data_General _audit_creation_date '2012-09-19' _audit_creation_method 'by CrystalStructure 3.6.0' _audit_update_record ? #============================================================================== # PROCESSING SUMMARY (IUCr Office Use Only) _journal_date_recd_electronic ? _journal_date_from_coeditor ? _journal_date_accepted ? _journal_coeditor_code ? #============================================================================== # SUBMISSION DETAILS _publ_contact_author_name 'Bao-Ming Ji' _publ_contact_author_address ; College of Chemistry, Chemical Engineering and Materials Science Suzhou University Suzhou 215123, Jiangsu P.R.China ; _publ_contact_author_email 'lyhxxjbm@126.com' _publ_contact_author_fax '86-372-65523821' _publ_contact_author_phone '86-372-65523821' _publ_contact_letter ; ENTER TEXT OF LETTER ; _publ_requested_journal ? _publ_requested_category 'FM' _publ_requested_coeditor_name ? #============================================================================== # TITLE AND AUTHOR LIST _publ_section_title ; ENTER SECTION TITLE ; _publ_section_title_footnote ; ENTER FOOTNOTE TO TITLE OF PAPER ; loop_ _publ_author_name _publ_author_footnote _publ_author_address ' FIRST AUTHORS NAME ' ; FIRST AUTHORS FOOTNOTES ; ; FIRST AUTHORS ADDRESS ; _publ_section_synopsis ; ENTER SYNOPSIS ; #============================================================================== data_1 #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 N4' _chemical_formula_sum 'C15 H12 N4' _chemical_formula_weight 248.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P-1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8839(15) _cell_length_b 8.8678(19) _cell_length_c 10.965(2) _cell_angle_alpha 90.466(3) _cell_angle_beta 102.738(3) _cell_angle_gamma 101.102(3) _cell_volume 639.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 896 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 24.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.289 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 260 _exptl_absorpt_coefficient_mu 0.081 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9746 _exptl_absorpt_correction_T_max 0.9880 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4770 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_sigmaI/netI 0.0398 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2358 _reflns_number_gt 1432 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0542P)^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 2358 _refine_ls_number_parameters 172 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0838 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.0967 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.7210(2) 0.2703(2) 0.67883(16) 0.0450(5) Uani 1 1 d . . . C2 C 0.7322(3) 0.2156(2) 0.56288(18) 0.0556(5) Uani 1 1 d . . . H2 H 0.7287 0.1114 0.5487 0.067 Uiso 1 1 calc R . . C3 C 0.7487(3) 0.3151(2) 0.46811(18) 0.0588(5) Uani 1 1 d . . . H3 H 0.7522 0.2741 0.3905 0.071 Uiso 1 1 calc R . . C4 C 0.7562(3) 0.5183(2) 0.59475(18) 0.0486(5) Uani 1 1 d . . . C5 C 0.7367(3) 0.4274(2) 0.69447(17) 0.0481(5) Uani 1 1 d . . . H5 H 0.7341 0.4712 0.7713 0.058 Uiso 1 1 calc R . . C6 C 0.7770(3) 0.6837(3) 0.61141(19) 0.0598(5) Uani 1 1 d . . . C7 C 0.6949(3) 0.1647(2) 0.78347(18) 0.0536(5) Uani 1 1 d . . . H7A H 0.6919 0.2257 0.8566 0.064 Uiso 1 1 calc R . . H7B H 0.8119 0.1162 0.8050 0.064 Uiso 1 1 calc R . . C8 C 0.5031(3) 0.0397(2) 0.75208(18) 0.0536(5) Uani 1 1 d . . . H8A H 0.5115 -0.0257 0.6829 0.064 Uiso 1 1 calc R . . H8B H 0.4995 -0.0235 0.8237 0.064 Uiso 1 1 calc R . . C9 C 0.3046(3) 0.0973(2) 0.71738(17) 0.0530(5) Uani 1 1 d . . . H9A H 0.3038 0.1556 0.6429 0.064 Uiso 1 1 calc R . . H9B H 0.1926 0.0094 0.6973 0.064 Uiso 1 1 calc R . . C10 C 0.2709(2) 0.1971(2) 0.81959(16) 0.0453(5) Uani 1 1 d . . . C11 C 0.2646(3) 0.3505(2) 0.80472(17) 0.0469(5) Uani 1 1 d . . . H11 H 0.2779 0.3947 0.7296 0.056 Uiso 1 1 calc R . . C12 C 0.2383(3) 0.4380(2) 0.90287(17) 0.0471(5) Uani 1 1 d . . . C13 C 0.2201(3) 0.2353(2) 1.02559(18) 0.0613(6) Uani 1 1 d . . . H13 H 0.2038 0.1931 1.1009 0.074 Uiso 1 1 calc R . . C14 C 0.2461(3) 0.1394(2) 0.93339(18) 0.0556(5) Uani 1 1 d . . . H14 H 0.2470 0.0363 0.9476 0.067 Uiso 1 1 calc R . . C15 C 0.2314(3) 0.5988(2) 0.88751(18) 0.0561(5) Uani 1 1 d . . . N1 N 0.7598(2) 0.46603(19) 0.48046(14) 0.0554(4) Uani 1 1 d . . . N2 N 0.7950(3) 0.8136(2) 0.62522(19) 0.0824(6) Uani 1 1 d . . . N3 N 0.2168(2) 0.38427(19) 1.01407(14) 0.0574(5) Uani 1 1 d . . . N4 N 0.2272(3) 0.7256(2) 0.87364(18) 0.0782(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0380(10) 0.0500(11) 0.0454(11) 0.0008(9) 0.0081(8) 0.0068(8) C2 0.0632(13) 0.0498(12) 0.0543(13) -0.0029(10) 0.0199(10) 0.0055(9) C3 0.0639(14) 0.0606(14) 0.0501(12) -0.0048(10) 0.0200(10) -0.0001(10) C4 0.0425(11) 0.0487(11) 0.0541(12) 0.0030(9) 0.0113(9) 0.0077(8) C5 0.0463(11) 0.0538(12) 0.0456(11) -0.0006(9) 0.0119(9) 0.0116(9) C6 0.0573(13) 0.0605(14) 0.0643(14) 0.0095(11) 0.0163(10) 0.0154(11) C7 0.0534(12) 0.0592(12) 0.0487(12) 0.0070(9) 0.0094(9) 0.0151(10) C8 0.0658(13) 0.0444(11) 0.0555(12) 0.0058(9) 0.0224(10) 0.0125(9) C9 0.0558(12) 0.0509(12) 0.0497(12) -0.0024(9) 0.0141(9) 0.0024(9) C10 0.0412(10) 0.0491(11) 0.0454(11) 0.0033(9) 0.0093(8) 0.0091(8) C11 0.0470(11) 0.0514(11) 0.0429(11) 0.0072(9) 0.0121(9) 0.0086(8) C12 0.0464(11) 0.0481(11) 0.0476(12) 0.0047(9) 0.0131(9) 0.0081(8) C13 0.0807(15) 0.0645(14) 0.0480(13) 0.0158(10) 0.0246(11) 0.0253(11) C14 0.0647(13) 0.0529(12) 0.0535(13) 0.0099(10) 0.0174(10) 0.0171(10) C15 0.0597(13) 0.0527(13) 0.0586(13) 0.0008(10) 0.0223(10) 0.0073(10) N1 0.0545(10) 0.0622(11) 0.0482(10) 0.0034(8) 0.0150(8) 0.0045(8) N2 0.0960(15) 0.0582(12) 0.0997(16) 0.0097(11) 0.0298(12) 0.0229(11) N3 0.0668(11) 0.0612(11) 0.0504(11) 0.0061(8) 0.0204(8) 0.0193(8) N4 0.0985(15) 0.0531(11) 0.0904(15) 0.0056(10) 0.0376(11) 0.0142(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.380(2) . ? C1 C5 1.383(2) . ? C1 C7 1.507(2) . ? C2 C3 1.379(3) . ? C2 H2 0.9300 . ? C3 N1 1.330(2) . ? C3 H3 0.9300 . ? C4 N1 1.340(2) . ? C4 C5 1.379(2) . ? C4 C6 1.452(3) . ? C5 H5 0.9300 . ? C6 N2 1.140(2) . ? C7 C8 1.523(2) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.521(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.507(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.379(2) . ? C10 C14 1.385(2) . ? C11 C12 1.386(2) . ? C11 H11 0.9300 . ? C12 N3 1.341(2) . ? C12 C15 1.446(3) . ? C13 N3 1.332(2) . ? C13 C14 1.379(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 N4 1.142(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 116.59(17) . . ? C2 C1 C7 121.80(17) . . ? C5 C1 C7 121.61(17) . . ? C1 C2 C3 120.06(19) . . ? C1 C2 H2 120.0 . . ? C3 C2 H2 120.0 . . ? N1 C3 C2 124.25(19) . . ? N1 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? N1 C4 C5 124.84(18) . . ? N1 C4 C6 115.75(17) . . ? C5 C4 C6 119.40(18) . . ? C4 C5 C1 119.18(17) . . ? C4 C5 H5 120.4 . . ? C1 C5 H5 120.4 . . ? N2 C6 C4 179.4(3) . . ? C1 C7 C8 113.98(15) . . ? C1 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C1 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 115.29(15) . . ? C9 C8 H8A 108.5 . . ? C7 C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? C7 C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 113.50(15) . . ? C10 C9 H9A 108.9 . . ? C8 C9 H9A 108.9 . . ? C10 C9 H9B 108.9 . . ? C8 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C14 116.74(17) . . ? C11 C10 C9 121.64(16) . . ? C14 C10 C9 121.62(18) . . ? C10 C11 C12 119.30(17) . . ? C10 C11 H11 120.3 . . ? C12 C11 H11 120.3 . . ? N3 C12 C11 124.59(17) . . ? N3 C12 C15 115.99(16) . . ? C11 C12 C15 119.43(17) . . ? N3 C13 C14 124.44(18) . . ? N3 C13 H13 117.8 . . ? C14 C13 H13 117.8 . . ? C13 C14 C10 119.86(19) . . ? C13 C14 H14 120.1 . . ? C10 C14 H14 120.1 . . ? N4 C15 C12 178.9(2) . . ? C3 N1 C4 115.01(16) . . ? C13 N3 C12 115.06(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C5 C1 C2 C3 -2.9(3) . . . . ? C7 C1 C2 C3 177.61(17) . . . . ? C1 C2 C3 N1 1.7(3) . . . . ? N1 C4 C5 C1 0.6(3) . . . . ? C6 C4 C5 C1 -178.70(16) . . . . ? C2 C1 C5 C4 1.8(2) . . . . ? C7 C1 C5 C4 -178.67(16) . . . . ? N1 C4 C6 N2 -115(24) . . . . ? C5 C4 C6 N2 64(24) . . . . ? C2 C1 C7 C8 -59.0(2) . . . . ? C5 C1 C7 C8 121.49(19) . . . . ? C1 C7 C8 C9 -59.1(2) . . . . ? C7 C8 C9 C10 -59.9(2) . . . . ? C8 C9 C10 C11 114.97(19) . . . . ? C8 C9 C10 C14 -64.6(2) . . . . ? C14 C10 C11 C12 1.2(2) . . . . ? C9 C10 C11 C12 -178.41(16) . . . . ? C10 C11 C12 N3 -0.3(3) . . . . ? C10 C11 C12 C15 -179.94(16) . . . . ? N3 C13 C14 C10 0.0(3) . . . . ? C11 C10 C14 C13 -1.0(3) . . . . ? C9 C10 C14 C13 178.57(17) . . . . ? N3 C12 C15 N4 167(12) . . . . ? C11 C12 C15 N4 -14(12) . . . . ? C2 C3 N1 C4 0.7(3) . . . . ? C5 C4 N1 C3 -1.9(3) . . . . ? C6 C4 N1 C3 177.45(16) . . . . ? C14 C13 N3 C12 0.9(3) . . . . ? C11 C12 N3 C13 -0.7(3) . . . . ? C15 C12 N3 C13 178.91(17) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.101 _refine_diff_density_min -0.143 _refine_diff_density_rms 0.033 #===END #============================================================================== data_2 #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 N2 O4 Pb' _chemical_formula_sum 'C15 H12 N2 O4 Pb' _chemical_formula_weight 491.46 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 'P 21/c' _symmetry_space_group_name_HALL '-P 2ybc' 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 12.5956(17) _cell_length_b 13.2999(18) _cell_length_c 9.7711(13) _cell_angle_alpha 90.00 _cell_angle_beta 101.025(2) _cell_angle_gamma 90.00 _cell_volume 1606.