# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1254 data_global # 1. SUBMISSION DETAILS _publ_contact_autor ; Prof. Dr. Manfred Weidenbruch Carl von Ossietzky Universitt Oldenburg Fachbereich Chemie Postfach 2503 D-26111 Oldenburg Bundesrepublik Deutschland ; _publ_contact_author_phone '049 441 798-3655' _publ_contact_author_fax '049 441 798-3329' _publ_contact_author_email 'stabenow@hrz2.uni-oldenburg.de' _publ_requested_journal 'Chemical Communications' _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication in " Chemical Communications" as a "New Crystal Structure". ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; A zwitterionic carbene-plumbylene adduct ; loop_ _publ_author_name _publ_author_address 'Weidenbruch, Manfred' ; Carl von Ossietzky Universitt Oldenburg Fachbereich Chemie Postfach 2503 D-26111 Oldenburg Bundesrepublik Deutschland ; 'Stabenow, Frank' ; Carl von Ossietzky Universitt Oldenburg Fachbereich Chemie Postfach 2503 D-26111 Oldenburg Bundesrepublik Deutschland ; 'Saak, Wolfgang' ; Carl von Ossietzky Universitt Oldenburg Fachbereich Chemie Postfach 2503 D-26111 Oldenburg Bundesrepublik Deutschland ; #============================================================================== # 4. TEXT _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; Sheldrick, G. M. (1997) Program SHELXL-97, University of Gttingen. T. Hahn (Ed.), International Tables for Crystallography, Space Group Symmetry, Kluwer Academic Publishers, Dordrecht-Boston-London, 1989, Bd. A ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #============================================================================== data_pbgelb _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H66 N2 Pb' _chemical_formula_weight 794.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' '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 10.5688(7) _cell_length_b 11.0820(6) _cell_length_c 17.9180(8) _cell_angle_alpha 72.784(6) _cell_angle_beta 88.671(7) _cell_angle_gamma 85.959(8) _cell_volume 1999.60(19) _cell_formula_units_Z 2 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description quader _exptl_crystal_colour yellow _exptl_crystal_size_max 0.71 _exptl_crystal_size_mid 0.63 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 4.246 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.1525 _exptl_absorpt_correction_T_max 0.3623 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDS' _diffrn_measurement_method 'imaging plate' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23622 _diffrn_reflns_av_R_equivalents 0.0564 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.00 _reflns_number_total 7260 _reflns_number_gt 6313 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'IPDS (Stoe, 1997)' _computing_cell_refinement 'IPDS (Stoe, 1997)' _computing_data_reduction 'XRED (Stoe, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'SHELX-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7260 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0393 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0733 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.155437(16) 0.118126(13) 0.793842(10) 0.02526(6) Uani 1 1 d . . . N1 N -0.1592(4) 0.2153(3) 0.7981(2) 0.0322(8) Uani 1 1 d . . . N2 N -0.1421(4) 0.1654(3) 0.6908(2) 0.0317(8) Uani 1 1 d . . . C1 C -0.0777(4) 0.1588(3) 0.7571(3) 0.0283(9) Uani 1 1 d . . . C2 C -0.2722(5) 0.2585(4) 0.7574(3) 0.0392(12) Uani 1 1 d . . . C3 C -0.3833(6) 0.3263(5) 0.7843(4) 0.0590(16) Uani 1 1 d . . . H3A H -0.3638 0.3379 0.8349 0.088 Uiso 1 1 calc R . . H3B H -0.4577 0.2762 0.7898 0.088 Uiso 1 1 calc R . . H3C H -0.4013 0.4092 0.7459 0.088 Uiso 1 1 calc R . . C4 C -0.2631(5) 0.2262(4) 0.6910(3) 0.0416(12) Uani 1 1 d . . . C5 C -0.3602(6) 0.2493(5) 0.6282(4) 0.0577(16) Uani 1 1 d . . . H5A H -0.3267 0.2150 0.5867 0.087 Uiso 1 1 calc R . . H5B H -0.3806 0.3406 0.6066 0.087 Uiso 1 1 calc R . . H5C H -0.4371 0.2075 0.6502 0.087 Uiso 1 1 calc R . . C6 C -0.1247(5) 0.2306(4) 0.8742(3) 0.0385(11) Uani 1 1 d . . . H6 H -0.0427 0.1792 0.8896 0.046 Uiso 1 1 calc R . . C7 C -0.0967(7) 0.3673(5) 0.8663(4) 0.0569(16) Uani 1 1 d . . . H7A H -0.0361 0.3965 0.8236 0.085 Uiso 1 1 calc R . . H7B H -0.0605 0.3717 0.9152 0.085 Uiso 1 1 calc R . . H7C H -0.1756 0.4214 0.8550 0.085 Uiso 1 1 calc R . . C8 C -0.2179(6) 0.1761(5) 0.9391(4) 0.0530(14) Uani 1 1 d . . . H8A H -0.2314 0.0886 0.9411 0.080 Uiso 1 1 calc R . . H8B H -0.2989 0.2270 0.9290 0.080 Uiso 1 1 calc R . . H8C H -0.1837 0.1776 0.9892 0.080 Uiso 1 1 calc R . . C9 C -0.0871(5) 0.1107(4) 0.6308(3) 0.0372(11) Uani 1 1 d . . . H9 H 0.0007 0.0761 0.6485 0.045 Uiso 1 1 calc R . . C10 C -0.0737(6) 0.2093(5) 0.5510(3) 0.0514(14) Uani 1 1 d . . . H10A H -0.0259 0.2786 0.5569 0.077 Uiso 1 1 calc R . . H10B H -0.1581 0.2427 0.5301 0.077 Uiso 1 1 calc R . . H10C H -0.0285 0.1696 0.5151 0.077 Uiso 1 1 calc R . . C11 C -0.1597(6) -0.0015(4) 0.6256(3) 0.0472(13) Uani 1 1 d . . . H11A H -0.1656 -0.0623 0.6777 0.071 Uiso 1 1 calc R . . H11B H -0.1147 -0.0427 0.5904 0.071 Uiso 1 1 calc R . . H11C H -0.2452 0.0289 0.6055 0.071 Uiso 1 1 calc R . . C12 C 0.2126(4) 0.1945(3) 0.6599(2) 0.0255(9) Uani 1 1 d . . . C13 C 0.1939(4) 0.3278(3) 0.6264(3) 0.0257(9) Uani 1 1 d . . . C14 C 0.2271(4) 0.3847(3) 0.5485(3) 0.0295(9) Uani 1 1 d . . . H14 H 0.2133 0.4739 0.5273 