# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name G.Robinson 'Brandon Quillian' 'Yuzhong Wang.' 'Pingrong Wei.' 'Xiao-Juan Yang.' _publ_contact_author_name 'G. Robinson' _publ_contact_author_address ; Department of Chemistry University of Georgia Athens GA 30602 UNITED STATES OF AMERICA ; _publ_contact_author_email ROBINSON@CHEM.UGA.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; Syntheses and structures of new diaryl lead(II) compounds PbR2 (1, R = 2,4,6-triphenylphenyl; 2, R = 2,6-bis(1'-napthyl)phenyl ; data_uga402_compound_2 _database_code_depnum_ccdc_archive 'CCDC 284966' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H34 Pb' _chemical_formula_weight 865.98 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' 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 11.4487(9) _cell_length_b 16.1126(13) _cell_length_c 21.3687(18) _cell_angle_alpha 90.00 _cell_angle_beta 100.3270(10) _cell_angle_gamma 90.00 _cell_volume 3878.0(5) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour orange _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.483 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 4.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2429 _exptl_absorpt_correction_T_max 0.3529 _exptl_absorpt_process_details 'BRUKER SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22876 _diffrn_reflns_av_R_equivalents 0.0217 _diffrn_reflns_av_sigmaI/netI 0.0180 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6716 _reflns_number_gt 5785 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0506P)^2^+0.8361P] 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 6716 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0319 _refine_ls_wR_factor_ref 0.0814 _refine_ls_wR_factor_gt 0.0789 _refine_ls_goodness_of_fit_ref 1.091 _refine_ls_restrained_S_all 1.091 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.717448(13) 0.300514(9) 0.029548(7) 0.06628(8) Uani 1 1 d . . . C1 C 0.7067(4) 0.2046(2) -0.05395(19) 0.0639(9) Uani 1 1 d . . . C2 C 0.8068(4) 0.2107(2) -0.08409(19) 0.0651(9) Uani 1 1 d . . . C3 C 0.8185(4) 0.1627(3) -0.1359(2) 0.0744(10) Uani 1 1 d . . . H3A H 0.8855 0.1676 -0.1546 0.089 Uiso 1 1 calc R . . C4 C 0.7296(4) 0.1069(3) -0.1598(2) 0.0824(12) Uani 1 1 d . . . H4A H 0.7381 0.0731 -0.1940 0.099 Uiso 1 1 calc R . . C5 C 0.6292(4) 0.1013(3) -0.1336(2) 0.0743(10) Uani 1 1 d . . . H5A H 0.5693 0.0645 -0.1506 0.089 Uiso 1 1 calc R . . C6 C 0.6158(3) 0.1508(2) -0.08100(18) 0.0667(9) Uani 1 1 d . . . C7 C 0.9028(4) 0.2706(3) -0.0569(2) 0.0716(10) Uani 1 1 d . . . C8 C 0.9674(4) 0.2570(3) 0.0019(2) 0.0809(12) Uani 1 1 d . . . H8A H 0.9527 0.2096 0.0241 0.097 Uiso 1 1 calc R . . C9 C 1.0554(5) 0.3122(4) 0.0302(3) 0.1006(17) Uani 1 1 d . . . H9A H 1.0982 0.3015 0.0706 0.121 Uiso 1 1 calc R . . C10 C 1.0782(5) 0.3821(4) -0.0019(3) 0.1082(18) Uani 1 1 d . . . H10A H 1.1371 0.4187 0.0168 0.130 Uiso 1 1 calc R . . C11 C 1.0132(5) 0.3995(3) -0.0633(3) 0.0924(14) Uani 1 1 d . . . C12 C 1.0349(7) 0.4719(4) -0.0968(4) 0.121(2) Uani 1 1 d . . . H12A H 1.0947 0.5084 -0.0790 0.145 Uiso 1 1 calc R . . C13 C 0.9693(9) 0.4882(4) -0.1544(5) 0.142(3) Uani 1 1 d . . . H13A H 0.9839 0.5363 -0.1758 0.171 Uiso 1 1 calc R . . C14 C 0.8790(7) 0.4336(4) -0.1825(3) 0.121(2) Uani 1 1 d . . . H14A H 0.8347 0.4458 -0.2223 0.145 Uiso 1 1 calc R . . C15 C 0.8561(5) 0.3633(3) -0.1520(2) 0.0870(13) Uani 1 1 d . . . H15A H 0.7961 0.3275 -0.1705 0.104 Uiso 1 1 calc R . . C16 C 0.9245(4) 0.3450(3) -0.0917(2) 0.0752(10) Uani 1 1 d . . . C17 C 0.5015(3) 0.1448(2) -0.05632(18) 0.0646(9) Uani 1 1 d . . . C18 C 0.4951(4) 0.1035(2) -0.0016(2) 0.0723(10) Uani 1 1 d . . . H18A H 0.5628 0.0778 0.0206 0.087 Uiso 1 1 calc R . . C19 C 0.3886(4) 0.0988(3) 0.0224(2) 0.0794(11) Uani 1 1 d . . . H19A H 0.3866 0.0701 0.0600 0.095 Uiso 1 1 calc R . . C20 C 0.2885(4) 0.1361(3) -0.0091(2) 0.0770(11) Uani 1 1 d . . . H20A H 0.2187 0.1336 0.0073 0.092 Uiso 1 1 calc R . . C21 C 0.2902(4) 0.1786(3) -0.0667(2) 0.0740(10) Uani 1 1 d . . . C22 C 0.1866(4) 0.2199(4) -0.1007(2) 0.0929(14) Uani 1 1 d . . . H22A H 0.1157 0.2167 -0.0854 0.112 Uiso 1 1 calc R . . C23 C 0.1902(5) 0.2619(5) -0.1528(2) 0.1109(19) Uani 1 1 d . . . H23A H 0.1212 0.2862 -0.1748 0.133 Uiso 1 1 calc R . . C24 C 0.2980(5) 0.2708(5) -0.1760(3) 