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 3458 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 22.03 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.29 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.032 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 10.519 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1504 _exptl_absorpt_correction_T_max 0.3908 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 12020 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_sigmaI/netI 0.0314 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.50 _reflns_number_total 2985 _reflns_number_gt 2349 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.1779P] 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 2985 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0410 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0716 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _refine_ls_shift/su_max 0.055 _refine_ls_shift/su_mean 0.004 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 0.021438(17) 0.358986(17) 0.12171(2) 0.05142(10) Uani 1 1 d . . . N1 N 0.2196(4) 0.3402(4) 0.1647(5) 0.0653(15) Uani 1 1 d . . . N2 N 0.9065(4) 0.5119(3) 0.6889(4) 0.0494(11) Uani 1 1 d . . . O1 O 0.1113(4) 0.4724(3) -0.0145(4) 0.0677(12) Uani 1 1 d . . . O2 O 0.2622(5) 0.5408(7) -0.0529(8) 0.167(4) Uani 1 1 d . . . O3 O 0.9601(4) 0.7049(3) 0.6396(4) 0.0653(12) Uani 1 1 d . . . O4 O 0.9269(4) 0.6744(3) 0.4112(5) 0.0711(12) Uani 1 1 d . . . C1 C 0.2764(6) 0.3987(7) 0.0937(7) 0.079(2) Uani 1 1 d . . . C2 C 0.3851(7) 0.3843(8) 0.1020(8) 0.111(3) Uani 1 1 d . . . H2 H 0.4228 0.4259 0.0514 0.133 Uiso 1 1 calc R . . C3 C 0.4392(6) 0.3098(9) 0.1832(8) 0.112(3) Uani 1 1 d . . . C4 C 0.3815(7) 0.2518(9) 0.2605(8) 0.117(3) Uani 1 1 d . . . H4 H 0.4160 0.2023 0.3201 0.140 Uiso 1 1 calc R . . C5 C 0.2706(6) 0.2685(7) 0.2479(7) 0.083(2) Uani 1 1 d . . . H5 H 0.2313 0.2288 0.2987 0.100 Uiso 1 1 calc R . . C6 C 0.2131(7) 0.4780(6) 0.0000(7) 0.081(2) Uani 1 1 d . . . C7 C 0.5606(6) 0.2927(9) 0.2032(8) 0.126(4) Uani 1 1 d . . . H7A H 0.5756 0.2215 0.2164 0.151 Uiso 1 1 calc R . . H7B H 0.5855 0.3137 0.1197 0.151 Uiso 1 1 calc R . . C8 C 0.6216(6) 0.3493(6) 0.3255(7) 0.092(3) Uani 1 1 d . . . H8A H 0.5944 0.3304 0.4083 0.110 Uiso 1 1 calc R . . H8B H 0.6089 0.4207 0.3104 0.110 Uiso 1 1 calc R . . C9 C 0.7452(5) 0.3287(5) 0.3502(6) 0.0575(15) Uani 1 1 d . . . H9A H 0.7588 0.2581 0.3715 0.069 Uiso 1 1 calc R . . H9B H 0.7723 0.3443 0.2662 0.069 Uiso 1 1 calc R . . C10 C 0.8035(4) 0.3924(4) 0.4699(6) 0.0461(13) Uani 1 1 d . . . C11 C 0.8391(4) 0.4880(4) 0.4470(6) 0.0486(13) Uani 1 1 d . . . H11 H 0.8287 0.5139 0.3570 0.058 Uiso 1 1 calc R . . C12 C 0.8899(4) 0.5444(4) 0.5574(6) 0.0432(13) Uani 1 1 d . . . C13 C 0.8749(5) 0.4189(4) 0.7101(6) 0.0533(15) Uani 1 1 d . . . H13 H 0.8887 0.3937 0.8005 0.064 Uiso 1 1 calc R . . C14 C 0.8221(5) 0.3575(4) 0.6034(6) 0.0572(15) Uani 1 1 d . . . H14 H 0.7998 0.2934 0.6229 0.069 Uiso 1 1 calc R . . C15 C 0.9279(5) 0.6509(4) 0.5343(7) 0.0548(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 0.04847(15) 0.04961(15) 0.05446(16) -0.00668(11) 0.00549(10) -0.00112(11) N1 0.048(3) 0.091(4) 0.056(3) 0.003(3) 0.005(3) -0.001(3) N2 0.061(3) 0.044(3) 0.045(3) -0.001(2) 0.014(2) -0.001(2) O1 0.062(3) 0.076(3) 0.066(3) 0.005(2) 0.015(2) 0.008(2) O2 0.098(5) 0.252(9) 0.156(6) 0.117(7) 0.032(4) -0.025(5) O3 0.090(3) 0.039(2) 0.074(3) -0.007(2) 0.034(3) -0.010(2) O4 0.088(3) 0.060(3) 0.067(3) 0.018(2) 0.019(3) -0.001(2) C1 0.053(4) 0.137(7) 0.049(4) 0.002(4) 0.012(3) -0.011(4) C2 0.054(5) 0.218(11) 0.060(5) 0.034(6) 0.010(4) 0.000(6) C3 0.054(5) 0.217(11) 0.063(5) -0.013(6) 0.006(4) -0.009(6) C4 0.061(5) 0.202(11) 0.083(6) 0.036(6) 0.002(4) 0.024(6) C5 0.052(4) 0.128(7) 0.066(4) 0.013(5) 0.001(3) 0.001(4) C6 0.082(5) 0.108(6) 0.051(4) 0.014(4) 0.012(4) -0.004(5) C7 0.065(5) 0.241(12) 0.070(5) -0.016(7) 0.007(4) 0.001(7) C8 0.056(4) 0.163(9) 0.054(4) -0.014(4) 0.006(3) -0.033(5) C9 0.050(4) 0.064(4) 0.056(4) -0.004(3) 0.004(3) -0.010(3) C10 0.033(3) 0.055(3) 0.050(3) -0.003(3) 0.008(2) 0.002(2) C11 0.042(3) 0.058(4) 0.045(3) 0.011(3) 0.007(2) 0.005(3) C12 0.046(3) 0.038(3) 0.050(3) 0.004(2) 0.020(3) 0.004(2) C13 0.075(4) 0.043(3) 0.041(3) 0.004(3) 0.009(3) -0.009(3) C14 0.065(4) 0.049(3) 0.058(4) 0.003(3) 0.014(3) -0.012(3) C15 0.053(4) 0.048(4) 0.068(4) 0.007(3) 0.022(3) 0.006(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 O1 2.430(4) . ? Pb1 O3 2.451(4) 3_666 ? Pb1 N1 2.463(5) . ? Pb1 N2 2.560(4) 3_666 ? Pb1 O4 2.575(4) 2_645 ? N1 C5 1.335(9) . ? N1 C1 1.338(9) . ? N2 C13 1.327(7) . ? N2 C12 1.334(7) . ? N2 Pb1 2.560(4) 3_666 ? O1 C6 1.265(8) . ? O2 C6 1.212(9) . ? O3 C15 1.257(7) . ? O3 Pb1 2.451(4) 3_666 ? O4 C15 1.240(7) . ? O4 Pb1 2.575(4) 2_655 ? C1 C2 1.369(10) . ? C1 C6 1.519(10) . ? C2 C3 1.367(13) . ? C2 H2 0.9300 . ? C3 C4 1.379(12) . ? C3 C7 1.521(11) . ? C4 C5 1.397(10) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.494(11) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.553(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.516(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C14 1.361(8) . ? C10 C11 1.381(8) . ? C11 C12 1.368(8) . ? C11 H11 0.9300 . ? C12 C15 1.525(7) . ? C13 C14 1.389(8) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O3 140.09(15) . 3_666 ? O1 Pb1 N1 66.01(17) . . ? O3 Pb1 N1 83.91(16) 3_666 . ? O1 Pb1 N2 80.88(15) . 3_666 ? O3 Pb1 N2 65.72(14) 3_666 3_666 ? N1 Pb1 N2 74.75(16) . 3_666 ? O1 Pb1 O4 111.59(15) . 2_645 ? O3 Pb1 O4 78.96(14) 3_666 2_645 ? N1 Pb1 O4 69.69(17) . 2_645 ? N2 Pb1 O4 131.81(15) 3_666 2_645 ? C5 N1 C1 119.2(6) . . ? C5 N1 Pb1 122.0(5) . . ? C1 N1 Pb1 118.5(5) . . ? C13 N2 C12 117.1(5) . . ? C13 N2 Pb1 126.0(3) . 3_666 ? C12 N2 Pb1 116.6(3) . 3_666 ? C6 O1 Pb1 122.9(4) . . ? C15 O3 Pb1 122.5(4) . 3_666 ? C15 O4 Pb1 114.0(4) . 2_655 ? N1 C1 C2 121.0(8) . . ? N1 C1 C6 116.4(6) . . ? C2 C1 C6 122.5(7) . . ? C1 C2 C3 121.2(8) . . ? C1 C2 H2 119.4 . . ? C3 C2 H2 119.4 . . ? C2 C3 C4 117.8(8) . . ? C2 C3 C7 124.1(9) . . ? C4 C3 C7 117.9(9) . . ? C3 C4 C5 119.1(8) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.6(7) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? O2 C6 O1 125.6(8) . . ? O2 C6 C1 118.9(8) . . ? O1 C6 C1 115.5(7) . . ? C8 C7 C3 112.2(8) . . ? C8 C7 H7A 109.2 . . ? C3 C7 H7A 109.2 . . ? C8 C7 H7B 109.2 . . ? C3 C7 H7B 109.2 . . ? H7A C7 H7B 107.9 . . ? C7 C8 C9 112.5(6) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 110.2(5) . . ? C10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? C10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? C14 C10 C11 117.9(5) . . ? C14 C10 C9 121.2(5) . . ? C11 C10 C9 121.0(5) . . ? C12 C11 C10 119.6(5) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? N2 C12 C11 123.0(5) . . ? N2 C12 C15 116.6(5) . . ? C11 C12 C15 120.3(5) . . ? N2 C13 C14 123.0(5) . . ? N2 C13 H13 118.5 . . ? C14 C13 H13 118.5 . . ? C10 C14 C13 119.3(5) . . ? C10 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? O4 C15 O3 126.2(6) . . ? O4 C15 C12 115.7(6) . . ? O3 C15 C12 118.1(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pb1 N1 C5 -175.2(6) . . . . ? O3 Pb1 N1 C5 31.7(5) 3_666 . . . ? N2 Pb1 N1 C5 98.1(5) 3_666 . . . ? O4 Pb1 N1 C5 -48.8(5) 2_645 . . . ? O1 Pb1 N1 C1 -0.6(5) . . . . ? O3 Pb1 N1 C1 -153.7(5) 3_666 . . . ? N2 Pb1 N1 C1 -87.3(5) 3_666 . . . ? O4 Pb1 N1 C1 125.8(5) 2_645 . . . ? O3 Pb1 O1 C6 40.0(6) 3_666 . . . ? N1 Pb1 O1 C6 -4.6(5) . . . . ? N2 Pb1 O1 C6 72.7(6) 3_666 . . . ? O4 Pb1 O1 C6 -58.8(6) 2_645 . . . ? C5 N1 C1 C2 1.9(11) . . . . ? Pb1 N1 C1 C2 -172.9(6) . . . . ? C5 N1 C1 C6 179.4(7) . . . . ? Pb1 N1 C1 C6 4.7(9) . . . . ? N1 C1 C2 C3 -0.1(14) . . . . ? C6 C1 C2 C3 -177.5(9) . . . . ? C1 C2 C3 C4 -2.2(16) . . . . ? C1 C2 C3 C7 -176.8(8) . . . . ? C2 C3 C4 C5 2.7(15) . . . . ? C7 C3 C4 C5 177.7(8) . . . . ? C1 N1 C5 C4 -1.3(12) . . . . ? Pb1 N1 C5 C4 173.3(6) . . . . ? C3 C4 C5 N1 -1.1(14) . . . . ? Pb1 O1 C6 O2 -170.9(7) . . . . ? Pb1 O1 C6 C1 8.4(9) . . . . ? N1 C1 C6 O2 170.9(8) . . . . ? C2 C1 C6 O2 -11.6(13) . . . . ? N1 C1 C6 O1 -8.5(10) . . . . ? C2 C1 C6 O1 169.0(8) . . . . ? C2 C3 C7 C8 90.8(11) . . . . ? C4 C3 C7 C8 -83.8(13) . . . . ? C3 C7 C8 C9 177.6(8) . . . . ? C7 C8 C9 C10 176.7(7) . . . . ? C8 C9 C10 C14 91.0(7) . . . . ? C8 C9 C10 C11 -88.7(7) . . . . ? C14 C10 C11 C12 -0.9(8) . . . . ? C9 C10 C11 C12 178.9(5) . . . . ? C13 N2 C12 C11 2.4(8) . . . . ? Pb1 N2 C12 C11 -171.5(4) 3_666 . . . ? C13 N2 C12 C15 -179.2(5) . . . . ? Pb1 N2 C12 C15 6.9(6) 3_666 . . . ? C10 C11 C12 N2 -0.5(8) . . . . ? C10 C11 C12 C15 -178.9(5) . . . . ? C12 N2 C13 C14 -2.9(9) . . . . ? Pb1 N2 C13 C14 170.4(4) 3_666 . . . ? C11 C10 C14 C13 0.4(9) . . . . ? C9 C10 C14 C13 -179.3(5) . . . . ? N2 C13 C14 C10 1.5(10) . . . . ? Pb1 O4 C15 O3 -6.7(8) 2_655 . . . ? Pb1 O4 C15 C12 175.7(3) 2_655 . . . ? Pb1 O3 C15 O4 -172.1(5) 3_666 . . . ? Pb1 O3 C15 C12 5.4(7) 3_666 . . . ? N2 C12 C15 O4 169.5(5) . . . . ? C11 C12 C15 O4 -12.1(8) . . . . ? N2 C12 C15 O3 -8.2(8) . . . . ? C11 C12 C15 O3 170.