# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_coden_Cambridge 1350 loop_ _publ_author_name 'Ward, Mike' 'Najar, Adel' 'Tidmarsh, Ian' _publ_contact_author_name 'Ward, Mike' _publ_contact_author_email m.d.ward@sheffield.ac.uk _publ_section_title ; Lead(II) complexes of bis- and tris-bidentate compartmental ligands based on pyridyl-pyrazole and pyridyl-triazole fragments: coordination networks and a discrete dimeric box ; # Attachment '- lead_networks.cif' data_imw1335_0m _database_code_depnum_ccdc_archive 'CCDC 778858' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H18 N8' _chemical_formula_weight 394.44 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 Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 9.8170(5) _cell_length_b 9.9754(5) _cell_length_c 38.6879(17) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3788.6(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 4489 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 27.34 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.383 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.089 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9695 _exptl_absorpt_correction_T_max 0.9956 _exptl_absorpt_process_details SABABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25030 _diffrn_reflns_av_R_equivalents 0.0561 _diffrn_reflns_av_sigmaI/netI 0.0351 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -47 _diffrn_reflns_limit_l_max 50 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.65 _reflns_number_total 4397 _reflns_number_gt 3410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. 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^)+(0.0431P)^2^+1.0133P] 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 4397 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0558 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1008 _refine_ls_wR_factor_gt 0.0934 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _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 N111 N 0.32850(12) 0.08663(11) 1.15369(3) 0.0218(3) Uani 1 1 d . . . N121 N 0.26213(11) 0.39757(11) 1.08175(3) 0.0195(2) Uani 1 1 d . . . N141 N 0.21910(11) 0.51228(11) 0.90707(3) 0.0178(2) Uani 1 1 d . . . N142 N 0.33538(12) 0.58212(12) 0.91143(3) 0.0219(3) Uani 1 1 d . . . N143 N 0.35562(12) 0.65027(12) 0.88273(3) 0.0219(3) Uani 1 1 d . . . N131 N 0.13245(12) 0.66375(12) 0.80751(3) 0.0233(3) Uani 1 1 d . . . N122 N 0.12516(11) 0.38619(12) 1.08142(3) 0.0235(3) Uani 1 1 d . . . N123 N 0.09292(12) 0.29245(12) 1.10386(3) 0.0231(3) Uani 1 1 d . . . C115 C 0.21013(16) -0.05974(15) 1.19286(4) 0.0280(3) Uani 1 1 d . . . H115 H 0.2147 -0.1293 1.2096 0.034 Uiso 1 1 calc R . . C116 C 0.32743(15) -0.01150(14) 1.17727(4) 0.0251(3) Uani 1 1 d . . . H116 H 0.4120 -0.0504 1.1837 0.030 Uiso 1 1 calc R . . C112 C 0.20722(14) 0.13814(13) 1.14454(3) 0.0199(3) Uani 1 1 d . . . C124 C 0.20951(13) 0.24374(14) 1.11823(3) 0.0190(3) Uani 1 1 d . . . C125 C 0.31829(13) 0.31067(13) 1.10411(3) 0.0189(3) Uani 1 1 d . . . H125 H 0.4122 0.2983 1.1090 0.023 Uiso 1 1 calc R . . C126 C 0.32927(14) 0.48878(13) 1.05741(3) 0.0214(3) Uani 1 1 d . . . H12A H 0.4208 0.5121 1.0663 0.026 Uiso 1 1 calc R . . H12B H 0.2757 0.5726 1.0556 0.026 Uiso 1 1 calc R . . C151 C 0.34276(14) 0.42588(13) 1.02206(3) 0.0186(3) Uani 1 1 d . . . C152 C 0.25016(14) 0.45721(13) 0.99595(3) 0.0188(3) Uani 1 1 d . . . H152 H 0.1785 0.5187 1.0005 0.023 Uiso 1 1 calc R . . C153 C 0.26119(13) 0.39982(13) 0.96330(3) 0.0182(3) Uani 1 1 d . . . C146 C 0.15901(13) 0.43401(13) 0.93564(3) 0.0198(3) Uani 1 1 d . . . H14A H 0.1201 0.3500 0.9262 0.024 Uiso 1 1 calc R . . H14B H 0.0837 0.4861 0.9461 0.024 Uiso 1 1 calc R . . C145 C 0.16415(14) 0.53563(13) 0.87584(3) 0.0188(3) Uani 1 1 d . . . H145 H 0.0826 0.4990 0.8666 0.023 Uiso 1 1 calc R . . C144 C 0.25227(14) 0.62450(13) 0.86024(3) 0.0185(3) Uani 1 1 d . . . C132 C 0.24418(14) 0.69034(13) 0.82639(3) 0.0199(3) Uani 1 1 d . . . C133 C 0.34575(15) 0.77813(14) 0.81529(4) 0.0239(3) Uani 1 1 d . . . H133 H 0.4243 0.7936 0.8291 0.029 Uiso 1 1 calc R . . C134 C 0.32976(16) 0.84224(14) 0.78385(4) 0.0279(3) Uani 1 1 d . . . H134 H 0.3973 0.9027 0.7757 0.034 Uiso 1 1 calc R . . C135 C 0.21405(17) 0.81711(15) 0.76442(4) 0.0299(3) Uani 1 1 d . . . H135 H 0.1998 0.8607 0.7429 0.036 Uiso 1 1 calc R . . C114 C 0.08654(16) -0.00454(15) 1.18356(4) 0.0293(3) Uani 1 1 d . . . H114 H 0.0045 -0.0346 1.1940 0.035 Uiso 1 1 calc R . . C113 C 0.08431(15) 0.09529(14) 1.15876(4) 0.0255(3) Uani 1 1 d . . . H113 H 0.0005 0.1339 1.1516 0.031 Uiso 1 1 calc R . . C136 C 0.12003(16) 0.72701(15) 0.77720(4) 0.0276(3) Uani 1 1 d . . . H136 H 0.0416 0.7088 0.7636 0.033 Uiso 1 1 calc R . . C154 C 0.36644(13) 0.30939(13) 0.95689(3) 0.0196(3) Uani 1 1 d . . . H154 H 0.3745 0.2688 0.9348 0.024 Uiso 1 1 calc R . . C155 C 0.45936(14) 0.27850(13) 0.98260(3) 0.0206(3) Uani 1 1 d . . . H155 H 0.5313 0.2174 0.9780 0.025 Uiso 1 1 calc R . . C156 C 0.44790(14) 0.33638(13) 1.01516(3) 0.0208(3) Uani 1 1 d . . . H156 H 0.5119 0.3148 1.0327 0.025 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N111 0.0223(6) 0.0231(6) 0.0200(6) -0.0017(5) 0.0010(5) 0.0000(5) N121 0.0186(6) 0.0236(6) 0.0163(5) -0.0025(4) -0.0015(4) 0.0014(5) N141 0.0157(6) 0.0196(5) 0.0181(5) -0.0006(4) -0.0016(4) -0.0004(4) N142 0.0188(6) 0.0255(6) 0.0214(6) 0.0014(5) -0.0024(5) -0.0041(5) N143 0.0197(6) 0.0252(6) 0.0208(6) 0.0011(5) -0.0023(5) -0.0009(5) N131 0.0248(6) 0.0257(6) 0.0193(6) 0.0007(5) -0.0016(5) 0.0018(5) N122 0.0183(6) 0.0299(6) 0.0223(6) -0.0029(5) -0.0031(5) 0.0022(5) N123 0.0192(6) 0.0286(6) 0.0215(6) -0.0030(5) -0.0016(5) 0.0016(5) C115 0.0387(9) 0.0231(7) 0.0223(7) -0.0012(6) 0.0058(6) -0.0041(6) C116 0.0303(8) 0.0235(7) 0.0215(7) -0.0015(6) 0.0008(6) 0.0017(6) C112 0.0210(7) 0.0200(7) 0.0187(6) -0.0067(5) 0.0006(5) -0.0010(5) C124 0.0173(6) 0.0220(7) 0.0176(6) -0.0068(5) -0.0001(5) 0.0015(5) C125 0.0176(7) 0.0224(7) 0.0167(6) -0.0030(5) -0.0022(5) 0.0013(5) C126 0.0239(7) 0.0203(7) 0.0200(7) 0.0000(5) -0.0029(5) -0.0011(6) C151 0.0212(7) 0.0170(6) 0.0177(6) 0.0012(5) -0.0004(5) -0.0026(5) C152 0.0173(6) 0.0175(6) 0.0215(7) 0.0014(5) 0.0015(5) 0.0010(5) C153 0.0175(6) 0.0181(6) 0.0191(6) 0.0022(5) -0.0002(5) -0.0023(5) C146 0.0177(7) 0.0237(7) 0.0180(6) 0.0027(5) 0.0004(5) -0.0008(5) C145 0.0182(6) 0.0209(6) 0.0172(6) -0.0013(5) -0.0026(5) 0.0015(5) C144 0.0169(6) 0.0194(7) 0.0191(6) -0.0012(5) 0.0010(5) 0.0022(5) C132 0.0220(7) 0.0188(6) 0.0188(6) -0.0017(5) 0.0027(5) 0.0035(5) C133 0.0268(7) 0.0214(7) 0.0233(7) -0.0031(5) 0.0030(6) -0.0014(6) C134 0.0393(9) 0.0200(7) 0.0245(7) 0.0003(6) 0.0081(6) -0.0017(6) C135 0.0460(10) 0.0252(7) 0.0187(7) 0.0028(6) 0.0020(6) 0.0049(7) C114 0.0307(8) 0.0287(8) 0.0286(8) -0.0050(6) 0.0113(6) -0.0081(6) C113 0.0203(7) 0.0271(7) 0.0290(8) -0.0061(6) 0.0042(6) -0.0025(6) C136 0.0342(8) 0.0296(8) 0.0190(7) 0.0017(6) -0.0037(6) 0.0043(6) C154 0.0204(7) 0.0200(7) 0.0186(6) -0.0002(5) 0.0019(5) -0.0020(5) C155 0.0191(7) 0.0189(7) 0.0239(7) 0.0026(5) 0.0025(5) 0.0032(5) C156 0.0194(7) 0.0211(7) 0.0221(7) 0.0049(5) -0.0032(5) -0.0006(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag N111 C116 1.3382(18) . ? N111 C112 1.3442(18) . ? N121 C125 1.3430(17) . ? N121 N122 1.3495(16) . ? N121 C126 1.4658(17) . ? N141 C145 1.3434(17) . ? N141 N142 1.3479(15) . ? N141 C146 1.4761(16) . ? N142 N143 1.3168(16) . ? N143 C144 1.3612(17) . ? N131 C136 1.3372(17) . ? N131 C132 1.3441(18) . ? N122 N123 1.3147(16) . ? N123 C124 1.3620(17) . ? C115 C114 1.380(2) . ? C115 C116 1.386(2) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C112 C113 1.3933(19) . ? C112 C124 1.4650(19) . ? C124 C125 1.3728(19) . ? C125 H125 0.9500 . ? C126 C151 1.5104(18) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C151 C156 1.3906(19) . ? C151 C152 1.3946(18) . ? C152 C153 1.3913(18) . ? C152 H152 0.9500 . ? C153 C154 1.3938(19) . ? C153 C146 1.5059(18) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? C145 C144 1.3778(19) . ? C145 H145 0.9500 . ? C144 C132 1.4672(18) . ? C132 C133 1.3949(19) . ? C133 C134 1.383(2) . ? C133 H133 0.9500 . ? C134 C135 1.385(2) . ? C134 H134 0.9500 . ? C135 C136 1.380(2) . ? C135 H135 0.9500 . ? C114 C113 1.383(2) . ? C114 H114 0.9500 . ? C113 H113 0.9500 . ? C136 H136 0.9500 . ? C154 C155 1.3843(18) . ? C154 H154 0.9500 . ? C155 C156 1.3903(18) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? 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 C116 N111 C112 116.89(12) . . ? C125 N121 N122 111.15(11) . . ? C125 N121 C126 129.04(12) . . ? N122 N121 C126 119.61(11) . . ? C145 N141 N142 111.27(11) . . ? C145 N141 C146 127.20(11) . . ? N142 N141 C146 121.21(10) . . ? N143 N142 N141 106.82(10) . . ? N142 N143 C144 109.20(11) . . ? C136 N131 C132 117.25(13) . . ? N123 N122 N121 107.07(11) . . ? N122 N123 C124 108.72(11) . . ? C114 C115 C116 118.58(14) . . ? C114 C115 H115 120.7 . . ? C116 C115 H115 120.7 . . ? N111 C116 C115 123.86(14) . . ? N111 C116 H116 118.1 . . ? C115 C116 H116 118.1 . . ? N111 C112 C113 123.07(13) . . ? N111 C112 C124 116.38(12) . . ? C113 C112 C124 120.55(13) . . ? N123 C124 C125 108.53(12) . . ? N123 C124 C112 121.81(12) . . ? C125 C124 C112 129.65(12) . . ? N121 C125 C124 104.53(12) . . ? N121 C125 H125 127.7 . . ? C124 C125 H125 127.7 . . ? N121 C126 C151 111.29(11) . . ? N121 C126 H12A 109.4 . . ? C151 C126 H12A 109.4 . . ? N121 C126 H12B 109.4 . . ? C151 C126 H12B 109.4 . . ? H12A C126 H12B 108.0 . . ? C156 C151 C152 119.25(12) . . ? C156 C151 C126 120.38(12) . . ? C152 C151 C126 120.37(12) . . ? C153 C152 C151 120.99(12) . . ? C153 C152 H152 119.5 . . ? C151 C152 H152 119.5 . . ? C152 C153 C154 119.04(12) . . ? C152 C153 C146 120.02(12) . . ? C154 C153 C146 120.93(12) . . ? N141 C146 C153 112.69(11) . . ? N141 C146 H14A 109.1 . . ? C153 C146 H14A 109.1 . . ? N141 C146 H14B 109.1 . . ? C153 C146 H14B 109.1 . . ? H14A C146 H14B 107.8 . . ? N141 C145 C144 104.69(12) . . ? N141 C145 H145 127.7 . . ? C144 C145 H145 127.7 . . ? N143 C144 C145 108.02(11) . . ? N143 C144 C132 121.76(12) . . ? C145 C144 C132 130.17(12) . . ? N131 C132 C133 122.68(12) . . ? N131 C132 C144 116.16(12) . . ? C133 C132 C144 121.14(13) . . ? C134 C133 C132 118.68(14) . . ? C134 C133 H133 120.7 . . ? C132 C133 H133 120.7 . . ? C133 C134 C135 119.12(14) . . ? C133 C134 H134 120.4 . . ? C135 C134 H134 120.4 . . ? C136 C135 C134 118.16(13) . . ? C136 C135 H135 120.9 . . ? C134 C135 H135 120.9 . . ? C115 C114 C113 118.82(14) . . ? C115 C114 H114 120.6 . . ? C113 C114 H114 120.6 . . ? C114 C113 C112 118.76(14) . . ? C114 C113 H113 120.6 . . ? C112 C113 H113 120.6 . . ? N131 C136 C135 124.10(14) . . ? N131 C136 H136 118.0 . . ? C135 C136 H136 118.0 . . ? C155 C154 C153 120.32(12) . . ? C155 C154 H154 119.8 . . ? C153 C154 H154 119.8 . . ? C154 C155 C156 120.35(12) . . ? C154 C155 H155 119.8 . . ? C156 C155 H155 119.8 . . ? C155 C156 C151 120.04(12) . . ? C155 C156 H156 120.0 . . ? C151 C156 H156 120.0 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.231 _refine_diff_density_min -0.277 _refine_diff_density_rms 0.054 #===END data_imw1379p-1 _database_code_depnum_ccdc_archive 'CCDC 778859' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H24 N12' _chemical_formula_weight 552.61 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.110(5) _cell_length_b 10.485(5) _cell_length_c 14.400(8) _cell_angle_alpha 74.055(7) _cell_angle_beta 81.433(7) _cell_angle_gamma 86.057(5) _cell_volume 1307.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1743 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 23.92 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.404 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 576 _exptl_absorpt_coefficient_mu 0.091 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9838 _exptl_absorpt_correction_T_max 0.9874 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9933 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0772 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 26.39 _reflns_number_total 4993 _reflns_number_gt 2929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The data was solved by direct methods. 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^)+(0.0541P)^2^+0.3717P] 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 4993 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1127 _refine_ls_R_factor_gt 0.0529 _refine_ls_wR_factor_ref 0.1364 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _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 N111 N 0.0455(3) 0.1910(2) 0.04889(18) 0.0415(6) Uani 1 1 d . . . C112 C 0.0815(3) 0.0906(3) 0.1227(2) 0.0326(7) Uani 1 1 d . . . C113 C 0.1720(3) -0.0159(3) 0.1094(2) 0.0402(8) Uani 1 1 d . . . H113 H 0.1941 -0.0858 0.1637 0.048 Uiso 1 1 calc R . . C114 C 0.2295(4) -0.0190(3) 0.0161(2) 0.0499(9) Uani 1 1 d . . . H114 H 0.2928 -0.0907 0.0050 0.060 Uiso 1 1 calc R . . C115 C 0.1944(4) 0.0825(3) -0.0602(2) 0.0513(9) Uani 1 1 d . . . H115 H 0.2322 0.0827 -0.1254 0.062 Uiso 1 1 calc R . . C116 C 0.1028(4) 0.1852(3) -0.0407(2) 0.0489(9) Uani 1 1 d . . . H116 H 0.0792 0.2558 -0.0943 0.059 Uiso 1 1 calc R . . N121 N -0.0607(2) 0.1664(2) 0.34809(16) 0.0306(6) Uani 1 1 d . . . N122 N -0.0284(3) 0.0361(2) 0.37854(17) 0.0374(6) Uani 1 1 d . . . N123 N 0.0222(3) -0.0043(2) 0.30057(17) 0.0363(6) Uani 1 1 d . . . C124 C 0.0224(3) 0.1009(3) 0.2205(2) 0.0292(6) Uani 1 1 d . . . C125 C -0.0321(3) 0.2093(3) 0.2511(2) 0.0344(7) Uani 1 1 d . . . H125 H -0.0465 0.2969 0.2116 0.041 Uiso 1 1 calc R . . C126 C -0.1233(3) 0.2375(3) 0.4196(2) 0.0341(7) Uani 1 1 d . . . H12A H -0.0935 0.1904 0.4839 0.041 Uiso 1 1 calc R . . H12B H -0.2330 0.2382 0.4259 0.041 Uiso 1 1 calc R . . N131 N 0.7093(3) 0.4747(2) 0.08647(18) 0.0412(6) Uani 1 1 d . . . C132 C 0.6183(3) 0.5819(3) 0.0648(2) 0.0317(7) Uani 1 1 d . . . C133 C 0.6139(3) 0.6607(3) -0.0285(2) 0.0382(7) Uani 1 1 d . . . H133 H 0.5482 0.7360 -0.0403 0.046 Uiso 1 1 calc R . . C134 C 0.7052(3) 0.6297(3) -0.1047(2) 0.0445(8) Uani 1 1 d . . . H134 H 0.7041 0.6831 -0.1697 0.053 Uiso 1 1 calc R . . C135 C 0.7980(3) 0.5201(3) -0.0848(2) 0.0456(8) Uani 1 1 d . . . H135 H 0.8613 0.4949 -0.1359 0.055 Uiso 1 1 calc R . . C136 C 0.7976(3) 0.4473(3) 0.0101(2) 0.0480(8) Uani 1 1 d . . . H136 H 0.8640 0.3726 0.0230 0.058 Uiso 1 1 calc R . . N141 N 0.3712(2) 0.5978(2) 0.28070(16) 0.0293(5) Uani 1 1 d . . . N142 N 0.3521(3) 0.7192(2) 0.22115(18) 0.0388(6) Uani 1 1 d . . . N143 N 0.4412(3) 0.7258(2) 0.13887(18) 0.0382(6) Uani 1 1 d . . . C144 C 0.5172(3) 0.6083(3) 0.1471(2) 0.0300(6) Uani 1 1 d . . . C145 C 0.4733(3) 0.5265(3) 0.2379(2) 0.0293(6) Uani 1 1 d . . . H145 H 0.5079 0.4384 0.2646 0.035 Uiso 1 1 calc R . . C146 C 0.2811(3) 0.5620(3) 0.37614(19) 0.0307(7) Uani 1 1 d . . . H14A H 0.2811 0.6352 0.4073 0.037 Uiso 1 1 calc R . . H14B H 0.3261 0.4821 0.4179 0.037 Uiso 1 1 calc R . . N151 N -0.3604(3) 0.9629(3) 0.6152(2) 0.0549(8) Uani 1 1 d . . . C152 C -0.4514(3) 0.8624(3) 0.6124(2) 0.0313(7) Uani 1 1 d . . . C153 C -0.5618(3) 0.8142(3) 0.68112(19) 0.0263(6) Uani 1 1 d . . . H153 H -0.6212 0.7460 0.6762 0.032 Uiso 1 1 calc R . . C154 C -0.5868(3) 0.8647(4) 0.7572(3) 0.0557(10) Uani 1 1 d . . . H154 H -0.6655 0.8302 0.8073 0.067 Uiso 1 1 calc R . . C155 C -0.5042(3) 0.9649(3) 0.7678(2) 0.0473(8) Uani 1 1 d . . . H155 H -0.5253 0.9985 0.8234 0.057 Uiso 1 1 calc R . . C156 C -0.3908(3) 1.0139(3) 0.6950(2) 0.0411(8) Uani 1 1 d . . . H156 H -0.3329 1.0834 0.6995 0.049 Uiso 1 1 calc R . . N161 N -0.3285(2) 0.7501(2) 0.39880(16) 0.0300(5) Uani 1 1 d . . . N162 N -0.4527(2) 0.6802(2) 0.43554(18) 0.0346(6) Uani 1 1 d . . . N163 N -0.5090(2) 0.7137(2) 0.51532(18) 0.0342(6) Uani 1 1 d . . . C164 C -0.4208(3) 0.8055(3) 0.5289(2) 0.0284(6) Uani 1 1 d . . . C165 C -0.3059(3) 0.8289(3) 0.4542(2) 0.0288(6) Uani 1 1 d . . . H165 H -0.2271 0.8882 0.4438 0.035 Uiso 1 1 calc R . . C166 C -0.2348(3) 0.7279(3) 0.31316(19) 0.0316(7) Uani 1 1 d . . . H16A H -0.1800 0.8094 0.2783 0.038 Uiso 1 1 calc R . . H16B H -0.2982 0.7093 0.2685 0.038 Uiso 1 1 calc R . . C171 C -0.1253(3) 0.6135(3) 0.33972(18) 0.0259(6) Uani 1 1 d . . . C172 C -0.1707(3) 0.4832(3) 0.36414(19) 0.0279(6) Uani 1 1 d . . . H172 H -0.2712 0.4661 0.3623 0.033 Uiso 1 1 calc R . . C173 C -0.0719(3) 0.3785(2) 0.39103(18) 0.0268(6) Uani 1 1 d . . . C174 C 0.0754(3) 0.4053(3) 0.39300(18) 0.0280(6) Uani 1 1 d . . . H174 H 0.1446 0.3337 0.4107 0.034 Uiso 1 1 calc R . . C175 C 0.1225(3) 0.5343(3) 0.36966(18) 0.0264(6) Uani 1 1 d . . . C176 C 0.0212(3) 0.6378(3) 0.34307(18) 0.0272(6) Uani 1 1 d . . . H176 H 0.0525 0.7268 0.3269 0.033 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 N111 0.0453(15) 0.0389(15) 0.0404(16) -0.0117(12) -0.0092(12) 0.0099(12) C112 0.0306(15) 0.0336(17) 0.0352(17) -0.0113(14) -0.0067(13) 0.0017(13) C113 0.0474(18) 0.0360(18) 0.0368(18) -0.0113(14) -0.0064(15) 0.0103(15) C114 0.059(2) 0.049(2) 0.041(2) -0.0172(17) -0.0070(17) 0.0206(17) C115 0.057(2) 0.058(2) 0.0379(19) -0.0156(17) -0.0056(16) 0.0147(18) C116 0.057(2) 0.050(2) 0.038(2) -0.0096(16) -0.0113(16) 0.0133(17) N121 0.0268(12) 0.0239(13) 0.0402(15) -0.0107(11) 0.0024(11) -0.0021(10) N122 0.0392(14) 0.0278(14) 0.0435(16) -0.0112(12) 0.0036(12) -0.0016(11) N123 0.0400(14) 0.0286(14) 0.0395(15) -0.0118(12) 0.0032(12) -0.0026(11) C124 0.0263(15) 0.0241(15) 0.0382(17) -0.0104(13) -0.0035(13) -0.0008(12) C125 0.0370(17) 0.0267(16) 0.0363(18) -0.0066(13) 0.0009(14) 0.0000(13) C126 0.0309(16) 0.0306(16) 0.0400(18) -0.0142(14) 0.0075(13) -0.0029(13) N131 0.0331(14) 0.0433(16) 0.0468(16) -0.0153(13) -0.0032(12) 0.0095(12) C132 0.0240(15) 0.0340(16) 0.0382(17) -0.0112(14) -0.0045(13) -0.0015(13) C133 0.0339(17) 0.0390(18) 0.0422(19) -0.0111(15) -0.0064(14) -0.0002(14) C134 0.0428(18) 0.051(2) 0.0411(19) -0.0146(16) -0.0050(15) -0.0042(16) C135 0.0368(18) 0.054(2) 0.047(2) -0.0212(17) 0.0060(15) -0.0012(16) C136 0.0390(18) 0.051(2) 0.054(2) -0.0204(18) -0.0005(16) 0.0128(16) N141 0.0221(12) 0.0273(13) 0.0391(14) -0.0100(11) -0.0041(10) -0.0009(10) N142 0.0385(14) 0.0288(14) 0.0447(16) -0.0064(12) -0.0001(12) 0.0025(11) N143 0.0363(14) 0.0324(14) 0.0419(15) -0.0081(12) 0.0028(12) 0.0014(11) C144 0.0225(14) 0.0287(16) 0.0395(18) -0.0099(13) -0.0051(13) 0.0002(12) C145 0.0220(14) 0.0274(15) 0.0412(18) -0.0132(13) -0.0065(12) 0.0014(12) C146 0.0252(14) 0.0366(17) 0.0322(16) -0.0127(13) -0.0033(12) -0.0004(12) N151 0.0577(18) 0.0456(17) 0.068(2) -0.0211(15) -0.0174(15) 0.0008(14) C152 0.0273(15) 0.0216(15) 0.0454(18) -0.0072(13) -0.0121(13) 0.0044(12) C153 0.0203(14) 0.0303(16) 0.0299(16) -0.0103(13) -0.0005(12) -0.0088(12) C154 0.0304(18) 0.065(2) 0.059(2) 0.0036(19) -0.0026(16) -0.0055(17) C155 0.0429(19) 0.060(2) 0.042(2) -0.0209(17) -0.0082(16) 0.0178(17) C156 0.0462(19) 0.0346(18) 0.052(2) -0.0252(16) -0.0136(16) 0.0029(15) N161 0.0210(12) 0.0272(13) 0.0411(15) -0.0069(11) -0.0072(11) 0.0020(10) N162 0.0204(12) 0.0314(14) 0.0536(17) -0.0148(12) -0.0033(11) -0.0017(10) N163 0.0226(12) 0.0326(14) 0.0492(16) -0.0145(12) -0.0043(11) 0.0004(11) C164 0.0175(13) 0.0246(15) 0.0427(18) -0.0074(13) -0.0062(13) 0.0009(11) C165 0.0221(14) 0.0236(15) 0.0419(17) -0.0078(13) -0.0092(13) -0.0013(11) C166 0.0265(15) 0.0355(16) 0.0332(16) -0.0095(13) -0.0049(13) -0.0002(12) C171 0.0232(14) 0.0292(15) 0.0259(15) -0.0093(12) -0.0022(11) -0.0007(12) C172 0.0187(13) 0.0355(16) 0.0317(16) -0.0135(13) -0.0007(12) -0.0036(12) C173 0.0278(15) 0.0257(15) 0.0277(15) -0.0105(12) 0.0006(12) -0.0024(12) C174 0.0260(15) 0.0286(15) 0.0291(16) -0.0100(12) -0.0009(12) 0.0033(12) C175 0.0224(14) 0.0304(16) 0.0285(15) -0.0118(12) -0.0021(12) -0.0012(12) C176 0.0286(15) 0.0250(15) 0.0293(16) -0.0095(12) -0.0026(12) -0.0031(12) _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 N111 C116 1.334(4) . ? N111 C112 1.337(3) . ? C112 C113 1.381(4) . ? C112 C124 1.461(4) . ? C113 C114 1.375(4) . ? C113 H113 0.9500 . ? C114 C115 1.363(4) . ? C114 H114 0.9500 . ? C115 C116 1.381(4) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.336(3) . ? N121 N122 1.341(3) . ? N121 C126 1.460(3) . ? N122 N123 1.317(3) . ? N123 C124 1.359(3) . ? C124 C125 1.366(4) . ? C125 H125 0.9500 . ? C126 C173 1.509(4) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C132 1.343(3) . ? N131 C136 1.348(4) . ? C132 C133 1.375(4) . ? C132 C144 1.467(4) . ? C133 C134 1.374(4) . ? C133 H133 0.9500 . ? C134 C135 1.369(4) . ? C134 H134 0.9500 . ? C135 C136 1.370(4) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.338(3) . ? N141 N142 1.342(3) . ? N141 C146 1.458(3) . ? N142 N143 1.320(3) . ? N143 C144 1.356(3) . ? C144 C145 1.370(4) . ? C145 H145 0.9500 . ? C146 C175 1.514(3) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? N151 C156 1.380(4) . ? N151 C152 1.398(4) . ? C152 C153 1.321(4) . ? C152 C164 1.466(4) . ? C153 C154 1.327(4) . ? C153 H153 0.9500 . ? C154 C155 1.388(5) . ? C154 H154 0.9500 . ? C155 C156 1.373(4) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? N161 C165 1.340(3) . ? N161 N162 1.349(3) . ? N161 C166 1.456(3) . ? N162 N163 1.315(3) . ? N163 C164 1.367(3) . ? C164 C165 1.367(4) . ? C165 H165 0.9500 . ? C166 C171 1.509(3) . ? C166 H16A 0.9900 . ? C166 H16B 0.9900 . ? C171 C176 1.386(3) . ? C171 C172 1.390(4) . ? C172 C173 1.379(3) . ? C172 H172 0.9500 . ? C173 C174 1.396(4) . ? C174 C175 1.383(4) . ? C174 H174 0.9500 . ? C175 C176 1.384(3) . ? C176 H176 0.9500 . ? 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 C116 N111 C112 116.7(3) . . ? N111 C112 C113 123.0(3) . . ? N111 C112 C124 116.0(2) . . ? C113 C112 C124 121.0(3) . . ? C114 C113 C112 118.9(3) . . ? C114 C113 H113 120.5 . . ? C112 C113 H113 120.5 . . ? C115 C114 C113 119.0(3) . . ? C115 C114 H114 120.5 . . ? C113 C114 H114 120.5 . . ? C114 C115 C116 118.6(3) . . ? C114 C115 H115 120.7 . . ? C116 C115 H115 120.7 . . ? N111 C116 C115 123.8(3) . . ? N111 C116 H116 118.1 . . ? C115 C116 H116 118.1 . . ? C125 N121 N122 110.7(2) . . ? C125 N121 C126 130.1(2) . . ? N122 N121 C126 119.2(2) . . ? N123 N122 N121 107.2(2) . . ? N122 N123 C124 108.8(2) . . ? N123 C124 C125 107.8(2) . . ? N123 C124 C112 122.3(2) . . ? C125 C124 C112 129.8(3) . . ? N121 C125 C124 105.5(2) . . ? N121 C125 H125 127.2 . . ? C124 C125 H125 127.2 . . ? N121 C126 C173 111.8(2) . . ? N121 C126 H12A 109.3 . . ? C173 C126 H12A 109.3 . . ? N121 C126 H12B 109.3 . . ? C173 C126 H12B 109.3 . . ? H12A C126 H12B 107.9 . . ? C132 N131 C136 115.7(3) . . ? N131 C132 C133 123.3(3) . . ? N131 C132 C144 115.8(2) . . ? C133 C132 C144 120.9(3) . . ? C134 C133 C132 119.5(3) . . ? C134 C133 H133 120.2 . . ? C132 C133 H133 120.2 . . ? C135 C134 C133 118.4(3) . . ? C135 C134 H134 120.8 . . ? C133 C134 H134 120.8 . . ? C134 C135 C136 118.7(3) . . ? C134 C135 H135 120.6 . . ? C136 C135 H135 120.6 . . ? N131 C136 C135 124.3(3) . . ? N131 C136 H136 117.8 . . ? C135 C136 H136 117.8 . . ? C145 N141 N142 110.8(2) . . ? C145 N141 C146 130.4(2) . . ? N142 N141 C146 118.8(2) . . ? N143 N142 N141 107.4(2) . . ? N142 N143 C144 108.4(2) . . ? N143 C144 C145 108.4(2) . . ? N143 C144 C132 121.3(2) . . ? C145 C144 C132 130.2(2) . . ? N141 C145 C144 105.1(2) . . ? N141 C145 H145 127.5 . . ? C144 C145 H145 127.5 . . ? N141 C146 C175 112.3(2) . . ? N141 C146 H14A 109.2 . . ? C175 C146 H14A 109.2 . . ? N141 C146 H14B 109.2 . . ? C175 C146 H14B 109.2 . . ? H14A C146 H14B 107.9 . . ? C156 N151 C152 116.8(3) . . ? C153 C152 N151 123.9(3) . . ? C153 C152 C164 118.1(2) . . ? N151 C152 C164 118.0(3) . . ? C152 C153 C154 117.6(3) . . ? C152 C153 H153 121.2 . . ? C154 C153 H153 121.2 . . ? C153 C154 C155 123.6(3) . . ? C153 C154 H154 118.2 . . ? C155 C154 H154 118.2 . . ? C156 C155 C154 117.7(3) . . ? C156 C155 H155 121.2 . . ? C154 C155 H155 121.2 . . ? C155 C156 N151 120.4(3) . . ? C155 C156 H156 119.8 . . ? N151 C156 H156 119.8 . . ? C165 N161 N162 111.1(2) . . ? C165 N161 C166 128.8(2) . . ? N162 N161 C166 120.0(2) . . ? N163 N162 N161 106.9(2) . . ? N162 N163 C164 108.9(2) . . ? N163 C164 C165 108.1(2) . . ? N163 C164 C152 122.8(2) . . ? C165 C164 C152 129.1(2) . . ? N161 C165 C164 105.0(2) . . ? N161 C165 H165 127.5 . . ? C164 C165 H165 127.5 . . ? N161 C166 C171 111.9(2) . . ? N161 C166 H16A 109.2 . . ? C171 C166 H16A 109.2 . . ? N161 C166 H16B 109.2 . . ? C171 C166 H16B 109.2 . . ? H16A C166 H16B 107.9 . . ? C176 C171 C172 119.3(2) . . ? C176 C171 C166 120.0(2) . . ? C172 C171 C166 120.6(2) . . ? C173 C172 C171 120.8(2) . . ? C173 C172 H172 119.6 . . ? C171 C172 H172 119.6 . . ? C172 C173 C174 118.9(2) . . ? C172 C173 C126 120.3(2) . . ? C174 C173 C126 120.8(2) . . ? C175 C174 C173 121.1(2) . . ? C175 C174 H174 119.4 . . ? C173 C174 H174 119.4 . . ? C174 C175 C176 118.9(2) . . ? C174 C175 C146 120.5(2) . . ? C176 C175 C146 120.5(2) . . ? C175 C176 C171 120.9(2) . . ? C175 C176 H176 119.5 . . ? C171 C176 H176 119.5 . . ? 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 C116 N111 C112 C113 -0.6(4) . . . . ? C116 N111 C112 C124 177.8(2) . . . . ? N111 C112 C113 C114 0.7(5) . . . . ? C124 C112 C113 C114 -177.6(3) . . . . ? C112 C113 C114 C115 -0.5(5) . . . . ? C113 C114 C115 C116 0.3(5) . . . . ? C112 N111 C116 C115 0.4(5) . . . . ? C114 C115 C116 N111 -0.3(5) . . . . ? C125 N121 N122 N123 0.5(3) . . . . ? C126 N121 N122 N123 178.4(2) . . . . ? N121 N122 N123 C124 0.2(3) . . . . ? N122 N123 C124 C125 -0.7(3) . . . . ? N122 N123 C124 C112 175.9(2) . . . . ? N111 C112 C124 N123 165.5(3) . . . . ? C113 C112 C124 N123 -16.0(4) . . . . ? N111 C112 C124 C125 -18.6(4) . . . . ? C113 C112 C124 C125 159.8(3) . . . . ? N122 N121 C125 C124 -0.9(3) . . . . ? C126 N121 C125 C124 -178.6(2) . . . . ? N123 C124 C125 N121 1.0(3) . . . . ? C112 C124 C125 N121 -175.4(3) . . . . ? C125 N121 C126 C173 -36.2(4) . . . . ? N122 N121 C126 C173 146.3(2) . . . . ? C136 N131 C132 C133 -0.4(4) . . . . ? C136 N131 C132 C144 177.2(2) . . . . ? N131 C132 C133 C134 0.5(4) . . . . ? C144 C132 C133 C134 -177.0(3) . . . . ? C132 C133 C134 C135 0.2(4) . . . . ? C133 C134 C135 C136 -1.1(4) . . . . ? C132 N131 C136 C135 -0.5(4) . . . . ? C134 C135 C136 N131 1.3(5) . . . . ? C145 N141 N142 N143 0.8(3) . . . . ? C146 N141 N142 N143 -177.7(2) . . . . ? N141 N142 N143 C144 -0.4(3) . . . . ? N142 N143 C144 C145 -0.1(3) . . . . ? N142 N143 C144 C132 175.9(2) . . . . ? N131 C132 C144 N143 167.0(2) . . . . ? C133 C132 C144 N143 -15.4(4) . . . . ? N131 C132 C144 C145 -18.0(4) . . . . ? C133 C132 C144 C145 159.7(3) . . . . ? N142 N141 C145 C144 -0.8(3) . . . . ? C146 N141 C145 C144 177.4(2) . . . . ? N143 C144 C145 N141 0.5(3) . . . . ? C132 C144 C145 N141 -175.0(3) . . . . ? C145 N141 C146 C175 -103.3(3) . . . . ? N142 N141 C146 C175 74.7(3) . . . . ? C156 N151 C152 C153 -0.5(4) . . . . ? C156 N151 C152 C164 -179.5(2) . . . . ? N151 C152 C153 C154 -0.2(4) . . . . ? C164 C152 C153 C154 178.8(2) . . . . ? C152 C153 C154 C155 0.4(5) . . . . ? C153 C154 C155 C156 0.0(5) . . . . ? C154 C155 C156 N151 -0.8(4) . . . . ? C152 N151 C156 C155 1.0(4) . . . . ? C165 N161 N162 N163 -0.5(3) . . . . ? C166 N161 N162 N163 175.8(2) . . . . ? N161 N162 N163 C164 0.3(3) . . . . ? N162 N163 C164 C165 0.0(3) . . . . ? N162 N163 C164 C152 -179.1(2) . . . . ? C153 C152 C164 N163 5.7(4) . . . . ? N151 C152 C164 N163 -175.2(2) . . . . ? C153 C152 C164 C165 -173.2(3) . . . . ? N151 C152 C164 C165 5.9(4) . . . . ? N162 N161 C165 C164 0.5(3) . . . . ? C166 N161 C165 C164 -175.4(2) . . . . ? N163 C164 C165 N161 -0.3(3) . . . . ? C152 C164 C165 N161 178.7(2) . . . . ? C165 N161 C166 C171 90.5(3) . . . . ? N162 N161 C166 C171 -85.1(3) . . . . ? N161 C166 C171 C176 -101.0(3) . . . . ? N161 C166 C171 C172 76.9(3) . . . . ? C176 C171 C172 C173 -0.3(4) . . . . ? C166 C171 C172 C173 -178.2(2) . . . . ? C171 C172 C173 C174 -0.3(4) . . . . ? C171 C172 C173 C126 178.6(2) . . . . ? N121 C126 C173 C172 111.6(3) . . . . ? N121 C126 C173 C174 -69.6(3) . . . . ? C172 C173 C174 C175 0.8(4) . . . . ? C126 C173 C174 C175 -178.1(2) . . . . ? C173 C174 C175 C176 -0.6(4) . . . . ? C173 C174 C175 C146 177.5(2) . . . . ? N141 C146 C175 C174 102.5(3) . . . . ? N141 C146 C175 C176 -79.4(3) . . . . ? C174 C175 C176 C171 0.0(4) . . . . ? C146 C175 C176 C171 -178.1(2) . . . . ? C172 C171 C176 C175 0.5(4) . . . . ? C166 C171 C176 C175 178.4(2) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 26.39 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 0.444 _refine_diff_density_min -0.466 _refine_diff_density_rms 0.049 #===END data_imw1362p-1 _database_code_depnum_ccdc_archive 'CCDC 778860' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C78 H81 Cl4 N27 O20 Pb2' _chemical_formula_weight 2272.