0.035 Uiso 1 1 calc R . . C15 C 0.2795(4) 0.3154(4) 0.5013(3) 0.0302(9) Uani 1 1 d . . . C16 C 0.2983(5) 0.1844(4) 0.5341(3) 0.0312(10) Uani 1 1 d . . . H16 H 0.3338 0.1350 0.5026 0.037 Uiso 1 1 calc R . . C17 C 0.2667(4) 0.1240(3) 0.6113(3) 0.0285(9) Uani 1 1 d . . . C18 C 0.1384(5) 0.4155(4) 0.6724(3) 0.0329(10) Uani 1 1 d . . . H18 H 0.1253 0.3629 0.7276 0.039 Uiso 1 1 calc R . . C19 C 0.0105(6) 0.4786(5) 0.6404(4) 0.0557(15) Uani 1 1 d . . . H19A H -0.0476 0.4135 0.6403 0.083 Uiso 1 1 calc R . . H19B H 0.0212 0.5335 0.5870 0.083 Uiso 1 1 calc R . . H19C H -0.0246 0.5293 0.6734 0.083 Uiso 1 1 calc R . . C20 C 0.2282(6) 0.5170(5) 0.6737(4) 0.0583(16) Uani 1 1 d . . . H20A H 0.3107 0.4764 0.6944 0.087 Uiso 1 1 calc R . . H20B H 0.1925 0.5667 0.7072 0.087 Uiso 1 1 calc R . . H20C H 0.2390 0.5729 0.6206 0.087 Uiso 1 1 calc R . . C21 C 0.3200(5) 0.3790(4) 0.4183(3) 0.0336(10) Uani 1 1 d . . . H21 H 0.2779 0.4664 0.4024 0.040 Uiso 1 1 calc R . . C22 C 0.2808(5) 0.3127(4) 0.3596(3) 0.0416(11) Uani 1 1 d . . . H22A H 0.3098 0.3590 0.3072 0.062 Uiso 1 1 calc R . . H22B H 0.1882 0.3109 0.3597 0.062 Uiso 1 1 calc R . . H22C H 0.3193 0.2259 0.3742 0.062 Uiso 1 1 calc R . . C23 C 0.4628(5) 0.3918(5) 0.4142(3) 0.0496(14) Uani 1 1 d . . . H23A H 0.4875 0.4336 0.3602 0.074 Uiso 1 1 calc R . . H23B H 0.5070 0.3076 0.4322 0.074 Uiso 1 1 calc R . . H23C H 0.4857 0.4426 0.4477 0.074 Uiso 1 1 calc R . . C24 C 0.2954(5) -0.0191(4) 0.6414(3) 0.0339(10) Uani 1 1 d . . . H24 H 0.2913 -0.0446 0.6998 0.041 Uiso 1 1 calc R . . C25 C 0.4256(8) -0.0605(6) 0.6182(6) 0.093(3) Uani 1 1 d . . . H25A H 0.4896 -0.0167 0.6370 0.140 Uiso 1 1 calc R . . H25B H 0.4308 -0.0394 0.5611 0.140 Uiso 1 1 calc R . . H25C H 0.4409 -0.1521 0.6413 0.140 Uiso 1 1 calc R . . C26 C 0.2002(9) -0.0908(5) 0.6134(6) 0.093(3) Uani 1 1 d . . . H26A H 0.1147 -0.0666 0.6286 0.139 Uiso 1 1 calc R . . H26B H 0.2188 -0.1819 0.6370 0.139 Uiso 1 1 calc R . . H26C H 0.2052 -0.0704 0.5564 0.139 Uiso 1 1 calc R . . C27 C 0.2083(4) -0.1041(3) 0.8301(2) 0.0250(8) Uani 1 1 d . . . C28 C 0.3364(4) -0.1405(4) 0.8484(3) 0.0299(9) Uani 1 1 d . . . C29 C 0.3776(5) -0.2683(4) 0.8820(3) 0.0365(11) Uani 1 1 d . . . H29 H 0.4649 -0.2909 0.8936 0.044 Uiso 1 1 calc R . . C30 C 0.2908(5) -0.3621(4) 0.8982(3) 0.0372(11) Uani 1 1 d . . . C31 C 0.1650(5) -0.3266(4) 0.8812(3) 0.0356(11) Uani 1 1 d . . . H31 H 0.1058 -0.3904 0.8929 0.043 Uiso 1 1 calc R . . C32 C 0.1203(4) -0.2003(4) 0.8473(3) 0.0295(9) Uani 1 1 d . . . C33 C 0.4355(5) -0.0421(4) 0.8359(3) 0.0399(11) Uani 1 1 d . . . H33 H 0.4039 0.0341 0.7932 0.048 Uiso 1 1 calc R . . C34 C 0.4468(7) -0.0019(6) 0.9096(4) 0.0656(19) Uani 1 1 d . . . H34A H 0.5106 0.0608 0.9014 0.098 Uiso 1 1 calc R . . H34B H 0.4725 -0.0760 0.9534 0.098 Uiso 1 1 calc R . . H34C H 0.3647 0.0353 0.9214 0.098 Uiso 1 1 calc R . . C35 C 0.5661(6) -0.0858(6) 0.8114(5) 0.068(2) Uani 1 1 d . . . H35A H 0.6242 -0.0182 0.8045 0.102 Uiso 1 1 calc R . . H35B H 0.5588 -0.1059 0.7620 0.102 Uiso 1 1 calc R . . H35C H 0.5991 -0.1614 0.8518 0.102 Uiso 1 1 calc R . . C36 C 0.3392(5) -0.5004(4) 0.9354(4) 0.0476(13) Uani 1 1 d . . . H36 H 0.4328 -0.5032 0.9436 0.057 Uiso 1 1 calc R . . C37 C 0.2795(10) -0.5579(6) 1.0103(5) 0.107(4) Uani 1 1 d . . . H37A H 0.3138 -0.6457 1.0315 0.161 Uiso 1 1 calc R . . H37B H 0.1877 -0.5564 1.0032 0.161 Uiso 1 1 calc R . . H37C H 0.2968 -0.5102 1.0467 0.161 Uiso 1 1 calc R . . C38 C 0.3139(11) -0.5844(7) 0.8827(6) 0.109(4) Uani 1 1 d . . . H38A H 0.3520 -0.5489 0.8311 0.163 Uiso 1 1 calc R . . H38B H 0.2222 -0.5872 0.8770 0.163 Uiso 1 1 calc R . . H38C H 0.3514 -0.6704 0.9065 0.163 Uiso 1 1 calc R . . C39 C -0.0201(4) -0.1667(4) 0.8344(3) 0.0334(10) Uani 1 1 d . . . H39 H -0.0298 -0.0858 0.7909 0.040 Uiso 1 1 calc R . . C40 C -0.0801(5) -0.1420(5) 0.9069(4) 0.0487(13) Uani 1 1 d . . . H40A H -0.1712 -0.1202 0.8981 0.073 Uiso 1 1 calc R . . H40B H -0.0404 -0.0716 0.9176 0.073 Uiso 1 1 calc R . . H40C H -0.0675 -0.2181 0.9516 0.073 Uiso 1 1 calc R . . C41 C -0.0892(5) -0.2660(4) 0.8101(3) 0.0447(13) Uani 1 1 d . . . H41A H -0.1794 -0.2386 0.8022 0.067 Uiso 1 1 calc R . . H41B H -0.0799 -0.3473 0.8511 0.067 Uiso 1 1 calc R . . H41C H -0.0525 -0.2756 0.7613 0.067 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 0.02699(9) 0.02318(8) 0.02541(10) -0.00607(5) 0.00043(5) -0.00525(5) N1 0.031(2) 0.0262(16) 0.037(2) -0.0053(14) 0.0062(16) -0.0033(14) N2 0.030(2) 0.0253(15) 0.036(2) -0.0024(14) -0.0063(16) -0.0045(14) C1 0.035(2) 0.0214(17) 0.027(2) -0.0046(14) 0.0008(18) -0.0047(16) C2 0.033(3) 0.028(2) 0.051(3) -0.0036(19) 0.003(2) -0.0006(18) C3 0.035(3) 0.057(3) 0.074(5) -0.008(3) 0.008(3) 0.014(3) C4 0.038(3) 0.032(2) 0.048(3) 0.0009(19) -0.007(2) -0.0075(19) C5 0.049(4) 0.050(3) 0.070(4) -0.011(3) -0.024(3) 0.000(3) C6 0.042(3) 0.037(2) 0.039(3) -0.0166(19) 0.009(2) -0.005(2) C7 0.073(4) 0.046(3) 0.061(4) -0.027(3) 0.015(3) -0.018(3) C8 0.057(4) 0.058(3) 0.045(4) -0.017(2) 0.015(3) -0.007(3) C9 0.050(3) 0.032(2) 0.033(3) -0.0122(17) -0.004(2) -0.010(2) C10 0.066(4) 0.054(3) 0.032(3) -0.005(2) -0.006(3) -0.021(3) C11 0.065(4) 0.038(2) 0.042(3) -0.012(2) -0.009(3) -0.016(2) C12 0.029(2) 0.0185(16) 0.028(2) -0.0059(14) 0.0011(17) -0.0019(15) C13 0.024(2) 0.0197(16) 0.033(3) -0.0080(15) 0.0042(17) -0.0024(15) C14 0.031(2) 0.0187(16) 0.035(3) -0.0036(15) 