0.114(2) Uani 1 1 d . . . H24A H 0.3002 0.3031 -0.2118 0.137 Uiso 1 1 calc R . . C25 C 0.3982(4) 0.2324(4) -0.1461(2) 0.0877(13) Uani 1 1 d . . . H25A H 0.4681 0.2377 -0.1621 0.105 Uiso 1 1 calc R . . C26 C 0.3974(4) 0.1843(2) -0.09069(19) 0.0673(9) Uani 1 1 d . . . C27 C 0.6711(4) 0.2153(2) 0.10922(19) 0.0663(9) Uani 1 1 d . . . C28 C 0.7301(3) 0.1439(3) 0.13614(18) 0.0672(9) Uani 1 1 d . . . C29 C 0.6808(4) 0.0964(3) 0.1793(2) 0.0795(11) Uani 1 1 d . . . H29A H 0.7182 0.0478 0.1956 0.095 Uiso 1 1 calc R . . C30 C 0.5768(4) 0.1211(3) 0.1983(2) 0.0861(13) Uani 1 1 d . . . H30A H 0.5440 0.0883 0.2266 0.103 Uiso 1 1 calc R . . C31 C 0.5225(4) 0.1925(3) 0.1761(2) 0.0807(12) Uani 1 1 d . . . H31A H 0.4547 0.2100 0.1906 0.097 Uiso 1 1 calc R . . C32 C 0.5686(3) 0.2409(3) 0.13064(18) 0.0674(9) Uani 1 1 d . . . C33 C 0.8456(4) 0.1158(2) 0.12113(18) 0.0665(9) Uani 1 1 d . . . C34 C 0.8511(4) 0.0443(3) 0.0862(2) 0.0796(11) Uani 1 1 d . . . H34A H 0.7816 0.0162 0.0695 0.095 Uiso 1 1 calc R . . C35 C 0.9617(5) 0.0134(3) 0.0755(2) 0.0899(13) Uani 1 1 d . . . H35A H 0.9635 -0.0352 0.0521 0.108 Uiso 1 1 calc R . . C36 C 1.0636(4) 0.0523(3) 0.0983(2) 0.0830(12) Uani 1 1 d . . . H36A H 1.1348 0.0309 0.0901 0.100 Uiso 1 1 calc R . . C37 C 1.0643(4) 0.1259(3) 0.13472(19) 0.0754(11) Uani 1 1 d . . . C38 C 1.1696(5) 0.1672(4) 0.1612(2) 0.0937(14) Uani 1 1 d . . . H38A H 1.2417 0.1469 0.1535 0.112 Uiso 1 1 calc R . . C39 C 1.1688(5) 0.2357(4) 0.1976(3) 0.0980(15) Uani 1 1 d . . . H39A H 1.2398 0.2613 0.2153 0.118 Uiso 1 1 calc R . . C40 C 1.0618(5) 0.2677(4) 0.2085(2) 0.0918(13) Uani 1 1 d . . . H40A H 1.0622 0.3150 0.2335 0.110 Uiso 1 1 calc R . . C41 C 0.9561(4) 0.2316(3) 0.18347(19) 0.0738(10) Uani 1 1 d . . . H41A H 0.8855 0.2549 0.1909 0.089 Uiso 1 1 calc R . . C42 C 0.9534(4) 0.1581(3) 0.14585(18) 0.0677(9) Uani 1 1 d . . . C43 C 0.5065(4) 0.3178(3) 0.1027(2) 0.0687(10) Uani 1 1 d . . . C44 C 0.4612(4) 0.3196(3) 0.0389(2) 0.0736(10) Uani 1 1 d . . . H44A H 0.4677 0.2724 0.0148 0.088 Uiso 1 1 calc R . . C45 C 0.4051(4) 0.3902(3) 0.0086(2) 0.0845(12) Uani 1 1 d . . . H45A H 0.3758 0.3893 -0.0349 0.101 Uiso 1 1 calc R . . C46 C 0.3938(4) 0.4592(3) 0.0427(3) 0.0921(13) Uani 1 1 d . . . H46A H 0.3569 0.5059 0.0224 0.111 Uiso 1 1 calc R . . C47 C 0.4369(4) 0.4614(3) 0.1082(3) 0.0897(13) Uani 1 1 d . . . C48 C 0.4270(6) 0.5330(4) 0.1455(4) 0.124(2) Uani 1 1 d . . . H48A H 0.3920 0.5802 0.1252 0.149 Uiso 1 1 calc R . . C49 C 0.4645(8) 0.5359(5) 0.2066(4) 0.143(3) Uani 1 1 d . . . H49A H 0.4533 0.5839 0.2289 0.171 Uiso 1 1 calc R . . C50 C 0.5208(7) 0.4682(6) 0.2387(3) 0.137(3) Uani 1 1 d . . . H50A H 0.5476 0.4717 0.2824 0.164 Uiso 1 1 calc R . . C51 C 0.5385(5) 0.3934(4) 0.2061(3) 0.1036(16) Uani 1 1 d . . . H51A H 0.5782 0.3485 0.2276 0.124 Uiso 1 1 calc R . . C52 C 0.4935(4) 0.3898(3) 0.1397(2) 0.0809(12) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.06385(11) 0.06564(11) 0.07069(11) -0.00034(6) 0.01567(7) 0.00002(6) C1 0.063(2) 0.065(2) 0.064(2) 0.0092(16) 0.0121(17) 0.0109(17) C2 0.061(2) 0.067(2) 0.068(2) 0.0129(17) 0.0123(17) 0.0078(17) C3 0.066(2) 0.089(3) 0.072(2) 0.004(2) 0.0223(19) 0.016(2) C4 0.086(3) 0.088(3) 0.074(2) -0.007(2) 0.016(2) 0.020(2) C5 0.071(2) 0.074(2) 0.078(2) -0.007(2) 0.0110(19) 0.008(2) C6 0.063(2) 0.068(2) 0.069(2) 0.0052(18) 0.0104(17) 0.0097(18) C7 0.060(2) 0.088(3) 0.071(2) 0.000(2) 0.0224(18) 0.008(2) C8 0.059(2) 0.116(4) 0.067(2) 0.008(2) 0.0109(19) 0.003(2) C9 0.076(3) 0.143(5) 0.082(3) -0.013(3) 0.012(3) -0.002(3) C10 0.081(3) 0.142(5) 0.105(4) -0.039(4) 0.027(3) -0.026(3) C11 0.086(3) 0.091(3) 0.109(4) -0.013(3) 0.041(3) -0.010(3) C12 0.138(6) 0.099(4) 0.140(6) -0.014(4) 0.064(5) -0.022(4) C13 0.199(9) 0.083(4) 0.168(7) 0.016(4) 0.094(7) 0.003(5) C14 0.146(6) 0.114(5) 0.110(4) 0.025(4) 0.042(4) 0.020(4) C15 0.096(3) 0.090(3) 0.077(3) 0.017(2) 0.022(2) 0.014(2) C16 0.067(2) 0.086(3) 0.077(3) 0.000(2) 0.026(2) 0.009(2) C17 0.063(2) 0.063(2) 0.067(2) -0.0064(17) 0.0108(17) -0.0011(17) C18 0.076(2) 0.061(2) 0.078(2) -0.002(2) 0.0086(19) -0.003(2) C19 0.094(3) 0.071(2) 0.076(2) -0.001(2) 0.022(2) -0.014(2) C20 0.070(3) 0.085(3) 0.079(2) -0.012(2) 0.022(2) -0.014(2) C21 0.065(2) 0.092(3) 0.064(2) -0.011(2) 0.0095(18) -0.005(2) C22 0.062(3) 0.137(4) 0.079(3) -0.015(3) 0.012(2) 