? C17 C15 C1 120.0(6) . . ? C16 C14 C12 126.8(6) . . ? C16 C14 C17 117.3(6) . . ? C12 C14 C17 115.5(6) . . ? C11 C13 C5 120.7(6) . . ? N2 C12 C14 124.2(6) . . ? N2 C12 C3 108.9(6) . . ? C14 C12 C3 126.9(6) . . ? C13 C11 C1 118.0(6) . . ? C13 C11 C21 119.6(6) . . ? C1 C11 C21 122.3(6) . . ? C7 C10 C19 121.5(6) . . ? N1 C9 C18 125.6(6) . . ? N1 C9 C8 107.5(6) . . ? C18 C9 C8 126.7(6) . . ? C4 C8 C9 107.4(6) . . ? C10 C7 C22 120.2(6) . . ? N2 C6 C18 126.2(6) . 3_476 ? N2 C6 C20 107.8(6) . . ? C18 C6 C20 125.8(6) 3_476 . ? C17 C5 C13 121.9(6) . . ? C8 C4 C16 109.1(6) . . ? C20 C3 C12 108.1(6) . . ? C23 C2 C19 120.8(7) . . ? C11 C1 C15 121.1(6) . . ? C23 C22 C7 118.7(6) . . ? C23 C22 C24 119.4(6) . . ? C7 C22 C24 121.8(6) . . ? C22 C23 C2 121.0(7) . . ? O3 C21 O4 121.7(6) . . ? O3 C21 C11 120.3(6) . . ? O4 C21 C11 118.0(6) . . ? C24 O1 Pb1 93.4(4) . . ? O5 C24 O1 122.3(6) . . ? O5 C24 C22 119.8(6) . . ? O1 C24 C22 118.0(6) . . ? O5 C24 Pb1 62.6(3) . . ? O1 C24 Pb1 60.0(3) . . ? C22 C24 Pb1 173.2(4) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.367 _refine_diff_density_min -1.062 _refine_diff_density_rms 0.132 # Attachment '- New2.cif' data_New2 _database_code_depnum_ccdc_archive 'CCDC 871467' #TrackingRef '- New2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H33 Co N5 O10 Pb2' _chemical_formula_weight 1349.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1613(9) _cell_length_b 24.1334(12) _cell_length_c 20.5794(15) _cell_angle_alpha 90.00 _cell_angle_beta 91.020(7) _cell_angle_gamma 90.00 _cell_volume 5542.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21037 _cell_measurement_theta_min 3.09 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.617 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2580 _exptl_absorpt_coefficient_mu 6.412 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.159 _exptl_absorpt_correction_T_max 0.527 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 21037 _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_sigmaI/netI 0.1071 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 25.06 _reflns_number_total 9706 _reflns_number_gt 4530 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.032 0.722 0.224 356 50 ' ' 2 -0.035 0.222 0.276 356 50 ' ' 3 0.030 0.778 0.724 356 50 ' ' 4 -0.035 0.278 0.776 356 50 ' ' _platon_squeeze_details ; ; _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^)+(0.0479P)^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 9706 _refine_ls_number_parameters 597 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1526 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1776 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _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 Pb1 Pb 0.66288(6) 0.45441(2) 0.47850(3) 0.0885(2) Uani 1 1 d . . . Pb2 Pb 1.98483(6) 0.43075(2) -0.44041(3) 0.0957(3) Uani 1 1 d . . . Co1 Co 1.2869(2) 0.44954(7) 0.00130(10) 0.0903(6) Uani 1 1 d . . . O1 O 1.7539(12) 0.4695(4) -0.4013(5) 0.110(4) Uani 1 1 d . . . O2 O 1.8774(14) 0.4189(5) -0.3430(5) 0.118(4) Uani 1 1 d . . . O3 O 1.2004(13) 0.8560(4) -0.0198(6) 0.118(4) Uani 1 1 d . . . O4 O 1.0243(13) 0.8333(4) -0.0567(6) 0.114(4) Uani 1 1 d . . . O5 O 0.7242(16) 0.4559(5) 0.3647(6) 0.123(4) Uani 1 1 d . . . O6 O 0.8908(12) 0.4546(4) 0.4242(6) 0.107(4) Uani 1 1 d . . . O7 O 1.2450(11) 0.0472(4) 0.0105(5) 0.092(3) Uani 1 1 d . . . O8 O 1.4348(10) 0.0469(4) 0.0433(5) 0.096(3) Uani 1 1 d . . . O9 O 2.1393(11) 0.4077(5) -0.3561(7) 0.146(5) Uani 1 1 d . . . N1 N 1.3519(14) 0.5085(4) -0.0555(6) 0.103(4) Uani 1 1 d . . . N2 N 1.2380(13) 0.3938(4) 0.0656(6) 0.098(4) Uani 1 1 d . . . N3 N 1.3841(13) 0.3936(4) -0.0449(6) 0.097(4) Uani 1 1 d . . . N4 N 1.1804(14) 0.5041(4) 0.0446(6) 0.109(5) Uani 1 1 d . . . C1 C 1.471(2) 0.5560(8) -0.1253(10) 0.133(7) Uani 1 1 d . . . H1A H 1.5279 0.5637 -0.1563 0.159 Uiso 1 1 calc R . . C2 C 1.2055(18) 0.6483(6) -0.0255(8) 0.096(5) Uani 1 1 d . . . C3 C 1.518(2) 0.4713(8) -0.2423(10) 0.142(8) Uani 1 1 d . . . H3A H 1.4416 0.4863 -0.2454 0.171 Uiso 1 1 calc R . . C4 C 1.1601(19) 0.5564(6) 0.0245(9) 0.113(6) Uani 1 1 d . . . C5 C 1.4354(16) 0.5025(6) -0.0998(8) 0.098(5) Uani 1 1 d . . . C6 C 1.3277(17) 0.5634(5) -0.0503(8) 0.095(5) Uani 1 1 d . . . C7 C 1.0389(18) 0.5425(6) 0.1068(9) 0.117(6) Uani 1 1 d . . . H7A H 0.9796 0.5464 0.1377 0.140 Uiso 1 1 calc R . . C8 C 1.2685(15) 0.3389(5) 0.0656(7) 0.092(4) Uani 1 1 d . . . C9 C 1.1505(17) 0.7603(6) -0.0357(8) 0.100(5) Uani 1 1 d . . . C10 C 1.1707(15) 0.4016(5) 0.1209(7) 0.089(4) Uani 1 1 d . . . C11 C 1.2342(16) 0.5881(6) -0.0187(7) 0.093(5) Uani 1 1 d . . . C12 C 1.4387(16) 0.3100(6) -0.0870(9) 0.109(6) Uani 1 1 d . . . H12A H 1.4465 0.2718 -0.0916 0.131 Uiso 1 1 calc R . . C13 C 1.1071(19) 0.4964(6) 0.0958(8) 0.121(7) Uani 1 1 d . . . C14 C 1.3785(15) 0.3379(5) -0.0370(7) 0.091(5) Uani 1 1 d . . . C15 C 1.1682(17) 0.3502(6) 0.1570(9) 0.116(6) Uani 1 1 d . . . H15A H 1.1308 0.3445 0.1965 0.139 Uiso 1 1 calc R . . C16 C 1.2607(16) 0.7432(6) -0.0075(8) 0.097(5) Uani 1 1 d . . . H16A H 1.3138 0.7691 0.0100 0.116 Uiso 1 1 calc R . . C17 C 1.586(2) 0.4677(8) -0.2991(9) 0.124(6) Uani 1 1 d . . . H17A H 1.5552 0.4789 -0.3392 0.149 Uiso 1 1 calc R . . C18 C 1.773(2) 0.4438(7) -0.3522(11) 0.104(6) Uani 1 1 d . . . C19 C 1.0700(16) 0.7208(6) -0.0556(9) 0.107(5) Uani 1 1 d . . . H19A H 0.9962 0.7314 -0.0732 0.128 Uiso 1 1 calc R . . C20 C 1.4801(18) 0.4530(6) -0.1260(8) 0.110(6) Uani 1 1 d . . . C21 C 1.2882(15) 0.6879(6) -0.0064(8) 0.097(5) Uani 1 1 d . . . H21A H 1.3642 0.6767 0.0075 0.116 Uiso 1 1 calc R . . C22 C 1.560(2) 0.4537(7) -0.1826(9) 0.113(6) Uani 1 1 d . . . C23 C 1.7018(18) 0.4466(6) -0.2928(7) 0.089(5) Uani 1 1 d . . . C24 C 1.4827(17) 0.3491(6) -0.1267(8) 0.110(6) Uani 1 1 d . . . H24A H 1.5273 0.3435 -0.1639 0.132 Uiso 1 1 calc R . . C25 C 1.1279(18) 0.8232(7) -0.0354(8) 0.090(5) Uani 1 1 d . . . C26 C 1.7469(17) 0.4275(6) -0.2325(8) 0.103(5) Uani 1 1 d . . . H26A H 1.8234 0.4125 -0.2284 0.123 Uiso 1 1 calc R . . C27 C 1.4465(17) 0.4010(6) -0.0994(7) 0.101(5) Uani 1 1 d . . . C28 C 1.0979(16) 0.6659(5) -0.0497(7) 0.089(4) Uani 1 1 d . . . H28A H 1.0414 0.6397 -0.0627 0.107 Uiso 1 1 calc R . . C29 C 1.4004(19) 0.5919(7) -0.0931(8) 0.118(6) Uani 1 1 d . . . H29A H 1.4006 0.6302 -0.0987 0.141 Uiso 1 1 calc R . . C30 C 1.674(2) 0.4321(6) -0.1805(8) 0.118(7) Uani 1 1 d . . . H30A H 1.7033 0.4197 -0.1405 0.141 Uiso 1 1 calc R . . C31 C 1.0733(18) 0.5798(5) 0.0657(9) 0.119(7) Uani 1 1 d . . . H31A H 1.0454 0.6161 0.0637 0.143 Uiso 1 1 calc R . . C32 C 1.2286(14) 0.3124(6) 0.1239(7) 0.091(4) Uani 1 1 d . . . H32A H 1.2424 0.2758 0.1361 0.110 Uiso 1 1 calc R . . C33 C 1.4399(15) 0.1651(6) 0.0523(8) 0.100(5) Uani 1 1 d . . . H33A H 1.5066 0.1488 0.0720 0.120 Uiso 1 1 calc R . . C34 C 1.256(2) 0.1623(6) -0.0004(10) 0.133(7) Uani 1 1 d . . . H34A H 1.1926 0.1416 -0.0173 0.159 Uiso 1 1 calc R . . C35 C 1.3457(15) 0.1333(5) 0.0256(8) 0.085(5) Uani 1 1 d . . . C36 C 1.3401(17) 0.0719(7) 0.0263(7) 0.086(4) Uani 1 1 d . . . C37 C 1.1096(17) 0.4491(5) 0.1341(7) 0.098(5) Uani 1 1 d . . . C38 C 0.8482(18) 0.4524(6) 0.2510(11) 0.111(6) Uani 1 1 d . . . H38A H 0.7649 0.4524 0.2494 0.133 Uiso 1 1 calc R . . C39 C 1.0929(17) 0.4488(6) 0.2550(9) 0.095(5) Uani 1 1 d . . . H39A H 1.1762 0.4480 0.2566 0.114 Uiso 1 1 calc R . . C40 C 1.032(2) 0.4491(5) 0.3130(9) 0.104(5) Uani 1 1 d . . . H40A H 1.0743 0.4468 0.3523 0.125 Uiso 1 1 calc R . . C41 C 1.037(2) 0.4497(5) 0.1959(10) 0.103(6) Uani 1 1 d . . . C42 C 0.912(2) 0.4526(6) 0.3124(8) 0.093(5) Uani 1 1 d . . . C43 C 0.840(2) 0.4551(6) 0.3722(12) 0.108(6) Uani 1 1 d . . . C44 C 0.916(2) 0.4524(6) 0.1923(8) 0.099(5) Uani 1 1 d . . . H44A H 0.8766 0.4541 0.1520 0.119 Uiso 1 1 calc R . . C45 C 1.3346(17) 0.2489(5) 0.0207(8) 0.093(5) Uani 1 1 d . . . C46 C 1.2443(17) 0.2189(6) -0.0059(9) 0.108(6) Uani 1 1 d . . . H46A H 1.1785 0.2354 -0.0265 0.130 Uiso 1 1 calc R . . C47 C 1.4282(18) 0.2221(7) 0.0476(9) 0.113(6) Uani 1 1 d . . . H47A H 1.4905 0.2435 0.0646 0.135 Uiso 1 1 calc R . . C48 C 1.3306(16) 0.3101(6) 0.0166(8) 0.100(5) Uani 1 1 d . . . O10 O 0.480(2) 0.4186(10) 0.4020(13) 0.196(9) Uiso 1 1 d . . . C49 C 0.502(3) 0.3865(15) 0.3566(15) 0.215(16) Uiso 1 1 d . . . H49A H 0.5821 0.3814 0.3467 0.257 Uiso 1 1 calc R . . N5 N 0.417(2) 0.3571(10) 0.3187(13) 0.157(8) Uiso 1 1 d . . . C50 C 0.298(3) 0.3443(18) 0.336(2) 0.25(2) Uiso 1 1 d . . . H50A H 0.2769 0.3650 0.3742 0.381 Uiso 1 1 calc R . . H50B H 0.2913 0.3054 0.3452 0.381 Uiso 1 1 calc R . . H50C H 0.2438 0.3538 0.3010 0.381 Uiso 1 1 calc R . . C51 C 0.449(4) 0.3237(16) 0.2644(16) 0.240(18) Uiso 1 1 d . . . H51A H 0.5299 0.3317 0.2526 0.359 Uiso 1 1 calc R . . H51B H 0.3960 0.3317 0.2283 0.359 Uiso 1 1 calc R . . H51C H 0.4421 0.2852 0.2757 0.359 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0967(5) 0.0674(3) 0.1022(5) 0.0040(3) 0.0246(4) 0.0012(3) Pb2 0.1250(6) 0.0751(4) 