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.925 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.099 #===END #============================================================================== data_3 #============================================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 N2 O4 Pb' _chemical_formula_sum 'C15 H12 N2 O4 Pb' _chemical_formula_weight 491.46 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 orthorhombic _symmetry_space_group_name_H-M 'F d d 2' _symmetry_space_group_name_HALL 'F 2 -2d' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x+1/4, y+1/4, z+1/4' 'x+3/4, -y+3/4, z+1/4' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' '-x+1/4, y+3/4, z+3/4' 'x+3/4, -y+5/4, z+3/4' 'x+1/2, y, z+1/2' '-x+1/2, -y, z+1/2' '-x+3/4, y+1/4, z+3/4' 'x+5/4, -y+3/4, z+3/4' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' '-x+3/4, y+3/4, z+1/4' 'x+5/4, -y+5/4, z+1/4' _cell_length_a 14.2347(12) _cell_length_b 19.772(2) _cell_length_c 10.8817(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3062.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 2986 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 24.27 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.132 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1840 _exptl_absorpt_coefficient_mu 11.036 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1056 _exptl_absorpt_correction_T_max 0.3280 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6854 _diffrn_reflns_av_R_equivalents 0.0337 _diffrn_reflns_av_sigmaI/netI 0.0399 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 28.31 _reflns_number_total 1875 _reflns_number_gt 1648 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SMART' _computing_publication_material 'Bruker SMART' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+9.8675P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.021(14) _refine_ls_number_reflns 1875 _refine_ls_number_parameters 101 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0254 _refine_ls_wR_factor_ref 0.0532 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.0000 -0.5000 -1.12408(9) 0.04547(9) Uani 1 2 d S . . O1 O 0.0941(3) -0.4045(2) -1.0553(5) 0.0680(13) Uani 1 1 d . . . O2 O 0.0881(3) -0.3025(2) -0.9692(5) 0.0669(13) Uani 1 1 d . . . N1 N -0.0708(3) -0.4401(2) -0.9464(4) 0.0437(11) Uani 1 1 d . . . C1 C -0.2500 -0.2500 -0.7698(10) 0.077(3) Uani 1 2 d S . . H1A H -0.2027 -0.2297 -0.8224 0.092 Uiso 0.50 1 calc PR . . H1B H -0.2973 -0.2703 -0.8224 0.092 Uiso 0.50 1 calc PR . . C2 C -0.2036(5) -0.3061(3) -0.6921(6) 0.0560(16) Uani 1 1 d . . . H2A H -0.1578 -0.2865 -0.6365 0.067 Uiso 1 1 calc R . . H2B H -0.2508 -0.3294 -0.6437 0.067 Uiso 1 1 calc R . . C3 C -0.1562(4) -0.3551(3) -0.7776(6) 0.0451(13) Uani 1 1 d . . . C4 C -0.1897(4) -0.4192(3) -0.7986(6) 0.0493(14) Uani 1 1 d . . . H4 H -0.2412 -0.4353 -0.7548 0.059 Uiso 1 1 calc R . . C5 C -0.1463(4) -0.4598(3) -0.8854(6) 0.0494(14) Uani 1 1 d . . . H5 H -0.1713 -0.5024 -0.9015 0.059 Uiso 1 1 calc R . . C6 C -0.0342(4) -0.3790(3) -0.9215(5) 0.0411(12) Uani 1 1 d . . . C7 C -0.0742(5) -0.3359(3) -0.8396(5) 0.0490(15) Uani 1 1 d . . . H7 H -0.0472 -0.2938 -0.8247 0.059 Uiso 1 1 calc R . . C8 C 0.0580(4) -0.3598(3) -0.9877(6) 0.0526(16) 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 0.04442(14) 0.05050(15) 0.04149(13) 0.000 0.000 0.01176(19) O1 0.058(3) 0.056(3) 0.090(4) 0.006(3) 0.028(3) 0.001(2) O2 0.055(3) 0.055(3) 0.090(4) 0.013(3) 0.007(2) -0.020(2) N1 0.047(3) 0.039(3) 0.045(3) 0.001(2) 0.006(2) -0.002(2) C1 0.070(7) 0.101(9) 0.059(6) 0.000 0.000 0.043(6) C2 0.052(4) 0.061(4) 0.055(4) -0.007(3) 0.001(3) 0.012(3) C3 0.049(3) 0.047(3) 0.039(3) -0.005(2) 0.000(2) 0.001(3) C4 0.044(3) 0.053(4) 0.051(4) -0.001(3) 0.010(3) -0.009(3) C5 0.047(3) 0.042(3) 0.060(4) 0.002(3) 0.000(3) -0.010(2) C6 0.039(3) 0.038(3) 0.046(3) 0.005(2) 0.001(2) -0.005(2) C7 0.054(4) 0.039(3) 0.054(4) -0.007(2) -0.003(3) -0.005(3) C8 0.045(4) 0.054(4) 0.059(4) 0.019(3) 0.006(3) -0.004(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 O1 2.434(5) 2_545 ? Pb1 O1 2.434(5) . ? Pb1 N1 2.481(5) 2_545 ? Pb1 N1 2.481(5) . ? Pb1 O2 2.731(5) 7_544 ? Pb1 O2 2.731(5) 8_434 ? O1 C8 1.259(8) . ? O2 C8 1.229(8) . ? O2 Pb1 2.731(5) 3 ? N1 C5 1.322(7) . ? N1 C6 1.343(7) . ? C1 C2 1.544(9) 14_445 ? C1 C2 1.544(9) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.502(8) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.373(8) . ? C3 C7 1.401(8) . ? C4 C5 1.385(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.359(8) . ? C6 C8 1.544(8) . ? C7 H7 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O1 144.2(3) 2_545 . ? O1 Pb1 N1 67.25(16) 2_545 2_545 ? O1 Pb1 N1 84.66(17) . 2_545 ? O1 Pb1 N1 84.66(17) 2_545 . ? O1 Pb1 N1 67.25(16) . . ? N1 Pb1 N1 77.6(2) 2_545 . ? O1 Pb1 O2 106.64(16) 2_545 7_544 ? O1 Pb1 O2 86.96(16) . 7_544 ? N1 Pb1 O2 76.79(15) 2_545 7_544 ? N1 Pb1 O2 145.02(17) . 7_544 ? O1 Pb1 O2 86.96(16) 2_545 8_434 ? O1 Pb1 O2 106.64(16) . 8_434 ? N1 Pb1 O2 145.02(17) 2_545 8_434 ? N1 Pb1 O2 76.79(15) . 8_434 ? O2 Pb1 O2 135.5(2) 7_544 8_434 ? C8 O1 Pb1 119.9(4) . . ? C8 O2 Pb1 135.0(4) . 3 ? C5 N1 C6 118.7(5) . . ? C5 N1 Pb1 125.5(4) . . ? C6 N1 Pb1 115.4(4) . . ? C2 C1 C2 113.6(8) 14_445 . ? C2 C1 H1A 108.8 14_445 . ? C2 C1 H1A 108.8 . . ? C2 C1 H1B 108.8 14_445 . ? C2 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? C3 C2 C1 108.5(6) . . ? C3 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? C3 C2 H2B 110.0 . . ? C1 C2 H2B 110.0 . . ? H2A C2 H2B 108.4 . . ? C4 C3 C7 117.4(5) . . ? C4 C3 C2 122.8(6) . . ? C7 C3 C2 119.8(6) . . ? C3 C4 C5 119.6(5) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? N1 C5 C4 122.3(5) . . ? N1 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? N1 C6 C7 122.3(5) . . ? N1 C6 C8 117.2(5) . . ? C7 C6 C8 120.5(5) . . ? C6 C7 C3 119.6(6) . . ? C6 C7 H7 120.2 . . ? C3 C7 H7 120.2 . . ? O2 C8 O1 126.9(6) . . ? O2 C8 C6 116.6(6) . . ? O1 C8 C6 116.6(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pb1 O1 C8 -58.5(5) 2_545 . . . ? N1 Pb1 O1 C8 -96.1(5) 2_545 . . . ? N1 Pb1 O1 C8 -17.3(5) . . . . ? O2 Pb1 O1 C8 -173.1(5) 7_544 . . . ? O2 Pb1 O1 C8 50.1(5) 8_434 . . . ? O1 Pb1 N1 C5 -16.6(5) 2_545 . . . ? O1 Pb1 N1 C5 -173.9(5) . . . . ? N1 Pb1 N1 C5 -84.5(5) 2_545 . . . ? O2 Pb1 N1 C5 -128.2(5) 7_544 . . . ? O2 Pb1 N1 C5 71.5(5) 8_434 . . . ? O1 Pb1 N1 C6 171.4(4) 2_545 . . . ? O1 Pb1 N1 C6 14.2(4) . . . . ? N1 Pb1 N1 C6 103.6(5) 2_545 . . . ? O2 Pb1 N1 C6 59.8(5) 7_544 . . . ? O2 Pb1 N1 C6 -100.5(4) 8_434 . . . ? C2 C1 C2 C3 -176.6(6) 14_445 . . . ? C1 C2 C3 C4 -108.4(7) . . . . ? C1 C2 C3 C7 71.6(7) . . . . ? C7 C3 C4 C5 -4.8(9) . . . . ? C2 C3 C4 C5 175.2(6) . . . . ? C6 N1 C5 C4 1.0(9) . . . . ? Pb1 N1 C5 C4 -170.7(5) . . . . ? C3 C4 C5 N1 2.7(10) . . . . ? C5 N1 C6 C7 -2.6(9) . . . . ? Pb1 N1 C6 C7 170.0(5) . . . . ? C5 N1 C6 C8 175.7(5) . . . . ? Pb1 N1 C6 C8 -11.7(7) . . . . ? N1 C6 C7 C3 0.3(9) . . . . ? C8 C6 C7 C3 -178.0(6) . . . . ? C4 C3 C7 C6 3.4(9) . . . . ? C2 C3 C7 C6 -176.7(6) . . . . ? Pb1 O2 C8 O1 -60.2(10) 3 . . . ? Pb1 O2 C8 C6 120.2(6) 3 . . . ? Pb1 O1 C8 O2 -161.9(6) . . . . ? Pb1 O1 C8 C6 17.7(7) . . . . ? N1 C6 C8 O2 176.3(6) . . . . ? C7 C6 C8 O2 -5.4(9) . . . . ? N1 C6 C8 O1 -3.4(8) . . . . ? C7 C6 C8 O1 174.9(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 28.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.955 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.091 #===END #============================================================================== data_4 #============================================================================== data_c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C45 H36 N6 O12 Pb3' _chemical_formula_weight 1474.37 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 'C 2/m' _symmetry_space_group_name_HALL '-C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z' _cell_length_a 22.976(13) _cell_length_b 19.587(11) _cell_length_c 10.776(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.912(7) _cell_angle_gamma 90.00 _cell_volume 4745(5) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 4558 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 22.22 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.064 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 10.685 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1364 _exptl_absorpt_correction_T_max 0.4819 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18162 _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.36 _diffrn_reflns_theta_max 25.50 _reflns_number_total 4544 _reflns_number_gt 3405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0729P)^2^+3.9854P] 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 4544 _refine_ls_number_parameters 333 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0482 _refine_ls_wR_factor_ref 0.1327 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.080 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.59103(2) 0.0000 0.55861(4) 0.05035(18) Uani 1 2 d S . . Pb2 Pb 1.01515(2) 0.0000 -0.31262(5) 0.05652(19) Uani 1 2 d S . . Pb3 Pb 1.5000 0.24821(3) 0.5000 0.0763(2) Uani 1 2 d S . . O1 O 0.5145(3) 0.0000 0.3749(8) 0.054(2) Uani 1 2 d S . . O2 O 0.4816(4) 0.0000 0.1697(8) 0.058(2) Uani 1 2 d S . . O3 O 0.9297(5) 0.0000 -0.4809(8) 0.070(3) Uani 1 2 d S . . O4 O 0.8311(5) 0.0000 -0.5510(9) 0.072(3) Uani 1 2 d S . . O5 O 1.0338(5) 0.0959(5) -0.1558(9) 0.117(3) Uani 1 1 d . . . O6 O 1.0051(4) 0.1433(4) -0.3431(10) 0.096(3) Uani 1 1 d . . . O7 O 1.4242(4) 0.1397(3) 0.4795(7) 0.081(2) Uani 1 1 d . . . O8 O 1.3324(4) 0.0976(4) 0.4096(9) 0.096(3) Uani 1 1 d . . . N1 N 0.6279(5) 0.0000 0.3547(9) 0.049(2) Uani 1 2 d S . . N2 N 0.9179(6) 0.0000 -0.2446(12) 0.081(3) Uani 1 2 d SU . . N3 N 1.0295(5) 0.2699(5) -0.2494(13) 0.112(4) Uani 1 1 d . . . N4 N 1.3836(5) 0.2701(4) 0.4375(10) 0.083(3) Uani 1 1 d . . . C1 C 0.5852(5) 0.0000 0.2457(11) 0.040(3) Uani 1 2 d S . . C2 C 0.5996(5) 0.0000 0.1289(12) 0.041(3) Uani 1 2 d S . . H2 H 0.5696 0.0000 0.0563 0.050 Uiso 1 2 calc SR . . C3 C 0.6584(5) 0.0000 0.1176(11) 0.050(3) Uani 1 2 d S . . C4 C 0.7013(6) 0.0000 0.2297(13) 0.054(3) Uani 1 2 d S . . H4 H 0.7414 0.0000 0.2262 0.064 Uiso 1 2 calc SR . . C5 C 0.6855(5) 0.0000 0.3415(12) 0.050(3) Uani 1 2 d S . . H5 H 0.7154 0.0000 0.4144 0.060 Uiso 1 2 calc SR . . C6 C 0.5231(5) 0.0000 0.2618(12) 0.042(3) Uani 1 2 d S . . C7 C 0.6727(6) 0.0000 -0.0148(13) 0.071(4) Uani 1 2 d S . . H7A H 0.6542 -0.0399 -0.0598 0.085 Uiso 0.50 1 calc PR . . H7B H 0.6542 0.0399 -0.0598 0.085 Uiso 0.50 1 calc PR . . C8 C 0.7365(6) 0.0000 -0.0219(13) 0.077(5) Uani 1 2 d S . . H8A H 0.7557 -0.0401 0.0212 0.092 Uiso 0.50 1 calc PR . . H8B H 0.7557 0.0401 0.0212 0.092 Uiso 0.50 1 calc PR . . C9 C 0.7439(7) 0.0000 -0.1556(14) 0.104(7) Uani 1 2 d S . . H9A H 0.7236 0.0399 -0.1971 0.125 Uiso 0.50 1 calc PR . . H9B H 0.7236 -0.0399 -0.1971 0.125 Uiso 0.50 1 calc PR . . C10 C 0.8692(6) 0.0000 -0.3314(13) 0.063(3) Uani 1 2 d SU . . C11 C 0.8152(7) 0.0000 -0.3011(15) 0.074(3) Uani 1 2 d SU . . H11 H 0.7819 0.0000 -0.3669 0.089 Uiso 1 2 calc SR . . C12 C 0.8063(7) 0.0000 -0.1791(16) 0.085(4) Uani 1 2 d SU . . C13 C 0.8587(9) 0.0000 -0.0873(19) 0.103(4) Uani 1 2 d SU . . H13 H 0.8567 0.0000 -0.0020 0.123 Uiso 1 2 calc SR . . C14 C 0.9148(8) 0.0000 -0.1209(17) 0.096(4) Uani 1 2 d SU . . H14 H 0.9494 0.0000 -0.0583 0.115 Uiso 1 2 calc SR . . C15 C 0.8759(7) 0.0000 -0.4669(12) 0.056(3) Uani 1 2 d S . . C16 C 1.0422(6) 0.2143(6) -0.1685(17) 0.097(5) Uani 1 1 d . . . C17 C 1.0648(6) 0.2231(7) -0.0449(16) 0.098(4) Uani 1 1 d . . . H17 H 1.0718 0.1850 0.0076 0.118 Uiso 1 1 calc R . . C18 C 1.0783(6) 0.2889(10) 0.0083(18) 0.115(6) Uani 1 1 d . . . C19 C 1.0624(7) 0.3421(7) -0.082(2) 0.115(6) Uani 1 1 d . . . H19 H 1.0678 0.3870 -0.0543 0.138 Uiso 1 1 calc R . . C20 C 1.0407(7) 0.3318(7) -0.2017(19) 0.115(5) Uani 1 1 d . . . H20 H 1.0326 0.3692 -0.2557 0.138 Uiso 1 1 calc R . . C21 C 1.0262(6) 0.1460(7) -0.2272(16) 0.090(4) Uani 1 1 d . . . C22 C 1.1026(6) 0.2974(9) 0.1443(19) 0.136(6) Uani 1 1 d . . . H22A H 1.0867 0.2623 0.1914 0.164 Uiso 1 1 calc R . . H22B H 1.0910 0.3415 0.1721 0.164 Uiso 1 1 calc R . . C23 C 1.1710(7) 0.2923(10) 0.1713(19) 0.137(6) Uani 1 1 d . . . H23A H 1.1829 0.2475 0.1470 0.164 Uiso 1 1 calc R . . H23B H 1.1870 0.3262 0.1220 0.164 Uiso 1 1 calc R . . C24 C 1.1934(8) 0.3030(8) 0.301(2) 0.135(6) Uani 1 1 d . . . H24A H 1.1722 0.2733 0.3479 0.162 Uiso 1 1 calc R . . H24B H 1.1846 0.3497 0.3206 0.162 Uiso 1 1 calc R . . C25 C 1.3446(6) 0.2167(5) 0.4072(12) 0.086(4) Uani 1 1 d . . . C26 C 1.2835(6) 0.2238(6) 0.3622(16) 0.117(6) Uani 1 1 d . . . H26 H 1.2592 0.1857 0.3428 0.141 Uiso 1 1 calc R . . C27 C 1.2591(8) 0.2911(8) 0.3465(18) 0.133(6) Uani 1 1 d . . . C28 C 1.3013(7) 0.3445(6) 0.3739(17) 0.122(5) Uani 1 1 d . . . H28 H 1.2883 0.3894 0.3614 0.147 Uiso 1 1 calc R . . C29 C 1.3601(6) 0.3323(6) 0.4181(14) 0.099(4) Uani 1 1 d . . . H29 H 1.3855 0.3696 0.4358 0.119 Uiso 1 1 calc R . . C30 C 1.3686(6) 0.1464(6) 0.4327(11) 0.078(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0480(3) 0.0489(3) 0.0507(3) 0.000 0.0021(2) 0.000 Pb2 0.0577(3) 0.0604(3) 0.0538(3) 0.000 0.0168(2) 0.000 Pb3 0.0631(4) 0.0437(3) 0.1093(5) 0.000 -0.0120(3) 0.000 O1 0.036(5) 0.074(6) 0.053(5) 0.000 0.009(4) 0.000 O2 0.042(5) 0.082(6) 0.047(5) 0.000 0.004(4) 0.000 O3 0.083(8) 0.081(7) 0.048(5) 0.000 0.014(5) 0.000 O4 0.070(7) 0.084(7) 0.058(6) 0.000 0.002(5) 0.000 O5 0.182(11) 0.059(5) 0.117(7) -0.015(5) 0.049(7) -0.026(6) O6 0.087(6) 0.052(5) 0.144(8) -0.015(5) 0.012(6) -0.012(4) O7 0.103(6) 0.045(4) 0.088(5) 0.006(3) 0.005(4) 0.010(4) O8 0.097(6) 0.048(4) 0.140(8) 0.008(4) 0.017(5) 0.004(4) N1 0.054(7) 0.041(5) 0.052(6) 0.000 0.011(5) 0.000 N2 0.071(5) 0.112(6) 0.063(5) 0.000 0.021(4) 0.000 N3 0.114(9) 0.059(6) 0.177(12) -0.039(7) 0.066(9) -0.020(6) N4 0.085(7) 0.048(5) 0.113(8) -0.005(5) 0.012(6) 0.000(5) C1 0.039(6) 0.029(5) 0.050(7) 0.000 0.007(5) 0.000 C2 0.024(6) 0.043(6) 0.062(7) 0.000 0.020(5) 0.000 C3 0.048(8) 0.048(7) 0.051(7) 0.000 0.004(6) 0.000 C4 0.038(7) 0.054(8) 0.066(8) 0.000 0.007(6) 0.000 C5 0.040(7) 0.057(8) 0.051(7) 0.000 0.005(5) 0.000 C6 0.026(6) 0.039(6) 0.060(8) 0.000 0.009(5) 0.000 C7 0.042(8) 0.111(13) 0.067(9) 0.000 0.028(7) 0.000 C8 0.051(9) 0.118(14) 0.062(9) 0.000 0.015(7) 0.000 C9 0.067(11) 0.20(2) 0.056(9) 0.000 0.032(8) 0.000 C10 0.056(5) 0.080(6) 0.052(5) 0.000 0.008(4) 0.000 C11 0.062(6) 0.096(6) 0.065(5) 0.000 0.016(5) 0.000 C12 0.067(6) 0.115(6) 0.074(6) 0.000 0.019(5) 0.000 C13 0.084(6) 0.139(7) 0.086(6) 0.000 0.021(5) 0.000 C14 0.081(6) 0.135(7) 0.075(6) 0.000 0.025(5) 0.000 C15 0.080(11) 0.038(7) 0.048(7) 0.000 0.012(7) 0.000 C16 0.078(8) 0.046(7) 0.181(15) -0.024(8) 0.056(10) -0.018(6) C17 0.101(10) 0.066(8) 0.134(12) -0.036(8) 0.037(9) -0.015(7) C18 0.055(7) 0.138(14) 0.160(15) -0.079(13) 0.045(9) -0.022(9) C19 0.094(11) 0.057(8) 0.202(19) -0.019(11) 0.051(12) -0.006(7) C20 0.128(13) 0.064(9) 0.168(16) -0.041(9) 0.067(12) -0.020(8) C21 0.077(8) 0.069(8) 0.127(12) -0.038(8) 0.030(8) -0.020(7) C22 0.079(10) 0.127(14) 0.206(19) -0.065(13) 0.038(11) -0.010(9) C23 0.098(12) 0.141(16) 0.162(17) -0.034(13) 0.004(11) -0.006(11) C24 0.109(13) 0.098(11) 0.181(17) -0.018(12) -0.009(11) -0.003(10) C25 0.094(9) 0.035(5) 0.123(10) -0.003(6) 0.007(7) 0.012(6) C26 0.096(10) 0.047(6) 0.181(15) -0.018(8) -0.039(9) 0.011(7) C27 0.115(12) 0.090(11) 0.172(16) -0.013(10) -0.024(11) 0.021(10) C28 0.096(10) 0.047(7) 0.204(16) 0.001(8) -0.013(10) 0.008(7) C29 0.092(9) 0.044(6) 0.157(12) -0.002(7) 0.015(8) 0.016(6) C30 0.099(9) 0.054(7) 0.075(7) -0.005(5) 0.003(6) 0.009(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.361(8) . ? Pb1 N1 2.514(10) . ? Pb1 O8 2.573(8) 2_756 ? Pb1 O8 2.573(8) 5_756 ? Pb1 O1 2.667(8) 5_656 ? Pb1 O7 2.778(7) 5_756 ? Pb1 O7 2.778(7) 2_756 ? Pb2 O3 2.381(10) . ? Pb2 N2 2.491(13) . ? Pb2 O5 2.503(8) . ? Pb2 O5 2.503(8) 6 ? Pb2 O3 2.778(10) 5_754 ? Pb2 O6 2.829(8) 6 ? Pb2 O6 2.829(8) . ? Pb3 N4 2.655(10) . ? Pb3 N4 2.655(10) 2_856 ? Pb3 N3 2.669(14) 8_556 ? Pb3 N3 2.669(14) 7_755 ? Pb3 O6 2.703(9) 8_556 ? Pb3 O6 2.703(9) 7_755 ? Pb3 O7 2.728(8) . ? Pb3 O7 2.728(8) 2_856 ? O1 C6 1.274(14) . ? O1 Pb1 2.667(8) 5_656 ? O2 C6 1.226(13) . ? O3 C15 1.277(17) . ? O3 Pb2 2.778(10) 5_754 ? O4 C15 1.222(16) . ? O5 C21 1.238(16) . ? O6 C21 1.244(15) . ? O6 Pb3 2.703(9) 7_755 ? O7 C30 1.280(14) . ? O7 Pb1 2.778(7) 5_756 ? O8 C30 1.258(13) . ? O8 Pb1 2.573(8) 5_756 ? N1 C5 1.360(16) . ? N1 C1 1.367(14) . ? N2 C10 1.302(17) . ? N2 C14 1.35(2) . ? N3 C20 1.320(16) . ? N3 C16 1.388(19) . ? N3 Pb3 2.669(14) 7_755 ? N4 C29 1.331(13) . ? N4 C25 1.373(14) . ? C1 C2 1.366(16) . ? C1 C6 1.473(16) . ? C2 C3 1.381(16) . ? C2 H2 0.9300 . ? C3 C4 1.392(16) . ? C3 C7 1.529(18) . ? C4 C5 1.328(18) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.483(19) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.49(2) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C12 1.51(2) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.35(2) . ? C10 C15 1.499(19) . ? C11 C12 1.37(2) . ? C11 H11 0.9300 . ? C12 C13 1.39(2) . ? C13 C14 1.41(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C16 C17 1.337(19) . ? C16 C21 1.494(16) . ? C17 C18 1.420(19) . ? C17 H17 0.9300 . ? C18 C19 1.42(2) . ? C18 C22 1.47(2) . ? C19 C20 1.30(2) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.54(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.40(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C27 1.51(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.393(18) . ? C25 C30 1.488(14) . ? C26 C27 1.429(19) . ? C26 H26 0.9300 . ? C27 C28 1.41(2) . ? C28 C29 1.358(18) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 N1 66.1(3) . . ? O1 Pb1 O8 118.8(2) . 2_756 ? N1 Pb1 O8 76.8(3) . 2_756 ? O1 Pb1 O8 118.8(2) . 5_756 ? N1 Pb1 O8 76.8(3) . 5_756 ? O8 Pb1 O8 96.0(4) 2_756 5_756 ? O1 Pb1 O1 70.4(3) . 5_656 ? N1 Pb1 O1 136.4(3) . 5_656 ? O8 Pb1 O1 126.8(2) 2_756 5_656 ? O8 Pb1 O1 126.8(2) 5_756 5_656 ? O1 Pb1 O7 80.02(16) . 