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6145(5) _cell_length_b 14.4977(6) _cell_length_c 28.1911(11) _cell_angle_alpha 78.018(2) _cell_angle_beta 81.577(2) _cell_angle_gamma 79.422(2) _cell_volume 4926.0(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9850 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 27.31 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.532 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2260 _exptl_absorpt_coefficient_mu 3.599 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5187 _exptl_absorpt_correction_T_max 0.6143 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 90954 _diffrn_reflns_av_R_equivalents 0.0657 _diffrn_reflns_av_sigmaI/netI 0.0778 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.69 _reflns_number_total 22672 _reflns_number_gt 15638 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a network of formula [Pb2(L)3(DMF)2](ClO4)4.DMF.Acetone. The data was solved by Patterson methods. The solution contains an acetone molecule disordered over two sites (O31 > O35; 58:42). Geometeric and displacement restraints have been applied to improve the apearance of the model. The appearance of the pyridyl rings N231 > C236 and N311 > C316 have been improved by the application of geometric and displacement restraints. The data indicated the presence of four additional acetone molecules all of which resided on special positions. These could not however be satisfactorily modelled and therefore the associated electron density was removed using a Platon SQUEEZE function: loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.500 0.000 134 37 ' ' 2 0.000 1.000 0.500 162 50 ' ' 3 0.500 0.500 0.500 152 48 ' ' 4 0.500 0.000 1.000 152 49 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0626P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 22672 _refine_ls_number_parameters 1144 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.0770 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1210 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.026 _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 Pb2 Pb 0.853045(15) 0.943904(15) 0.855202(8) 0.02085(7) Uani 1 1 d . . . Pb1 Pb 0.145127(15) 0.603346(15) 0.637960(8) 0.02042(6) Uani 1 1 d . . . N111 N -0.0045(3) 0.7679(3) 0.63199(17) 0.0241(11) Uani 1 1 d . . . C112 C 0.0080(4) 0.8376(4) 0.6543(2) 0.0227(12) Uani 1 1 d . . . C113 C -0.0578(5) 0.9261(4) 0.6488(2) 0.0308(14) Uani 1 1 d . . . H113 H -0.0448 0.9749 0.6640 0.037 Uiso 1 1 calc R . . C114 C -0.1430(5) 0.9420(5) 0.6205(2) 0.0352(16) Uani 1 1 d . . . H114 H -0.1912 1.0010 0.6171 0.042 Uiso 1 1 calc R . . C115 C -0.1561(4) 0.8707(4) 0.5975(2) 0.0291(14) Uani 1 1 d . . . H115 H -0.2127 0.8803 0.5773 0.035 Uiso 1 1 calc R . . C116 C -0.0863(4) 0.7850(4) 0.6040(2) 0.0244(13) Uani 1 1 d . . . H116 H -0.0964 0.7361 0.5881 0.029 Uiso 1 1 calc R . . N121 N 0.2191(3) 0.8120(3) 0.73118(17) 0.0241(11) Uani 1 1 d . . . N122 N 0.2340(4) 0.7249(4) 0.71990(17) 0.0283(11) Uani 1 1 d . . . N123 N 0.1592(4) 0.7267(3) 0.69136(17) 0.0245(11) Uani 1 1 d . . . C124 C 0.0971(4) 0.8153(4) 0.6846(2) 0.0219(12) Uani 1 1 d . . . C125 C 0.1353(4) 0.8697(4) 0.7108(2) 0.0254(13) Uani 1 1 d . . . H125 H 0.1082 0.9340 0.7138 0.030 Uiso 1 1 calc R . . C126 C 0.2861(4) 0.8332(5) 0.7651(2) 0.0303(14) Uani 1 1 d . . . H12A H 0.2492 0.8211 0.7988 0.036 Uiso 1 1 calc R . . H12B H 0.2940 0.9016 0.7566 0.036 Uiso 1 1 calc R . . N131 N 0.9972(3) 0.7842(3) 0.84234(17) 0.0247(11) Uani 1 1 d . . . C132 C 0.9833(4) 0.7304(4) 0.8104(2) 0.0214(12) Uani 1 1 d . . . C133 C 1.0471(5) 0.6437(4) 0.8069(2) 0.0337(15) Uani 1 1 d . . . H133 H 1.0351 0.6073 0.7844 0.040 Uiso 1 1 calc R . . C134 C 1.1295(5) 0.6104(5) 0.8370(2) 0.0369(16) Uani 1 1 d . . . H134 H 1.1749 0.5509 0.8352 0.044 Uiso 1 1 calc R . . C135 C 1.1445(5) 0.6656(5) 0.8696(2) 0.0339(15) Uani 1 1 d . . . H135 H 1.2000 0.6446 0.8906 0.041 Uiso 1 1 calc R . . C136 C 1.0771(4) 0.7511(4) 0.8707(2) 0.0289(14) Uani 1 1 d . . . H136 H 1.0879 0.7889 0.8929 0.035 Uiso 1 1 calc R . . N141 N 0.7681(3) 0.7956(3) 0.73301(16) 0.0225(10) Uani 1 1 d . . . N142 N 0.7577(3) 0.8737(3) 0.75321(17) 0.0237(11) Uani 1 1 d . . . N143 N 0.8352(3) 0.8570(3) 0.78222(17) 0.0244(11) Uani 1 1 d . . . C144 C 0.8935(4) 0.7686(4) 0.7810(2) 0.0213(12) Uani 1 1 d . . . C145 C 0.8498(4) 0.7293(4) 0.7492(2) 0.0240(13) Uani 1 1 d . . . H145 H 0.8729 0.6682 0.7406 0.029 Uiso 1 1 calc R . . C146 C 0.6857(4) 0.7907(4) 0.7025(2) 0.0260(13) Uani 1 1 d . . . H14A H 0.7178 0.7494 0.6784 0.031 Uiso 1 1 calc R . . H14B H 0.6608 0.8554 0.6843 0.031 Uiso 1 1 calc R . . C151 C 0.3990(5) 0.7718(4) 0.7631(2) 0.0260(13) Uani 1 1 d . . . C152 C 0.4868(4) 0.8079(4) 0.7347(2) 0.0263(13) Uani 1 1 d . . . H152 H 0.4777 0.8710 0.7161 0.032 Uiso 1 1 calc R . . C153 C 0.5889(4) 0.7506(4) 0.7336(2) 0.0260(13) Uani 1 1 d . . . C154 C 0.6011(4) 0.6597(4) 0.7607(2) 0.0259(13) Uani 1 1 d . . . H154 H 0.6706 0.6209 0.7600 0.031 Uiso 1 1 calc R . . C155 C 0.5130(5) 0.6240(4) 0.7892(2) 0.0294(14) Uani 1 1 d . . . H155 H 0.5221 0.5610 0.8077 0.035 Uiso 1 1 calc R . . C156 C 0.4120(5) 0.6803(4) 0.7904(2) 0.0281(14) Uani 1 1 d . . . H156 H 0.3515 0.6561 0.8099 0.034 Uiso 1 1 calc R . . N211 N 0.3611(3) 0.5389(3) 0.63785(17) 0.0213(10) Uani 1 1 d . . . C212 C 0.4027(4) 0.4523(4) 0.62832(19) 0.0196(12) Uani 1 1 d . . . C213 C 0.5070(4) 0.4071(4) 0.6381(2) 0.0271(14) Uani 1 1 d . . . H213 H 0.5346 0.3455 0.6309 0.033 Uiso 1 1 calc R . . C214 C 0.5693(5) 0.4545(4) 0.6586(2) 0.0295(14) Uani 1 1 d . . . H214 H 0.6409 0.4261 0.6653 0.035 Uiso 1 1 calc R . . C215 C 0.5264(4) 0.5432(4) 0.6691(2) 0.0265(13) Uani 1 1 d . . . H215 H 0.5675 0.5767 0.6834 0.032 Uiso 1 1 calc R . . C216 C 0.4224(4) 0.5827(4) 0.6584(2) 0.0261(13) Uani 1 1 d . . . H216 H 0.3928 0.6438 0.6659 0.031 Uiso 1 1 calc R . . N221 N 0.2603(3) 0.3082(3) 0.57748(17) 0.0218(10) Uani 1 1 d . . . N222 N 0.1869(4) 0.3875(4) 0.57914(18) 0.0294(12) Uani 1 1 d . . . N223 N 0.2310(4) 0.4465(3) 0.59723(18) 0.0278(12) Uani 1 1 d . . . C224 C 0.3335(4) 0.4052(4) 0.60695(19) 0.0185(12) Uani 1 1 d . . . C225 C 0.3526(4) 0.3149(4) 0.5945(2) 0.0260(13) Uani 1 1 d . . . H225 H 0.4163 0.2685 0.5974 0.031 Uiso 1 1 calc R . . C226 C 0.2374(5) 0.2306(4) 0.5567(2) 0.0264(13) Uani 1 1 d . . . H22A H 0.1583 0.2370 0.5556 0.032 Uiso 1 1 calc R . . H22B H 0.2615 0.1685 0.5775 0.032 Uiso 1 1 calc R . . N231 N 0.1165(3) 0.6498(2) 0.54155(10) 0.0234(11) Uani 1 1 d G . . C232 C 0.1759(3) 0.7151(3) 0.51099(13) 0.0319(15) Uani 1 1 d G . . C233 C 0.1682(4) 0.7351(4) 0.46110(13) 0.075(3) Uani 1 1 d GU . . H233 H 0.2088 0.7797 0.4402 0.091 Uiso 1 1 calc R . . C234 C 0.1012(4) 0.6898(4) 0.44176(10) 0.080(3) Uani 1 1 d GU . . H234 H 0.0959 0.7034 0.4077 0.096 Uiso 1 1 calc R . . C235 C 0.0418(3) 0.6245(3) 0.47232(14) 0.0418(18) Uani 1 1 d GU . . H235 H -0.0040 0.5935 0.4591 0.050 Uiso 1 1 calc R . . C236 C 0.0495(3) 0.6045(3) 0.52222(13) 0.0303(14) Uani 1 1 d G . . H236 H 0.0089 0.5599 0.5431 0.036 Uiso 1 1 calc R . . N241 N 0.3529(3) 0.8351(3) 0.55385(18) 0.0234(11) Uani 1 1 d . . . N242 N 0.3106(4) 0.7852(3) 0.59598(18) 0.0274(11) Uani 1 1 d . . . N243 N 0.2429(3) 0.7383(3) 0.58357(17) 0.0219(10) Uani 1 1 d . . . C244 C 0.2419(4) 0.7573(4) 0.5351(2) 0.0246(13) Uani 1 1 d . . . C245 C 0.3137(4) 0.8194(4) 0.5153(2) 0.0277(14) Uani 1 1 d . . . H245 H 0.3315 0.8452 0.4819 0.033 Uiso 1 1 calc R . . C246 C 0.4414(4) 0.8884(4) 0.5547(2) 0.0296(14) Uani 1 1 d . . . H24A H 0.4336 0.9100 0.5863 0.036 Uiso 1 1 calc R . . H24B H 0.4373 0.9456 0.5283 0.036 Uiso 1 1 calc R . . C251 C 0.2958(4) 0.2332(4) 0.5056(2) 0.0221(12) Uani 1 1 d . . . C252 C 0.3919(4) 0.1704(4) 0.4981(2) 0.0228(12) Uani 1 1 d . . . H252 H 0.4177 0.1241 0.5247 0.027 Uiso 1 1 calc R . . C253 C 0.5500(4) 0.8255(4) 0.5476(2) 0.0250(13) Uani 1 1 d . . . C254 C 0.5911(4) 0.7613(4) 0.5862(2) 0.0292(14) Uani 1 1 d . . . H254 H 0.5540 0.7607 0.6181 0.035 Uiso 1 1 calc R . . C255 C 0.6850(5) 0.6977(5) 0.5795(2) 0.0314(15) Uani 1 1 d . . . H255 H 0.7104 0.6518 0.6064 0.038 Uiso 1 1 calc R . . C256 C 0.2573(4) 0.2994(4) 0.4665(2) 0.0273(14) Uani 1 1 d . . . H256 H 0.1919 0.3425 0.4712 0.033 Uiso 1 1 calc R . . N311 N 0.6358(4) 1.0024(3) 0.85731(18) 0.0251(11) Uani 1 1 d . . . C312 C 0.5913(4) 1.0839(4) 0.8737(2) 0.0255(13) Uani 1 1 d . . . C313 C 0.4864(5) 1.1260(4) 0.8676(2) 0.0331(15) Uani 1 1 d . . . H313 H 0.4565 1.1823 0.8802 0.040 Uiso 1 1 calc R . . C314 C 0.4232(5) 1.0855(4) 0.8427(2) 0.0360(16) Uani 1 1 d . . . H314 H 0.3504 1.1138 0.8380 0.043 Uiso 1 1 calc R . . C315 C 0.4696(4) 1.0044(4) 0.8253(2) 0.0316(15) Uani 1 1 d . . . H315 H 0.4300 0.9758 0.8077 0.038 Uiso 1 1 calc R . . C316 C 0.5747(4) 0.9645(4) 0.8337(2) 0.0312(15) Uani 1 1 d . . . H316 H 0.6054 0.9072 0.8221 0.037 Uiso 1 1 calc R . . N321 N 0.7318(4) 1.2095(3) 0.93461(17) 0.0266(11) Uani 1 1 d . . . N322 N 0.8068(4) 1.1320(4) 0.92992(19) 0.0323(12) Uani 1 1 d . . . N323 N 0.7619(4) 1.0801(4) 0.90774(18) 0.0309(12) Uani 1 1 d . . . C324 C 0.6598(4) 1.1235(4) 0.8990(2) 0.0230(12) Uani 1 1 d . . . C325 C 0.6401(4) 1.2073(4) 0.9164(2) 0.0280(14) Uani 1 1 d . . . H325 H 0.5759 1.2534 0.9158 0.034 Uiso 1 1 calc R . . C326 C 0.7535(5) 1.2801(4) 0.9615(2) 0.0300(14) Uani 1 1 d . . . H32A H 0.7264 1.3454 0.9447 0.036 Uiso 1 1 calc R . . H32B H 0.8326 1.2745 0.9622 0.036 Uiso 1 1 calc R . . N331 N 0.8857(3) 0.8654(3) 0.94815(10) 0.0255(11) Uani 1 1 d G . . C332 C 0.8292(3) 0.7925(3) 0.97279(13) 0.0352(16) Uani 1 1 d G . . C333 C 0.8378(4) 0.7569(3) 1.02204(14) 0.070(3) Uani 1 1 d GU . . H333 H 0.7992 0.7072 1.0389 0.084 Uiso 1 1 calc R . . C334 C 0.9029(4) 0.7942(4) 1.04666(11) 0.075(3) Uani 1 1 d GU . . H334 H 0.9088 0.7698 1.0803 0.091 Uiso 1 1 calc R . . C335 C 0.9594(3) 0.8670(3) 1.02202(13) 0.0407(17) Uani 1 1 d GU . . H335 H 1.0039 0.8924 1.0388 0.049 Uiso 1 1 calc R . . C336 C 0.9508(3) 0.9026(3) 0.97276(13) 0.0317(15) Uani 1 1 d G . . H336 H 0.9895 0.9524 0.9559 0.038 Uiso 1 1 calc R . . N341 N 0.6502(4) 0.6939(4) 0.91826(18) 0.0276(11) Uani 1 1 d . . . N342 N 0.6907(4) 0.7537(4) 0.87994(18) 0.0291(12) Uani 1 1 d . . . N343 N 0.7600(3) 0.7942(3) 0.89578(17) 0.0259(11) Uani 1 1 d . . . C344 C 0.7633(4) 0.7613(4) 0.9442(2) 0.0271(13) Uani 1 1 d . . . C345 C 0.6915(5) 0.6964(5) 0.9589(2) 0.0345(15) Uani 1 1 d . . . H345 H 0.6751 0.6615 0.9908 0.041 Uiso 1 1 calc R . . C346 C 0.5623(4) 0.6438(4) 0.9139(2) 0.0273(14) Uani 1 1 d . . . H34A H 0.5698 0.5806 0.9358 0.033 Uiso 1 1 calc R . . H34B H 0.5670 0.6334 0.8800 0.033 Uiso 1 1 calc R . . C351 C 0.3024(4) 0.7372(4) 0.9868(2) 0.0237(13) Uani 1 1 d . . . C352 C 0.3984(4) 0.6820(4) 0.9727(2) 0.0229(12) Uani 1 1 d . . . H352 H 0.4269 0.6285 0.9955 0.027 Uiso 1 1 calc R . . C353 C 0.4548(5) 0.7009(4) 0.9271(2) 0.0258(13) Uani 1 1 d . . . C354 C 0.4092(5) 0.7765(4) 0.8937(2) 0.0266(13) Uani 1 1 d . . . H354 H 0.4462 0.7907 0.8618 0.032 Uiso 1 1 calc R . . C355 C 0.3115(5) 0.8319(5) 0.9056(2) 0.0313(15) Uani 1 1 d . . . H355 H 0.2810 0.8828 0.8819 0.038 Uiso 1 1 calc R . . C356 C 0.2583(5) 0.8126(4) 0.9522(2) 0.0318(15) Uani 1 1 d . . . H356 H 0.1914 0.8508 0.9607 0.038 Uiso 1 1 calc R . . Cl11 Cl 0.41692(12) 0.43563(10) 0.91169(6) 0.0312(3) Uani 1 1 d . . . O12 O 0.3931(3) 0.3406(3) 0.91985(16) 0.0336(10) Uani 1 1 d . . . O13 O 0.3968(5) 0.4697(3) 0.95682(17) 0.0581(15) Uani 1 1 d . . . O14 O 0.5300(3) 0.4343(3) 0.89461(19) 0.0500(13) Uani 1 1 d . . . O15 O 0.3547(4) 0.4966(3) 0.87580(18) 0.0527(14) Uani 1 1 d . . . Cl21 Cl 0.10164(10) 0.04620(10) 0.82290(5) 0.0265(3) Uani 1 1 d . . . O22 O 0.0752(4) 0.1463(3) 0.8188(2) 0.0545(14) Uani 1 1 d . . . O23 O 0.2170(3) 0.0193(3) 0.81525(16) 0.0405(11) Uani 1 1 d . . . O24 O 0.0605(3) -0.0016(3) 0.86985(15) 0.0416(12) Uani 1 1 d . . . O25 O 0.0539(3) 0.0157(4) 0.78649(16) 0.0473(13) Uani 1 1 d . . . Cl31 Cl 0.88292(10) 0.50760(10) 0.67403(5) 0.0271(3) Uani 1 1 d . . . O32 O 0.8629(4) 0.4129(3) 0.67736(19) 0.0525(14) Uani 1 1 d . . . O33 O 0.9555(3) 0.5119(3) 0.70821(17) 0.0478(13) Uani 1 1 d . . . O34 O 0.9323(3) 0.5419(3) 0.62542(16) 0.0423(12) Uani 1 1 d . . . O35 O 0.7828(3) 0.5691(3) 0.68384(16) 0.0391(11) Uani 1 1 d . . . Cl41 Cl 0.54807(11) 0.06830(10) 0.61623(6) 0.0283(3) Uani 1 1 d . . . O42 O 0.4311(3) 0.0761(3) 0.62041(16) 0.0367(11) Uani 1 1 d . . . O43 O 0.5864(4) 0.0209(3) 0.66141(17) 0.0522(13) Uani 1 1 d . . . O44 O 0.5742(3) 0.1629(3) 0.60402(16) 0.0337(10) Uani 1 1 d . . . O45 O 0.5970(3) 0.0169(3) 0.57766(17) 0.0413(12) Uani 1 1 d . . . O11S O 0.8035(4) 1.1068(3) 0.79466(17) 0.0471(13) Uani 1 1 d . . . N12S N 0.7569(4) 1.1634(4) 0.7187(2) 0.0400(14) Uani 1 1 d . . . C13S C 0.8272(6) 1.1263(5) 0.7502(3) 0.0468(18) Uani 1 1 d . . . H13S H 0.9016 1.1136 0.7378 0.056 Uiso 1 1 calc R . . C14S C 0.7911(6) 1.1883(5) 0.6673(2) 0.0487(19) Uani 1 1 d . . . H14C H 0.8687 1.1645 0.6608 0.073 Uiso 1 1 calc R . . H14D H 0.7780 1.2579 0.6570 0.073 Uiso 1 1 calc R . . H14E H 0.7499 1.1593 0.6490 0.073 Uiso 1 1 calc R . . C15S C 0.6407(5) 1.1800(7) 0.7339(3) 0.068(3) Uani 1 1 d . . . H15A H 0.6027 1.1538 0.7131 0.102 Uiso 1 1 calc R . . H15B H 0.6151 1.2488 0.7308 0.102 Uiso 1 1 calc R . . H15C H 0.6260 1.1486 0.7679 0.102 Uiso 1 1 calc R . . O21S O 0.2042(4) 0.4797(4) 0.71849(17) 0.0495(13) Uani 1 1 d . . . N22S N 0.2446(4) 0.3865(4) 0.79010(18) 0.0327(12) Uani 1 1 d . . . C23S C 0.1778(5) 0.4338(4) 0.7584(2) 0.0299(14) Uani 1 1 d . . . H23S H 0.1026 0.4319 0.7674 0.036 Uiso 1 1 calc R . . C24S C 0.2070(6) 0.3314(5) 0.8367(2) 0.0494(19) Uani 1 1 d . . . H24C H 0.1277 0.3465 0.8426 0.074 Uiso 1 1 calc R . . H24D H 0.2396 0.3474 0.8628 0.074 Uiso 1 1 calc R . . H24E H 0.2281 0.2631 0.8361 0.074 Uiso 1 1 calc R . . C25S C 0.3612(5) 0.3822(6) 0.7781(3) 0.052(2) Uani 1 1 d . . . H25A H 0.3763 0.4271 0.7477 0.078 Uiso 1 1 calc R . . H25B H 0.3942 0.3173 0.7740 0.078 Uiso 1 1 calc R . . H25C H 0.3916 0.3994 0.8045 0.078 Uiso 1 1 calc R . . O31X O 0.7379(8) 0.3541(7) 0.8015(4) 0.103(3) Uiso 0.584(5) 1 d PDU A 1 C32X C 0.8000(6) 0.3794(5) 0.8243(3) 0.0599(18) Uiso 0.584(5) 1 d PDU A 1 C33X C 0.7859(10) 0.4820(6) 0.8324(5) 0.0601(19) Uiso 0.584(5) 1 d PDU A 1 H33A H 0.7230 0.5197 0.8170 0.090 Uiso 0.584(5) 1 calc PR A 1 H33B H 0.8512 0.5096 0.8179 0.090 Uiso 0.584(5) 1 calc PR A 1 H33C H 0.7744 0.4825 0.8675 0.090 Uiso 0.584(5) 1 calc PR A 1 C34X C 0.8942(8) 0.3103(7) 0.8460(4) 0.0603(18) Uiso 0.584(5) 1 d PDU A 1 H34C H 0.8955 0.2471 0.8384 0.090 Uiso 0.584(5) 1 calc PR A 1 H34D H 0.8853 0.3059 0.8815 0.090 Uiso 0.584(5) 1 calc PR A 1 H34E H 0.9625 0.3333 0.8321 0.090 Uiso 0.584(5) 1 calc PR A 1 O31Y O 0.7994(11) 0.4124(8) 0.8318(5) 0.103(3) Uiso 0.416(5) 1 d PDU A 2 C32Y C 0.8655(7) 0.4211(4) 0.8580(3) 0.0607(18) Uiso 0.416(5) 1 d PDU A 2 C33Y C 0.9600(11) 0.3420(6) 0.8708(6) 0.0588(19) Uiso 0.416(5) 1 d PDU A 2 H33D H 0.9594 0.2896 0.8538 0.088 Uiso 0.416(5) 1 calc PR A 2 H33E H 0.9528 0.3184 0.9062 0.088 Uiso 0.416(5) 1 calc PR A 2 H33F H 1.0284 0.3672 0.8608 0.088 Uiso 0.416(5) 1 calc PR A 2 C34Y C 0.8567(3) 0.5111(2) 0.87905(11) 0.063(2) Uiso 0.416(5) 1 d PDU A 2 H34F H 0.7938 0.5569 0.8680 0.094 Uiso 0.416(5) 1 calc PR A 2 H34G H 0.9228 0.5396 0.8680 0.094 Uiso 0.416(5) 1 calc PR A 2 H34H H 0.8479 0.4948 0.9148 0.094 Uiso 0.416(5) 1 calc PR A 2 O41S O 0.0778(3) 0.1078(2) 0.66361(11) 0.0539(14) Uani 1 1 d R . . N42S N 0.1768(3) 0.1952(2) 0.69426(11) 0.0393(14) Uani 1 1 d R . . C43S C 0.1641(3) 0.1169(2) 0.67833(11) 0.053(2) Uani 1 1 d R . . H43S H 0.2233 0.0660 0.6782 0.063 Uiso 1 1 calc R . . C44S C 0.2721(6) 0.1981(5) 0.7167(3) 0.052(2) Uani 1 1 d . . . H44A H 0.2515 0.2001 0.7514 0.078 Uiso 1 1 calc R . . H44B H 0.3037 0.2551 0.7006 0.078 Uiso 1 1 calc R . . H44C H 0.3256 0.1409 0.7132 0.078 Uiso 1 1 calc R . . C45S C 0.0880(6) 0.2742(5) 0.6979(3) 0.056(2) Uani 1 1 d . . . H45A H 0.0314 0.2694 0.6785 0.084 Uiso 1 1 calc R . . H45B H 0.1152 0.3349 0.6855 0.084 Uiso 1 1 calc R . . H45C H 0.0575 0.2716 0.7321 0.084 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb2 0.01059(10) 0.02513(13) 0.02853(13) -0.00751(10) -0.00282(9) -0.00388(8) Pb1 0.01070(10) 0.02374(13) 0.03000(13) -0.01106(10) -0.00452(9) -0.00224(8) N111 0.014(2) 0.028(3) 0.032(3) -0.010(2) -0.004(2) -0.002(2) C112 0.013(3) 0.021(3) 0.034(3) -0.007(3) 0.006(2) -0.008(2) C113 0.026(3) 0.025(3) 0.047(4) -0.014(3) -0.009(3) -0.003(3) C114 0.019(3) 0.030(4) 0.057(4) -0.008(3) -0.007(3) -0.003(3) C115 0.015(3) 0.034(4) 0.039(4) -0.007(3) -0.007(3) -0.003(3) C116 0.011(3) 0.024(3) 0.037(4) -0.005(3) -0.005(2) 0.002(2) N121 0.018(2) 0.026(3) 0.033(3) -0.012(2) -0.003(2) -0.006(2) N122 0.026(3) 0.032(3) 0.032(3) -0.015(2) -0.007(2) -0.004(2) N123 0.018(2) 0.029(3) 0.029(3) -0.012(2) -0.007(2) 0.000(2) C124 0.022(3) 0.016(3) 0.030(3) -0.008(2) 0.000(2) -0.006(2) C125 0.016(3) 0.023(3) 0.038(4) -0.012(3) 0.000(3) -0.001(2) C126 0.020(3) 0.039(4) 0.037(4) -0.018(3) -0.007(3) -0.003(3) N131 0.016(2) 0.031(3) 0.030(3) -0.010(2) -0.004(2) -0.006(2) C132 0.013(3) 0.023(3) 0.027(3) -0.005(3) -0.001(2) -0.001(2) C133 0.030(3) 0.032(4) 0.042(4) -0.018(3) -0.010(3) 0.006(3) C134 0.027(3) 0.035(4) 0.047(4) -0.011(3) -0.013(3) 0.011(3) C135 0.019(3) 0.041(4) 0.042(4) -0.011(3) -0.011(3) 0.004(3) C136 0.013(3) 0.045(4) 0.032(3) -0.016(3) -0.004(2) -0.003(3) N141 0.020(2) 0.023(3) 0.026(3) -0.004(2) -0.006(2) -0.006(2) N142 0.016(2) 0.025(3) 0.031(3) -0.006(2) -0.005(2) -0.005(2) N143 0.017(2) 0.028(3) 0.030(3) -0.008(2) -0.003(2) -0.002(2) C144 0.013(3) 0.018(3) 0.031(3) -0.002(2) -0.002(2) 0.002(2) C145 0.016(3) 0.024(3) 0.032(3) -0.008(3) 0.002(2) -0.004(2) C146 0.020(3) 0.036(4) 0.027(3) -0.007(3) -0.009(2) -0.011(3) C151 0.025(3) 0.035(4) 0.025(3) -0.014(3) -0.007(3) -0.009(3) C152 0.025(3) 0.029(3) 0.030(3) -0.007(3) -0.011(3) -0.008(3) C153 0.020(3) 0.034(4) 0.026(3) -0.008(3) -0.006(2) -0.006(3) C154 0.021(3) 0.035(4) 0.026(3) -0.011(3) -0.010(2) -0.005(3) C155 0.028(3) 0.034(4) 0.029(3) -0.002(3) -0.007(3) -0.011(3) C156 0.022(3) 0.039(4) 0.027(3) -0.011(3) 0.000(3) -0.012(3) N211 0.012(2) 0.024(3) 0.030(3) -0.011(2) -0.006(2) -0.0007(19) C212 0.013(2) 0.026(3) 0.021(3) -0.005(2) -0.001(2) -0.007(2) C213 0.021(3) 0.027(3) 0.037(4) -0.013(3) -0.012(3) 0.002(2) C214 0.019(3) 0.038(4) 0.034(4) -0.007(3) -0.010(3) -0.005(3) C215 0.015(3) 0.030(3) 0.039(4) -0.013(3) -0.006(3) -0.004(2) C216 0.022(3) 0.024(3) 0.034(3) -0.008(3) -0.003(3) -0.005(2) N221 0.018(2) 0.022(3) 0.028(3) -0.010(2) -0.005(2) -0.001(2) N222 0.019(2) 0.036(3) 0.040(3) -0.023(3) -0.007(2) -0.002(2) N223 0.015(2) 0.031(3) 0.041(3) -0.018(2) -0.009(2) 0.005(2) C224 0.015(3) 0.018(3) 0.023(3) -0.006(2) -0.004(2) 0.000(2) C225 0.018(3) 0.025(3) 0.039(4) -0.012(3) -0.008(3) -0.001(2) C226 0.028(3) 0.018(3) 0.038(4) -0.009(3) -0.005(3) -0.011(2) N231 0.018(2) 0.018(2) 0.037(3) -0.008(2) -0.004(2) -0.0048(19) C232 0.026(3) 0.031(4) 0.041(4) -0.003(3) -0.008(3) -0.009(3) C233 0.106(7) 0.104(7) 0.037(4) 0.008(4) -0.031(4) -0.075(6) C234 0.107(7) 0.112(7) 0.040(5) 0.004(5) -0.038(5) -0.063(6) C235 0.042(4) 0.050(4) 0.043(4) 0.000(3) -0.024(3) -0.027(3) C236 0.024(3) 0.029(3) 0.042(4) -0.011(3) -0.009(3) -0.005(3) N241 0.015(2) 0.021(3) 0.036(3) -0.005(2) -0.003(2) -0.0066(19) N242 0.020(2) 0.027(3) 0.038(3) -0.006(2) 0.000(2) -0.011(2) N243 0.013(2) 0.028(3) 0.028(3) -0.013(2) -0.004(2) -0.0019(19) C244 0.018(3) 0.021(3) 0.037(4) -0.004(3) -0.010(3) -0.004(2) C245 0.024(3) 0.032(3) 0.031(3) -0.008(3) -0.007(3) -0.009(3) C246 0.019(3) 0.023(3) 0.051(4) -0.013(3) -0.004(3) -0.007(2) C251 0.021(3) 0.018(3) 0.033(3) -0.011(3) -0.006(2) -0.010(2) C252 0.023(3) 0.020(3) 0.031(3) -0.010(3) -0.009(3) -0.009(2) C253 0.017(3) 0.028(3) 0.038(4) -0.018(3) -0.007(3) -0.007(2) C254 0.017(3) 0.048(4) 0.034(4) -0.019(3) -0.004(3) -0.019(3) C255 0.025(3) 0.038(4) 0.035(4) -0.009(3) -0.012(3) -0.007(3) C256 0.015(3) 0.035(4) 0.034(4) -0.011(3) -0.003(3) -0.003(2) N311 0.018(2) 0.022(3) 0.038(3) -0.009(2) -0.002(2) -0.006(2) C312 0.019(3) 0.024(3) 0.032(3) -0.001(3) -0.007(3) -0.003(2) C313 0.024(3) 0.022(3) 0.054(4) -0.010(3) -0.015(3) 0.008(3) C314 0.015(3) 0.034(4) 0.062(5) -0.016(3) -0.010(3) 0.002(3) C315 0.019(3) 0.040(4) 0.041(4) -0.014(3) -0.005(3) -0.010(3) C316 0.013(3) 0.035(4) 0.048(4) -0.014(3) -0.004(3) -0.003(3) N321 0.024(3) 0.026(3) 0.032(3) -0.010(2) 0.001(2) -0.006(2) N322 0.022(3) 0.039(3) 0.039(3) -0.022(3) -0.002(2) 0.002(2) N323 0.018(2) 0.039(3) 0.041(3) -0.021(3) -0.010(2) 0.004(2) C324 0.018(3) 0.024(3) 0.023(3) 0.000(3) 0.000(2) 0.000(2) C325 0.018(3) 0.027(3) 0.039(4) -0.009(3) -0.009(3) 0.003(2) C326 0.024(3) 0.034(4) 0.035(4) -0.016(3) 0.004(3) -0.008(3) N331 0.019(2) 0.028(3) 0.031(3) -0.011(2) 0.000(2) -0.003(2) C332 0.026(3) 0.052(4) 0.032(4) -0.003(3) -0.008(3) -0.019(3) C333 0.082(6) 0.100(6) 0.043(4) 0.016(4) -0.026(4) -0.070(5) C334 0.079(6) 0.120(7) 0.038(4) 0.016(5) -0.027(4) -0.063(5) C335 0.031(3) 0.059(5) 0.040(4) -0.004(3) -0.013(3) -0.026(3) C336 0.023(3) 0.038(4) 0.038(4) -0.009(3) -0.006(3) -0.011(3) N341 0.017(2) 0.034(3) 0.034(3) -0.011(2) 0.000(2) -0.007(2) N342 0.020(2) 0.037(3) 0.033(3) -0.013(2) 0.005(2) -0.011(2) N343 0.016(2) 0.031(3) 0.033(3) -0.007(2) -0.005(2) -0.005(2) C344 0.021(3) 0.031(3) 0.030(3) -0.005(3) -0.009(3) -0.003(3) C345 0.029(3) 0.047(4) 0.033(4) -0.003(3) -0.006(3) -0.023(3) C346 0.020(3) 0.026(3) 0.042(4) -0.015(3) 0.001(3) -0.013(2) C351 0.021(3) 0.025(3) 0.029(3) -0.008(3) -0.008(3) -0.005(2) C352 0.020(3) 0.021(3) 0.031(3) -0.008(3) -0.004(2) -0.008(2) C353 0.035(3) 0.020(3) 0.029(3) -0.018(3) 0.000(3) -0.010(3) C354 0.029(3) 0.038(4) 0.019(3) -0.009(3) -0.009(3) -0.011(3) C355 0.023(3) 0.041(4) 0.033(4) -0.007(3) -0.014(3) -0.006(3) C356 0.021(3) 0.037(4) 0.040(4) -0.015(3) -0.001(3) -0.006(3) Cl11 0.0317(8) 0.0217(8) 0.0390(9) -0.0023(7) -0.0063(7) -0.0029(6) O12 0.030(2) 0.021(2) 0.053(3) -0.009(2) -0.007(2) -0.0076(18) O13 0.099(4) 0.037(3) 0.043(3) -0.014(2) 0.001(3) -0.024(3) O14 0.022(2) 0.032(3) 0.092(4) -0.002(3) -0.004(2) -0.007(2) O15 0.039(3) 0.048(3) 0.058(3) 0.015(3) -0.019(2) 0.008(2) Cl21 0.0166(6) 0.0304(8) 0.0323(8) -0.0050(7) -0.0013(6) -0.0051(6) O22 0.043(3) 0.023(3) 0.091(4) -0.010(3) 0.011(3) -0.003(2) O23 0.016(2) 0.049(3) 0.057(3) -0.013(2) -0.001(2) -0.0021(19) O24 0.035(3) 0.059(3) 0.032(3) -0.001(2) 0.000(2) -0.022(2) O25 0.029(2) 0.081(4) 0.039(3) -0.019(3) -0.006(2) -0.017(2) Cl31 0.0165(6) 0.0275(8) 0.0373(9) -0.0065(7) -0.0048(6) -0.0015(6) O32 0.038(3) 0.037(3) 0.086(4) -0.007(3) -0.020(3) -0.007(2) O33 0.031(2) 0.061(3) 0.055(3) -0.012(3) -0.023(2) 0.000(2) O34 0.036(3) 0.056(3) 0.039(3) -0.020(2) 0.015(2) -0.020(2) O35 0.018(2) 0.053(3) 0.045(3) -0.016(2) -0.0061(19) 0.008(2) Cl41 0.0216(7) 0.0218(7) 0.0427(9) -0.0062(7) -0.0120(6) 0.0008(6) O42 0.018(2) 0.040(3) 0.051(3) -0.009(2) -0.005(2) -0.0019(19) O43 0.055(3) 0.045(3) 0.051(3) 0.006(2) -0.026(3) 0.006(2) O44 0.029(2) 0.020(2) 0.055(3) -0.012(2) -0.009(2) -0.0029(18) O45 0.029(2) 0.042(3) 0.059(3) -0.028(2) -0.001(2) -0.004(2) O11S 0.036(3) 0.057(3) 0.038(3) 0.004(2) 0.000(2) 0.002(2) N12S 0.029(3) 0.051(4) 0.037(3) 0.003(3) -0.009(3) -0.009(3) C13S 0.035(4) 0.059(5) 0.044(5) -0.004(4) -0.003(3) -0.009(4) C14S 0.060(5) 0.046(5) 0.039(4) -0.004(4) -0.003(4) -0.011(4) C15S 0.026(4) 0.115(8) 0.052(5) 0.008(5) -0.005(4) -0.008(4) O21S 0.032(3) 0.065(4) 0.046(3) 0.014(3) -0.014(2) -0.015(2) N22S 0.026(3) 0.040(3) 0.031(3) -0.004(3) -0.006(2) -0.004(2) C23S 0.024(3) 0.027(3) 0.037(4) -0.008(3) -0.002(3) -0.001(3) C24S 0.063(5) 0.047(5) 0.038(4) 0.007(4) -0.008(4) -0.023(4) C25S 0.031(4) 0.077(6) 0.044(4) 0.002(4) -0.002(3) -0.012(4) O41S 0.060(3) 0.059(3) 0.053(3) -0.016(3) -0.006(3) -0.028(3) N42S 0.047(3) 0.031(3) 0.041(3) -0.002(3) -0.008(3) -0.013(3) C43S 0.070(5) 0.041(4) 0.047(5) -0.011(4) 0.016(4) -0.024(4) C44S 0.045(4) 0.053(5) 0.059(5) 0.000(4) -0.003(4) -0.022(4) C45S 0.065(5) 0.031(4) 0.071(6) -0.015(4) -0.006(4) -0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb2 N343 2.629(5) . ? Pb2 O11S 2.641(5) . ? Pb2 N143 2.681(5) . ? Pb2 N331 2.690(3) . ? Pb2 N323 2.701(5) . ? Pb2 N311 2.712(4) . ? Pb2 N131 2.722(5) . ? Pb1 N243 2.605(5) . ? Pb1 N123 2.609(5) . ? Pb1 O21S 2.690(4) . ? Pb1 N211 2.713(4) . ? Pb1 N231 2.722(3) . ? Pb1 N223 2.735(5) . ? Pb1 N111 2.748(4) . ? N111 C112 1.339(7) . ? N111 C116 1.347(6) . ? C112 C113 1.387(8) . ? C112 C124 1.461(7) . ? C113 C114 1.389(8) . ? C113 H113 0.9500 . ? C114 C115 1.375(8) . ? C114 H114 0.9500 . ? C115 C116 1.380(8) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.340(6) . ? N121 C125 1.342(7) . ? N121 C126 1.477(6) . ? N122 N123 1.320(6) . ? N123 C124 1.368(7) . ? C124 C125 1.372(7) . ? C125 H125 0.9500 . ? C126 C151 1.534(8) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C136 1.336(7) . ? N131 C132 1.355(7) . ? C132 C133 1.376(8) . ? C132 C144 1.460(7) . ? C133 C134 1.392(8) . ? C133 H133 0.9500 . ? C134 C135 1.390(8) . ? C134 H134 0.9500 . ? C135 C136 1.372(8) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.336(7) . ? N141 N142 1.348(6) . ? N141 C146 1.464(6) . ? N142 N143 1.322(6) . ? N143 C144 1.359(7) . ? C144 C145 1.381(7) . ? C145 H145 0.9500 . ? C146 C153 1.527(8) . ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? C151 C156 1.383(8) . ? C151 C152 1.387(8) . ? C152 C153 1.399(8) . ? C152 H152 0.9500 . ? C153 C154 1.374(8) . ? C154 C155 1.388(8) . ? C154 H154 0.9500 . ? C155 C156 1.381(8) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? N211 C212 1.334(7) . ? N211 C216 1.341(7) . ? C212 C213 1.398(7) . ? C212 C224 1.461(7) . ? C213 C214 1.384(7) . ? C213 H213 0.9500 . ? C214 C215 1.374(8) . ? C214 H214 0.9500 . ? C215 C216 1.382(7) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 N222 1.342(6) . ? N221 C225 1.349(6) . ? N221 C226 1.462(6) . ? N222 N223 1.318(6) . ? N223 C224 1.364(6) . ? C224 C225 1.394(7) . ? C225 H225 0.9500 . ? C226 C251 1.514(8) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? N231 C232 1.3900 . ? N231 C236 1.3900 . ? C232 C233 1.3900 . ? C232 C244 1.433(6) . ? C233 C234 1.3900 . ? C233 H233 0.9500 . ? C234 C235 1.3900 . ? C234 H234 0.9500 . ? C235 C236 1.3900 . ? C235 H235 0.9500 . ? C236 H236 0.9500 . ? N241 C245 1.333(7) . ? N241 N242 1.348(6) . ? N241 C246 1.475(6) . ? N242 N243 1.309(6) . ? N243 C244 1.339(7) . ? C244 C245 1.373(8) . ? C245 H245 0.9500 . ? C246 C253 1.512(7) . ? C246 H24A 0.9900 . ? C246 H24B 0.9900 . ? C251 C256 1.385(8) . ? C251 C252 1.394(7) . ? C252 C253 1.381(8) 2_666 ? C252 H252 0.9500 . ? C253 C254 1.375(8) . ? C253 C252 1.381(8) 2_666 ? C254 C255 1.376(8) . ? C254 H254 0.9500 . ? C255 C256 1.388(8) 2_666 ? C255 H255 0.9500 . ? C256 C255 1.388(8) 2_666 ? C256 H256 0.9500 . ? N311 C316 1.340(7) . ? N311 C312 1.354(7) . ? C312 C313 1.370(7) . ? C312 C324 1.455(8) . ? C313 C314 1.408(8) . ? C313 H313 0.9500 . ? C314 C315 1.366(8) . ? C314 H314 0.9500 . ? C315 C316 1.378(7) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C325 1.339(7) . ? N321 N322 1.346(6) . ? N321 C326 1.476(7) . ? N322 N323 1.317(6) . ? N323 C324 1.359(7) . ? C324 C325 1.372(8) . ? C325 H325 0.9500 . ? C326 C351 1.515(8) 2_677 ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? N331 C332 1.3900 . ? N331 C336 1.3900 . ? C332 C333 1.3900 . ? C332 C344 1.426(6) . ? C333 C334 1.3900 . ? C333 H333 0.9500 . ? C334 C335 1.3900 . ? C334 H334 0.9500 . ? C335 C336 1.3900 . ? C335 H335 0.9500 . ? C336 H336 0.9500 . ? N341 C345 1.336(7) . ? N341 N342 1.339(7) . ? N341 C346 1.465(6) . ? N342 N343 1.311(6) . ? N343 C344 1.354(7) . ? C344 C345 1.384(8) . ? C345 H345 0.9500 . ? C346 C353 1.494(8) . ? C346 H34A 0.9900 . ? C346 H34B 0.9900 . ? C351 C352 1.378(7) . ? C351 C356 1.397(8) . ? C351 C326 1.515(8) 2_677 ? C352 C353 1.377(8) . ? C352 H352 0.9500 . ? C353 C354 1.384(8) . ? C354 C355 1.379(8) . ? C354 H354 0.9500 . ? C355 C356 1.383(8) . ? C355 H355 0.9500 . ? C356 H356 0.9500 . ? Cl11 O15 1.425(4) . ? Cl11 O12 1.429(4) . ? Cl11 O13 1.431(5) . ? Cl11 O14 1.434(4) . ? Cl21 O22 1.413(5) . ? Cl21 O24 1.432(4) . ? Cl21 O23 1.432(4) . ? Cl21 O25 1.442(4) . ? Cl31 O32 1.423(5) . ? Cl31 O35 1.433(4) . ? Cl31 O33 1.440(4) . ? Cl31 O34 1.447(4) . ? Cl41 O43 1.422(4) . ? Cl41 O44 1.429(4) . ? Cl41 O45 1.445(4) . ? Cl41 O42 1.448(4) . ? O11S C13S 1.230(8) . ? N12S C13S 1.312(8) . ? N12S C14S 1.442(8) . ? N12S C15S 1.456(8) . ? C13S H13S 0.9500 . ? C14S H14C 0.9800 . ? C14S H14D 0.9800 . ? C14S H14E 0.9800 . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? O21S C23S 1.216(7) . ? N22S C23S 1.317(7) . ? N22S C25S 1.452(8) . ? N22S C24S 1.452(8) . ? C23S H23S 0.9500 . ? C24S H24C 0.9800 . ? C24S H24D 0.9800 . ? C24S H24E 0.9800 . ? C25S H25A 0.9800 . ? C25S H25B 0.9800 . ? C25S H25C 0.9800 . ? O31X C32X 1.2312(18) . ? C32X C34X 1.5200(18) . ? C32X C33X 1.5250(18) . ? C33X H33A 0.9800 . ? C33X H33B 0.9800 . ? C33X H33C 0.9800 . ? C34X H34C 0.9800 . ? C34X H34D 0.9800 . ? C34X H34E 0.9800 . ? O31Y C32Y 1.2300(18) . ? C32Y C34Y 1.5225(18) . ? C32Y C33Y 1.5226(18) . ? C33Y H33D 0.9800 . ? C33Y H33E 0.9800 . ? C33Y H33F 0.9800 . ? C34Y H34F 0.9800 . ? C34Y H34G 0.9800 . ? C34Y H34H 0.9800 . ? O41S C43S 1.2578 . ? N42S C43S 1.3474 . ? N42S C44S 1.448(7) . ? N42S C45S 1.457(7) . ? C43S H43S 0.9500 . ? C44S H44A 0.9800 . ? C44S H44B 0.9800 . ? C44S H44C 0.9800 . ? C45S H45A 0.9800 . ? C45S H45B 0.9800 . ? C45S H45C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N343 Pb2 O11S 137.09(14) . . ? N343 Pb2 N143 73.94(14) . . ? O11S Pb2 N143 86.71(15) . . ? N343 Pb2 N331 62.79(12) . . ? O11S Pb2 N331 144.21(13) . . ? N143 Pb2 N331 128.68(13) . . ? N343 Pb2 N323 105.15(15) . . ? O11S Pb2 N323 71.14(15) . . ? N143 Pb2 N323 146.32(13) . . ? N331 Pb2 N323 74.67(13) . . ? N343 Pb2 N311 73.20(14) . . ? O11S Pb2 N311 67.54(14) . . ? N143 Pb2 N311 86.29(14) . . ? N331 Pb2 N311 105.13(13) . . ? N323 Pb2 N311 62.17(14) . . ? N343 Pb2 N131 71.82(14) . . ? O11S Pb2 N131 130.93(14) . . ? N143 Pb2 N131 61.53(13) . . ? N331 Pb2 N131 79.11(13) . . ? N323 Pb2 N131 151.42(14) . . ? N311 Pb2 N131 137.60(13) . . ? N243 Pb1 N123 71.54(14) . . ? N243 Pb1 O21S 129.64(13) . . ? N123 Pb1 O21S 81.50(15) . . ? N243 Pb1 N211 73.66(14) . . ? N123 Pb1 N211 90.16(13) . . ? O21S Pb1 N211 64.52(14) . . ? N243 Pb1 N231 61.94(12) . . ? N123 Pb1 N231 124.24(13) . . ? O21S Pb1 N231 152.99(14) . . ? N211 Pb1 N231 103.81(12) . . ? N243 Pb1 N223 103.59(14) . . ? N123 Pb1 N223 151.16(13) . . ? O21S Pb1 N223 80.62(15) . . ? N211 Pb1 N223 61.68(13) . . ? N231 Pb1 N223 72.54(13) . . ? N243 Pb1 N111 73.56(13) . . ? N123 Pb1 N111 61.72(13) . . ? O21S Pb1 N111 128.23(15) . . ? N211 Pb1 N111 142.15(13) . . ? N231 Pb1 N111 76.51(12) . . ? N223 Pb1 N111 145.73(13) . . ? C112 N111 C116 117.7(5) . . ? C112 N111 Pb1 119.7(3) . . ? C116 N111 Pb1 122.3(4) . . ? N111 C112 C113 122.8(5) . . ? N111 C112 C124 115.7(5) . . ? C113 C112 C124 121.5(5) . . ? C112 C113 C114 118.7(6) . . ? C112 C113 H113 120.6 . . ? C114 C113 H113 120.6 . . ? C115 C114 C113 118.6(6) . . ? C115 C114 H114 120.7 . . ? C113 C114 H114 120.7 . . ? C114 C115 C116 119.4(5) . . ? C114 C115 H115 120.3 . . ? C116 C115 H115 120.3 . . ? N111 C116 C115 122.7(5) . . ? N111 C116 H116 118.7 . . ? C115 C116 H116 118.7 . . ? N122 N121 C125 111.8(4) . . ? N122 N121 C126 120.5(5) . . ? C125 N121 C126 127.5(5) . . ? N123 N122 N121 106.3(4) . . ? N122 N123 C124 109.5(4) . . ? N122 N123 Pb1 128.8(3) . . ? C124 N123 Pb1 120.5(3) . . ? N123 C124 C125 107.5(5) . . ? N123 C124 C112 121.2(5) . . ? C125 C124 C112 131.4(5) . . ? N121 C125 C124 104.9(5) . . ? N121 C125 H125 127.5 . . ? C124 C125 H125 127.5 . . ? N121 C126 C151 111.5(5) . . ? N121 C126 H12A 109.3 . . ? C151 C126 H12A 109.3 . . ? N121 C126 H12B 109.3 . . ? C151 C126 H12B 109.3 . . ? H12A C126 H12B 108.0 . . ? C136 N131 C132 117.8(5) . . ? C136 N131 Pb2 121.0(4) . . ? C132 N131 Pb2 120.8(3) . . ? N131 C132 C133 122.4(5) . . ? N131 C132 C144 115.7(5) . . ? C133 C132 C144 121.9(5) . . ? C132 C133 C134 118.8(6) . . ? C132 C133 H133 120.6 . . ? C134 C133 H133 120.6 . . ? C135 C134 C133 119.0(6) . . ? C135 C134 H134 120.5 . . ? C133 C134 H134 120.5 . . ? C136 C135 C134 118.4(5) . . ? C136 C135 H135 120.8 . . ? C134 C135 H135 120.8 . . ? N131 C136 C135 123.6(6) . . ? N131 C136 H136 118.2 . . ? C135 C136 H136 118.2 . . ? C145 N141 N142 111.4(4) . . ? C145 N141 C146 130.1(5) . . ? N142 N141 C146 118.1(4) . . ? N143 N142 N141 106.4(4) . . ? N142 N143 C144 109.7(4) . . ? N142 N143 Pb2 129.3(3) . . ? C144 N143 Pb2 118.5(3) . . ? N143 C144 C145 107.3(5) . . ? N143 C144 C132 121.6(5) . . ? C145 C144 C132 131.1(5) . . ? N141 C145 C144 105.3(5) . . ? N141 C145 H145 127.3 . . ? C144 C145 H145 127.3 . . ? N141 C146 C153 110.8(4) . . ? N141 C146 H14A 109.5 . . ? C153 C146 H14A 109.5 . . ? N141 C146 H14B 109.5 . . ? C153 C146 H14B 109.5 . . ? H14A C146 H14B 108.1 . . ? C156 C151 C152 120.5(5) . . ? C156 C151 C126 119.0(5) . . ? C152 C151 C126 120.5(6) . . ? C151 C152 C153 119.3(6) . . ? C151 C152 H152 120.3 . . ? C153 C152 H152 120.3 . . ? C154 C153 C152 119.8(5) . . ? C154 C153 C146 120.9(5) . . ? C152 C153 C146 119.3(5) . . ? C153 C154 C155 120.6(5) . . ? C153 C154 H154 119.7 . . ? C155 C154 H154 119.7 . . ? C156 C155 C154 119.8(6) . . ? C156 C155 H155 120.1 . . ? C154 C155 H155 120.1 . . ? C155 C156 C151 119.9(5) . . ? C155 C156 H156 120.0 . . ? C151 C156 H156 120.0 . . ? C212 N211 C216 117.9(5) . . ? C212 N211 Pb1 120.3(3) . . ? C216 N211 Pb1 119.9(4) . . ? N211 C212 C213 122.6(5) . . ? N211 C212 C224 116.9(4) . . ? C213 C212 C224 120.5(5) . . ? C214 C213 C212 118.3(5) . . ? C214 C213 H213 120.8 . . ? C212 C213 H213 120.8 . . ? C215 C214 C213 119.3(5) . . ? C215 C214 H214 120.3 . . ? C213 C214 H214 120.3 . . ? C214 C215 C216 118.7(5) . . ? C214 C215 H215 120.6 . . ? C216 C215 H215 120.6 . . ? N211 C216 C215 123.1(5) . . ? N211 C216 H216 118.4 . . ? C215 C216 H216 118.4 . . ? N222 N221 C225 111.3(4) . . ? N222 N221 C226 120.5(4) . . ? C225 N221 C226 128.1(5) . . ? N223 N222 N221 107.4(4) . . ? N222 N223 C224 109.3(4) . . ? N222 N223 Pb1 132.7(3) . . ? C224 N223 Pb1 115.9(3) . . ? N223 C224 C225 107.6(4) . . ? N223 C224 C212 122.3(5) . . ? C225 C224 C212 130.1(5) . . ? N221 C225 C224 104.5(5) . . ? N221 C225 H225 127.7 . . ? C224 C225 H225 127.7 . . ? N221 C226 C251 110.2(4) . . ? N221 C226 H22A 109.6 . . ? C251 C226 H22A 109.6 . . ? N221 C226 H22B 109.6 . . ? C251 C226 H22B 109.6 . . ? H22A C226 H22B 108.1 . . ? C232 N231 C236 120.0 . . ? C232 N231 Pb1 118.96(16) . . ? C236 N231 Pb1 120.89(16) . . ? C233 C232 N231 120.0 . . ? C233 C232 C244 125.1(3) . . ? N231 C232 C244 114.9(3) . . ? C232 C233 C234 120.0 . . ? C232 C233 H233 120.0 . . ? C234 C233 H233 120.0 . . ? C235 C234 C233 120.0 . . ? C235 C234 H234 120.0 . . ? C233 C234 H234 120.0 . . ? C236 C235 C234 120.0 . . ? C236 C235 H235 120.0 . . ? C234 C235 H235 120.0 . . ? C235 C236 N231 120.0 . . ? C235 C236 H236 120.0 . . ? N231 C236 H236 120.0 . . ? C245 N241 N242 111.8(4) . . ? C245 N241 C246 128.5(5) . . ? N242 N241 C246 119.3(5) . . ? N243 N242 N241 105.7(4) . . ? N242 N243 C244 110.1(5) . . ? N242 N243 Pb1 128.1(4) . . ? C244 N243 Pb1 120.9(3) . . ? N243 C244 C245 108.2(5) . . ? N243 C244 C232 122.5(5) . . ? C245 C244 C232 129.2(5) . . ? N241 C245 C244 104.2(5) . . ? N241 C245 H245 127.9 . . ? C244 C245 H245 127.9 . . ? N241 C246 C253 110.0(4) . . ? N241 C246 H24A 109.7 . . ? C253 C246 H24A 109.7 . . ? N241 C246 H24B 109.7 . . ? C253 C246 H24B 109.7 . . ? H24A C246 H24B 108.2 . . ? C256 C251 C252 119.4(5) . . ? C256 C251 C226 121.0(5) . . ? C252 C251 C226 119.6(5) . . ? C253 C252 C251 120.9(5) 2_666 . ? C253 C252 H252 119.6 2_666 . ? C251 C252 H252 119.6 . . ? C254 C253 C252 118.8(5) . 