0.0032(18) -0.0003(16) C15 0.031(2) 0.0258(18) 0.031(3) -0.0030(16) 0.0031(18) -0.0023(16) C16 0.038(3) 0.0227(18) 0.032(3) -0.0076(16) 0.0026(19) 0.0030(17) C17 0.032(2) 0.0212(17) 0.031(3) -0.0054(15) 0.0009(18) -0.0009(16) C18 0.040(3) 0.0235(18) 0.033(3) -0.0059(16) 0.006(2) -0.0021(17) C19 0.047(3) 0.052(3) 0.072(4) -0.029(3) 0.004(3) 0.016(3) C20 0.059(4) 0.058(3) 0.072(5) -0.041(3) 0.013(3) -0.012(3) C21 0.041(3) 0.0251(18) 0.033(3) -0.0057(16) 0.005(2) -0.0024(17) C22 0.049(3) 0.039(2) 0.035(3) -0.0079(19) -0.001(2) -0.002(2) C23 0.047(3) 0.048(3) 0.051(4) -0.008(2) 0.015(3) -0.019(2) C24 0.051(3) 0.0216(18) 0.027(3) -0.0065(15) 0.005(2) 0.0039(18) C25 0.070(5) 0.037(3) 0.145(8) 0.007(4) 0.029(5) 0.026(3) C26 0.107(7) 0.026(2) 0.148(8) -0.028(3) -0.049(6) 0.001(3) C27 0.023(2) 0.0241(17) 0.025(2) -0.0011(14) -0.0012(16) -0.0051(15) C28 0.023(2) 0.036(2) 0.026(2) -0.0013(16) 0.0005(17) -0.0034(17) C29 0.029(2) 0.034(2) 0.038(3) 0.0004(18) -0.002(2) 0.0015(18) C30 0.037(3) 0.032(2) 0.038(3) -0.0033(18) 0.001(2) 0.0000(19) C31 0.039(3) 0.0229(18) 0.041(3) -0.0032(17) 0.002(2) -0.0077(18) C32 0.031(2) 0.0279(18) 0.030(3) -0.0064(16) 0.0010(18) -0.0087(17) C33 0.029(3) 0.042(2) 0.039(3) 0.0035(19) -0.001(2) -0.010(2) C34 0.066(4) 0.077(4) 0.050(4) -0.005(3) -0.016(3) -0.043(3) C35 0.030(3) 0.052(3) 0.102(6) 0.008(3) 0.013(3) -0.005(2) C36 0.037(3) 0.033(2) 0.063(4) 0.000(2) -0.003(2) 0.006(2) C37 0.118(8) 0.052(4) 0.107(7) 0.031(4) 0.055(6) 0.038(4) C38 0.141(9) 0.067(4) 0.124(8) -0.047(5) -0.025(7) 0.045(5) C39 0.028(2) 0.0245(18) 0.042(3) -0.0009(17) -0.0047(19) -0.0073(17) C40 0.027(3) 0.053(3) 0.068(4) -0.023(3) 0.001(2) 0.000(2) C41 0.038(3) 0.033(2) 0.060(4) -0.007(2) -0.008(2) -0.013(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 C12 2.376(4) . ? Pb1 C27 2.383(4) . ? Pb1 C1 2.540(5) . ? N1 C1 1.357(6) . ? N1 C2 1.393(7) . ? N1 C6 1.480(7) . ? N2 C1 1.363(6) . ? N2 C4 1.403(7) . ? N2 C9 1.473(6) . ? C2 C4 1.340(8) . ? C2 C3 1.497(8) . ? C4 C5 1.494(8) . ? C6 C8 1.518(7) . ? C6 C7 1.529(6) . ? C9 C10 1.531(7) . ? C9 C11 1.533(6) . ? C12 C17 1.419(6) . ? C12 C13 1.421(5) . ? C13 C14 1.400(6) . ? C13 C18 1.530(6) . ? C14 C15 1.383(6) . ? C15 C16 1.397(5) . ? C15 C21 1.511(6) . ? C16 C17 1.392(6) . ? C17 C24 1.527(5) . ? C18 C19 1.519(8) . ? C18 C20 1.527(7) . ? C21 C23 1.524(7) . ? C21 C22 1.529(7) . ? C24 C26 1.505(8) . ? C24 C25 1.508(8) . ? C27 C28 1.403(6) . ? C27 C32 1.423(5) . ? C28 C29 1.406(6) . ? C28 C33 1.530(6) . ? C29 C30 1.397(6) . ? C30 C31 1.374(7) . ? C30 C36 1.535(6) . ? C31 C32 1.404(6) . ? C32 C39 1.510(6) . ? C33 C34 1.523(9) . ? C33 C35 1.529(8) . ? C36 C37 1.455(9) . ? C36 C38 1.549(10) . ? C39 C40 1.520(8) . ? C39 C41 1.532(6) . ? 