5_756 ? N1 Pb1 O7 85.76(17) . 5_756 ? O8 Pb1 O7 144.4(3) 2_756 5_756 ? O8 Pb1 O7 49.4(2) 5_756 5_756 ? O1 Pb1 O7 86.88(19) 5_656 5_756 ? O1 Pb1 O7 80.02(16) . 2_756 ? N1 Pb1 O7 85.76(17) . 2_756 ? O8 Pb1 O7 49.4(2) 2_756 2_756 ? O8 Pb1 O7 144.4(3) 5_756 2_756 ? O1 Pb1 O7 86.88(19) 5_656 2_756 ? O7 Pb1 O7 160.0(3) 5_756 2_756 ? O3 Pb2 N2 64.9(4) . . ? O3 Pb2 O5 120.9(3) . . ? N2 Pb2 O5 80.8(3) . . ? O3 Pb2 O5 120.9(3) . 6 ? N2 Pb2 O5 80.8(3) . 6 ? O5 Pb2 O5 97.2(5) . 6 ? O3 Pb2 O3 80.2(4) . 5_754 ? N2 Pb2 O3 145.1(4) . 5_754 ? O5 Pb2 O3 119.9(3) . 5_754 ? O5 Pb2 O3 119.9(3) 6 5_754 ? O3 Pb2 O6 82.94(19) . 6 ? N2 Pb2 O6 88.74(18) . 6 ? O5 Pb2 O6 145.2(4) . 6 ? O5 Pb2 O6 48.2(3) 6 6 ? O3 Pb2 O6 86.9(2) 5_754 6 ? O3 Pb2 O6 82.94(19) . . ? N2 Pb2 O6 88.74(18) . . ? O5 Pb2 O6 48.2(3) . . ? O5 Pb2 O6 145.2(4) 6 . ? O3 Pb2 O6 86.9(2) 5_754 . ? O6 Pb2 O6 165.4(4) 6 . ? N4 Pb3 N4 161.4(4) . 2_856 ? N4 Pb3 N3 108.1(3) . 8_556 ? N4 Pb3 N3 74.5(3) 2_856 8_556 ? N4 Pb3 N3 74.5(3) . 7_755 ? N4 Pb3 N3 108.1(3) 2_856 7_755 ? N3 Pb3 N3 164.7(5) 8_556 7_755 ? N4 Pb3 O6 86.8(3) . 8_556 ? N4 Pb3 O6 78.6(3) 2_856 8_556 ? N3 Pb3 O6 60.2(3) 8_556 8_556 ? N3 Pb3 O6 135.0(3) 7_755 8_556 ? N4 Pb3 O6 78.6(3) . 7_755 ? N4 Pb3 O6 86.8(3) 2_856 7_755 ? N3 Pb3 O6 135.0(3) 8_556 7_755 ? N3 Pb3 O6 60.2(3) 7_755 7_755 ? O6 Pb3 O6 76.3(4) 8_556 7_755 ? N4 Pb3 O7 60.8(3) . . ? N4 Pb3 O7 137.7(3) 2_856 . ? N3 Pb3 O7 90.2(3) 8_556 . ? N3 Pb3 O7 77.8(3) 7_755 . ? O6 Pb3 O7 127.5(3) 8_556 . ? O6 Pb3 O7 128.1(3) 7_755 . ? N4 Pb3 O7 137.7(3) . 2_856 ? N4 Pb3 O7 60.8(3) 2_856 2_856 ? N3 Pb3 O7 77.8(3) 8_556 2_856 ? N3 Pb3 O7 90.2(3) 7_755 2_856 ? O6 Pb3 O7 128.1(3) 8_556 2_856 ? O6 Pb3 O7 127.5(3) 7_755 2_856 ? O7 Pb3 O7 77.6(3) . 2_856 ? C6 O1 Pb1 124.5(7) . . ? C6 O1 Pb1 125.9(7) . 5_656 ? Pb1 O1 Pb1 109.6(3) . 5_656 ? C15 O3 Pb2 125.2(8) . . ? C15 O3 Pb2 135.0(8) . 5_754 ? Pb2 O3 Pb2 99.8(4) . 5_754 ? C21 O5 Pb2 101.1(8) . . ? C21 O6 Pb3 123.5(8) . 7_755 ? C21 O6 Pb2 85.4(8) . . ? Pb3 O6 Pb2 147.6(4) 7_755 . ? C30 O7 Pb3 121.4(7) . . ? C30 O7 Pb1 87.5(6) . 5_756 ? Pb3 O7 Pb1 147.0(3) . 5_756 ? C30 O8 Pb1 97.5(7) . 5_756 ? C5 N1 C1 116.9(10) . . ? C5 N1 Pb1 127.1(8) . . ? C1 N1 Pb1 116.1(8) . . ? C10 N2 C14 119.8(14) . . ? C10 N2 Pb2 118.5(10) . . ? C14 N2 Pb2 121.7(11) . . ? C20 N3 C16 118.5(15) . . ? C20 N3 Pb3 120.3(12) . 7_755 ? C16 N3 Pb3 120.5(9) . 7_755 ? C29 N4 C25 115.9(11) . . ? C29 N4 Pb3 122.8(8) . . ? C25 N4 Pb3 120.8(7) . . ? C2 C1 N1 121.6(10) . . ? C2 C1 C6 122.3(10) . . ? N1 C1 C6 116.1(10) . . ? C1 C2 C3 120.6(11) . . ? C1 C2 H2 119.7 . . ? C3 C2 H2 119.7 . . ? C2 C3 C4 117.0(12) . . ? C2 C3 C7 119.0(10) . . ? C4 C3 C7 124.0(11) . . ? C5 C4 C3 120.7(12) . . ? C5 C4 H4 119.6 . . ? C3 C4 H4 119.6 . . ? C4 C5 N1 123.2(11) . . ? C4 C5 H5 118.4 . . ? N1 C5 H5 118.4 . . ? O2 C6 O1 121.8(10) . . ? O2 C6 C1 120.9(11) . . ? O1 C6 C1 117.3(10) . . ? C8 C7 C3 117.0(12) . . ? C8 C7 H7A 108.1 . . ? C3 C7 H7A 108.1 . . ? C8 C7 H7B 108.1 . . ? C3 C7 H7B 108.1 . . ? H7A C7 H7B 107.3 . . ? C7 C8 C9 111.2(12) . . ? C7 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? C7 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? C8 C9 C12 117.8(13) . . ? C8 C9 H9A 107.9 . . ? C12 C9 H9A 107.9 . . ? C8 C9 H9B 107.9 . . ? C12 C9 H9B 107.9 . . ? H9A C9 H9B 107.2 . . ? N2 C10 C11 121.5(13) . . ? N2 C10 C15 117.1(13) . . ? C11 C10 C15 121.4(13) . . ? C10 C11 C12 124.0(15) . . ? C10 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C11 C12 C13 113.8(16) . . ? C11 C12 C9 119.7(15) . . ? C13 C12 C9 126.5(16) . . ? C12 C13 C14 121.3(18) . . ? C12 C13 H13 119.3 . . ? C14 C13 H13 119.3 . . ? N2 C14 C13 119.5(17) . . ? N2 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? O4 C15 O3 126.9(13) . . ? O4 C15 C10 118.9(14) . . ? O3 C15 C10 114.2(12) . . ? C17 C16 N3 120.9(12) . . ? C17 C16 C21 123.2(14) . . ? N3 C16 C21 115.8(15) . . ? C16 C17 C18 121.8(16) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C19 112.5(15) . . ? C17 C18 C22 120.8(19) . . ? C19 C18 C22 126.6(17) . . ? C20 C19 C18 124.0(15) . . ? C20 C19 H19 118.0 . . ? C18 C19 H19 118.0 . . ? C19 C20 N3 122.2(17) . . ? C19 C20 H20 118.9 . . ? N3 C20 H20 118.9 . . ? O5 C21 O6 124.5(11) . . ? O5 C21 C16 117.2(14) . . ? O6 C21 C16 118.3(14) . . ? C18 C22 C23 110.1(14) . . ? C18 C22 H22A 109.6 . . ? C23 C22 H22A 109.6 . . ? C18 C22 H22B 109.6 . . ? C23 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? C24 C23 C22 109.2(17) . . ? C24 C23 H23A 109.8 . . ? C22 C23 H23A 109.8 . . ? C24 C23 H23B 109.8 . . ? C22 C23 H23B 109.8 . . ? H23A C23 H23B 108.3 . . ? C23 C24 C27 116.2(17) . . ? C23 C24 H24A 108.2 . . ? C27 C24 H24A 108.2 . . ? C23 C24 H24B 108.2 . . ? C27 C24 H24B 108.2 . . ? H24A C24 H24B 107.4 . . ? N4 C25 C26 124.6(10) . . ? N4 C25 C30 117.5(11) . . ? C26 C25 C30 117.8(11) . . ? C25 C26 C27 118.4(13) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C28 C27 C26 114.9(14) . . ? C28 C27 C24 123.5(14) . . ? C26 C27 C24 121.6(15) . . ? C29 C28 C27 122.2(12) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? N4 C29 C28 123.9(12) . . ? N4 C29 H29 118.1 . . ? C28 C29 H29 118.1 . . ? O8 C30 O7 124.5(10) . . ? O8 C30 C25 117.4(11) . . ? O7 C30 C25 118.0(11) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Pb1 O1 C6 0.0 . . . . ? O8 Pb1 O1 C6 58.0(2) 2_756 . . . ? O8 Pb1 O1 C6 -58.0(2) 5_756 . . . ? O1 Pb1 O1 C6 180.0 5_656 . . . ? O7 Pb1 O1 C6 -89.77(18) 5_756 . . . ? O7 Pb1 O1 C6 89.77(18) 2_756 . . . ? N1 Pb1 O1 Pb1 180.0 . . . 5_656 ? O8 Pb1 O1 Pb1 -122.0(2) 2_756 . . 5_656 ? O8 Pb1 O1 Pb1 122.0(2) 5_756 . . 5_656 ? O1 Pb1 O1 Pb1 0.0 5_656 . . 5_656 ? O7 Pb1 O1 Pb1 90.23(18) 5_756 . . 5_656 ? O7 Pb1 O1 Pb1 -90.23(18) 2_756 . . 5_656 ? N2 Pb2 O3 C15 0.000(1) . . . . ? O5 Pb2 O3 C15 -60.9(3) . . . . ? O5 Pb2 O3 C15 60.9(3) 6 . . . ? O3 Pb2 O3 C15 180.000(2) 5_754 . . . ? O6 Pb2 O3 C15 91.9(2) 6 . . . ? O6 Pb2 O3 C15 -91.9(2) . . . . ? N2 Pb2 O3 Pb2 180.0 . . . 5_754 ? O5 Pb2 O3 Pb2 119.1(3) . . . 5_754 ? O5 Pb2 O3 Pb2 -119.1(3) 6 . . 5_754 ? O3 Pb2 O3 Pb2 0.0 5_754 . . 5_754 ? O6 Pb2 O3 Pb2 -88.1(2) 6 . . 5_754 ? O6 Pb2 O3 Pb2 88.1(2) . . . 5_754 ? O3 Pb2 O5 C21 -48.2(10) . . . . ? N2 Pb2 O5 C21 -101.5(9) . . . . ? O5 Pb2 O5 C21 179.1(7) 6 . . . ? O3 Pb2 O5 C21 48.4(10) 5_754 . . . ? O6 Pb2 O5 C21 -175.7(7) 6 . . . ? O6 Pb2 O5 C21 -4.9(8) . . . . ? O3 Pb2 O6 C21 148.5(8) . . . . ? N2 Pb2 O6 C21 83.6(8) . . . . ? O5 Pb2 O6 C21 4.8(8) . . . . ? O5 Pb2 O6 C21 11.7(11) 6 . . . ? O3 Pb2 O6 C21 -131.0(8) 5_754 . . . ? O6 Pb2 O6 C21 163.7(12) 6 . . . ? O3 Pb2 O6 Pb3 -56.2(6) . . . 7_755 ? N2 Pb2 O6 Pb3 -121.1(7) . . . 7_755 ? O5 Pb2 O6 Pb3 160.1(8) . . . 7_755 ? O5 Pb2 O6 Pb3 167.0(6) 6 . . 7_755 ? O3 Pb2 O6 Pb3 24.3(6) 5_754 . . 7_755 ? O6 Pb2 O6 Pb3 -41.0(19) 6 . . 7_755 ? N4 Pb3 O7 C30 9.9(8) . . . . ? N4 Pb3 O7 C30 -172.6(8) 2_856 . . . ? N3 Pb3 O7 C30 120.6(9) 8_556 . . . ? N3 Pb3 O7 C30 -69.0(9) 7_755 . . . ? O6 Pb3 O7 C30 69.3(9) 8_556 . . . ? O6 Pb3 O7 C30 -33.6(10) 7_755 . . . ? O7 Pb3 O7 C30 -161.9(10) 2_856 . . . ? N4 Pb3 O7 Pb1 157.8(7) . . . 5_756 ? N4 Pb3 O7 Pb1 -24.6(8) 2_856 . . 5_756 ? N3 Pb3 O7 Pb1 -91.4(6) 8_556 . . 5_756 ? N3 Pb3 O7 Pb1 79.0(6) 7_755 . . 5_756 ? O6 Pb3 O7 Pb1 -142.8(5) 8_556 . . 5_756 ? O6 Pb3 O7 Pb1 114.3(5) 7_755 . . 5_756 ? O7 Pb3 O7 Pb1 -13.9(3) 2_856 . . 5_756 ? O1 Pb1 N1 C5 180.000(1) . . . . ? O8 Pb1 N1 C5 49.7(2) 2_756 . . . ? O8 Pb1 N1 C5 -49.7(2) 5_756 . . . ? O1 Pb1 N1 C5 180.000(1) 5_656 . . . ? O7 Pb1 N1 C5 -99.04(17) 5_756 . . . ? O7 Pb1 N1 C5 99.04(17) 2_756 . . . ? O1 Pb1 N1 C1 0.0 . . . . ? O8 Pb1 N1 C1 -130.3(2) 2_756 . . . ? O8 Pb1 N1 C1 130.3(2) 5_756 . . . ? O1 Pb1 N1 C1 0.0 5_656 . . . ? O7 Pb1 N1 C1 80.96(17) 5_756 . . . ? O7 Pb1 N1 C1 -80.96(17) 2_756 . . . ? O3 Pb2 N2 C10 0.000(1) . . . . ? O5 Pb2 N2 C10 130.6(2) . . . . ? O5 Pb2 N2 C10 -130.6(2) 6 . . . ? O3 Pb2 N2 C10 0.000(1) 5_754 . . . ? O6 Pb2 N2 C10 -82.8(2) 6 . . . ? O6 Pb2 N2 C10 82.8(2) . . . . ? O3 Pb2 N2 C14 180.0 . . . . ? O5 Pb2 N2 C14 -49.4(2) . . . . ? O5 Pb2 N2 C14 49.4(2) 6 . . . ? O3 Pb2 N2 C14 180.0 5_754 . . . ? O6 Pb2 N2 C14 97.2(2) 6 . . . ? O6 Pb2 N2 C14 -97.2(2) . . . . ? N4 Pb3 N4 C29 3.8(10) 2_856 . . . ? N3 Pb3 N4 C29 98.8(11) 8_556 . . . ? N3 Pb3 N4 C29 -96.9(11) 7_755 . . . ? O6 Pb3 N4 C29 41.7(11) 8_556 . . . ? O6 Pb3 N4 C29 -35.0(10) 7_755 . . . ? O7 Pb3 N4 C29 178.5(11) . . . . ? O7 Pb3 N4 C29 -169.5(9) 2_856 . . . ? N4 Pb3 N4 C25 175.1(10) 2_856 . . . ? N3 Pb3 N4 C25 -89.8(10) 8_556 . . . ? N3 Pb3 N4 C25 74.4(9) 7_755 . . . ? O6 Pb3 N4 C25 -147.0(10) 8_556 . . . ? O6 Pb3 N4 C25 136.3(10) 7_755 . . . ? O7 Pb3 N4 C25 -10.1(9) . . . . ? O7 Pb3 N4 C25 1.9(11) 2_856 . . . ? C5 N1 C1 C2 0.000(1) . . . . ? Pb1 N1 C1 C2 180.0 . . . . ? C5 N1 C1 C6 180.0 . . . . ? Pb1 N1 C1 C6 0.000(1) . . . . ? N1 C1 C2 C3 0.000(1) . . . . ? C6 C1 C2 C3 180.0 . . . . ? C1 C2 C3 C4 0.0 . . . . ? C1 C2 C3 C7 180.0 . . . . ? C2 C3 C4 C5 0.000(1) . . . . ? C7 C3 C4 C5 180.000(1) . . . . ? C3 C4 C5 N1 0.000(1) . . . . ? C1 N1 C5 C4 0.000(2) . . . . ? Pb1 N1 C5 C4 180.000(1) . . . . ? Pb1 O1 C6 O2 180.0 . . . . ? Pb1 O1 C6 O2 0.000(1) 5_656 . . . ? Pb1 O1 C6 C1 0.000(1) . . . . ? Pb1 O1 C6 C1 