2_666 ? C254 C253 C246 120.6(6) . . ? C252 C253 C246 120.5(5) 2_666 . ? C253 C254 C255 121.2(6) . . ? C253 C254 H254 119.4 . . ? C255 C254 H254 119.4 . . ? C254 C255 C256 120.0(6) . 2_666 ? C254 C255 H255 120.0 . . ? C256 C255 H255 120.0 2_666 . ? C251 C256 C255 119.6(6) . 2_666 ? C251 C256 H256 120.2 . . ? C255 C256 H256 120.2 2_666 . ? C316 N311 C312 117.9(5) . . ? C316 N311 Pb2 121.5(4) . . ? C312 N311 Pb2 119.2(3) . . ? N311 C312 C313 121.7(5) . . ? N311 C312 C324 116.6(5) . . ? C313 C312 C324 121.7(5) . . ? C312 C313 C314 119.8(6) . . ? C312 C313 H313 120.1 . . ? C314 C313 H313 120.1 . . ? C315 C314 C313 118.0(5) . . ? C315 C314 H314 121.0 . . ? C313 C314 H314 121.0 . . ? C314 C315 C316 119.2(6) . . ? C314 C315 H315 120.4 . . ? C316 C315 H315 120.4 . . ? N311 C316 C315 123.3(6) . . ? N311 C316 H316 118.4 . . ? C315 C316 H316 118.3 . . ? C325 N321 N322 112.4(5) . . ? C325 N321 C326 128.0(5) . . ? N322 N321 C326 119.4(5) . . ? N323 N322 N321 105.3(4) . . ? N322 N323 C324 110.2(5) . . ? N322 N323 Pb2 130.6(3) . . ? C324 N323 Pb2 116.0(4) . . ? N323 C324 C325 107.6(5) . . ? N323 C324 C312 122.6(5) . . ? C325 C324 C312 129.7(5) . . ? N321 C325 C324 104.4(5) . . ? N321 C325 H325 127.8 . . ? C324 C325 H325 127.8 . . ? N321 C326 C351 109.9(5) . 2_677 ? N321 C326 H32A 109.7 . . ? C351 C326 H32A 109.7 2_677 . ? N321 C326 H32B 109.7 . . ? C351 C326 H32B 109.7 2_677 . ? H32A C326 H32B 108.2 . . ? C332 N331 C336 120.0 . . ? C332 N331 Pb2 119.25(17) . . ? C336 N331 Pb2 120.50(17) . . ? N331 C332 C333 120.0 . . ? N331 C332 C344 115.2(3) . . ? C333 C332 C344 124.8(3) . . ? C332 C333 C334 120.0 . . ? C332 C333 H333 120.0 . . ? C334 C333 H333 120.0 . . ? C335 C334 C333 120.0 . . ? C335 C334 H334 120.0 . . ? C333 C334 H334 120.0 . . ? C334 C335 C336 120.0 . . ? C334 C335 H335 120.0 . . ? C336 C335 H335 120.0 . . ? C335 C336 N331 120.0 . . ? C335 C336 H336 120.0 . . ? N331 C336 H336 120.0 . . ? C345 N341 N342 111.4(5) . . ? C345 N341 C346 127.5(5) . . ? N342 N341 C346 120.7(5) . . ? N343 N342 N341 106.9(5) . . ? N342 N343 C344 109.5(5) . . ? N342 N343 Pb2 130.9(4) . . ? C344 N343 Pb2 118.2(4) . . ? N343 C344 C345 107.5(5) . . ? N343 C344 C332 123.6(5) . . ? C345 C344 C332 128.9(5) . . ? N341 C345 C344 104.6(5) . . ? N341 C345 H345 127.7 . . ? C344 C345 H345 127.7 . . ? N341 C346 C353 110.2(4) . . ? N341 C346 H34A 109.6 . . ? C353 C346 H34A 109.6 . . ? N341 C346 H34B 109.6 . . ? C353 C346 H34B 109.6 . . ? H34A C346 H34B 108.1 . . ? C352 C351 C356 118.0(5) . . ? C352 C351 C326 122.1(5) . 2_677 ? C356 C351 C326 119.9(5) . 2_677 ? C353 C352 C351 123.0(5) . . ? C353 C352 H352 118.5 . . ? C351 C352 H352 118.5 . . ? C352 C353 C354 117.5(5) . . ? C352 C353 C346 121.7(5) . . ? C354 C353 C346 120.8(5) . . ? C355 C354 C353 121.7(6) . . ? C355 C354 H354 119.2 . . ? C353 C354 H354 119.2 . . ? C354 C355 C356 119.3(6) . . ? C354 C355 H355 120.3 . . ? C356 C355 H355 120.3 . . ? C355 C356 C351 120.4(6) . . ? C355 C356 H356 119.8 . . ? C351 C356 H356 119.8 . . ? O15 Cl11 O12 110.6(3) . . ? O15 Cl11 O13 111.4(3) . . ? O12 Cl11 O13 109.4(3) . . ? O15 Cl11 O14 108.7(3) . . ? O12 Cl11 O14 109.0(3) . . ? O13 Cl11 O14 107.7(3) . . ? O22 Cl21 O24 110.9(3) . . ? O22 Cl21 O23 109.7(3) . . ? O24 Cl21 O23 109.8(3) . . ? O22 Cl21 O25 110.0(3) . . ? O24 Cl21 O25 107.9(3) . . ? O23 Cl21 O25 108.5(3) . . ? O32 Cl31 O35 109.8(3) . . ? O32 Cl31 O33 111.6(3) . . ? O35 Cl31 O33 108.6(3) . . ? O32 Cl31 O34 109.6(3) . . ? O35 Cl31 O34 109.2(3) . . ? O33 Cl31 O34 108.0(3) . . ? O43 Cl41 O44 109.9(3) . . ? O43 Cl41 O45 110.6(3) . . ? O44 Cl41 O45 109.0(3) . . ? O43 Cl41 O42 109.8(3) . . ? O44 Cl41 O42 107.7(2) . . ? O45 Cl41 O42 109.7(3) . . ? C13S O11S Pb2 128.9(5) . . ? C13S N12S C14S 121.4(6) . . ? C13S N12S C15S 121.8(6) . . ? C14S N12S C15S 116.8(5) . . ? O11S C13S N12S 124.5(7) . . ? O11S C13S H13S 117.8 . . ? N12S C13S H13S 117.8 . . ? N12S C14S H14C 109.5 . . ? N12S C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? N12S C14S H14E 109.5 . . ? H14C C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? N12S C15S H15A 109.5 . . ? N12S C15S H15B 109.5 . . ? H15A C15S H15B 109.5 . . ? N12S C15S H15C 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? C23S O21S Pb1 148.7(4) . . ? C23S N22S C25S 120.5(5) . . ? C23S N22S C24S 122.3(5) . . ? C25S N22S C24S 117.0(5) . . ? O21S C23S N22S 125.6(6) . . ? O21S C23S H23S 117.2 . . ? N22S C23S H23S 117.2 . . ? N22S C24S H24C 109.5 . . ? N22S C24S H24D 109.5 . . ? H24C C24S H24D 109.5 . . ? N22S C24S H24E 109.5 . . ? H24C C24S H24E 109.5 . . ? H24D C24S H24E 109.5 . . ? N22S C25S H25A 109.5 . . ? N22S C25S H25B 109.5 . . ? H25A C25S H25B 109.5 . . ? N22S C25S H25C 109.5 . . ? H25A C25S H25C 109.5 . . ? H25B C25S H25C 109.5 . . ? O31X C32X C34X 121.86(19) . . ? O31X C32X C33X 121.45(19) . . ? C34X C32X C33X 116.68(16) . . ? C32X C33X H33A 109.5 . . ? C32X C33X H33B 109.5 . . ? H33A C33X H33B 109.5 . . ? C32X C33X H33C 109.5 . . ? H33A C33X H33C 109.5 . . ? H33B C33X H33C 109.5 . . ? C32X C34X H34C 109.5 . . ? C32X C34X H34D 109.5 . . ? H34C C34X H34D 109.5 . . ? C32X C34X H34E 109.5 . . ? H34C C34X H34E 109.5 . . ? H34D C34X H34E 109.5 . . ? O31Y C32Y C34Y 121.72(19) . . ? O31Y C32Y C33Y 121.38(19) . . ? C34Y C32Y C33Y 116.90(17) . . ? C32Y C33Y H33D 109.5 . . ? C32Y C33Y H33E 109.5 . . ? H33D C33Y H33E 109.5 . . ? C32Y C33Y H33F 109.5 . . ? H33D C33Y H33F 109.5 . . ? H33E C33Y H33F 109.5 . . ? C32Y C34Y H34F 109.5 . . ? C32Y C34Y H34G 109.5 . . ? H34F C34Y H34G 109.5 . . ? C32Y C34Y H34H 109.5 . . ? H34F C34Y H34H 109.5 . . ? H34G C34Y H34H 109.5 . . ? C43S N42S C44S 121.6(3) . . ? C43S N42S C45S 121.5(3) . . ? C44S N42S C45S 116.0(5) . . ? O41S C43S N42S 123.4 . . ? O41S C43S H43S 118.3 . . ? N42S C43S H43S 118.3 . . ? N42S C44S H44A 109.5 . . ? N42S C44S H44B 109.5 . . ? H44A C44S H44B 109.5 . . ? N42S C44S H44C 109.5 . . ? H44A C44S H44C 109.5 . . ? H44B C44S H44C 109.5 . . ? N42S C45S H45A 109.5 . . ? N42S C45S H45B 109.5 . . ? H45A C45S H45B 109.5 . . ? N42S C45S H45C 109.5 . . ? H45A C45S H45C 109.5 . . ? H45B C45S H45C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N243 Pb1 N111 C112 -69.5(4) . . . . ? N123 Pb1 N111 C112 8.0(4) . . . . ? O21S Pb1 N111 C112 58.4(4) . . . . ? N211 Pb1 N111 C112 -38.6(5) . . . . ? N231 Pb1 N111 C112 -133.8(4) . . . . ? N223 Pb1 N111 C112 -159.7(4) . . . . ? N243 Pb1 N111 C116 104.9(4) . . . . ? N123 Pb1 N111 C116 -177.5(5) . . . . ? O21S Pb1 N111 C116 -127.2(4) . . . . ? N211 Pb1 N111 C116 135.9(4) . . . . ? N231 Pb1 N111 C116 40.6(4) . . . . ? N223 Pb1 N111 C116 14.8(5) . . . . ? C116 N111 C112 C113 -1.5(8) . . . . ? Pb1 N111 C112 C113 173.2(4) . . . . ? C116 N111 C112 C124 179.4(5) . . . . ? Pb1 N111 C112 C124 -5.9(6) . . . . ? N111 C112 C113 C114 2.6(9) . . . . ? C124 C112 C113 C114 -178.3(5) . . . . ? C112 C113 C114 C115 -2.6(9) . . . . ? C113 C114 C115 C116 1.5(9) . . . . ? C112 N111 C116 C115 0.3(8) . . . . ? Pb1 N111 C116 C115 -174.2(4) . . . . ? C114 C115 C116 N111 -0.4(9) . . . . ? C125 N121 N122 N123 0.6(6) . . . . ? C126 N121 N122 N123 176.6(5) . . . . ? N121 N122 N123 C124 0.1(6) . . . . ? N121 N122 N123 Pb1 167.2(3) . . . . ? N243 Pb1 N123 N122 -94.6(5) . . . . ? O21S Pb1 N123 N122 42.3(5) . . . . ? N211 Pb1 N123 N122 -21.9(5) . . . . ? N231 Pb1 N123 N122 -128.8(4) . . . . ? N223 Pb1 N123 N122 -9.9(7) . . . . ? N111 Pb1 N123 N122 -175.4(5) . . . . ? N243 Pb1 N123 C124 71.4(4) . . . . ? O21S Pb1 N123 C124 -151.8(4) . . . . ? N211 Pb1 N123 C124 144.0(4) . . . . ? N231 Pb1 N123 C124 37.1(5) . . . . ? N223 Pb1 N123 C124 156.0(4) . . . . ? N111 Pb1 N123 C124 -9.5(4) . . . . ? N122 N123 C124 C125 -0.7(6) . . . . ? Pb1 N123 C124 C125 -169.1(3) . . . . ? N122 N123 C124 C112 179.8(5) . . . . ? Pb1 N123 C124 C112 11.4(7) . . . . ? N111 C112 C124 N123 -3.3(8) . . . . ? C113 C112 C124 N123 177.6(5) . . . . ? N111 C112 C124 C125 177.3(6) . . . . ? C113 C112 C124 C125 -1.8(10) . . . . ? N122 N121 C125 C124 -1.1(6) . . . . ? C126 N121 C125 C124 -176.7(5) . . . . ? N123 C124 C125 N121 1.1(6) . . . . ? C112 C124 C125 N121 -179.5(6) . . . . ? N122 N121 C126 C151 29.3(7) . . . . ? C125 N121 C126 C151 -155.3(5) . . . . ? N343 Pb2 N131 C136 -100.8(4) . . . . ? O11S Pb2 N131 C136 121.9(4) . . . . ? N143 Pb2 N131 C136 178.0(5) . . . . ? N331 Pb2 N131 C136 -36.1(4) . . . . ? N323 Pb2 N131 C136 -12.4(6) . . . . ? N311 Pb2 N131 C136 -136.6(4) . . . . ? N343 Pb2 N131 C132 72.3(4) . . . . ? O11S Pb2 N131 C132 -65.1(4) . . . . ? N143 Pb2 N131 C132 -8.9(4) . . . . ? N331 Pb2 N131 C132 137.0(4) . . . . ? N323 Pb2 N131 C132 160.7(4) . . . . ? N311 Pb2 N131 C132 36.4(5) . . . . ? C136 N131 C132 C133 0.8(8) . . . . ? Pb2 N131 C132 C133 -172.5(4) . . . . ? C136 N131 C132 C144 178.8(5) . . . . ? Pb2 N131 C132 C144 5.5(6) . . . . ? N131 C132 C133 C134 -0.5(9) . . . . ? C144 C132 C133 C134 -178.3(6) . . . . ? C132 C133 C134 C135 0.1(10) . . . . ? C133 C134 C135 C136 -0.1(10) . . . . ? C132 N131 C136 C135 -0.8(9) . . . . ? Pb2 N131 C136 C135 172.5(5) . . . . ? C134 C135 C136 N131 0.5(10) . . . . ? C145 N141 N142 N143 0.8(6) . . . . ? C146 N141 N142 N143 174.3(4) . . . . ? N141 N142 N143 C144 -0.8(6) . . . . ? N141 N142 N143 Pb2 -162.1(3) . . . . ? N343 Pb2 N143 N142 94.0(4) . . . . ? O11S Pb2 N143 N142 -47.2(4) . . . . ? N331 Pb2 N143 N142 126.9(4) . . . . ? N323 Pb2 N143 N142 0.7(6) . . . . ? N311 Pb2 N143 N142 20.5(4) . . . . ? N131 Pb2 N143 N142 171.7(5) . . . . ? N343 Pb2 N143 C144 -65.9(4) . . . . ? O11S Pb2 N143 C144 152.8(4) . . . . ? N331 Pb2 N143 C144 -33.0(4) . . . . ? N323 Pb2 N143 C144 -159.3(4) . . . . ? N311 Pb2 N143 C144 -139.5(4) . . . . ? N131 Pb2 N143 C144 11.8(4) . . . . ? N142 N143 C144 C145 0.5(6) . . . . ? Pb2 N143 C144 C145 164.2(3) . . . . ? N142 N143 C144 C132 -178.8(5) . . . . ? Pb2 N143 C144 C132 -15.2(7) . . . . ? N131 C132 C144 N143 6.5(8) . . . . ? C133 C132 C144 N143 -175.5(6) . . . . ? N131 C132 C144 C145 -172.7(6) . . . . ? C133 C132 C144 C145 5.3(10) . . . . ? N142 N141 C145 C144 -0.4(6) . . . . ? C146 N141 C145 C144 -173.0(5) . . . . ? N143 C144 C145 N141 -0.1(6) . . . . ? C132 C144 C145 N141 179.2(5) . . . . ? C145 N141 C146 C153 86.4(7) . . . . ? N142 N141 C146 C153 -85.8(6) . . . . ? N121 C126 C151 C156 -83.4(7) . . . . ? N121 C126 C151 C152 97.1(6) . . . . ? C156 C151 C152 C153 0.3(8) . . . . ? C126 C151 C152 C153 179.8(5) . . . . ? C151 C152 C153 C154 -0.2(8) . . . . ? C151 C152 C153 C146 -179.7(5) . . . . ? N141 C146 C153 C154 -62.1(7) . . . . ? N141 C146 C153 C152 117.3(6) . . . . ? C152 C153 C154 C155 0.1(9) . . . . ? C146 C153 C154 C155 179.6(5) . . . . ? C153 C154 C155 C156 -0.1(9) . . . . ? C154 C155 C156 C151 0.2(9) . . . . ? C152 C151 C156 C155 -0.3(9) . . . . ? C126 C151 C156 C155 -179.8(5) . . . . ? N243 Pb1 N211 C212 -130.4(4) . . . . ? N123 Pb1 N211 C212 159.0(4) . . . . ? O21S Pb1 N211 C212 78.5(4) . . . . ? N231 Pb1 N211 C212 -75.6(4) . . . . ? N223 Pb1 N211 C212 -14.5(4) . . . . ? N111 Pb1 N211 C212 -161.3(4) . . . . ? N243 Pb1 N211 C216 65.6(4) . . . . ? N123 Pb1 N211 C216 -5.1(4) . . . . ? O21S Pb1 N211 C216 -85.6(4) . . . . ? N231 Pb1 N211 C216 120.3(4) . . . . ? N223 Pb1 N211 C216 -178.6(5) . . . . ? N111 Pb1 N211 C216 34.6(5) . . . . ? C216 N211 C212 C213 -1.1(8) . . . . ? Pb1 N211 C212 C213 -165.5(4) . . . . ? C216 N211 C212 C224 178.7(5) . . . . ? Pb1 N211 C212 C224 14.3(6) . . . . ? N211 C212 C213 C214 0.1(9) . . . . ? C224 C212 C213 C214 -179.7(5) . . . . ? C212 C213 C214 C215 0.8(9) . . . . ? C213 C214 C215 C216 -0.6(9) . . . . ? C212 N211 C216 C215 1.4(9) . . . . ? Pb1 N211 C216 C215 165.8(4) . . . . ? C214 C215 C216 N211 -0.5(9) . . . . ? C225 N221 N222 N223 0.1(7) . . . . ? C226 N221 N222 N223 -176.9(5) . . . . ? N221 N222 N223 C224 0.4(6) . . . . ? N221 N222 N223 Pb1 -161.9(4) . . . . ? N243 Pb1 N223 N222 -122.7(5) . . . . ? N123 Pb1 N223 N222 161.0(4) . . . . ? O21S Pb1 N223 N222 108.6(5) . . . . ? N211 Pb1 N223 N222 174.7(6) . . . . ? N231 Pb1 N223 N222 -68.4(5) . . . . ? N111 Pb1 N223 N222 -42.0(6) . . . . ? N243 Pb1 N223 C224 75.9(4) . . . . ? N123 Pb1 N223 C224 -0.5(6) . . . . ? O21S Pb1 N223 C224 -52.8(4) . . . . ? N211 Pb1 N223 C224 13.2(4) . . . . ? N231 Pb1 N223 C224 130.2(4) . . . . ? N111 Pb1 N223 C224 156.5(3) . . . . ? N222 N223 C224 C225 -0.7(7) . . . . ? Pb1 N223 C224 C225 164.9(4) . . . . ? N222 N223 C224 C212 -178.7(5) . . . . ? Pb1 N223 C224 C212 -13.1(7) . . . . ? N211 C212 C224 N223 -0.4(8) . . . . ? C213 C212 C224 N223 179.4(5) . . . . ? N211 C212 C224 C225 -177.8(6) . . . . ? C213 C212 C224 C225 2.0(9) . . . . ? N222 N221 C225 C224 -0.5(6) . . . . ? C226 N221 C225 C224 176.2(5) . . . . ? N223 C224 C225 N221 0.8(6) . . . . ? C212 C224 C225 N221 178.5(5) . . . . ? N222 N221 C226 C251 102.1(6) . . . . ? C225 N221 C226 C251 -74.3(7) . . . . ? N243 Pb1 N231 C232 6.0(2) . . . . ? N123 Pb1 N231 C232 43.2(3) . . . . ? O21S Pb1 N231 C232 -117.1(3) . . . . ? N211 Pb1 N231 C232 -56.6(2) . . . . ? N223 Pb1 N231 C232 -110.5(2) . . . . ? N111 Pb1 N231 C232 84.4(2) . . . . ? N243 Pb1 N231 C236 -178.4(2) . . . . ? N123 Pb1 N231 C236 -141.2(2) . . . . ? O21S Pb1 N231 C236 58.5(3) . . . . ? N211 Pb1 N231 C236 119.0(2) . . . . ? N223 Pb1 N231 C236 65.1(2) . . . . ? N111 Pb1 N231 C236 -100.0(2) . . . . ? C236 N231 C232 C233 0.0 . . . . ? Pb1 N231 C232 C233 175.6(3) . . . . ? C236 N231 C232 C244 179.9(4) . . . . ? Pb1 N231 C232 C244 -4.5(4) . . . . ? N231 C232 C233 C234 0.0 . . . . ? C244 C232 C233 C234 -179.9(5) . . . . ? C232 C233 C234 C235 0.0 . . . . ? C233 C234 C235 C236 0.0 . . . . ? C234 C235 C236 N231 0.0 . . . . ? C232 N231 C236 C235 0.0 . . . . ? Pb1 N231 C236 C235 -175.5(3) . . . . ? C245 N241 N242 N243 -0.7(6) . . . . ? C246 N241 N242 N243 -173.8(4) . . . . ? N241 N242 N243 C244 0.1(6) . . . . ? N241 N242 N243 Pb1 169.7(3) . . . . ? N123 Pb1 N243 N242 35.8(4) . . . . ? O21S Pb1 N243 N242 -25.6(5) . . . . ? N211 Pb1 N243 N242 -60.0(4) . . . . ? N231 Pb1 N243 N242 -176.0(5) . . . . ? N223 Pb1 N243 N242 -114.6(4) . . . . ? N111 Pb1 N243 N242 100.8(4) . . . . ? N123 Pb1 N243 C244 -155.6(4) . . . . ? O21S Pb1 N243 C244 143.0(4) . . . . ? N211 Pb1 N243 C244 108.6(4) . . . . ? N231 Pb1 N243 C244 -7.4(4) . . . . ? N223 Pb1 N243 C244 54.0(4) . . . . ? N111 Pb1 N243 C244 -90.6(4) . . . . ? N242 N243 C244 C245 0.5(6) . . . . ? Pb1 N243 C244 C245 -170.0(4) . . . . ? N242 N243 C244 C232 179.3(5) . . . . ? Pb1 N243 C244 C232 8.9(7) . . . . ? C233 C232 C244 N243 177.3(4) . . . . ? N231 C232 C244 N243 -2.6(7) . . . . ? C233 C232 C244 C245 -4.2(8) . . . . ? N231 C232 C244 C245 176.0(5) . . . . ? N242 N241 C245 C244 1.0(6) . . . . ? C246 N241 C245 C244 173.2(5) . . . . ? N243 C244 C245 N241 -0.9(6) . . . . ? C232 C244 C245 N241 -179.6(5) . . . . ? C245 N241 C246 C253 -81.7(7) . . . . ? N242 N241 C246 C253 90.0(6) . . . . ? N221 C226 C251 C256 -76.7(6) . . . . ? N221 C226 C251 C252 101.0(5) . . . . ? C256 C251 C252 C253 1.2(7) . . . 2_666 ? C226 C251 C252 C253 -176.5(5) . . . 2_666 ? N241 C246 C253 C254 -81.7(6) . . . . ? N241 C246 C253 C252 96.4(6) . . . 2_666 ? C252 C253 C254 C255 -4.0(8) 2_666 . . . ? C246 C253 C254 C255 174.1(5) . . . . ? C253 C254 C255 C256 3.0(8) . . . 2_666 ? C252 C251 C256 C255 -0.1(8) . . . 2_666 ? C226 C251 C256 C255 177.6(5) . . . 2_666 ? N343 Pb2 N311 C316 -61.2(4) . . . . ? O11S Pb2 N311 C316 101.1(5) . . . . ? N143 Pb2 N311 C316 13.1(4) . . . . ? N331 Pb2 N311 C316 -116.0(4) . . . . ? N323 Pb2 N311 C316 -179.1(5) . . . . ? N131 Pb2 N311 C316 -25.7(5) . . . . ? N343 Pb2 N311 C312 132.6(4) . . . . ? O11S Pb2 N311 C312 -65.1(4) . . . . ? N143 Pb2 N311 C312 -153.1(4) . . . . ? N331 Pb2 N311 C312 77.7(4) . . . . ? N323 Pb2 N311 C312 14.6(4) . . . . ? N131 Pb2 N311 C312 168.1(4) . . . . ? C316 N311 C312 C313 1.5(9) . . . . ? Pb2 N311 C312 C313 168.2(5) . . . . ? C316 N311 C312 C324 -179.7(5) . . . . ? Pb2 N311 C312 C324 -13.0(7) . . . . ? N311 C312 C313 C314 -1.6(10) . . . . ? C324 C312 C313 C314 179.6(6) . . . . ? C312 C313 C314 C315 0.2(10) . . . . ? C313 C314 C315 C316 1.3(10) . . . . ? C312 N311 C316 C315 0.1(9) . . . . ? Pb2 N311 C316 C315 -166.3(5) . . . . ? C314 C315 C316 N311 -1.5(10) . . . . ? C325 N321 N322 N323 0.7(7) . . . . ? C326 N321 N322 N323 175.7(5) . . . . ? N321 N322 N323 C324 -0.6(7) . . . . ? N321 N322 N323 Pb2 158.0(4) . . . . ? N343 Pb2 N323 N322 126.2(5) . . . . ? O11S Pb2 N323 N322 -98.6(5) . . . . ? N143 Pb2 N323 N322 -150.2(4) . . . . ? N331 Pb2 N323 N322 70.6(5) . . . . ? N311 Pb2 N323 N322 -172.6(6) . . . . ? N131 Pb2 N323 N322 46.5(7) . . . . ? N343 Pb2 N323 C324 -76.2(4) . . . . ? O11S Pb2 N323 C324 59.0(4) . . . . ? N143 Pb2 N323 C324 7.4(6) . . . . ? N331 Pb2 N323 C324 -131.8(4) . . . . ? N311 Pb2 N323 C324 -15.0(4) . . . . ? N131 Pb2 N323 C324 -155.9(4) . . . . ? N322 N323 C324 C325 0.3(7) . . . . ? Pb2 N323 C324 C325 -161.8(4) . . . . ? N322 N323 C324 C312 178.4(5) . . . . ? Pb2 N323 C324 C312 16.4(7) . . . . ? N311 C312 C324 N323 -2.6(8) . . . . ? C313 C312 C324 N323 176.3(6) . . . . ? N311 C312 C324 C325 175.1(6) . . . . ? C313 C312 C324 C325 -6.0(10) . . . . ? N322 N321 C325 C324 -0.6(7) . . . . ? C326 N321 C325 C324 -174.9(5) . . . . ? N323 C324 C325 N321 0.2(7) . . . . ? C312 C324 C325 N321 -177.8(6) . . . . ? C325 N321 C326 C351 75.3(7) . . . 2_677 ? N322 N321 C326 C351 -98.8(6) . . . 2_677 ? N343 Pb2 N331 C332 -6.7(2) . . . . ? O11S Pb2 N331 C332 127.4(3) . . . . ? N143 Pb2 N331 C332 -42.6(3) . . . . ? N323 Pb2 N331 C332 109.8(2) . . . . ? N311 Pb2 N331 C332 54.9(2) . . . . ? N131 Pb2 N331 C332 -81.7(2) . . . . ? N343 Pb2 N331 C336 179.0(3) . . . . ? O11S Pb2 N331 C336 -47.0(3) . . . . ? N143 Pb2 N331 C336 143.1(2) . . . . ? N323 Pb2 N331 C336 -64.5(2) . . . . ? N311 Pb2 N331 C336 -119.4(2) . . . . ? N131 Pb2 N331 C336 104.0(2) . . . . ? C336 N331 C332 C333 0.0 . . . . ? Pb2 N331 C332 C333 -174.3(3) . . . . ? C336 N331 C332 C344 178.7(4) . . . . ? Pb2 N331 C332 C344 4.4(4) . . . . ? N331 C332 C333 C334 0.0 . . . . ? C344 C332 C333 C334 -178.6(5) . . . . ? C332 C333 C334 C335 0.0 . . . . ? C333 C334 C335 C336 0.0 . . . . ? C334 C335 C336 N331 0.0 . . . . ? C332 N331 C336 C335 0.0 . . . . ? Pb2 N331 C336 C335 174.3(3) . . . . ? C345 N341 N342 N343 1.0(6) . . . . ? C346 N341 N342 N343 174.2(5) . . . . ? N341 N342 N343 C344 -0.6(6) . . . . ? N341 N342 N343 Pb2 -166.4(3) . . . . ? O11S Pb2 N343 N342 31.5(6) . . . . ? N143 Pb2 N343 N342 -35.1(4) . . . . ? N331 Pb2 N343 N342 173.4(5) . . . . ? N323 Pb2 N343 N342 109.9(5) . . . . ? N311 Pb2 N343 N342 55.9(4) . . . . ? N131 Pb2 N343 N342 -99.8(5) . . . . ? O11S Pb2 N343 C344 -133.3(4) . . . . ? N143 Pb2 N343 C344 160.1(4) . . . . ? N331 Pb2 N343 C344 8.6(4) . . . . ? N323 Pb2 N343 C344 -54.9(4) . . . . ? N311 Pb2 N343 C344 -108.9(4) . . . . ? N131 Pb2 N343 C344 95.4(4) . . . . ? N342 N343 C344 C345 0.1(7) . . . . ? Pb2 N343 C344 C345 167.9(4) . . . . ? N342 N343 C344 C332 -178.8(5) . . . . ? Pb2 N343 C344 C332 -10.9(7) . . . . ? N331 C332 C344 N343 4.3(7) . . . . ? C333 C332 C344 N343 -177.0(4) . . . . ? N331 C332 C344 C345 -174.2(6) . . . . ? C333 C332 C344 C345 4.4(8) . . . . ? N342 N341 C345 C344 -0.9(7) . . . . ? C346 N341 C345 C344 -173.5(5) . . . . ? N343 C344 C345 N341 0.5(7) . . . . ? C332 C344 C345 N341 179.3(6) . . . . ? C345 N341 C346 C353 80.7(7) . . . . ? N342 N341 C346 C353 -91.3(6) . . . . ? C356 C351 C352 C353 3.3(8) . . . . ? C326 C351 C352 C353 -174.9(5) 2_677 . . . ? C351 C352 C353 C354 -2.9(8) . . . . ? C351 C352 C353 C346 175.8(5) . . . . ? N341 C346 C353 C352 -98.2(6) . . . . ? N341 C346 C353 C354 80.4(6) . . . . ? C352 C353 C354 C355 0.6(8) . . . . ? C346 C353 C354 C355 -178.1(5) . . . . ? C353 C354 C355 C356 1.1(8) . . . . ? C354 C355 C356 C351 -0.7(9) . . . . ? C352 C351 C356 C355 -1.5(8) . . . . ? C326 C351 C356 C355 176.8(5) 2_677 . . . ? N343 Pb2 O11S C13S -96.5(6) . . . . ? N143 Pb2 O11S C13S -34.4(6) . . . . ? N331 Pb2 O11S C13S 153.4(5) . . . . ? N323 Pb2 O11S C13S 171.3(6) . . . . ? N311 Pb2 O11S C13S -121.8(6) . . . . ? N131 Pb2 O11S C13S 12.6(6) . . . . ? Pb2 O11S C13S N12S 127.0(7) . . . . ? C14S N12S C13S O11S 177.3(7) . . . . ? C15S N12S C13S O11S -3.8(12) . . . . ? N243 Pb1 O21S C23S 144.7(8) . . . . ? N123 Pb1 O21S C23S 87.3(9) . . . . ? N211 Pb1 O21S C23S -178.4(9) . . . . ? N231 Pb1 O21S C23S -109.1(9) . . . . ? N223 Pb1 O21S C23S -115.4(9) . . . . ? N111 Pb1 O21S C23S 44.0(9) . . . . ? Pb1 O21S C23S N22S -170.7(5) . . . . ? C25S N22S C23S O21S -2.9(10) . . . . ? C24S N22S C23S O21S -178.6(6) . . . . ? C44S N42S C43S O41S 171.9(4) . . . . ? C45S N42S C43S O41S 3.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 27.69 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 2.733 _refine_diff_density_min -2.320 _refine_diff_density_rms 0.155 #===END data_imw1381p-1 _database_code_depnum_ccdc_archive 'CCDC 778861' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H36 Cl2 N16 O8 Pb' _chemical_formula_weight 1194.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.2078(5) _cell_length_b 15.0213(6) _cell_length_c 15.6798(6) _cell_angle_alpha 117.794(2) _cell_angle_beta 90.479(2) _cell_angle_gamma 116.858(2) _cell_volume 2537.23(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8614 _cell_measurement_theta_min 2.560 _cell_measurement_theta_max 22.833 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 3.497 _exptl_absorpt_correction_type Multi-Scan _exptl_absorpt_correction_T_min 0.4634 _exptl_absorpt_correction_T_max 0.5718 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30572 _diffrn_reflns_av_R_equivalents 0.0424 _diffrn_reflns_av_sigmaI/netI 0.0468 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.53 _diffrn_reflns_theta_max 24.71 _reflns_number_total 8649 _reflns_number_gt 7429 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a {[Pb(L)2](ClO4)}n coordination polymer. The structure has been solved by direct methods. Data processing was conducted to a resolution of 0.85 angstroms as the data was only complete to this resolution. Two disordered perchlorate anions exist in the lattice (Cl1 > O15 and Cl2 > O25; 80:20 and 65:35 respectively. These are fully disordered over two sites and have benefitted from the application of geometric and displacement restraints. Global displacement restrints have been applied to carbon and nitrogen atoms and all five and six membered rings have been idealised. A Platon SQUEEZE function was used to eleiminat two regions of highly disordered solvent molecules that could not be satisfactorily modelled: 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 0.500 1.000 0.500 81 29 ' ' 2 0.500 0.500 1.000 264 119 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0394P)^2^+68.2211P] 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 8649 _refine_ls_number_parameters 549 _refine_ls_number_restraints 743 _refine_ls_R_factor_all 0.1093 _refine_ls_R_factor_gt 0.0976 _refine_ls_wR_factor_ref 0.2245 _refine_ls_wR_factor_gt 0.2187 _refine_ls_goodness_of_fit_ref 1.167 _refine_ls_restrained_S_all 1.136 _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 0.45793(5) 0.14605(6) 0.32102(4) 0.0479(2) Uani 1 1 d . . . N111 N 0.5845(6) 0.1838(7) 0.1969(5) 0.046(3) Uani 1 1 d GU . . C112 C 0.5330(4) 0.1485(7) 0.1018(5) 0.040(3) Uani 1 1 d GDU . . C113 C 0.5950(6) 0.1849(8) 0.0442(5) 0.045(3) Uani 1 1 d GU . . H113 H 0.5598 0.1608 -0.0208 0.054 Uiso 1 1 calc R . . C114 C 0.7086(6) 0.2566(8) 0.0815(6) 0.050(3) Uani 1 1 d GU . . H114 H 0.7509 0.2815 0.0421 0.060 Uiso 1 1 calc R . . C115 C 0.7601(4) 0.2919(8) 0.1766(6) 0.057(4) Uani 1 1 d GU . . H115 H 0.8377 0.3409 0.2021 0.068 Uiso 1 1 calc R . . C116 C 0.6981(6) 0.2555(8) 0.2342(5) 0.058(4) Uani 1 1 d GU . . H116 H 0.7333 0.2796 0.2992 0.069 Uiso 1 1 calc R . . N121 N 0.2362(4) -0.0417(7) -0.0102(5) 0.037(2) Uani 1 1 d GU . . N122 N 0.2517(5) -0.0348(6) 0.0828(5) 0.036(2) Uani 1 1 d GU . . N123 N 0.3656(5) 0.0397(7) 0.1334(4) 0.037(2) Uani 1 1 d GU . . C124 C 0.4206(4) 0.0788(7) 0.0718(6) 0.035(2) Uani 1 1 d GDU . . C125 C 0.3406(6) 0.0285(7) -0.0170(5) 0.035(3) Uani 1 1 d GU . . H125 H 0.3544 0.0399 -0.0713 0.042 Uiso 1 1 calc R . . C126 C 0.1294(9) -0.1099(12) -0.0734(10) 0.040(3) Uani 1 1 d U . . H12A H 0.0919 -0.1869 -0.0787 0.048 Uiso 1 1 calc R . . H12B H 0.1327 -0.1243 -0.1413 0.048 Uiso 1 1 calc R . . C131 C 0.0643(10) -0.0509(12) -0.0350(10) 0.037(2) Uani 1 1 d U . . C132 C 0.0802(11) 0.0417(12) -0.0425(11) 0.045(3) Uani 1 1 d U . . H132 H 0.1350 0.0707 -0.0722 0.054 Uiso 1 1 calc R . . C133 C -0.0182(10) -0.0949(12) 0.0077(10) 0.041(3) Uani 1 1 d U . . H133 H -0.0315 -0.1599 0.0127 0.050 Uiso 1 1 calc R . . N211 N 0.4508(6) -0.0567(5) 0.2441(6) 0.033(2) Uani 1 1 d GU . . C212 C 0.3496(4) -0.1607(6) 0.1992(7) 0.040(3) Uani 1 1 d GDU . . C213 C 0.3440(5) -0.2679(5) 0.1435(7) 0.052(3) Uani 1 1 d GU . . H213 H 0.2749 -0.3390 0.1128 0.063 Uiso 1 1 calc R . . C214 C 0.4397(7) -0.2710(5) 0.1327(8) 0.061(4) Uani 1 1 d GU . . H214 H 0.4359 -0.3442 0.0946 0.074 Uiso 1 1 calc R . . C215 C 0.5409(5) -0.1670(7) 0.1776(8) 0.058(4) Uani 1 1 d GU . . H215 H 0.6063 -0.1691 0.1702 0.069 Uiso 1 1 calc R . . C216 C 0.5465(4) -0.0599(6) 0.2333(7) 0.043(3) Uani 1 1 d GU . . H216 H 0.6157 0.0112 0.2640 0.052 Uiso 1 1 calc R . . N221 N 0.0873(4) -0.1755(7) 0.2112(6) 0.043(2) Uani 1 1 d GU . . N222 N 0.1653(6) -0.0542(6) 0.2769(6) 0.047(3) Uani 1 1 d GU . . N223 N 0.2719(5) -0.0383(6) 0.2787(6) 0.045(3) Uani 1 1 d GU . . C224 C 0.2597(5) -0.1498(7) 0.2140(7) 0.037(3) Uani 1 1 d GDU . . C225 C 0.1457(6) -0.2346(5) 0.1723(6) 0.038(3) Uani 1 1 d GU . . H225 H 0.1140 -0.3166 0.1265 0.046 Uiso 1 1 calc R . . C226 C -0.0250(11) -0.2173(14) 0.1983(11) 0.046(3) Uani 1 1 d U . . H22A H -0.0661 -0.2876 0.1300 0.056 Uiso 1 1 calc R . . H22B H -0.0398 -0.1565 0.2045 0.056 Uiso 1 1 calc R . . C231 C -0.0644(11) -0.2484(12) 0.2737(10) 0.042(3) Uani 1 1 d U . . C232 C -0.1181(14) -0.3629(14) 0.2501(12) 0.062(4) Uani 1 1 d U . . H232 H -0.1290 -0.4235 0.1848 0.074 Uiso 1 1 calc R . . C233 C -0.0450(13) -0.1660(14) 0.3687(12) 0.064(4) Uani 1 1 d U . . H233 H -0.0025 -0.0856 0.3894 0.077 Uiso 1 1 calc R . . N311 N 0.3563(6) 0.2626(7) 0.3133(6) 0.044(2) Uani 1 1 d GU . . C312 C 0.4163(5) 0.3804(7) 0.3434(6) 0.043(3) Uani 1 1 d GDU . . C313 C 0.3641(7) 0.4326(6) 0.3274(8) 0.056(3) Uani 1 1 d GU . . H313 H 0.4051 0.5131 0.3480 0.067 Uiso 1 1 calc R . . C314 C 0.2519(7) 0.3670(8) 0.2814(8) 0.060(4) Uani 1 1 d GU . . H314 H 0.2162 0.4027 0.2705 0.073 Uiso 1 1 calc R . . C315 C 0.1918(5) 0.2492(8) 0.2514(7) 0.057(3) Uani 1 1 d GU . . H315 H 0.1151 0.2044 0.2199 0.068 Uiso 1 1 calc R . . C316 C 0.2440(6) 0.1970(6) 0.2673(7) 0.047(3) Uani 1 1 d GU . . H316 H 0.2030 0.1165 0.2467 0.056 Uiso 1 1 calc R . . N321 N 0.7125(5) 0.5703(6) 0.4557(7) 0.050(3) Uani 1 1 d GU . . N322 N 0.6917(6) 0.4641(7) 0.4468(6) 0.049(3) Uani 1 1 d GU . . N323 N 0.5772(6) 0.3820(6) 0.4043(7) 0.048(3) Uani 1 1 d GU . . C324 C 0.5271(5) 0.4374(8) 0.3868(7) 0.043(3) Uani 1 1 d GDU . . C325 C 0.6107(7) 0.5537(7) 0.4186(7) 0.050(3) Uani 1 1 d GU . . H325 H 0.6004 0.6106 0.4156 0.060 Uiso 1 1 calc R . . C326 C 0.8188(12) 0.6628(15) 0.4934(12) 0.057(4) Uani 1 1 d U . . H32A H 0.8673 0.6434 0.5173 0.068 Uiso 1 1 calc R . . H32B H 0.8237 0.7329 0.5514 0.068 Uiso 1 1 calc R . . C331 C 0.8580(12) 0.6907(13) 0.4141(11) 