0.0873(4) 0.0031(3) 0.0127(4) -0.0112(3) Co1 0.1306(18) 0.0605(10) 0.0804(14) -0.0002(9) 0.0206(12) 0.0024(10) O1 0.176(12) 0.095(7) 0.058(7) 0.008(5) 0.018(7) 0.000(7) O2 0.158(12) 0.128(9) 0.070(7) 0.004(6) 0.037(8) -0.033(9) O3 0.156(12) 0.075(7) 0.125(10) -0.007(6) 0.010(9) -0.009(7) O4 0.143(11) 0.072(6) 0.128(10) 0.027(6) 0.024(9) 0.014(7) O5 0.168(13) 0.121(9) 0.082(8) -0.013(6) 0.028(9) -0.029(9) O6 0.150(11) 0.101(8) 0.069(8) 0.002(6) 0.015(8) 0.004(7) O7 0.096(8) 0.072(6) 0.109(8) -0.005(5) 0.014(7) 0.001(5) O8 0.081(7) 0.075(6) 0.133(9) 0.007(6) 0.001(7) -0.004(5) O9 0.095(9) 0.162(11) 0.181(13) -0.047(9) 0.023(8) -0.059(8) N1 0.153(13) 0.069(8) 0.086(9) 0.005(6) 0.020(9) 0.011(7) N2 0.154(12) 0.064(7) 0.077(8) 0.008(6) 0.029(8) -0.001(7) N3 0.152(12) 0.059(7) 0.082(9) -0.001(6) 0.035(8) -0.010(7) N4 0.184(14) 0.051(6) 0.096(10) 0.009(6) 0.049(10) 0.008(7) C1 0.165(19) 0.113(14) 0.122(16) -0.007(11) 0.059(14) -0.003(12) C2 0.132(15) 0.068(10) 0.089(11) 0.014(8) 0.018(11) 0.010(10) C3 0.21(2) 0.134(15) 0.087(14) 0.022(11) 0.055(14) 0.076(15) C4 0.162(17) 0.081(11) 0.097(13) -0.001(9) 0.047(12) 0.001(10) C5 0.136(14) 0.065(9) 0.095(12) 0.001(8) 0.042(11) 0.004(9) C6 0.137(15) 0.064(8) 0.086(11) 0.010(8) 0.032(11) -0.001(9) C7 0.173(18) 0.065(9) 0.113(14) -0.002(9) 0.021(13) 0.004(11) C8 0.126(13) 0.064(8) 0.086(11) 0.002(8) 0.023(10) -0.006(8) C9 0.119(15) 0.064(9) 0.117(13) 0.016(8) 0.030(11) 0.024(10) C10 0.125(13) 0.070(9) 0.073(10) -0.002(7) 0.020(9) 0.001(8) C11 0.121(13) 0.082(9) 0.077(10) 0.011(8) 0.012(10) 0.015(9) C12 0.146(16) 0.053(8) 0.130(15) -0.018(9) 0.006(13) 0.005(9) C13 0.20(2) 0.063(9) 0.099(13) 0.017(8) 0.074(13) 0.034(10) C14 0.136(14) 0.058(8) 0.079(10) 0.005(7) 0.019(10) 0.011(8) C15 0.153(16) 0.061(9) 0.136(15) 0.016(9) 0.054(13) 0.002(9) C16 0.101(13) 0.066(9) 0.123(13) -0.017(8) 0.001(11) -0.004(8) C17 0.16(2) 0.132(15) 0.078(13) 0.010(10) 0.009(13) 0.045(14) C18 0.117(16) 0.085(11) 0.110(17) -0.012(10) 0.015(14) 0.004(10) C19 0.102(13) 0.063(9) 0.155(16) -0.009(9) 0.015(11) -0.009(9) C20 0.178(18) 0.067(9) 0.085(11) 0.013(8) 0.029(12) 0.030(10) C21 0.100(12) 0.079(10) 0.112(13) 0.000(9) -0.002(10) 0.005(9) C22 0.18(2) 0.080(10) 0.082(13) -0.009(9) 0.060(13) 0.029(11) C23 0.142(16) 0.070(8) 0.057(10) 0.006(7) 0.024(10) -0.007(9) C24 0.162(17) 0.062(9) 0.105(13) -0.003(8) 0.021(12) 0.011(10) C25 0.086(13) 0.091(12) 0.094(12) 0.012(9) 0.009(10) 0.006(10) C26 0.148(16) 0.087(10) 0.074(11) 0.005(8) 0.032(11) 0.008(10) C27 0.156(16) 0.072(9) 0.075(10) 0.025(8) 0.027(11) 0.025(9) C28 0.124(14) 0.048(8) 0.097(11) 0.011(7) -0.010(10) 0.008(8) C29 0.177(19) 0.099(11) 0.078(11) -0.014(9) 0.037(12) 0.003(12) C30 0.21(2) 0.079(10) 0.061(10) -0.013(8) 0.021(13) 0.001(13) C31 0.186(19) 0.044(7) 0.129(14) -0.011(8) 0.056(14) 0.030(9) C32 0.120(13) 0.077(9) 0.078(10) 0.012(8) 0.013(9) 0.010(9) C33 0.099(12) 0.076(10) 0.125(14) -0.009(9) 0.001(10) -0.028(9) C34 0.162(18) 0.066(10) 0.173(19) -0.017(11) 0.078(15) -0.009(11) C35 0.104(12) 0.041(7) 0.112(12) 0.005(7) 0.040(10) 0.020(8) C36 0.094(13) 0.106(12) 0.060(9) 0.029(8) 0.021(9) 0.023(11) C37 0.169(16) 0.061(8) 0.065(9) -0.011(7) 0.029(10) 0.005(9) C38 0.130(15) 0.066(8) 0.137(17) -0.012(10) 0.012(14) -0.001(9) C39 0.131(14) 0.083(10) 0.071(11) 0.020(8) 0.028(11) -0.005(9) C40 0.135(17) 0.065(9) 0.114(15) -0.013(8) 0.028(13) -0.005(9) C41 0.151(18) 0.052(8) 0.108(16) -0.009(8) 0.044(14) 0.013(9) C42 0.134(16) 0.077(9) 0.069(11) 0.009(7) 0.021(12) 0.015(10) C43 0.15(2) 0.052(8) 0.123(19) 0.002(10) 0.047(18) -0.002(10) C44 0.157(19) 0.088(10) 0.054(10) 0.001(7) 0.020(11) 0.014(11) C45 0.125(14) 0.048(8) 0.105(12) 0.001(7) -0.018(11) 0.005(9) C46 0.127(15) 0.056(9) 0.141(15) 0.006(9) -0.018(12) 0.029(9) C47 0.122(15) 0.080(11) 0.136(16) 0.011(10) 0.027(12) 0.002(10) C48 0.134(14) 0.065(9) 0.101(12) -0.001(8) 0.018(11) -0.005(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 Pb1 O5 2.452(12) . ? Pb1 O7 2.472(9) 2_755 ? Pb1 O8 2.520(9) 2_755 ? Pb1 O1 2.683(11) 1_456 ? Pb1 O10 2.70(3) . ? Pb1 C36 2.837(16) 2_755 ? Pb2 O4 2.354(10) 2_844 ? Pb2 O2 2.371(10) . ? Pb2 O9 2.488(15) . ? Co1 N2 1.971(11) . ? Co1 N3 1.985(12) . ? Co1 N1 1.986(13) . ? Co1 N4 1.993(12) . ? O1 C18 1.20(2) . ? O1 Pb1 2.683(11) 1_654 ? O2 C18 1.32(2) . ? O3 C25 1.172(18) . ? O4 C25 1.254(18) . ? O4 Pb2 2.354(9) 2_854 ? O5 C43 1.30(2) . ? O6 C43 1.20(2) . ? O7 C36 1.256(18) . ? O7 Pb1 2.472(9) 2_745 ? O8 C36 1.262(16) . ? O8 Pb1 2.520(9) 2_745 ? N1 C5 1.324(18) . ? N1 C6 1.357(17) . ? N2 C8 1.368(16) . ? N2 C10 1.387(17) . ? N3 C27 1.343(17) . ? N3 C14 1.356(16) . ? N4 C4 1.347(18) . ? N4 C13 1.359(18) . ? C1 C29 1.35(2) . ? C1 C5 1.45(2) . ? C1 H1A 0.9300 . ? C2 C28 1.36(2) . ? C2 C21 1.38(2) . ? C2 C11 1.49(2) . ? C3 C22 1.37(2) . ? C3 C17 1.41(2) . ? C3 H3A 0.9300 . ? C4 C31 1.42(2) . ? C4 C11 1.44(2) . ? C5 C20 1.406(19) . ? C6 C11 1.38(2) . ? C6 C29 1.39(2) . ? C7 C31 1.30(2) . ? C7 C13 1.37(2) . ? C7 H7A 0.9300 . ? C8 C48 1.42(2) . ? C8 C32 1.438(19) . ? C9 C19 1.37(2) . ? C9 C16 1.41(2) . ? C9 C25 1.54(2) . ? C10 C37 1.362(19) . ? C10 C15 1.448(19) . ? C12 C24 1.35(2) . ? C12 C14 1.41(2) . ? C12 H12A 0.9300 . ? C13 C37 1.388(19) . ? C14 C48 1.405(19) . ? C15 C32 1.33(2) . ? C15 H15A 0.9300 . ? C16 C21 1.370(19) . ? C16 H16A 0.9300 . ? C17 C23 1.39(2) . ? C17 H17A 0.9300 . ? C18 C23 1.47(2) . ? C19 C28 1.367(18) . ? C19 H19A 0.9300 . ? C20 C27 1.42(2) . ? C20 C22 1.48(2) . ? C21 H21A 0.9300 . ? C22 C30 1.38(3) . ? C23 C26 1.41(2) . ? C24 C27 1.434(19) . ? C24 H24A 0.9300 . ? C26 C30 1.36(2) . ? C26 H26A 0.9300 . ? C28 H28A 0.9300 . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C47 1.38(2) . ? C33 C35 1.41(2) . ? C33 H33A 0.9300 . ? C34 C35 1.33(2) . ? C34 C46 1.38(2) . ? C34 H34A 0.9300 . ? C35 C36 1.48(2) . ? C36 Pb1 2.837(16) 2_745 ? C37 C41 1.52(2) . ? C38 C44 1.44(2) . ? C38 C42 1.44(2) . ? C38 H38A 0.9300 . ? C39 C41 1.36(2) . ? C39 C40 1.38(2) . ? C39 H39A 0.9300 . ? C40 C42 1.34(2) . ? C40 H40A 0.9300 . ? C41 C44 1.35(2) . ? C42 C43 1.48(2) . ? C44 H44A 0.9300 . ? C45 C47 1.34(2) . ? C45 C46 1.35(2) . ? C45 C48 1.479(19) . ? C46 H46A 0.9300 . ? C47 H47A 0.9300 . ? O10 C49 1.241(10) . ? C49 N5 1.410(10) . ? C49 H49A 0.9300 . ? N5 C50 1.419(10) . ? N5 C51 1.429(10) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Pb1 O7 87.2(4) . 2_755 ? O5 Pb1 O8 86.8(4) . 2_755 ? O7 Pb1 O8 52.6(3) 2_755 2_755 ? O5 Pb1 O1 140.5(5) . 1_456 ? O7 Pb1 O1 69.0(3) 2_755 1_456 ? O8 Pb1 O1 101.5(4) 2_755 1_456 ? O5 Pb1 O10 70.7(7) . . ? O7 Pb1 O10 130.7(6) 2_755 . ? O8 Pb1 O10 81.9(6) 2_755 . ? O1 Pb1 O10 148.4(6) 1_456 . ? O5 Pb1 C36 87.4(4) . 2_755 ? O7 Pb1 C36 26.2(4) 2_755 2_755 ? O8 Pb1 C36 26.4(4) 2_755 2_755 ? O1 Pb1 C36 84.3(4) 1_456 2_755 ? O10 Pb1 C36 106.9(6) . 2_755 ? O4 Pb2 O2 83.0(4) 2_844 . ? O4 Pb2 O9 79.8(5) 2_844 . ? O2 Pb2 O9 74.8(5) . . ? N2 Co1 N3 91.0(5) . . ? N2 Co1 N1 172.8(6) . . ? N3 Co1 N1 89.8(5) . . ? N2 Co1 N4 88.6(5) . . ? N3 Co1 N4 176.5(6) . . ? N1 Co1 N4 91.0(5) . . ? C18 O1 Pb1 139.9(11) . 1_654 ? C18 O2 Pb2 106.4(12) . . ? C25 O4 Pb2 104.1(11) . 2_854 ? C43 O5 Pb1 100.4(13) . . ? C36 O7 Pb1 93.4(9) . 2_745 ? C36 O8 Pb1 91.0(10) . 2_745 ? C5 N1 C6 107.7(12) . . ? C5 N1 Co1 126.6(9) . . ? C6 N1 Co1 125.3(11) . . ? C8 N2 C10 105.7(11) . . ? C8 N2 Co1 126.0(10) . . ? C10 N2 Co1 128.2(9) . . ? C27 N3 C14 104.9(11) . . ? C27 N3 Co1 127.3(9) . . ? C14 N3 Co1 126.2(10) . . ? C4 N4 C13 105.4(12) . . ? C4 N4 Co1 125.5(11) . . ? C13 N4 Co1 128.9(8) . . ? C29 C1 C5 103.3(17) . . ? C29 C1 H1A 128.4 . . ? C5 C1 H1A 128.4 . . ? C28 C2 C21 118.1(13) . . ? C28 C2 C11 121.6(16) . . ? C21 C2 C11 120.3(17) . . ? C22 C3 C17 123.1(19) . . ? C22 C3 H3A 118.5 . . ? C17 C3 H3A 118.5 . . ? N4 C4 C31 107.6(14) . . ? N4 C4 C11 126.2(16) . . ? C31 C4 C11 124.2(15) . . ? N1 C5 C20 128.0(14) . . ? N1 C5 C1 110.6(13) . . ? C20 C5 C1 121.1(16) . . ? N1 C6 C11 128.0(15) . . ? N1 C6 C29 108.4(15) . . ? C11 C6 C29 122.6(15) . . ? C31 C7 C13 106.5(17) . . ? C31 C7 H7A 126.8 . . ? C13 C7 H7A 126.8 . . ? N2 C8 C48 126.9(13) . . ? N2 C8 C32 110.5(13) . . ? C48 C8 C32 122.6(13) . . ? C19 C9 C16 118.8(13) . . ? C19 C9 C25 125.6(17) . . ? C16 C9 C25 115.4(16) . . ? C37 C10 N2 124.0(13) . . ? C37 C10 C15 127.1(15) . . ? N2 C10 C15 108.6(12) . . ? C6 C11 C4 120.5(14) . . ? C6 C11 C2 122.8(14) . . ? C4 C11 C2 116.7(15) . . ? C24 C12 C14 106.9(13) . . ? C24 C12 H12A 126.5 . . ? C14 C12 H12A 126.5 . . ? N4 C13 C7 111.2(13) . . ? N4 C13 C37 123.2(14) . . ? C7 C13 C37 125.5(16) . . ? N3 C14 C48 125.9(13) . . ? N3 C14 C12 111.3(13) . . ? C48 C14 C12 122.5(13) . . ? C32 C15 C10 108.1(15) . . ? C32 C15 H15A 125.9 . . ? C10 C15 H15A 125.9 . . ? C21 C16 C9 119.1(14) . . ? C21 C16 H16A 120.5 . . ? C9 C16 H16A 120.5 . . ? C23 C17 C3 117.3(17) . . ? C23 C17 H17A 121.3 . . ? C3 C17 H17A 121.3 . . ? O1 C18 O2 120.1(19) . . ? O1 C18 C23 125.5(18) . . ? O2 C18 C23 113.0(18) . . ? C28 C19 C9 