0.011(3) C23 0.084(3) 0.171(6) 0.076(3) 0.005(3) 0.009(2) 0.046(4) C24 0.104(4) 0.169(5) 0.072(3) 0.022(3) 0.021(3) 0.059(4) C25 0.075(3) 0.116(4) 0.075(3) 0.010(3) 0.021(2) 0.023(3) C26 0.064(2) 0.076(2) 0.062(2) -0.0065(17) 0.0100(17) 0.0013(18) C27 0.061(2) 0.073(2) 0.064(2) -0.0086(17) 0.0096(17) -0.0018(17) C28 0.062(2) 0.076(2) 0.062(2) -0.0022(18) 0.0073(17) -0.0003(18) C29 0.076(3) 0.085(3) 0.076(2) 0.012(2) 0.008(2) -0.004(2) C30 0.075(3) 0.107(4) 0.078(3) 0.012(2) 0.019(2) -0.017(3) C31 0.062(2) 0.105(3) 0.079(3) -0.009(2) 0.021(2) -0.007(2) C32 0.062(2) 0.079(2) 0.060(2) -0.0092(18) 0.0074(16) -0.0035(19) C33 0.067(2) 0.068(2) 0.063(2) 0.0071(17) 0.0075(17) 0.0042(17) C34 0.082(3) 0.077(3) 0.078(3) -0.002(2) 0.010(2) 0.002(2) C35 0.105(4) 0.079(3) 0.087(3) -0.007(2) 0.020(3) 0.015(3) C36 0.077(3) 0.092(3) 0.080(3) 0.014(2) 0.015(2) 0.022(2) C37 0.069(2) 0.090(3) 0.066(2) 0.014(2) 0.0093(19) 0.011(2) C38 0.068(3) 0.128(4) 0.083(3) 0.009(3) 0.006(2) 0.001(3) C39 0.075(3) 0.128(4) 0.086(3) 0.003(3) 0.001(2) -0.018(3) C40 0.093(4) 0.104(3) 0.076(3) -0.007(3) 0.011(2) -0.021(3) C41 0.071(3) 0.086(3) 0.064(2) -0.002(2) 0.0104(19) -0.004(2) C42 0.064(2) 0.077(2) 0.060(2) 0.0073(18) 0.0071(17) -0.0015(19) C43 0.053(2) 0.080(3) 0.073(2) -0.0125(19) 0.0104(17) -0.0020(17) C44 0.065(2) 0.076(2) 0.078(3) -0.010(2) 0.006(2) 0.0058(19) C45 0.072(3) 0.087(3) 0.090(3) -0.005(2) 0.002(2) 0.010(2) C46 0.069(3) 0.087(3) 0.119(4) -0.003(3) 0.014(3) 0.010(2) C47 0.072(3) 0.076(3) 0.123(4) -0.025(3) 0.024(3) 0.005(2) C48 0.124(5) 0.100(4) 0.148(6) -0.040(4) 0.025(4) 0.010(3) C49 0.166(7) 0.115(5) 0.145(7) -0.051(5) 0.020(5) 0.017(5) C50 0.140(6) 0.172(7) 0.096(4) -0.059(5) 0.014(4) -0.012(5) C51 0.100(4) 0.119(4) 0.093(3) -0.039(3) 0.022(3) -0.011(3) C52 0.064(2) 0.097(3) 0.083(3) -0.025(2) 0.016(2) -0.006(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 C27 2.322(4) . ? Pb1 C1 2.347(4) . ? C1 C2 1.415(6) . ? C1 C6 1.398(6) . ? C2 C3 1.376(6) . ? C2 C7 1.499(6) . ? C3 C4 1.385(7) . ? C4 C5 1.369(6) . ? C5 C6 1.408(6) . ? C6 C17 1.500(5) . ? C7 C8 1.358(6) . ? C7 C16 1.456(7) . ? C8 C9 1.398(8) . ? C9 C10 1.369(8) . ? C10 C11 1.416(8) . ? C11 C16 1.396(7) . ? C11 C12 1.413(8) . ? C12 C13 1.348(11) . ? C13 C14 1.408(11) . ? C14 C15 1.356(8) . ? C15 C16 1.413(6) . ? C17 C18 1.359(6) . ? C17 C26 1.432(6) . ? C18 C19 1.407(6) . ? C19 C20 1.360(6) . ? C20 C21 1.411(6) . ? C21 C26 1.416(6) . ? C21 C22 1.437(7) . ? C22 C23 1.310(8) . ? C23 C24 1.417(8) . ? C24 C25 1.358(7) . ? C25 C26 1.416(6) . ? C27 C32 1.396(6) . ? C27 C28 1.404(6) . ? C28 C29 1.394(6) . ? C28 C33 1.487(6) . ? C29 C30 1.383(7) . ? C30 C31 1.354(7) . ? C31 C32 1.418(6) . ? C32 C43 1.499(6) . ? C33 C34 1.381(6) . ? C33 C42 1.426(6) . ? C34 C35 1.416(7) . ? C35 C36 1.337(7) . ? C36 C37 1.418(7) . ? C37 C38 1.404(7) . ? C37 C42 1.431(6) . ? C38 C39 1.350(8) . ? C39 C40 1.387(8) . ? C40 C41 1.363(7) . ? C41 C42 1.429(6) . ? C43 C44 1.369(6) . ? C43 C52 1.426(6) . ? C44 C45 1.406(6) . ? C45 C46 1.348(7) . ? C46 C47 1.400(7) . ? C47 C48 1.419(7) . ? C47 C52 1.431(7) . ? C48 C49 1.299(10) . ? C49 C50 1.385(11) . ? C50 C51 1.425(8) . ? C51 C52 1.422(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C27 Pb1 C1 100.40(13) . . ? C2 C1 C6 117.3(4) . . ? C2 C1 Pb1 111.4(3) . . ? C6 C1 Pb1 131.0(3) . . ? C3 C2 C1 122.1(4) . . ? C3 C2 C7 120.2(4) . . ? C1 C2 C7 117.7(4) . . ? C2 C3 C4 119.4(4) . . ? C5 C4 C3 120.4(4) . . ? C4 C5 C6 120.6(4) . . ? C1 C6 C5 120.1(4) . . ? C1 C6 C17 121.8(3) . . ? C5 C6 C17 118.1(4) . . ? C8 C7 C16 119.5(4) . . ? C8 C7 C2 119.6(4) . . ? C16 C7 C2 120.9(4) . . ? C7 C8 C9 121.9(5) . . ? C10 C9 C8 119.7(5) . . ? C9 C10 C11 120.8(5) . . ? C10 C11 C16 120.0(5) . . ? C10 C11 C12 121.4(6) . . ? C16 C11 C12 118.6(6) . . ? C13 C12 C11 120.2(7) . . ? C12 C13 C14 120.9(6) . . ? C15 C14 C13 120.5(7) . . ? C14 C15 C16 119.3(6) . . ? C11 C16 C15 120.4(5) . . ? C11 C16 C7 118.2(4) . . ? C15 C16 C7 121.3(4) . . ? C18 C17 C26 119.4(4) . . ? C18 C17 C6 121.2(4) . . ? C26 C17 C6 119.3(3) . . ? C17 C18 C19 121.6(4) . . ? C20 C19 C18 120.2(4) . . ? C19 C20 C21 120.3(4) . . ? C20 C21 C26 119.7(4) . . ? C20 C21 C22 121.8(4) . . ? C26 C21 C22 118.5(4) . . ? C23 C22 C21 121.4(5) . . ? C22 C23 C24 120.7(5) . . ? C25 C24 C23 120.3(5) . . ? C24 