180.0 5_656 . . . ? C2 C1 C6 O2 0.000(1) . . . . ? N1 C1 C6 O2 180.000(1) . . . . ? C2 C1 C6 O1 180.0 . . . . ? N1 C1 C6 O1 0.000(1) . . . . ? C2 C3 C7 C8 180.0 . . . . ? C4 C3 C7 C8 0.0 . . . . ? C3 C7 C8 C9 180.0 . . . . ? C7 C8 C9 C12 180.0 . . . . ? C14 N2 C10 C11 0.000(2) . . . . ? Pb2 N2 C10 C11 180.000(1) . . . . ? C14 N2 C10 C15 180.000(1) . . . . ? Pb2 N2 C10 C15 0.000(1) . . . . ? N2 C10 C11 C12 0.000(2) . . . . ? C15 C10 C11 C12 180.000(2) . . . . ? C10 C11 C12 C13 0.000(2) . . . . ? C10 C11 C12 C9 180.000(1) . . . . ? C8 C9 C12 C11 180.000(1) . . . . ? C8 C9 C12 C13 0.000(1) . . . . ? C11 C12 C13 C14 0.000(1) . . . . ? C9 C12 C13 C14 180.0 . . . . ? C10 N2 C14 C13 0.000(1) . . . . ? Pb2 N2 C14 C13 180.0 . . . . ? C12 C13 C14 N2 0.000(1) . . . . ? Pb2 O3 C15 O4 180.000(2) . . . . ? Pb2 O3 C15 O4 0.000(3) 5_754 . . . ? Pb2 O3 C15 C10 0.000(2) . . . . ? Pb2 O3 C15 C10 180.000(1) 5_754 . . . ? N2 C10 C15 O4 180.000(2) . . . . ? C11 C10 C15 O4 0.000(2) . . . . ? N2 C10 C15 O3 0.000(2) . . . . ? C11 C10 C15 O3 180.000(1) . . . . ? C20 N3 C16 C17 0(2) . . . . ? Pb3 N3 C16 C17 170.8(10) 7_755 . . . ? C20 N3 C16 C21 177.5(12) . . . . ? Pb3 N3 C16 C21 -12.2(14) 7_755 . . . ? N3 C16 C17 C18 -2(2) . . . . ? C21 C16 C17 C18 -178.6(11) . . . . ? C16 C17 C18 C19 3(2) . . . . ? C16 C17 C18 C22 179.5(13) . . . . ? C17 C18 C19 C20 -3(2) . . . . ? C22 C18 C19 C20 -179.6(15) . . . . ? C18 C19 C20 N3 2(3) . . . . ? C16 N3 C20 C19 -1(2) . . . . ? Pb3 N3 C20 C19 -171.0(12) 7_755 . . . ? Pb2 O5 C21 O6 10.2(16) . . . . ? Pb2 O5 C21 C16 -171.3(9) . . . . ? Pb3 O6 C21 O5 -173.3(10) 7_755 . . . ? Pb2 O6 C21 O5 -8.8(14) . . . . ? Pb3 O6 C21 C16 8.2(16) 7_755 . . . ? Pb2 O6 C21 C16 172.6(11) . . . . ? C17 C16 C21 O5 1(2) . . . . ? N3 C16 C21 O5 -175.9(12) . . . . ? C17 C16 C21 O6 179.7(13) . . . . ? N3 C16 C21 O6 2.7(18) . . . . ? C17 C18 C22 C23 87.9(18) . . . . ? C19 C18 C22 C23 -96.1(18) . . . . ? C18 C22 C23 C24 177.8(16) . . . . ? C22 C23 C24 C27 172.6(15) . . . . ? C29 N4 C25 C26 -2(2) . . . . ? Pb3 N4 C25 C26 -173.8(12) . . . . ? C29 N4 C25 C30 -177.4(12) . . . . ? Pb3 N4 C25 C30 10.7(15) . . . . ? N4 C25 C26 C27 0(3) . . . . ? C30 C25 C26 C27 175.3(15) . . . . ? C25 C26 C27 C28 3(3) . . . . ? C25 C26 C27 C24 -178.9(18) . . . . ? C23 C24 C27 C28 103(2) . . . . ? C23 C24 C27 C26 -75(2) . . . . ? C26 C27 C28 C29 -3(3) . . . . ? C24 C27 C28 C29 178.4(18) . . . . ? C25 N4 C29 C28 1(2) . . . . ? Pb3 N4 C29 C28 173.2(13) . . . . ? C27 C28 C29 N4 1(3) . . . . ? Pb1 O8 C30 O7 -10.7(14) 5_756 . . . ? Pb1 O8 C30 C25 171.1(10) 5_756 . . . ? Pb3 O7 C30 O8 173.0(9) . . . . ? Pb1 O7 C30 O8 9.8(13) 5_756 . . . ? Pb3 O7 C30 C25 -8.9(15) . . . . ? Pb1 O7 C30 C25 -172.0(10) 5_756 . . . ? N4 C25 C30 O8 177.2(11) . . . . ? C26 C25 C30 O8 1(2) . . . . ? N4 C25 C30 O7 -1.1(18) . . . . ? C26 C25 C30 O7 -176.9(13) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.195 _refine_diff_density_min -1.723 _refine_diff_density_rms 0.214 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 0.250 0.250 0.000 117 16 ' ' 2 0.750 0.250 0.000 117 16 ' ' 3 0.250 0.750 0.000 116 15 ' ' 4 0.750 0.750 0.000 116 15 ' ' 5 0.135 0.145 0.265 18 3 ' ' 6 0.635 0.355 0.265 17 3 ' ' 7 0.635 0.645 0.265 18 3 ' ' 8 0.135 0.855 0.265 17 3 ' ' 9 0.865 0.145 0.735 17 3 ' ' 10 0.365 0.355 0.735 17 3 ' ' 11 0.365 0.645 0.735 17 3 ' ' 12 0.865 0.855 0.735 17 3 ' ' _platon_squeeze_details ; ; #===END #============================================================================== data_5 #============================================================================== data_b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H28 N4 O10 Pb2' _chemical_formula_weight 1018.94 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 Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_HALL '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.795(2) _cell_length_b 13.2729(11) _cell_length_c 13.9455(12) _cell_angle_alpha 118.0390(10) _cell_angle_beta 105.7820(10) _cell_angle_gamma 92.5540(10) _cell_volume 1815.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 5939 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 9.315 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1220 _exptl_absorpt_correction_T_max 0.6049 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13017 _diffrn_reflns_av_R_equivalents 0.0257 _diffrn_reflns_av_sigmaI/netI 0.0402 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.28 _diffrn_reflns_theta_max 25.50 _reflns_number_total 6528 _reflns_number_gt 5330 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+1.3574P] 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 6528 _refine_ls_number_parameters 415 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0656 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 1.083 _refine_ls_restrained_S_all 1.090 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.180775(17) 0.538049(18) 0.561342(16) 0.03495(7) Uani 1 1 d D . . Pb2 Pb 0.023691(17) 0.512640(18) 0.172165(16) 0.03293(7) Uani 1 1 d . . . N1 N 0.9583(4) 1.2719(4) 0.6955(4) 0.0357(11) Uani 1 1 d . . . N2 N 0.3729(4) 0.5624(4) 0.7176(4) 0.0369(11) Uani 1 1 d . . . N3 N 0.7703(4) 1.2359(4) 1.2948(5) 0.0520(14) Uani 1 1 d . . . N4 N 0.2534(4) 0.6110(4) 0.2346(3) 0.0357(11) Uani 1 1 d . . . O1 O 0.1472(3) 0.5148(4) 0.7221(3) 0.0535(11) Uani 1 1 d . . . O2 O 0.2222(4) 0.5203(4) 0.8878(4) 0.0605(13) Uani 1 1 d . . . O3 O 1.0695(4) 1.2206(5) 1.3056(5) 0.095(2) Uani 1 1 d . . . O4 O 0.9950(4) 1.3571(4) 1.4251(4) 0.0579(12) Uani 1 1 d . . . O5 O 0.1622(3) 0.5550(4) 0.3672(3) 0.0484(8) Uani 1 1 d U . . O6 O 0.3411(4) 0.6162(4) 0.5017(3) 0.0564(9) Uani 1 1 d U . . O7 O 1.0020(5) 1.1969(4) 0.9124(4) 0.0679(14) Uani 1 1 d . . . O8 O 0.9989(3) 1.3708(3) 0.9254(3) 0.0432(10) Uani 1 1 d . . . O9 O 0.1111(5) 0.3014(5) 0.1459(4) 0.0879(17) Uani 1 1 d . . . H1W H 0.0713 0.2528 0.1522 0.132 Uiso 1 1 d R . . H2W H 0.1121 0.2744 0.0790 0.132 Uiso 1 1 d R . . O10 O 0.2942(6) 0.3470(6) 0.4347(6) 0.123(2) Uani 1 1 d . . . H3W H 0.2780 0.3464 0.3726 0.185 Uiso 1 1 d RD . . H4W H 0.2512 0.2908 0.4276 0.185 Uiso 1 1 d RD . . C1 C 0.3602(5) 0.5613(5) 0.8104(4) 0.0327(12) Uani 1 1 d . . . C2 C 0.4597(5) 0.5901(5) 0.9060(5) 0.0379(13) Uani 1 1 d . . . H2 H 0.4491 0.5887 0.9691 0.045 Uiso 1 1 calc R . . C3 C 0.5749(5) 0.6208(5) 0.9082(5) 0.0390(13) Uani 1 1 d . . . C4 C 0.5855(5) 0.6191(5) 0.8108(5) 0.0397(14) Uani 1 1 d . . . H4 H 0.6609 0.6381 0.8079 0.048 Uiso 1 1 calc R . . C5 C 0.4838(5) 0.5891(5) 0.7187(5) 0.0415(14) Uani 1 1 d . . . H5 H 0.4927 0.5873 0.6536 0.050 Uiso 1 1 calc R . . C6 C 0.2339(5) 0.5298(5) 0.8069(5) 0.0396(13) Uani 1 1 d . . . C7 C 0.6828(5) 0.6623(5) 1.0142(5) 0.0466(15) Uani 1 1 d . . . H7A H 0.7546 0.6494 0.9924 0.056 Uiso 1 1 calc R . . H7B H 0.6742 0.6179 1.0515 0.056 Uiso 1 1 calc R . . C8 C 0.6968(6) 0.7947(5) 1.1001(5) 0.0502(16) Uani 1 1 d . . . H8A H 0.6275 0.8061 1.1260 0.060 Uiso 1 1 calc R . . H8B H 0.7677 0.8193 1.1669 0.060 Uiso 1 1 calc R . . C9 C 0.7080(6) 0.8704(5) 1.0475(5) 0.0554(17) Uani 1 1 d . . . H9A H 0.7742 0.8555 1.0172 0.067 Uiso 1 1 calc R . . H9B H 0.6349 0.8493 0.9837 0.067 Uiso 1 1 calc R . . C10 C 0.7293(6) 0.9983(5) 1.1330(5) 0.0527(16) Uani 1 1 d . . . C11 C 0.6366(6) 1.0525(6) 1.1569(7) 0.076(2) Uani 1 1 d . . . H11 H 0.5578 1.0103 1.1189 0.091 Uiso 1 1 calc R . . C12 C 0.6592(6) 1.1694(6) 1.2371(7) 0.083(3) Uani 1 1 d . . . H12 H 0.5944 1.2038 1.2520 0.099 Uiso 1 1 calc R . . C13 C 0.8625(5) 1.1844(5) 1.2733(5) 0.0421(14) Uani 1 1 d . . . C14 C 0.8442(6) 1.0667(5) 1.1940(5) 0.0507(16) Uani 1 1 d . . . H14 H 0.9102 1.0332 1.1815 0.061 Uiso 1 1 calc R . . C15 C 0.9851(6) 1.2593(6) 1.3399(5) 0.0534(17) Uani 1 1 d . . . C16 C 0.3276(5) 0.6305(5) 0.3368(4) 0.0330(12) Uani 1 1 d . . . C17 C 0.4501(5) 0.6751(5) 0.3759(5) 0.0383(13) Uani 1 1 d . . . H17 H 0.4980 0.6883 0.4474 0.046 Uiso 1 1 calc R . . C18 C 0.5012(5) 0.6998(5) 0.3096(5) 0.0395(13) Uani 1 1 d . . . C19 C 0.4234(5) 0.6828(5) 0.2072(5) 0.0469(15) Uani 1 1 d . . . H19 H 0.4528 0.7020 0.1611 0.056 Uiso 1 1 calc R . . C20 C 0.3016(5) 0.6373(5) 0.1719(5) 0.0467(15) Uani 1 1 d . . . H20 H 0.2519 0.6248 0.1013 0.056 Uiso 1 1 calc R . . C21 C 0.2731(5) 0.5976(6) 0.4059(5) 0.0511(9) Uani 1 1 d U . . C22 C 0.6355(5) 0.7410(5) 0.3484(5) 0.0455(15) Uani 1 1 d . . . H22A H 0.6587 0.7204 0.2809 0.055 Uiso 1 1 calc R . . H22B H 0.6753 0.6995 0.3849 0.055 Uiso 1 1 calc R . . C23 C 0.6806(5) 0.8715(5) 0.4317(5) 0.0509(16) Uani 1 1 d . . . H23A H 0.6483 0.9140 0.3934 0.061 Uiso 1 1 calc R . . H23B H 0.6525 0.8944 0.4969 0.061 Uiso 1 1 calc R . . C24 C 0.8175(5) 0.9024(5) 0.4743(5) 0.0504(16) Uani 1 1 d . . . H24A H 0.8487 0.8627 0.5161 0.061 Uiso 1 1 calc R . . H24B H 0.8449 0.8737 0.4083 0.061 Uiso 1 1 calc R . . C25 C 0.8690(5) 1.0318(5) 0.5518(5) 0.0420(14) Uani 1 1 d . . . C26 C 0.9056(5) 1.0825(5) 0.6710(5) 0.0431(14) Uani 1 1 d . . . H26 H 0.9018 1.0366 0.7044 0.052 Uiso 1 1 calc R . . C27 C 0.9481(5) 1.2023(5) 0.7400(5) 0.0362(13) Uani 1 1 d . . . C28 C 0.9274(5) 1.2214(5) 0.5811(5) 0.0419(14) Uani 1 1 d . . . H28 H 0.9369 1.2680 0.5495 0.050 Uiso 1 1 calc R . . C29 C 0.8818(5) 1.1032(5) 0.5072(5) 0.0468(15) Uani 