120.1(16) . . ? C28 C19 H19A 119.9 . . ? C9 C19 H19A 119.9 . . ? C5 C20 C27 120.4(15) . . ? C5 C20 C22 121.0(13) . . ? C27 C20 C22 118.7(13) . . ? C16 C21 C2 121.3(16) . . ? C16 C21 H21A 119.3 . . ? C2 C21 H21A 119.3 . . ? C3 C22 C30 116.2(16) . . ? C3 C22 C20 121(2) . . ? C30 C22 C20 122.8(18) . . ? C17 C23 C26 121.2(16) . . ? C17 C23 C18 117.1(16) . . ? C26 C23 C18 121.7(18) . . ? C12 C24 C27 105.4(15) . . ? C12 C24 H24A 127.3 . . ? C27 C24 H24A 127.3 . . ? O3 C25 O4 126.3(17) . . ? O3 C25 C9 123.7(18) . . ? O4 C25 C9 110.0(17) . . ? C30 C26 C23 117.1(18) . . ? C30 C26 H26A 121.4 . . ? C23 C26 H26A 121.4 . . ? N3 C27 C20 125.6(13) . . ? N3 C27 C24 111.4(12) . . ? C20 C27 C24 122.9(15) . . ? C2 C28 C19 122.2(15) . . ? C2 C28 H28A 118.9 . . ? C19 C28 H28A 118.9 . . ? C1 C29 C6 110.0(17) . . ? C1 C29 H29A 125.0 . . ? C6 C29 H29A 125.0 . . ? C26 C30 C22 125.0(17) . . ? C26 C30 H30A 117.5 . . ? C22 C30 H30A 117.5 . . ? C7 C31 C4 109.2(14) . . ? C7 C31 H31A 125.4 . . ? C4 C31 H31A 125.4 . . ? C15 C32 C8 106.8(14) . . ? C15 C32 H32A 126.6 . . ? C8 C32 H32A 126.6 . . ? C47 C33 C35 116.6(16) . . ? C47 C33 H33A 121.7 . . ? C35 C33 H33A 121.7 . . ? C35 C34 C46 129(2) . . ? C35 C34 H34A 115.5 . . ? C46 C34 H34A 115.5 . . ? C34 C35 C33 114.9(14) . . ? C34 C35 C36 120.0(17) . . ? C33 C35 C36 125.1(16) . . ? O7 C36 O8 123.0(15) . . ? O7 C36 C35 120.6(15) . . ? O8 C36 C35 116.5(17) . . ? O7 C36 Pb1 60.4(8) . 2_745 ? O8 C36 Pb1 62.6(8) . 2_745 ? C35 C36 Pb1 176.8(10) . 2_745 ? C10 C37 C13 125.7(14) . . ? C10 C37 C41 116.9(13) . . ? C13 C37 C41 117.4(13) . . ? C44 C38 C42 118.7(18) . . ? C44 C38 H38A 120.6 . . ? C42 C38 H38A 120.6 . . ? C41 C39 C40 123.1(19) . . ? C41 C39 H39A 118.4 . . ? C40 C39 H39A 118.4 . . ? C42 C40 C39 119.8(19) . . ? C42 C40 H40A 120.1 . . ? C39 C40 H40A 120.1 . . ? C44 C41 C39 119.6(17) . . ? C44 C41 C37 120(2) . . ? C39 C41 C37 120(2) . . ? C40 C42 C38 119.1(17) . . ? C40 C42 C43 123(2) . . ? C38 C42 C43 118(2) . . ? O6 C43 O5 124(2) . . ? O6 C43 C42 119(2) . . ? O5 C43 C42 117(2) . . ? C41 C44 C38 119.5(18) . . ? C41 C44 H44A 120.3 . . ? C38 C44 H44A 120.3 . . ? C47 C45 C46 118.7(14) . . ? C47 C45 C48 121.9(16) . . ? C46 C45 C48 119.4(15) . . ? C45 C46 C34 115.4(17) . . ? C45 C46 H46A 122.3 . . ? C34 C46 H46A 122.3 . . ? C45 C47 C33 125.4(17) . . ? C45 C47 H47A 117.3 . . ? C33 C47 H47A 117.3 . . ? C14 C48 C8 121.5(13) . . ? C14 C48 C45 120.7(14) . . ? C8 C48 C45 117.6(14) . . ? C49 O10 Pb1 119(2) . . ? O10 C49 N5 126(3) . . ? O10 C49 H49A 116.9 . . ? N5 C49 H49A 116.9 . . ? C49 N5 C50 127(3) . . ? C49 N5 C51 123(3) . . ? C50 N5 C51 109(3) . . ? N5 C50 H50A 109.5 . . ? N5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.489 _refine_diff_density_min -0.998 _refine_diff_density_rms 0.145 # Attachment '- New3.cif' data_New3 _database_code_depnum_ccdc_archive 'CCDC 871468' #TrackingRef '- New3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H33 N5 Ni O10 Pb2' _chemical_formula_weight 1348.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.2406(5) _cell_length_b 24.0590(10) _cell_length_c 21.2577(8) _cell_angle_alpha 90.00 _cell_angle_beta 93.328(4) _cell_angle_gamma 90.00 _cell_volume 5228.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 21877 _cell_measurement_theta_min 3.31 _cell_measurement_theta_max 25.06 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2584 _exptl_absorpt_coefficient_mu 6.839 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.304 _exptl_absorpt_correction_T_max 0.471 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 21877 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0844 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.31 _diffrn_reflns_theta_max 25.06 _reflns_number_total 9200 _reflns_number_gt 5943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.152 0.779 0.215 319 78 ' ' 2 -0.166 0.279 0.285 320 76 ' ' 3 0.150 0.721 0.715 319 78 ' ' 4 -0.165 0.221 0.785 320 76 ' ' _platon_squeeze_details ; ; _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^)+(0.0597P)^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 9200 _refine_ls_number_parameters 602 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1193 _refine_ls_R_factor_gt 0.0858 _refine_ls_wR_factor_ref 0.1888 _refine_ls_wR_factor_gt 0.1783 _refine_ls_goodness_of_fit_ref 1.297 _refine_ls_restrained_S_all 1.297 _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 Pb1 Pb -0.97276(6) -0.43438(2) -0.56120(3) 0.0593(2) Uani 1 1 d . . . Pb2 Pb -1.35472(6) 0.05331(2) -0.03236(3) 0.0582(2) Uani 1 1 d . . . Ni1 Ni -0.71760(18) 0.05406(7) -0.49653(7) 0.0494(4) Uani 1 1 d . . . O1 O -1.2818(13) 0.0515(5) -0.1368(5) 0.080(3) Uani 1 1 d . . . O2 O -1.0974(14) 0.0502(5) -0.0817(5) 0.086(4) Uani 1 1 d . . . O3 O -0.7902(14) -0.3542(5) -0.5189(6) 0.090(4) Uani 1 1 d . . . O4 O -0.9871(14) -0.3365(4) -0.5610(6) 0.083(3) Uani 1 1 d . . . O5 O -0.1370(12) 0.0837(5) -0.8456(5) 0.070(3) Uani 1 1 d . . . O6 O -0.2834(12) 0.0316(4) -0.8990(4) 0.070(3) Uani 1 1 d . . . O7 O -0.5730(10) 0.4595(4) -0.4560(5) 0.059(2) Uani 1 1 d . . . O8 O -0.7785(12) 0.4582(4) -0.4899(4) 0.062(3) Uani 1 1 d . . . O9 O -1.5655(10) 0.0625(5) -0.1009(4) 0.070(3) Uani 1 1 d . . . O10 O -1.1449(12) -0.4179(6) -0.6406(5) 0.087(4) Uani 1 1 d D . . N1 N -0.8227(11) 0.0005(4) -0.4537(4) 0.047(3) Uani 1 1 d . . . N2 N -0.6611(11) -0.0025(4) -0.5534(4) 0.049(3) Uani 1 1 d . . . N3 N -0.6394(12) 0.1104(4) -0.5478(5) 0.053(3) Uani 1 1 d . . . N4 N -0.7495(11) 0.1088(4) -0.4326(4) 0.045(3) Uani 1 1 d . . . N5 N -1.171(2) -0.3618(8) -0.7253(9) 0.121(6) Uiso 1 1 d D . . C1 C -1.162(2) 0.0515(6) -0.1327(7) 0.065(4) Uani 1 1 d . . . C2 C -1.0853(16) 0.0525(6) -0.1910(7) 0.061(4) Uani 1 1 d . . . C3 C -1.1528(16) 0.0548(6) -0.2502(6) 0.058(4) Uani 1 1 d . . . H3A H -1.2437 0.0559 -0.2527 0.070 Uiso 1 1 calc R . . C4 C -1.0878(18) 0.0555(6) -0.3039(7) 0.068(4) Uani 1 1 d . . . H4A H -1.1354 0.0568 -0.3425 0.081 Uiso 1 1 calc R . . C5 C -0.9527(16) 0.0544(5) -0.3028(6) 0.054(4) Uani 1 1 d . . . C6 C -0.8839(16) 0.0540(6) -0.2448(7) 0.058(4) Uani 1 1 d . . . H6A H -0.7930 0.0547 -0.2421 0.069 Uiso 1 1 calc R . . C7 C -0.9539(18) 0.0524(5) -0.1907(7) 0.061(4) Uani 1 1 d . . . H7A H -0.9069 0.0511 -0.1520 0.073 Uiso 1 1 calc R . . C8 C -0.8791(16) 0.0539(6) -0.3627(7) 0.060(4) Uani 1 1 d . . . C9 C -0.8949(14) 0.0084(5) -0.4029(6) 0.049(3) Uani 1 1 d . . . C10 C -0.9752(17) -0.0372(6) -0.3939(7) 0.063(4) Uani 1 1 d . . . H10A H -1.0393 -0.0394 -0.3647 0.076 Uiso 1 1 calc R . . C11 C -0.9463(14) -0.0761(6) -0.4325(9) 0.067(5) Uani 1 1 d . . . H11A H -0.9808 -0.1118 -0.4342 0.080 Uiso 1 1 calc R . . C12 C -0.8488(15) -0.0532(6) -0.4732(6) 0.052(3) Uani 1 1 d . . . C13 C -0.7765(15) -0.0845(6) -0.5151(6) 0.054(4) Uani 1 1 d . . . C14 C -0.8036(15) -0.1454(5) -0.5218(6) 0.049(3) Uani 1 1 d . . . C15 C -0.9160(14) -0.1659(6) -0.5425(6) 0.052(3) Uani 1 1 d . . . H15A H -0.9840 -0.1413 -0.5525 0.063 Uiso 1 1 calc R . . C16 C -0.9394(17) -0.2213(6) -0.5501(7) 0.062(4) Uani 1 1 d . . . H16A H -1.0194 -0.2331 -0.5684 0.075 Uiso 1 1 calc R . . C17 C -0.8491(16) -0.2592(6) -0.5316(7) 0.057(4) Uani 1 1 d . . . C18 C -0.7297(18) -0.2407(6) -0.5083(8) 0.072(5) Uani 1 1 d . . . H18A H -0.6651 -0.2663 -0.4961 0.086 Uiso 1 1 calc R . . C19 C -0.7031(18) -0.1835(6) -0.5024(8) 0.076(5) Uani 1 1 d . . . H19A H -0.6221 -0.1709 -0.4862 0.091 Uiso 1 1 calc R . . C20 C -0.874(2) -0.3207(7) -0.5365(8) 0.067(4) Uani 1 1 d . . . C21 C -0.6832(15) -0.0582(6) -0.5494(6) 0.053(4) Uani 1 1 d . . . C22 C -0.6059(14) -0.0868(6) -0.5932(5) 0.051(3) Uani 1 1 d . . . H22A H -0.6001 -0.1251 -0.5979 0.061 Uiso 1 1 calc R . . C23 C -0.5434(17) -0.0488(7) -0.6260(7) 0.070(4) Uani 1 1 d . . . H23A H -0.4874 -0.0551 -0.6581 0.083 Uiso 1 1 calc R . . C24 C -0.5816(15) 0.0041(6) -0.6010(6) 0.051(3) Uani 1 1 d . . . C25 C -0.5445(15) 0.0529(6) -0.6265(7) 0.059(4) Uani 1 1 d . . . C26 C -0.4657(15) 0.0539(5) -0.6859(6) 0.053(4) Uani 1 1 d . . . C27 C -0.3366(16) 0.0712(6) -0.6832(7) 0.061(4) Uani 1 1 d . . . H27A H -0.2967 0.0829 -0.6451 0.074 Uiso 1 1 calc R . . C28 C -0.2705(16) 0.0710(6) -0.7341(6) 0.058(4) Uani 1 1 d . . . H28A H -0.1820 0.0798 -0.7304 0.070 Uiso 1 1 calc R . . C29 C -0.3253(15) 0.0585(6) -0.7920(6) 0.054(4) Uani 1 1 d . . . C30 C -0.4531(18) 0.0433(7) -0.7964(7) 0.072(5) Uani 1 1 d . . . H30A H -0.4922 0.0351 -0.8359 0.086 Uiso 1 1 calc R . . C31 C -0.5246(19) 0.0398(7) -0.7461(7) 0.072(5) Uani 1 1 d . . . H31A H -0.6115 0.0284 -0.7503 0.087 Uiso 1 1 calc R . . C32 C -0.2404(16) 0.0583(6) -0.8497(6) 0.053(4) Uani 1 1 d . . . C33 C -0.5804(16) 0.1031(6) -0.6018(6) 0.057(4) Uani 1 1 d . . . C34 C -0.5514(18) 0.1566(6) -0.6285(7) 0.070(4) Uani 1 1 d . . . H34A H -0.5102 0.1627 -0.6657 0.084 Uiso 1 1 calc R . . C35 C -0.5947(19) 0.1960(6) -0.5898(7) 0.072(5) Uani 1 1 d . . . H35A H -0.5929 0.2344 -0.5955 0.086 Uiso 1 1 calc R . . C36 C -0.6432(14) 0.1667(6) -0.5391(7) 