C25 C26 120.8(5) . . ? C21 C26 C25 118.3(4) . . ? C21 C26 C17 118.8(4) . . ? C25 C26 C17 122.9(4) . . ? C32 C27 C28 118.6(4) . . ? C32 C27 Pb1 112.4(3) . . ? C28 C27 Pb1 129.0(3) . . ? C29 C28 C27 119.9(4) . . ? C29 C28 C33 117.2(4) . . ? C27 C28 C33 122.9(4) . . ? C30 C29 C28 120.6(4) . . ? C31 C30 C29 120.4(4) . . ? C30 C31 C32 120.2(4) . . ? C27 C32 C31 120.0(4) . . ? C27 C32 C43 118.7(4) . . ? C31 C32 C43 121.3(4) . . ? C34 C33 C42 118.6(4) . . ? C34 C33 C28 120.0(4) . . ? C42 C33 C28 121.2(4) . . ? C33 C34 C35 120.6(4) . . ? C36 C35 C34 121.5(5) . . ? C35 C36 C37 120.7(4) . . ? C38 C37 C36 122.5(4) . . ? C38 C37 C42 119.0(4) . . ? C36 C37 C42 118.5(4) . . ? C39 C38 C37 121.7(5) . . ? C38 C39 C40 119.9(5) . . ? C41 C40 C39 121.6(5) . . ? C40 C41 C42 120.2(4) . . ? C33 C42 C41 122.4(4) . . ? C33 C42 C37 120.0(4) . . ? C41 C42 C37 117.6(4) . . ? C44 C43 C52 118.4(4) . . ? C44 C43 C32 118.8(4) . . ? C52 C43 C32 122.8(4) . . ? C43 C44 C45 122.4(4) . . ? C46 C45 C44 119.9(5) . . ? C45 C46 C47 120.7(5) . . ? C46 C47 C48 122.2(6) . . ? C46 C47 C52 120.0(4) . . ? C48 C47 C52 117.8(6) . . ? C49 C48 C47 123.2(7) . . ? C48 C49 C50 120.7(6) . . ? C49 C50 C51 121.2(6) . . ? C52 C51 C50 117.7(6) . . ? C43 C52 C47 118.6(4) . . ? C43 C52 C51 122.1(5) . . ? C47 C52 C51 119.3(5) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.920 _refine_diff_density_min -0.392 _refine_diff_density_rms 0.073 #====END data_uga404_compound_1 _database_code_depnum_ccdc_archive 'CCDC 284967' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C120 H86 Pb2' _chemical_formula_weight 1942.27 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' 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 11.337(4) _cell_length_b 14.978(5) _cell_length_c 26.833(9) _cell_angle_alpha 92.280(6) _cell_angle_beta 100.708(5) _cell_angle_gamma 90.038(6) _cell_volume 4473(2) _cell_formula_units_Z 2 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour dark/red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1940 _exptl_absorpt_coefficient_mu 3.811 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.061882 _exptl_absorpt_correction_T_max 1.0 _exptl_absorpt_process_details 'Bruker SADABS' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18841 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.1414 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 23.50 _reflns_number_total 10852 _reflns_number_gt 5509 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0780P)^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 10852 _refine_ls_number_parameters 979 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1504 _refine_ls_R_factor_gt 0.0744 _refine_ls_wR_factor_ref 0.1951 _refine_ls_wR_factor_gt 0.1564 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 1.092 _refine_ls_shift/su_mean 0.037 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 0.56080(5) 0.53832(4) 0.24233(3) 0.0799(3) Uani 1 1 d . . . Pb2 Pb 0.15410(5) 0.03689(4) 0.24325(3) 0.0802(3) Uani 1 1 d . . . C1 C 0.4128(13) 0.4338(9) 0.2477(6) 0.066(4) Uani 1 1 d . . . C2 C 0.3599(14) 0.4334(10) 0.2912(6) 0.073(4) Uani 1 1 d . . . C3 C 0.2507(13) 0.4080(11) 0.2961(5) 0.077(5) Uani 1 1 d . . . H3A H 0.2232 0.4107 0.3267 0.092 Uiso 1 1 calc R . . C4 C 0.1769(10) 0.3746(11) 0.2468(6) 0.074(4) Uani 1 1 d . . . C5 C 0.2137(14) 0.3801(10) 0.2022(5) 0.069(4) Uani 1 1 d . . . H5A H 0.1613 0.3687 0.1716 0.083 Uiso 1 1 calc R . . C6 C 0.3327(11) 0.4036(8) 0.2037(5) 0.054(3) Uani 1 1 d . . . C7 C 0.4470(11) 0.4588(10) 0.3443(6) 0.066(4) Uani 1 1 d . . . C8 C 0.4012(18) 0.5132(11) 0.3796(7) 0.092(5) Uani 1 1 d . . . H8A H 0.3217 0.5315 0.3727 0.110 Uiso 1 1 calc R . . C9 C 0.475(3) 0.5401(14) 0.4257(7) 0.109(6) Uani 1 1 d . . . H9A H 0.4453 0.5742 0.4501 0.130 Uiso 1 1 calc R . . C10 C 0.590(3) 0.5155(19) 0.4335(8) 0.128(8) Uani 1 1 d . . . H10A H 0.6404 0.5359 0.4633 0.153 Uiso 1 1 calc R . . C11 C 0.640(2) 0.4610(17) 0.3994(11) 0.138(9) Uani 1 1 d . . . H11A H 0.7189 0.4424 0.4070 0.166 Uiso 1 1 calc R . . C12 C 0.5651(13) 0.4351(12) 0.3534(8) 0.084(5) Uani 1 1 d . . . H12A H 0.5963 0.4018 0.3289 0.101 Uiso 1 1 calc R . . C13 C 0.0449(17) 0.3468(12) 0.2475(7) 0.095(5) Uani 1 1 d . . . C14 C 0.0055(14) 0.3015(11) 0.2827(6) 0.077(4) Uani 1 1 d . . . H14A H 0.0636 0.2816 0.3090 