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 C12 Pb1 C27 105.25(14) . . ? C12 Pb1 C1 90.11(14) . . ? C27 Pb1 C1 108.78(13) . . ? C1 N1 C2 110.9(4) . . ? C1 N1 C6 122.1(4) . . ? C2 N1 C6 126.9(4) . . ? C1 N2 C4 110.7(4) . . ? C1 N2 C9 121.9(4) . . ? C4 N2 C9 127.4(4) . . ? N1 C1 N2 104.6(4) . . ? N1 C1 Pb1 120.2(3) . . ? N2 C1 Pb1 133.0(3) . . ? C4 C2 N1 107.3(5) . . ? C4 C2 C3 126.9(5) . . ? N1 C2 C3 125.8(5) . . ? C2 C4 N2 106.5(4) . . ? C2 C4 C5 127.9(5) . . ? N2 C4 C5 125.6(5) . . ? N1 C6 C8 113.4(4) . . ? N1 C6 C7 111.4(4) . . ? C8 C6 C7 113.7(4) . . ? N2 C9 C10 113.1(4) . . ? N2 C9 C11 111.3(4) . . ? C10 C9 C11 112.1(4) . . ? C17 C12 C13 117.2(4) . . ? C17 C12 Pb1 127.8(3) . . ? C13 C12 Pb1 115.0(3) . . ? C14 C13 C12 120.4(4) . . ? C14 C13 C18 116.8(3) . . ? C12 C13 C18 122.7(4) . . ? C15 C14 C13 122.1(3) . . ? C14 C15 C16 117.6(4) . . ? C14 C15 C21 121.4(3) . . ? C16 C15 C21 120.9(4) . . ? C17 C16 C15 122.1(4) . . ? C16 C17 C12 120.6(3) . . ? C16 C17 C24 117.4(4) . . ? C12 C17 C24 122.0(4) . . ? C19 C18 C20 109.4(4) . . ? C19 C18 C13 111.9(4) . . ? C20 C18 C13 111.9(4) . . ? C15 C21 C23 110.4(4) . . ? C15 C21 C22 113.9(4) . . ? C23 C21 C22 110.0(4) . . ? C26 C24 C25 107.8(6) . . ? C26 C24 C17 112.3(4) . . ? C25 C24 C17 112.8(4) . . ? C28 C27 C32 118.1(4) . . ? C28 C27 Pb1 115.1(3) . . ? C32 C27 Pb1 125.8(3) . . ? C27 C28 C29 121.2(4) . . ? C27 C28 C33 121.2(4) . . ? C29 C28 C33 117.5(4) . . ? C30 C29 C28 120.3(4) . . ? C31 C30 C29 118.6(4) . . ? C31 C30 C36 122.6(4) . . ? C29 C30 C36 118.7(4) . . ? C30 C31 C32 122.8(4) . . ? C31 C32 C27 119.0(4) . . ? C31 C32 C39 120.1(4) . . ? C27 C32 C39 120.8(4) . . ? C34 C33 C35 110.0(5) . . ? C34 C33 C28 109.7(4) . . ? C35 C33 C28 114.2(4) . . ? C37 C36 C30 112.8(5) . . ? C37 C36 C38 106.5(7) . . ? C30 C36 C38 111.9(5) . . ? C32 C39 C40 109.9(4) . . ? C32 C39 C41 113.4(4) . . ? C40 C39 C41 111.2(4) . . ? 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 C2 N1 C1 N2 -1.0(4) . . . . ? C6 N1 C1 N2 -178.7(3) . . . . ? C2 N1 C1 Pb1 164.4(3) . . . . ? C6 N1 C1 Pb1 -13.3(5) . . . . ? C4 N2 C1 N1 0.1(4) . . . . ? C9 N2 C1 N1 -178.4(3) . . . . ? C4 N2 C1 Pb1 -162.5(3) . . . . ? C9 N2 C1 Pb1 19.0(5) . . . . ? C12 Pb1 C1 N1 -135.2(3) . . . . ? C27 Pb1 C1 N1 118.6(3) . . . . ? C12 Pb1 C1 N2 25.3(3) . . . . ? C27 Pb1 C1 N2 -80.9(4) . . . . ? C1 N1 C2 C4 1.5(5) . . . . ? C6 N1 C2 C4 179.1(4) . . . . ? C1 N1 C2 C3 -179.5(4) . . . . ? C6 N1 C2 C3 -1.9(7) . . . . ? N1 C2 C4 N2 -1.3(5) . . . . ? C3 C2 C4 N2 179.7(4) . . . . ? N1 C2 C4 C5 178.9(4) . . . . ? C3 C2 C4 C5 0.0(8) . . . . ? C1 N2 C4 C2 0.8(5) . . . . ? C9 N2 C4 C2 