1 1 d . . . H29 H 0.8599 1.0721 0.4280 0.056 Uiso 1 1 calc R . . C30 C 0.9857(5) 1.2604(6) 0.8697(5) 0.0432(14) 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 0.03076(12) 0.03739(14) 0.03009(12) 0.01644(10) 0.00310(9) -0.00338(9) Pb2 0.02850(12) 0.03593(13) 0.03043(12) 0.01641(10) 0.00533(8) 0.00176(9) N1 0.035(2) 0.033(3) 0.034(2) 0.013(2) 0.011(2) 0.003(2) N2 0.029(2) 0.043(3) 0.033(2) 0.016(2) 0.0077(19) 0.002(2) N3 0.035(3) 0.033(3) 0.067(3) 0.015(3) 0.008(2) -0.004(2) N4 0.034(2) 0.044(3) 0.031(2) 0.020(2) 0.011(2) 0.002(2) O1 0.030(2) 0.087(3) 0.049(2) 0.043(2) 0.0077(19) 0.000(2) O2 0.048(3) 0.100(4) 0.058(3) 0.058(3) 0.019(2) 0.011(3) O3 0.049(3) 0.080(4) 0.104(4) 0.010(3) 0.025(3) -0.002(3) O4 0.039(2) 0.048(3) 0.055(3) 0.007(2) 0.006(2) -0.010(2) O5 0.0355(15) 0.075(2) 0.0391(15) 0.0366(15) 0.0056(13) -0.0027(14) O6 0.0405(15) 0.083(2) 0.0428(15) 0.0367(16) 0.0026(13) -0.0053(15) O7 0.096(4) 0.055(3) 0.049(3) 0.033(2) 0.007(3) 0.005(3) O8 0.052(2) 0.040(3) 0.034(2) 0.0177(19) 0.0090(18) 0.0073(19) O9 0.102(4) 0.094(4) 0.066(3) 0.035(3) 0.033(3) 0.017(3) O10 0.092(5) 0.113(5) 0.119(5) 0.044(4) -0.002(4) 0.006(4) C1 0.033(3) 0.033(3) 0.031(3) 0.015(2) 0.011(2) 0.006(2) C2 0.041(3) 0.030(3) 0.034(3) 0.013(3) 0.007(2) 0.005(3) C3 0.037(3) 0.026(3) 0.039(3) 0.011(3) 0.002(2) 0.003(2) C4 0.030(3) 0.035(3) 0.046(3) 0.015(3) 0.011(3) 0.003(2) C5 0.039(3) 0.045(4) 0.038(3) 0.019(3) 0.012(3) 0.003(3) C6 0.039(3) 0.040(3) 0.044(3) 0.025(3) 0.012(3) 0.004(3) C7 0.043(3) 0.036(3) 0.045(3) 0.018(3) -0.004(3) -0.004(3) C8 0.047(4) 0.045(4) 0.037(3) 0.013(3) -0.001(3) -0.004(3) C9 0.073(5) 0.035(4) 0.045(4) 0.015(3) 0.011(3) 0.003(3) C10 0.060(4) 0.034(4) 0.049(4) 0.015(3) 0.009(3) -0.004(3) C11 0.047(4) 0.039(4) 0.098(6) 0.012(4) 0.007(4) -0.012(3) C12 0.040(4) 0.045(4) 0.113(6) 0.009(4) 0.012(4) -0.004(3) C13 0.043(3) 0.041(4) 0.036(3) 0.017(3) 0.010(3) 0.000(3) C14 0.051(4) 0.045(4) 0.045(3) 0.018(3) 0.010(3) 0.007(3) C15 0.040(4) 0.064(5) 0.046(4) 0.022(4) 0.010(3) -0.001(3) C16 0.034(3) 0.034(3) 0.034(3) 0.020(3) 0.011(2) 0.006(2) C17 0.036(3) 0.034(3) 0.037(3) 0.015(3) 0.008(2) 0.001(2) C18 0.038(3) 0.036(3) 0.041(3) 0.016(3) 0.015(3) 0.003(3) C19 0.048(4) 0.054(4) 0.046(3) 0.028(3) 0.022(3) 0.000(3) C20 0.044(3) 0.061(4) 0.040(3) 0.030(3) 0.013(3) 0.004(3) C21 0.0374(15) 0.078(2) 0.0400(15) 0.0369(15) 0.0047(12) -0.0035(14) C22 0.034(3) 0.043(4) 0.049(3) 0.014(3) 0.018(3) -0.002(3) C23 0.039(3) 0.046(4) 0.054(4) 0.016(3) 0.014(3) -0.001(3) C24 0.036(3) 0.037(4) 0.057(4) 0.010(3) 0.012(3) 0.001(3) C25 0.027(3) 0.038(3) 0.047(3) 0.013(3) 0.009(2) 0.000(2) C26 0.035(3) 0.049(4) 0.046(3) 0.027(3) 0.009(3) 0.001(3) C27 0.033(3) 0.037(3) 0.038(3) 0.020(3) 0.009(2) 0.007(2) C28 0.047(3) 0.044(4) 0.038(3) 0.020(3) 0.020(3) 0.009(3) C29 0.049(4) 0.047(4) 0.037(3) 0.014(3) 0.016(3) 0.006(3) C30 0.033(3) 0.052(4) 0.046(3) 0.028(3) 0.009(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 O1 2.531(4) . ? Pb1 O4 2.549(4) 2_677 ? Pb1 N2 2.564(4) . ? Pb1 O6 2.614(4) . ? Pb1 N3 2.630(5) 2_677 ? Pb1 O4 2.675(4) 1_444 ? Pb1 O5 2.771(4) . ? Pb1 O10 2.952(7) . ? Pb2 O8 2.477(4) 2_676 ? Pb2 N1 2.530(4) 2_676 ? Pb2 O5 2.539(4) . ? Pb2 N4 2.671(4) . ? Pb2 O2 2.743(4) 2_566 ? Pb2 O1 2.902(4) 2_566 ? Pb2 O9 2.925(6) . ? Pb2 O8 2.964(4) 1_444 ? N1 C28 1.336(7) . ? N1 C27 1.349(7) . ? N1 Pb2 2.530(4) 2_676 ? N2 C5 1.334(7) . ? N2 C1 1.348(6) . ? N3 C13 1.337(7) . ? N3 C12 1.341(8) . ? N3 Pb1 2.630(5) 2_677 ? N4 C20 1.322(7) . ? N4 C16 1.348(6) . ? O1 C6 1.259(7) . ? O1 Pb2 2.902(4) 2_566 ? O2 C6 1.234(6) . ? O2 Pb2 2.743(4) 2_566 ? O3 C15 1.248(8) . ? O4 C15 1.253(7) . ? O4 Pb1 2.549(4) 2_677 ? O4 Pb1 2.675(4) 1_666 ? O5 C21 1.258(6) . ? O6 C21 1.256(6) . ? O7 C30 1.235(7) . ? O8 C30 1.272(7) . ? O8 Pb2 2.477(4) 2_676 ? O8 Pb2 2.964(4) 1_666 ? O9 H1W 0.8321 . ? O9 H2W 0.8307 . ? O10 H3W 0.8304 . ? O10 H4W 0.8324 . ? C1 C2 1.391(7) . ? C1 C6 1.511(7) . ? C2 C3 1.389(8) . ? C2 H2 0.9300 . ? C3 C4 1.386(8) . ? C3 C7 1.502(7) . ? C4 C5 1.374(7) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C7 C8 1.561(8) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.517(9) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.504(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.367(9) . ? C10 C14 1.387(8) . ? C11 C12 1.378(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.388(8) . ? C13 C15 1.489(8) . ? C14 H14 0.9300 . ? C16 C17 1.388(7) . ? C16 C21 1.497(7) . ? C17 C18 1.377(7) . ? C17 H17 0.9300 . ? C18 C19 1.378(8) . ? C18 C22 1.510(7) . ? C19 C20 1.389(8) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C22 C23 1.524(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.522(8) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.514(8) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C29 1.379(8) . ? C25 C26 1.391(8) . ? C26 C27 1.390(8) . ? C26 H26 0.9300 . ? C27 C30 1.512(8) . ? C28 C29 1.384(8) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O4 84.15(14) . 2_677 ? O1 Pb1 N2 64.89(13) . . ? O4 Pb1 N2 131.02(14) 2_677 . ? O1 Pb1 O6 143.93(12) . . ? O4 Pb1 O6 114.58(15) 2_677 . ? N2 Pb1 O6 80.28(13) . . ? O1 Pb1 N3 86.58(16) . 2_677 ? O4 Pb1 N3 62.23(14) 2_677 2_677 ? N2 Pb1 N3 78.18(15) . 2_677 ? O6 Pb1 N3 77.00(15) . 2_677 ? O1 Pb1 O4 84.37(14) . 1_444 ? O4 Pb1 O4 79.42(15) 2_677 1_444 ? N2 Pb1 O4 129.78(15) . 1_444 ? O6 Pb1 O4 127.73(13) . 1_444 ? N3 Pb1 O4 141.29(14) 2_677 1_444 ? O1 Pb1 O5 167.24(12) . . ? O4 Pb1 O5 85.75(14) 2_677 . ? N2 Pb1 O5 127.87(12) . . ? O6 Pb1 O5 48.38(11) . . ? N3 Pb1 O5 95.59(15) 2_677 . ? O4 Pb1 O5 86.12(13) 1_444 . ? O1 Pb1 O10 108.11(18) . . ? O4 Pb1 O10 151.93(15) 2_677 . ? N2 Pb1 O10 76.54(15) . . ? O6 Pb1 O10 70.30(18) . . ? N3 Pb1 O10 141.35(17) 2_677 . ? O4 Pb1 O10 76.89(15) 1_444 . ? O5 Pb1 O10 77.87(17) . . ? O8 Pb2 N1 65.71(13) 2_676 2_676 ? O8 Pb2 O5 131.79(13) 2_676 . ? N1 Pb2 O5 75.24(14) 2_676 . ? O8 Pb2 N4 79.48(13) 2_676 . ? N1 Pb2 N4 74.15(14) 2_676 . ? O5 Pb2 N4 63.04(12) . . ? O8 Pb2 O2 84.73(13) 2_676 2_566 ? N1 Pb2 O2 90.23(14) 2_676 2_566 ? O5 Pb2 O2 123.62(12) . 2_566 ? N4 Pb2 O2 161.26(15) . 2_566 ? O8 Pb2 O1 122.28(12) 2_676 2_566 ? N1 Pb2 O1 83.98(13) 2_676 2_566 ? O5 Pb2 O1 78.25(11) . 2_566 ? N4 Pb2 O1 139.06(12) . 2_566 ? O2 Pb2 O1 45.80(11) 2_566 2_566 ? O8 Pb2 O9 138.08(13) 2_676 . ? N1 Pb2 O9 146.25(14) 2_676 . ? O5 Pb2 O9 71.37(14) . . ? N4 Pb2 O9 86.40(15) . . ? O2 Pb2 O9 112.20(15) 2_566 . ? O1 Pb2 O9 93.83(14) 2_566 . ? O8 Pb2 O8 67.69(14) 2_676 1_444 ? N1 Pb2 O8 133.22(13) 2_676 1_444 ? O5 Pb2 O8 139.10(12) . 1_444 ? N4 Pb2 O8 93.71(11) . 1_444 ? O2 Pb2 O8 89.52(12) 2_566 1_444 ? O1 Pb2 O8 125.76(11) 2_566 1_444 ? O9 Pb2 O8 74.17(12) . 1_444 ? C28 N1 C27 117.5(5) . . ? C28 N1 Pb2 123.8(4) . 2_676 ? C27 N1 Pb2 116.2(3) . 2_676 ? C5 N2 C1 118.4(5) . . ? C5 N2 Pb1 123.9(4) . . ? C1 N2 Pb1 117.3(3) . . ? C13 N3 C12 117.6(5) . . ? C13 N3 Pb1 117.6(4) . 2_677 ? C12 N3 Pb1 124.8(4) . 2_677 ? C20 N4 C16 117.3(5) . . ? C20 N4 Pb2 125.7(4) . . ? C16 N4 Pb2 116.9(3) . . ? C6 O1 Pb1 121.5(3) . . ? C6 O1 Pb2 90.9(3) . 2_566 ? Pb1 O1 Pb2 147.12(16) . 2_566 ? C6 O2 Pb2 99.1(4) . 2_566 ? C15 O4 Pb1 121.6(4) . 2_677 ? C15 O4 Pb1 131.5(4) . 1_666 ? Pb1 O4 Pb1 100.58(15) 2_677 1_666 ? C21 O5 Pb2 123.7(3) . . ? C21 O5 Pb1 90.5(3) . . ? Pb2 O5 Pb1 145.70(15) . . ? C21 O6 Pb1 98.0(3) . . ? C30 O8 Pb2 121.8(3) . 2_676 ? C30 O8 Pb2 125.4(3) . 1_666 ? Pb2 O8 Pb2 112.31(14) 2_676 1_666 ? Pb2 O9 H1W 119.5 . . ? Pb2 O9 H2W 98.3 . . ? H1W O9 H2W 111.3 . . ? Pb1 O10 H3W 100.8 . . ? Pb1 O10 H4W 100.1 . . ? H3W O10 H4W 110.9 . . ? N2 C1 C2 121.0(5) . . ? N2 C1 C6 117.5(5) . . ? C2 C1 C6 121.5(5) . . ? C3 C2 C1 120.6(5) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 117.2(5) . . ? C4 C3 C7 121.1(5) . . ? C2 C3 C7 121.6(5) . . ? C5 C4 C3 119.5(5) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? N2 C5 C4 123.4(5) . . ? N2 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? O2 C6 O1 124.0(5) . . ? O2 C6 C1 117.7(5) . . ? O1 C6 C1 118.3(5) . . ? C3 C7 C8 110.8(5) . . ? C3 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 . . ? C3 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 108.1 . . ? C9 C8 C7 112.9(5) . . ? C9 C8 H8A 109.0 . . ? C7 C8 H8A 109.0 . . ? C9 C8 H8B 109.0 . . ? C7 C8 H8B 109.0 . . ? H8A C8 H8B 107.8 . . ? C10 C9 C8 112.5(5) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? C11 C10 C14 116.5(6) . . ? C11 C10 C9 121.8(6) . . ? C14 C10 C9 121.7(6) . . ? C10 C11 C12 120.3(6) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? N3 C12 C11 123.1(7) . . ? N3 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? N3 C13 C14 121.4(5) . . ? N3 C13 C15 116.7(5) . . ? C14 C13 C15 121.9(6) . . ? C10 C14 C13 121.1(6) . . ? C10 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? O3 C15 O4 125.2(6) . . ? O3 C15 C13 117.5(6) . . ? O4 C15 C13 117.3(6) . . ? N4 C16 C17 122.4(5) . . ? N4 C16 C21 117.0(5) . . ? C17 C16 C21 120.5(5) . . ? C18 C17 C16 120.5(5) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C17 C18 C19 116.2(5) . . ? C17 C18 C22 120.7(5) . . ? C19 C18 C22 123.1(5) . . ? C18 C19 C20 120.8(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? N4 C20 C19 122.7(5) . . ? N4 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? O6 C21 O5 123.1(5) . . ? O6 C21 C16 117.6(5) . . ? O5 C21 C16 119.2(5) . . ? O6 C21 Pb1 58.0(3) . . ? O5 C21 Pb1 65.2(3) . . ? C16 C21 Pb1 175.6(4) . . ? C18 C22 C23 114.8(5) . . ? C18 C22 H22A 108.6 . . ? C23 C22 H22A 108.6 . . ? C18 C22 H22B 108.6 . . ? C23 C22 H22B 108.6 . . ? H22A C22 H22B 107.5 . . ? C24 C23 C22 110.8(5) . . ? C24 C23 H23A 109.5 . . ? C22 C23 H23A 109.5 . . ? C24 C23 H23B 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 108.1 . . ? C25 C24 C23 113.9(5) . . ? C25 C24 H24A 108.8 . . ? C23 C24 H24A 108.8 . . ? C25 C24 H24B 108.8 . . ? C23 C24 H24B 108.8 . . ? H24A C24 H24B 107.7 . . ? C29 C25 C26 117.8(5) . . ? C29 C25 C24 121.4(5) . . ? C26 C25 C24 120.8(6) . . ? C27 C26 C25 119.5(6) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? N1 C27 C26 122.3(5) . . ? N1 C27 C30 116.9(5) . . ? C26 C27 C30 120.8(5) . . ? N1 C28 C29 123.2(6) . . ? N1 C28 H28 118.4 . . ? C29 C28 H28 118.4 . . ? C25 C29 C28 119.6(5) . . ? C25 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? O7 C30 O8 125.7(6) . . ? O7 C30 C27 117.3(6) . . ? O8 C30 C27 117.