0.093 Uiso 1 1 calc R . . C15 C -0.1095(16) 0.2812(18) 0.2847(11) 0.132(9) Uani 1 1 d . . . H15A H -0.1303 0.2427 0.3081 0.158 Uiso 1 1 calc R . . C16 C -0.1945(16) 0.3225(12) 0.2489(9) 0.095(6) Uani 1 1 d . . . H16A H -0.2743 0.3080 0.2488 0.114 Uiso 1 1 calc R . . C17 C -0.1774(16) 0.3732(14) 0.2189(9) 0.112(7) Uani 1 1 d . . . H17A H -0.2399 0.4027 0.1988 0.134 Uiso 1 1 calc R . . C18 C -0.0520(13) 0.3873(13) 0.2148(8) 0.099(6) Uani 1 1 d . . . H18A H -0.0348 0.4242 0.1900 0.119 Uiso 1 1 calc R . . C19 C 0.3780(13) 0.3905(9) 0.1543(6) 0.068(4) Uani 1 1 d . . . C20 C 0.3079(14) 0.4089(9) 0.1087(6) 0.070(4) Uani 1 1 d . . . H20A H 0.2313 0.4313 0.1083 0.085 Uiso 1 1 calc R . . C21 C 0.3478(17) 0.3950(10) 0.0623(6) 0.084(5) Uani 1 1 d . . . H21A H 0.2998 0.4081 0.0315 0.100 Uiso 1 1 calc R . . C22 C 0.4628(17) 0.3606(12) 0.0651(7) 0.086(5) Uani 1 1 d . . . H22A H 0.4918 0.3483 0.0354 0.103 Uiso 1 1 calc R . . C23 C 0.5311(16) 0.3451(11) 0.1092(9) 0.097(6) Uani 1 1 d . . . H23A H 0.6078 0.3227 0.1096 0.116 Uiso 1 1 calc R . . C24 C 0.4937(13) 0.3607(11) 0.1543(7) 0.080(5) Uani 1 1 d . . . H24A H 0.5456 0.3514 0.1847 0.096 Uiso 1 1 calc R . . C25 C 0.4548(11) 0.6066(9) 0.1714(5) 0.059(3) Uani 1 1 d . . . C26 C 0.4976(10) 0.6079(7) 0.1253(4) 0.043(3) Uani 1 1 d . . . C27 C 0.4190(9) 0.6262(8) 0.0814(4) 0.046(3) Uani 1 1 d . . . H27A H 0.4495 0.6290 0.0516 0.055 Uiso 1 1 calc R . . C28 C 0.2950(11) 0.6410(8) 0.0787(4) 0.050(3) Uani 1 1 d . . . C29 C 0.2550(12) 0.6442(8) 0.1247(6) 0.064(4) Uani 1 1 d . . . H29A H 0.1751 0.6579 0.1248 0.077 Uiso 1 1 calc R . . C30 C 0.3342(11) 0.6267(9) 0.1728(5) 0.059(3) Uani 1 1 d . . . C31 C 0.6262(11) 0.5951(8) 0.1250(4) 0.049(3) Uani 1 1 d . . . C32 C 0.7137(10) 0.6360(8) 0.1603(5) 0.056(3) Uani 1 1 d . . . H32A H 0.6906 0.6734 0.1852 0.067 Uiso 1 1 calc R . . C33 C 0.8362(12) 0.6248(9) 0.1608(6) 0.065(4) Uani 1 1 d . . . H33A H 0.8932 0.6526 0.1861 0.078 Uiso 1 1 calc R . . C34 C 0.8724(12) 0.5690(13) 0.1213(7) 0.085(5) Uani 1 1 d . . . H34A H 0.9531 0.5583 0.1212 0.102 Uiso 1 1 calc R . . C35 C 0.7851(13) 0.5321(10) 0.0840(6) 0.066(4) Uani 1 1 d . . . H35A H 0.8084 0.4990 0.0575 0.079 Uiso 1 1 calc R . . C36 C 0.6631(13) 0.5419(8) 0.0841(6) 0.067(4) Uani 1 1 d . . . H36A H 0.6062 0.5150 0.0585 0.080 Uiso 1 1 calc R . . C37 C 0.2124(13) 0.6510(9) 0.0291(6) 0.067(4) Uani 1 1 d . . . C38 C 0.2498(15) 0.7024(10) -0.0087(7) 0.084(5) Uani 1 1 d . . . H38A H 0.3276 0.7250 -0.0045 0.101 Uiso 1 1 calc R . . C39 C 0.1659(13) 0.7176(11) -0.0520(6) 0.077(4) Uani 1 1 d . . . H39A H 0.1881 0.7517 -0.0770 0.092 Uiso 1 1 calc R . . C40 C 0.0522(16) 0.6843(10) -0.0591(7) 0.084(5) Uani 1 1 d . . . H40A H -0.0016 0.6950 -0.0889 0.100 Uiso 1 1 calc R . . C41 C 0.0160(12) 0.6334(11) -0.0213(8) 0.087(5) Uani 1 1 d . . . H41A H -0.0612 0.6095 -0.0264 0.104 Uiso 1 1 calc R . . C42 C 0.0941(12) 0.6196(10) 0.0223(6) 0.071(4) Uani 1 1 d . . . H42A H 0.0688 0.5891 0.0480 0.086 Uiso 1 1 calc R . . C43 C 0.2872(11) 0.6388(8) 0.2201(7) 0.065(4) Uani 1 1 d . . . C44 C 0.1740(17) 0.6108(10) 0.2241(8) 0.092(5) Uani 1 1 d . . . H44A H 0.1244 0.5818 0.1967 0.111 Uiso 1 1 calc R . . C45 C 0.1353(16) 0.6265(14) 0.2695(8) 0.102(6) Uani 1 1 d . . . H45A H 0.0581 0.6077 0.2714 0.123 Uiso 1 1 calc R . . C46 C 0.1996(17) 0.6662(12) 0.3102(6) 0.083(5) Uani 1 1 d . . . H46A H 0.1694 0.6722 0.3401 0.100 Uiso 1 1 calc R . . C47 C 0.3105(17) 0.6981(13) 0.3082(8) 0.097(5) Uani 1 1 d . . . H47A H 0.3557 0.7298 0.3357 0.116 Uiso 1 1 calc R . . C48 C 0.3552(16) 0.6816(10) 0.2630(6) 0.078(4) Uani 1 1 d . . . H48A H 0.4330 0.7000 0.2618 0.094 Uiso 1 1 calc R . . C49 C 0.3112(13) -0.0642(9) 0.2472(7) 0.078(5) Uani 1 1 d . . . C50 C 0.3976(14) -0.0698(9) 0.2934(7) 0.079(5) Uani 1 1 d . . . C51 C 0.5141(12) -0.0995(9) 0.2925(4) 0.054(3) Uani 1 1 d . . . H51A H 0.5691 -0.1050 0.3226 0.065 Uiso 1 1 calc R . . C52 C 0.5464(13) -0.1207(11) 0.2464(9) 0.090(6) Uani 1 1 d . . . C53 C 0.4710(14) -0.1247(11) 0.2051(6) 0.073(4) Uani 1 1 d . . . H53A H 0.4956 -0.1464 0.1758 0.087 Uiso 1 1 calc R . . C54 C 0.3509(13) -0.0973(8) 0.2021(6) 0.066(4) Uani 1 1 d . . . C55 C 0.3609(14) -0.0419(9) 0.3446(6) 0.067(4) Uani 1 1 d . . . C56 C 0.431(2) 0.0070(14) 0.3770(8) 0.111(7) Uani 1 1 d . . . H56A H 0.5013 0.0306 0.3701 0.133 Uiso 1 