0.056(4) Uani 1 1 d . . . C37 C -0.6776(16) 0.1939(6) -0.4835(7) 0.062(4) Uani 1 1 d . . . C38 C -0.6730(18) 0.2557(6) -0.4808(7) 0.061(4) Uani 1 1 d . . . C39 C -0.7595(16) 0.2846(6) -0.5134(7) 0.056(4) Uani 1 1 d . . . H39A H -0.8236 0.2668 -0.5388 0.067 Uiso 1 1 calc R . . C40 C -0.7564(12) 0.3390(6) -0.5104(4) 0.043(3) Uani 1 1 d . . . H40A H -0.8204 0.3576 -0.5351 0.052 Uiso 1 1 calc R . . C41 C -0.6716(16) 0.3715(5) -0.4758(6) 0.054(4) Uani 1 1 d . . . C42 C -0.6774(18) 0.4325(7) -0.4729(6) 0.059(4) Uani 1 1 d . . . C43 C -0.5749(14) 0.3422(6) -0.4427(5) 0.049(3) Uani 1 1 d . . . H43A H -0.5088 0.3608 -0.4194 0.058 Uiso 1 1 calc R . . C44 C -0.5771(14) 0.2857(7) -0.4445(6) 0.053(4) Uani 1 1 d . . . H44A H -0.5132 0.2660 -0.4209 0.064 Uiso 1 1 calc R . . C45 C -0.7136(14) 0.1639(6) -0.4316(6) 0.050(3) Uani 1 1 d . . . C46 C -0.7355(17) 0.1883(7) -0.3715(6) 0.068(4) Uani 1 1 d . . . H46A H -0.7141 0.2243 -0.3587 0.081 Uiso 1 1 calc R . . C47 C -0.7926(17) 0.1493(7) -0.3373(7) 0.068(4) Uani 1 1 d . . . H47A H -0.8190 0.1529 -0.2964 0.082 Uiso 1 1 calc R . . C48 C -0.8051(15) 0.1000(6) -0.3772(6) 0.052(4) Uani 1 1 d . . . C49 C -1.126(4) -0.4121(13) -0.6930(9) 0.106(15) Uiso 1 1 d . . . H49A H -1.0821 -0.4394 -0.7145 0.127 Uiso 1 1 calc R . . C50 C -1.136(5) -0.3738(14) -0.7906(8) 0.195(18) Uiso 1 1 d . . . H50A H -1.1134 -0.4123 -0.7941 0.234 Uiso 1 1 calc R . . H50D H -1.0633 -0.3511 -0.8008 0.234 Uiso 1 1 calc R . . H50B H -1.2098 -0.3656 -0.8193 0.234 Uiso 1 1 calc R . . C51 C -1.195(6) -0.3038(11) -0.747(2) 0.24(2) Uiso 1 1 d . . . H51D H -1.2217 -0.2816 -0.7126 0.289 Uiso 1 1 calc R . . H51A H -1.2620 -0.3035 -0.7804 0.289 Uiso 1 1 calc R . . H51B H -1.1156 -0.2887 -0.7623 0.289 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0583(4) 0.0581(4) 0.0632(4) -0.0036(3) 0.0164(3) -0.0024(3) Pb2 0.0593(4) 0.0563(4) 0.0605(3) -0.0015(2) 0.0157(3) -0.0053(3) Ni1 0.0525(12) 0.0483(10) 0.0492(9) 0.0000(7) 0.0180(8) -0.0012(9) O1 0.061(8) 0.095(9) 0.087(8) 0.012(6) 0.030(6) 0.001(7) O2 0.094(10) 0.102(9) 0.065(7) 0.012(6) 0.030(7) 0.008(7) O3 0.094(11) 0.046(7) 0.129(10) 0.014(6) 0.000(8) 0.008(7) O4 0.089(11) 0.050(7) 0.111(9) -0.005(6) 0.011(7) 0.010(7) O5 0.060(8) 0.073(7) 0.079(7) -0.003(5) 0.027(5) -0.018(6) O6 0.095(9) 0.075(7) 0.045(6) -0.006(5) 0.030(5) 0.009(6) O7 0.048(6) 0.052(6) 0.079(6) -0.005(5) 0.029(5) -0.009(5) O8 0.068(8) 0.053(6) 0.064(6) 0.005(4) 0.014(5) -0.008(6) O9 0.054(7) 0.110(9) 0.047(5) -0.017(5) 0.018(4) -0.006(6) O10 0.065(8) 0.131(10) 0.066(7) 0.000(6) 0.019(6) -0.017(7) N1 0.048(8) 0.049(7) 0.045(6) 0.000(5) 0.010(5) 0.002(6) N2 0.056(8) 0.039(7) 0.052(6) -0.004(5) 0.019(6) 0.000(6) N3 0.065(9) 0.039(7) 0.056(7) -0.001(5) 0.018(6) -0.007(6) N4 0.055(8) 0.040(6) 0.039(6) 0.006(4) 0.011(5) 0.003(5) C1 0.089(14) 0.059(10) 0.048(9) 0.021(7) 0.024(9) 0.014(9) C2 0.059(10) 0.062(9) 0.066(9) 0.015(7) 0.035(8) 0.002(8) C3 0.054(10) 0.062(9) 0.060(9) -0.007(7) 0.025(7) -0.007(8) C4 0.067(12) 0.069(11) 0.069(10) 0.002(7) 0.017(8) 0.002(9) C5 0.061(10) 0.048(8) 0.057(8) 0.002(6) 0.024(7) 0.002(7) C6 0.050(9) 0.056(9) 0.069(9) 0.011(7) 0.017(7) 0.012(7) C7 0.076(12) 0.042(8) 0.063(9) 0.007(6) -0.002(8) -0.005(8) C8 0.063(10) 0.050(9) 0.068(9) 0.013(7) 0.021(7) 0.002(8) C9 0.050(9) 0.038(7) 0.063(8) -0.009(6) 0.018(7) 0.000(7) C10 0.073(12) 0.051(9) 0.066(9) 0.003(7) 0.006(8) 0.000(9) C11 0.030(8) 0.043(9) 0.130(14) 0.028(9) 0.016(8) -0.007(7) C12 0.056(9) 0.050(9) 0.051(7) 0.010(6) 0.010(6) 0.003(7) C13 0.053(10) 0.044(8) 0.067(9) 0.008(6) 0.008(7) 0.013(7) C14 0.053(9) 0.044(8) 0.050(8) -0.006(6) 0.007(6) -0.015(7) C15 0.028(8) 0.058(9) 0.070(9) -0.018(7) -0.001(6) -0.001(7) C16 0.066(11) 0.050(9) 0.069(9) -0.006(7) -0.013(8) -0.004(8) C17 0.044(9) 0.058(9) 0.068(9) 0.010(7) 0.009(7) 0.003(8) C18 0.057(12) 0.044(9) 0.115(13) -0.005(8) 0.007(9) 0.007(8) C19 0.064(12) 0.048(10) 0.116(13) 0.003(9) 0.013(10) -0.002(9) C20 0.069(13) 0.057(10) 0.076(10) -0.012(8) 0.019(9) 0.001(10) C21 0.055(9) 0.056(9) 0.051(8) 0.001(6) 0.022(6) 0.007(7) C22 0.039(8) 0.076(10) 0.038(7) -0.013(6) 0.012(6) 0.002(7) C23 0.055(10) 0.086(12) 0.068(10) 0.002(8) 0.007(8) -0.003(9) C24 0.057(10) 0.049(8) 0.048(8) 0.002(6) 0.011(7) 0.004(7) C25 0.049(9) 0.070(10) 0.059(8) 0.002(7) 0.012(7) 0.000(8) C26 0.060(10) 0.044(8) 0.057(8) 0.002(6) 0.018(7) -0.005(7) C27 0.051(10) 0.068(10) 0.066(9) 0.008(7) 0.007(7) 0.002(8) C28 0.054(10) 0.079(10) 0.043(8) -0.010(6) 0.012(7) -0.010(8) C29 0.053(9) 0.065(9) 0.046(8) 0.004(6) 0.025(6) 0.012(8) C30 0.079(13) 0.079(11) 0.060(9) -0.014(7) 0.034(8) 0.001(10) C31 0.075(12) 0.076(11) 0.068(10) -0.011(8) 0.013(9) -0.005(9) C32 0.064(11) 0.043(8) 0.055(9) 0.020(6) 0.029(7) 0.016(8) C33 0.067(11) 0.057(9) 0.051(8) 0.000(6) 0.026(7) -0.002(8) C34 0.074(12) 0.063(10) 0.075(10) 0.003(8) 0.021(8) -0.019(9) C35 0.099(15) 0.045(9) 0.074(10) -0.005(7) 0.029(9) -0.006(9) C36 0.038(9) 0.066(10) 0.064(9) 0.008(7) -0.010(7) -0.004(7) C37 0.055(10) 0.065(10) 0.069(9) -0.013(7) 0.028(7) -0.010(8) C38 0.076(13) 0.043(8) 0.066(9) 0.004(7) 0.037(9) 0.009(8) C39 0.057(10) 0.031(8) 0.080(10) -0.018(7) 0.009(8) -0.017(7) C40 0.025(7) 0.090(11) 0.016(5) -0.019(5) 0.007(4) -0.023(7) C41 0.068(11) 0.037(8) 0.061(9) -0.005(6) 0.024(8) -0.010(7) C42 0.069(12) 0.070(11) 0.039(8) 0.002(6) 0.011(7) 0.006(9) C43 0.046(9) 0.061(10) 0.037(7) 0.012(6) -0.018(6) -0.014(7) C44 0.026(7) 0.086(12) 0.047(8) -0.002(7) -0.002(6) -0.003(7) C45 0.043(8) 0.057(9) 0.052(8) -0.002(6) 0.021(6) 0.009(7) C46 0.075(12) 0.075(11) 0.054(9) -0.005(7) 0.011(8) -0.005(9) C47 0.074(12) 0.072(11) 0.061(9) -0.002(8) 0.020(8) 0.002(9) C48 0.051(9) 0.054(9) 0.053(8) 0.006(6) 0.019(7) 0.011(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 Pb1 O4 2.359(10) . ? Pb1 O5 2.375(10) 2_443 ? Pb1 O10 2.401(12) . ? Pb2 O7 2.383(9) 2_344 ? Pb2 O1 2.384(11) . ? Pb2 O9 2.543(10) . ? Pb2 O8 2.691(10) 2_344 ? Ni1 N2 1.931(10) . ? Ni1 N4 1.934(10) . ? Ni1 N1 1.939(11) . ? Ni1 N3 1.941(11) . ? O1 C1 1.23(2) . ? O2 C1 1.235(19) . ? O3 C20 1.22(2) . ? O4 C20 1.30(2) . ? O5 C32 1.222(18) . ? O5 Pb1 2.375(10) 2_453 ? O6 C32 1.285(18) . ? O7 C42 1.284(19) . ? O7 Pb2 2.383(9) 2_354 ? O8 C42 1.242(18) . ? O8 Pb2 2.691(10) 2_354 ? O10 C49 1.151(10) . ? N1 C9 1.358(15) . ? N1 C12 1.379(16) . ? N2 C24 1.344(16) . ? N2 C21 1.361(16) . ? N3 C33 1.341(16) . ? N3 C36 1.368(17) . ? N4 C48 1.354(15) . ? N4 C45 1.374(16) . ? N5 C49 1.453(10) . ? N5 C50 1.482(10) . ? N5 C51 1.487(10) . ? C1 C2 1.50(2) . ? C2 C7 1.35(2) . ? C2 C3 1.40(2) . ? C3 C4 1.35(2) . ? C3 H3A 0.9300 . ? C4 C5 1.38(2) . ? C4 H4A 0.9300 . ? C5 C6 1.38(2) . ? C5 C8 1.516(19) . ? C6 C7 1.39(2) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C48 1.388(19) . ? C8 C9 1.391(19) . ? C9 C10 1.39(2) . ? C10 C11 1.29(2) . ? C10 H10A 0.9300 . ? C11 C12 1.465(19) . ? C11 H11A 0.9300 . ? C12 C13 1.409(19) . ? C13 C21 1.388(19) . ? C13 C14 1.497(19) . ? C14 C15 1.305(19) . ? C14 C19 1.42(2) . ? C15 C16 1.363(19) . ? C15 H15A 0.9300 . ? C16 C17 1.34(2) . ? C16 H16A 0.9300 . ? C17 C18 1.37(2) . ? C17 C20 1.50(2) . ? C18 C19 1.41(2) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.432(18) . ? C22 C23 1.34(2) . ? C22 H22A 0.9300 . ? C23 C24 1.44(2) . ? C23 H23A 0.9300 . ? C24 C25 1.357(19) . ? C25 C33 1.376(19) . ? C25 C26 1.538(19) . ? C26 C27 1.38(2) . ? C26 C31 1.42(2) . ? C27 C28 1.309(19) . ? C27 H27A 0.9300 . ? C28 C29 1.357(19) . ? C28 H28A 0.9300 . ? C29 C30 1.36(2) . ? C29 C32 1.545(18) . ? C30 C31 1.33(2) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C33 C34 1.44(2) . ? C34 C35 1.35(2) . ? C34 H34A 0.9300 . ? C35 C36 1.40(2) . ? C35 H35A 0.9300 . ? C36 C37 1.412(19) . ? C37 C45 1.388(19) . ? C37 C38 1.49(2) . ? C38 C39 1.29(2) . ? C38 C44 1.41(2) . ? C39 C40 1.311(18) . ? C39 H39A 0.9300 . ? C40 C41 1.354(18) . ? C40 H40A 0.9300 . ? C41 C43 1.375(19) . ? C41 C42 1.47(2) . ? C43 C44 1.362(19) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C46 1.434(18) . ? C46 C47 1.34(2) . ? C46 H46A 0.9300 . ? C47 C48 1.46(2) . ? C47 H47A 0.9300 . ? C49 H49A 0.9300 . ? C50 H50A 0.9600 . ? C50 H50D 0.9600 . ? C50 H50B 0.9600 . ? C51 H51D 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Pb1 O5 81.4(4) . 2_443 ? O4 Pb1 O10 78.1(5) . . ? O5 Pb1 O10 75.4(4) 2_443 . ? O7 Pb2 O1 89.9(4) 2_344 . ? O7 Pb2 O9 77.0(4) 2_344 . ? O1 Pb2 O9 76.7(4) . . ? O7 Pb2 O8 50.6(4) 2_344 2_344 ? O1 Pb2 O8 88.0(4) . 2_344 ? O9 Pb2 O8 125.4(3) . 2_344 ? N2 Ni1 N4 171.4(5) . . ? N2 Ni1 N1 91.1(4) . . ? N4 Ni1 N1 90.1(4) . . ? N2 Ni1 N3 89.6(4) . . ? N4 Ni1 N3 90.6(4) . . ? N1 Ni1 N3 170.3(5) . . ? C1 O1 Pb2 107.4(10) . . ? C20 O4 Pb1 103.9(10) . . ? C32 O5 Pb1 107.3(9) . 2_453 ? C42 O7 Pb2 101.6(10) . 2_354 ? C42 O8 Pb2 88.1(10) . 