0.048(3) Uani 1 1 d U . . C332 C 0.9138(13) 0.8042(14) 0.4389(12) 0.062(4) Uani 1 1 d U . . H332 H 0.9254 0.8646 0.5046 0.075 Uiso 1 1 calc R . . C333 C 0.8432(15) 0.6087(14) 0.3207(13) 0.065(4) Uani 1 1 d U . . H333 H 0.8052 0.5287 0.3018 0.078 Uiso 1 1 calc R . . N411 N 0.4258(10) 0.1790(12) 0.5072(7) 0.087(4) Uani 1 1 d GU . . C412 C 0.5221(8) 0.2529(13) 0.5852(9) 0.088(5) Uani 1 1 d GDU . . C413 C 0.5182(9) 0.3054(12) 0.6841(8) 0.096(5) Uani 1 1 d GU . . H413 H 0.5840 0.3559 0.7374 0.115 Uiso 1 1 calc R . . C414 C 0.4180(12) 0.2840(13) 0.7051(7) 0.101(5) Uani 1 1 d GU . . H414 H 0.4153 0.3199 0.7727 0.122 Uiso 1 1 calc R . . C415 C 0.3217(9) 0.2101(14) 0.6272(10) 0.098(5) Uani 1 1 d GU . . H415 H 0.2532 0.1955 0.6415 0.118 Uiso 1 1 calc R . . C416 C 0.3256(8) 0.1576(12) 0.5282(9) 0.091(5) Uani 1 1 d GU . . H416 H 0.2598 0.1071 0.4750 0.109 Uiso 1 1 calc R . . N421 N 0.7849(7) 0.2884(11) 0.5455(8) 0.078(4) Uani 1 1 d GU . . N422 N 0.7169(8) 0.2206(11) 0.4458(6) 0.084(4) Uani 1 1 d GU . . N423 N 0.6102(7) 0.2016(11) 0.4507(7) 0.086(4) Uani 1 1 d GU . . C424 C 0.6123(8) 0.2576(13) 0.5534(9) 0.081(4) Uani 1 1 d GDU . . C425 C 0.7203(10) 0.3113(12) 0.6120(6) 0.077(4) Uani 1 1 d GU . . H425 H 0.7450 0.3548 0.6832 0.093 Uiso 1 1 calc R . . C426 C 0.8954(16) 0.325(2) 0.5622(17) 0.094(5) Uani 1 1 d U . . H42A H 0.9050 0.2570 0.5229 0.112 Uiso 1 1 calc R . . H42B H 0.9293 0.3617 0.6342 0.112 Uiso 1 1 calc R . . C431 C 0.9542(18) 0.421(2) 0.5276(18) 0.097(5) Uani 1 1 d U . . C432 C 0.9898(17) 0.539(2) 0.5944(17) 0.092(5) Uani 1 1 d U . . H432 H 0.9816 0.5633 0.6603 0.110 Uiso 1 1 calc R . . C433 C 0.9650(16) 0.383(2) 0.4327(17) 0.090(5) Uani 1 1 d U . . H433 H 0.9410 0.3024 0.3871 0.108 Uiso 1 1 calc R . . Cl1X Cl 0.8596(4) 0.0142(5) 0.2932(3) 0.0468(14) Uiso 0.805(14) 1 d PDU A 1 O12X O 0.8081(9) -0.1107(7) 0.2225(7) 0.054(3) Uiso 0.805(14) 1 d PDU A 1 O13X O 0.8432(10) 0.0352(11) 0.3892(7) 0.075(4) Uiso 0.805(14) 1 d PDU A 1 O14X O 0.9753(7) 0.0689(10) 0.3009(9) 0.076(4) Uiso 0.805(14) 1 d PDU A 1 O15X O 0.8114(11) 0.0609(11) 0.2572(10) 0.074(5) Uiso 0.805(14) 1 d PDU A 1 Cl1Y Cl 0.8764(15) 0.055(2) 0.2927(13) 0.046(5) Uiso 0.195(14) 1 d PDU A 2 O12Y O 0.975(2) 0.097(4) 0.263(3) 0.071(14) Uiso 0.195(14) 1 d PDU A 2 O13Y O 0.897(4) 0.135(4) 0.3975(16) 0.077(13) Uiso 0.195(14) 1 d PDU A 2 O14Y O 0.843(4) -0.059(3) 0.276(4) 0.078(12) Uiso 0.195(14) 1 d PDU A 2 O15Y O 0.791(3) 0.047(4) 0.234(3) 0.054(12) Uiso 0.195(14) 1 d PDU A 2 Cl2X Cl 0.0630(5) 0.4434(6) 0.1011(5) 0.0506(19) Uiso 0.654(15) 1 d PDU B 1 O22X O -0.0452(10) 0.3428(12) 0.0551(13) 0.106(7) Uiso 0.654(15) 1 d PDU B 1 O23X O 0.1372(14) 0.4167(18) 0.1328(15) 0.136(9) Uiso 0.654(15) 1 d PDU B 1 O24X O 0.0650(17) 0.5399(13) 0.1866(10) 0.104(7) Uiso 0.654(15) 1 d PDU B 1 O25X O 0.0996(12) 0.4763(13) 0.0293(10) 0.069(5) Uiso 0.654(15) 1 d PDU B 1 Cl2Y Cl 0.0688(10) 0.4378(11) 0.1237(10) 0.055(4) Uiso 0.346(15) 1 d PDU B 2 O22Y O 0.072(3) 0.400(3) 0.1929(18) 0.091(11) Uiso 0.346(15) 1 d PDU B 2 O23Y O 0.007(2) 0.3348(18) 0.0246(13) 0.071(9) Uiso 0.346(15) 1 d PDU B 2 O24Y O 0.015(3) 0.505(3) 0.154(2) 0.117(12) Uiso 0.346(15) 1 d PDU B 2 O25Y O 0.1784(15) 0.507(3) 0.123(3) 0.132(12) Uiso 0.346(15) 1 d PDU B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0556(4) 0.0605(4) 0.0330(3) 0.0165(2) 0.0135(2) 0.0421(3) N111 0.024(5) 0.054(6) 0.035(5) 0.009(5) 0.002(4) 0.018(4) C112 0.021(5) 0.037(5) 0.040(5) 0.007(4) 0.003(4) 0.014(4) C113 0.024(5) 0.035(6) 0.048(6) 0.013(5) 0.001(5) 0.005(5) C114 0.026(6) 0.040(6) 0.057(7) 0.014(6) 0.007(5) 0.010(5) C115 0.032(6) 0.049(7) 0.050(6) 0.000(6) 0.002(5) 0.020(5) C116 0.024(6) 0.063(7) 0.039(6) 0.000(6) -0.001(5) 0.017(5) N121 0.021(4) 0.039(5) 0.046(5) 0.020(4) 0.011(4) 0.014(4) N122 0.023(4) 0.040(5) 0.042(5) 0.020(4) 0.010(4) 0.016(4) N123 0.021(4) 0.044(5) 0.037(5) 0.016(4) 0.006(4) 0.016(4) C124 0.023(5) 0.039(5) 0.034(5) 0.015(4) 0.005(4) 0.015(4) C125 0.020(5) 0.040(6) 0.041(6) 0.020(5) 0.008(4) 0.013(4) C126 0.016(5) 0.043(6) 0.047(6) 0.020(5) 0.007(4) 0.009(4) C131 0.020(5) 0.043(5) 0.045(6) 0.025(5) 0.010(4) 0.014(4) C132 0.031(6) 0.044(7) 0.057(7) 0.030(6) 0.020(6) 0.013(6) C133 0.026(6) 0.040(7) 0.053(7) 0.029(6) 0.011(5) 0.010(5) N211 0.022(4) 0.029(5) 0.037(5) 0.016(4) 0.006(4) 0.008(4) C212 0.021(5) 0.043(5) 0.047(6) 0.022(5) 0.002(4) 0.012(4) C213 0.028(6) 0.038(6) 0.074(8) 0.026(6) 0.011(6) 0.009(5) C214 0.041(6) 0.040(6) 0.087(8) 0.023(6) 0.015(6) 0.021(5) C215 0.040(6) 0.036(6) 0.081(8) 0.021(6) 0.010(6) 0.018(5) C216 0.027(5) 0.037(6) 0.054(7) 0.020(5) 0.003(5) 0.012(5) N221 0.030(5) 0.052(5) 0.054(5) 0.036(4) 0.020(4) 0.017(4) N222 0.028(5) 0.056(6) 0.057(6) 0.030(5) 0.019(4) 0.021(4) N223 0.028(5) 0.056(6) 0.052(6) 0.030(5) 0.018(4) 0.021(4) C224 0.023(5) 0.049(5) 0.043(5) 0.029(5) 0.008(4) 0.016(4) C225 0.022(5) 0.051(6) 0.048(6) 0.034(5) 0.016(5) 0.015(5) C226 0.030(5) 0.059(7) 0.054(6) 0.034(5) 0.018(5) 0.021(5) C231 0.033(6) 0.047(6) 0.048(6) 0.026(5) 0.021(5) 0.020(5) C232 0.072(9) 0.045(7) 0.052(8) 0.022(6) 0.032(7) 0.021(7) C233 0.050(8) 0.042(7) 0.055(7) 0.017(6) 0.015(7) 0.000(7) N311 0.049(6) 0.046(5) 0.035(5) 0.015(5) 0.007(4) 0.031(5) C312 0.047(6) 0.051(5) 0.037(5) 0.023(5) 0.016(5) 0.029(5) C313 0.058(7) 0.056(7) 0.061(7) 0.034(6) 0.015(6) 0.031(6) C314 0.057(7) 0.061(7) 0.064(8) 0.033(6) 0.010(6) 0.031(6) C315 0.049(7) 0.061(7) 0.048(7) 0.022(6) 0.006(6) 0.027(6) C316 0.047(6) 0.048(6) 0.037(6) 0.016(5) 0.006(5) 0.025(5) N321 0.040(5) 0.063(6) 0.043(5) 0.034(5) 0.013(4) 0.018(4) N322 0.033(5) 0.054(6) 0.046(6) 0.020(5) 0.011(5) 0.019(5) N323 0.041(5) 0.054(6) 0.039(5) 0.018(5) 0.011(4) 0.025(5) C324 0.039(5) 0.050(6) 0.036(5) 0.022(5) 0.015(5) 0.023(4) C325 0.038(6) 0.062(7) 0.050(6) 0.036(6) 0.016(5) 0.019(5) C326 0.036(6) 0.065(7) 0.056(7) 0.037(6) 0.013(5) 0.010(5) C331 0.041(6) 0.049(6) 0.048(6) 0.027(5) 0.014(5) 0.017(5) C332 0.048(8) 0.045(7) 0.045(7) 0.015(6) 0.014(6) -0.002(6) C333 0.072(9) 0.043(7) 0.063(8) 0.026(6) 0.035(7) 0.020(7) N411 0.070(6) 0.107(8) 0.068(7) 0.034(6) 0.020(5) 0.046(6) C412 0.074(6) 0.097(7) 0.078(7) 0.038(6) 0.029(5) 0.042(6) C413 0.089(8) 0.106(8) 0.083(7) 0.049(7) 0.034(6) 0.044(7) C414 0.096(8) 0.115(9) 0.088(8) 0.056(7) 0.037(6) 0.048(7) C415 0.091(8) 0.105(9) 0.090(8) 0.052(7) 0.037(6) 0.044(7) C416 0.082(7) 0.100(8) 0.078(7) 0.049(6) 0.030(6) 0.037(7) N421 0.054(5) 0.093(7) 0.063(6) 0.023(5) 0.011(5) 0.039(5) N422 0.054(6) 0.079(7) 0.064(6) 0.011(5) 0.037(5) 0.021(5) N423 0.072(6) 0.082(7) 0.073(6) 0.025(6) 0.018(6) 0.035(6) C424 0.068(6) 0.088(7) 0.070(6) 0.038(6) 0.028(5) 0.033(6) C425 0.061(6) 0.090(8) 0.062(7) 0.031(6) 0.019(5) 0.034(6) C426 0.058(7) 0.103(8) 0.086(8) 0.033(6) 0.005(6) 0.035(6) C431 0.066(7) 0.105(8) 0.086(7) 0.035(6) 0.014(6) 0.036(6) C432 0.068(9) 0.099(9) 0.084(9) 0.042(7) 0.014(7) 0.033(7) C433 0.055(8) 0.107(10) 0.084(8) 0.037(7) 0.015(7) 0.037(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N423 2.495(9) . ? Pb1 N123 2.566(5) . ? Pb1 N223 2.596(6) . ? Pb1 N211 2.653(6) . ? Pb1 N323 2.713(6) . ? Pb1 N111 2.741(6) . ? Pb1 N311 2.766(6) . ? Pb1 N411 2.803(9) . ? N111 C112 1.3900 . ? N111 C116 1.3900 . ? C112 C124 1.373(7) . ? C112 C113 1.3900 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C126 1.399(13) . ? N121 N122 1.4200 . ? N121 C125 1.4200 . ? N122 N123 1.4200 . ? N123 C124 1.4200 . ? C124 C125 1.4200 . ? C125 H125 0.9500 . ? C126 C131 1.503(17) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.367(19) . ? C131 C133 1.409(18) . ? C132 C133 1.395(19) 2 ? C132 H132 0.9500 . ? C133 C132 1.395(19) 2 ? C133 H133 0.9500 . ? N211 C212 1.3900 . ? N211 C216 1.3900 . ? C212 C224 1.367(7) . ? C212 C213 1.3900 . ? C213 C214 1.3900 . ? C213 H213 0.9500 . ? C214 C215 1.3900 . ? C214 H214 0.9500 . ? C215 C216 1.3900 . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C226 1.397(14) . ? N221 N222 1.4200 . ? N221 C225 1.4200 . ? N222 N223 1.4200 . ? N223 C224 1.4200 . ? C224 C225 1.4200 . ? C225 H225 0.9500 . ? C226 C231 1.489(19) . ? C226 H22A 0.9900 . ? C226 H22B 0.9900 . ? C231 C233 1.34(2) . ? C231 C232 1.38(2) . ? C232 C333 1.40(2) 1_445 ? C232 H232 0.9500 . ? C233 C332 1.41(2) 1_445 ? C233 H233 0.9500 . ? N311 C312 1.3900 . ? N311 C316 1.3900 . ? C312 C324 1.377(8) . ? C312 C313 1.3900 . ? C313 C314 1.3900 . ? C313 H313 0.9500 . ? C314 C315 1.3900 . ? C314 H314 0.9500 . ? C315 C316 1.3900 . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 C326 1.373(15) . ? N321 N322 1.4200 . ? N321 C325 1.4200 . ? N322 N323 1.4200 . ? N323 C324 1.4200 . ? C324 C325 1.4200 . ? C325 H325 0.9500 . ? C326 C331 1.52(2) . ? C326 H32A 0.9900 . ? C326 H32B 0.9900 . ? C331 C333 1.34(2) . ? C331 C332 1.36(2) . ? C332 C233 1.41(2) 1_665 ? C332 H332 0.9500 . ? C333 C232 1.40(2) 1_665 ? C333 H333 0.9500 . ? N411 C412 1.3900 . ? N411 C416 1.3900 . ? C412 C424 1.363(10) . ? C412 C413 1.3900 . ? C413 C414 1.3900 . ? C413 H413 0.9500 . ? C414 C415 1.3900 . ? C414 H414 0.9500 . ? C415 C416 1.3900 . ? C415 H415 0.9500 . ? C416 H416 0.9500 . ? N421 C426 1.38(2) . ? N421 N422 1.4200 . ? N421 C425 1.4200 . ? N422 N423 1.4200 . ? N423 C424 1.4200 . ? C424 C425 1.4200 . ? C425 H425 0.9500 . ? C426 C431 1.65(3) . ? C426 H42A 0.9900 . ? C426 H42B 0.9900 . ? C431 C433 1.36(3) . ? C431 C432 1.39(3) . ? C432 C433 1.33(3) 2_766 ? C432 H432 0.9500 . ? C433 C432 1.33(3) 2_766 ? C433 H433 0.9500 . ? Cl1X O13X 1.430(8) . ? Cl1X O15X 1.440(8) . ? Cl1X O14X 1.441(8) . ? Cl1X O12X 1.446(8) . ? Cl1Y O15Y 1.435(10) . ? Cl1Y O12Y 1.439(10) . ? Cl1Y O13Y 1.439(10) . ? Cl1Y O14Y 1.444(10) . ? Cl2X O22X 1.426(9) . ? Cl2X O24X 1.432(9) . ? Cl2X O23X 1.440(9) . ? Cl2X O25X 1.442(9) . ? Cl2Y O25Y 1.432(10) . ? Cl2Y O24Y 1.433(10) . ? Cl2Y O23Y 1.445(10) . ? Cl2Y O22Y 1.447(10) . ? 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 N423 Pb1 N123 146.8(3) . . ? N423 Pb1 N223 115.0(4) . . ? N123 Pb1 N223 73.2(3) . . ? N423 Pb1 N211 79.7(3) . . ? N123 Pb1 N211 76.6(3) . . ? N223 Pb1 N211 62.2(2) . . ? N423 Pb1 N323 79.3(4) . . ? N123 Pb1 N323 111.2(3) . . ? N223 Pb1 N323 148.2(2) . . ? N211 Pb1 N323 149.2(2) . . ? N423 Pb1 N111 95.0(3) . . ? N123 Pb1 N111 60.7(2) . . ? N223 Pb1 N111 129.0(2) . . ? N211 Pb1 N111 86.0(3) . . ? N323 Pb1 N111 73.7(3) . . ? N423 Pb1 N311 132.5(3) . . ? N123 Pb1 N311 76.0(2) . . ? N223 Pb1 N311 92.3(2) . . ? N211 Pb1 N311 147.0(2) . . ? N323 Pb1 N311 60.2(2) . . ? N111 Pb1 N311 96.2(3) . . ? N423 Pb1 N411 60.9(4) . . ? N123 Pb1 N411 145.7(3) . . ? N223 Pb1 N411 74.8(3) . . ? N211 Pb1 N411 99.0(3) . . ? N323 Pb1 N411 90.1(3) . . ? N111 Pb1 N411 153.6(3) . . ? N311 Pb1 N411 93.4(3) . . ? C112 N111 C116 120.0 . . ? C112 N111 Pb1 118.6(4) . . ? C116 N111 Pb1 120.3(4) . . ? C124 C112 N111 115.8(6) . . ? C124 C112 C113 124.2(6) . . ? N111 C112 C113 120.0 . . ? C114 C113 C112 120.0 . . ? C114 C113 H113 120.0 . . ? C112 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C114 C115 C116 120.0 . . ? C114 C115 H115 120.0 . . ? C116 C115 H115 120.0 . . ? C115 C116 N111 120.0 . . ? C115 C116 H116 120.0 . . ? N111 C116 H116 120.0 . . ? C126 N121 N122 118.5(8) . . ? C126 N121 C125 133.5(8) . . ? N122 N121 C125 108.0 . . ? N121 N122 N123 108.0 . . ? C124 N123 N122 108.0 . . ? C124 N123 Pb1 121.2(4) . . ? N122 N123 Pb1 127.9(4) . . ? C112 C124 C125 132.2(6) . . ? C112 C124 N123 119.7(6) . . ? C125 C124 N123 108.0 . . ? C124 C125 N121 108.0 . . ? C124 C125 H125 126.0 . . ? N121 C125 H125 126.0 . . ? N121 C126 C131 111.6(11) . . ? N121 C126 H12A 109.3 . . ? C131 C126 H12A 109.3 . . ? N121 C126 H12B 109.3 . . ? C131 C126 H12B 109.3 . . ? H12A C126 H12B 108.0 . . ? C132 C131 C133 118.9(12) . . ? C132 C131 C126 122.5(12) . . ? C133 C131 C126 118.6(12) . . ? C131 C132 C133 121.9(12) . 2 ? C131 C132 H132 119.0 . . ? C133 C132 H132 119.0 2 . ? C132 C133 C131 119.2(13) 2 . ? C132 C133 H133 120.4 2 . ? C131 C133 H133 120.4 . . ? C212 N211 C216 120.0 . . ? C212 N211 Pb1 119.4(3) . . ? C216 N211 Pb1 119.7(3) . . ? C224 C212 N211 116.2(6) . . ? C224 C212 C213 123.8(6) . . ? N211 C212 C213 120.0 . . ? C214 C213 C212 120.0 . . ? C214 C213 H213 120.0 . . ? C212 C213 H213 120.0 . . ? C215 C214 C213 120.0 . . ? C215 C214 H214 120.0 . . ? C213 C214 H214 120.0 . . ? C214 C215 C216 120.0 . . ? C214 C215 H215 120.0 . . ? C216 C215 H215 120.0 . . ? C215 C216 N211 120.0 . . ? C215 C216 H216 120.0 . . ? N211 C216 H216 120.0 . . ? C226 N221 N222 120.4(8) . . ? C226 N221 C225 131.5(8) . . ? N222 N221 C225 108.0 . . ? N223 N222 N221 108.0 . . ? N222 N223 C224 108.0 . . ? N222 N223 Pb1 130.3(4) . . ? C224 N223 Pb1 117.5(4) . . ? C212 C224 C225 131.1(6) . . ? C212 C224 N223 120.8(6) . . ? C225 C224 N223 108.0 . . ? C224 C225 N221 108.0 . . ? C224 C225 H225 126.0 . . ? N221 C225 H225 126.0 . . ? N221 C226 C231 111.7(11) . . ? N221 C226 H22A 109.3 . . ? C231 C226 H22A 109.3 . . ? N221 C226 H22B 109.3 . . ? C231 C226 H22B 109.3 . . ? H22A C226 H22B 107.9 . . ? C233 C231 C232 116.8(14) . . ? C233 C231 C226 121.7(14) . . ? C232 C231 C226 121.4(13) . . ? C231 C232 C333 121.0(14) . 1_445 ? C231 C232 H232 119.5 . . ? C333 C232 H232 119.5 1_445 . ? C231 C233 C332 121.6(15) . 1_445 ? C231 C233 H233 119.2 . . ? C332 C233 H233 119.2 1_445 . ? C312 N311 C316 120.0 . . ? C312 N311 Pb1 121.5(4) . . ? C316 N311 Pb1 118.0(4) . . ? C324 C312 N311 115.6(7) . . ? C324 C312 C313 124.4(7) . . ? N311 C312 C313 120.0 . . ? C314 C313 C312 120.0 . . ? C314 C313 H313 120.0 . . ? C312 C313 H313 120.0 . . ? C315 C314 C313 120.0 . . ? C315 C314 H314 120.0 . . ? C313 C314 H314 120.0 . . ? C314 C315 C316 120.0 . . ? C314 C315 H315 120.0 . . ? C316 C315 H315 120.0 . . ? C315 C316 N311 120.0 . . ? C315 C316 H316 120.0 . . ? N311 C316 H316 120.0 . . ? C326 N321 N322 118.8(10) . . ? C326 N321 C325 133.2(10) . . ? N322 N321 C325 108.0 . . ? N323 N322 N321 108.0 . . ? C324 N323 N322 108.0 . . ? C324 N323 Pb1 118.6(4) . . ? N322 N323 Pb1 131.8(4) . . ? C312 C324 C325 129.2(7) . . ? C312 C324 N323 122.8(7) . . ? C325 C324 N323 108.0 . . ? C324 C325 N321 108.0 . . ? C324 C325 H325 126.0 . . ? N321 C325 H325 126.0 . . ? N321 C326 C331 111.2(12) . . ? N321 C326 H32A 109.4 . . ? C331 C326 H32A 109.4 . . ? N321 C326 H32B 109.4 . . ? C331 C326 H32B 109.4 . . ? H32A C326 H32B 108.0 . . ? C333 C331 C332 117.4(15) . . ? C333 C331 C326 123.2(14) . . ? C332 C331 C326 119.4(14) . . ? C331 C332 C233 121.1(15) . 1_665 ? C331 C332 H332 119.4 . . ? C233 C332 H332 119.4 1_665 . ? C331 C333 C232 121.9(15) . 1_665 ? C331 C333 H333 119.0 . . ? C232 C333 H333 119.0 1_665 . ? C412 N411 C416 120.0 . . ? C412 N411 Pb1 114.2(6) . . ? C416 N411 Pb1 122.6(6) . . ? C424 C412 N411 113.2(10) . . ? C424 C412 C413 126.6(10) . . ? N411 C412 C413 120.0 . . ? C412 C413 C414 120.0 . . ? C412 C413 H413 120.0 . . ? C414 C413 H413 120.0 . . ? C415 C414 C413 120.0 . . ? C415 C414 H414 120.0 . . ? C413 C414 H414 120.0 . . ? C414 C415 C416 120.0 . . ? C414 C415 H415 120.0 . . ? C416 C415 H415 120.0 . . ? C415 C416 N411 120.0 . . ? C415 C416 H416 120.0 . . ? N411 C416 H416 120.0 . . ? C426 N421 N422 119.8(12) . . ? C426 N421 C425 132.0(12) . . ? N422 N421 C425 108.0 . . ? N421 N422 N423 108.0 . . ? C424 N423 N422 108.0 . . ? C424 N423 Pb1 119.7(6) . . ? N422 N423 Pb1 129.3(6) . . ? C412 C424 N423 123.5(10) . . ? C412 C424 C425 128.5(10) . . ? N423 C424 C425 108.0 . . ? N421 C425 C424 108.0 . . ? N421 C425 H425 126.0 . . ? C424 C425 H425 126.0 . . ? N421 C426 C431 107.9(18) . . ? N421 C426 H42A 110.1 . . ? C431 C426 H42A 110.1 . . ? N421 C426 H42B 110.1 . . ? C431 C426 H42B 110.1 . . ? H42A C426 H42B 108.4 . . ? C433 C431 C432 121(2) . . ? C433 C431 C426 119(2) . . ? C432 C431 C426 120(2) . . ? C433 C432 C431 121(2) 2_766 . ? C433 C432 H432 119.4 2_766 . ? C431 C432 H432 119.4 . . ? C432 C433 C431 118(2) 2_766 . ? C432 C433 H433 120.9 2_766 . ? C431 C433 H433 120.9 . . ? O13X Cl1X O15X 109.9(5) . . ? O13X Cl1X O14X 110.0(5) . . ? O15X Cl1X O14X 109.7(6) . . ? O13X Cl1X O12X 109.6(5) . . ? O15X Cl1X O12X 109.0(5) . . ? O14X Cl1X O12X 108.6(5) . . ? O15Y Cl1Y O12Y 109.7(7) . . ? O15Y Cl1Y O13Y 109.8(7) . . ? O12Y Cl1Y O13Y 109.5(7) . . ? O15Y Cl1Y O14Y 109.4(7) . . ? O12Y Cl1Y O14Y 109.3(7) . . ? O13Y Cl1Y O14Y 109.2(7) . . ? O22X Cl2X O24X 110.8(6) . . ? O22X Cl2X O23X 110.1(6) . . ? O24X Cl2X O23X 108.9(6) . . ? O22X Cl2X O25X 109.2(6) . . ? O24X Cl2X O25X 109.2(6) . . ? O23X Cl2X O25X 108.7(6) . . ? O25Y Cl2Y O24Y 110.6(7) . . ? O25Y Cl2Y O23Y 109.8(7) . . ? O24Y Cl2Y O23Y 109.5(7) . . ? O25Y Cl2Y O22Y 109.3(7) . . ? O24Y Cl2Y O22Y 109.2(7) . . ? O23Y Cl2Y O22Y 108.5(7) . . ? 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 N423 Pb1 N111 C112 170.9(5) . . . . ? N123 Pb1 N111 C112 14.8(4) . . . . ? N223 Pb1 N111 C112 42.8(6) . . . . ? N211 Pb1 N111 C112 91.7(5) . . . . ? N323 Pb1 N111 C112 -111.8(5) . . . . ? N311 Pb1 N111 C112 -55.3(5) . . . . ? N411 Pb1 N111 C112 -166.1(7) . . . . ? N423 Pb1 N111 C116 -20.8(5) . . . . ? N123 Pb1 N111 C116 -177.0(5) . . . . ? N223 Pb1 N111 C116 -148.9(4) . . . . ? N211 Pb1 N111 C116 -100.1(4) . . . . ? N323 Pb1 N111 C116 56.5(4) . . . . ? N311 Pb1 N111 C116 113.0(4) . . . . ? N411 Pb1 N111 C116 2.2(9) . . . . ? C116 N111 C112 C124 -179.4(8) . . . . ? Pb1 N111 C112 C124 -11.1(8) . . . . ? C116 N111 C112 C113 0.0 . . . . ? Pb1 N111 C112 C113 168.3(5) . . . . ? C124 C112 C113 C114 179.3(9) . . . . ? N111 C112 C113 C114 0.0 . . . . ? C112 C113 C114 C115 0.0 . . . . ? C113 C114 C115 C116 0.0 . . . . ? C114 C115 C116 N111 0.0 . . . . ? C112 N111 C116 C115 0.0 . . . . ? Pb1 N111 C116 C115 -168.1(5) . . . . ? C126 N121 N122 N123 -179.5(10) . . . . ? C125 N121 N122 N123 0.0 . . . . ? N121 N122 N123 C124 0.0 . . . . ? N121 N122 N123 Pb1 160.7(6) . . . . ? N423 Pb1 N123 C124 -64.9(8) . . . . ? N223 Pb1 N123 C124 -175.0(5) . . . . ? N211 Pb1 N123 C124 -110.4(5) . . . . ? N323 Pb1 N123 C124 38.4(5) . . . . ? N111 Pb1 N123 C124 -17.4(4) . . . . ? N311 Pb1 N123 C124 88.2(5) . . . . ? N411 Pb1 N123 C124 163.3(6) . . . . ? N423 Pb1 N123 N122 136.7(7) . . . . ? N223 Pb1 N123 N122 26.6(5) . . . . ? N211 Pb1 N123 N122 91.2(5) . . . . ? N323 Pb1 N123 N122 -120.0(5) . . . . ? N111 Pb1 N123 N122 -175.8(6) . . . . ? N311 Pb1 N123 N122 -70.2(5) . . . . ? N411 Pb1 N123 N122 4.9(9) . . . . ? N111 C112 C124 C125 178.5(6) . . . . ? C113 C112 C124 C125 -0.9(12) . . . . ? N111 C112 C124 N123 -5.1(9) . . . . ? C113 C112 C124 N123 175.5(5) . . . . ? N122 N123 C124 C112 -177.2(9) . . . . ? Pb1 N123 C124 C112 20.5(9) . . . . ? N122 N123 C124 C125 0.0 . . . . ? Pb1 N123 C124 C125 -162.2(6) . . . . ? C112 C124 C125 N121 176.7(11) . . . . ? N123 C124 C125 N121 0.0 . . . . ? C126 N121 C125 C124 179.3(12) . . . . ? N122 N121 C125 C124 0.0 . . . . ? N122 N121 C126 C131 74.3(12) . . . . ? C125 N121 C126 C131 -105.0(12) . . . . ? N121 C126 C131 C132 75.1(16) . . . . ? N121 C126 C131 C133 -106.7(13) . . . . ? C133 C131 C132 C133 1(2) . . . 2 ? C126 C131 C132 C133 179.2(12) . . . 2 ? C132 C131 C133 C132 -1(2) . . . 2 ? C126 C131 C133 C132 -179.2(12) . . . 2 ? N423 Pb1 N211 C212 140.4(5) . . . . ? N123 Pb1 N211 C212 -63.0(5) . . . . ? N223 Pb1 N211 C212 14.8(5) . . . . ? N323 Pb1 N211 C212 -172.0(5) . . . . ? N111 Pb1 N211 C212 -123.8(5) . . . . ? N311 Pb1 N211 C212 -28.5(7) . . . . ? N411 Pb1 N211 C212 82.3(5) . . . . ? N423 Pb1 N211 C216 -50.8(5) . . . . ? N123 Pb1 N211 C216 105.8(5) . . . . ? N223 Pb1 N211 C216 -176.4(6) . . . . ? N323 Pb1 N211 C216 -3.2(8) . . . . ? N111 Pb1 N211 C216 45.1(5) . . . . ? N311 Pb1 N211 C216 140.3(5) . . . . ? N411 Pb1 N211 C216 -108.9(5) . . . . ? C216 N211 C212 C224 179.7(9) . . . . ? Pb1 N211 C212 C224 -11.5(8) . . . . ? C216 N211 C212 C213 0.0 . . . . ? Pb1 N211 C212 C213 168.8(6) . . . . ? C224 C212 C213 C214 -179.7(10) . . . . ? N211 C212 C213 C214 0.0 . . . . ? C212 C213 C214 C215 0.0 . . . . ? C213 C214 C215 C216 0.0 . . . . ? C214 C215 C216 N211 0.0 . . . . ? C212 N211 C216 C215 0.0 . . . . ? Pb1 N211 C216 C215 -168.7(6) . . . . ? C226 N221 N222 N223 177.3(10) . . . . ? C225 N221 N222 N223 0.0 . . . . ? N221 N222 N223 C224 0.0 . . . . ? N221 N222 N223 Pb1 155.7(7) . . . . ? N423 Pb1 N223 N222 127.7(6) . . . . ? N123 Pb1 N223 N222 -86.9(6) . . . . ? N211 Pb1 N223 N222 -170.3(6) . . . . ? N323 Pb1 N223 N222 16.3(9) . . . . ? N111 Pb1 N223 N222 -112.2(6) . . . . ? N311 Pb1 N223 N222 -12.3(6) . . . . ? N411 Pb1 N223 N222 80.7(6) . . . . ? N423 Pb1 N223 C224 -78.5(6) . . . . ? N123 Pb1 N223 C224 67.0(5) . . . . ? N211 Pb1 N223 C224 -16.5(5) . . . . ? N323 Pb1 N223 C224 170.1(5) . . . . ? N111 Pb1 N223 C224 41.6(6) . . . . ? N311 Pb1 N223 C224 141.5(5) . . . . ? N411 Pb1 N223 C224 -125.5(6) . . . . ? N211 C212 C224 C225 173.1(6) . . . . ? C213 C212 C224 C225 -7.2(12) . . . . ? N211 C212 C224 N223 -5.0(10) . . . . ? C213 C212 C224 N223 174.7(6) . . . . ? N222 N223 C224 C212 178.5(10) . . . . ? Pb1 N223 C224 C212 19.2(9) . . . . ? N222 N223 C224 C225 0.0 . . . . ? Pb1 N223 C224 C225 -159.3(6) . . . . ? C212 C224 C225 N221 -178.3(11) . . . . ? N223 C224 C225 N221 0.0 . . . . ? C226 N221 C225 C224 -176.9(12) . . . . ? N222 N221 C225 C224 0.0 . . . . ? N222 N221 C226 C231 -88.3(13) . . . . ? C225 N221 C226 C231 88.3(14) . . . . ? N221 C226 C231 C233 76.8(18) . . . . ? N221 C226 C231 C232 -100.1(17) . . . . ? C233 C231 C232 C333 4(3) . . . 1_445 ? C226 C231 C232 C333 -178.6(15) . . . 1_445 ? C232 C231 C233 C332 -6(3) . . . 1_445 ? C226 C231 C233 C332 177.4(15) . . . 1_445 ? N423 Pb1 N311 C312 43.8(7) . . . . ? N123 Pb1 N311 C312 -116.5(5) . . . . ? N223 Pb1 N311 C312 171.5(5) . . . . ? N211 Pb1 N311 C312 -151.1(5) . . . . ? N323 Pb1 N311 C312 8.3(4) . . . . ? N111 Pb1 N311 C312 -58.9(5) . . . . ? N411 Pb1 N311 C312 96.5(5) . . . . ? N423 Pb1 N311 C316 -143.7(5) . . . . ? N123 Pb1 N311 C316 56.0(4) . . . . ? N223 Pb1 N311 C316 -16.0(5) . . . . ? N211 Pb1 N311 C316 21.4(7) . . . . ? N323 Pb1 N311 C316 -179.2(5) . . . . ? N111 Pb1 N311 C316 113.6(4) . . . . ? N411 Pb1 N311 C316 -91.0(5) . . . . ? C316 N311 C312 C324 -179.1(9) . . . . ? Pb1 N311 C312 C324 -6.7(8) . . . . ? C316 N311 C312 C313 0.0 . . . . ? Pb1 N311 C312 C313 172.3(6) . . . . ? C324 C312 C313 C314 179.0(10) . . . . ? N311 C312 C313 C314 0.0 . . . . ? C312 C313 C314 C315 0.0 . . . . ? C313 C314 C315 C316 0.0 . . . . ? C314 C315 C316 N311 0.0 . . . . ? C312 N311 C316 C315 0.0 . . . . ? Pb1 N311 C316 C315 -172.6(5) . . . . ? C326 N321 N322 N323 -178.6(11) . . . . ? C325 N321 N322 N323 0.0 . . . . ? N321 N322 N323 C324 0.0 . . . . ? N321 N322 N323 Pb1 165.3(7) . . . . ? N423 Pb1 N323 C324 -163.2(6) . . . . ? N123 Pb1 N323 C324 49.6(5) . . . . ? N223 Pb1 N323 C324 -42.4(8) . . . . ? N211 Pb1 N323 C324 149.0(5) . . . . ? N111 Pb1 N323 C324 98.3(5) . . . . ? N311 Pb1 N323 C324 -9.0(5) . . . . ? N411 Pb1 N323 C324 -102.9(5) . . . . ? N423 Pb1 N323 N322 32.7(6) . . . . ? N123 Pb1 N323 N322 -114.5(6) . . . . ? N223 Pb1 N323 N322 153.5(6) . . . . ? N211 Pb1 N323 N322 -15.0(9) . . . . ? N111 Pb1 N323 N322 -65.8(6) . . . . ? N311 Pb1 N323 N322 -173.1(7) . . . . ? N411 Pb1 N323 N322 93.0(6) . . . . ? N311 C312 C324 C325 175.2(6) . . . . ? C313 C312 C324 C325 -3.8(12) . . . . ? N311 C312 C324 N323 -2.6(11) . . . . ? C313 C312 C324 N323 178.3(6) . . . . ? N322 N323 C324 C312 178.2(10) . . . . ? Pb1 N323 C324 C312 10.6(10) . . . . ? N322 N323 C324 C325 0.0 . . . . ? Pb1 N323 C324 C325 -167.6(6) . . . . ? C312 C324 C325 N321 -178.1(11) . . . . ? N323 C324 C325 N321 0.0 . . . . ? C326 N321 C325 C324 178.4(13) . . . . ? N322 N321 C325 C324 0.0 . . . . ? N322 N321 C326 C331 114.2(12) . . . . ? C325 N321 C326 C331 -64.0(18) . . . . ? N321 C326 C331 C333 -47(2) . . . . ? N321 C326 C331 C332 135.3(16) . . . . ? C333 C331 C332 C233 0(3) . . . 1_665 ? C326 C331 C332 C233 177.6(16) . . . 1_665 ? C332 C331 C333 C232 -1(3) . . . 1_665 ? C326 C331 C333 C232 -178.7(16) . . . 1_665 ? N423 Pb1 N411 C412 25.0(7) . . . . ? N123 Pb1 N411 C412 177.2(6) . . . . ? N223 Pb1 N411 C412 155.6(7) . . . . ? N211 Pb1 N411 C412 97.8(6) . . . . ? N323 Pb1 N411 C412 -52.7(7) . . . . ? N111 Pb1 N411 C412 -1.5(11) . . . . ? N311 Pb1 N411 C412 -112.9(6) . . . . ? N423 Pb1 N411 C416 -175.3(9) . . . . ? N123 Pb1 N411 C416 -23.1(10) . . . . ? N223 Pb1 N411 C416 -44.6(7) . . . . ? N211 Pb1 N411 C416 -102.5(7) . . . . ? N323 Pb1 N411 C416 107.0(7) . . . . ? N111 Pb1 N411 C416 158.3(8) . . . . ? N311 Pb1 N411 C416 46.8(7) . . . . ? C416 N411 C412 C424 174.8(15) . . . . ? Pb1 N411 C412 C424 -24.9(12) . . . . ? C416 N411 C412 C413 0.0 . . . . ? Pb1 N411 C412 C413 160.3(8) . . . . ? C424 C412 C413 C414 -174.1(17) . . . . ? N411 C412 C413 C414 0.0 . . . . ? C412 C413 C414 C415 0.0 . . . . ? C413 C414 C415 C416 0.0 . . . . ? C414 C415 C416 N411 0.0 . . . . ? C412 N411 C416 C415 0.0 . . . . ? Pb1 N411 C416 C415 -158.6(9) . . . . ? C426 N421 N422 N423 -176.5(18) . . . . ? C425 N421 N422 N423 0.0 . . . . ? N421 N422 N423 C424 0.0 . . . . ? N421 N422 N423 Pb1 160.0(11) . . . . ? N123 Pb1 N423 C424 -173.2(7) . . . . ? N223 Pb1 N423 C424 -75.8(8) . . . . ? N211 Pb1 N423 C424 -128.4(8) . . . . ? N323 Pb1 N423 C424 74.3(8) . . . . ? N111 Pb1 N423 C424 146.6(7) . . . . ? N311 Pb1 N423 C424 43.4(9) . . . . ? N411 Pb1 N423 C424 -21.9(7) . . . . ? N123 Pb1 N423 N422 28.8(13) . . . . ? N223 Pb1 N423 N422 126.2(8) . . . . ? N211 Pb1 N423 N422 73.6(9) . . . . ? N323 Pb1 N423 N422 -83.7(9) . . . . ? N111 Pb1 N423 N422 -11.3(9) . . . . ? N311 Pb1 N423 N422 -114.6(9) . . . . ? N411 Pb1 N423 N422 -179.9(11) . . . . ? N411 C412 C424 N423 5.6(17) . . . . ? C413 C412 C424 N423 -180.0(9) . . . . ? N411 C412 C424 C425 -171.3(10) . . . . ? C413 C412 C424 C425 3(2) . . . . ? N422 N423 C424 C412 -177.4(17) . . . . ? Pb1 N423 C424 C412 20.3(16) . . . . ? N422 N423 C424 C425 0.0 . . . . ? Pb1 N423 C424 C425 -162.2(10) . . . . ? C426 N421 C425 C424 176(2) . . . . ? N422 N421 C425 C424 0.0 . . . . ? C412 C424 C425 N421 177.2(18) . . . . ? N423 C424 C425 N421 0.0 . . . . ? N422 N421 C426 C431 67(2) . . . . ? C425 N421 C426 C431 -108.2(19) . . . . ? N421 C426 C431 C433 -93(2) . . . . ? N421 C426 C431 C432 85(2) . . . . ? C433 C431 C432 C433 0(4) . . . 2_766 ? C426 C431 C432 C433 -178.2(19) . . . 2_766 ? C432 C431 C433 C432 0(4) . . . 2_766 ? C426 C431 C433 C432 178.3(18) . . . 2_766 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.866 _refine_diff_density_min -3.230 _refine_diff_density_rms 0.202 #===END data_imw1426_0m _database_code_depnum_ccdc_archive 'CCDC 778862' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H36 Cl2 N13 O9.50 Pb' _chemical_formula_weight 1068.86 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.4736(5) _cell_length_b 22.5686(11) _cell_length_c 15.6899(6) _cell_angle_alpha 90.00 _cell_angle_beta 103.555(3) _cell_angle_gamma 90.00 _cell_volume 4293.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3046 _cell_measurement_theta_min 2.94 _cell_measurement_theta_max 19.12 _exptl_crystal_description Plate _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.653 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2116 _exptl_absorpt_coefficient_mu 4.122 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4928 _exptl_absorpt_correction_T_max 0.6833 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28195 _diffrn_reflns_av_R_equivalents 0.0974 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.25 _diffrn_reflns_theta_max 25.03 _reflns_number_total 7509 _reflns_number_gt 4511 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a polymer of repeat unit [PbL(DMF)(ClO4)2].0.5(Et2O) The data was solved by direct methods. Data processing was conducted to a resolution of 50 2theta as the data was only complete to this resolution. The structure contains two fully disordered perchlorate anions (Cl1 > O15 and Cl2 > O25) both of which have been modelled to reside over two sites with 50:50 occupancy. Geometric and displacement restraints have been employed to improve the appearance of these disordered residues. The structure contains a coordinated DMF (O11S > c15S) and a free diethyl ether molecule. The ether molecule has had its occupancy set to 50 % to bring their thermal parameters in line with the average. Geometric and displacement restrains have been used to improve the molecules. 