1 calc R . . C57 C 0.394(3) 0.0246(14) 0.4265(6) 0.144(11) Uani 1 1 d . . . H57A H 0.4446 0.0569 0.4521 0.172 Uiso 1 1 calc R . . C58 C 0.282(3) -0.007(3) 0.4358(11) 0.187(16) Uani 1 1 d . . . H58A H 0.2550 0.0051 0.4661 0.225 Uiso 1 1 calc R . . C59 C 0.219(2) -0.0542(17) 0.3972(8) 0.120(7) Uani 1 1 d . . . H59A H 0.1456 -0.0776 0.4017 0.144 Uiso 1 1 calc R . . C60 C 0.2512(16) -0.0717(13) 0.3524(7) 0.090(5) Uani 1 1 d . . . H60A H 0.2001 -0.1036 0.3267 0.108 Uiso 1 1 calc R . . C61 C 0.6854(12) -0.1496(9) 0.2498(8) 0.081(5) Uani 1 1 d . . . C62 C 0.7542(15) -0.1966(11) 0.2905(8) 0.094(5) Uani 1 1 d . . . H62A H 0.7250 -0.2153 0.3185 0.113 Uiso 1 1 calc R . . C63 C 0.8640(15) -0.2101(15) 0.2830(8) 0.104(6) Uani 1 1 d . . . H63A H 0.9069 -0.2505 0.3047 0.125 Uiso 1 1 calc R . . C64 C 0.9218(12) -0.1789(14) 0.2521(7) 0.088(5) Uani 1 1 d . . . H64A H 1.0037 -0.1891 0.2553 0.106 Uiso 1 1 calc R . . C65 C 0.8617(17) -0.1291(14) 0.2132(11) 0.119(8) Uani 1 1 d . . . H65A H 0.9032 -0.1089 0.1889 0.143 Uiso 1 1 calc R . . C66 C 0.7390(14) -0.1079(12) 0.2093(9) 0.099(6) Uani 1 1 d . . . H66A H 0.6967 -0.0724 0.1845 0.118 Uiso 1 1 calc R . . C67 C 0.2601(11) -0.1082(8) 0.1541(5) 0.060(3) Uani 1 1 d . . . C68 C 0.1449(12) -0.1390(12) 0.1530(7) 0.085(5) Uani 1 1 d . . . H68A H 0.1203 -0.1484 0.1836 0.102 Uiso 1 1 calc R . . C69 C 0.0616(15) -0.1570(12) 0.1065(7) 0.089(5) Uani 1 1 d . . . H69A H -0.0151 -0.1798 0.1058 0.107 Uiso 1 1 calc R . . C70 C 0.1028(16) -0.1384(12) 0.0634(8) 0.098(7) Uani 1 1 d . . . H70A H 0.0504 -0.1482 0.0326 0.118 Uiso 1 1 calc R . . C71 C 0.2136(14) -0.1069(10) 0.0619(7) 0.079(4) Uani 1 1 d . . . H71A H 0.2380 -0.0976 0.0313 0.094 Uiso 1 1 calc R . . C72 C 0.2877(12) -0.0894(9) 0.1070(6) 0.065(4) Uani 1 1 d . . . H72A H 0.3619 -0.0631 0.1066 0.078 Uiso 1 1 calc R . . C73 C 0.2001(14) 0.1022(9) 0.1728(4) 0.061(3) Uani 1 1 d . . . C74 C 0.3170(12) 0.1289(9) 0.1711(5) 0.062(3) Uani 1 1 d . . . C75 C 0.3574(12) 0.1437(8) 0.1267(6) 0.061(3) Uani 1 1 d . . . H75A H 0.4383 0.1562 0.1280 0.073 Uiso 1 1 calc R . . C76 C 0.2774(11) 0.1403(8) 0.0786(5) 0.054(3) Uani 1 1 d . . . C77 C 0.1533(11) 0.1285(9) 0.0816(5) 0.060(3) Uani 1 1 d . . . H77A H 0.0968 0.1365 0.0522 0.072 Uiso 1 1 calc R . . C78 C 0.1108(9) 0.1061(8) 0.1251(4) 0.044(3) Uani 1 1 d . . . C79 C 0.4023(10) 0.1396(7) 0.2207(5) 0.048(3) Uani 1 1 d . . . C80 C 0.3686(18) 0.1827(10) 0.2605(7) 0.087(5) Uani 1 1 d . . . H80A H 0.2901 0.2023 0.2582 0.105 Uiso 1 1 calc R . . C81 C 0.4553(18) 0.1985(9) 0.3070(6) 0.088(6) Uani 1 1 d . . . H81A H 0.4321 0.2256 0.3354 0.106 Uiso 1 1 calc R . . C82 C 0.5751(17) 0.1723(15) 0.3087(8) 0.105(6) Uani 1 1 d . . . H82A H 0.6332 0.1871 0.3371 0.125 Uiso 1 1 calc R . . C83 C 0.6028(17) 0.1298(16) 0.2725(7) 0.106(7) Uani 1 1 d . . . H83A H 0.6808 0.1085 0.2760 0.127 Uiso 1 1 calc R . . C84 C 0.5229(10) 0.1110(10) 0.2253(6) 0.069(4) Uani 1 1 d . . . H84A H 0.5493 0.0810 0.1984 0.083 Uiso 1 1 calc R . . C85 C 0.3174(11) 0.1515(9) 0.0317(6) 0.064(3) Uani 1 1 d . . . C86 C 0.2479(15) 0.2014(10) -0.0094(6) 0.079(4) Uani 1 1 d . . . H86A H 0.1744 0.2246 -0.0048 0.094 Uiso 1 1 calc R . . C87 C 0.2829(14) 0.2155(11) -0.0523(6) 0.077(4) Uani 1 1 d . . . H87A H 0.2321 0.2445 -0.0778 0.093 Uiso 1 1 calc R . . C88 C 0.3973(14) 0.1871(11) -0.0604(8) 0.084(5) Uani 1 1 d . . . H88A H 0.4278 0.2013 -0.0890 0.101 Uiso 1 1 calc R . . C89 C 0.4631(15) 0.1341(11) -0.0205(7) 0.086(5) Uani 1 1 d . . . H89A H 0.5349 0.1088 -0.0256 0.103 Uiso 1 1 calc R . . C90 C 0.4271(11) 0.1190(9) 0.0237(6) 0.062(3) Uani 1 1 d . . . H90A H 0.4755 0.0870 0.0485 0.075 Uiso 1 1 calc R . . C91 C -0.0207(12) 0.0930(9) 0.1242(6) 0.064(4) Uani 1 1 d . . . C92 C -0.0906(11) 0.0410(9) 0.0834(6) 0.067(4) Uani 1 1 d . . . H92A H -0.0568 0.0143 0.0576 0.081 Uiso 1 1 calc R . . C93 C -0.2107(12) 0.0329(10) 0.0847(7) 0.075(4) Uani 1 1 d . . . H93A H -0.2576 -0.0015 0.0588 0.090 Uiso 1 1 calc R . . C94 C -0.2659(12) 0.0710(12) 0.1207(7) 0.083(5) Uani 1 1 d . . . H94A H -0.3479 0.0629 0.1192 0.100 Uiso 1 1 calc R . . C95 C -0.2004(12) 0.1208(11) 0.1586(5) 0.067(4) Uani 1 1 d . . . H95A H -0.2367 0.1502 0.1829 0.080 Uiso 1 1 calc R . . C96 C -0.0777(10) 0.1277(9) 0.1609(5) 0.057(3) Uani 1 1 d . . . H96A H -0.0318 0.1576 0.1889 0.069 Uiso 1 1 calc R . . C97 C 0.254(3) 0.287(2) 0.4547(15) 0.176(12) Uiso 1 1 d . . . C98 C 0.223(5) 0.388(3) 0.459(2) 0.249(19) Uiso 1 1 d . . . C99 C 0.108(10) 0.380(7) 0.423(4) 0.42(4) Uiso 1 1 d . . . C100 C -0.010(6) 0.314(5) 0.418(3) 0.29(3) Uiso 1 1 d . . . C101 C 0.042(3) 0.230(2) 0.4240(14) 0.170(11) Uiso 1 1 d . . . C102 C 0.162(4) 0.219(2) 0.4414(16) 0.182(12) Uiso 1 1 d . . . C103 C 0.370(2) 0.2798(16) 0.4771(11) 0.131(7) Uiso 1 1 d . . . C104 C 0.408(3) 0.218(2) 0.5284(13) 0.163(10) Uiso 1 1 d . . . C105 C 0.527(3) 0.2035(16) 0.5458(10) 0.125(7) Uiso 1 1 d . . . C106 C 0.608(3) 0.222(2) 0.5273(15) 0.176(12) Uiso 1 1 d . . . C107 C 0.588(3) 0.281(2) 0.4694(13) 0.153(9) Uiso 1 1 d . . . C108 C 0.468(2) 0.2933(14) 0.4582(9) 0.112(6) Uiso 1 1 d . . . C109 C 0.047(3) 0.489(2) 0.4143(13) 0.154(9) Uiso 1 1 d . . . C110 C 0.109(4) 0.560(4) 0.444(2) 0.220(17) Uiso 1 1 d . . . C111 C 0.074(7) 0.624(5) 0.454(3) 0.26(2) Uiso 1 1 d . . . C112 C -0.009(7) 0.641(4) 0.429(3) 0.28(3) Uiso 1 1 d . . . C113 C -0.097(4) 0.578(3) 0.3649(18) 0.215(15) Uiso 1 1 d . . . C114 C -0.042(3) 0.505(2) 0.3710(13) 0.151(9) Uiso 1 1 d . . . C115 C -0.065(5) 0.137(4) 0.414(2) 0.241(19) Uiso 1 1 d . . . C116 C -0.126(9) 0.156(6) 0.453(4) 0.36(4) Uiso 1 1 d . . . C117 C -0.217(5) 0.097(4) 0.425(2) 0.244(19) Uiso 1 1 d . . . C118 C -0.203(4) 0.007(3) 0.3903(16) 0.188(13) Uiso 1 1 d . . . C119 C -0.110(3) 0.0084(19) 0.3709(12) 0.143(9) Uiso 1 1 d . . . C120 C -0.031(3) 0.079(3) 0.3707(16) 0.192(13) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0622(4) 0.0999(5) 0.0729(5) 0.0181(4) -0.0027(3) -0.0104(3) Pb2 0.0694(4) 0.0983(4) 0.0758(5) 0.0164(4) 0.0182(3) 0.0181(3) C1 0.070(9) 0.060(7) 0.067(10) 0.005(7) 0.012(8) -0.014(6) C2 0.071(10) 0.092(10) 0.049(9) -0.008(8) -0.007(7) 0.013(8) C3 0.069(9) 0.121(12) 0.037(7) -0.040(8) 0.011(6) -0.049(9) C4 0.015(6) 0.122(12) 0.075(11) 0.017(9) -0.016(6) -0.009(6) C5 0.081(10) 0.101(10) 0.026(7) 0.019(7) 0.009(7) 0.001(8) C6 0.054(8) 0.058(7) 0.054(8) 0.018(6) 0.016(6) -0.001(6) C7 0.037(7) 0.093(9) 0.073(10) 0.004(8) 0.018(6) 0.001(6) C8 0.116(14) 0.078(10) 0.079(13) 0.021(9) 0.010(11) 0.015(9) C9 0.16(2) 0.114(14) 0.044(10) -0.021(10) 0.008(12) 0.001(14) C10 0.14(2) 0.16(2) 0.066(13) -0.010(14) -0.007(14) -0.059(18) C11 0.103(16) 0.154(19) 0.15(2) -0.078(19) 0.019(16) -0.033(14) C12 0.055(9) 0.099(11) 0.102(14) 0.032(10) 0.019(9) 0.005(8) C13 0.113(14) 0.091(11) 0.077(12) 0.038(10) 0.002(10) 0.014(9) C14 0.082(10) 0.105(11) 0.048(9) 0.016(8) 0.018(7) -0.008(9) C15 0.050(10) 0.19(2) 0.17(2) 0.035(19) 0.057(13) -0.020(12) C16 0.065(11) 0.075(10) 0.142(18) 0.013(11) 0.011(11) -0.015(8) C17 0.076(12) 0.105(13) 0.138(19) 0.041(14) -0.028(11) -0.029(10) C18 0.041(8) 0.116(12) 0.124(16) 0.002(12) -0.023(9) 0.023(8) C19 0.067(9) 0.068(8) 0.067(10) -0.016(7) 0.009(7) -0.022(7) C20 0.071(9) 0.073(8) 0.063(10) -0.007(8) 0.005(8) -0.010(7) C21 0.112(14) 0.085(10) 0.042(9) -0.025(8) -0.010(8) -0.019(9) C22 0.087(12) 0.110(12) 0.061(10) 0.006(10) 0.015(9) -0.013(10) C23 0.077(11) 0.089(11) 0.128(18) 0.020(11) 0.024(12) 0.022(9) C24 0.044(8) 0.099(10) 0.107(13) -0.015(10) 0.041(8) -0.017(7) C25 0.040(7) 0.073(8) 0.057(9) 0.003(7) -0.010(6) -0.003(6) C26 0.052(7) 0.045(6) 0.031(7) 0.008(5) 0.000(5) -0.007(5) C27 0.030(6) 0.075(7) 0.037(6) 0.012(6) 0.018(5) 0.003(5) C28 0.053(7) 0.072(7) 0.031(6) 0.009(6) 0.019(5) 0.008(6) C29 0.057(8) 0.064(7) 0.076(10) 0.016(7) 0.021(7) 0.002(6) C30 0.049(8) 0.078(8) 0.052(8) 0.010(7) 0.011(6) 0.011(6) C31 0.053(7) 0.079(8) 0.020(6) 0.020(6) 0.015(5) -0.010(6) C32 0.041(7) 0.065(7) 0.058(8) 0.013(7) 0.003(6) 0.010(6) C33 0.051(8) 0.076(8) 0.065(9) 0.014(8) -0.002(7) -0.002(6) C34 0.039(8) 0.124(13) 0.093(13) 0.028(11) 0.011(8) 0.020(8) C35 0.064(9) 0.084(9) 0.059(9) 0.001(7) 0.032(7) -0.009(7) C36 0.077(10) 0.055(7) 0.064(9) 0.014(7) 0.001(7) -0.027(6) C37 0.068(9) 0.067(8) 0.066(10) -0.014(7) 0.014(7) 0.004(7) C38 0.076(10) 0.075(9) 0.099(14) -0.003(9) 0.016(10) 0.001(8) C39 0.063(9) 0.096(10) 0.071(10) -0.013(9) 0.013(8) 0.022(8) C40 0.088(12) 0.081(9) 0.079(12) 0.022(9) 0.003(9) 0.015(8) C41 0.034(7) 0.098(11) 0.122(15) -0.005(11) 0.003(9) 0.001(7) C42 0.045(8) 0.096(10) 0.075(10) -0.023(8) 0.022(7) -0.010(7) C43 0.043(7) 0.048(6) 0.102(12) -0.002(7) 0.010(7) 0.006(6) C44 