2_354 ? C49 O10 Pb1 123(2) . . ? C9 N1 C12 105.3(11) . . ? C9 N1 Ni1 128.6(9) . . ? C12 N1 Ni1 125.9(8) . . ? C24 N2 C21 105.9(10) . . ? C24 N2 Ni1 127.1(9) . . ? C21 N2 Ni1 126.7(8) . . ? C33 N3 C36 105.3(11) . . ? C33 N3 Ni1 127.6(9) . . ? C36 N3 Ni1 126.9(9) . . ? C48 N4 C45 105.2(10) . . ? C48 N4 Ni1 127.0(9) . . ? C45 N4 Ni1 127.7(8) . . ? C49 N5 C50 101.2(9) . . ? C49 N5 C51 166(3) . . ? C50 N5 C51 86(3) . . ? O1 C1 O2 122.9(14) . . ? O1 C1 C2 120.5(15) . . ? O2 C1 C2 116.6(17) . . ? C7 C2 C3 116.4(13) . . ? C7 C2 C1 124.4(16) . . ? C3 C2 C1 119.2(15) . . ? C4 C3 C2 121.1(16) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 121.8(15) . . ? C3 C4 H4A 119.1 . . ? C5 C4 H4A 119.1 . . ? C4 C5 C6 118.1(13) . . ? C4 C5 C8 122.2(14) . . ? C6 C5 C8 119.7(14) . . ? C5 C6 C7 118.5(15) . . ? C5 C6 H6A 120.7 . . ? C7 C6 H6A 120.7 . . ? C2 C7 C6 124.1(14) . . ? C2 C7 H7A 118.0 . . ? C6 C7 H7A 118.0 . . ? C48 C8 C9 122.5(13) . . ? C48 C8 C5 119.0(12) . . ? C9 C8 C5 118.4(12) . . ? N1 C9 C8 123.3(13) . . ? N1 C9 C10 110.6(11) . . ? C8 C9 C10 125.8(13) . . ? C11 C10 C9 109.0(15) . . ? C11 C10 H10A 125.5 . . ? C9 C10 H10A 125.5 . . ? C10 C11 C12 107.0(14) . . ? C10 C11 H11A 126.5 . . ? C12 C11 H11A 126.5 . . ? N1 C12 C13 126.2(13) . . ? N1 C12 C11 107.6(12) . . ? C13 C12 C11 125.0(14) . . ? C21 C13 C12 119.4(13) . . ? C21 C13 C14 121.7(12) . . ? C12 C13 C14 118.8(13) . . ? C15 C14 C19 117.7(13) . . ? C15 C14 C13 123.8(14) . . ? C19 C14 C13 118.4(13) . . ? C14 C15 C16 123.7(14) . . ? C14 C15 H15A 118.1 . . ? C16 C15 H15A 118.1 . . ? C17 C16 C15 121.1(15) . . ? C17 C16 H16A 119.5 . . ? C15 C16 H16A 119.5 . . ? C16 C17 C18 118.1(15) . . ? C16 C17 C20 122.5(16) . . ? C18 C17 C20 119.3(14) . . ? C17 C18 C19 121.1(16) . . ? C17 C18 H18A 119.5 . . ? C19 C18 H18A 119.5 . . ? C18 C19 C14 118.1(16) . . ? C18 C19 H19A 121.0 . . ? C14 C19 H19A 121.0 . . ? O3 C20 O4 121.5(16) . . ? O3 C20 C17 121.2(17) . . ? O4 C20 C17 117.4(16) . . ? N2 C21 C13 127.1(12) . . ? N2 C21 C22 109.4(12) . . ? C13 C21 C22 123.0(13) . . ? C23 C22 C21 108.1(14) . . ? C23 C22 H22A 126.0 . . ? C21 C22 H22A 126.0 . . ? C22 C23 C24 105.2(14) . . ? C22 C23 H23A 127.4 . . ? C24 C23 H23A 127.4 . . ? N2 C24 C25 126.9(12) . . ? N2 C24 C23 111.2(12) . . ? C25 C24 C23 121.8(13) . . ? C24 C25 C33 121.3(13) . . ? C24 C25 C26 121.0(12) . . ? C33 C25 C26 117.6(12) . . ? C27 C26 C31 117.6(13) . . ? C27 C26 C25 121.0(13) . . ? C31 C26 C25 121.3(14) . . ? C28 C27 C26 120.2(14) . . ? C28 C27 H27A 119.9 . . ? C26 C27 H27A 119.9 . . ? C27 C28 C29 123.0(15) . . ? C27 C28 H28A 118.5 . . ? C29 C28 H28A 118.5 . . ? C28 C29 C30 118.0(13) . . ? C28 C29 C32 120.0(14) . . ? C30 C29 C32 122.0(13) . . ? C31 C30 C29 122.3(16) . . ? C31 C30 H30A 118.9 . . ? C29 C30 H30A 118.9 . . ? C30 C31 C26 118.8(17) . . ? C30 C31 H31A 120.6 . . ? C26 C31 H31A 120.6 . . ? O5 C32 O6 124.3(12) . . ? O5 C32 C29 117.8(14) . . ? O6 C32 C29 117.9(14) . . ? N3 C33 C25 125.8(12) . . ? N3 C33 C34 109.4(12) . . ? C25 C33 C34 124.6(13) . . ? C35 C34 C33 107.8(14) . . ? C35 C34 H34A 126.1 . . ? C33 C34 H34A 126.1 . . ? C34 C35 C36 105.0(14) . . ? C34 C35 H35A 127.5 . . ? C36 C35 H35A 127.5 . . ? N3 C36 C35 112.3(13) . . ? N3 C36 C37 125.6(13) . . ? C35 C36 C37 121.8(14) . . ? C45 C37 C36 121.0(14) . . ? C45 C37 C38 119.9(12) . . ? C36 C37 C38 119.1(13) . . ? C39 C38 C44 116.8(14) . . ? C39 C38 C37 119.7(15) . . ? C44 C38 C37 123.4(15) . . ? C38 C39 C40 119.7(14) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C39 C40 C41 128.0(14) . . ? C39 C40 H40A 116.0 . . ? C41 C40 H40A 116.0 . . ? C40 C41 C43 113.7(13) . . ? C40 C41 C42 125.0(14) . . ? C43 C41 C42 121.3(13) . . ? O8 C42 O7 119.8(15) . . ? O8 C42 C41 121.3(15) . . ? O7 C42 C41 118.8(15) . . ? C44 C43 C41 119.2(12) . . ? C44 C43 H43A 120.4 . . ? C41 C43 H43A 120.4 . . ? C43 C44 C38 122.4(14) . . ? C43 C44 H44A 118.8 . . ? C38 C44 H44A 118.8 . . ? N4 C45 C37 124.9(11) . . ? N4 C45 C46 110.7(11) . . ? C37 C45 C46 123.9(14) . . ? C47 C46 C45 106.9(14) . . ? C47 C46 H46A 126.5 . . ? C45 C46 H46A 126.5 . . ? C46 C47 C48 106.2(13) . . ? C46 C47 H47A 126.9 . . ? C48 C47 H47A 126.9 . . ? N4 C48 C8 125.4(13) . . ? N4 C48 C47 110.6(12) . . ? C8 C48 C47 123.4(13) . . ? O10 C49 N5 119(2) . . ? O10 C49 H49A 120.3 . . ? N5 C49 H49A 120.3 . . ? N5 C50 H50A 109.5 . . ? N5 C50 H50D 109.5 . . ? H50A C50 H50D 109.5 . . ? N5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? H50D C50 H50B 109.5 . . ? N5 C51 H51D 109.5 . . ? N5 C51 H51A 109.5 . . ? H51D C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51D C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 2.141 _refine_diff_density_min -1.075 _refine_diff_density_rms 0.200 # Attachment '- New4.cif' data_New4 _database_code_depnum_ccdc_archive 'CCDC 871469' #TrackingRef '- New4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H33 Cu N5 O10 Pb2' _chemical_formula_weight 1353.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9008(2) _cell_length_b 24.1824(5) _cell_length_c 20.8565(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.678(2) _cell_angle_gamma 90.00 _cell_volume 5495.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 22552 _cell_measurement_theta_min 3.14 _cell_measurement_theta_max 25.36 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.636 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2588 _exptl_absorpt_coefficient_mu 6.551 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.212 _exptl_absorpt_correction_T_max 0.374 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 22552 _diffrn_reflns_av_R_equivalents 0.0352 _diffrn_reflns_av_sigmaI/netI 0.0520 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 25.35 _reflns_number_total 10016 _reflns_number_gt 6960 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.079 0.222 0.217 362 57 ' ' 2 -0.123 0.722 0.283 362 57 ' ' 3 0.076 0.278 0.717 362 57 ' ' 4 -0.124 0.778 0.783 362 57 ' ' _platon_squeeze_details ; ; _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^)+(0.0603P)^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 10016 _refine_ls_number_parameters 602 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0802 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1410 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _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 Pb1 Pb 0.98332(3) 0.567280(15) 0.561277(19) 0.06447(14) Uani 1 1 d . . . Pb2 Pb 0.65964(3) 1.546944(14) 0.477260(19) 0.06287(14) Uani 1 1 d . . . Cu1 Cu 0.71625(10) 1.05036(4) 0.49769(6) 0.0570(3) Uani 1 1 d . . . O1 O 0.7956(7) 0.6438(3) 0.5197(4) 0.092(2) Uani 1 1 d . . . O2 O 0.9811(6) 0.6631(3) 0.5583(4) 0.087(2) Uani 1 1 d . . . O3 O 1.2790(7) 1.0433(3) 0.1338(4) 0.090(2) Uani 1 1 d . . . O4 O 1.1066(8) 1.0460(3) 0.0781(4) 0.085(2) Uani 1 1 d . . . O5 O 0.7622(6) 1.4540(3) 0.4884(4) 0.0717(18) Uani 1 1 d . . . O6 O 0.5655(6) 1.4544(3) 0.4594(4) 0.0751(19) Uani 1 1 d . . . O7 O 0.1242(7) 1.0804(3) 0.8444(3) 0.0793(19) Uani 1 1 d . . . O8 O 0.2596(7) 1.0320(3) 0.9007(4) 0.083(2) Uani 1 1 d . . . O9 O 1.1421(7) 0.5881(4) 0.6395(4) 0.090(2) Uani 1 1 d . . . O10 O 0.4811(9) 1.5913(6) 0.3900(8) 0.190(7) Uani 1 1 d . . . N1 N 0.8252(6) 0.9955(3) 0.4558(4) 0.0575(18) Uani 1 1 d . . . N2 N 0.7629(6) 1.1071(3) 0.4335(4) 0.0589(18) Uani 1 1 d . . . N3 N 0.6241(6) 1.1073(3) 0.5457(4) 0.0598(18) Uani 1 1 d . . . N4 N 0.6564(6) 0.9917(3) 0.5566(4) 0.0606(19) Uani 1 1 d . . . N5 N 1.2018(9) 0.6315(4) 0.7306(6) 0.099(3) Uiso 1 1 d . . . C1 C 0.8762(11) 0.6764(4) 0.5370(6) 0.072(3) Uani 1 1 d . . . C2 C 0.8473(9) 0.7380(4) 0.5327(5) 0.068(3) Uani 1 1 d . . . C3 C 0.9355(9) 0.7760(4) 0.5511(5) 0.074(3) Uani 1 1 d . . . H3A H 1.0115 0.7640 0.5672 0.089 Uiso 1 1 calc R . . C4 C 0.9112(8) 0.8321(4) 0.5457(5) 0.063(2) Uani 1 1 d . . . H4A H 0.9728 0.8574 0.5564 0.076 Uiso 1 1 calc R . . C5 C 0.7981(8) 0.8514(4) 0.5249(5) 0.059(2) Uani 1 1 d . . . C6 C 0.7096(9) 0.8126(4) 0.5069(5) 0.070(3) Uani 1 1 d . . . H6A H 0.6328 0.8245 0.4920 0.084 Uiso 1 1 calc R . . C7 C 0.7339(9) 0.7568(4) 0.5107(5) 0.074(3) Uani 1 1 d . . . H7A H 0.6734 0.7315 0.4984 0.088 Uiso 1 1 calc R . . C8 C 0.7739(8) 0.9125(4) 0.5174(4) 0.056(2) Uani 1 1 d . . . C9 C 0.8434(8) 0.9420(4) 0.4733(5) 0.060(2) Uani 1 1 d . . . C10 C 0.9384(8) 0.9184(4) 0.4339(5) 0.069(3) Uani 1 1 d . . . H10A H 0.9707 0.8829 0.4370 0.083 Uiso 1 1 calc R . . C11 C 0.9698(9) 0.9575(4) 0.3928(5) 0.068(3) Uani 1 1 d . . . H11A H 1.0289 0.9542 0.3617 0.082 Uiso 1 1 calc R . . C12 C 0.8990(8) 1.0049(4) 0.4041(5) 0.062(2) Uani 1 1 d . . . C13 C 0.8956(8) 1.0513(3) 0.3650(5) 0.058(2) Uani 1 1 d . . . C14 C 0.9668(9) 1.0507(3) 0.3047(5) 0.061(2) Uani 1 1 d . . . C15 C 1.0954(9) 1.0494(4) 0.3067(5) 0.068(3) Uani 1 1 d . . . H15A H 1.1387 1.0497 0.3458 0.081 Uiso 1 1 calc R . . C16 C 1.1563(10) 1.0476(4) 0.2502(6) 0.074(3) Uani 1 1 d . . . H16A H 1.2416 1.0463 0.2515 0.088 Uiso 1 1 calc R . . C17 C 1.0941(10) 1.0478(4) 0.1910(5) 0.068(3) Uani 1 1 d . . . C18 C 1.1626(12) 1.0460(4) 0.1299(7) 0.078(3) Uani 1 1 d . . . C19 C 0.9693(9) 1.0510(4) 0.1899(5) 0.068(3) Uani 1 1 d . . . H19A H 0.9259 1.0533 