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^)+(0.0987P)^2^+10.0825P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7509 _refine_ls_number_parameters 562 _refine_ls_number_restraints 190 _refine_ls_R_factor_all 0.1169 _refine_ls_R_factor_gt 0.0610 _refine_ls_wR_factor_ref 0.1861 _refine_ls_wR_factor_gt 0.1567 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.008 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.36696(4) 0.950822(19) 0.20895(3) 0.04405(18) Uani 1 1 d . . . N111 N 0.3281(9) 0.9492(5) 0.3689(6) 0.055(3) Uani 1 1 d . . . C112 C 0.4094(12) 0.9363(5) 0.4418(8) 0.053(3) Uani 1 1 d . . . C113 C 0.3864(13) 0.9295(6) 0.5252(8) 0.061(4) Uani 1 1 d . . . H113 H 0.4432 0.9200 0.5751 0.073 Uiso 1 1 calc R . . C114 C 0.2799(15) 0.9370(6) 0.5321(9) 0.070(4) Uani 1 1 d . . . H114 H 0.2622 0.9313 0.5872 0.084 Uiso 1 1 calc R A . C115 C 0.1983(13) 0.9528(6) 0.4605(9) 0.068(4) Uani 1 1 d . . . H115 H 0.1253 0.9607 0.4657 0.081 Uiso 1 1 calc R . . C116 C 0.2265(13) 0.9567(6) 0.3798(9) 0.066(4) Uani 1 1 d . . . H116 H 0.1695 0.9653 0.3295 0.079 Uiso 1 1 calc R A . N121 N 0.6907(9) 0.9113(5) 0.4335(6) 0.057(3) Uani 1 1 d . . . N122 N 0.6439(9) 0.9273(5) 0.3498(6) 0.055(3) Uani 1 1 d . . . N123 N 0.5396(9) 0.9371(4) 0.3471(6) 0.051(3) Uani 1 1 d . A . C124 C 0.5201(11) 0.9284(6) 0.4269(7) 0.051(3) Uani 1 1 d . A . C125 C 0.6168(12) 0.9126(6) 0.4839(8) 0.058(3) Uani 1 1 d . . . H125 H 0.6289 0.9045 0.5448 0.070 Uiso 1 1 calc R A . C126 C 0.8120(11) 0.8972(7) 0.4546(8) 0.066(4) Uani 1 1 d . . . H12A H 0.8544 0.9328 0.4458 0.080 Uiso 1 1 calc R A . H12B H 0.8365 0.8848 0.5167 0.080 Uiso 1 1 calc R . . N131 N 0.5482(9) 0.9607(4) 0.1378(7) 0.055(3) Uani 1 1 d . . . C132 C 0.5524(10) 0.9357(5) 0.0628(7) 0.047(3) Uani 1 1 d . . . C133 C 0.6399(12) 0.9449(7) 0.0227(9) 0.068(4) Uani 1 1 d . . . H133 H 0.6408 0.9273 -0.0320 0.081 Uiso 1 1 calc R . . C134 C 0.7258(14) 0.9813(9) 0.0667(13) 0.093(6) Uani 1 1 d . . . H134 H 0.7871 0.9887 0.0419 0.111 Uiso 1 1 calc R A . C135 C 0.7220(13) 1.0058(7) 0.1442(11) 0.081(5) Uani 1 1 d . . . H135 H 0.7803 1.0303 0.1750 0.098 Uiso 1 1 calc R . . C136 C 0.6318(13) 0.9947(7) 0.1777(9) 0.073(4) Uani 1 1 d . . . H136 H 0.6290 1.0122 0.2322 0.087 Uiso 1 1 calc R A . N141 N 0.3357(9) 0.8481(4) -0.0716(6) 0.051(2) Uani 1 1 d . . . N142 N 0.2910(9) 0.8652(5) -0.0049(7) 0.057(3) Uani 1 1 d . . . N143 N 0.3635(8) 0.8973(4) 0.0490(6) 0.046(2) Uani 1 1 d . A . C144 C 0.4576(10) 0.9006(5) 0.0186(6) 0.043(3) Uani 1 1 d . A . C145 C 0.4371(11) 0.8690(5) -0.0603(7) 0.052(3) Uani 1 1 d . . . H145 H 0.4859 0.8638 -0.0980 0.062 Uiso 1 1 calc R A . C146 C 0.2726(12) 0.8153(6) -0.1450(8) 0.070(4) Uani 1 1 d . . . H14A H 0.2745 0.8367 -0.1997 0.084 Uiso 1 1 calc R A . H14B H 0.1949 0.8137 -0.1404 0.084 Uiso 1 1 calc R . . N151 N 0.4050(8) 0.8377(4) 0.2242(6) 0.047(2) Uani 1 1 d . . . C152 C 0.3190(11) 0.8007(6) 0.2094(8) 0.055(3) Uani 1 1 d . . . C153 C 0.3348(12) 0.7409(6) 0.1949(10) 0.074(4) Uani 1 1 d . . . H153 H 0.2734 0.7147 0.1830 0.089 Uiso 1 1 calc R . . C154 C 0.4402(18) 0.7191(9) 0.1979(15) 0.118(7) Uani 1 1 d . . . H154 H 0.4527 0.6782 0.1897 0.142 Uiso 1 1 calc R A . C155 C 0.5261(13) 0.7597(7) 0.2131(10) 0.077(4) Uani 1 1 d . . . H155 H 0.5991 0.7470 0.2144 0.093 Uiso 1 1 calc R . . C156 C 0.5057(11) 0.8175(6) 0.2262(7) 0.056(3) Uani 1 1 d . . . H156 H 0.5656 0.8446 0.2373 0.067 Uiso 1 1 calc R A . N161 N 0.0371(9) 0.8417(5) 0.1905(7) 0.056(3) Uani 1 1 d . . . N162 N 0.0861(9) 0.8932(5) 0.1885(7) 0.062(3) Uani 1 1 d . . . N163 N 0.1917(8) 0.8817(4) 0.1965(7) 0.050(2) Uani 1 1 d . A . C164 C 0.2098(10) 0.8237(5) 0.2023(8) 0.050(3) Uani 1 1 d . A . C165 C 0.1081(12) 0.7983(6) 0.1975(9) 0.064(4) Uani 1 1 d . . . H165 H 0.0925 0.7571 0.1991 0.077 Uiso 1 1 calc R A . C166 C -0.0834(11) 0.8395(8) 0.1790(9) 0.072(4) Uani 1 1 d . . . H16A H -0.1147 0.8108 0.1320 0.086 Uiso 1 1 calc R A . H16B H -0.1148 0.8789 0.1600 0.086 Uiso 1 1 calc R . . C171 C 0.8328(10) 0.8483(6) 0.3959(7) 0.049(3) Uani 1 1 d . . . C172 C 0.8041(10) 0.7893(6) 0.4072(8) 0.052(3) Uani 1 1 d . . . H172 H 0.7776 0.7788 0.4572 0.062 Uiso 1 1 calc R A . C173 C 0.8135(10) 0.7473(6) 0.3487(8) 0.057(3) Uani 1 1 d . . . C174 C 0.8519(10) 0.7625(6) 0.2750(8) 0.054(3) Uani 1 1 d . . . H174 H 0.8576 0.7330 0.2330 0.064 Uiso 1 1 calc R A . C175 C 0.8825(9) 0.8215(6) 0.2626(7) 0.050(3) Uani 1 1 d . . . C176 C 0.8715(9) 0.8640(5) 0.3242(8) 0.049(3) Uani 1 1 d . . . H176 H 0.8909 0.9040 0.3165 0.059 Uiso 1 1 calc R A . Cl1X Cl 0.4331(5) 1.1259(3) 0.2616(4) 0.0686(12) Uiso 0.50 1 d PDU A 1 O12X O 0.3777(10) 1.1489(6) 0.3254(7) 0.0733(18) Uiso 0.50 1 d PDU A 1 O13X O 0.4221(12) 1.0625(3) 0.2575(9) 0.0703(14) Uiso 0.50 1 d PDU A 1 O14X O 0.3848(11) 1.1510(6) 0.1770(5) 0.074(2) Uiso 0.50 1 d PDU A 1 O15X O 0.5482(6) 1.1414(6) 0.2868(9) 0.079(2) Uiso 0.50 1 d PDU A 1 Cl1Y Cl 0.3910(5) 1.1187(3) 0.2534(4) 0.0663(12) Uiso 0.50 1 d PDU B 2 O12Y O 0.4561(10) 1.1596(5) 0.3150(7) 0.0742(19) Uiso 0.50 1 d PDU B 2 O13Y O 0.4628(10) 1.0757(5) 0.2273(8) 0.070(2) Uiso 0.50 1 d PDU B 2 O14Y O 0.3319(10) 1.1506(6) 0.1774(6) 0.076(2) Uiso 0.50 1 d PDU B 2 O15Y O 0.3140(9) 1.0888(6) 0.2940(8) 0.075(2) Uiso 0.50 1 d PDU B 2 Cl2X Cl 0.5528(5) 0.5709(3) 0.1454(4) 0.0687(13) Uiso 0.50 1 d PDU C 1 O22X O 0.4505(8) 0.5697(7) 0.1729(9) 0.072(2) Uiso 0.50 1 d PDU C 1 O23X O 0.6337(11) 0.6038(6) 0.2082(7) 0.077(2) Uiso 0.50 1 d PDU C 1 O24X O 0.5914(12) 0.5113(4) 0.1397(9) 0.071(2) Uiso 0.50 1 d PDU C 1 O25X O 0.5356(11) 0.5990(6) 0.0609(5) 0.074(2) Uiso 0.50 1 d PDU C 1 Cl2Y Cl 0.5289(5) 0.5539(3) 0.1708(4) 0.0684(13) Uiso 0.50 1 d PDU D 2 O22Y O 0.5383(11) 0.5047(4) 0.2307(7) 0.074(3) Uiso 0.50 1 d PDU D 2 O23Y O 0.6129(11) 0.5969(5) 0.2054(8) 0.074(2) Uiso 0.50 1 d PDU D 2 O24Y O 0.4217(8) 0.5807(6) 0.1599(9) 0.071(2) Uiso 0.50 1 d PDU D 2 O25Y O 0.5423(12) 0.5329(6) 0.0872(5) 0.0731(19) Uiso 0.50 1 d PDU D 2 O11S O 0.1989(12) 1.0095(7) 0.1166(11) 0.157(3) Uani 1 1 d DU A . N12S N 0.0666(12) 1.0798(7) 0.0915(10) 0.157(3) Uani 1 1 d DU A . C13S C 0.1250(16) 1.0377(9) 0.1360(11) 0.157(3) Uani 1 1 d DU . . H13S H 0.1081 1.0278 0.1902 0.189 Uiso 1 1 calc R A . C14S C 0.1008(17) 1.1099(10) 0.0185(14) 0.158(3) Uani 1 1 d DU . . H14C H 0.1664 1.0903 0.0076 0.236 Uiso 1 1 calc R A . H14D H 0.1178 1.1515 0.0339 0.236 Uiso 1 1 calc R . . H14E H 0.0408 1.1078 -0.0344 0.236 Uiso 1 1 calc R . . C15S C -0.0265(16) 1.1024(10) 0.1218(15) 0.158(3) Uani 1 1 d DU . . H15A H -0.0950 1.0914 0.0800 0.236 Uiso 1 1 calc R A . H15B H -0.0214 1.1457 0.1264 0.236 Uiso 1 1 calc R . . H15C H -0.0260 1.0855 0.1794 0.236 Uiso 1 1 calc R . . O21S O 0.3164(11) 0.7586(8) 0.5032(10) 0.072(3) Uani 0.50 1 d PDU . . C22S C 0.3677(17) 0.7726(12) 0.4332(10) 0.072(3) Uani 0.50 1 d PDU . . H22A H 0.3474 0.8129 0.4102 0.087 Uiso 0.50 1 calc PR . . H22B H 0.3468 0.7436 0.3847 0.087 Uiso 0.50 1 calc PR . . C23S C 0.4915(17) 0.7686(12) 0.4772(16) 0.072(3) Uani 0.50 1 d PDU . . H23A H 0.5071 0.7915 0.5317 0.109 Uiso 0.50 1 calc PR . . H23B H 0.5343 0.7847 0.4375 0.109 Uiso 0.50 1 calc PR . . H23C H 0.5119 0.7271 0.4902 0.109 Uiso 0.50 1 calc PR . . C24S C 0.2037(13) 0.7705(11) 0.4617(12) 0.073(3) Uani 0.50 1 d PDU . . H24A H 0.1781 0.7453 0.4092 0.087 Uiso 0.50 1 calc PR . . H24B H 0.1930 0.8127 0.4443 0.087 Uiso 0.50 1 calc PR . . C25S C 0.143(2) 0.7551(12) 0.5335(15) 0.073(3) Uani 0.50 1 d PDU . . H25A H 0.1614 0.7146 0.5542 0.109 Uiso 0.50 1 calc PR . . H25B H 0.0630 0.7581 0.5094 0.109 Uiso 0.50 1 calc PR . . H25C H 0.1650 0.7829 0.5825 0.109 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0507(3) 0.0389(3) 0.0419(2) 0.0006(2) 0.00966(18) 0.0052(2) N111 0.059(7) 0.062(7) 0.045(5) -0.001(5) 0.015(5) 0.012(6) C112 0.077(9) 0.035(7) 0.052(7) 0.000(5) 0.026(7) 0.000(6) C113 0.075(10) 0.063(9) 0.048(7) 0.000(6) 0.017(7) 0.004(7) C114 0.103(13) 0.057(9) 0.056(8) 0.006(7) 0.032(8) 0.005(8) C115 0.079(10) 0.067(9) 0.061(8) -0.012(7) 0.023(7) 0.013(8) C116 0.070(10) 0.069(10) 0.063(8) 0.000(7) 0.023(7) 0.016(8) N121 0.073(8) 0.046(6) 0.044(5) -0.006(5) -0.001(5) 0.004(5) N122 0.052(7) 0.068(7) 0.044(5) 0.000(5) 0.007(5) 0.001(5) N123 0.054(7) 0.049(7) 0.051(6) -0.002(5) 0.015(5) 0.007(5) C124 0.064(9) 0.049(7) 0.039(6) -0.003(5) 0.012(6) 0.005(6) C125 0.078(10) 0.056(8) 0.037(6) -0.002(6) 0.005(6) 0.007(7) C126 0.052(8) 0.081(10) 0.055(7) -0.003(7) -0.010(6) -0.004(7) N131 0.056(7) 0.053(7) 0.054(6) -0.002(5) 0.005(5) -0.016(5) C132 0.055(8) 0.040(7) 0.043(6) 0.006(5) 0.008(6) -0.010(6) C133 0.072(10) 0.070(10) 0.059(8) 0.006(7) 0.012(7) -0.006(8) C134 0.073(12) 0.106(14) 0.096(13) 0.041(11) 0.011(10) -0.022(10) C135 0.073(11) 0.065(10) 0.088(11) 0.031(9) -0.016(9) -0.020(8) C136 0.078(11) 0.073(10) 0.057(8) 0.016(7) -0.004(7) -0.029(9) N141 0.061(7) 0.040(6) 0.046(5) -0.004(5) 0.003(5) 0.002(5) N142 0.060(7) 0.050(7) 0.057(6) 0.001(5) 0.003(5) -0.011(5) N143 0.052(6) 0.044(6) 0.040(5) -0.005(4) 0.004(5) -0.010(5) C144 0.061(8) 0.036(6) 0.033(5) 0.007(5) 0.011(5) 0.002(6) C145 0.066(9) 0.044(7) 0.045(6) 0.007(6) 0.012(6) 0.011(6) C146 0.079(10) 0.049(8) 0.061(8) -0.012(7) -0.027(7) 0.017(7) N151 0.052(6) 0.043(6) 0.041(5) -0.005(4) 0.002(4) 0.000(5) C152 0.062(9) 0.051(8) 0.050(7) 0.004(6) 0.010(6) 0.007(7) C153 0.060(10) 0.038(8) 0.119(12) 0.003(8) 0.012(9) -0.001(7) C154 0.105(17) 0.071(13) 0.17(2) -0.023(13) 0.016(14) 0.001(12) C155 0.053(9) 0.077(11) 0.097(11) -0.011(9) 0.007(8) 0.023(8) C156 0.046(8) 0.063(9) 0.053(7) -0.013(6) 0.000(6) 0.012(7) N161 0.055(7) 0.045(7) 0.070(7) 0.011(5) 0.016(5) 0.000(6) N162 0.054(7) 0.054(7) 0.081(7) 0.007(6) 0.024(6) 0.014(6) N163 0.040(6) 0.042(6) 0.069(6) -0.004(5) 0.014(5) 0.005(5) C164 0.051(8) 0.039(7) 0.060(7) -0.005(6) 0.013(6) 0.006(6) C165 0.071(10) 0.043(8) 0.082(9) 0.000(7) 0.026(8) -0.023(7) C166 0.046(8) 0.099(12) 0.066(8) 0.016(8) 0.005(7) -0.006(8) C171 0.044(7) 0.047(7) 0.053(7) 0.000(6) 0.001(6) 0.000(6) C172 0.041(7) 0.055(8) 0.052(7) 0.001(6) -0.004(5) -0.011(6) C173 0.057(8) 0.045(8) 0.057(7) 0.014(6) -0.011(6) 0.001(6) C174 0.046(7) 0.049(8) 0.057(7) 0.001(6) -0.007(6) 0.008(6) C175 0.037(7) 0.060(8) 0.051(7) 0.012(6) 0.005(5) 0.008(6) C176 0.038(7) 0.036(7) 0.070(8) 0.008(6) 0.006(6) 0.004(5) O11S 0.148(7) 0.145(8) 0.202(8) 0.069(6) 0.087(6) 0.057(6) N12S 0.148(7) 0.145(8) 0.202(8) 0.069(6) 0.087(6) 0.057(6) C13S 0.148(7) 0.145(8) 0.202(8) 0.069(6) 0.087(6) 0.057(6) C14S 0.148(7) 0.145(8) 0.202(8) 0.069(6) 0.087(6) 0.057(6) C15S 0.148(7) 0.145(8) 0.202(8) 0.069(6) 0.087(6) 0.057(6) O21S 0.105(7) 0.045(6) 0.060(6) -0.018(5) 0.003(5) -0.010(6) C22S 0.105(7) 0.045(6) 0.060(6) -0.018(5) 0.003(5) -0.010(6) C23S 0.105(7) 0.045(6) 0.059(6) -0.018(5) 0.004(5) -0.010(6) C24S 0.105(7) 0.045(6) 0.060(6) -0.019(5) 0.003(5) -0.010(6) C25S 0.105(7) 0.046(6) 0.060(6) -0.018(5) 0.003(5) -0.010(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 N151 2.596(10) . ? Pb1 O11S 2.613(11) . ? Pb1 N163 2.655(10) . ? Pb1 N111 2.665(9) . ? Pb1 O13X 2.675(7) . ? Pb1 N123 2.691(10) . ? Pb1 N131 2.755(11) . ? Pb1 N143 2.776(9) . ? N111 C116 1.329(17) . ? N111 C112 1.371(16) . ? C112 C113 1.412(16) . ? C112 C124 1.465(18) . ? C113 C114 1.37(2) . ? C113 H113 0.9500 . ? C114 C115 1.37(2) . ? C114 H114 0.9500 . ? C115 C116 1.394(18) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C125 1.348(16) . ? N121 N122 1.355(13) . ? N121 C126 1.505(16) . ? N122 N123 1.309(13) . ? N123 C124 1.345(14) . ? C124 C125 1.369(17) . ? C125 H125 0.9500 . ? C126 C171 1.499(18) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C132 1.316(15) . ? N131 C136 1.328(16) . ? C132 C133 1.397(18) . ? C132 C144 1.457(16) . ? C133 C134 1.40(2) . ? C133 H133 0.9500 . ? C134 C135 1.35(2) . ? C134 H134 0.9500 . ? C135 C136 1.37(2) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 C145 1.323(15) . ? N141 N142 1.353(14) . ? N141 C146 1.438(15) . ? N142 N143 1.303(13) . ? N143 C144 1.368(14) . ? C144 C145 1.399(15) . ? C145 H145 0.9500 . ? C146 C173 1.511(17) 4_575 ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? N151 C156 1.330(15) . ? N151 C152 1.337(16) . ? C152 C153 1.391(18) . ? C152 C164 1.437(17) . ? C153 C154 1.39(2) . ? C153 H153 0.9500 . ? C154 C155 1.39(2) . ? C154 H154 0.9500 . ? C155 C156 1.352(19) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? N161 C165 1.309(17) . ? N161 N162 1.315(14) . ? N161 C166 1.473(16) . ? N162 N163 1.320(13) . ? N163 C164 1.327(14) . ? C164 C165 1.379(17) . ? C165 H165 0.9500 . ? C166 C175 1.525(17) 1_455 ? C166 H16A 0.9900 . ? C166 H16B 0.9900 . ? C171 C176 1.371(16) . ? C171 C172 1.400(17) . ? C172 C173 1.343(17) . ? C172 H172 0.9500 . ? C173 C174 1.396(17) . ? C173 C146 1.511(17) 4_676 ? C174 C175 1.412(17) . ? C174 H174 0.9500 . ? C175 C176 1.390(17) . ? C175 C166 1.525(17) 1_655 ? C176 H176 0.9500 . ? Cl1X O14X 1.438(2) . ? Cl1X O13X 1.439(2) . ? Cl1X O15X 1.440(2) . ? Cl1X O12X 1.440(2) . ? Cl1Y O15Y 1.439(2) . ? Cl1Y O14Y 1.439(2) . ? Cl1Y O13Y 1.441(2) . ? Cl1Y O12Y 1.441(2) . ? Cl2X O23X 1.440(2) . ? Cl2X O25X 1.440(2) . ? Cl2X O24X 1.440(2) . ? Cl2X O22X 1.440(2) . ? Cl2Y O23Y 1.438(2) . ? Cl2Y O24Y 1.441(2) . ? Cl2Y O22Y 1.441(2) . ? Cl2Y O25Y 1.441(2) . ? O11S C13S 1.217(2) . ? N12S C13S 1.2966(19) . ? N12S C15S 1.4457(19) . ? N12S C14S 1.4783(19) . ? C13S H13S 0.9500 . ? C14S H14C 0.9800 . ? C14S H14D 0.9800 . ? C14S H14E 0.9800 . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? O21S C22S 1.429(2) . ? O21S C24S 1.430(2) . ? C22S C23S 1.539(2) . ? C22S H22A 0.9900 . ? C22S H22B 0.9900 . ? C23S H23A 0.9800 . ? C23S H23B 0.9800 . ? C23S H23C 0.9800 . ? C24S C25S 1.539(2) . ? C24S H24A 0.9900 . ? C24S H24B 0.9900 . ? C25S H25A 0.9800 . ? C25S H25B 0.9800 . ? C25S H25C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N151 Pb1 O11S 130.9(5) . . ? N151 Pb1 N163 63.8(3) . . ? O11S Pb1 N163 73.6(4) . . ? N151 Pb1 N111 88.3(3) . . ? O11S Pb1 N111 103.3(4) . . ? N163 Pb1 N111 74.5(3) . . ? N151 Pb1 O13X 150.5(4) . . ? O11S Pb1 O13X 78.4(5) . . ? N163 Pb1 O13X 136.6(4) . . ? N111 Pb1 O13X 80.5(4) . . ? N151 Pb1 N123 73.6(3) . . ? O11S Pb1 N123 153.1(5) . . ? N163 Pb1 N123 118.8(3) . . ? N111 Pb1 N123 61.8(3) . . ? O13X Pb1 N123 77.0(4) . . ? N151 Pb1 N131 88.1(3) . . ? O11S Pb1 N131 111.2(4) . . ? N163 Pb1 N131 139.2(3) . . ? N111 Pb1 N131 136.9(3) . . ? O13X Pb1 N131 81.9(4) . . ? N123 Pb1 N131 76.0(3) . . ? N151 Pb1 N143 67.7(3) . . ? O11S Pb1 N143 83.0(4) . . ? N163 Pb1 N143 80.8(3) . . ? N111 Pb1 N143 151.4(3) . . ? O13X Pb1 N143 128.0(3) . . ? N123 Pb1 N143 121.2(3) . . ? N131 Pb1 N143 60.6(3) . . ? C116 N111 C112 117.4(10) . . ? C116 N111 Pb1 120.6(8) . . ? C112 N111 Pb1 121.8(8) . . ? N111 C112 C113 121.7(12) . . ? N111 C112 C124 115.7(10) . . ? C113 C112 C124 122.6(12) . . ? C114 C113 C112 118.2(13) . . ? C114 C113 H113 120.9 . . ? C112 C113 H113 120.9 . . ? C113 C114 C115 120.9(13) . . ? C113 C114 H114 119.6 . . ? C115 C114 H114 119.6 . . ? C114 C115 C116 117.6(14) . . ? C114 C115 H115 121.2 . . ? C116 C115 H115 121.2 . . ? N111 C116 C115 124.1(14) . . ? N111 C116 H116 118.0 . . ? C115 C116 H116 118.0 . . ? C125 N121 N122 111.3(10) . . ? C125 N121 C126 131.8(10) . . ? N122 N121 C126 116.9(10) . . ? N123 N122 N121 106.0(9) . . ? N122 N123 C124 109.8(10) . . ? N122 N123 Pb1 130.3(7) . . ? C124 N123 Pb1 118.8(8) . . ? N123 C124 C125 108.8(12) . . ? N123 C124 C112 120.9(11) . . ? C125 C124 C112 130.2(11) . . ? N121 C125 C124 103.9(10) . . ? N121 C125 H125 128.0 . . ? C124 C125 H125 128.0 . . ? C171 C126 N121 109.4(10) . . ? C171 C126 H12A 109.8 . . ? N121 C126 H12A 109.8 . . ? C171 C126 H12B 109.8 . . ? N121 C126 H12B 109.8 . . ? H12A C126 H12B 108.2 . . ? C132 N131 C136 118.6(12) . . ? C132 N131 Pb1 122.4(8) . . ? C136 N131 Pb1 118.9(10) . . ? N131 C132 C133 122.5(11) . . ? N131 C132 C144 117.5(11) . . ? C133 C132 C144 119.9(11) . . ? C134 C133 C132 117.1(14) . . ? C134 C133 H133 121.5 . . ? C132 C133 H133 121.5 . . ? C135 C134 C133 120.1(16) . . ? C135 C134 H134 120.0 . . ? C133 C134 H134 120.0 . . ? C134 C135 C136 118.4(15) . . ? C134 C135 H135 120.8 . . ? C136 C135 H135 120.8 . . ? N131 C136 C135 123.3(15) . . ? N131 C136 H136 118.3 . . ? C135 C136 H136 118.3 . . ? C145 N141 N142 110.4(9) . . ? C145 N141 C146 128.2(11) . . ? N142 N141 C146 121.3(11) . . ? N143 N142 N141 108.1(10) . . ? N142 N143 C144 109.0(9) . . ? N142 N143 Pb1 133.6(8) . . ? C144 N143 Pb1 117.3(7) . . ? N143 C144 C145 106.7(11) . . ? N143 C144 C132 122.0(10) . . ? C145 C144 C132 131.1(11) . . ? N141 C145 C144 105.7(11) . . ? N141 C145 H145 127.2 . . ? C144 C145 H145 127.2 . . ? N141 C146 C173 113.8(10) . 4_575 ? N141 C146 H14A 108.8 . . ? C173 C146 H14A 108.8 4_575 . ? N141 C146 H14B 108.8 . . ? C173 C146 H14B 108.8 4_575 . ? H14A C146 H14B 107.7 . . ? C156 N151 C152 120.2(11) . . ? C156 N151 Pb1 119.4(8) . . ? C152 N151 Pb1 118.5(8) . . ? N151 C152 C153 119.8(13) . . ? N151 C152 C164 119.6(12) . . ? C153 C152 C164 120.5(13) . . ? C154 C153 C152 120.3(15) . . ? C154 C153 H153 119.8 . . ? C152 C153 H153 119.8 . . ? C155 C154 C153 117.2(16) . . ? C155 C154 H154 121.4 . . ? C153 C154 H154 121.4 . . ? C156 C155 C154 119.8(15) . . ? C156 C155 H155 120.1 . . ? C154 C155 H155 120.1 . . ? N151 C156 C155 122.6(13) . . ? N151 C156 H156 118.7 . . ? C155 C156 H156 118.7 . . ? C165 N161 N162 110.8(11) . . ? C165 N161 C166 129.4(12) . . ? N162 N161 C166 119.6(11) . . ? N161 N162 N163 106.5(10) . . ? N162 N163 C164 110.5(10) . . ? N162 N163 Pb1 132.7(8) . . ? C164 N163 Pb1 116.7(8) . . ? N163 C164 C165 105.5(11) . . ? N163 C164 C152 120.4(12) . . ? C165 C164 C152 134.1(12) . . ? N161 C165 C164 106.7(11) . . ? N161 C165 H165 126.6 . . ? C164 C165 H165 126.6 . . ? N161 C166 C175 112.7(10) . 1_455 ? N161 C166 H16A 109.0 . . ? C175 C166 H16A 109.0 1_455 . ? N161 C166 H16B 109.0 . . ? C175 C166 H16B 109.0 1_455 . ? H16A C166 H16B 107.8 . . ? C176 C171 C172 119.9(11) . . ? C176 C171 C126 117.3(12) . . ? C172 C171 C126 122.4(12) . . ? C173 C172 C171 121.2(12) . . ? C173 C172 H172 119.4 . . ? C171 C172 H172 119.4 . . ? C172 C173 C174 119.6(12) . . ? C172 C173 C146 122.0(13) . 4_676 ? C174 C173 C146 118.1(12) . 4_676 ? C173 C174 C175 120.2(12) . . ? C173 C174 H174 119.9 . . ? C175 C174 H174 119.9 . . ? C176 C175 C174 118.7(11) . . ? C176 C175 C166 120.5(12) . 1_655 ? C174 C175 C166 120.5(12) . 1_655 ? C171 C176 C175 120.2(11) . . ? C171 C176 H176 119.9 . . ? C175 C176 H176 119.9 . . ? O14X Cl1X O13X 109.63(15) . . ? O14X Cl1X O15X 109.45(15) . . ? O13X Cl1X O15X 109.41(15) . . ? O14X Cl1X O12X 109.53(15) . . ? O13X Cl1X O12X 109.40(15) . . ? O15X Cl1X O12X 109.40(15) . . ? Cl1X O13X Pb1 164.9(8) . . ? O15Y Cl1Y O14Y 109.57(15) . . ? O15Y Cl1Y O13Y 109.51(15) . . ? O14Y Cl1Y O13Y 109.47(15) . . ? O15Y Cl1Y O12Y 109.45(15) . . ? O14Y Cl1Y O12Y 109.49(15) . . ? O13Y Cl1Y O12Y 109.35(15) . . ? O23X Cl2X O25X 109.49(15) . . ? O23X Cl2X O24X 109.48(15) . . ? O25X Cl2X O24X 109.49(15) . . ? O23X Cl2X O22X 109.47(15) . . ? O25X Cl2X O22X 109.45(15) . . ? O24X Cl2X O22X 109.45(15) . . ? O23Y Cl2Y O24Y 109.58(15) . . ? O23Y Cl2Y O22Y 109.54(15) . . ? O24Y Cl2Y O22Y 109.40(15) . . ? O23Y Cl2Y O25Y 109.55(15) . . ? O24Y Cl2Y O25Y 109.39(15) . . ? O22Y Cl2Y O25Y 109.37(15) . . ? C13S O11S Pb1 133.1(10) . . ? C13S N12S C15S 118.3(2) . . ? C13S N12S C14S 121.7(2) . . ? C15S N12S C14S 119.5(2) . . ? O11S C13S N12S 127.7(3) . . ? O11S C13S H13S 116.2 . . ? N12S C13S H13S 116.2 . . ? N12S C14S H14C 109.5 . . ? N12S C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? N12S C14S H14E 109.5 . . ? H14C C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? N12S C15S H15A 109.5 . . ? N12S C15S H15B 109.5 . . ? H15A C15S H15B 109.5 . . ? N12S C15S H15C 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? C22S O21S C24S 100.2(16) . . ? O21S C22S C23S 103.1(12) . . ? O21S C22S H22A 111.2 . . ? C23S C22S H22A 111.2 . . ? O21S C22S H22B 111.2 . . ? C23S C22S H22B 111.2 . . ? H22A C22S H22B 109.1 . . ? C22S C23S H23A 109.5 . . ? C22S C23S H23B 109.5 . . ? H23A C23S H23B 109.5 . . ? C22S C23S H23C 109.5 . . ? H23A C23S H23C 109.5 . . ? H23B C23S H23C 109.5 . . ? O21S C24S C25S 103.0(12) . . ? O21S C24S H24A 111.2 . . ? C25S C24S H24A 111.2 . . ? O21S C24S H24B 111.2 . . ? C25S C24S H24B 111.2 . . ? H24A C24S H24B 109.1 . . ? C24S C25S H25A 109.5 . . ? C24S C25S H25B 109.5 . . ? H25A C25S H25B 109.5 . . ? C24S C25S H25C 109.5 . . ? H25A C25S H25C 109.5 . . ? H25B C25S H25C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N151 Pb1 N111 C116 -109.5(10) . . . . ? O11S Pb1 N111 C116 22.3(11) . . . . ? N163 Pb1 N111 C116 -46.2(10) . . . . ? O13X Pb1 N111 C116 97.9(10) . . . . ? N123 Pb1 N111 C116 178.2(11) . . . . ? N131 Pb1 N111 C116 165.1(9) . . . . ? N143 Pb1 N111 C116 -77.7(12) . . . . ? N151 Pb1 N111 C112 65.3(9) . . . . ? O11S Pb1 N111 C112 -162.9(10) . . . . ? N163 Pb1 N111 C112 128.6(9) . . . . ? O13X Pb1 N111 C112 -87.2(9) . . . . ? N123 Pb1 N111 C112 -7.0(8) . . . . ? N131 Pb1 N111 C112 -20.0(11) . . . . ? N143 Pb1 N111 C112 97.2(10) . . . . ? C116 N111 C112 C113 1.6(18) . . . . ? Pb1 N111 C112 C113 -173.4(9) . . . . ? C116 N111 C112 C124 180.0(11) . . . . ? Pb1 N111 C112 C124 5.0(14) . . . . ? N111 C112 C113 C114 -0.9(19) . . . . ? C124 C112 C113 C114 -179.2(12) . . . . ? C112 C113 C114 C115 -2(2) . . . . ? C113 C114 C115 C116 4(2) . . . . ? C112 N111 C116 C115 1(2) . . . . ? Pb1 N111 C116 C115 175.8(10) . . . . ? C114 C115 C116 N111 -4(2) . . . . ? C125 N121 N122 N123 -1.7(14) . . . . ? C126 N121 N122 N123 179.7(10) . . . . ? N121 N122 N123 C124 0.8(13) . . . . ? N121 N122 N123 Pb1 -167.0(7) . . . . ? N151 Pb1 N123 N122 78.6(10) . . . . ? O11S Pb1 N123 N122 -123.0(11) . . . . ? N163 Pb1 N123 N122 125.3(10) . . . . ? N111 Pb1 N123 N122 175.6(11) . . . . ? O13X Pb1 N123 N122 -98.3(10) . . . . ? N131 Pb1 N123 N122 -13.6(10) . . . . ? N143 Pb1 N123 N122 28.5(11) . . . . ? N151 Pb1 N123 C124 -88.3(9) . . . . ? O11S Pb1 N123 C124 70.1(12) . . . . ? N163 Pb1 N123 C124 -41.6(9) . . . . ? N111 Pb1 N123 C124 8.7(8) . . . . ? O13X Pb1 N123 C124 94.8(9) . . . . ? N131 Pb1 N123 C124 179.5(9) . . . . ? N143 Pb1 N123 C124 -138.4(8) . . . . ? N122 N123 C124 C125 0.4(14) . . . . ? Pb1 N123 C124 C125 169.8(8) . . . . ? N122 N123 C124 C112 -179.9(11) . . . . ? Pb1 N123 C124 C112 -10.5(15) . . . . ? N111 C112 C124 N123 3.8(17) . . . . ? C113 C112 C124 N123 -177.8(12) . . . . ? N111 C112 C124 C125 -176.5(13) . . . . ? C113 C112 C124 C125 2(2) . . . . ? N122 N121 C125 C124 1.9(14) . . . . ? C126 N121 C125 C124 -179.8(12) . . . . ? N123 C124 C125 N121 -1.4(14) . . . . ? C112 C124 C125 N121 178.9(12) . . . . ? C125 N121 C126 C171 124.2(14) . . . . ? N122 N121 C126 C171 -57.6(15) . . . . ? N151 Pb1 N131 C132 64.3(9) . . . . ? O11S Pb1 N131 C132 -69.3(10) . . . . ? N163 Pb1 N131 C132 19.9(11) . . . . ? N111 Pb1 N131 C132 149.8(8) . . . . ? O13X Pb1 N131 C132 -143.5(9) . . . . ? N123 Pb1 N131 C132 137.9(9) . . . . ? N143 Pb1 N131 C132 -0.9(8) . . . . ? N151 Pb1 N131 C136 -119.8(10) . . . . ? O11S Pb1 N131 C136 106.5(10) . . . . ? N163 Pb1 N131 C136 -164.3(9) . . . . ? N111 Pb1 N131 C136 -34.4(12) . . . . ? O13X Pb1 N131 C136 32.3(10) . . . . ? N123 Pb1 N131 C136 -46.2(10) . . . . ? N143 Pb1 N131 C136 174.9(11) . . . . ? C136 N131 C132 C133 -1.7(19) . . . . ? Pb1 N131 C132 C133 174.1(9) . . . . ? C136 N131 C132 C144 -177.5(11) . . . . ? Pb1 N131 C132 C144 -1.7(14) . . . . ? N131 C132 C133 C134 1(2) . . . . ? C144 C132 C133 C134 177.1(13) . . . . ? C132 C133 C134 C135 0(2) . . . . ? C133 C134 C135 C136 -1(2) . . . . ? C132 N131 C136 C135 1(2) . . . . ? Pb1 N131 C136 C135 -175.2(11) . . . . ? C134 C135 C136 N131 0(2) . . . . ? C145 N141 N142 N143 0.4(13) . . . . ? C146 N141 N142 N143 -175.8(10) . . . . ? N141 N142 N143 C144 -1.2(12) . . . . ? N141 N142 N143 Pb1 -176.8(7) . . . . ? N151 Pb1 N143 N142 77.8(10) . . . . ? O11S Pb1 N143 N142 -61.9(10) . . . . ? N163 Pb1 N143 N142 12.5(10) . . . . ? N111 Pb1 N143 N142 43.1(13) . . . . ? O13X Pb1 N143 N142 -131.4(10) . . . . ? N123 Pb1 N143 N142 130.6(10) . . . . ? N131 Pb1 N143 N142 178.8(11) . . . . ? N151 Pb1 N143 C144 -97.4(8) . . . . ? O11S Pb1 N143 C144 122.8(8) . . . . ? N163 Pb1 N143 C144 -162.8(8) . . . . ? N111 Pb1 N143 C144 -132.2(8) . . . . ? O13X Pb1 N143 C144 53.4(9) . . . . ? N123 Pb1 N143 C144 -44.6(9) . . . . ? N131 Pb1 N143 C144 3.6(7) . . . . ? N142 N143 C144 C145 1.6(12) . . . . ? Pb1 N143 C144 C145 178.0(7) . . . . ? N142 N143 C144 C132 177.3(10) . . . . ? Pb1 N143 C144 C132 -6.4(13) . . . . ? N131 C132 C144 N143 5.5(16) . . . . ? C133 C132 C144 N143 -170.4(11) . . . . ? N131 C132 C144 C145 -180.0(11) . . . . ? C133 C132 C144 C145 4.1(19) . . . . ? N142 N141 C145 C144 0.6(13) . . . . ? C146 N141 C145 C144 176.4(11) . . . . ? N143 C144 C145 N141 -1.3(12) . . . . ? C132 C144 C145 N141 -176.5(11) . . . . ? C145 N141 C146 C173 71.0(18) . . . 4_575 ? N142 N141 C146 C173 -113.6(14) . . . 4_575 ? O11S Pb1 N151 C156 138.9(8) . . . . ? N163 Pb1 N151 C156 171.5(9) . . . . ? N111 Pb1 N151 C156 -114.9(8) . . . . ? O13X Pb1 N151 C156 -47.7(11) . . . . ? N123 Pb1 N151 C156 -53.8(8) . . . . ? N131 Pb1 N151 C156 22.1(8) . . . . ? N143 Pb1 N151 C156 80.9(8) . . . . ? O11S Pb1 N151 C152 -25.7(10) . . . . ? N163 Pb1 N151 C152 6.8(8) . . . . ? N111 Pb1 N151 C152 80.5(8) . . . . ? O13X Pb1 N151 C152 147.7(9) . . . . ? N123 Pb1 N151 C152 141.6(8) . . . . ? N131 Pb1 N151 C152 -142.5(8) . . . . ? N143 Pb1 N151 C152 -83.7(8) . . . . ? C156 N151 C152 C153 -0.8(17) . . . . ? Pb1 N151 C152 C153 163.7(10) . . . . ? C156 N151 C152 C164 -176.4(10) . . . . ? Pb1 N151 C152 C164 -11.9(14) . . . . ? N151 C152 C153 C154 2(2) . . . . ? C164 C152 C153 C154 177.0(15) . . . . ? C152 C153 C154 C155 -2(3) . . . . ? C153 C154 C155 C156 1(3) . . . . ? C152 N151 C156 C155 0.5(18) . . . . ? Pb1 N151 C156 C155 -163.9(11) . . . . ? C154 C155 C156 N151 -1(2) . . . . ? C165 N161 N162 N163 -1.3(14) . . . . ? C166 N161 N162 N163 -177.3(10) . . . . ? N161 N162 N163 C164 0.7(13) . . . . ? N161 N162 N163 Pb1 -176.3(8) . . . . ? N151 Pb1 N163 N162 175.6(11) . . . . ? O11S Pb1 N163 N162 -29.5(10) . . . . ? N111 Pb1 N163 N162 79.8(10) . . . . ? O13X Pb1 N163 N162 22.5(13) . . . . ? N123 Pb1 N163 N162 124.5(10) . . . . ? N131 Pb1 N163 N162 -133.2(10) . . . . ? N143 Pb1 N163 N162 -114.9(10) . . . . ? N151 Pb1 N163 C164 -1.4(8) . . . . ? O11S Pb1 N163 C164 153.6(10) . . . . ? N111 Pb1 N163 C164 -97.2(9) . . . . ? O13X Pb1 N163 C164 -154.4(8) . . . . ? N123 Pb1 N163 C164 -52.5(9) . . . . ? N131 Pb1 N163 C164 49.9(10) . . . . ? N143 Pb1 N163 C164 68.2(9) . . . . ? N162 N163 C164 C165 0.1(14) . . . . ? Pb1 N163 C164 C165 177.7(8) . . . . ? N162 N163 C164 C152 178.6(10) . . . . ? Pb1 N163 C164 C152 -3.8(14) . . . . ? N151 C152 C164 N163 10.7(17) . . . . ? C153 C152 C164 N163 -164.8(13) . . . . ? N151 C152 C164 C165 -171.3(13) . . . . ? C153 C152 C164 C165 13(2) . . . . ? N162 N161 C165 C164 1.3(15) . . . . ? C166 N161 C165 C164 176.8(11) . . . . ? N163 C164 C165 N161 -0.8(14) . . . . ? C152 C164 C165 N161 -179.0(13) . . . . ? C165 N161 C166 C175 73.9(18) . . . 1_455 ? N162 N161 C166 C175 -111.0(14) . . . 1_455 ? N121 C126 C171 C176 99.7(13) . . . . ? N121 C126 C171 C172 -73.8(15) . . . . ? C176 C171 C172 C173 -0.1(18) . . . . ? C126 C171 C172 C173 173.2(11) . . . . ? C171 C172 C173 C174 -0.3(18) . . . . ? C171 C172 C173 C146 -173.9(11) . . . 4_676 ? C172 C173 C174 C175 1.0(18) . . . . ? C146 C173 C174 C175 174.8(11) 4_676 . . . ? C173 C174 C175 C176 -1.2(17) . . . . ? C173 C174 C175 C166 -175.5(11) . . . 1_655 ? C172 C171 C176 C175 -0.1(17) . . . . ? C126 C171 C176 C175 -173.8(11) . . . . ? C174 C175 C176 C171 0.7(17) . . . . ? C166 C175 C176 C171 175.1(11) 1_655 . . . ? O14X Cl1X O13X Pb1 -10(3) . . . . ? O15X Cl1X O13X Pb1 -130(3) . . . . ? O12X Cl1X O13X Pb1 110(3) . . . . ? N151 Pb1 O13X Cl1X 160(3) . . . . ? O11S Pb1 O13X Cl1X -25(3) . . . . ? N163 Pb1 O13X Cl1X -75(3) . . . . ? N111 Pb1 O13X Cl1X -131(3) . . . . ? N123 Pb1 O13X Cl1X 166(3) . . . . ? N131 Pb1 O13X Cl1X 89(3) . . . . ? N143 Pb1 O13X Cl1X 47(3) . . . . ? N151 Pb1 O11S C13S 109(2) . . . . ? N163 Pb1 O11S C13S 78(2) . . . . ? N111 Pb1 O11S C13S 9(2) . . . . ? O13X Pb1 O11S C13S -68(2) . . . . ? N123 Pb1 O11S C13S -43(3) . . . . ? N131 Pb1 O11S C13S -144(2) . . . . ? N143 Pb1 O11S C13S 161(2) . . . . ? Pb1 O11S C13S N12S 156.2(18) . . . . ? C15S N12S C13S O11S 172(3) . . . . ? C14S N12S C13S O11S -15(4) . . . . ? C24S O21S C22S C23S 172.8(19) . . . . ? C22S O21S C24S C25S 179.0(19) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.647 _refine_diff_density_min -1.670 _refine_diff_density_rms 0.154 #===END data_imw1382_0m _database_code_depnum_ccdc_archive 'CCDC 778863' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H37 Cl2 N13 O9 Pb' _chemical_formula_weight 1073.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 'Pbca ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 17.4206(4) _cell_length_b 22.1469(5) _cell_length_c 24.5102(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9456.3(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6931 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 23.49 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.509 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4256 _exptl_absorpt_coefficient_mu 3.743 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3805 _exptl_absorpt_correction_T_max 0.5070 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 46102 _diffrn_reflns_av_R_equivalents 0.0594 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 25.76 _reflns_number_total 9032 _reflns_number_gt 5931 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a coordination polymer of formula {[Pb(L)(DMF)](ClO4)2}n. The data was solved by direct methods. The lattice contains to disordered perchlorate anions (Cl11 > O15 and Cl21 > O25). The anions display rotational disorder along the B11-F12 and B21-F22 bonds respectively (80:20 for both). Geometric and displacement restraints were applied improve the appearence of the disordered residues. Global displacement restraints were added to carbon and nitrogen atoms to remove the higher fluxionallity displayed by the rings N151 > C156 and N161 > C165. Attempts to split the residue over two sites were unsussesfull; the apparent higher fluxionallity may be a result of an ineffective absorption correction. The lattice contained a number of highly disordered solvent molecules that could be modelled as methanol disordered over four sites. Unfortunatally a stable refinement could not be obtained and so the corresponding electron density was eliminated by used of a Platon SQUEEZE function, details below. 