179.2(4) . . . . ? C1 N2 C4 C5 -179.5(4) . . . . ? C9 N2 C4 C5 -1.1(7) . . . . ? C1 N1 C6 C8 -125.4(5) . . . . ? C2 N1 C6 C8 57.2(6) . . . . ? C1 N1 C6 C7 104.8(5) . . . . ? C2 N1 C6 C7 -72.5(6) . . . . ? C1 N2 C9 C10 -119.4(5) . . . . ? C4 N2 C9 C10 62.3(6) . . . . ? C1 N2 C9 C11 113.3(5) . . . . ? C4 N2 C9 C11 -64.9(5) . . . . ? C27 Pb1 C12 C17 0.0(4) . . . . ? C1 Pb1 C12 C17 -109.6(4) . . . . ? C27 Pb1 C12 C13 -177.5(3) . . . . ? C1 Pb1 C12 C13 73.0(3) . . . . ? C17 C12 C13 C14 0.6(6) . . . . ? Pb1 C12 C13 C14 178.3(3) . . . . ? C17 C12 C13 C18 -179.1(4) . . . . ? Pb1 C12 C13 C18 -1.4(5) . . . . ? C12 C13 C14 C15 -0.4(7) . . . . ? C18 C13 C14 C15 179.3(4) . . . . ? C13 C14 C15 C16 0.2(7) . . . . ? C13 C14 C15 C21 -177.4(4) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C21 C15 C16 C17 177.4(4) . . . . ? C15 C16 C17 C12 0.5(7) . . . . ? C15 C16 C17 C24 -178.1(4) . . . . ? C13 C12 C17 C16 -0.6(6) . . . . ? Pb1 C12 C17 C16 -178.0(3) . . . . ? C13 C12 C17 C24 177.9(4) . . . . ? Pb1 C12 C17 C24 0.6(6) . . . . ? C14 C13 C18 C19 65.7(5) . . . . ? C12 C13 C18 C19 -114.6(5) . . . . ? C14 C13 C18 C20 -57.5(6) . . . . ? C12 C13 C18 C20 122.1(5) . . . . ? C14 C15 C21 C23 99.5(5) . . . . ? C16 C15 C21 C23 -78.0(5) . . . . ? C14 C15 C21 C22 -136.1(5) . . . . ? C16 C15 C21 C22 46.4(6) . . . . ? C16 C17 C24 C26 -77.2(7) . . . . ? C12 C17 C24 C26 104.2(6) . . . . ? C16 C17 C24 C25 44.9(7) . . . . ? C12 C17 C24 C25 -133.7(6) . . . . ? C12 Pb1 C27 C28 81.7(3) . . . . ? C1 Pb1 C27 C28 177.1(3) . . . . ? C12 Pb1 C27 C32 -109.8(4) . . . . ? C1 Pb1 C27 C32 -14.3(4) . . . . ? C32 C27 C28 C29 0.8(7) . . . . ? Pb1 C27 C28 C29 170.3(4) . . . . ? C32 C27 C28 C33 -176.6(4) . . . . ? Pb1 C27 C28 C33 -7.1(6) . . . . ? C27 C28 C29 C30 -0.4(7) . . . . ? C33 C28 C29 C30 177.0(5) . . . . ? C28 C29 C30 C31 -0.4(8) . . . . ? C28 C29 C30 C36 -179.5(5) . . . . ? C29 C30 C31 C32 0.8(8) . . . . ? C36 C30 C31 C32 179.9(5) . . . . ? C30 C31 C32 C27 -0.4(7) . . . . ? C30 C31 C32 C39 -176.5(5) . . . . ? C28 C27 C32 C31 -0.4(7) . . . . ? Pb1 C27 C32 C31 -168.7(3) . . . . ? C28 C27 C32 C39 175.6(4) . . . . ? Pb1 C27 C32 C39 7.4(6) . . . . ? C27 C28 C33 C34 90.4(6) . . . . ? C29 C28 C33 C34 -87.1(6) . . . . ? C27 C28 C33 C35 -145.6(5) . . . . ? C29 C28 C33 C35 36.9(7) . . . . ? C31 C30 C36 C37 -58.4(9) . . . . ? C29 C30 C36 C37 120.8(7) . . . . ? C31 C30 C36 C38 61.6(8) . . . . ? C29 C30 C36 C38 -119.2(7) . . . . ? C31 C32 C39 C40 88.1(5) . . . . ? C27 C32 C39 C40 -87.8(5) . . . . ? C31 C32 C39 C41 -37.0(6) . . . . ? C27 C32 C39 C41 147.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 1.283 _refine_diff_density_min -1.292 _refine_diff_density_rms 0.109