0.1510 0.082 Uiso 1 1 calc R . . C20 C 0.9069(9) 1.0509(4) 0.2471(5) 0.066(2) Uani 1 1 d . . . H20A H 0.8215 1.0510 0.2456 0.079 Uiso 1 1 calc R . . C21 C 0.8294(8) 1.0988(4) 0.3800(5) 0.060(2) Uani 1 1 d . . . C22 C 0.8335(9) 1.1494(4) 0.3442(5) 0.068(3) Uani 1 1 d . . . H22A H 0.8704 1.1544 0.3049 0.082 Uiso 1 1 calc R . . C23 C 0.7745(8) 1.1885(4) 0.3775(5) 0.063(2) Uani 1 1 d . . . H23A H 0.7647 1.2255 0.3664 0.075 Uiso 1 1 calc R . . C24 C 0.7303(8) 1.1617(4) 0.4330(5) 0.062(2) Uani 1 1 d . . . C25 C 0.6749(8) 1.1903(4) 0.4837(5) 0.062(2) Uani 1 1 d . . . C26 C 0.6685(8) 1.2512(3) 0.4798(4) 0.056(2) Uani 1 1 d . . . C27 C 0.7591(9) 1.2821(4) 0.5067(6) 0.074(3) Uani 1 1 d . . . H27A H 0.8247 1.2641 0.5272 0.089 Uiso 1 1 calc R . . C28 C 0.7592(10) 1.3388(4) 0.5053(6) 0.083(3) Uani 1 1 d . . . H28A H 0.8247 1.3582 0.5241 0.099 Uiso 1 1 calc R . . C29 C 0.6633(8) 1.3675(4) 0.4763(5) 0.062(2) Uani 1 1 d . . . C30 C 0.6630(9) 1.4290(4) 0.4747(5) 0.064(3) Uani 1 1 d . . . C31 C 0.5664(9) 1.3370(4) 0.4484(5) 0.070(3) Uani 1 1 d . . . H31A H 0.4993 1.3547 0.4290 0.083 Uiso 1 1 calc R . . C32 C 0.5730(9) 1.2791(4) 0.4502(6) 0.074(3) Uani 1 1 d . . . H32A H 0.5100 1.2588 0.4306 0.089 Uiso 1 1 calc R . . C33 C 0.6252(8) 1.1643(4) 0.5355(5) 0.060(2) Uani 1 1 d . . . C34 C 0.5639(8) 1.1911(4) 0.5865(5) 0.070(3) Uani 1 1 d . . . H34A H 0.5551 1.2291 0.5918 0.084 Uiso 1 1 calc R . . C35 C 0.5215(9) 1.1521(4) 0.6253(5) 0.067(2) Uani 1 1 d . . . H35A H 0.4763 1.1580 0.6618 0.081 Uiso 1 1 calc R . . C36 C 0.5579(8) 1.0992(4) 0.6006(5) 0.063(2) Uani 1 1 d . . . C37 C 0.5296(8) 1.0483(4) 0.6274(5) 0.062(2) Uani 1 1 d . . . C38 C 0.4508(9) 1.0490(4) 0.6848(5) 0.062(2) Uani 1 1 d . . . C39 C 0.3308(8) 1.0673(4) 0.6806(5) 0.067(2) Uani 1 1 d . . . H39A H 0.2967 1.0781 0.6412 0.080 Uiso 1 1 calc R . . C40 C 0.2618(9) 1.0696(4) 0.7344(5) 0.069(3) Uani 1 1 d . . . H40A H 0.1817 1.0827 0.7307 0.083 Uiso 1 1 calc R . . C41 C 0.3065(9) 1.0535(4) 0.7928(5) 0.065(2) Uani 1 1 d . . . C42 C 0.2254(11) 1.0555(4) 0.8511(6) 0.070(3) Uani 1 1 d . . . C43 C 0.4258(9) 1.0351(5) 0.7986(6) 0.081(3) Uani 1 1 d . . . H43A H 0.4593 1.0246 0.8383 0.097 Uiso 1 1 calc R . . C44 C 0.4949(10) 1.0328(5) 0.7437(6) 0.081(3) Uani 1 1 d . . . H44A H 0.5750 1.0196 0.7473 0.097 Uiso 1 1 calc R . . C45 C 0.5707(8) 0.9983(4) 0.6028(5) 0.064(2) Uani 1 1 d . . . C46 C 0.5379(10) 0.9454(4) 0.6282(6) 0.078(3) Uani 1 1 d . . . H46A H 0.4822 0.9384 0.6602 0.094 Uiso 1 1 calc R . . C47 C 0.6043(9) 0.9082(4) 0.5963(5) 0.073(3) Uani 1 1 d . . . H47A H 0.6002 0.8701 0.6014 0.088 Uiso 1 1 calc R . . C48 C 0.6818(8) 0.9365(4) 0.5537(5) 0.062(2) Uani 1 1 d . . . C49 C 1.1292(15) 0.5977(7) 0.6927(9) 0.129(5) Uiso 1 1 d . . . H49A H 1.0630 0.5809 0.7121 0.155 Uiso 1 1 calc R . . C50 C 1.3039(17) 0.6580(8) 0.7092(10) 0.161(7) Uiso 1 1 d . . . H50A H 1.3154 0.6487 0.6650 0.241 Uiso 1 1 calc R . . H50B H 1.3746 0.6465 0.7344 0.241 Uiso 1 1 calc R . . H50C H 1.2935 0.6972 0.7133 0.241 Uiso 1 1 calc R . . C51 C 1.1777(18) 0.6372(8) 0.8004(10) 0.165(7) Uiso 1 1 d . . . H51A H 1.1025 0.6186 0.8099 0.248 Uiso 1 1 calc R . . H51B H 1.1708 0.6756 0.8112 0.248 Uiso 1 1 calc R . . H51C H 1.2441 0.6209 0.8251 0.248 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0743(2) 0.0569(2) 0.0631(3) 0.00209(17) 0.01488(18) 0.00368(17) Pb2 0.0687(2) 0.0546(2) 0.0662(3) -0.00225(17) 0.01837(18) -0.00317(16) Cu1 0.0647(6) 0.0498(6) 0.0573(7) -0.0001(5) 0.0163(5) 0.0033(5) O1 0.110(5) 0.048(4) 0.119(7) -0.001(4) 0.016(5) -0.003(4) O2 0.070(4) 0.068(4) 0.124(7) 0.018(4) 0.014(4) 0.017(3) O3 0.094(5) 0.098(5) 0.081(6) -0.014(4) 0.040(4) -0.017(4) O4 0.119(6) 0.079(5) 0.056(5) -0.005(4) 0.022(5) -0.006(4) O5 0.074(4) 0.060(4) 0.082(5) -0.007(3) 0.013(4) -0.003(3) O6 0.075(4) 0.061(4) 0.091(6) 0.003(4) 0.021(4) 0.007(3) O7 0.083(4) 0.091(5) 0.065(5) 0.009(4) 0.028(4) 0.016(4) O8 0.104(5) 0.074(4) 0.071(5) 0.000(4) 0.020(4) 0.001(4) O9 0.085(5) 0.115(6) 0.071(5) -0.008(5) 0.010(4) 0.017(4) O10 0.090(6) 0.172(11) 0.308(19) -0.102(12) -0.007(9) 0.030(7) N1 0.067(4) 0.048(4) 0.058(5) 0.004(3) 0.012(4) 0.004(3) N2 0.066(4) 0.050(4) 0.061(5) 0.002(3) 0.021(4) 0.005(3) N3 0.067(4) 0.053(4) 0.060(5) -0.004(4) 0.013(4) 0.001(3) N4 0.068(4) 0.054(4) 0.061(5) 0.000(4) 0.015(4) -0.001(4) C1 0.091(7) 0.039(5) 0.089(8) -0.004(5) 0.025(6) -0.014(5) C2 0.078(6) 0.053(5) 0.074(7) 0.008(5) 0.021(5) 0.002(5) C3 0.071(6) 0.057(6) 0.094(8) 0.002(5) -0.006(6) 0.002(5) C4 0.057(5) 0.065(6) 0.067(6) -0.002(5) -0.003(4) -0.005(4) C5 0.063(5) 0.056(5) 0.060(6) -0.004(4) 0.014(4) -0.004(4) C6 0.081(6) 0.057(6) 0.072(7) 0.000(5) 0.006(5) -0.003(5) C7 0.074(6) 0.062(6) 0.085(8) -0.005(5) -0.004(5) -0.008(5) C8 0.060(5) 0.052(5) 0.057(6) 0.001(4) 0.000(4) -0.003(4) C9 0.070(5) 0.051(5) 0.061(6) -0.006(4) 0.010(5) 0.002(4) C10 0.073(6) 0.047(5) 0.089(8) -0.008(5) 0.019(5) 0.019(4) C11 0.071(6) 0.057(5) 0.078(7) 0.000(5) 0.025(5) 0.004(5) C12 0.071(5) 0.057(5) 0.058(6) 0.008(4) 0.017(5) 0.006(4) C13 0.070(5) 0.053(5) 0.053(6) -0.005(4) 0.014(4) -0.002(4) C14 0.077(6) 0.042(4) 0.066(7) 0.001(4) 0.026(5) -0.008(4) C15 0.075(6) 0.068(6) 0.062(7) -0.003(5) 0.021(5) -0.003(5) C16 0.075(6) 0.073(6) 0.074(8) -0.004(5) 0.023(6) 0.003(5) C17 0.098(7) 0.049(5) 0.057(7) -0.009(4) 0.029(6) -0.005(5) C18 0.095(8) 0.056(6) 0.085(9) -0.014(6) 0.033(7) -0.006(5) C19 0.076(6) 0.055(5) 0.073(7) -0.013(5) 0.010(5) 0.005(5) C20 0.074(6) 0.064(6) 0.061(7) -0.001(5) 0.014(5) -0.001(5) C21 0.067(5) 0.055(5) 0.059(6) 0.000(4) 0.017(5) 0.000(4) C22 0.079(6) 0.055(5) 0.072(7) 0.004(5) 0.017(5) -0.006(5) C23 0.076(6) 0.047(5) 0.065(6) 0.005(4) 0.018(5) 0.008(4) C24 0.068(5) 0.048(5) 0.071(7) -0.002(4) 0.020(5) -0.003(4) C25 0.066(5) 0.055(5) 0.067(7) -0.001(4) 0.011(5) 0.007(4) C26 0.058(5) 0.047(5) 0.063(6) 0.003(4) 0.013(4) 0.008(4) C27 0.066(6) 0.052(5) 0.104(9) 0.005(5) 0.000(6) 0.018(5) C28 0.075(6) 0.059(6) 0.115(10) 0.004(6) 0.029(6) 0.007(5) C29 0.065(5) 0.052(5) 0.071(7) -0.009(4) 0.025(5) -0.001(4) C30 0.074(6) 0.058(5) 0.062(6) -0.003(5) 0.033(5) 0.002(5) C31 0.064(5) 0.063(6) 0.082(7) 0.001(5) 0.004(5) 0.004(5) C32 0.076(6) 0.053(5) 0.095(8) -0.004(5) 0.012(6) 0.004(5) C33 0.061(5) 0.056(5) 0.064(6) -0.004(4) 0.009(4) 0.003(4) C34 0.067(5) 0.062(6) 0.081(8) -0.014(5) 0.011(5) 0.004(5) C35 0.077(6) 0.066(6) 0.059(6) -0.005(5) 0.025(5) 0.004(5) C36 0.064(5) 0.062(6) 0.064(6) -0.006(5) 0.018(5) -0.001(4) C37 0.067(5) 0.065(6) 0.055(6) 0.003(5) 0.011(4) 0.002(4) C38 0.078(6) 0.058(5) 0.052(6) 0.011(4) 0.014(5) 0.013(5) C39 0.066(6) 0.074(6) 0.062(7) -0.008(5) 0.014(5) 0.002(5) C40 0.070(6) 0.067(6) 0.071(7) 0.001(5) 0.020(5) 0.007(5) C41 0.073(6) 0.060(5) 0.062(7) 0.008(5) 0.022(5) 0.000(5) C42 0.094(7) 0.046(5) 0.069(7) 0.005(5) 0.014(6) 0.002(5) C43 0.079(7) 0.104(8) 0.061(7) 0.019(6) 0.010(5) 0.010(6) C44 0.083(6) 0.093(8) 0.069(8) 0.004(6) 0.025(6) 0.024(6) C45 0.066(5) 0.059(5) 0.068(7) 0.007(5) 0.020(5) 0.007(4) C46 0.081(6) 0.063(6) 0.092(9) 0.004(6) 0.027(6) 0.001(5) C47 0.081(6) 0.062(6) 0.078(7) -0.002(5) 0.025(6) 0.003(5) C48 0.073(6) 0.052(5) 0.061(6) 0.002(4) 0.015(5) -0.002(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 Pb1 O2 2.318(7) . ? Pb1 O7 2.340(7) 2_646 ? Pb1 O9 2.397(8) . ? Pb2 O3 2.430(8) 2_755 ? Pb2 O6 2.486(7) . ? Pb2 O5 2.518(6) . ? Pb2 O8 2.693(8) 2_656 ? Pb2 C30 2.852(10) . ? Cu1 N3 1.992(7) . ? Cu1 N2 1.995(7) . ? Cu1 N1 1.998(7) . ? Cu1 N4 1.999(7) . ? O1 C1 1.228(12) . ? O2 C1 1.257(12) . ? O3 C18 1.271(13) . ? O3 Pb2 2.430(8) 2_745 ? O4 C18 1.226(14) . ? O5 C30 1.264(11) . ? O6 C30 1.260(11) . ? O7 C42 1.260(12) . ? O7 Pb1 2.340(7) 2_656 ? O8 C42 1.229(12) . ? O8 Pb2 2.693(8) 2_646 ? O9 C49 1.145(18) . ? N1 C9 1.357(11) . ? N1 C12 1.383(11) . ? N2 C21 1.362(11) . ? N2 C24 1.365(11) . ? N3 C36 1.386(12) . ? N3 C33 1.394(11) . ? N4 C48 1.364(11) . ? N4 C45 1.371(11) . ? N5 C50 1.370(19) . ? N5 C49 1.373(18) . ? N5 C51 1.49(2) . ? C1 C2 1.523(13) . ? C2 C3 1.377(14) . ? C2 C7 1.383(14) . ? C3 C4 1.387(13) . ? C3 H3A 0.9300 . ? C4 C5 1.376(12) . ? C4 H4A 0.9300 . ? C5 C6 1.389(13) . ? C5 C8 1.508(12) . ? C6 C7 1.376(13) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C48 1.401(13) . ? C8 C9 1.405(13) . ? C9 C10 1.457(13) . ? C10 C11 1.330(14) . ? C10 H10A 0.9300 . ? C11 C12 1.405(12) . ? C11 H11A 0.9300 . ? C12 C13 1.388(12) . ? C13 C21 1.395(12) . ? C13 C14 1.498(13) . ? C14 C20 1.351(14) . ? C14 C15 1.402(13) . ? C15 C16 1.371(14) . ? C15 H15A 0.9300 . ? C16 C17 1.392(15) . ? C16 H16A 0.9300 . ? C17 C19 1.362(14) . ? C17 C18 1.496(15) . ? C19 C20 1.390(14) . ? C19 H19A 0.9300 . ? C20 H20A 0.9300 . ? C21 C22 1.437(13) . ? C22 C23 1.346(13) . ? C22 H22A 0.9300 . ? C23 C24 1.423(13) . ? C23 H23A 0.9300 . ? C24 C25 1.414(12) . ? C25 C33 1.374(13) . ? C25 C26 1.479(12) . ? C26 C27 1.347(13) . ? C26 C32 1.371(13) . ? C27 C28 1.372(14) . ? C27 H27A 0.9300 . ? C28 C29 1.378(14) . ? C28 H28A 0.9300 . ? C29 C31 1.401(13) . ? C29 C30 1.489(13) . ? C31 C32 1.401(13) . ? C31 H31A 0.9300 . ? C32 H32A 0.9300 . ? C33 C34 1.430(13) . ? C34 C35 1.335(14) . ? C34 H34A 0.9300 . ? C35 C36 1.439(13) . ? C35 H35A 0.9300 . ? C36 C37 1.390(13) . ? C37 C45 1.394(13) . ? C37 C38 1.493(13) . ? C38 C44 1.364(14) . ? C38 C39 1.381(13) . ? C39 C40 1.369(13) . ? C39 H39A 0.9300 . ? C40 C41 1.357(14) . ? C40 H40A 0.9300 . ? C41 C43 1.375(14) . ? C41 C42 1.526(14) . ? C43 C44 1.391(14) . ? C43 H43A 0.9300 . ? C44 H44A 0.9300 . ? C45 C46 1.432(13) . ? C46 C47 1.343(14) . ? C46 H46A 0.9300 . ? C47 C48 1.421(13) . ? C47 H47A 0.9300 . ? C49 H49A 0.9300 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Pb1 O7 83.3(3) . 