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 0.163 0.149 0.790 214 55 ' ' 2 0.163 0.351 0.290 214 55 ' ' 3 -0.164 0.649 0.710 214 55 ' ' 4 -0.164 0.851 0.210 214 55 ' ' 5 0.336 0.851 0.290 214 55 ' ' 6 0.336 0.649 0.790 214 55 ' ' 7 0.664 0.149 0.710 214 55 ' ' 8 0.663 0.351 0.210 214 55 ' ' _platon_squeeze_details ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0946P)^2^+18.4494P] 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 9032 _refine_ls_number_parameters 535 _refine_ls_number_restraints 530 _refine_ls_R_factor_all 0.0936 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1832 _refine_ls_wR_factor_gt 0.1709 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.131 _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 0.530675(16) 0.734504(14) 0.569374(15) 0.03447(15) Uani 1 1 d . . . N111 N 0.6743(4) 0.6859(3) 0.5496(4) 0.0501(10) Uani 1 1 d U . . C112 C 0.7383(5) 0.7174(4) 0.5587(5) 0.0494(9) Uani 1 1 d U . . C113 C 0.8091(5) 0.6961(4) 0.5436(5) 0.0511(10) Uani 1 1 d U . . H113 H 0.8536 0.7204 0.5481 0.061 Uiso 1 1 calc R . . C114 C 0.8147(5) 0.6383(4) 0.5215(5) 0.0525(10) Uani 1 1 d U . . H114 H 0.8636 0.6223 0.5121 0.063 Uiso 1 1 calc R . . C115 C 0.7500(5) 0.6046(4) 0.5132(5) 0.0526(11) Uani 1 1 d U . . H115 H 0.7524 0.5651 0.4981 0.063 Uiso 1 1 calc R . . C116 C 0.6806(5) 0.6308(4) 0.5277(5) 0.0515(10) Uani 1 1 d U . . H116 H 0.6350 0.6082 0.5219 0.062 Uiso 1 1 calc R . . N121 N 0.7360(4) 0.8675(3) 0.6152(3) 0.0448(8) Uani 1 1 d U . . N122 N 0.6616(4) 0.8522(3) 0.6172(4) 0.0460(9) Uani 1 1 d U . . N123 N 0.6575(4) 0.7970(3) 0.5971(4) 0.0467(9) Uani 1 1 d U . . C124 C 0.7278(5) 0.7782(4) 0.5823(5) 0.0473(8) Uani 1 1 d U . . C125 C 0.7785(5) 0.8231(4) 0.5934(5) 0.0461(9) Uani 1 1 d U . . H125 H 0.8323 0.8231 0.5870 0.055 Uiso 1 1 calc R . . C126 C 0.7585(5) 0.9295(4) 0.6310(4) 0.0434(8) Uani 1 1 d U . . H12A H 0.7267 0.9428 0.6623 0.052 Uiso 1 1 calc R . . H12B H 0.7489 0.9573 0.6002 0.052 Uiso 1 1 calc R . . N131 N 0.3799(4) 0.7234(3) 0.5913(4) 0.0412(9) Uani 1 1 d U . . C132 C 0.3454(5) 0.6688(4) 0.5923(4) 0.0398(8) Uani 1 1 d U . . C133 C 0.2669(5) 0.6643(4) 0.6021(4) 0.0414(9) Uani 1 1 d U . . H133 H 0.2431 0.6257 0.6043 0.050 Uiso 1 1 calc R . . C134 C 0.2244(5) 0.7150(4) 0.6084(4) 0.0424(10) Uani 1 1 d U . . H134 H 0.1706 0.7121 0.6144 0.051 Uiso 1 1 calc R . . C135 C 0.2591(5) 0.7709(4) 0.6060(4) 0.0424(10) Uani 1 1 d U . . H135 H 0.2301 0.8068 0.6110 0.051 Uiso 1 1 calc R . . C136 C 0.3366(5) 0.7734(4) 0.5963(5) 0.0420(9) Uani 1 1 d U . . H136 H 0.3605 0.8118 0.5930 0.050 Uiso 1 1 calc R . . N141 N 0.4466(4) 0.5287(3) 0.5792(3) 0.0363(8) Uani 1 1 d U . . N142 N 0.5008(4) 0.5684(3) 0.5656(3) 0.0357(8) Uani 1 1 d U . . N143 N 0.4692(3) 0.6220(3) 0.5701(3) 0.0361(8) Uani 1 1 d U . . C144 C 0.3949(4) 0.6165(4) 0.5861(4) 0.0373(8) Uani 1 1 d U . . C145 C 0.3801(5) 0.5566(4) 0.5924(4) 0.0369(8) Uani 1 1 d U . . H145 H 0.3334 0.5384 0.6037 0.044 Uiso 1 1 calc R . . C146 C 0.4654(4) 0.4638(4) 0.5799(4) 0.0365(10) Uani 1 1 d U . . H14A H 0.4848 0.4514 0.5436 0.044 Uiso 1 1 calc R . . H14B H 0.4185 0.4401 0.5877 0.044 Uiso 1 1 calc R . . N151 N 0.5675(6) 0.6810(4) 0.6660(4) 0.0620(11) Uani 1 1 d U . . C152 C 0.5561(7) 0.7119(5) 0.7137(5) 0.0612(10) Uani 1 1 d U . . C153 C 0.5766(7) 0.6888(4) 0.7628(5) 0.0651(11) Uani 1 1 d U . . H153 H 0.5744 0.7133 0.7946 0.078 Uiso 1 1 calc R . . C154 C 0.6008(7) 0.6291(5) 0.7666(5) 0.0669(12) Uani 1 1 d U . . H154 H 0.6080 0.6105 0.8011 0.080 Uiso 1 1 calc R . . C155 C 0.6142(7) 0.5974(5) 0.7187(5) 0.0665(12) Uani 1 1 d U . . H155 H 0.6356 0.5580 0.7194 0.080 Uiso 1 1 calc R . . C156 C 0.5957(7) 0.6249(4) 0.6704(5) 0.0642(11) Uani 1 1 d U . . H156 H 0.6033 0.6026 0.6377 0.077 Uiso 1 1 calc R . . N161 N 0.4851(5) 0.8643(3) 0.7103(4) 0.0531(10) Uani 1 1 d U . . N162 N 0.4811(5) 0.8483(3) 0.6586(4) 0.0522(10) Uani 1 1 d U . . N163 N 0.5055(5) 0.7929(4) 0.6563(4) 0.0530(10) Uani 1 1 d U . . C164 C 0.5260(6) 0.7737(4) 0.7047(5) 0.0561(10) Uani 1 1 d U . . C165 C 0.5126(6) 0.8197(4) 0.7410(5) 0.0550(10) Uani 1 1 d U . . H165 H 0.5211 0.8197 0.7793 0.066 Uiso 1 1 calc R . . C166 C 0.4635(6) 0.9264(4) 0.7250(4) 0.0533(12) Uani 1 1 d U . . H16A H 0.4201 0.9394 0.7017 0.064 Uiso 1 1 calc R . . H16B H 0.5074 0.9536 0.7176 0.064 Uiso 1 1 calc R . . C171 C 0.8429(5) 0.9322(4) 0.6468(4) 0.0417(8) Uani 1 1 d U . . C172 C 0.8966(5) 0.9453(4) 0.6069(4) 0.0398(8) Uani 1 1 d U . . C173 C 0.9746(5) 0.9505(4) 0.6226(4) 0.0396(9) Uani 1 1 d U . . C174 C 0.9966(5) 0.9443(4) 0.6767(4) 0.0409(9) Uani 1 1 d U . . C175 C 0.9408(5) 0.9320(4) 0.7159(4) 0.0420(9) Uani 1 1 d U . . C176 C 0.8624(5) 0.9233(4) 0.7017(4) 0.0426(9) Uani 1 1 d U . . C177 C 0.8751(5) 0.9515(4) 0.5474(4) 0.0409(13) Uani 1 1 d U . . H17A H 0.8974 0.9180 0.5266 0.061 Uiso 1 1 calc R . . H17B H 0.8950 0.9898 0.5332 0.061 Uiso 1 1 calc R . . H17C H 0.8191 0.9508 0.5437 0.061 Uiso 1 1 calc R . . C178 C 1.0801(5) 0.9498(4) 0.6919(4) 0.0441(14) Uani 1 1 d U . . H17D H 1.1117 0.9305 0.6637 0.066 Uiso 1 1 calc R . . H17E H 1.0890 0.9298 0.7270 0.066 Uiso 1 1 calc R . . H17F H 1.0939 0.9925 0.6948 0.066 Uiso 1 1 calc R . . C179 C 0.8054(5) 0.9030(4) 0.7435(4) 0.0488(14) Uani 1 1 d U . . H17G H 0.7793 0.9383 0.7590 0.073 Uiso 1 1 calc R . . H17H H 0.8320 0.8810 0.7725 0.073 Uiso 1 1 calc R . . H17I H 0.7675 0.8764 0.7262 0.073 Uiso 1 1 calc R . . Cl11 Cl 0.51376(13) 0.71112(11) 0.40714(11) 0.0523(6) Uiso 1 1 d DU . . O12 O 0.5764(2) 0.6784(2) 0.3829(2) 0.0613(17) Uiso 1 1 d DU A . O13X O 0.4494(3) 0.7122(3) 0.3694(2) 0.0587(19) Uiso 0.799(9) 1 d PDU A 1 O14X O 0.4887(4) 0.6824(3) 0.4565(2) 0.0624(19) Uiso 0.799(9) 1 d PDU A 1 O15X O 0.5353(4) 0.77224(16) 0.4186(3) 0.063(2) Uiso 0.799(9) 1 d PDU A 1 O13Y O 0.4741(10) 0.7461(9) 0.3665(3) 0.060(2) Uiso 0.201(9) 1 d PDU A 2 O14Y O 0.5421(5) 0.7517(9) 0.4486(8) 0.059(2) Uiso 0.201(9) 1 d PDU A 2 O15Y O 0.4601(8) 0.6702(3) 0.4320(9) 0.058(2) Uiso 0.201(9) 1 d PDU A 2 Cl21 Cl 0.68067(13) 0.48871(10) 0.88447(10) 0.0521(6) Uiso 1 1 d DU . . O22 O 0.7163(3) 0.5098(2) 0.93391(15) 0.0489(15) Uiso 1 1 d DU B . O23X O 0.7171(4) 0.5146(3) 0.83728(18) 0.0582(16) Uiso 0.795(6) 1 d PDU B 1 O24X O 0.60065(17) 0.5068(3) 0.8832(3) 0.0627(17) Uiso 0.795(6) 1 d PDU B 1 O25X O 0.6836(4) 0.42437(13) 0.8802(3) 0.0619(17) Uiso 0.795(6) 1 d PDU B 1 O23Y O 0.6470(10) 0.5378(3) 0.8545(5) 0.060(2) Uiso 0.205(6) 1 d PDU B 2 O24Y O 0.6212(8) 0.4455(7) 0.8963(3) 0.058(2) Uiso 0.205(6) 1 d PDU B 2 O25Y O 0.7362(4) 0.4596(8) 0.8497(4) 0.060(2) Uiso 0.205(6) 1 d PDU B 2 O11S O 0.4822(3) 0.8370(3) 0.5347(3) 0.0461(17) Uani 1 1 d . . . N12S N 0.5591(5) 0.9173(4) 0.5212(4) 0.0597(15) Uani 1 1 d U . . C13S C 0.5031(6) 0.8882(5) 0.5451(5) 0.0589(16) Uani 1 1 d U . . H13S H 0.4763 0.9089 0.5732 0.071 Uiso 1 1 calc R . . C14S C 0.5822(6) 0.9776(4) 0.5367(5) 0.0610(18) Uani 1 1 d U . . H14C H 0.5416 0.9963 0.5587 0.092 Uiso 1 1 calc R . . H14D H 0.5909 1.0018 0.5038 0.092 Uiso 1 1 calc R . . H14E H 0.6296 0.9756 0.5581 0.092 Uiso 1 1 calc R . . C15S C 0.6124(6) 0.8854(5) 0.4865(5) 0.0662(19) Uani 1 1 d U . . H15A H 0.6050 0.8418 0.4908 0.099 Uiso 1 1 calc R . . H15B H 0.6651 0.8960 0.4968 0.099 Uiso 1 1 calc R . . H15C H 0.6034 0.8967 0.4484 0.099 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02437(19) 0.0233(2) 0.0557(3) -0.00655(15) 0.00523(15) -0.00180(13) N111 0.0325(17) 0.0328(18) 0.085(2) -0.0172(18) 0.0123(18) -0.0038(15) C112 0.0321(15) 0.0321(16) 0.084(2) -0.0159(16) 0.0113(16) -0.0033(14) C113 0.0333(17) 0.0334(18) 0.087(2) -0.0161(18) 0.0142(18) -0.0035(16) C114 0.0348(18) 0.0342(19) 0.088(3) -0.0168(19) 0.016(2) -0.0033(17) C115 0.0355(18) 0.0340(19) 0.088(3) -0.017(2) 0.015(2) -0.0037(17) C116 0.0342(18) 0.0335(19) 0.087(3) -0.0177(19) 0.0136(19) -0.0041(17) N121 0.0304(14) 0.0280(14) 0.076(2) -0.0119(15) 0.0041(15) -0.0017(13) N122 0.0305(15) 0.0293(16) 0.078(2) -0.0134(16) 0.0047(16) -0.0023(14) N123 0.0307(15) 0.0300(16) 0.080(2) -0.0143(17) 0.0061(16) -0.0024(14) C124 0.0310(14) 0.0304(15) 0.081(2) -0.0141(15) 0.0074(15) -0.0025(13) C125 0.0306(15) 0.0291(16) 0.078(2) -0.0128(16) 0.0058(16) -0.0015(14) C126 0.0323(15) 0.0263(15) 0.071(2) -0.0099(16) 0.0014(15) -0.0012(14) N131 0.0277(16) 0.0277(15) 0.068(2) -0.0017(17) 0.0045(17) 0.0020(13) C132 0.0259(14) 0.0274(14) 0.066(2) -0.0017(16) 0.0047(15) 0.0018(12) C133 0.0263(15) 0.0294(17) 0.068(2) -0.0020(18) 0.0043(17) 0.0025(14) C134 0.0270(17) 0.0306(17) 0.069(2) -0.0021(19) 0.0042(18) 0.0036(14) C135 0.0276(17) 0.0301(17) 0.070(2) -0.0021(19) 0.0041(19) 0.0040(15) C136 0.0280(17) 0.0288(16) 0.069(2) -0.0019(18) 0.0042(18) 0.0030(15) N141 0.0242(15) 0.0240(15) 0.061(2) -0.0009(16) 0.0063(16) -0.0012(13) N142 0.0236(15) 0.0236(16) 0.060(2) -0.0014(17) 0.0055(16) -0.0012(13) N143 0.0239(15) 0.0239(15) 0.060(2) -0.0012(16) 0.0053(16) -0.0009(13) C144 0.0242(14) 0.0253(14) 0.062(2) -0.0016(15) 0.0055(15) -0.0002(12) C145 0.0241(15) 0.0251(15) 0.062(2) -0.0012(17) 0.0062(16) -0.0008(13) C146 0.0249(19) 0.0237(17) 0.061(3) -0.001(2) 0.007(2) -0.0011(17) N151 0.097(3) 0.0318(18) 0.057(2) -0.0033(17) -0.016(2) 0.010(2) C152 0.096(2) 0.0318(17) 0.056(2) -0.0024(15) -0.015(2) 0.0092(18) C153 0.102(3) 0.0351(19) 0.058(2) -0.0019(17) -0.016(2) 0.011(2) C154 0.105(3) 0.036(2) 0.060(2) -0.0016(18) -0.017(2) 0.013(2) C155 0.104(3) 0.035(2) 0.060(3) -0.0021(18) -0.018(2) 0.012(2) C156 0.100(3) 0.0331(19) 0.059(2) -0.0031(18) -0.017(2) 0.012(2) N161 0.081(2) 0.0270(17) 0.051(2) -0.0017(16) -0.008(2) 0.0035(18) N162 0.079(2) 0.0266(18) 0.051(2) -0.0016(16) -0.008(2) 0.0038(18) N163 0.080(2) 0.0269(17) 0.052(2) -0.0017(16) -0.009(2) 0.0043(18) C164 0.087(2) 0.0290(16) 0.053(2) -0.0019(15) -0.011(2) 0.0055(17) C165 0.085(2) 0.0284(17) 0.052(2) -0.0015(16) -0.009(2) 0.0043(18) C166 0.081(3) 0.027(2) 0.051(3) -0.0023(19) -0.006(2) 0.003(2) C171 0.0342(14) 0.0237(15) 0.067(2) -0.0070(15) -0.0011(15) -0.0007(13) C172 0.0332(16) 0.0215(16) 0.065(2) -0.0054(17) -0.0029(15) 0.0000(15) C173 0.0344(16) 0.0205(17) 0.064(2) -0.0043(18) -0.0041(16) 0.0003(16) C174 0.0369(16) 0.0213(17) 0.064(2) -0.0037(18) -0.0046(16) 0.0004(16) C175 0.0386(16) 0.0223(17) 0.065(2) -0.0046(18) -0.0032(16) 0.0002(16) C176 0.0377(16) 0.0236(16) 0.067(2) -0.0056(17) -0.0007(16) -0.0008(15) C177 0.033(3) 0.025(3) 0.065(2) -0.005(3) -0.004(2) 0.002(3) C178 0.040(2) 0.027(3) 0.065(3) -0.001(3) -0.009(2) -0.002(3) C179 0.046(3) 0.031(3) 0.069(3) -0.006(3) 0.005(2) -0.003(3) O11S 0.041(3) 0.038(4) 0.060(5) 0.003(3) -0.004(3) -0.001(3) N12S 0.050(3) 0.042(3) 0.087(5) 0.002(3) 0.002(3) -0.006(2) C13S 0.049(3) 0.041(3) 0.086(5) 0.003(3) 0.001(3) -0.005(3) C14S 0.052(4) 0.042(3) 0.088(5) 0.004(3) -0.003(4) -0.007(3) C15S 0.057(4) 0.049(4) 0.093(5) 0.000(3) 0.007(3) -0.005(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 N163 2.531(9) . ? Pb1 O11S 2.567(6) . ? Pb1 N131 2.693(7) . ? Pb1 N123 2.695(7) . ? Pb1 N143 2.711(7) . ? Pb1 N151 2.726(9) . ? Pb1 N111 2.766(7) . ? N111 C112 1.334(11) . ? N111 C116 1.338(11) . ? C112 C113 1.371(12) . ? C112 C124 1.476(12) . ? C113 C114 1.394(12) . ? C113 H113 0.9500 . ? C114 C115 1.368(12) . ? C114 H114 0.9500 . ? C115 C116 1.387(12) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 N122 1.342(9) . ? N121 C125 1.343(11) . ? N121 C126 1.478(10) . ? N122 N123 1.319(10) . ? N123 C124 1.344(11) . ? C124 C125 1.358(12) . ? C125 H125 0.9500 . ? C126 C171 1.522(12) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N131 C136 1.344(10) . ? N131 C132 1.352(11) . ? C132 C133 1.393(11) . ? C132 C144 1.451(11) . ? C133 C134 1.354(11) . ? C133 H133 0.9500 . ? C134 C135 1.378(12) . ? C134 H134 0.9500 . ? C135 C136 1.372(12) . ? C135 H135 0.9500 . ? C136 H136 0.9500 . ? N141 N142 1.332(10) . ? N141 C145 1.353(10) . ? N141 C146 1.474(11) . ? N142 N143 1.314(10) . ? N143 C144 1.359(9) . ? C144 C145 1.360(11) . ? C145 H145 0.9500 . ? C146 C173 1.508(12) 6_755 ? C146 H14A 0.9900 . ? C146 H14B 0.9900 . ? N151 C156 1.339(12) . ? N151 C152 1.369(14) . ? C152 C153 1.356(15) . ? C152 C164 1.481(14) . ? C153 C154 1.390(14) . ? C153 H153 0.9500 . ? C154 C155 1.387(15) . ? C154 H154 0.9500 . ? C155 C156 1.370(15) . ? C155 H155 0.9500 . ? C156 H156 0.9500 . ? N161 N162 1.317(12) . ? N161 C165 1.329(12) . ? N161 C166 1.471(12) . ? N162 N163 1.299(10) . ? N163 C164 1.310(14) . ? C164 C165 1.374(14) . ? C165 H165 0.9500 . ? C166 C175 1.508(14) 8_557 ? C166 H16A 0.9900 . ? C166 H16B 0.9900 . ? C171 C172 1.383(13) . ? C171 C176 1.401(14) . ? C172 C173 1.416(11) . ? C172 C177 1.514(14) . ? C173 C174 1.388(13) . ? C173 C146 1.508(12) 6_765 ? C174 C175 1.393(13) . ? C174 C178 1.507(12) . ? C175 C176 1.423(12) . ? C175 C166 1.508(14) 8_657 ? C176 C179 1.496(13) . ? C177 H17A 0.9800 . ? C177 H17B 0.9800 . ? C177 H17C 0.9800 . ? C178 H17D 0.9800 . ? C178 H17E 0.9800 . ? C178 H17F 0.9800 . ? C179 H17G 0.9800 . ? C179 H17H 0.9800 . ? C179 H17I 0.9800 . ? Cl11 O15X 1.4320(18) . ? Cl11 O14X 1.4343(18) . ? Cl11 O12 1.438(2) . ? Cl11 O13Y 1.4386(19) . ? Cl11 O15Y 1.4387(19) . ? Cl11 O14Y 1.4421(19) . ? Cl11 O13X 1.4534(18) . ? Cl21 O25X 1.4297(18) . ? Cl21 O23Y 1.4363(19) . ? Cl21 O23X 1.4385(18) . ? Cl21 O22 1.439(2) . ? Cl21 O24Y 1.4401(19) . ? Cl21 O25Y 1.4422(19) . ? Cl21 O24X 1.4506(18) . ? O11S C13S 1.217(12) . ? N12S C13S 1.307(13) . ? N12S C15S 1.445(13) . ? N12S C14S 1.446(12) . ? C13S H13S 0.9500 . ? C14S H14C 0.9800 . ? C14S H14D 0.9800 . ? C14S H14E 0.9800 . ? C15S H15A 0.9800 . ? C15S H15B 0.9800 . ? C15S H15C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N163 Pb1 O11S 76.7(2) . . ? N163 Pb1 N131 73.1(3) . . ? O11S Pb1 N131 80.0(2) . . ? N163 Pb1 N123 70.5(3) . . ? O11S Pb1 N123 84.2(2) . . ? N131 Pb1 N123 142.8(2) . . ? N163 Pb1 N143 113.3(3) . . ? O11S Pb1 N143 133.2(2) . . ? N131 Pb1 N143 61.9(2) . . ? N123 Pb1 N143 142.6(2) . . ? N163 Pb1 N151 62.1(3) . . ? O11S Pb1 N151 138.6(2) . . ? N131 Pb1 N151 90.9(3) . . ? N123 Pb1 N151 79.1(3) . . ? N143 Pb1 N151 71.8(2) . . ? N163 Pb1 N111 120.2(3) . . ? O11S Pb1 N111 125.7(2) . . ? N131 Pb1 N111 151.9(2) . . ? N123 Pb1 N111 60.2(2) . . ? N143 Pb1 N111 90.1(2) . . ? N151 Pb1 N111 76.7(3) . . ? C112 N111 C116 118.3(8) . . ? C112 N111 Pb1 121.6(6) . . ? C116 N111 Pb1 120.0(6) . . ? N111 C112 C113 121.8(8) . . ? N111 C112 C124 116.0(8) . . ? C113 C112 C124 122.1(8) . . ? C112 C113 C114 119.0(9) . . ? C112 C113 H113 120.5 . . ? C114 C113 H113 120.5 . . ? C115 C114 C113 120.1(8) . . ? C115 C114 H114 119.9 . . ? C113 C114 H114 119.9 . . ? C114 C115 C116 116.8(8) . . ? C114 C115 H115 121.6 . . ? C116 C115 H115 121.6 . . ? N111 C116 C115 123.8(8) . . ? N111 C116 H116 118.1 . . ? C115 C116 H116 118.1 . . ? N122 N121 C125 111.2(7) . . ? N122 N121 C126 118.8(7) . . ? C125 N121 C126 129.7(7) . . ? N123 N122 N121 105.8(6) . . ? N122 N123 C124 109.9(7) . . ? N122 N123 Pb1 127.9(5) . . ? C124 N123 Pb1 121.3(6) . . ? N123 C124 C125 108.1(8) . . ? N123 C124 C112 120.2(8) . . ? C125 C124 C112 131.7(8) . . ? N121 C125 C124 105.0(7) . . ? N121 C125 H125 127.5 . . ? C124 C125 H125 127.5 . . ? N121 C126 C171 111.1(7) . . ? N121 C126 H12A 109.4 . . ? C171 C126 H12A 109.4 . . ? N121 C126 H12B 109.4 . . ? C171 C126 H12B 109.4 . . ? H12A C126 H12B 108.0 . . ? C136 N131 C132 119.1(7) . . ? C136 N131 Pb1 119.4(6) . . ? C132 N131 Pb1 121.2(5) . . ? N131 C132 C133 120.2(8) . . ? N131 C132 C144 116.7(7) . . ? C133 C132 C144 123.0(8) . . ? C134 C133 C132 119.8(8) . . ? C134 C133 H133 120.1 . . ? C132 C133 H133 120.1 . . ? C133 C134 C135 120.0(8) . . ? C133 C134 H134 120.0 . . ? C135 C134 H134 120.0 . . ? C136 C135 C134 118.4(8) . . ? C136 C135 H135 120.8 . . ? C134 C135 H135 120.8 . . ? N131 C136 C135 122.3(8) . . ? N131 C136 H136 118.9 . . ? C135 C136 H136 118.9 . . ? N142 N141 C145 111.4(7) . . ? N142 N141 C146 119.3(6) . . ? C145 N141 C146 129.3(7) . . ? N143 N142 N141 106.3(6) . . ? N142 N143 C144 110.0(7) . . ? N142 N143 Pb1 131.7(5) . . ? C144 N143 Pb1 117.5(5) . . ? N143 C144 C145 107.5(7) . . ? N143 C144 C132 121.6(8) . . ? C145 C144 C132 130.8(8) . . ? N141 C145 C144 104.9(7) . . ? N141 C145 H145 127.6 . . ? C144 C145 H145 127.6 . . ? N141 C146 C173 110.6(7) . 6_755 ? N141 C146 H14A 109.5 . . ? C173 C146 H14A 109.5 6_755 . ? N141 C146 H14B 109.5 . . ? C173 C146 H14B 109.5 6_755 . ? H14A C146 H14B 108.1 . . ? C156 N151 C152 116.7(9) . . ? C156 N151 Pb1 124.0(7) . . ? C152 N151 Pb1 119.3(6) . . ? C153 C152 N151 122.0(10) . . ? C153 C152 C164 125.0(10) . . ? N151 C152 C164 112.7(9) . . ? C152 C153 C154 119.8(11) . . ? C152 C153 H153 120.1 . . ? C154 C153 H153 120.1 . . ? C155 C154 C153 118.4(11) . . ? C155 C154 H154 120.8 . . ? C153 C154 H154 120.8 . . ? C156 C155 C154 117.8(10) . . ? C156 C155 H155 121.1 . . ? C154 C155 H155 121.1 . . ? N151 C156 C155 124.6(11) . . ? N151 C156 H156 117.7 . . ? C155 C156 H156 117.7 . . ? N162 N161 C165 111.4(8) . . ? N162 N161 C166 118.2(8) . . ? C165 N161 C166 130.4(9) . . ? N163 N162 N161 106.1(8) . . ? N162 N163 C164 110.9(9) . . ? N162 N163 Pb1 125.2(7) . . ? C164 N163 Pb1 123.2(7) . . ? N163 C164 C165 107.3(9) . . ? N163 C164 C152 122.2(10) . . ? C165 C164 C152 130.5(10) . . ? N161 C165 C164 104.2(10) . . ? N161 C165 H165 127.9 . . ? C164 C165 H165 127.9 . . ? N161 C166 C175 112.3(8) . 8_557 ? N161 C166 H16A 109.1 . . ? C175 C166 H16A 109.1 8_557 . ? N161 C166 H16B 109.1 . . ? C175 C166 H16B 109.1 8_557 . ? H16A C166 H16B 107.9 . . ? C172 C171 C176 122.9(8) . . ? C172 C171 C126 118.8(9) . . ? C176 C171 C126 118.2(9) . . ? C171 C172 C173 118.3(9) . . ? C171 C172 C177 122.3(8) . . ? C173 C172 C177 119.4(8) . . ? C174 C173 C172 121.0(9) . . ? C174 C173 C146 119.4(8) . 6_765 ? C172 C173 C146 119.5(9) . 6_765 ? C173 C174 C175 119.0(8) . . ? C173 C174 C178 119.7(9) . . ? C175 C174 C178 121.3(9) . . ? C174 C175 C176 121.8(10) . . ? C174 C175 C166 119.7(9) . 8_657 ? C176 C175 C166 118.5(9) . 8_657 ? C171 C176 C175 116.7(9) . . ? C171 C176 C179 122.6(8) . . ? C175 C176 C179 120.7(9) . . ? C172 C177 H17A 109.5 . . ? C172 C177 H17B 109.5 . . ? H17A C177 H17B 109.5 . . ? C172 C177 H17C 109.5 . . ? H17A C177 H17C 109.5 . . ? H17B C177 H17C 109.5 . . ? C174 C178 H17D 109.5 . . ? C174 C178 H17E 109.5 . . ? H17D C178 H17E 109.5 . . ? C174 C178 H17F 109.5 . . ? H17D C178 H17F 109.5 . . ? H17E C178 H17F 109.5 . . ? C176 C179 H17G 109.5 . . ? C176 C179 H17H 109.5 . . ? H17G C179 H17H 109.5 . . ? C176 C179 H17I 109.5 . . ? H17G C179 H17I 109.5 . . ? H17H C179 H17I 109.5 . . ? O15X Cl11 O14X 109.5(3) . . ? O15X Cl11 O12 111.0(2) . . ? O14X Cl11 O12 110.8(2) . . ? O15X Cl11 O13Y 75.7(9) . . ? O14X Cl11 O13Y 132.5(6) . . ? O12 Cl11 O13Y 110.5(3) . . ? O15X Cl11 O15Y 133.1(6) . . ? O14X Cl11 O15Y 33.4(9) . . ? O12 Cl11 O15Y 110.5(3) . . ? O13Y Cl11 O15Y 108.7(3) . . ? O15X Cl11 O14Y 35.4(9) . . ? O14X Cl11 O14Y 77.7(9) . . ? O12 Cl11 O14Y 110.2(3) . . ? O13Y Cl11 O14Y 108.5(3) . . ? O15Y Cl11 O14Y 108.4(3) . . ? O15X Cl11 O13X 108.1(2) . . ? O14X Cl11 O13X 108.0(2) . . ? O12 Cl11 O13X 109.3(2) . . ? O13Y Cl11 O13X 34.9(9) . . ? O15Y Cl11 O13X 77.2(9) . . ? O14Y Cl11 O13X 134.5(6) . . ? O25X Cl21 O23Y 137.0(5) . . ? O25X Cl21 O23X 108.8(3) . . ? O23Y Cl21 O23X 57.9(8) . . ? O25X Cl21 O22 111.7(3) . . ? O23Y Cl21 O22 111.2(3) . . ? O23X Cl21 O22 110.9(3) . . ? O25X Cl21 O24Y 51.6(8) . . ? O23Y Cl21 O24Y 108.2(3) . . ? O23X Cl21 O24Y 138.1(5) . . ? O22 Cl21 O24Y 110.8(3) . . ? O25X Cl21 O25Y 59.2(8) . . ? O23Y Cl21 O25Y 108.0(3) . . ? O23X Cl21 O25Y 53.5(8) . . ? O22 Cl21 O25Y 110.7(3) . . ? O24Y Cl21 O25Y 107.8(3) . . ? O25X Cl21 O24X 107.9(3) . . ? O23Y Cl21 O24X 52.3(8) . . ? O23X Cl21 O24X 107.3(3) . . ? O22 Cl21 O24X 110.1(3) . . ? O24Y Cl21 O24X 59.7(8) . . ? O25Y Cl21 O24X 139.1(5) . . ? C13S O11S Pb1 130.9(7) . . ? C13S N12S C15S 120.1(9) . . ? C13S N12S C14S 123.1(10) . . ? C15S N12S C14S 115.3(8) . . ? O11S C13S N12S 126.1(12) . . ? O11S C13S H13S 117.0 . . ? N12S C13S H13S 117.0 . . ? N12S C14S H14C 109.5 . . ? N12S C14S H14D 109.5 . . ? H14C C14S H14D 109.5 . . ? N12S C14S H14E 109.5 . . ? H14C C14S H14E 109.5 . . ? H14D C14S H14E 109.5 . . ? N12S C15S H15A 109.5 . . ? N12S C15S H15B 109.5 . . ? H15A C15S H15B 109.5 . . ? N12S C15S H15C 109.5 . . ? H15A C15S H15C 109.5 . . ? H15B C15S H15C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N163 Pb1 N111 C112 -44.2(9) . . . . ? O11S Pb1 N111 C112 50.9(9) . . . . ? N131 Pb1 N111 C112 -156.3(8) . . . . ? N123 Pb1 N111 C112 -5.4(8) . . . . ? N143 Pb1 N111 C112 -161.5(9) . . . . ? N151 Pb1 N111 C112 -90.3(9) . . . . ? N163 Pb1 N111 C116 139.1(8) . . . . ? O11S Pb1 N111 C116 -125.7(8) . . . . ? N131 Pb1 N111 C116 27.0(12) . . . . ? N123 Pb1 N111 C116 178.0(10) . . . . ? N143 Pb1 N111 C116 21.8(8) . . . . ? N151 Pb1 N111 C116 93.1(9) . . . . ? C116 N111 C112 C113 3.8(17) . . . . ? Pb1 N111 C112 C113 -172.9(9) . . . . ? C116 N111 C112 C124 179.4(10) . . . . ? Pb1 N111 C112 C124 2.7(13) . . . . ? N111 C112 C113 C114 -4.5(18) . . . . ? C124 C112 C113 C114 -179.8(11) . . . . ? C112 C113 C114 C115 2.5(18) . . . . ? C113 C114 C115 C116 0.0(17) . . . . ? C112 N111 C116 C115 -1.2(17) . . . . ? Pb1 N111 C116 C115 175.6(9) . . . . ? C114 C115 C116 N111 -0.7(18) . . . . ? C125 N121 N122 N123 1.0(11) . . . . ? C126 N121 N122 N123 175.2(9) . . . . ? N121 N122 N123 C124 -0.5(12) . . . . ? N121 N122 N123 Pb1 -169.2(6) . . . . ? N163 Pb1 N123 N122 -39.6(8) . . . . ? O11S Pb1 N123 N122 38.3(8) . . . . ? N131 Pb1 N123 N122 -26.7(11) . . . . ? N143 Pb1 N123 N122 -142.8(7) . . . . ? N151 Pb1 N123 N122 -103.6(9) . . . . ? N111 Pb1 N123 N122 175.6(10) . . . . ? N163 Pb1 N123 C124 152.9(9) . . . . ? O11S Pb1 N123 C124 -129.2(8) . . . . ? N131 Pb1 N123 C124 165.8(7) . . . . ? N143 Pb1 N123 C124 49.6(10) . . . . ? N151 Pb1 N123 C124 88.8(8) . . . . ? N111 Pb1 N123 C124 8.0(8) . . . . ? N122 N123 C124 C125 -0.1(13) . . . . ? Pb1 N123 C124 C125 169.5(7) . . . . ? N122 N123 C124 C112 179.8(10) . . . . ? Pb1 N123 C124 C112 -10.6(14) . . . . ? N111 C112 C124 N123 5.1(16) . . . . ? C113 C112 C124 N123 -179.3(11) . . . . ? N111 C112 C124 C125 -175.1(12) . . . . ? C113 C112 C124 C125 1(2) . . . . ? N122 N121 C125 C124 -1.0(12) . . . . ? C126 N121 C125 C124 -174.4(10) . . . . ? N123 C124 C125 N121 0.6(13) . . . . ? C112 C124 C125 N121 -179.2(12) . . . . ? N122 N121 C126 C171 158.7(9) . . . . ? C125 N121 C126 C171 -28.3(15) . . . . ? N163 Pb1 N131 C136 57.2(8) . . . . ? O11S Pb1 N131 C136 -21.8(8) . . . . ? N123 Pb1 N131 C136 44.5(10) . . . . ? N143 Pb1 N131 C136 -173.7(9) . . . . ? N151 Pb1 N131 C136 117.6(8) . . . . ? N111 Pb1 N131 C136 -179.6(7) . . . . ? N163 Pb1 N131 C132 -129.2(8) . . . . ? O11S Pb1 N131 C132 151.8(8) . . . . ? N123 Pb1 N131 C132 -141.9(7) . . . . ? N143 Pb1 N131 C132 -0.1(7) . . . . ? N151 Pb1 N131 C132 -68.9(8) . . . . ? N111 Pb1 N131 C132 -6.0(12) . . . . ? C136 N131 C132 C133 -4.4(16) . . . . ? Pb1 N131 C132 C133 -178.0(7) . . . . ? C136 N131 C132 C144 179.3(9) . . . . ? Pb1 N131 C132 C144 5.7(13) . . . . ? N131 C132 C133 C134 2.8(16) . . . . ? C144 C132 C133 C134 178.9(10) . . . . ? C132 C133 C134 C135 -1.1(16) . . . . ? C133 C134 C135 C136 1.1(16) . . . . ? C132 N131 C136 C135 4.5(16) . . . . ? Pb1 N131 C136 C135 178.2(8) . . . . ? C134 C135 C136 N131 -2.8(17) . . . . ? C145 N141 N142 N143 -0.1(10) . . . . ? C146 N141 N142 N143 -178.1(7) . . . . ? N141 N142 N143 C144 -0.4(10) . . . . ? N141 N142 N143 Pb1 168.2(6) . . . . ? N163 Pb1 N143 N142 -119.8(8) . . . . ? O11S Pb1 N143 N142 146.7(7) . . . . ? N131 Pb1 N143 N142 -173.8(8) . . . . ? N123 Pb1 N143 N142 -31.8(10) . . . . ? N151 Pb1 N143 N142 -72.5(8) . . . . ? N111 Pb1 N143 N142 3.4(8) . . . . ? N163 Pb1 N143 C144 48.0(7) . . . . ? O11S Pb1 N143 C144 -45.5(8) . . . . ? N131 Pb1 N143 C144 -5.9(6) . . . . ? N123 Pb1 N143 C144 136.1(6) . . . . ? N151 Pb1 N143 C144 95.3(7) . . . . ? N111 Pb1 N143 C144 171.3(7) . . . . ? N142 N143 C144 C145 0.7(11) . . . . ? Pb1 N143 C144 C145 -169.7(6) . . . . ? N142 N143 C144 C132 -177.7(9) . . . . ? Pb1 N143 C144 C132 11.9(12) . . . . ? N131 C132 C144 N143 -11.9(15) . . . . ? C133 C132 C144 N143 171.9(10) . . . . ? N131 C132 C144 C145 170.1(11) . . . . ? C133 C132 C144 C145 -6.2(18) . . . . ? N142 N141 C145 C144 0.5(11) . . . . ? C146 N141 C145 C144 178.2(9) . . . . ? N143 C144 C145 N141 -0.7(11) . . . . ? C132 C144 C145 N141 177.5(10) . . . . ? N142 N141 C146 C173 63.7(10) . . . 6_755 ? C145 N141 C146 C173 -113.8(10) . . . 6_755 ? N163 Pb1 N151 C156 177.6(11) . . . . ? O11S Pb1 N151 C156 -176.8(8) . . . . ? N131 Pb1 N151 C156 107.4(9) . . . . ? N123 Pb1 N151 C156 -108.8(10) . . . . ? N143 Pb1 N151 C156 47.4(9) . . . . ? N111 Pb1 N151 C156 -47.1(9) . . . . ? N163 Pb1 N151 C152 -1.3(8) . . . . ? O11S Pb1 N151 C152 4.3(11) . . . . ? N131 Pb1 N151 C152 -71.6(9) . . . . ? N123 Pb1 N151 C152 72.3(9) . . . . ? N143 Pb1 N151 C152 -131.6(9) . . . . ? N111 Pb1 N151 C152 133.9(9) . . . . ? C156 N151 C152 C153 4.1(18) . . . . ? Pb1 N151 C152 C153 -176.9(10) . . . . ? C156 N151 C152 C164 179.1(11) . . . . ? Pb1 N151 C152 C164 -1.9(13) . . . . ? N151 C152 C153 C154 -9(2) . . . . ? C164 C152 C153 C154 177.0(12) . . . . ? C152 C153 C154 C155 9.5(19) . . . . ? C153 C154 C155 C156 -6.3(18) . . . . ? C152 N151 C156 C155 -0.9(18) . . . . ? Pb1 N151 C156 C155 -179.8(9) . . . . ? C154 C155 C156 N151 2.1(19) . . . . ? C165 N161 N162 N163 0.5(12) . . . . ? C166 N161 N162 N163 177.7(9) . . . . ? N161 N162 N163 C164 -1.0(12) . . . . ? N161 N162 N163 Pb1 -172.0(6) . . . . ? O11S Pb1 N163 N162 -1.1(8) . . . . ? N131 Pb1 N163 N162 -84.5(8) . . . . ? N123 Pb1 N163 N162 87.4(8) . . . . ? N143 Pb1 N163 N162 -132.7(8) . . . . ? N151 Pb1 N163 N162 175.1(10) . . . . ? N111 Pb1 N163 N162 122.7(8) . . . . ? O11S Pb1 N163 C164 -171.1(9) . . . . ? N131 Pb1 N163 C164 105.5(9) . . . . ? N123 Pb1 N163 C164 -82.6(9) . . . . ? N143 Pb1 N163 C164 57.3(9) . . . . ? N151 Pb1 N163 C164 5.1(8) . . . . ? N111 Pb1 N163 C164 -47.3(9) . . . . ? N162 N163 C164 C165 1.0(13) . . . . ? Pb1 N163 C164 C165 172.3(7) . . . . ? N162 N163 C164 C152 179.9(11) . . . . ? Pb1 N163 C164 C152 -8.8(15) . . . . ? C153 C152 C164 N163 -178.4(13) . . . . ? N151 C152 C164 N163 6.7(16) . . . . ? C153 C152 C164 C165 0(2) . . . . ? N151 C152 C164 C165 -174.6(12) . . . . ? N162 N161 C165 C164 0.1(12) . . . . ? C166 N161 C165 C164 -176.6(11) . . . . ? N163 C164 C165 N161 -0.6(13) . . . . ? C152 C164 C165 N161 -179.4(12) . . . . ? N162 N161 C166 C175 157.5(9) . . . 8_557 ? C165 N161 C166 C175 -26.0(16) . . . 8_557 ? N121 C126 C171 C172 91.0(10) . . . . ? N121 C126 C171 C176 -91.1(10) . . . . ? C176 C171 C172 C173 -0.7(13) . . . . ? C126 C171 C172 C173 177.1(8) . . . . ? C176 C171 C172 C177 176.7(8) . . . . ? C126 C171 C172 C177 -5.5(12) . . . . ? C171 C172 C173 C174 -1.7(12) . . . . ? C177 C172 C173 C174 -179.2(7) . . . . ? C171 C172 C173 C146 179.0(7) . . . 6_765 ? C177 C172 C173 C146 1.6(12) . . . 6_765 ? C172 C173 C174 C175 0.7(13) . . . . ? C146 C173 C174 C175 -180.0(8) 6_765 . . . ? C172 C173 C174 C178 179.7(7) . . . . ? C146 C173 C174 C178 -1.0(12) 6_765 . . . ? C173 C174 C175 C176 2.5(13) . . . . ? C178 C174 C175 C176 -176.4(8) . . . . ? C173 C174 C175 C166 -178.7(8) . . . 8_657 ? C178 C174 C175 C166 2.4(12) . . . 8_657 ? C172 C171 C176 C175 3.7(13) . . . . ? C126 C171 C176 C175 -174.1(7) . . . . ? C172 C171 C176 C179 -173.5(8) . . . . ? C126 C171 C176 C179 8.7(12) . . . . ? C174 C175 C176 C171 -4.6(12) . . . . ? C166 C175 C176 C171 176.6(8) 8_657 . . . ? C174 C175 C176 C179 172.7(8) . . . . ? C166 C175 C176 C179 -6.1(12) 8_657 . . . ? N163 Pb1 O11S C13S 52.3(10) . . . . ? N131 Pb1 O11S C13S 127.2(10) . . . . ? N123 Pb1 O11S C13S -19.0(10) . . . . ? N143 Pb1 O11S C13S 162.0(9) . . . . ? N151 Pb1 O11S C13S 47.3(11) . . . . ? N111 Pb1 O11S C13S -65.5(10) . . . . ? Pb1 O11S C13S N12S 85.6(15) . . . . ? C15S N12S C13S O11S -12.9(18) . . . . ? C14S N12S C13S O11S -178.3(11) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.76 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.701 _refine_diff_density_min -1.583 _refine_diff_density_rms 0.162 #===END data_imw1271c2c _database_code_depnum_ccdc_archive 'CCDC 778864' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H33 Cl2 N10 O8 Pb' _chemical_formula_weight 1035.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 19.6201(7) _cell_length_b 19.7818(7) _cell_length_c 21.6058(8) _cell_angle_alpha 90.00 _cell_angle_beta 92.690(3) _cell_angle_gamma 90.00 _cell_volume 8376.4(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9888 _cell_measurement_theta_min 2.27 _cell_measurement_theta_max 23.29 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4088 _exptl_absorpt_coefficient_mu 4.218 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4183 _exptl_absorpt_correction_T_max 0.4856 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 68947 _diffrn_reflns_av_R_equivalents 0.0554 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 27.40 _reflns_number_total 9492 _reflns_number_gt 6398 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a polymer of unit [Pb2(L)3][ClO4]4.MeCN2.H2O2. The data was solved by Patterson methods. The structure contains two fully disordered perchlorate anions (Cl1 > O15 and Cl2 > O25). These have been modelled as being split over two sites (50:50). The main part of the ligand also suffers disorder; the ring systems N11 > C16 and N21 > C25 are modelled over two sites (50:50). All disordered atoms have benefited from the application of geometric and displacement restrains. 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^)+(0.0938P)^2^+104.1441P] 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 9492 _refine_ls_number_parameters 419 _refine_ls_number_restraints 296 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0621 _refine_ls_wR_factor_ref 0.1905 _refine_ls_wR_factor_gt 0.1646 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.452 _refine_ls_shift/su_max 0.043 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.69189(2) 0.89786(2) 0.81340(2) 0.04534(19) Uani 1 1 d D . . N11X N 0.7698(7) 0.8042(6) 0.8672(6) 0.042(5) Uiso 0.50 1 d PGD A 1 C12X C 0.7609(6) 0.7364(7) 0.8519(5) 0.048(6) Uiso 0.50 1 d PGD A 1 C13X C 0.7972(9) 0.6870(5) 0.8852(7) 0.051(6) Uiso 0.50 1 d PGD A 1 H13X H 0.7912 0.6407 0.8748 0.061 Uiso 0.50 1 calc PR A 1 C14X C 0.8423(8) 0.7054(6) 0.9339(7) 0.055(7) Uiso 0.50 1 d PGD A 1 H14X H 0.8671 0.6717 0.9567 0.066 Uiso 0.50 1 calc PR A 1 C15X C 0.8512(7) 0.7732(8) 0.9491(6) 0.061(7) Uiso 0.50 1 d PGD A 1 H15X H 0.8820 0.7858 0.9824 0.073 Uiso 0.50 1 calc PR A 1 C16X C 0.8149(8) 0.8226(5) 0.9158(7) 0.048(6) Uiso 0.50 1 d PGD A 1 H16X H 0.8210 0.8689 0.9262 0.057 Uiso 0.50 1 calc PR A 1 N21X N 0.6411(11) 0.7369(6) 0.7212(9) 0.059(17) Uiso 0.50 1 d PGD A 1 N22X N 0.6844(9) 0.7729(4) 0.7643(8) 0.031(5) Uiso 0.50 1 d PGD A 1 C23X C 0.7173(10) 0.7251(9) 0.8046(7) 0.040(7) Uiso 0.50 1 d PGD A 1 C24X C 0.6944(12) 0.6596(6) 0.7864(10) 0.057(12) Uiso 0.50 1 d PGD A 1 H24X H 0.7081 0.6182 0.8054 0.068 Uiso 0.50 1 calc PR A 1 C25X C 0.6473(11) 0.6669(5) 0.7349(10) 0.036(8) Uiso 0.50 1 d PGD A 1 H25X H 0.6240 0.6313 0.7134 0.043 Uiso 0.50 1 calc PR A 1 N11Y N 0.7453(7) 0.8012(5) 0.8847(5) 0.031(4) Uiso 0.50 1 d PGD A 2 C12Y C 0.7414(6) 0.7340(6) 0.8662(5) 0.034(5) Uiso 0.50 1 d PGD A 2 C13Y C 0.7729(9) 0.6841(4) 0.9027(7) 0.046(6) Uiso 0.50 1 d PGD A 2 H13Y H 0.7703 0.6381 0.8900 0.055 Uiso 0.50 1 calc PR A 2 C14Y C 0.8082(9) 0.7014(6) 0.9576(7) 0.054(6) Uiso 0.50 1 d PGD A 2 H14Y H 0.8297 0.6673 0.9826 0.065 Uiso 0.50 1 calc PR A 2 C15Y C 0.8121(8) 0.7687(7) 0.9761(5) 0.064(8) Uiso 0.50 1 d PGD A 2 H15Y H 0.8362 0.7805 1.0137 0.076 Uiso 0.50 1 calc PR A 2 C16Y C 0.7806(8) 0.8186(5) 0.9396(6) 0.046(6) Uiso 0.50 1 d PGD A 2 H16Y H 0.7832 0.8645 0.9523 0.055 Uiso 0.50 1 calc PR A 2 N21Y N 0.6429(8) 0.7413(6) 0.7234(6) 0.025(9) Uiso 0.50 1 d PGD A 2 N22Y N 0.6761(9) 0.7682(4) 0.7779(7) 0.035(6) Uiso 0.50 1 d PGD A 2 C23Y C 0.7051(9) 0.7135(8) 0.8126(5) 0.032(6) Uiso 0.50 1 d PGD A 2 C24Y C 0.6898(10) 0.6528(5) 0.7796(8) 0.030(7) Uiso 0.50 1 d PGD A 2 H24Y H 0.7030 0.6085 0.7922 0.036 Uiso 0.50 1 calc PR A 2 C25Y C 0.6514(10) 0.6700(6) 0.7245(7) 0.042(10) Uiso 0.50 1 d PGD A 2 H25Y H 0.6343 0.6393 0.6938 0.051 Uiso 0.50 1 calc PR A 2 C126 C 0.6001(6) 0.7775(6) 0.6812(5) 0.042(3) Uani 1 1 d D . . H12A H 0.5769 0.7487 0.6493 0.050 Uiso 1 1 calc R A 1 H12B H 0.6292 0.8102 0.6600 0.050 Uiso 1 1 calc R A 1 C131 C 0.5471(5) 0.8156(5) 0.7166(5) 0.033(2) Uani 1 1 d . A . C132 C 0.5000 0.7806(8) 0.7500 0.032(3) Uani 1 2 d S . . H132 H 0.5000 0.7326 0.7500 0.039 Uiso 1 2 calc SR A . C133 C 0.5468(6) 0.8865(5) 0.7164(5) 0.037(2) Uani 1 1 d . . . H133 H 0.5787 0.9105 0.6931 0.045 Uiso 1 1 calc R A . C134 C 0.5000 0.9215(9) 0.7500 0.040(4) Uani 1 2 d S . . H134 H 0.5000 0.9695 0.7500 0.048 Uiso 1 2 calc SR . . N11W N 0.7575(7) 0.9694(7) 0.8989(6) 0.043(6) Uiso 0.50 1 d PGD A 1 C12W C 0.8191(7) 0.9966(8) 0.8815(6) 0.032(5) Uiso 0.50 1 d PGD A 1 C13W C 0.8508(7) 1.0471(8) 0.9171(8) 0.049(6) Uiso 0.50 1 d PGD A 1 H13W H 0.8929 1.0656 0.9051 0.059 Uiso 0.50 1 calc PR A 1 C14W C 0.8210(10) 1.0704(8) 0.9701(8) 0.053(7) Uiso 0.50 1 d PGD A 1 H14W H 0.8427 1.1049 0.9944 0.064 Uiso 0.50 1 calc PR A 1 C15W C 0.7595(10) 1.0433(10) 0.9876(7) 0.062(8) Uiso 0.50 1 d PGD A 1 H15W H 0.7391 1.0593 1.0238 0.074 Uiso 0.50 1 calc PR A 1 C16W C 0.7277(7) 0.9928(9) 0.9520(7) 0.060(8) Uiso 0.50 1 d PGD A 1 H16W H 0.6856 0.9743 0.9639 0.071 Uiso 0.50 1 calc PR A 1 N21W N 0.8575(6) 0.9087(7) 0.7433(7) 0.038(4) Uiso 0.50 1 d PGD A 1 N22W N 0.8194(4) 0.9221(8) 0.7962(8) 0.046(6) Uiso 0.50 1 d PGD A 1 C23W C 0.8516(7) 0.9761(7) 0.8295(6) 0.062(8) Uiso 0.50 1 d PGD A 1 C24W C 0.9097(8) 0.9961(8) 0.7972(9) 0.055(7) Uiso 0.50 1 d PGD A 1 H24W H 0.9407 1.0311 0.8091 0.065 Uiso 0.50 1 calc PR A 1 C25W C 0.9133(7) 0.9544(8) 0.7439(8) 0.056(7) Uiso 0.50 1 d PGD A 1 H25W H 0.9471 0.9567 0.7139 0.068 Uiso 0.50 1 calc PR A 1 C26W C 0.8358(11) 0.8532(8) 0.7070(11) 0.032(5) Uiso 0.50 1 d PD A 1 H26A H 0.8560 0.8570 0.6660 0.038 Uiso 0.50 1 calc PR A 1 H26B H 0.7856 0.8556 0.7003 0.038 Uiso 0.50 1 calc PR A 1 C31W C 0.8544(11) 0.7837(10) 0.7345(12) 0.038(6) Uiso 0.50 1 d PD A 1 C32W C 0.8334(13) 0.7250(11) 0.7044(13) 0.036(7) Uiso 0.50 1 d PD . 