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Pb1 N2 C5 -177.9(5) . . . . ? O4 Pb1 N2 C5 -121.8(4) 2_677 . . . ? O6 Pb1 N2 C5 -7.5(4) . . . . ? N3 Pb1 N2 C5 -86.2(5) 2_677 . . . ? O4 Pb1 N2 C5 124.2(4) 1_444 . . . ? O5 Pb1 N2 C5 1.7(5) . . . . ? O10 Pb1 N2 C5 64.4(5) . . . . ? C21 Pb1 N2 C5 -3.2(5) . . . . ? Pb1 Pb1 N2 C5 178.3(3) 2_566 . . . ? O1 Pb1 N2 C1 -5.9(4) . . . . ? O4 Pb1 N2 C1 50.3(4) 2_677 . . . ? O6 Pb1 N2 C1 164.5(4) . . . . ? N3 Pb1 N2 C1 85.9(4) 2_677 . . . ? O4 Pb1 N2 C1 -63.8(4) 1_444 . . . ? O5 Pb1 N2 C1 173.8(3) . . . . ? O10 Pb1 N2 C1 -123.6(4) . . . . ? C21 Pb1 N2 C1 168.8(4) . . . . ? Pb1 Pb1 N2 C1 -9.7(5) 2_566 . . . ? O8 Pb2 N4 C20 -32.7(5) 2_676 . . . ? N1 Pb2 N4 C20 -100.2(5) 2_676 . . . ? O5 Pb2 N4 C20 178.6(5) . . . . ? O2 Pb2 N4 C20 -65.7(7) 2_566 . . . ? O1 Pb2 N4 C20 -160.7(4) 2_566 . . . ? O9 Pb2 N4 C20 107.6(5) . . . . ? O8 Pb2 N4 C20 33.8(5) 1_444 . . . ? O8 Pb2 N4 C16 150.5(4) 2_676 . . . ? N1 Pb2 N4 C16 83.0(4) 2_676 . . . ? O5 Pb2 N4 C16 1.7(4) . . . . ? O2 Pb2 N4 C16 117.5(5) 2_566 . . . ? O1 Pb2 N4 C16 22.5(5) 2_566 . . . ? O9 Pb2 N4 C16 -69.2(4) . . . . ? O8 Pb2 N4 C16 -143.0(4) 1_444 . . . ? O4 Pb1 O1 C6 -137.7(5) 2_677 . . . ? N2 Pb1 O1 C6 3.3(4) . . . . ? O6 Pb1 O1 C6 -13.0(6) . . . . ? N3 Pb1 O1 C6 -75.2(5) 2_677 . . . ? O4 Pb1 O1 C6 142.4(5) 1_444 . . . ? O5 Pb1 O1 C6 -175.5(5) . . . . ? O10 Pb1 O1 C6 68.2(5) . . . . ? C21 Pb1 O1 C6 -21.7(11) . . . . ? Pb1 Pb1 O1 C6 -178.8(5) 2_566 . . . ? O4 Pb1 O1 Pb2 31.3(3) 2_677 . . 2_566 ? N2 Pb1 O1 Pb2 172.2(4) . . . 2_566 ? O6 Pb1 O1 Pb2 156.0(3) . . . 2_566 ? N3 Pb1 O1 Pb2 93.7(4) 2_677 . . 2_566 ? O4 Pb1 O1 Pb2 -48.6(3) 1_444 . . 2_566 ? O5 Pb1 O1 Pb2 -6.6(9) . . . 2_566 ? O10 Pb1 O1 Pb2 -122.8(3) . . . 2_566 ? C21 Pb1 O1 Pb2 147.2(7) . . . 2_566 ? Pb1 Pb1 O1 Pb2 -9.8(3) 2_566 . . 2_566 ? O8 Pb2 O5 C21 -45.5(6) 2_676 . . . ? N1 Pb2 O5 C21 -81.8(5) 2_676 . . . ? N4 Pb2 O5 C21 -2.3(5) . . . . ? O2 Pb2 O5 C21 -162.0(5) 2_566 . . . ? O1 Pb2 O5 C21 -168.6(5) 2_566 . . . ? O9 Pb2 O5 C21 93.2(5) . . . . ? O8 Pb2 O5 C21 59.2(6) 1_444 . . . ? O8 Pb2 O5 Pb1 138.6(3) 2_676 . . . ? N1 Pb2 O5 Pb1 102.3(3) 2_676 . . . ? N4 Pb2 O5 Pb1 -178.2(4) . . . . ? O2 Pb2 O5 Pb1 22.1(4) 2_566 . . . ? O1 Pb2 O5 Pb1 15.5(3) 2_566 . . . ? O9 Pb2 O5 Pb1 -82.7(3) . . . . ? O8 Pb2 O5 Pb1 -116.7(3) 1_444 . . . ? O1 Pb1 O5 C21 166.9(6) . . . . ? O4 Pb1 O5 C21 129.1(4) 2_677 . . . ? N2 Pb1 O5 C21 -11.7(5) . . . . ? O6 Pb1 O5 C21 0.5(4) . . . . ? N3 Pb1 O5 C21 67.6(4) 2_677 . . . ? O4 Pb1 O5 C21 -151.2(4) 1_444 . . . ? O10 Pb1 O5 C21 -73.8(4) . . . . ? Pb1 Pb1 O5 C21 170.1(4) 2_566 . . . ? O1 Pb1 O5 Pb2 -16.5(9) . . . . ? O4 Pb1 O5 Pb2 -54.3(3) 2_677 . . . ? N2 Pb1 O5 Pb2 164.8(3) . . . . ? O6 Pb1 O5 Pb2 177.1(4) . . . . ? N3 Pb1 O5 Pb2 -115.8(3) 2_677 . . . ? O4 Pb1 O5 Pb2 25.4(3) 1_444 . . . ? O10 Pb1 O5 Pb2 102.8(3) . . . . ? C21 Pb1 O5 Pb2 176.6(6) . . . . ? Pb1 Pb1 O5 Pb2 -13.3(3) 2_566 . . . ? O1 Pb1 O6 C21 -175.5(4) . . . . ? O4 Pb1 O6 C21 -59.5(4) 2_677 . . . ? N2 Pb1 O6 C21 169.6(4) . . . . ? N3 Pb1 O6 C21 -110.4(4) 2_677 . . . ? O4 Pb1 O6 C21 36.1(5) 1_444 . . . ? O5 Pb1 O6 C21 -0.5(4) . . . . ? O10 Pb1 O6 C21 90.6(4) . . . . ? Pb1 Pb1 O6 C21 -14.6(5) 2_566 . . . ? C5 N2 C1 C2 1.6(8) . . . . ? Pb1 N2 C1 C2 -170.9(4) . . . . ? C5 N2 C1 C6 -179.5(5) . . . . ? Pb1 N2 C1 C6 8.0(6) . . . . ? N2 C1 C2 C3 0.1(8) . . . . ? C6 C1 C2 C3 -178.8(5) . . . . ? C1 C2 C3 C4 -1.3(8) . . . . ? C1 C2 C3 C7 174.5(5) . . . . ? C2 C3 C4 C5 0.8(8) . . . . ? C7 C3 C4 C5 -175.1(5) . . . . ? C1 N2 C5 C4 -2.1(9) . . . . ? Pb1 N2 C5 C4 169.9(4) . . . . ? C3 C4 C5 N2 0.9(9) . . . . ? Pb2 O2 C6 O1 -5.9(7) 2_566 . . . ? Pb2 O2 C6 C1 174.2(4) 2_566 . . . ? Pb1 O1 C6 O2 179.5(5) . . . . ? Pb2 O1 C6 O2 5.5(6) 2_566 . . . ? Pb1 O1 C6 C1 -0.6(7) . . . . ? Pb2 O1 C6 C1 -174.6(5) 2_566 . . . ? N2 C1 C6 O2 174.7(5) . . . . ? C2 C1 C6 O2 -6.3(8) . . . . ? N2 C1 C6 O1 -5.2(8) . . . . ? C2 C1 C6 O1 173.8(5) . . . . ? C4 C3 C7 C8 93.5(7) . . . . ? C2 C3 C7 C8 -82.2(7) . . . . ? C3 C7 C8 C9 -57.8(7) . . . . ? C7 C8 C9 C10 -176.4(5) . . . . ? C8 C9 C10 C11 -83.7(9) . . . . ? C8 C9 C10 C14 94.5(8) . . . . ? C14 C10 C11 C12 0.6(12) . . . . ? C9 C10 C11 C12 178.9(7) . . . . ? C13 N3 C12 C11 -0.9(12) . . . . ? Pb1 N3 C12 C11 175.8(6) 2_677 . . . ? C10 C11 C12 N3 0.4(14) . . . . ? C12 N3 C13 C14 0.3(10) . . . . ? Pb1 N3 C13 C14 -176.6(4) 2_677 . . . ? C12 N3 C13 C15 -178.9(7) . . . . ? Pb1 N3 C13 C15 4.2(7) 2_677 . . . ? C11 C10 C14 C13 -1.2(10) . . . . ? C9 C10 C14 C13 -179.5(6) . . . . ? N3 C13 C14 C10 0.7(10) . . . . ? C15 C13 C14 C10 179.9(6) . . . . ? Pb1 O4 C15 O3 153.6(6) 2_677 . . . ? Pb1 O4 C15 O3 7.3(11) 1_666 . . . ? Pb1 O4 C15 C13 -25.5(8) 2_677 . . . ? Pb1 O4 C15 C13 -171.8(4) 1_666 . . . ? N3 C13 C15 O3 -165.8(7) . . . . ? C14 C13 C15 O3 15.0(10) . . . . ? N3 C13 C15 O4 13.4(9) . . . . ? C14 C13 C15 O4 -165.9(6) . . . . ? C20 N4 C16 C17 -0.7(8) . . . . ? Pb2 N4 C16 C17 176.3(4) . . . . ? C20 N4 C16 C21 -178.4(6) . . . . ? Pb2 N4 C16 C21 -1.3(6) . . . . ? N4 C16 C17 C18 -0.9(9) . . . . ? C21 C16 C17 C18 176.7(6) . . . . ? C16 C17 C18 C19 2.9(8) . . . . ? C16 C17 C18 C22 -176.1(5) . . . . ? C17 C18 C19 C20 -3.3(9) . . . . ? C22 C18 C19 C20 175.6(6) . . . . ? C16 N4 C20 C19 0.3(9) . . . . ? Pb2 N4 C20 C19 -176.5(4) . . . . ? C18 C19 C20 N4 1.8(10) . . . . ? Pb1 O6 C21 O5 1.1(8) . . . . ? Pb1 O6 C21 C16 179.7(5) . . . . ? Pb2 O5 C21 O6 -178.7(5) . . . . ? Pb1 O5 C21 O6 -1.0(7) . . . . ? Pb2 O5 C21 C16 2.7(9) . . . . ? Pb1 O5 C21 C16 -179.7(6) . . . . ? Pb2 O5 C21 Pb1 -177.7(4) . . . . ? N4 C16 C21 O6 -179.5(6) . . . . ? C17 C16 C21 O6 2.8(9) . . . . ? N4 C16 C21 O5 -0.7(9) . . . . ? C17 C16 C21 O5 -178.4(6) . . . . ? N4 C16 C21 Pb1 -177(6) . . . . ? C17 C16 C21 Pb1 6(6) . . . . ? O1 Pb1 C21 O6 12.7(11) . . . . ? O4 Pb1 C21 O6 127.0(4) 2_677 . . . ? N2 Pb1 C21 O6 -10.5(4) . . . . ? N3 Pb1 C21 O6 66.3(4) 2_677 . . . ? O4 Pb1 C21 O6 -150.7(4) 1_444 . . . ? O5 Pb1 C21 O6 179.0(7) . . . . ? O10 Pb1 C21 O6 -81.2(4) . . . . ? Pb1 Pb1 C21 O6 168.6(4) 2_566 . . . ? O1 Pb1 C21 O5 -166.3(6) . . . . ? O4 Pb1 C21 O5 -52.0(4) 2_677 . . . ? N2 Pb1 C21 O5 170.5(4) . . . . ? O6 Pb1 C21 O5 -179.0(7) . . . . ? N3 Pb1 C21 O5 -112.7(4) 2_677 . . . ? O4 Pb1 C21 O5 30.2(4) 1_444 . . . ? O10 Pb1 C21 O5 99.8(4) . . . . ? Pb1 Pb1 C21 O5 -10.4(4) 2_566 . . . ? O1 Pb1 C21 C16 10(7) . . . . ? O4 Pb1 C21 C16 124(6) 2_677 . . . ? N2 Pb1 C21 C16 -13(6) . . . . ? O6 Pb1 C21 C16 -3(6) . . . . ? N3 Pb1 C21 C16 63(6) 2_677 . . . ? O4 Pb1 C21 C16 -154(6) 1_444 . . . ? O5 Pb1 C21 C16 176(6) . . . . ? O10 Pb1 C21 C16 -84(6) . . . . ? Pb1 Pb1 C21 C16 166(6) 2_566 . . . ? C17 C18 C22 C23 -84.0(7) . . . . ? C19 C18 C22 C23 97.2(7) . . . . ? C18 C22 C23 C24 174.6(5) . . . . ? C22 C23 C24 C25 176.3(5) . . . . ? C23 C24 C25 C29 -84.8(7) . . . . ? C23 C24 C25 C26 95.5(7) . . . . ? C29 C25 C26 C27 2.9(8) . . . . ? C24 C25 C26 C27 -177.4(5) . . . . ? C28 N1 C27 C26 -0.9(8) . . . . ? Pb2 N1 C27 C26 162.3(4) 2_676 . . . ? C28 N1 C27 C30 178.8(5) . . . . ? Pb2 N1 C27 C30 -18.1(6) 2_676 . . . ? C25 C26 C27 N1 -1.8(8) . . . . ? C25 C26 C27 C30 178.5(5) . . . . ? C27 N1 C28 C29 2.4(8) . . . . ? Pb2 N1 C28 C29 -159.3(4) 2_676 . . . ? C26 C25 C29 C28 -1.4(8) . . . . ? C24 C25 C29 C28 178.9(5) . . . . ? N1 C28 C29 C25 -1.3(9) . . . . ? Pb2 O8 C30 O7 175.7(5) 2_676 . . . ? Pb2 O8 C30 O7 -13.5(8) 1_666 . . . ? Pb2 O8 C30 C27 -3.6(7) 2_676 . . . ? Pb2 O8 C30 C27 167.1(3) 1_666 . . . ? N1 C27 C30 O7 -164.6(5) . . . . ? C26 C27 C30 O7 15.1(8) . . . . ? N1 C27 C30 O8 14.8(7) . . . . ? C26 C27 C30 O8 -165.5(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H1W O3 0.83 2.38 3.024(9) 135.3 1_444 O9 H2W O7 0.83 2.03 2.738(7) 142.2 1_444 O10 H4W O3 0.83 2.17 2.692(8) 120.9 1_444 _diffrn_measured_fraction_theta_max 0.968 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.968 _refine_diff_density_max 1.121 _refine_diff_density_min -1.127 _refine_diff_density_rms 0.142 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 -0.004 0.000 -0.004 363 70 ' ' _platon_squeeze_details ; ; #===END