2_646 ? O2 Pb1 O9 79.4(3) . . ? O7 Pb1 O9 76.6(3) 2_646 . ? O3 Pb2 O6 87.1(3) 2_755 . ? O3 Pb2 O5 85.5(2) 2_755 . ? O6 Pb2 O5 52.4(2) . . ? O3 Pb2 O8 143.5(3) 2_755 2_656 ? O6 Pb2 O8 98.2(2) . 2_656 ? O5 Pb2 O8 70.2(2) . 2_656 ? O3 Pb2 C30 86.7(3) 2_755 . ? O6 Pb2 C30 26.2(2) . . ? O5 Pb2 C30 26.3(2) . . ? O8 Pb2 C30 83.1(3) 2_656 . ? N3 Cu1 N2 90.2(3) . . ? N3 Cu1 N1 173.5(3) . . ? N2 Cu1 N1 89.8(3) . . ? N3 Cu1 N4 90.2(3) . . ? N2 Cu1 N4 174.7(3) . . ? N1 Cu1 N4 90.4(3) . . ? C1 O2 Pb1 106.0(6) . . ? C18 O3 Pb2 103.9(8) . 2_745 ? C30 O5 Pb2 91.8(6) . . ? C30 O6 Pb2 93.4(6) . . ? C42 O7 Pb1 107.5(7) . 2_656 ? C42 O8 Pb2 144.7(7) . 2_646 ? C49 O9 Pb1 126.5(10) . . ? C9 N1 C12 106.3(7) . . ? C9 N1 Cu1 126.8(6) . . ? C12 N1 Cu1 126.8(6) . . ? C21 N2 C24 106.4(7) . . ? C21 N2 Cu1 126.8(6) . . ? C24 N2 Cu1 126.8(6) . . ? C36 N3 C33 105.9(7) . . ? C36 N3 Cu1 126.9(6) . . ? C33 N3 Cu1 126.8(6) . . ? C48 N4 C45 106.7(7) . . ? C48 N4 Cu1 126.6(6) . . ? C45 N4 Cu1 126.2(6) . . ? C50 N5 C49 123.5(15) . . ? C50 N5 C51 116.3(14) . . ? C49 N5 C51 120.1(14) . . ? O1 C1 O2 125.1(9) . . ? O1 C1 C2 117.8(10) . . ? O2 C1 C2 117.2(9) . . ? C3 C2 C7 118.9(9) . . ? C3 C2 C1 119.6(9) . . ? C7 C2 C1 121.5(9) . . ? C2 C3 C4 120.0(9) . . ? C2 C3 H3A 120.0 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 121.6(9) . . ? C5 C4 H4A 119.2 . . ? C3 C4 H4A 119.2 . . ? C4 C5 C6 117.7(9) . . ? C4 C5 C8 121.1(8) . . ? C6 C5 C8 121.1(8) . . ? C7 C6 C5 121.0(9) . . ? C7 C6 H6A 119.5 . . ? C5 C6 H6A 119.5 . . ? C6 C7 C2 120.7(9) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C48 C8 C9 123.4(8) . . ? C48 C8 C5 118.5(8) . . ? C9 C8 C5 118.1(8) . . ? N1 C9 C8 125.7(8) . . ? N1 C9 C10 108.9(8) . . ? C8 C9 C10 125.1(8) . . ? C11 C10 C9 106.6(8) . . ? C11 C10 H10A 126.7 . . ? C9 C10 H10A 126.7 . . ? C10 C11 C12 108.6(8) . . ? C10 C11 H11A 125.7 . . ? C12 C11 H11A 125.7 . . ? N1 C12 C13 125.7(8) . . ? N1 C12 C11 109.5(8) . . ? C13 C12 C11 124.5(9) . . ? C12 C13 C21 122.7(9) . . ? C12 C13 C14 118.6(8) . . ? C21 C13 C14 118.7(8) . . ? C20 C14 C15 118.9(9) . . ? C20 C14 C13 119.9(9) . . ? C15 C14 C13 121.2(9) . . ? C16 C15 C14 119.0(10) . . ? C16 C15 H15A 120.5 . . ? C14 C15 H15A 120.5 . . ? C15 C16 C17 121.8(10) . . ? C15 C16 H16A 119.1 . . ? C17 C16 H16A 119.1 . . ? C19 C17 C16 118.4(9) . . ? C19 C17 C18 120.8(11) . . ? C16 C17 C18 120.9(10) . . ? O4 C18 O3 121.8(11) . . ? O4 C18 C17 120.2(11) . . ? O3 C18 C17 118.1(12) . . ? C17 C19 C20 120.0(10) . . ? C17 C19 H19A 120.0 . . ? C20 C19 H19A 120.0 . . ? C14 C20 C19 121.8(9) . . ? C14 C20 H20A 119.1 . . ? C19 C20 H20A 119.1 . . ? N2 C21 C13 126.6(8) . . ? N2 C21 C22 108.9(8) . . ? C13 C21 C22 124.1(9) . . ? C23 C22 C21 107.9(9) . . ? C23 C22 H22A 126.1 . . ? C21 C22 H22A 126.1 . . ? C22 C23 C24 106.2(8) . . ? C22 C23 H23A 126.9 . . ? C24 C23 H23A 126.9 . . ? N2 C24 C25 125.7(9) . . ? N2 C24 C23 110.6(8) . . ? C25 C24 C23 123.3(8) . . ? C33 C25 C24 123.5(8) . . ? C33 C25 C26 118.7(8) . . ? C24 C25 C26 117.8(8) . . ? C27 C26 C32 116.9(8) . . ? C27 C26 C25 119.7(8) . . ? C32 C26 C25 123.4(8) . . ? C26 C27 C28 123.1(10) . . ? C26 C27 H27A 118.5 . . ? C28 C27 H27A 118.5 . . ? C27 C28 C29 120.7(11) . . ? C27 C28 H28A 119.7 . . ? C29 C28 H28A 119.7 . . ? C28 C29 C31 118.1(9) . . ? C28 C29 C30 120.9(9) . . ? C31 C29 C30 121.0(9) . . ? O6 C30 O5 122.3(9) . . ? O6 C30 C29 119.6(9) . . ? O5 C30 C29 118.1(9) . . ? O6 C30 Pb2 60.5(5) . . ? O5 C30 Pb2 61.9(5) . . ? C29 C30 Pb2 177.5(6) . . ? C32 C31 C29 118.4(9) . . ? C32 C31 H31A 120.8 . . ? C29 C31 H31A 120.8 . . ? C26 C32 C31 122.8(10) . . ? C26 C32 H32A 118.6 . . ? C31 C32 H32A 118.6 . . ? C25 C33 N3 125.3(8) . . ? C25 C33 C34 125.5(9) . . ? N3 C33 C34 109.2(8) . . ? C35 C34 C33 107.9(9) . . ? C35 C34 H34A 126.0 . . ? C33 C34 H34A 126.0 . . ? C34 C35 C36 108.0(9) . . ? C34 C35 H35A 126.0 . . ? C36 C35 H35A 126.0 . . ? N3 C36 C37 125.8(8) . . ? N3 C36 C35 109.0(8) . . ? C37 C36 C35 125.2(9) . . ? C36 C37 C45 122.8(9) . . ? C36 C37 C38 116.8(8) . . ? C45 C37 C38 120.3(8) . . ? C44 C38 C39 117.2(9) . . ? C44 C38 C37 121.5(9) . . ? C39 C38 C37 121.3(9) . . ? C40 C39 C38 120.2(10) . . ? C40 C39 H39A 119.9 . . ? C38 C39 H39A 119.9 . . ? C41 C40 C39 122.2(10) . . ? C41 C40 H40A 118.9 . . ? C39 C40 H40A 118.9 . . ? C40 C41 C43 119.0(10) . . ? C40 C41 C42 120.4(9) . . ? C43 C41 C42 120.6(10) . . ? O8 C42 O7 123.9(10) . . ? O8 C42 C41 119.1(10) . . ? O7 C42 C41 116.9(10) . . ? C41 C43 C44 118.3(10) . . ? C41 C43 H43A 120.9 . . ? C44 C43 H43A 120.9 . . ? C38 C44 C43 123.0(10) . . ? C38 C44 H44A 118.5 . . ? C43 C44 H44A 118.5 . . ? N4 C45 C37 126.4(8) . . ? N4 C45 C46 109.9(8) . . ? C37 C45 C46 123.4(9) . . ? C47 C46 C45 105.6(9) . . ? C47 C46 H46A 127.2 . . ? C45 C46 H46A 127.2 . . ? C46 C47 C48 109.1(9) . . ? C46 C47 H47A 125.5 . . ? C48 C47 H47A 125.5 . . ? N4 C48 C8 125.4(8) . . ? N4 C48 C47 108.5(8) . . ? C8 C48 C47 125.9(8) . . ? O9 C49 N5 126.4(17) . . ? O9 C49 H49A 116.8 . . ? N5 C49 H49A 116.8 . . ? N5 C50 H50A 109.5 . . ? N5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.611 _refine_diff_density_min -0.728 _refine_diff_density_rms 0.168 # Attachment '- New5.cif' data_New5 _database_code_depnum_ccdc_archive 'CCDC 871470' #TrackingRef '- New5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H28 N4 O11 Pb2 V' _chemical_formula_weight 1302.06 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.0753 8.5060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2432(15) _cell_length_b 11.5390(18) _cell_length_c 16.397(2) _cell_angle_alpha 100.295(12) _cell_angle_beta 90.639(13) _cell_angle_gamma 107.891(15) _cell_volume 1456.7(4) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8547 _cell_measurement_theta_min 5.65 _cell_measurement_theta_max 63.69 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.484 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 619 _exptl_absorpt_coefficient_mu 12.801 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.198 _exptl_absorpt_correction_T_max 0.408 _exptl_absorpt_process_details CrysAlisPro _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Atlas, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3592 _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% ? _diffrn_reflns_number 8547 _diffrn_reflns_av_R_equivalents 0.0890 _diffrn_reflns_av_sigmaI/netI 0.1191 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 5.65 _diffrn_reflns_theta_max 63.69 _reflns_number_total 4633 _reflns_number_gt 3063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_cell_refinement 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_data_reduction 'CrysAlisPro (Oxford Diffraction Ltd., 2010)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 -0.033 0.000 279 61 ' ' 2 0.500 -0.036 0.250 284 60 ' ' 3 0.000 -0.021 0.500 279 61 ' ' 4 0.500 -0.045 0.750 284 60 ' ' _platon_squeeze_details ; ; _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^)+(0.0653P)^2^+6.1170P] 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 4633 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1097 _refine_ls_R_factor_gt 0.0898 _refine_ls_wR_factor_ref 0.2161 _refine_ls_wR_factor_gt 0.2043 _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_restrained_S_all 1.006 _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 Pb1 Pb 2.21340(9) 0.43080(6) 0.99981(4) 0.0964(3) Uani 1 1 d . . . V1 V 0.9814(10) 0.0372(6) 0.5106(5) 0.107(3) Uani 0.50 1 d P . . O1 O 2.0637(19) 0.2813(14) 0.8674(9) 0.129(5) Uani 1 1 d . . . O2 O 1.9174(16) 0.3846(11) 0.9402(8) 0.104(3) Uani 1 1 d . . . O3 O 0.4583(16) -0.5215(11) 0.9005(8) 0.103(3) Uani 1 1 d . . . O4 O 0.2765(18) -0.4161(12) 0.9079(8) 0.113(4) Uani 1 1 d . . . O5 O 0.944(3) 0.152(2) 0.5526(17) 0.113(7) Uani 0.50 1 d P . . O6 O 2.308(4) 0.211(4) 0.9952(16) 0.256(14) Uani 1 1 d . . . N1 N 1.0511(18) -0.0341(11) 0.6126(8) 0.090(3) Uani 1 1 d . . . N2 N 0.7512(17) -0.1028(12) 0.5020(8) 0.092(3) Uani 1 1 d . . . C1 C 1.931(3) 0.3119(19) 0.8794(12) 0.104(5) Uani 1 1 d . . . C2 C 1.783(2) 0.2460(14) 0.8172(10) 0.088(4) Uani 1 1 d . . . C3 C 1.793(2) 0.1706(16) 0.7442(12) 0.100(5) Uani 1 1 d . . . H3A H 1.8951 0.1541 0.7331 0.121 Uiso 1 1 calc R . . C4 C 1.655(3) 0.1188(16) 0.6871(10) 0.100(5) Uani 1 1 d . . . H4A