1 H32W H 0.8045 0.7279 0.6679 0.043 Uiso 0.50 1 calc PR . 1 C33W C 0.8966(11) 0.7770(11) 0.7880(11) 0.038(5) Uiso 0.50 1 d PD A 1 H33W H 0.9132 0.8165 0.8087 0.046 Uiso 0.50 1 calc PR A 1 C34W C 0.9148(12) 0.7138(11) 0.8119(12) 0.041(5) Uiso 0.50 1 d PD . 1 H34W H 0.9415 0.7103 0.8496 0.050 Uiso 0.50 1 calc PR . 1 C26Y C 0.6662(10) 1.0976(12) 0.8064(13) 0.040(9) Uiso 0.50 1 d PD A 1 H29W H 0.6782 1.0636 0.7751 0.048 Uiso 0.50 1 calc PR A 1 H27W H 0.7076 1.1061 0.8333 0.048 Uiso 0.50 1 calc PR A 1 C31Y C 0.6464(11) 1.1624(11) 0.7735(12) 0.031(6) Uiso 0.50 1 d PD . 1 C32Y C 0.6059(12) 1.1575(14) 0.7192(12) 0.043(6) Uiso 0.50 1 d PD . 1 H32Y H 0.5927 1.1143 0.7038 0.052 Uiso 0.50 1 calc PR . 1 N11V N 0.7701(6) 0.9764(6) 0.8837(6) 0.028(4) Uiso 0.50 1 d PGD A 2 C12V C 0.8305(7) 1.0037(7) 0.8635(6) 0.037(5) Uiso 0.50 1 d PGD A 2 C13V C 0.8664(7) 1.0508(8) 0.9000(8) 0.046(6) Uiso 0.50 1 d PGD A 2 H13V H 0.9077 1.0694 0.8862 0.055 Uiso 0.50 1 calc PR A 2 C14V C 0.8420(9) 1.0706(8) 0.9565(7) 0.057(7) Uiso 0.50 1 d PGD A 2 H14V H 0.8665 1.1028 0.9814 0.068 Uiso 0.50 1 calc PR A 2 C15V C 0.7816(9) 1.0433(9) 0.9767(6) 0.052(7) Uiso 0.50 1 d PGD A 2 H15V H 0.7649 1.0569 1.0153 0.062 Uiso 0.50 1 calc PR A 2 C16V C 0.7456(6) 0.9962(8) 0.9402(7) 0.038(5) Uiso 0.50 1 d PGD A 2 H16V H 0.7044 0.9776 0.9540 0.046 Uiso 0.50 1 calc PR A 2 N21V N 0.8460(6) 0.9122(7) 0.7198(6) 0.047(5) Uiso 0.50 1 d PGD A 2 N22V N 0.8122(5) 0.9258(7) 0.7752(7) 0.040(5) Uiso 0.50 1 d PGD A 2 C23V C 0.8496(6) 0.9768(6) 0.8083(5) 0.023(4) Uiso 0.50 1 d PGD A 2 C24V C 0.9065(6) 0.9946(6) 0.7734(7) 0.035(5) Uiso 0.50 1 d PGD A 2 H24V H 0.9401 1.0275 0.7846 0.042 Uiso 0.50 1 calc PR A 2 C25V C 0.9042(6) 0.9547(7) 0.7187(7) 0.040(5) Uiso 0.50 1 d PGD A 2 H25V H 0.9361 0.9562 0.6870 0.048 Uiso 0.50 1 calc PR A 2 C26V C 0.8351(12) 0.8563(8) 0.6806(11) 0.036(5) Uiso 0.50 1 d PD A 2 H26C H 0.8594 0.8633 0.6419 0.044 Uiso 0.50 1 calc PR A 2 H26D H 0.7858 0.8519 0.6695 0.044 Uiso 0.50 1 calc PR A 2 C31V C 0.8611(10) 0.7914(9) 0.7126(12) 0.032(5) Uiso 0.50 1 d PD A 2 C32V C 0.8366(13) 0.7318(10) 0.6865(13) 0.034(7) Uiso 0.50 1 d PD . 2 H32V H 0.8045 0.7337 0.6522 0.041 Uiso 0.50 1 calc PR . 2 C33V C 0.9091(10) 0.7896(10) 0.7624(11) 0.034(5) Uiso 0.50 1 d PD A 2 H33V H 0.9264 0.8304 0.7800 0.041 Uiso 0.50 1 calc PR A 2 C34V C 0.9316(12) 0.7276(11) 0.7860(12) 0.042(5) Uiso 0.50 1 d PD . 2 H34V H 0.9645 0.7255 0.8197 0.051 Uiso 0.50 1 calc PR . 2 C26X C 0.6706(9) 1.1070(11) 0.8203(13) 0.030(7) Uiso 0.50 1 d PD A 2 H26E H 0.6934 1.0797 0.7889 0.036 Uiso 0.50 1 calc PR A 2 H26F H 0.7046 1.1177 0.8543 0.036 Uiso 0.50 1 calc PR A 2 C31X C 0.6427(12) 1.1713(12) 0.7915(13) 0.037(7) Uiso 0.50 1 d PD . 2 C32X C 0.5959(12) 1.1674(15) 0.7413(13) 0.047(7) Uiso 0.50 1 d PD . 2 H32X H 0.5822 1.1246 0.7253 0.056 Uiso 0.50 1 calc PR . 2 N311 N 0.5926(5) 0.8708(5) 0.8896(5) 0.046(3) Uani 1 1 d . A . C312 C 0.5481(7) 0.9178(6) 0.9072(5) 0.042(3) Uani 1 1 d . . . C313 C 0.4913(9) 0.9026(7) 0.9412(6) 0.058(4) Uani 1 1 d . A . H313 H 0.4610 0.9372 0.9533 0.070 Uiso 1 1 calc R . . C314 C 0.4800(10) 0.8345(8) 0.9572(6) 0.069(5) Uani 1 1 d . . . H314 H 0.4419 0.8223 0.9804 0.083 Uiso 1 1 calc R A . C315 C 0.5251(9) 0.7860(8) 0.9386(7) 0.068(5) Uani 1 1 d . A . H315 H 0.5188 0.7399 0.9491 0.082 Uiso 1 1 calc R . . C316 C 0.5809(8) 0.8056(7) 0.9037(6) 0.061(4) Uani 1 1 d . . . H316 H 0.6111 0.7718 0.8898 0.073 Uiso 1 1 calc R A . N321 N 0.6130(5) 1.0691(5) 0.8447(5) 0.040(2) Uani 1 1 d D . . N322 N 0.6150(5) 1.0021(5) 0.8549(4) 0.040(2) Uani 1 1 d . A . C323 C 0.5611(6) 0.9885(6) 0.8885(5) 0.038(2) Uani 1 1 d . A . C324 C 0.5241(7) 1.0477(6) 0.8997(6) 0.050(3) Uani 1 1 d . . . H324 H 0.4835 1.0517 0.9217 0.060 Uiso 1 1 calc R A . C325 C 0.5593(7) 1.0985(6) 0.8721(7) 0.053(3) Uani 1 1 d . A . H325 H 0.5483 1.1453 0.8720 0.064 Uiso 1 1 calc R . . Cl1X Cl 0.6904(5) 0.9909(4) 0.6402(3) 0.0543(10) Uani 0.50 1 d PDU B 1 O12X O 0.6900(8) 0.9184(4) 0.6345(6) 0.0540(17) Uiso 0.50 1 d PDU B 1 O13X O 0.6557(8) 1.0195(8) 0.5861(6) 0.0560(18) Uiso 0.50 1 d PDU B 1 O14X O 0.7602(5) 1.0139(8) 0.6426(6) 0.0552(17) Uiso 0.50 1 d PDU B 1 O15X O 0.6604(8) 1.0090(8) 0.6974(6) 0.0564(17) Uiso 0.50 1 d PDU B 1 Cl1Y Cl 0.6967(4) 0.9829(4) 0.6353(3) 0.0542(10) Uani 0.50 1 d PDU C 2 O12Y O 0.6898(8) 0.9147(5) 0.6125(6) 0.0548(18) Uiso 0.50 1 d PDU C 2 O13Y O 0.6444(6) 1.0249(7) 0.6063(8) 0.0563(18) Uiso 0.50 1 d PDU C 2 O14Y O 0.7630(5) 1.0089(8) 0.6221(6) 0.0554(18) Uiso 0.50 1 d PDU C 2 O15Y O 0.6880(9) 0.9841(8) 0.7011(4) 0.0577(17) Uiso 0.50 1 d PDU C 2 Cl2X Cl 0.9887(5) 0.8536(5) 0.5608(4) 0.0908(17) Uani 0.50 1 d PDU D 1 O22X O 0.9642(9) 0.7939(7) 0.5909(8) 0.092(2) Uiso 0.50 1 d PDU D 1 O23X O 0.9680(10) 0.8527(13) 0.4960(5) 0.092(2) Uiso 0.50 1 d PDU D 1 O24X O 1.0618(5) 0.8578(10) 0.5685(9) 0.096(3) Uiso 0.50 1 d PDU D 1 O25X O 0.9574(10) 0.9130(7) 0.5852(12) 0.092(2) Uiso 0.50 1 d PDU D 1 Cl2Y Cl 0.9639(5) 0.8327(5) 0.5697(4) 0.0920(17) Uani 0.50 1 d PDU E 2 O22Y O 0.9834(10) 0.7629(6) 0.5773(9) 0.094(3) Uiso 0.50 1 d PDU E 2 O23Y O 0.8907(5) 0.8394(11) 0.5686(11) 0.098(3) Uiso 0.50 1 d PDU E 2 O24Y O 0.9905(9) 0.8602(10) 0.5142(6) 0.092(2) Uiso 0.50 1 d PDU E 2 O25Y O 0.9869(13) 0.8716(9) 0.6230(7) 0.094(2) Uiso 0.50 1 d PDU E 2 N11S N 0.5154(7) 0.6269(7) 0.8490(6) 0.068(3) Uiso 1 1 d . . . C12S C 0.5499(8) 0.5992(7) 0.8826(7) 0.055(3) Uiso 1 1 d . . . C13S C 0.5963(11) 0.5651(11) 0.9275(9) 0.096(6) Uiso 1 1 d . . . H13A H 0.6435 0.5765 0.9190 0.143 Uiso 1 1 calc R . . H13B H 0.5899 0.5160 0.9241 0.143 Uiso 1 1 calc R . . H13C H 0.5864 0.5798 0.9695 0.143 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0382(3) 0.0314(3) 0.0642(3) -0.0095(2) -0.0211(2) 0.00637(18) C126 0.039(6) 0.046(7) 0.040(6) -0.003(5) 0.001(5) 0.001(5) C131 0.026(5) 0.038(6) 0.036(6) 0.001(4) -0.009(4) 0.001(4) C132 0.033(7) 0.031(7) 0.032(8) 0.000 -0.008(6) 0.000 C133 0.036(6) 0.037(6) 0.038(6) 0.008(5) -0.011(5) -0.005(5) C134 0.037(8) 0.036(8) 0.046(9) 0.000 -0.011(7) 0.000 N311 0.054(6) 0.026(5) 0.056(6) 0.012(4) -0.023(5) -0.007(4) C312 0.060(8) 0.037(6) 0.028(6) 0.004(5) -0.014(5) -0.007(5) C313 0.082(10) 0.056(8) 0.037(7) 0.002(6) 0.005(7) -0.020(7) C314 0.113(14) 0.056(9) 0.040(7) 0.003(6) 0.014(8) -0.035(9) C315 0.098(12) 0.048(8) 0.054(8) 0.025(7) -0.035(8) -0.028(8) C316 0.078(10) 0.044(7) 0.056(8) 0.006(6) -0.038(7) -0.003(7) N321 0.038(5) 0.027(5) 0.054(6) 0.006(4) -0.002(4) 0.004(4) N322 0.043(5) 0.030(5) 0.046(6) 0.000(4) -0.004(4) 0.003(4) C323 0.046(6) 0.036(6) 0.032(6) 0.004(5) -0.002(5) -0.003(5) C324 0.050(7) 0.045(7) 0.056(8) 0.000(6) 0.013(6) 0.002(6) C325 0.047(7) 0.035(6) 0.077(9) -0.003(6) 0.001(6) 0.010(5) Cl1X 0.0525(14) 0.0535(15) 0.0575(14) 0.0044(12) 0.0079(12) -0.0014(12) Cl1Y 0.0528(14) 0.0537(15) 0.0577(14) 0.0153(12) 0.0199(12) 0.0078(12) Cl2X 0.090(2) 0.092(2) 0.091(2) 0.0100(14) 0.0081(14) 0.0107(14) Cl2Y 0.092(2) 0.092(2) 0.093(2) 0.0165(13) 0.0136(13) 0.0205(13) _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 N22W 2.590(7) . ? Pb1 N22V 2.597(6) . ? Pb1 N11W 2.618(6) . ? Pb1 N11V 2.618(6) . ? Pb1 N11X 2.637(7) . ? Pb1 N11Y 2.640(7) . ? Pb1 N311 2.663(11) . ? Pb1 N22Y 2.692(6) . ? Pb1 N22X 2.692(6) . ? Pb1 N322 2.731(9) . ? N11X C12X 1.3900 . ? N11X C16X 1.3900 . ? C12X C23X 1.322(11) . ? C12X C13X 1.3900 . ? C13X C14X 1.3900 . ? C13X H13X 0.9500 . ? C14X C15X 1.3900 . ? C14X H14X 0.9500 . ? C15X C16X 1.3900 . ? C15X H15X 0.9500 . ? C16X H16X 0.9500 . ? N21X C126 1.405(13) . ? N21X N22X 1.4200 . ? N21X C25X 1.4200 . ? N22X C23X 1.4200 . ? C23X C24X 1.4200 . ? C24X C25X 1.4200 . ? C24X H24X 0.9500 . ? C25X H25X 0.9500 . ? N11Y C12Y 1.3900 . ? N11Y C16Y 1.3900 . ? C12Y C13Y 1.3900 . ? C12Y C23Y 1.392(11) . ? C13Y C14Y 1.3900 . ? C13Y H13Y 0.9500 . ? C14Y C15Y 1.3900 . ? C14Y H14Y 0.9500 . ? C15Y C16Y 1.3900 . ? C15Y H15Y 0.9500 . ? C16Y H16Y 0.9500 . ? N21Y C126 1.406(13) . ? N21Y N22Y 1.4200 . ? N21Y C25Y 1.4200 . ? N22Y C23Y 1.4200 . ? C23Y C24Y 1.4200 . ? C24Y C25Y 1.4200 . ? C24Y H24Y 0.9500 . ? C25Y H25Y 0.9500 . ? C126 C131 1.521(15) . ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? C131 C132 1.384(13) . ? C131 C133 1.402(15) . ? C132 C131 1.384(13) 2_656 ? C132 H132 0.9500 . ? C133 C134 1.382(15) . ? C133 H133 0.9500 . ? C134 C133 1.382(15) 2_656 ? C134 H134 0.9500 . ? N11W C12W 1.3900 . ? N11W C16W 1.3900 . ? C12W C23W 1.378(13) . ? C12W C13W 1.3900 . ? C13W C14W 1.3900 . ? C13W H13W 0.9500 . ? C14W C15W 1.3900 . ? C14W H14W 0.9500 . ? C15W C16W 1.3900 . ? C15W H15W 0.9500 . ? C16W H16W 0.9500 . ? N21W C26W 1.403(17) . ? N21W N22W 1.4200 . ? N21W C25W 1.4200 . ? N22W C23W 1.4200 . ? C23W C24W 1.4200 . ? C24W C25W 1.4200 . ? C24W H24W 0.9500 . ? C25W H25W 0.9500 . ? C26W C31W 1.53(2) . ? C26W H26A 0.9900 . ? C26W H26B 0.9900 . ? C31W C32W 1.384(17) . ? C31W C33W 1.40(2) . ? C32W C31Y 1.38(3) 4_646 ? C32W H32W 0.9500 . ? C33W C34W 1.39(2) . ? C33W H33W 0.9500 . ? C34W C32Y 1.35(3) 4_646 ? C34W H34W 0.9500 . ? C26Y N321 1.474(15) . ? C26Y C31Y 1.507(16) . ? C26Y H29W 0.9900 . ? C26Y H27W 0.9900 . ? C31Y C32W 1.38(4) 4_656 ? C31Y C32Y 1.39(2) . ? C32Y C34W 1.35(3) 4_656 ? C32Y H32Y 0.9500 . ? N11V C12V 1.3900 . ? N11V C16V 1.3900 . ? C12V C23V 1.376(13) . ? C12V C13V 1.3900 . ? C13V C14V 1.3900 . ? C13V H13V 0.9500 . ? C14V C15V 1.3900 . ? C14V H14V 0.9500 . ? C15V C16V 1.3900 . ? C15V H15V 0.9500 . ? C16V H16V 0.9500 . ? N21V C26V 1.402(17) . ? N21V N22V 1.4200 . ? N21V C25V 1.4200 . ? N22V C23V 1.4200 . ? C23V C24V 1.4200 . ? C24V C25V 1.4200 . ? C24V H24V 0.9500 . ? C25V H25V 0.9500 . ? C26V C31V 1.53(2) . ? C26V H26C 0.9900 . ? C26V H26D 0.9900 . ? C31V C32V 1.384(17) . ? C31V C33V 1.40(2) . ? C32V C31X 1.34(4) 4_646 ? C32V H32V 0.9500 . ? C33V C34V 1.39(2) . ? C33V H33V 0.9500 . ? C34V C32X 1.42(4) 4_646 ? C34V H34V 0.9500 . ? C26X N321 1.474(15) . ? C26X C31X 1.507(16) . ? C26X H26E 0.9900 . ? C26X H26F 0.9900 . ? C31X C32V 1.34(4) 4_656 ? C31X C32X 1.39(2) . ? C32X C34V 1.42(4) 4_656 ? C32X H32X 0.9500 . ? N311 C312 1.344(17) . ? N311 C316 1.347(16) . ? C312 C313 1.40(2) . ? C312 C323 1.480(16) . ? C313 C314 1.410(19) . ? C313 H313 0.9500 . ? C314 C315 1.38(2) . ? C314 H314 0.9500 . ? C315 C316 1.41(2) . ? C315 H315 0.9500 . ? C316 H316 0.9500 . ? N321 N322 1.343(12) . ? N321 C325 1.364(16) . ? N322 C323 1.338(15) . ? C323 C324 1.406(17) . ? C324 C325 1.372(18) . ? C324 H324 0.9500 . ? C325 H325 0.9500 . ? Cl1X O12X 1.440(3) . ? Cl1X O15X 1.440(3) . ? Cl1X O14X 1.441(3) . ? Cl1X O13X 1.440(3) . ? Cl1Y O12Y 1.440(3) . ? Cl1Y O13Y 1.440(3) . ? Cl1Y O14Y 1.440(3) . ? Cl1Y O15Y 1.440(3) . ? Cl2X O24X 1.438(3) . ? Cl2X O25X 1.438(3) . ? Cl2X O23X 1.441(3) . ? Cl2X O22X 1.442(3) . ? Cl2Y O24Y 1.439(3) . ? Cl2Y O25Y 1.440(3) . ? Cl2Y O23Y 1.441(3) . ? Cl2Y O22Y 1.441(3) . ? N11S C12S 1.114(18) . ? C12S C13S 1.46(2) . ? C13S H13A 0.9800 . ? C13S H13B 0.9800 . ? C13S H13C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N22W Pb1 N22V 10.5(4) . . ? N22W Pb1 N11W 63.6(5) . . ? N22V Pb1 N11W 71.6(5) . . ? N22W Pb1 N11V 55.2(5) . . ? N22V Pb1 N11V 62.7(4) . . ? N11W Pb1 N11V 9.7(4) . . ? N22W Pb1 N11X 69.5(5) . . ? N22V Pb1 N11X 76.9(5) . . ? N11W Pb1 N11X 79.2(5) . . ? N11V Pb1 N11X 81.3(5) . . ? N22W Pb1 N11Y 81.9(5) . . ? N22V Pb1 N11Y 89.9(5) . . ? N11W Pb1 N11Y 79.1(5) . . ? N11V Pb1 N11Y 83.4(4) . . ? N11X Pb1 N11Y 13.7(4) . . ? N22W Pb1 N311 149.9(4) . . ? N22V Pb1 N311 160.3(4) . . ? N11W Pb1 N311 91.3(4) . . ? N11V Pb1 N311 100.7(4) . . ? N11X Pb1 N311 90.7(4) . . ? N11Y Pb1 N311 77.0(4) . . ? N22W Pb1 N22Y 103.6(5) . . ? N22V Pb1 N22Y 101.9(5) . . ? N11W Pb1 N22Y 139.7(5) . . ? N11V Pb1 N22Y 142.0(5) . . ? N11X Pb1 N22Y 60.8(4) . . ? N11Y Pb1 N22Y 60.9(4) . . ? N311 Pb1 N22Y 84.6(5) . . ? N22W Pb1 N22X 98.6(5) . . ? N22V Pb1 N22X 96.0(5) . . ? N11W Pb1 N22X 142.3(5) . . ? N11V Pb1 N22X 142.5(5) . . ? N11X Pb1 N22X 63.1(5) . . ? N11Y Pb1 N22X 65.0(4) . . ? N311 Pb1 N22X 91.8(5) . . ? N22Y Pb1 N22X 7.6(6) . . ? N22W Pb1 N322 117.3(4) . . ? N22V Pb1 N322 117.9(4) . . ? N11W Pb1 N322 67.7(4) . . ? N11V Pb1 N322 71.3(4) . . ? N11X Pb1 N322 134.7(4) . . ? N11Y Pb1 N322 124.4(4) . . ? N311 Pb1 N322 61.2(3) . . ? N22Y Pb1 N322 139.0(4) . . ? N22X Pb1 N322 143.3(5) . . ? C12X N11X C16X 120.0 . . ? C12X N11X Pb1 120.7(7) . . ? C16X N11X Pb1 119.0(7) . . ? C23X C12X N11X 114.6(13) . . ? C23X C12X C13X 125.4(13) . . ? N11X C12X C13X 120.0 . . ? C14X C13X C12X 120.0 . . ? C14X C13X H13X 120.0 . . ? C12X C13X H13X 120.0 . . ? C15X C14X C13X 120.0 . . ? C15X C14X H14X 120.0 . . ? C13X C14X H14X 120.0 . . ? C14X C15X C16X 120.0 . . ? C14X C15X H15X 120.0 . . ? C16X C15X H15X 120.0 . . ? C15X C16X N11X 120.0 . . ? C15X C16X H16X 120.0 . . ? N11X C16X H16X 120.0 . . ? C126 N21X N22X 115.1(13) . . ? C126 N21X C25X 136.6(13) . . ? N22X N21X C25X 108.0 . . ? N21X N22X C23X 108.0 . . ? N21X N22X Pb1 137.6(10) . . ? C23X N22X Pb1 110.8(10) . . ? C12X C23X C24X 123.6(16) . . ? C12X C23X N22X 128.4(16) . . ? C24X C23X N22X 108.0 . . ? C25X C24X C23X 108.0 . . ? C25X C24X H24X 126.0 . . ? C23X C24X H24X 126.0 . . ? C24X C25X N21X 108.0 . . ? C24X C25X H25X 126.0 . . ? N21X C25X H25X 126.0 . . ? C12Y N11Y C16Y 120.0 . . ? C12Y N11Y Pb1 120.7(6) . . ? C16Y N11Y Pb1 119.2(6) . . ? C13Y C12Y N11Y 120.0 . . ? C13Y C12Y C23Y 117.5(11) . . ? N11Y C12Y C23Y 122.5(11) . . ? C14Y C13Y C12Y 120.0 . . ? C14Y C13Y H13Y 120.0 . . ? C12Y C13Y H13Y 120.0 . . ? C15Y C14Y C13Y 120.0 . . ? C15Y C14Y H14Y 120.0 . . ? C13Y C14Y H14Y 120.0 . . ? C14Y C15Y C16Y 120.0 . . ? C14Y C15Y H15Y 120.0 . . ? C16Y C15Y H15Y 120.0 . . ? C15Y C16Y N11Y 120.0 . . ? C15Y C16Y H16Y 120.0 . . ? N11Y C16Y H16Y 120.0 . . ? C126 N21Y N22Y 125.7(13) . . ? C126 N21Y C25Y 125.6(13) . . ? N22Y N21Y C25Y 108.0 . . ? C23Y N22Y N21Y 108.0 . . ? C23Y N22Y Pb1 122.5(10) . . ? N21Y N22Y Pb1 129.4(10) . . ? C12Y C23Y N22Y 113.2(14) . . ? C12Y C23Y C24Y 138.7(14) . . ? N22Y C23Y C24Y 108.0 . . ? C25Y C24Y C23Y 108.0 . . ? C25Y C24Y H24Y 126.0 . . ? C23Y C24Y H24Y 126.0 . . ? C24Y C25Y N21Y 108.0 . . ? C24Y C25Y H25Y 126.0 . . ? N21Y C25Y H25Y 126.0 . . ? N21X C126 N21Y 4.3(9) . . ? N21X C126 C131 111.1(13) . . ? N21Y C126 C131 109.1(11) . . ? N21X C126 H12A 109.4 . . ? N21Y C126 H12A 113.7 . . ? C131 C126 H12A 109.4 . . ? N21X C126 H12B 109.4 . . ? N21Y C126 H12B 107.1 . . ? C131 C126 H12B 109.4 . . ? H12A C126 H12B 108.0 . . ? C132 C131 C133 120.0(11) . . ? C132 C131 C126 120.2(10) . . ? C133 C131 C126 119.8(10) . . ? C131 C132 C131 119.9(14) . 2_656 ? C131 C132 H132 120.0 . . ? C131 C132 H132 120.0 2_656 . ? C134 C133 C131 120.1(11) . . ? C134 C133 H133 119.9 . . ? C131 C133 H133 119.9 . . ? C133 C134 C133 119.9(15) . 2_656 ? C133 C134 H134 120.0 . . ? C133 C134 H134 120.0 2_656 . ? C12W N11W C16W 120.0 . . ? C12W N11W Pb1 115.0(8) . . ? C16W N11W Pb1 123.3(8) . . ? C23W C12W C13W 116.7(12) . . ? C23W C12W N11W 123.3(12) . . ? C13W C12W N11W 120.0 . . ? C12W C13W C14W 120.0 . . ? C12W C13W H13W 120.0 . . ? C14W C13W H13W 120.0 . . ? C15W C14W C13W 120.0 . . ? C15W C14W H14W 120.0 . . ? C13W C14W H14W 120.0 . . ? C16W C15W C14W 120.0 . . ? C16W C15W H15W 120.0 . . ? C14W C15W H15W 120.0 . . ? C15W C16W N11W 120.0 . . ? C15W C16W H16W 120.0 . . ? N11W C16W H16W 120.0 . . ? C26W N21W N22W 116.0(14) . . ? C26W N21W C25W 135.7(14) . . ? N22W N21W C25W 108.0 . . ? N21W N22W C23W 108.0 . . ? N21W N22W Pb1 129.0(9) . . ? C23W N22W Pb1 118.5(9) . . ? C12W C23W C24W 137.1(13) . . ? C12W C23W N22W 114.9(13) . . ? C24W C23W N22W 108.0 . . ? C23W C24W C25W 108.0 . . ? C23W C24W H24W 126.0 . . ? C25W C24W H24W 126.0 . . ? C24W C25W N21W 108.0 . . ? C24W C25W H25W 126.0 . . ? N21W C25W H25W 126.0 . . ? N21W C26W C31W 115.2(19) . . ? N21W C26W H26A 108.5 . . ? C31W C26W H26A 108.5 . . ? N21W C26W H26B 108.5 . . ? C31W C26W H26B 108.5 . . ? H26A C26W H26B 107.5 . . ? C32W C31W C33W 118(2) . . ? C32W C31W C26W 121(2) . . ? C33W C31W C26W 121.7(17) . . ? C31Y C32W C31W 121(2) 4_646 . ? C31Y C32W H32W 119.5 4_646 . ? C31W C32W H32W 119.5 . . ? C34W C33W C31W 122(2) . . ? C34W C33W H33W 119.2 . . ? C31W C33W H33W 119.2 . . ? C32Y C34W C33W 119(2) 4_646 . ? C32Y C34W H34W 120.4 4_646 . ? C33W C34W H34W 120.4 . . ? N321 C26Y C31Y 114.6(17) . . ? N321 C26Y H29W 108.6 . . ? C31Y C26Y H29W 108.6 . . ? N321 C26Y H27W 108.6 . . ? C31Y C26Y H27W 108.6 . . ? H29W C26Y H27W 107.6 . . ? C32W C31Y C32Y 120(2) 4_656 . ? C32W C31Y C26Y 122(2) 4_656 . ? C32Y C31Y C26Y 118(2) . . ? C34W C32Y C31Y 121(2) 4_656 . ? C34W C32Y H32Y 119.7 4_656 . ? C31Y C32Y H32Y 119.7 . . ? C12V N11V C16V 120.0 . . ? C12V N11V Pb1 122.3(7) . . ? C16V N11V Pb1 117.4(7) . . ? C23V C12V N11V 113.1(10) . . ? C23V C12V C13V 126.8(10) . . ? N11V C12V C13V 120.0 . . ? C14V C13V C12V 120.0 . . ? C14V C13V H13V 120.0 . . ? C12V C13V H13V 120.0 . . ? C15V C14V C13V 120.0 . . ? C15V C14V H14V 120.0 . . ? C13V C14V H14V 120.0 . . ? C14V C15V C16V 120.0 . . ? C14V C15V H15V 120.0 . . ? C16V C15V H15V 120.0 . . ? C15V C16V N11V 120.0 . . ? C15V C16V H16V 120.0 . . ? N11V C16V H16V 120.0 . . ? C26V N21V N22V 126.6(14) . . ? C26V N21V C25V 123.8(14) . . ? N22V N21V C25V 108.0 . . ? N21V N22V C23V 108.0 . . ? N21V N22V Pb1 134.0(7) . . ? C23V N22V Pb1 116.5(7) . . ? C12V C23V C24V 128.1(11) . . ? C12V C23V N22V 123.8(11) . . ? C24V C23V N22V 108.0 . . ? C25V C24V C23V 108.0 . . ? C25V C24V H24V 126.0 . . ? C23V C24V H24V 126.0 . . ? C24V C25V N21V 108.0 . . ? C24V C25V H25V 126.0 . . ? N21V C25V H25V 126.0 . . ? N21V C26V C31V 110.4(19) . . ? N21V C26V H26C 109.6 . . ? C31V C26V H26C 109.6 . . ? N21V C26V H26D 109.6 . . ? C31V C26V H26D 109.6 . . ? H26C C26V H26D 108.1 . . ? C32V C31V C33V 120(2) . . ? C32V C31V C26V 115.4(19) . . ? C33V C31V C26V 124.6(17) . . ? C31X C32V C31V 122(2) 4_646 . ? C31X C32V H32V 119.2 4_646 . ? C31V C32V H32V 119.2 . . ? C34V C33V C31V 119.8(19) . . ? C34V C33V H33V 120.1 . . ? C31V C33V H33V 120.1 . . ? C33V C34V C32X 118(2) . 4_646 ? C33V C34V H34V 120.8 . . ? C32X C34V H34V 120.8 4_646 . ? N321 C26X C31X 107.9(16) . . ? N321 C26X H26E 110.1 . . ? C31X C26X H26E 110.1 . . ? N321 C26X H26F 110.1 . . ? C31X C26X H26F 110.1 . . ? H26E C26X H26F 108.4 . . ? C32V C31X C32X 120(2) 4_656 . ? C32V C31X C26X 121(2) 4_656 . ? C32X C31X C26X 119(2) . . ? C31X C32X C34V 120(2) . 4_656 ? C31X C32X H32X 119.9 . . ? C34V C32X H32X 119.9 4_656 . ? C312 N311 C316 118.6(13) . . ? C312 N311 Pb1 122.6(8) . . ? C316 N311 Pb1 118.0(10) . . ? N311 C312 C313 123.0(12) . . ? N311 C312 C323 117.0(11) . . ? C313 C312 C323 120.0(12) . . ? C312 C313 C314 118.2(15) . . ? C312 C313 H313 120.9 . . ? C314 C313 H313 120.9 . . ? C315 C314 C313 118.9(15) . . ? C315 C314 H314 120.6 . . ? C313 C314 H314 120.6 . . ? C314 C315 C316 119.3(13) . . ? C314 C315 H315 120.3 . . ? C316 C315 H315 120.3 . . ? N311 C316 C315 121.8(15) . . ? N311 C316 H316 119.1 . . ? C315 C316 H316 119.1 . . ? N322 N321 C325 111.5(10) . . ? N322 N321 C26X 123.0(12) . . ? C325 N321 C26X 124.0(13) . . ? N322 N321 C26Y 117.1(12) . . ? C325 N321 C26Y 131.4(13) . . ? C26X N321 C26Y 14.0(17) . . ? C323 N322 N321 105.7(9) . . ? C323 N322 Pb1 119.3(7) . . ? N321 N322 Pb1 134.6(7) . . ? N322 C323 C324 110.7(10) . . ? N322 C323 C312 119.3(11) . . ? C324 C323 C312 130.0(11) . . ? C325 C324 C323 105.1(11) . . ? C325 C324 H324 127.4 . . ? C323 C324 H324 127.4 . . ? N321 C325 C324 106.9(11) . . ? N321 C325 H325 126.5 . . ? C324 C325 H325 126.5 . . ? O12X Cl1X O15X 108.7(3) . . ? O12X Cl1X O14X 108.6(3) . . ? O15X Cl1X O14X 108.6(3) . . ? O12X Cl1X O13X 108.6(3) . . ? O15X Cl1X O13X 113.7(13) . . ? O14X Cl1X O13X 108.6(3) . . ? O12Y Cl1Y O13Y 109.8(3) . . ? O12Y Cl1Y O14Y 109.8(3) . . ? O13Y Cl1Y O14Y 109.8(3) . . ? O12Y Cl1Y O15Y 109.8(3) . . ? O13Y Cl1Y O15Y 107.8(13) . . ? O14Y Cl1Y O15Y 109.8(3) . . ? O24X Cl2X O25X 110.6(4) . . ? O24X Cl2X O23X 110.4(4) . . ? O25X Cl2X O23X 105.1(17) . . ? O24X Cl2X O22X 110.3(4) . . ? O25X Cl2X O22X 110.2(4) . . ? O23X Cl2X O22X 110.1(4) . . ? O24Y Cl2Y O25Y 110.6(4) . . ? O24Y Cl2Y O23Y 110.6(4) . . ? O25Y Cl2Y O23Y 103.8(17) . . ? O24Y Cl2Y O22Y 110.6(4) . . ? O25Y Cl2Y O22Y 110.5(4) . . ? O23Y Cl2Y O22Y 110.5(4) . . ? N11S C12S C13S 177.9(18) . . ? C12S C13S H13A 109.5 . . ? C12S C13S H13B 109.5 . . ? H13A C13S H13B 109.5 . . ? C12S C13S H13C 109.5 . . ? H13A C13S H13C 109.5 . . ? H13B C13S H13C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N22W Pb1 N11X C12X -122.6(10) . . . . ? N22V Pb1 N11X C12X -114.8(9) . . . . ? N11W Pb1 N11X C12X 171.8(10) . . . . ? N11V Pb1 N11X C12X -178.6(9) . . . . ? N11Y Pb1 N11X C12X 84(2) . . . . ? N311 Pb1 N11X C12X 80.6(9) . . . . ? N22Y Pb1 N11X C12X -2.9(8) . . . . ? N22X Pb1 N11X C12X -11.0(9) . . . . ? N322 Pb1 N11X C12X 128.8(8) . . . . ? N22W Pb1 N11X C16X 64.3(7) . . . . ? N22V Pb1 N11X C16X 72.1(7) . . . . ? N11W Pb1 N11X C16X -1.3(7) . . . . ? N11V Pb1 N11X C16X 8.3(6) . . . . ? N11Y Pb1 N11X C16X -89.6(19) . . . . ? N311 Pb1 N11X C16X -92.5(6) . . . . ? N22Y Pb1 N11X C16X -176.0(8) . . . . ? N22X Pb1 N11X C16X 175.9(8) . . . . ? N322 Pb1 N11X C16X -44.3(8) . . . . ? C16X N11X C12X C23X -179.4(15) . . . . ? Pb1 N11X C12X C23X 7.6(16) . . . . ? C16X N11X C12X C13X 0.0 . . . . ? Pb1 N11X C12X C13X -173.0(10) . . . . ? C23X C12X C13X C14X 179.3(16) . . . . ? N11X C12X C13X C14X 0.0 . . . . ? C12X C13X C14X C15X 0.0 . . . . ? C13X C14X C15X C16X 0.0 . . . . ? C14X C15X C16X N11X 0.0 . . . . ? C12X N11X C16X C15X 0.0 . . . . ? Pb1 N11X C16X C15X 173.1(10) . . . . ? C126 N21X N22X C23X 175(2) . . . . ? C25X N21X N22X C23X 0.0 . . . . ? C126 N21X N22X Pb1 19(3) . . . . ? C25X N21X N22X Pb1 -155.2(18) . . . . ? N22W Pb1 N22X N21X -131.3(16) . . . . ? N22V Pb1 N22X N21X -121.1(16) . . . . ? N11W Pb1 N22X N21X 171.4(15) . . . . ? N11V Pb1 N22X N21X -172.6(15) . . . . ? N11X Pb1 N22X N21X 166.9(17) . . . . ? N11Y Pb1 N22X N21X 151.9(17) . . . . ? N311 Pb1 N22X N21X 77.1(16) . . . . ? N22Y Pb1 N22X N21X 97(5) . . . . ? N322 Pb1 N22X N21X 37.2(19) . . . . ? N22W Pb1 N22X C23X 73.9(12) . . . . ? N22V Pb1 N22X C23X 84.2(12) . . . . ? N11W Pb1 N22X C23X 16.7(16) . . . . ? N11V Pb1 N22X C23X 32.6(16) . . . . ? N11X Pb1 N22X C23X 12.2(11) . . . . ? N11Y Pb1 N22X C23X -2.9(11) . . . . ? N311 Pb1 N22X C23X -77.7(12) . . . . ? N22Y Pb1 N22X C23X -58(4) . . . . ? N322 Pb1 N22X C23X -117.6(12) . . . . ? N11X C12X C23X C24X -171.7(13) . . . . ? C13X C12X C23X C24X 9(2) . . . . ? N11X C12X C23X N22X 7(3) . . . . ? C13X C12X C23X N22X -172.4(15) . . . . ? N21X N22X C23X C12X -179(3) . . . . ? Pb1 N22X C23X C12X -16(2) . . . . ? N21X N22X C23X C24X 0.0 . . . . ? Pb1 N22X C23X C24X 162.4(13) . . . . ? C12X C23X C24X C25X 179(2) . . . . ? N22X C23X C24X C25X 0.0 . . . . ? C23X C24X C25X N21X 0.0 . . . . ? C126 N21X C25X C24X -173(3) . . . . ? N22X N21X C25X C24X 0.0 . . . . ? N22W Pb1 N11Y C12Y -107.0(9) . . . . ? N22V Pb1 N11Y C12Y -100.1(9) . . . . ? N11W Pb1 N11Y C12Y -171.4(9) . . . . ? N11V Pb1 N11Y C12Y -162.6(9) . . . . ? N11X Pb1 N11Y C12Y -82(2) . . . . ? N311 Pb1 N11Y C12Y 94.7(8) . . . . ? N22Y Pb1 N11Y C12Y 3.6(8) . . . . ? N22X Pb1 N11Y C12Y -3.5(9) . . . . ? N322 Pb1 N11Y C12Y 135.4(7) . . . . ? N22W Pb1 N11Y C16Y 69.7(6) . . . . ? N22V Pb1 N11Y C16Y 76.5(6) . . . . ? N11W Pb1 N11Y C16Y 5.2(6) . . . . ? N11V Pb1 N11Y C16Y 14.0(6) . . . . ? N11X Pb1 N11Y C16Y 94(2) . . . . ? N311 Pb1 N11Y C16Y -88.7(6) . . . . ? N22Y Pb1 N11Y C16Y -179.8(8) . . . . ? N22X Pb1 N11Y C16Y 173.1(8) . . . . ? N322 Pb1 N11Y C16Y -48.0(7) . . . . ? C16Y N11Y C12Y C13Y 0.0 . . . . ? Pb1 N11Y C12Y C13Y 176.6(10) . . . . ? C16Y N11Y C12Y C23Y 178.0(14) . . . . ? Pb1 N11Y C12Y C23Y -5.4(15) . . . . ? N11Y C12Y C13Y C14Y 0.0 . . . . ? C23Y C12Y C13Y C14Y -178.1(13) . . . . ? C12Y C13Y C14Y C15Y 0.0 . . . . ? C13Y C14Y C15Y C16Y 0.0 . . . . ? C14Y C15Y C16Y N11Y 0.0 . . . . ? C12Y N11Y C16Y C15Y 0.0 . . . . ? Pb1 N11Y C16Y C15Y -176.6(9) . . . . ? C126 N21Y N22Y C23Y 170.7(19) . . . . ? C25Y N21Y N22Y C23Y 0.0 . . . . ? C126 N21Y N22Y Pb1 -12(2) . . . . ? C25Y N21Y N22Y Pb1 177.0(15) . . . . ? N22W Pb1 N22Y C23Y 70.4(11) . . . . ? N22V Pb1 N22Y C23Y 81.0(11) . . . . ? N11W Pb1 N22Y C23Y 5.4(15) . . . . ? N11V Pb1 N22Y C23Y 20.4(15) . . . . ? N11X Pb1 N22Y C23Y 13.6(10) . . . . ? N11Y Pb1 N22Y C23Y -2.1(10) . . . . ? N311 Pb1 N22Y C23Y -80.2(11) . . . . ? N22X Pb1 N22Y C23Y 119(5) . . . . ? N322 Pb1 N22Y C23Y -112.3(10) . . . . ? N22W Pb1 N22Y N21Y -106.2(13) . . . . ? N22V Pb1 N22Y N21Y -95.6(14) . . . . ? N11W Pb1 N22Y N21Y -171.2(12) . . . . ? N11V Pb1 N22Y N21Y -156.2(12) . . . . ? N11X Pb1 N22Y N21Y -163.0(15) . . . . ? N11Y Pb1 N22Y N21Y -178.7(15) . . . . ? N311 Pb1 N22Y N21Y 103.2(13) . . . . ? N22X Pb1 N22Y N21Y -57(4) . . . . ? N322 Pb1 N22Y N21Y 71.1(15) . . . . ? C13Y C12Y C23Y N22Y -178.8(10) . . . . ? N11Y C12Y C23Y N22Y 3.2(18) . . . . ? C13Y C12Y C23Y C24Y -2(3) . . . . ? N11Y C12Y C23Y C24Y 179.9(16) . . . . ? N21Y N22Y C23Y C12Y 177.7(18) . . . . ? Pb1 N22Y C23Y C12Y 0.5(16) . . . . ? N21Y N22Y C23Y C24Y 0.0 . . . . ? Pb1 N22Y C23Y C24Y -177.2(14) . . . . ? C12Y C23Y C24Y C25Y -177(3) . . . . ? N22Y C23Y C24Y C25Y 0.0 . . . . ? C23Y C24Y C25Y N21Y 0.0 . . . . ? C126 N21Y C25Y C24Y -170.7(19) . . . . ? N22Y N21Y C25Y C24Y 0.0 . . . . ? N22X N21X C126 N21Y -3(23) . . . . ? C25X N21X C126 N21Y 169(26) . . . . ? N22X N21X C126 C131 -67.2(19) . . . . ? C25X N21X C126 C131 106(2) . . . . ? N22Y N21Y C126 N21X -168(26) . . . . ? C25Y N21Y C126 N21X 2(24) . . . . ? N22Y N21Y C126 C131 -49.8(19) . . . . ? C25Y N21Y C126 C131 119.3(14) . . . . ? N21X C126 C131 C132 -59.4(14) . . . . ? N21Y C126 C131 C132 -63.5(13) . . . . ? N21X C126 C131 C133 119.4(13) . . . . ? N21Y C126 C131 C133 115.3(12) . . . . ? C133 C131 C132 C131 -0.4(7) . . . 2_656 ? C126 C131 C132 C131 178.4(10) . . . 2_656 ? C132 C131 C133 C134 0.8(14) . . . . ? C126 C131 C133 C134 -178.0(8) . . . . ? C131 C133 C134 C133 -0.4(7) . . . 2_656 ? N22W Pb1 N11W C12W 16.2(9) . . . . ? N22V Pb1 N11W C12W 8.9(8) . . . . ? N11V Pb1 N11W C12W -13(3) . . . . ? N11X Pb1 N11W C12W 88.5(9) . . . . ? N11Y Pb1 N11W C12W 102.4(9) . . . . ? N311 Pb1 N11W C12W 178.9(8) . . . . ? N22Y Pb1 N11W C12W 95.7(11) . . . . ? N22X Pb1 N11W C12W 84.4(12) . . . . ? N322 Pb1 N11W C12W -123.1(9) . . . . ? N22W Pb1 N11W C16W -178.6(10) . . . . ? N22V Pb1 N11W C16W 174.1(10) . . . . ? N11V Pb1 N11W C16W 152(4) . . . . ? N11X Pb1 N11W C16W -106.3(10) . . . . ? N11Y Pb1 N11W C16W -92.4(9) . . . . ? N311 Pb1 N11W C16W -15.9(9) . . . . ? N22Y Pb1 N11W C16W -99.1(11) . . . . ? N22X Pb1 N11W C16W -110.4(11) . . . . ? N322 Pb1 N11W C16W 42.1(8) . . . . ? C16W N11W C12W C23W -179.9(17) . . . . ? Pb1 N11W C12W C23W -14.2(15) . . . . ? C16W N11W C12W C13W 0.0 . . . . ? Pb1 N11W C12W C13W 165.7(10) . . . . ? C23W C12W C13W C14W 179.9(16) . . . . ? N11W C12W C13W C14W 0.0 . . . . ? C12W C13W C14W C15W 0.0 . . . . ? C13W C14W C15W C16W 0.0 . . . . ? C14W C15W C16W N11W 0.0 . . . . ? C12W N11W C16W C15W 0.0 . . . . ? Pb1 N11W C16W C15W -164.5(11) . . . . ? C26W N21W N22W C23W 175.5(16) . . . . ? C25W N21W N22W C23W 0.0 . . . . ? C26W N21W N22W Pb1 -29.1(14) . . . . ? C25W N21W N22W Pb1 155.4(12) . . . . ? N22V Pb1 N22W N21W -33(3) . . . . ? N11W Pb1 N22W N21W -172.0(9) . . . . ? N11V Pb1 N22W N21W -166.2(10) . . . . ? N11X Pb1 N22W N21W 100.1(9) . . . . ? N11Y Pb1 N22W N21W 106.1(8) . . . . ? N311 Pb1 N22W N21W 151.8(7) . . . . ? N22Y Pb1 N22W N21W 48.8(9) . . . . ? N22X Pb1 N22W N21W 43.0(9) . . . . ? N322 Pb1 N22W N21W -129.2(8) . . . . ? N22V Pb1 N22W C23W 120(3) . . . . ? N11W Pb1 N22W C23W -18.8(9) . . . . ? N11V Pb1 N22W C23W -13.0(8) . . . . ? N11X Pb1 N22W C23W -106.7(10) . . . . ? N11Y Pb1 N22W C23W -100.7(9) . . . . ? N311 Pb1 N22W C23W -55.0(13) . . . . ? N22Y Pb1 N22W C23W -158.0(9) . . . . ? N22X Pb1 N22W C23W -163.8(9) . . . . ? N322 Pb1 N22W C23W 24.0(10) . . . . ? C13W C12W C23W C24W -5.8(19) . . . . ? N11W C12W C23W C24W 174.0(11) . . . . ? C13W C12W C23W N22W 176.9(9) . . . . ? N11W C12W C23W N22W -3.2(17) . . . . ? N21W N22W C23W C12W 178.0(11) . . . . ? Pb1 N22W C23W C12W 19.6(14) . . . . ? N21W N22W C23W C24W 0.0 . . . . ? Pb1 N22W C23W C24W -158.4(11) . . . . ? C12W C23W C24W C25W -177.3(15) . . . . ? N22W C23W C24W C25W 0.0 . . . . ? C23W C24W C25W N21W 0.0 . . . . ? C26W N21W C25W C24W -174(2) . . . . ? N22W N21W C25W C24W 0.0 . . . . ? N22W N21W C26W C31W -75(2) . . . . ? C25W N21W C26W C31W 98(2) . . . . ? N21W C26W C31W C32W 177(2) . . . . ? N21W C26W C31W C33W -7(3) . . . . ? C33W C31W C32W C31Y 0(4) . . . 4_646 ? C26W C31W C32W C31Y 176(2) . . . 4_646 ? C32W C31W C33W C34W -2(4) . . . . ? C26W C31W C33W C34W -178(2) . . . . ? C31W C33W C34W C32Y 3(4) . . . 4_646 ? N321 C26Y C31Y C32W 99(3) . . . 4_656 ? N321 C26Y C31Y C32Y -80(3) . . . . ? C32W C31Y C32Y C34W -1(4) 4_656 . . 4_656 ? C26Y C31Y C32Y C34W 179(2) . . . 4_656 ? N22W Pb1 N11V C12V 19.4(8) . . . . ? N22V Pb1 N11V C12V 10.8(9) . . . . ? N11W Pb1 N11V C12V 167(4) . . . . ? N11X Pb1 N11V C12V 90.4(9) . . . . ? N11Y Pb1 N11V C12V 104.0(9) . . . . ? N311 Pb1 N11V C12V 179.4(8) . . . . ? N22Y Pb1 N11V C12V 84.4(11) . . . . ? N22X Pb1 N11V C12V 72.0(12) . . . . ? N322 Pb1 N11V C12V -126.2(9) . . . . ? N22W Pb1 N11V C16V -167.3(10) . . . . ? N22V Pb1 N11V C16V -176.0(9) . . . . ? N11W Pb1 N11V C16V -20(3) . . . . ? N11X Pb1 N11V C16V -96.3(8) . . . . ? N11Y Pb1 N11V C16V -82.7(8) . . . . ? N311 Pb1 N11V C16V -7.3(8) . . . . ? N22Y Pb1 N11V C16V -102.4(10) . . . . ? N22X Pb1 N11V C16V -114.7(10) . . . . ? N322 Pb1 N11V C16V 47.0(8) . . . . ? C16V N11V C12V C23V 177.1(14) . . . . ? Pb1 N11V C12V C23V -9.8(13) . . . . ? C16V N11V C12V C13V 0.0 . . . . ? Pb1 N11V C12V C13V 173.1(10) . . . . ? C23V C12V C13V C14V -176.7(16) . . . . ? N11V C12V C13V C14V 0.0 . . . . ? C12V C13V C14V C15V 0.0 . . . . ? C13V C14V C15V C16V 0.0 . . . . ? C14V C15V C16V N11V 0.0 . . . . ? C12V N11V C16V C15V 0.0 . . . . ? Pb1 N11V C16V C15V -173.4(10) . . . . ? C26V N21V N22V C23V 165.5(18) . . . . ? C25V N21V N22V C23V 0.0 . . . . ? C26V N21V N22V Pb1 -29.5(16) . . . . ? C25V N21V N22V Pb1 165.0(12) . . . . ? N22W Pb1 N22V N21V 144(3) . . . . ? N11W Pb1 N22V N21V -178.0(9) . . . . ? N11V Pb1 N22V N21V -173.9(9) . . . . ? N11X Pb1 N22V N21V 99.2(8) . . . . ? N11Y Pb1 N22V N21V 103.4(8) . . . . ? N311 Pb1 N22V N21V 151.1(9) . . . . ? N22Y Pb1 N22V N21V 43.3(9) . . . . ? N22X Pb1 N22V N21V 38.5(8) . . . . ? N322 Pb1 N22V N21V -126.9(7) . . . . ? N22W Pb1 N22V C23V -52(3) . . . . ? N11W Pb1 N22V C23V -14.0(8) . . . . ? N11V Pb1 N22V C23V -9.9(8) . . . . ? N11X Pb1 N22V C23V -96.8(9) . . . . ? N11Y Pb1 N22V C23V -92.6(8) . . . . ? N311 Pb1 N22V C23V -44.9(16) . . . . ? N22Y Pb1 N22V C23V -152.7(8) . . . . ? N22X Pb1 N22V C23V -157.4(8) . . . . ? N322 Pb1 N22V C23V 37.1(10) . . . . ? N11V C12V C23V C24V 177.3(9) . . . . ? C13V C12V C23V C24V -5.8(18) . . . . ? N11V C12V C23V N22V -0.7(15) . . . . ? C13V C12V C23V N22V 176.2(10) . . . . ? N21V N22V C23V C12V 178.3(12) . . . . ? Pb1 N22V C23V C12V 10.3(14) . . . . ? N21V N22V C23V C24V 0.0 . . . . ? Pb1 N22V C23V C24V -168.0(10) . . . . ? C12V C23V C24V C25V -178.2(12) . . . . ? N22V C23V C24V C25V 0.0 . . . . ? C23V C24V C25V N21V 0.0 . . . . ? C26V N21V C25V C24V -166.0(18) . . . . ? N22V N21V C25V C24V 0.0 . . . . ? N22V N21V C26V C31V -69(2) . . . . ? C25V N21V C26V C31V 94(2) . . . . ? N21V C26V C31V C32V 163(2) . . . . ? N21V C26V C31V C33V -21(3) . . . . ? C33V C31V C32V C31X 1(4) . . . 4_646 ? C26V C31V C32V C31X 177(3) . . . 4_646 ? C32V C31V C33V C34V -1(4) . . . . ? C26V C31V C33V C34V -177(2) . . . . ? C31V C33V C34V C32X -1(4) . . . 4_646 ? N321 C26X C31X C32V 119(3) . . . 4_656 ? N321 C26X C31X C32X -62(3) . . . . ? C32V C31X C32X C34V -1(4) 4_656 . . 4_656 ? C26X C31X C32X C34V 179(2) . . . 4_656 ? N22W Pb1 N311 C312 102.4(11) . . . . ? N22V Pb1 N311 C312 99.7(13) . . . . ? N11W Pb1 N311 C312 70.5(9) . . . . ? N11V Pb1 N311 C312 68.4(9) . . . . ? N11X Pb1 N311 C312 149.7(9) . . . . ? N11Y Pb1 N311 C312 149.0(9) . . . . ? N22Y Pb1 N311 C312 -149.6(9) . . . . ? N22X Pb1 N311 C312 -147.1(9) . . . . ? N322 Pb1 N311 C312 6.9(8) . . . . ? N22W Pb1 N311 C316 -87.3(12) . . . . ? N22V Pb1 N311 C316 -90.1(14) . . . . ? N11W Pb1 N311 C316 -119.2(9) . . . . ? N11V Pb1 N311 C316 -121.3(9) . . . . ? N11X Pb1 N311 C316 -40.0(9) . . . . ? N11Y Pb1 N311 C316 -40.7(8) . . . . ? N22Y Pb1 N311 C316 20.6(9) . . . . ? N22X Pb1 N311 C316 23.1(9) . . . . ? N322 Pb1 N311 C316 177.2(9) . . . . ? C316 N311 C312 C313 2.2(17) . . . . ? Pb1 N311 C312 C313 172.4(9) . . . . ? C316 N311 C312 C323 -177.4(10) . . . . ? Pb1 N311 C312 C323 -7.2(13) . . . . ? N311 C312 C313 C314 -0.7(19) . . . . ? C323 C312 C313 C314 178.9(12) . . . . ? C312 C313 C314 C315 0(2) . . . . ? C313 C314 C315 C316 -1(2) . . . . ? C312 N311 C316 C315 -2.8(17) . . . . ? Pb1 N311 C316 C315 -173.5(9) . . . . ? C314 C315 C316 N311 2.1(19) . . . . ? C31X C26X N321 N322 157.9(17) . . . . ? C31X C26X N321 C325 -37(3) . . . . ? C31X C26X N321 C26Y 89(6) . . . . ? C31Y C26Y N321 N322 154.6(19) . . . . ? C31Y C26Y N321 C325 -24(4) . . . . ? C31Y C26Y N321 C26X -87(6) . . . . ? C325 N321 N322 C323 0.9(13) . . . . ? C26X N321 N322 C323 167.3(16) . . . . ? C26Y N321 N322 C323 -178.0(16) . . . . ? C325 N321 N322 Pb1 173.3(9) . . . . ? C26X N321 N322 Pb1 -20(2) . . . . ? C26Y N321 N322 Pb1 -6(2) . . . . ? N22W Pb1 N322 C323 -151.9(8) . . . . ? N22V Pb1 N322 C323 -163.8(8) . . . . ? N11W Pb1 N322 C323 -110.8(9) . . . . ? N11V Pb1 N322 C323 -120.5(9) . . . . ? N11X Pb1 N322 C323 -64.4(10) . . . . ? N11Y Pb1 N322 C323 -52.7(9) . . . . ? N311 Pb1 N322 C323 -6.2(7) . . . . ? N22Y Pb1 N322 C323 31.0(11) . . . . ? N22X Pb1 N322 C323 40.9(11) . . . . ? N22W Pb1 N322 N321 36.5(11) . . . . ? N22V Pb1 N322 N321 24.7(11) . . . . ? N11W Pb1 N322 N321 77.6(10) . . . . ? N11V Pb1 N322 N321 68.0(10) . . . . ? N11X Pb1 N322 N321 124.0(10) . . . . ? N11Y Pb1 N322 N321 135.8(10) . . . . ? N311 Pb1 N322 N321 -177.7(11) . . . . ? N22Y Pb1 N322 N321 -140.6(10) . . . . ? N22X Pb1 N322 N321 -130.6(11) . . . . ? N321 N322 C323 C324 0.1(13) . . . . ? Pb1 N322 C323 C324 -173.6(8) . . . . ? N321 N322 C323 C312 179.3(9) . . . . ? Pb1 N322 C323 C312 5.5(13) . . . . ? N311 C312 C323 N322 0.9(15) . . . . ? C313 C312 C323 N322 -178.8(11) . . . . ? N311 C312 C323 C324 179.9(12) . . . . ? C313 C312 C323 C324 0.2(19) . . . . ? N322 C323 C324 C325 -1.1(15) . . . . ? C312 C323 C324 C325 179.8(12) . . . . ? N322 N321 C325 C324 -1.7(15) . . . . ? C26X N321 C325 C324 -167.8(16) . . . . ? C26Y N321 C325 C324 177(2) . . . . ? C323 C324 C325 N321 1.6(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.40 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.446 _refine_diff_density_min -1.716 _refine_diff_density_rms 0.180 #===END data_imw1255p-1 _database_code_depnum_ccdc_archive 'CCDC 778865' #TrackingRef '- lead_networks.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H47 Cl4 N17 O22 Pb2' _chemical_formula_weight 1782.22 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' Cl Cl 0.1484 0.1585 '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 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6268(6) _cell_length_b 12.1895(6) _cell_length_c 13.5805(7) _cell_angle_alpha 102.909(3) _cell_angle_beta 102.681(3) _cell_angle_gamma 102.962(2) _cell_volume 1753.04(15) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 2846 _cell_measurement_theta_min 2.72 _cell_measurement_theta_max 21.71 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 868 _exptl_absorpt_coefficient_mu 5.029 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5000 _exptl_absorpt_correction_T_max 0.6891 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21014 _diffrn_reflns_av_R_equivalents 0.0670 _diffrn_reflns_av_sigmaI/netI 0.0982 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7816 _reflns_number_gt 5679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; The structure is of a polymer or unit {[Pb2L2](ClO4)4}.3MeNO2. The data has been solved by Patterson methods. The lattice contains 1.5 MeNO2 molecules in the asymmetric unit. These have been modelled as three molecules of 50 % occupancy, each of which is further disordered over two sites (O11 > C14, 25:25; O21 > C24, 40:10, and O31 > C34, 20:30). The occupancies were determined experimentally and then rounded and fixed. The lattice also contains a disordered perchlorate anion, displaying pivital disorder about the Cl11 atom (Cl11 > O15; 62:38). All disordered residues have benefited from the application of geometric and displacement restraints and have been left isotropic. There is higher than usual residual density. This resides next to the metal and is presumably a result of the metals diffuse electron cloud. 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^)+(0.0867P)^2^+4.2541P] 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 7816 _refine_ls_number_parameters 467 _refine_ls_number_restraints 92 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0584 _refine_ls_wR_factor_ref 0.1610 _refine_ls_wR_factor_gt 0.1423 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.013 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.20092(3) 0.14484(3) 0.26052(3) 0.02678(13) Uani 1 1 d . . . N111 N 0.2591(7) 0.3656(7) 0.3528(6) 0.0298(18) Uani 1 1 d . A . C112 C 0.2259(8) 0.4410(8) 0.3010(8) 0.030(2) Uani 1 1 d . . . C113 C 0.2557(10) 0.5609(9) 0.3521(9) 0.040(3) Uani 1 1 d . A . H113 H 0.2334 0.6126 0.3134 0.048 Uiso 1 1 calc R . . C114 C 0.3171(9) 0.6051(8) 0.4579(9) 0.037(2) Uani 1 1 d . . . H114 H 0.3350 0.6859 0.4940 0.045 Uiso 1 1 calc R A . C115 C 0.3511(10) 0.5269(9) 0.5089(9) 0.045(3) Uani 1 1 d . A . H115 H 0.3941 0.5533 0.5819 0.054 Uiso 1 1 calc R . . C116 C 0.3226(9) 0.4099(9) 0.4539(8) 0.036(2) Uani 1 1 d . . . H116 H 0.3499 0.3581 0.4902 0.043 Uiso 1 1 calc R A . N121 N 0.1166(7) 0.2785(7) 0.1439(6) 0.0272(17) Uani 1 1 d . A . N122 N 0.0621(7) 0.2647(7) 0.0415(6) 0.0311(18) Uani 1 1 d . . . C123 C 0.1600(9) 0.3940(8) 0.1883(8) 0.032(2) Uani 1 1 d . A . C124 C 0.1322(11) 0.4541(10) 0.1146(10) 0.050(3) Uani 1 1 d . . . H124 H 0.1515 0.5369 0.1271 0.060 Uiso 1 1 calc R A . C125 C 0.0708(11) 0.3693(9) 0.0195(9) 0.045(3) Uani 1 1 d . A . H125 H 0.0412 0.3814 -0.0470 0.054 Uiso 1 1 calc R . . C126 C 0.0147(8) 0.1498(8) -0.0330(8) 0.031(2) Uani 1 1 d . . . H12A H -0.0491 0.1514 -0.0940 0.038 Uiso 1 1 calc R . . H12B H -0.0247 0.0932 0.0004 0.038 Uiso 1 1 calc R . . N211 N 0.2887(7) 0.1414(7) 0.4453(6) 0.0302(18) Uani 1 1 d . A . C212 C 0.2165(8) 0.1403(8) 0.5109(8) 0.032(2) Uani 1 1 d . . . C213 C 0.2564(11) 0.1326(11) 0.6133(9) 0.048(3) Uani 1 1 d . A . H213 H 0.2041 0.1339 0.6581 0.058 Uiso 1 1 calc R . . C214 C 0.3754(10) 0.1230(12) 0.6484(10) 0.054(3) Uani 1 1 d . . . H214 H 0.4053 0.1160 0.7170 0.064 Uiso 1 1 calc R A . C215 C 0.4491(9) 0.1240(10) 0.5793(9) 0.044(3) Uani 1 1 d . A . H215 H 0.5311 0.1201 0.6017 0.053 Uiso 1 1 calc R . . C216 C 0.4027(8) 0.1307(9) 0.4788(9) 0.037(2) Uani 1 1 d . . . H216 H 0.4524 0.1277 0.4319 0.045 Uiso 1 1 calc R A . N221 N 0.0608(6) 0.1592(6) 0.3697(6) 0.0288(18) Uani 1 1 d . A . N222 N -0.0561(7) 0.1667(7) 0.3503(7) 0.0314(19) Uani 1 1 d . . . C223 C 0.0927(8) 0.1501(8) 0.4661(8) 0.032(2) Uani 1 1 d . A . C224 C -0.0069(9) 0.1505(9) 0.5104(9) 0.038(2) Uani 1 1 d . . . H224 H -0.0095 0.1451 0.5786 0.046 Uiso 1 1 calc R A . C225 C -0.0974(9) 0.1604(9) 0.4341(9) 0.041(3) Uani 1 1 d . A . H225 H -0.1772 0.1625 0.4391 0.049 Uiso 1 1 calc R . . C226 C -0.1208(9) 0.1662(9) 0.2460(8) 0.036(2) Uani 1 1 d . A . H17A H -0.0652 0.2187 0.2193 0.044 Uiso 1 1 calc R . . H17B H -0.1921 0.1969 0.2500 0.044 Uiso 1 1 calc R . . N251 N -0.0800(7) 0.0026(7) 0.1352(6) 0.0286(18) Uani 1 1 d . A . C252 C -0.1653(9) 0.0439(9) 0.1703(8) 0.032(2) Uani 1 1 d . . . C253 C -0.2879(10) -0.0219(11) 0.1438(9) 0.048(3) Uani 1 1 d . A . H253 H -0.3462 0.0101 0.1701 0.058 Uiso 1 1 calc R . . C254 C -0.3214(10) -0.1329(12) 0.0796(11) 0.061(4) Uani 1 1 d . . . H254 H -0.4043 -0.1801 0.0605 0.074 Uiso 1 1 calc R A . C255 C -0.2343(10) -0.1786(11) 0.0412(10) 0.054(3) Uani 1 1 d . A . H255 H -0.2570 -0.2560 -0.0047 0.065 Uiso 1 1 calc R . . C256 C -0.1157(9) -0.1084(9) 0.0717(8) 0.035(2) Uani 1 1 d . . . Cl11 Cl 0.5261(2) 0.1955(2) 0.2376(2) 0.0416(6) Uani 1 1 d D . . O12X O 0.5825(12) 0.1366(13) 0.3071(8) 0.048(4) Uiso 0.62(3) 1 d PD A 1 O13X O 0.4597(10) 0.1120(12) 0.1366(7) 0.064(5) Uiso 0.62(3) 1 d PD A 1 O14X O 0.4423(9) 0.2471(11) 0.2822(9) 0.054(9) Uiso 0.62(3) 1 d PD A 1 O15X O 0.6200(10) 0.2863(8) 0.2249(15) 0.070(5) Uiso 0.62(3) 1 d PD A 1 O12Y O 0.6167(14) 0.1804(19) 0.3206(8) 0.038(6) Uiso 0.38(3) 1 d PD A 2 O13Y O 0.4497(12) 0.0820(9) 0.1693(17) 0.058(8) Uiso 0.38(3) 1 d PD A 2 O14Y O 0.4507(12) 0.2593(14) 0.2825(11) 0.029(10) Uiso 0.38(3) 1 d PD A 2 O15Y O 0.5870(18) 0.2601(18) 0.1776(18) 0.054(8) Uiso 0.38(3) 1 d PD A 2 Cl21 Cl 0.1984(2) 0.8522(2) 0.2888(2) 0.0383(6) Uani 1 1 d . . . O22 O 0.2399(6) 0.8366(6) 0.3903(6) 0.0386(17) Uani 1 1 d . . . O23 O 0.1509(9) 0.7410(7) 0.2093(7) 0.076(3) Uani 1 1 d . . . O24 O 0.1034(6) 0.9115(6) 0.2873(6) 0.0357(16) Uani 1 1 d . . . O25 O 0.2994(8) 0.9276(8) 0.2653(7) 0.053(2) Uani 1 1 d . . . O11V O 0.390(2) 0.688(2) 0.068(2) 0.042(5) Uiso 0.25 1 d PDU B 1 O12V O 0.2134(19) 0.647(2) -0.049(2) 0.044(5) Uiso 0.25 1 d PDU B 1 N13V N 0.308(2) 0.7163(15) 0.016(2) 0.042(4) Uiso 0.25 1 d PDU B 1 C14V C 0.329(4) 0.8422(17) 0.024(5) 0.041(5) Uiso 0.25 1 d PDU B 1 H14A H 0.3935 0.8664 -0.0100 0.062 Uiso 0.25 1 calc PR B 1 H14B H 0.3562 0.8882 0.0979 0.062 Uiso 0.25 1 calc PR B 1 H14C H 0.2532 0.8556 -0.0121 0.062 Uiso 0.25 1 calc PR B 1 O11W O 0.1838(18) 0.696(2) -0.068(2) 0.044(5) Uiso 0.25 1 d PDU C 2 O12W O 0.341(2) 0.662(2) 0.028(2) 0.046(5) Uiso 0.25 1 d PDU C 2 N13W N 0.286(2) 0.7275(15) -0.006(2) 0.043(4) Uiso 0.25 1 d PDU C 2 C14W C 0.345(4) 0.8551(16) 0.039(5) 0.043(5) Uiso 0.25 1 d PDU C 2 H14D H 0.3835 0.8851 -0.0109 0.064 Uiso 0.25 1 calc PR C 2 H14E H 0.4076 0.8705 0.1055 0.064 Uiso 0.25 1 calc PR C 2 H14F H 0.2824 0.8944 0.0513 0.064 Uiso 0.25 1 calc PR C 2 O21X O 0.3496(17) 0.392(2) 0.8334(15) 0.070(4) Uiso 0.40 1 d PDU D 1 O22X O 0.4174(19) 0.422(2) 0.7020(13) 0.072(4) Uiso 0.40 1 d PDU D 1 N23X N 0.4245(16) 0.4430(19) 0.7964(12) 0.068(4) Uiso 0.40 1 d PDU D 1 C24X C 0.535(2) 0.532(3) 0.8712(18) 0.065(5) Uiso 0.40 1 d PDU D 1 H24A H 0.5174 0.5614 0.9380 0.097 Uiso 0.40 1 calc PR D 1 H24B H 0.5581 0.5977 0.8418 0.097 Uiso 0.40 1 calc PR D 1 H24C H 0.6029 0.4972 0.8836 0.097 Uiso 0.40 1 calc PR D 1 O21Y O 0.445(4) 0.338(4) 0.887(5) 0.046(11) Uiso 0.10 1 d PDU E 2 O22Y O 0.562(4) 0.356(5) 0.783(5) 0.044(11) Uiso 0.10 1 d PDU E 2 N23Y N 0.509(4) 0.395(3) 0.846(4) 0.045(10) Uiso 0.10 1 d PDU E 2 C24Y C 0.510(10) 0.520(4) 0.862(8) 0.044(11) Uiso 0.10 1 d PDU E 2 H24D H 0.5189 0.5429 0.7989 0.067 Uiso 0.10 1 calc PR E 2 H24E H 0.5796 0.5690 0.9225 0.067 Uiso 0.10 1 calc PR E 2 H24F H 0.4331 0.5291 0.8753 0.067 Uiso 0.10 1 calc PR E 2 O31X O -0.257(3) 0.585(4) 0.303(4) 0.081(9) Uiso 0.20 1 d PDU F 1 O32X O -0.092(4) 0.528(4) 0.304(4) 0.080(9) Uiso 0.20 1 d PDU F 1 N33X N -0.164(3) 0.583(3) 0.276(3) 0.080(9) Uiso 0.20 1 d PDU F 1 C34X C -0.126(6) 0.665(6) 0.216(5) 0.079(10) Uiso 0.20 1 d PDU F 1 H34A H -0.0414 0.7143 0.2519 0.118 Uiso 0.20 1 calc PR F 1 H34B H -0.1812 0.7143 0.2101 0.118 Uiso 0.20 1 calc PR F 1 H34C H -0.1297 0.6198 0.1447 0.118 Uiso 0.20 1 calc PR F 1 O31Y O -0.009(2) 0.421(2) 0.402(2) 0.066(5) Uiso 0.30 1 d PDU . 2 O32Y O -0.041(3) 0.568(2) 0.5042(17) 0.066(5) Uiso 0.30 1 d PDU . 2 N33Y N -0.052(3) 0.503(2) 0.4170(14) 0.066(5) Uiso 0.30 1 d PDU . 2 C34Y C -0.112(5) 0.534(4) 0.324(2) 0.065(6) Uiso 0.30 1 d PDU G 2 H34D H -0.1344 0.6062 0.3462 0.098 Uiso 0.30 1 calc PR G 2 H34E H -0.1858 0.4698 0.2817 0.098 Uiso 0.30 1 calc PR G 2 H34F H -0.0547 0.5459 0.2808 0.098 Uiso 0.30 1 calc PR G 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.02819(18) 0.02211(18) 0.0275(2) 0.00074(13) 0.00656(13) 0.00998(12) N111 0.030(4) 0.024(4) 0.031(4) 0.000(4) 0.005(3) 0.012(3) C112 0.034(5) 0.026(5) 0.028(5) 0.002(4) 0.005(4) 0.016(4) C113 0.052(6) 0.026(5) 0.036(6) 0.006(5) 0.004(5) 0.012(5) C114 0.044(6) 0.015(5) 0.043(6) -0.004(4) 0.011(5) 0.003(4) C115 0.051(6) 0.033(6) 0.033(6) -0.010(5) 0.001(5) 0.010(5) C116 0.044(5) 0.029(5) 0.027(5) -0.001(4) 0.001(4) 0.015(4) N121 0.031(4) 0.025(4) 0.026(4) 0.003(3) 0.008(3) 0.013(3) N122 0.045(5) 0.023(4) 0.026(4) 0.003(3) 0.007(3) 0.017(4) C123 0.037(5) 0.022(5) 0.033(6) -0.003(4) 0.005(4) 0.014(4) C124 0.059(7) 0.025(6) 0.055(8) 0.007(5) -0.003(6) 0.013(5) C125 0.068(7) 0.024(5) 0.036(6) 0.004(5) 0.002(5) 0.017(5) C126 0.034(5) 0.028(5) 0.030(5) 0.003(4) 0.007(4) 0.014(4) N211 0.029(4) 0.022(4) 0.032(5) 0.000(3) 0.002(3) 0.007(3) C212 0.030(5) 0.020(5) 0.038(6) 0.006(4) -0.002(4) 0.002(4) C213 0.054(7) 0.051(7) 0.039(7) 0.016(6) 0.013(5) 0.010(6) C214 0.043(6) 0.067(9) 0.049(8) 0.026(7) 0.003(5) 0.012(6) C215 0.033(5) 0.042(6) 0.048(7) 0.013(6) -0.003(5) 0.010(5) C216 0.025(4) 0.038(6) 0.042(6) 0.010(5) -0.001(4) 0.006(4) N221 0.026(4) 0.018(4) 0.035(5) -0.005(3) 0.009(3) 0.005(3) N222 0.029(4) 0.033(5) 0.035(5) 0.002(4) 0.013(3) 0.017(3) C223 0.032(5) 0.024(5) 0.033(6) 0.002(4) 0.006(4) 0.006(4) C224 0.042(6) 0.034(6) 0.038(6) 0.005(5) 0.020(5) 0.007(4) C225 0.026(5) 0.039(6) 0.052(7) 0.000(5) 0.014(5) 0.009(4) C226 0.034(5) 0.039(6) 0.041(6) 0.005(5) 0.016(4) 0.022(4) N251 0.030(4) 0.027(4) 0.025(4) 0.003(3) 0.003(3) 0.012(3) C252 0.035(5) 0.038(6) 0.029(5) 0.009(4) 0.011(4) 0.020(4) C253 0.047(6) 0.051(7) 0.039(7) -0.006(6) 0.017(5) 0.013(5) C254 0.033(6) 0.061(9) 0.070(9) -0.011(7) 0.014(6) 0.006(5) C255 0.042(6) 0.041(7) 0.055(8) -0.015(6) 0.009(5) -0.004(5) C256 0.033(5) 0.035(6) 0.035(6) 0.010(5) 0.005(4) 0.010(4) Cl11 0.0372(12) 0.0407(15) 0.0436(15) 0.0009(12) 0.0105(11) 0.0167(11) Cl21 0.0490(14) 0.0283(12) 0.0307(13) -0.0013(11) -0.0022(11) 0.0208(11) O22 0.047(4) 0.037(4) 0.036(4) 0.015(3) 0.008(3) 0.021(3) O23 0.100(7) 0.039(5) 0.057(6) -0.020(4) -0.034(5) 0.044(5) O24 0.037(3) 0.027(4) 0.039(4) 0.003(3) 0.003(3) 0.014(3) O25 0.065(5) 0.064(6) 0.052(5) 0.027(5) 0.028(4) 0.039(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 N221 2.440(8) . ? Pb1 N211 2.506(8) . ? Pb1 N111 2.564(8) . ? Pb1 N121 2.704(7) . ? Pb1 O14X 2.724(10) . ? N111 C116 1.328(12) . ? N111 C112 1.348(12) . ? C112 C113 1.398(13) . ? C112 C123 1.468(13) . ? C113 C114 1.376(15) . ? C113 H113 0.9500 . ? C114 C115 1.375(15) . ? C114 H114 0.9500 . ? C115 C116 1.381(14) . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? N121 C123 1.329(12) . ? N121 N122 1.351(11) . ? N122 C125 1.360(13) . ? N122 C126 1.437(12) . ? C123 C124 1.391(15) . ? C124 C125 1.384(15) . ? C124 H124 0.9500 . ? C125 H125 0.9500 . ? C126 C256 1.526(13) 2 ? C126 H12A 0.9900 . ? C126 H12B 0.9900 . ? N211 C216 1.349(11) . ? N211 C212 1.351(13) . ? C212 C213 1.397(15) . ? C212 C223 1.477(12) . ? C213 C214 1.401(15) . ? C213 H213 0.9500 . ? C214 C215 1.403(17) . ? C214 H214 0.9500 . ? C215 C216 1.381(15) . ? C215 H215 0.9500 . ? C216 H216 0.9500 . ? N221 C223 1.317(13) . ? N221 N222 1.354(10) . ? N222 C225 1.339(14) . ? N222 C226 1.449(13) . ? C223 C224 1.417(14) . ? C224 C225 1.353(15) . ? C224 H224 0.9500 . ? C225 H225 0.9500 . ? C226 C252 1.511(14) . ? C226 H17A 0.9900 . ? C226 H17B 0.9900 . ? N251 C252 1.338(11) . ? N251 C256 1.347(13) . ? C252 C253 1.392(15) . ? C253 C254 1.353(16) . ? C253 H253 0.9500 . ? C254 C255 1.400(16) . ? C254 H254 0.9500 . ? C255 C256 1.366(14) . ? C255 H255 0.9500 . ? C256 C126 1.526(13) 2 ? Cl11 O13X 1.4391(19) . ? Cl11 O12Y 1.4393(19) . ? Cl11 O15X 1.4396(19) . ? Cl11 O15Y 1.4398(19) . ? Cl11 O14Y 1.4408(19) . ? Cl11 O13Y 1.4409(19) . ? Cl11 O12X 1.4410(19) . ? Cl11 O14X 1.4412(19) . ? Cl21 O22 1.426(7) . ? Cl21 O23 1.434(8) . ? Cl21 O24 1.448(6) . ? Cl21 O25 1.462(9) . ? O11V N13V 1.219(2) . ? O12V N13V 1.231(2) . ? N13V C14V 1.474(2) . ? C14V H14A 0.9800 . ? C14V H14B 0.9800 . ? C14V H14C 0.9800 . ? O11W N13W 1.2181(19) . ? O12W N13W 1.2311(19) . ? N13W C14W 1.4741(19) . ? C14W H14D 0.9800 . ? C14W H14E 0.9800 . ? C14W H14F 0.9800 . ? O21X N23X 1.2177(18) . ? O22X N23X 1.2310(18) . ? N23X C24X 1.4737(19) . ? C24X H24A 0.9800 . ? C24X H24B 0.9800 . ? C24X H24C 0.9800 . ? O21Y N23Y 1.218(2) . ? O22Y N23Y 1.232(2) . ? N23Y C24Y 1.474(2) . ? C24Y H24D 0.9800 . ? C24Y H24E 0.9800 . ? C24Y H24F 0.9800 . ? O31X N33X 1.219(2) . ? O32X N33X 1.232(2) . ? N33X C34X 1.475(2) . ? C34X H34A 0.9800 . ? C34X H34B 0.9800 . ? C34X H34C 0.9800 . ? O31Y N33Y 1.2183(19) . ? O31Y O32Y 1.24(3) 2_566 ? O32Y N33Y 1.2311(19) . ? O32Y O31Y 1.24(3) 2_566 ? O32Y N33Y 1.84(4) 2_566 ? N33Y C34Y 1.4740(19) . ? N33Y O32Y 1.84(4) 2_566 ? C34Y H34D 0.9800 . ? C34Y H34E 0.9800 . ? C34Y H34F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N221 Pb1 N211 66.1(3) . . ? N221 Pb1 N111 76.4(3) . . ? N211 Pb1 N111 81.4(2) . . ? N221 Pb1 N121 94.8(2) . . ? N211 Pb1 N121 143.7(2) . . ? N111 Pb1 N121 63.6(2) . . ? N221 Pb1 O14X 136.3(3) . . ? N211 Pb1 O14X 81.7(3) . . ? N111 Pb1 O14X 69.9(2) . . ? N121 Pb1 O14X 94.4(3) . . ? C116 N111 C112 117.5(8) . . ? C116 N111 Pb1 121.1(6) . . ? C112 N111 Pb1 121.4(6) . . ? N111 C112 C113 121.2(9) . . ? N111 C112 C123 118.1(8) . . ? C113 C112 C123 120.7(9) . . ? C114 C113 C112 120.8(10) . . ? C114 C113 H113 119.6 . . ? C112 C113 H113 119.6 . . ? C115 C114 C113 117.0(9) . . ? C115 C114 H114 121.5 . . ? C113 C114 H114 121.5 . . ? C114 C115 C116 119.8(10) . . ? C114 C115 H115 120.1 . . ? C116 C115 H115 120.1 . . ? N111 C116 C115 123.6(10) . . ? N111 C116 H116 118.2 . . ? C115 C116 H116 118.2 . . ? C123 N121 N122 105.5(8) . . ? C123 N121 Pb1 115.6(6) . . ? N122 N121 Pb1 137.0(5) . . ? N121 N122 C125 112.2(8) . . ? N121 N122 C126 120.7(8) . . ? C125 N122 C126 126.7(9) . . ? N121 C123 C124 110.7(9) . . ? N121 C123 C112 120.1(9) . . ? C124 C123 C112 129.1(9) . . ? C125 C124 C123 106.2(9) . . ? C125 C124 H124 126.9 . . ? C123 C124 H124 126.9 . . ? N122 C125 C124 105.3(10) . . ? N122 C125 H125 127.3 . . ? C124 C125 H125 127.3 . . ? N122 C126 C256 111.8(8) . 2 ? N122 C126 H12A 109.2 . . ? C256 C126 H12A 109.2 2 . ? N122 C126 H12B 109.2 . . ? C256 C126 H12B 109.2 2 . ? H12A C126 H12B 107.9 . . ? C216 N211 C212 118.6(9) . . ? C216 N211 Pb1 121.9(7) . . ? C212 N211 Pb1 119.2(6) . . ? N211 C212 C213 122.8(9) . . ? N211 C212 C223 114.5(9) . . ? C213 C212 C223 122.7(10) . . ? C212 C213 C214 118.4(11) . . ? C212 C213 H213 120.8 . . ? C214 C213 H213 120.8 . . ? C213 C214 C215 118.1(11) . . ? C213 C214 H214 121.0 . . ? C215 C214 H214 121.0 . . ? C216 C215 C214 120.0(10) . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? N211 C216 C215 121.9(11) . . ? N211 C216 H216 119.0 . . ? C215 C216 H216 119.0 . . ? C223 N221 N222 107.0(8) . . ? C223 N221 Pb1 119.8(6) . . ? N222 N221 Pb1 133.0(6) . . ? C225 N222 N221 109.9(8) . . ? C225 N222 C226 130.0(8) . . ? N221 N222 C226 119.6(8) . . ? N221 C223 C224 109.6(8) . . ? N221 C223 C212 120.1(9) . . ? C224 C223 C212 130.3(10) . . ? C225 C224 C223 104.8(10) . . ? C225 C224 H224 127.6 . . ? C223 C224 H224 127.6 . . ? N222 C225 C224 108.8(9) . . ? N222 C225 H225 125.6 . . ? C224 C225 H225 125.6 . . ? N222 C226 C252 111.4(8) . . ? N222 C226 H17A 109.3 . . ? C252 C226 H17A 109.3 . . ? N222 C226 H17B 109.3 . . ? C252 C226 H17B 109.3 . . ? H17A C226 H17B 108.0 . . ? C252 N251 C256 117.7(8) . . ? N251 C252 C253 123.1(9) . . ? N251 C252 C226 116.3(8) . . ? C253 C252 C226 120.5(9) . . ? C254 C253 C252 118.0(10) . . ? C254 C253 H253 121.0 . . ? C252 C253 H253 121.0 . . ? C253 C254 C255 120.3(11) . . ? C253 C254 H254 119.9 . . ? C255 C254 H254 119.9 . . ? C256 C255 C254 118.0(11) . . ? C256 C255 H255 121.0 . . ? C254 C255 H255 121.0 . . ? N251 C256 C255 122.9(10) . . ? N251 C256 C126 115.2(8) . 2 ? C255 C256 C126 121.9(10) . 2 ? O13X Cl11 O12Y 127.3(8) . . ? O13X Cl11 O15X 109.6(3) . . ? O12Y Cl11 O15X 89.5(7) . . ? O13X Cl11 O15Y 84.6(8) . . ? O12Y Cl11 O15Y 109.6(3) . . ? O15X Cl11 O15Y 25.6(7) . . ? O13X Cl11 O14Y 112.7(10) . . ? O12Y Cl11 O14Y 109.5(3) . . ? O15X Cl11 O14Y 103.2(10) . . ? O15Y Cl11 O14Y 109.5(3) . . ? O13X Cl11 O13Y 26.0(7) . . ? O12Y Cl11 O13Y 109.5(3) . . ? O15X Cl11 O13Y 133.1(9) . . ? O15Y Cl11 O13Y 109.4(3) . . ? O14Y Cl11 O13Y 109.4(3) . . ? O13X Cl11 O12X 109.5(3) . . ? O12Y Cl11 O12X 22.1(7) . . ? O15X Cl11 O12X 109.5(3) . . ? O15Y Cl11 O12X 125.3(9) . . ? O14Y Cl11 O12X 112.2(9) . . ? O13Y Cl11 O12X 88.5(8) . . ? O13X Cl11 O14X 109.5(3) . . ? O12Y Cl11 O14X 109.1(10) . . ? O15X Cl11 O14X 109.5(3) . . ? O15Y Cl11 O14X 114.9(11) . . ? O14Y Cl11 O14X 6.2(10) . . ? O13Y Cl11 O14X 104.1(9) . . ? O12X Cl11 O14X 109.4(3) . . ? Cl11 O14X Pb1 128.0(6) . . ? O22 Cl21 O23 110.6(5) . . ? O22 Cl21 O24 110.2(4) . . ? O23 Cl21 O24 109.4(4) . . ? O22 Cl21 O25 110.1(5) . . ? O23 Cl21 O25 109.9(6) . . ? O24 Cl21 O25 106.6(4) . . ? O11V N13V O12V 125.0(3) . . ? O11V N13V C14V 117.1(2) . . ? O12V N13V C14V 117.5(2) . . ? N13V C14V H14A 109.5 . . ? N13V C14V H14B 109.5 . . ? H14A C14V H14B 109.5 . . ? N13V C14V H14C 109.5 . . ? H14A C14V H14C 109.5 . . ? H14B C14V H14C 109.5 . . ? O11W N13W O12W 125.2(3) . . ? O11W N13W C14W 117.1(2) . . ? O12W N13W C14W 117.5(2) . . ? N13W C14W H14D 109.5 . . ? N13W C14W H14E 109.5 . . ? H14D C14W H14E 109.5 . . ? N13W C14W H14F 109.5 . . ? H14D C14W H14F 109.5 . . ? H14E C14W H14F 109.5 . . ? O21X N23X O22X 125.2(2) . . ? O21X N23X C24X 117.2(2) . . ? O22X N23X C24X 117.6(2) . . ? N23X C24X H24A 109.5 . . ? N23X C24X H24B 109.5 . . ? H24A C24X H24B 109.5 . . ? N23X C24X H24C 109.5 . . ? H24A C24X H24C 109.5 . . ? H24B C24X H24C 109.5 . . ? O21Y N23Y O22Y 125.0(3) . . ? O21Y N23Y C24Y 117.1(3) . . ? O22Y N23Y C24Y 117.5(3) . . ? N23Y C24Y H24D 109.5 . . ? N23Y C24Y H24E 109.5 . . ? H24D C24Y H24E 109.5 . . ? N23Y C24Y H24F 109.5 . . ? H24D C24Y H24F 109.5 . . ? H24E C24Y H24F 109.5 . . ? O31X N33X O32X 125.0(3) . . ? O31X N33X C34X 117.0(3) . . ? O32X N33X C34X 117.5(3) . . ? N33X C34X H34A 109.5 . . ? N33X C34X H34B 109.5 . . ? H34A C34X H34B 109.5 . . ? N33X C34X H34C 109.5 . . ? H34A C34X H34C 109.5 . . ? H34B C34X H34C 109.5 . . ? N33Y O31Y O32Y 97(2) . 2_566 ? N33Y O32Y O31Y 138(2) . 2_566 ? N33Y O32Y N33Y 97.1(15) . 2_566 ? O31Y O32Y N33Y 41.0(13) 2_566 2_566 ? O31Y N33Y O32Y 125.1(3) . . ? O31Y N33Y C34Y 117.1(2) . . ? O32Y N33Y C34Y 117.6(2) . . ? O31Y N33Y O32Y 42.1(15) . 2_566 ? O32Y N33Y O32Y 82.9(15) . 2_566 ? C34Y N33Y O32Y 158.7(16) . 2_566 ? N33Y C34Y H34D 109.5 . . ? N33Y C34Y H34E 109.5 . . ? H34D C34Y H34E 109.5 . . ? N33Y C34Y H34F 109.5 . . ? H34D C34Y H34F 109.5 . . ? H34E C34Y H34F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N221 Pb1 N111 C116 74.6(8) . . . . ? N211 Pb1 N111 C116 7.2(7) . . . . ? N121 Pb1 N111 C116 177.1(8) . . . . ? O14X Pb1 N111 C116 -77.1(8) . . . . ? N221 Pb1 N111 C112 -105.0(7) . . . . ? N211 Pb1 N111 C112 -172.4(7) . . . . ? N121 Pb1 N111 C112 -2.5(7) . . . . ? O14X Pb1 N111 C112 103.3(8) . . . . ? C116 N111 C112 C113 -0.9(14) . . . . ? Pb1 N111 C112 C113 178.7(7) . . . . ? C116 N111 C112 C123 177.6(9) . . . . ? Pb1 N111 C112 C123 -2.8(12) . . . . ? N111 C112 C113 C114 -1.8(16) . . . . ? C123 C112 C113 C114 179.7(10) . . . . ? C112 C113 C114 C115 2.4(16) . . . . ? C113 C114 C115 C116 -0.4(17) . . . . ? C112 N111 C116 C115 3.0(15) . . . . ? Pb1 N111 C116 C115 -176.6(8) . . . . ? C114 C115 C116 N111 -2.4(18) . . . . ? N221 Pb1 N121 C123 80.3(7) . . . . ? N211 Pb1 N121 C123 25.1(9) . . . . ? N111 Pb1 N121 C123 8.1(6) . . . . ? O14X Pb1 N121 C123 -56.9(7) . . . . ? N221 Pb1 N121 N122 -118.7(8) . . . . ? N211 Pb1 N121 N122 -173.9(7) . . . . ? N111 Pb1 N121 N122 169.1(9) . . . . ? O14X Pb1 N121 N122 104.1(9) . . . . ? C123 N121 N122 C125 0.5(11) . . . . ? Pb1 N121 N122 C125 -161.8(7) . . . . ? C123 N121 N122 C126 174.1(8) . . . . ? Pb1 N121 N122 C126 11.8(13) . . . . ? N122 N121 C123 C124 0.6(11) . . . . ? Pb1 N121 C123 C124 167.3(7) . . . . ? N122 N121 C123 C112 -179.8(8) . . . . ? Pb1 N121 C123 C112 -13.1(11) . . . . ? N111 C112 C123 N121 11.2(14) . . . . ? C113 C112 C123 N121 -170.3(9) . . . . ? N111 C112 C123 C124 -169.4(11) . . . . ? C113 C112 C123 C124 9.1(17) . . . . ? N121 C123 C124 C125 -1.5(13) . . . . ? C112 C123 C124 C125 179.0(10) . . . . ? N121 N122 C125 C124 -1.4(13) . . . . ? C126 N122 C125 C124 -174.6(10) . . . . ? C123 C124 C125 N122 1.7(13) . . . . ? N121 N122 C126 C256 -81.7(11) . . . 2 ? C125 N122 C126 C256 90.9(12) . . . 2 ? N221 Pb1 N211 C216 179.1(8) . . . . ? N111 Pb1 N211 C216 -102.0(7) . . . . ? N121 Pb1 N211 C216 -117.4(7) . . . . ? O14X Pb1 N211 C216 -31.2(7) . . . . ? N221 Pb1 N211 C212 4.7(6) . . . . ? N111 Pb1 N211 C212 83.6(7) . . . . ? N121 Pb1 N211 C212 68.2(8) . . . . ? O14X Pb1 N211 C212 154.4(7) . . . . ? C216 N211 C212 C213 2.3(14) . . . . ? Pb1 N211 C212 C213 176.8(8) . . . . ? C216 N211 C212 C223 -178.9(8) . . . . ? Pb1 N211 C212 C223 -4.3(10) . . . . ? N211 C212 C213 C214 -1.5(17) . . . . ? C223 C212 C213 C214 179.7(10) . . . . ? C212 C213 C214 C215 1.3(18) . . . . ? C213 C214 C215 C216 -1.9(18) . . . . ? C212 N211 C216 C215 -2.9(15) . . . . ? Pb1 N211 C216 C215 -177.3(8) . . . . ? C214 C215 C216 N211 2.8(17) . . . . ? N211 Pb1 N221 C223 -4.7(7) . . . . ? N111 Pb1 N221 C223 -91.2(7) . . . . ? N121 Pb1 N221 C223 -152.5(7) . . . . ? O14X Pb1 N221 C223 -51.0(9) . . . . ? N211 Pb1 N221 N222 -178.7(8) . . . . ? N111 Pb1 N221 N222 94.8(8) . . . . ? N121 Pb1 N221 N222 33.5(8) . . . . ? O14X Pb1 N221 N222 135.0(8) . . . . ? C223 N221 N222 C225 -1.0(11) . . . . ? Pb1 N221 N222 C225 173.5(7) . . . . ? C223 N221 N222 C226 -174.1(8) . . . . ? Pb1 N221 N222 C226 0.5(13) . . . . ? N222 N221 C223 C224 0.6(11) . . . . ? Pb1 N221 C223 C224 -174.8(6) . . . . ? N222 N221 C223 C212 180.0(8) . . . . ? Pb1 N221 C223 C212 4.6(11) . . . . ? N211 C212 C223 N221 -0.1(13) . . . . ? C213 C212 C223 N221 178.8(10) . . . . ? N211 C212 C223 C224 179.1(10) . . . . ? C213 C212 C223 C224 -2.0(16) . . . . ? N221 C223 C224 C225 0.0(11) . . . . ? C212 C223 C224 C225 -179.3(10) . . . . ? N221 N222 C225 C224 1.0(12) . . . . ? C226 N222 C225 C224 173.1(9) . . . . ? C223 C224 C225 N222 -0.6(12) . . . . ? C225 N222 C226 C252 -94.7(12) . . . . ? N221 N222 C226 C252 76.8(11) . . . . ? C256 N251 C252 C253 -0.4(15) . . . . ? C256 N251 C252 C226 176.8(9) . . . . ? N222 C226 C252 N251 -75.9(11) . . . . ? N222 C226 C252 C253 101.4(11) . . . . ? N251 C252 C253 C254 0.1(18) . . . . ? C226 C252 C253 C254 -177.0(12) . . . . ? C252 C253 C254 C255 0(2) . . . . ? C253 C254 C255 C256 1(2) . . . . ? C252 N251 C256 C255 0.9(16) . . . . ? C252 N251 C256 C126 179.2(8) . . . 2 ? C254 C255 C256 N251 -1.2(19) . . . . ? C254 C255 C256 C126 -179.3(12) . . . 2 ? O13X Cl11 O14X Pb1 32.9(12) . . . . ? O12Y Cl11 O14X Pb1 -110.5(12) . . . . ? O15X Cl11 O14X Pb1 153.1(9) . . . . ? O15Y Cl11 O14X Pb1 126.0(12) . . . . ? O14Y Cl11 O14X Pb1 155(9) . . . . ? O13Y Cl11 O14X Pb1 6.3(15) . . . . ? O12X Cl11 O14X Pb1 -87.0(10) . . . . ? N221 Pb1 O14X Cl11 146.7(7) . . . . ? N211 Pb1 O14X Cl11 104.8(9) . . . . ? N111 Pb1 O14X Cl11 -171.4(10) . . . . ? N121 Pb1 O14X Cl11 -111.6(9) . . . . ? O32Y O31Y N33Y O32Y 0(5) 2_566 . . . ? O32Y O31Y N33Y C34Y 174(3) 2_566 . . . ? O31Y O32Y N33Y O31Y 0(7) 2_566 . . . ? N33Y O32Y N33Y O31Y 0(3) 2_566 . . . ? O31Y O32Y N33Y C34Y -174(5) 2_566 . . . ? N33Y O32Y N33Y C34Y -174(4) 2_566 . . . ? O31Y O32Y N33Y O32Y 0(4) 2_566 . . 2_566 ? N33Y O32Y N33Y O32Y 0.000(3) 2_566 . . 2_566 ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 4.593 _refine_diff_density_min -1.029 _refine_diff_density_rms 0.215 #===END