H 1.6660 0.0678 0.6382 0.120 Uiso 1 1 calc R . . C5 C 1.503(2) 0.1392(15) 0.6992(10) 0.090(4) Uani 1 1 d . . . C6 C 1.485(2) 0.2142(16) 0.7764(11) 0.100(5) Uani 1 1 d . . . H6A H 1.3823 0.2291 0.7871 0.121 Uiso 1 1 calc R . . C7 C 1.619(3) 0.2627(15) 0.8330(12) 0.104(5) Uani 1 1 d . . . H7A H 1.6056 0.3082 0.8838 0.125 Uiso 1 1 calc R . . C8 C 1.355(2) 0.0902(15) 0.6368(10) 0.094(4) Uani 1 1 d . . . C9 C 1.202(2) 0.0097(15) 0.6593(10) 0.094(4) Uani 1 1 d . . . C10 C 1.188(2) -0.0418(16) 0.7329(11) 0.100(5) Uani 1 1 d . . . H10A H 1.2754 -0.0284 0.7730 0.120 Uiso 1 1 calc R . . C11 C 1.025(2) -0.1128(18) 0.7339(11) 0.107(5) Uani 1 1 d . . . H11A H 0.9788 -0.1559 0.7753 0.129 Uiso 1 1 calc R . . C12 C 0.937(2) -0.1096(15) 0.6586(10) 0.096(4) Uani 1 1 d . . . C13 C 0.767(2) -0.1703(16) 0.6348(11) 0.099(5) Uani 1 1 d . . . C14 C 0.665(2) -0.2439(16) 0.6957(10) 0.093(4) Uani 1 1 d . . . C15 C 0.536(3) -0.2094(17) 0.7357(12) 0.106(5) Uani 1 1 d . . . H15A H 0.5068 -0.1422 0.7237 0.127 Uiso 1 1 calc R . . C16 C 0.448(2) -0.2752(17) 0.7941(13) 0.105(5) Uani 1 1 d . . . H16A H 0.3614 -0.2512 0.8210 0.126 Uiso 1 1 calc R . . C17 C 0.489(2) -0.3746(14) 0.8118(10) 0.083(4) Uani 1 1 d . . . C18 C 0.610(2) -0.4143(15) 0.7680(10) 0.096(5) Uani 1 1 d . . . H18A H 0.6318 -0.4857 0.7764 0.116 Uiso 1 1 calc R . . C19 C 0.699(2) -0.3463(17) 0.7108(11) 0.098(5) Uani 1 1 d . . . H19A H 0.7831 -0.3719 0.6826 0.118 Uiso 1 1 calc R . . C20 C 0.406(2) -0.4408(15) 0.8777(10) 0.087(4) Uani 1 1 d . . . C21 C 0.681(2) -0.1687(14) 0.5635(10) 0.091(4) Uani 1 1 d . . . C22 C 0.511(2) -0.2351(19) 0.5372(13) 0.119(6) Uani 1 1 d . . . H22A H 0.4361 -0.2889 0.5659 0.143 Uiso 1 1 calc R . . C23 C 0.471(2) -0.2097(19) 0.4635(12) 0.123(7) Uani 1 1 d . . . H23A H 0.3647 -0.2376 0.4344 0.148 Uiso 1 1 calc R . . C24 C 1.373(2) 0.1309(14) 0.5605(10) 0.093(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0901(5) 0.1075(5) 0.0827(4) 0.0308(3) 0.0056(3) 0.0113(3) V1 0.100(5) 0.121(7) 0.089(5) 0.028(5) 0.010(3) 0.014(5) O1 0.093(9) 0.160(11) 0.105(9) -0.017(8) -0.026(7) 0.023(8) O2 0.101(8) 0.121(8) 0.077(7) 0.009(6) -0.007(6) 0.021(6) O3 0.099(8) 0.107(7) 0.111(8) 0.034(7) 0.019(7) 0.036(7) O4 0.111(9) 0.144(9) 0.108(8) 0.070(7) 0.030(7) 0.048(8) O5 0.100(17) 0.112(16) 0.120(18) 0.033(14) 0.007(14) 0.015(13) O6 0.18(2) 0.42(4) 0.159(18) 0.06(2) -0.028(16) 0.06(2) N1 0.091(9) 0.099(8) 0.073(7) 0.028(6) 0.012(6) 0.013(7) N2 0.083(8) 0.104(8) 0.073(7) 0.024(6) 0.001(6) 0.002(6) C1 0.092(13) 0.125(13) 0.084(11) 0.023(11) 0.013(9) 0.016(10) C2 0.081(10) 0.096(9) 0.076(9) 0.015(8) -0.007(7) 0.014(8) C3 0.087(11) 0.106(11) 0.103(12) 0.019(10) 0.007(9) 0.022(9) C4 0.107(14) 0.108(11) 0.072(9) 0.009(8) 0.002(9) 0.021(10) C5 0.084(11) 0.099(10) 0.074(9) 0.021(8) 0.003(8) 0.007(8) C6 0.091(11) 0.114(11) 0.089(11) 0.025(9) -0.005(9) 0.018(9) C7 0.112(14) 0.096(10) 0.101(12) 0.028(9) 0.005(11) 0.021(9) C8 0.098(11) 0.105(10) 0.074(9) 0.030(8) 0.006(8) 0.017(9) C9 0.084(10) 0.107(10) 0.078(9) 0.023(8) 0.007(8) 0.007(8) C10 0.084(11) 0.125(12) 0.086(10) 0.046(9) 0.000(8) 0.009(9) C11 0.094(12) 0.135(13) 0.085(10) 0.038(10) 0.004(9) 0.014(10) C12 0.095(11) 0.103(10) 0.080(9) 0.026(8) 0.005(8) 0.014(9) C13 0.097(12) 0.109(11) 0.084(10) 0.022(8) 0.011(9) 0.019(9) C14 0.091(11) 0.100(10) 0.090(10) 0.036(8) 0.014(9) 0.021(9) C15 0.109(13) 0.116(12) 0.117(13) 0.060(10) 0.027(11) 0.048(11) C16 0.088(11) 0.112(11) 0.125(14) 0.042(10) 0.043(10) 0.034(9) C17 0.076(9) 0.093(9) 0.088(9) 0.037(8) 0.011(8) 0.028(8) C18 0.113(13) 0.100(10) 0.080(9) 0.040(8) 0.023(9) 0.026(9) C19 0.086(10) 0.115(12) 0.088(10) 0.021(9) 0.015(8) 0.022(9) C20 0.089(11) 0.088(9) 0.085(9) 0.021(8) 0.016(8) 0.025(8) C21 0.086(10) 0.097(9) 0.081(9) 0.027(8) 0.011(8) 0.011(8) C22 0.086(12) 0.146(15) 0.114(13) 0.065(12) -0.005(10) -0.001(10) C23 0.086(11) 0.150(15) 0.105(12) 0.063(11) -0.025(10) -0.025(10) C24 0.090(11) 0.098(10) 0.081(9) 0.030(8) 0.008(8) 0.008(8) _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 Pb1 O4 2.463(11) 1_765 ? Pb1 O2 2.481(12) . ? Pb1 O1 2.551(12) . ? Pb1 O3 2.597(11) 1_765 ? Pb1 O2 2.712(14) 2_967 ? Pb1 C1 2.86(2) . ? V1 V1 1.004(13) 2_756 ? V1 O5 1.50(3) . ? V1 N1 2.027(15) 2_756 ? V1 N2 2.063(14) . ? V1 N2 2.125(15) 2_756 ? V1 N1 2.136(16) . ? O1 C1 1.25(2) . ? O2 C1 1.21(2) . ? O2 Pb1 2.712(13) 2_967 ? O3 C20 1.251(19) . ? O3 Pb1 2.597(11) 1_345 ? O4 C20 1.27(2) . ? O4 Pb1 2.463(11) 1_345 ? N1 C9 1.36(2) . ? N1 C12 1.40(2) . ? N1 V1 2.027(15) 2_756 ? N2 C24 1.36(2) 2_756 ? N2 C21 1.397(19) . ? N2 V1 2.125(15) 2_756 ? C1 C2 1.50(3) . ? C2 C3 1.37(2) . ? C2 C7 1.44(3) . ? C3 C4 1.38(3) . ? C3 H3A 0.9300 . ? C4 C5 1.35(3) . ? C4 H4A 0.9300 . ? C5 C6 1.44(2) . ? C5 C8 1.48(2) . ? C6 C7 1.34(3) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C24 1.41(2) . ? C8 C9 1.42(2) . ? C9 C10 1.43(2) . ? C10 C11 1.34(2) . ? C10 H10A 0.9300 . ? C11 C12 1.44(2) . ? C11 H11A 0.9300 . ? C12 C13 1.38(2) . ? C13 C21 1.37(2) . ? C13 C14 1.52(2) . ? C14 C19 1.36(2) . ? C14 C15 1.38(3) . ? C15 C16 1.40(2) . ? C15 H15A 0.9300 . ? C16 C17 1.37(2) . ? C16 H16A 0.9300 . ? C17 C18 1.38(2) . ? C17 C20 1.49(2) . ? C18 C19 1.40(2) . ? C18 H18A 0.9300 . ? C19 H19A 0.9300 . ? C21 C22 1.39(2) . ? C22 C23 1.35(3) . ? C22 H22A 0.9300 . ? C23 C24 1.43(2) 2_756 ? C23 H23A 0.9300 . ? C24 N2 1.36(2) 2_756 ? C24 C23 1.43(2) 2_756 ? 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 O4 Pb1 O2 82.5(4) 1_765 . ? O4 Pb1 O1 83.2(5) 1_765 . ? O2 Pb1 O1 51.1(5) . . ? O4 Pb1 O3 51.3(4) 1_765 1_765 ? O2 Pb1 O3 117.4(4) . 1_765 ? O1 Pb1 O3 80.3(5) . 1_765 ? O4 Pb1 O2 70.7(4) 1_765 2_967 ? O2 Pb1 O2 68.8(4) . 2_967 ? O1 Pb1 O2 116.9(5) . 2_967 ? O3 Pb1 O2 117.6(4) 1_765 2_967 ? O4 Pb1 C1 81.4(5) 1_765 . ? O2 Pb1 C1 25.0(5) . . ? O1 Pb1 C1 26.0(5) . . ? O3 Pb1 C1 99.3(5) 1_765 . ? O2 Pb1 C1 92.2(6) 2_967 . ? V1 V1 O5 171.6(16) 2_756 . ? V1 V1 N1 82.2(10) 2_756 2_756 ? O5 V1 N1 104.8(12) . 2_756 ? V1 V1 N2 79.6(9) 2_756 . ? O5 V1 N2 104.8(11) . . ? N1 V1 N2 89.0(6) 2_756 . ? V1 V1 N2 72.7(9) 2_756 2_756 ? O5 V1 N2 102.7(10) . 2_756 ? N1 V1 N2 87.2(6) 2_756 2_756 ? N2 V1 N2 152.3(4) . 2_756 ? V1 V1 N1 70.1(10) 2_756 . ? O5 V1 N1 102.8(11) . . ? N1 V1 N1 152.2(4) 2_756 . ? N2 V1 N1 86.0(6) . . ? N2 V1 N1 84.6(6) 2_756 . ? C1 O1 Pb1 90.7(11) . . ? C1 O2 Pb1 95.1(13) . . ? C1 O2 Pb1 146.0(14) . 2_967 ? Pb1 O2 Pb1 111.2(4) . 2_967 ? C20 O3 Pb1 90.8(9) . 1_345 ? C20 O4 Pb1 96.7(11) . 1_345 ? C9 N1 C12 105.4(13) . . ? C9 N1 V1 126.2(10) . 2_756 ? C12 N1 V1 125.6(11) . 2_756 ? C9 N1 V1 126.9(10) . . ? C12 N1 V1 125.5(12) . . ? V1 N1 V1 27.8(4) 2_756 . ? C24 N2 C21 107.2(12) 2_756 . ? C24 N2 V1 124.4(10) 2_756 . ? C21 N2 V1 127.4(11) . . ? C24 N2 V1 125.6(10) 2_756 2_756 ? C21 N2 V1 122.7(12) . 2_756 ? V1 N2 V1 27.7(4) . 2_756 ? O2 C1 O1 123.1(19) . . ? O2 C1 C2 121(2) . . ? O1 C1 C2 116.1(18) . . ? O2 C1 Pb1 59.9(10) . . ? O1 C1 Pb1 63.3(10) . . ? C2 C1 Pb1 178.2(14) . . ? C3 C2 C7 117.0(16) . . ? C3 C2 C1 123.6(17) . . ? C7 C2 C1 119.4(16) . . ? C2 C3 C4 120.8(17) . . ? C2 C3 H3A 119.6 . . ? C4 C3 H3A 119.6 . . ? C5 C4 C3 122.7(16) . . ? C5 C4 H4A 118.7 . . ? C3 C4 H4A 118.7 . . ? C4 C5 C6 117.9(16) . . ? C4 C5 C8 123.7(15) . . ? C6 C5 C8 118.3(16) . . ? C7 C6 C5 119.5(18) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C6 C7 C2 121.8(17) . . ? C6 C7 H7A 119.1 . . ? C2 C7 H7A 119.1 . . ? C24 C8 C9 124.3(16) . . ? C24 C8 C5 117.9(14) . . ? C9 C8 C5 117.7(13) . . ? N1 C9 C8 125.0(15) . . ? N1 C9 C10 110.5(13) . . ? C8 C9 C10 124.4(16) . . ? C11 C10 C9 107.9(16) . . ? C11 C10 H10A 126.0 . . ? C9 C10 H10A 126.0 . . ? C10 C11 C12 106.8(16) . . ? C10 C11 H11A 126.6 . . ? C12 C11 H11A 126.6 . . ? C13 C12 N1 124.8(16) . . ? C13 C12 C11 125.9(16) . . ? N1 C12 C11 109.4(15) . . ? C21 C13 C12 126.7(16) . . ? C21 C13 C14 117.4(16) . . ? C12 C13 C14 115.9(16) . . ? C19 C14 C15 118.9(15) . . ? C19 C14 C13 120.1(16) . . ? C15 C14 C13 121.0(16) . . ? C14 C15 C16 120.3(16) . . ? C14 C15 H15A 119.9 . . ? C16 C15 H15A 119.9 . . ? C17 C16 C15 120.2(15) . . ? C17 C16 H16A 119.9 . . ? C15 C16 H16A 119.9 . . ? C16 C17 C18 119.6(14) . . ? C16 C17 C20 121.2(15) . . ? C18 C17 C20 119.2(15) . . ? C17 C18 C19 119.5(16) . . ? C17 C18 H18A 120.2 . . ? C19 C18 H18A 120.2 . . ? C14 C19 C18 121.2(16) . . ? C14 C19 H19A 119.4 . . ? C18 C19 H19A 119.4 . . ? O3 C20 O4 121.2(15) . . ? O3 C20 C17 120.7(15) . . ? O4 C20 C17 118.1(16) . . ? C13 C21 C22 126.9(16) . . ? C13 C21 N2 125.4(15) . . ? C22 C21 N2 107.6(15) . . ? C23 C22 C21 109.9(16) . . ? C23 C22 H22A 125.1 . . ? C21 C22 H22A 125.1 . . ? C22 C23 C24 106.0(16) . 2_756 ? C22 C23 H23A 127.0 . . ? C24 C23 H23A 127.0 2_756 . ? N2 C24 C8 126.4(14) 2_756 . ? N2 C24 C23 109.1(14) 2_756 2_756 ? C8 C24 C23 124.6(16) . 2_756 ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 63.69 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 2.199 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.196