0.095(13) 0.063(8) 0.119(16) 0.022(9) 0.016(11) 0.009(8) C45 0.072(11) 0.143(16) 0.099(16) 0.010(13) 0.032(11) 0.061(11) C46 0.108(13) 0.120(13) 0.028(8) 0.002(8) 0.028(8) 0.028(11) C47 0.085(12) 0.123(14) 0.083(13) -0.015(11) 0.023(10) 0.005(11) C48 0.112(12) 0.078(9) 0.044(9) -0.010(8) 0.015(8) -0.005(9) C49 0.055(8) 0.066(8) 0.110(14) -0.031(9) 0.015(9) -0.001(6) C50 0.082(11) 0.056(8) 0.091(12) -0.017(8) 0.003(9) -0.030(7) C51 0.063(8) 0.078(8) 0.014(6) 0.014(6) -0.018(5) 0.000(6) C52 0.035(8) 0.097(11) 0.15(2) 0.027(12) 0.051(10) -0.008(7) C53 0.063(10) 0.099(11) 0.054(9) -0.002(8) 0.009(8) -0.002(8) C54 0.079(10) 0.054(7) 0.078(11) 0.011(7) 0.044(9) -0.022(7) C55 0.083(11) 0.061(7) 0.048(9) -0.012(7) -0.010(8) 0.009(7) C56 0.145(18) 0.119(14) 0.083(15) 0.028(12) 0.055(14) 0.009(13) C57 0.30(4) 0.099(13) 0.015(8) -0.004(8) -0.017(13) 0.030(16) C58 0.15(2) 0.33(5) 0.11(2) -0.03(2) 0.10(2) -0.02(3) C59 0.140(19) 0.159(19) 0.058(13) 0.021(13) 0.006(12) -0.017(15) C60 0.085(12) 0.117(13) 0.077(13) 0.015(10) 0.037(9) 0.001(10) C61 0.048(8) 0.061(8) 0.142(16) 0.036(9) 0.038(9) 0.026(6) C62 0.073(11) 0.088(10) 0.126(16) 0.026(11) 0.024(10) 0.017(8) C63 0.055(10) 0.168(18) 0.086(13) 0.056(13) -0.004(9) 0.050(11) C64 0.028(7) 0.151(15) 0.084(12) 0.025(12) 0.004(8) 0.033(9) C65 0.078(12) 0.118(14) 0.18(2) 0.016(15) 0.072(15) 0.010(11) C66 0.057(9) 0.095(11) 0.160(19) 0.008(12) 0.062(11) 0.018(8) C67 0.055(8) 0.059(7) 0.059(9) -0.004(7) -0.003(7) 0.017(6) C68 0.050(8) 0.125(13) 0.074(11) -0.003(10) -0.002(7) -0.003(8) C69 0.063(9) 0.121(13) 0.073(12) -0.012(10) -0.009(9) -0.029(9) C70 0.071(11) 0.118(13) 0.091(14) -0.057(12) -0.010(10) 0.034(10) C71 0.061(10) 0.090(10) 0.078(11) -0.012(9) 0.000(8) 0.024(8) C72 0.056(8) 0.066(8) 0.081(11) 0.011(7) 0.030(8) 0.023(6) C73 0.092(10) 0.073(8) 0.024(6) 0.009(6) 0.024(6) 0.014(7) C74 0.062(9) 0.084(9) 0.036(7) -0.015(7) 0.000(6) -0.006(7) C75 0.047(7) 0.064(7) 0.076(10) 0.008(7) 0.025(7) 0.002(6) C76 0.061(8) 0.053(6) 0.043(7) -0.008(6) -0.002(6) -0.020(6) C77 0.059(8) 0.080(8) 0.032(7) -0.011(6) -0.011(6) 0.006(6) C78 0.029(6) 0.062(7) 0.039(7) -0.011(6) 0.007(5) 0.006(5) C79 0.049(7) 0.050(6) 0.041(7) 0.004(6) 0.003(6) -0.013(5) C80 0.128(14) 0.072(9) 0.074(12) 0.006(8) 0.050(11) 0.008(9) C81 0.155(17) 0.062(8) 0.031(8) 0.013(7) -0.029(9) -0.007(9) C82 0.081(12) 0.142(16) 0.071(14) 0.021(13) -0.042(10) -0.022(11) C83 0.086(12) 0.178(19) 0.052(10) -0.008(12) 0.011(9) -0.085(13) C84 0.034(7) 0.091(9) 0.079(10) -0.010(8) 0.006(7) -0.001(6) C85 0.051(8) 0.067(7) 0.075(10) 0.013(7) 0.014(7) 0.003(6) C86 0.082(10) 0.074(9) 0.076(11) -0.016(8) 0.011(9) -0.038(8) C87 0.070(10) 0.110(11) 0.053(9) 0.018(8) 0.012(7) -0.001(8) C88 0.063(10) 0.087(10) 0.103(14) -0.005(10) 0.016(9) -0.023(8) C89 0.077(11) 0.094(10) 0.095(13) -0.030(10) 0.046(10) -0.005(9) C90 0.040(7) 0.076(8) 0.076(10) 0.020(7) 0.023(7) 0.005(6) C91 0.058(8) 0.064(7) 0.073(10) 0.004(7) 0.018(7) 0.020(6) C92 0.044(7) 0.077(8) 0.081(10) -0.023(8) 0.019(7) 0.020(6) C93 0.049(8) 0.085(9) 0.088(11) -0.022(9) 0.012(8) -0.009(7) C94 0.037(7) 0.123(13) 0.096(13) 0.046(11) 0.023(8) 0.011(8) C95 0.049(8) 0.108(10) 0.046(8) -0.011(8) 0.019(7) 0.002(7) C96 0.039(7) 0.090(9) 0.046(8) 0.006(7) 0.015(6) 0.001(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 C1 2.322(13) . ? Pb1 C25 2.327(13) . ? Pb2 C73 2.305(12) . ? Pb2 C49 2.329(14) . ? C1 C6 1.409(19) . ? C1 C2 1.41(2) . ? C2 C3 1.33(2) . ? C2 C7 1.61(2) . ? C3 C4 1.494(19) . ? C4 C5 1.34(2) . ? C4 C13 1.56(2) . ? C5 C6 1.387(18) . ? C6 C19 1.51(2) . ? C7 C12 1.366(19) . ? C7 C8 1.40(2) . ? C8 C9 1.40(3) . ? C9 C10 1.34(3) . ? C10 C11 1.39(3) . ? C11 C12 1.40(3) . ? C13 C14 1.33(2) . ? C13 C18 1.42(2) . ? C14 C15 1.35(2) . ? C15 C16 1.39(3) . ? C16 C17 1.17(3) . ? C17 C18 1.46(2) . ? C19 C24 1.39(2) . ? C19 C20 1.37(2) . ? C20 C21 1.41(2) . ? C21 C22 1.39(2) . ? C22 C23 1.32(3) . ? C23 C24 1.37(3) . ? C25 C30 1.408(17) . ? C25 C26 1.410(19) . ? C26 C27 1.376(15) . ? C26 C31 1.473(16) . ? C27 C28 1.412(15) . ? C28 C29 1.390(19) . ? C28 C37 1.490(19) . ? C29 C30 1.462(19) . ? C30 C43 1.47(2) . ? C31 C36 1.45(2) . ? C31 C32 1.364(17) . ? C32 C33 1.396(18) . ? C33 C34 1.44(2) . ? C34 C35 1.37(2) . ? C35 C36 1.391(19) . ? C37 C38 1.42(2) . ? C37 C42 1.398(19) . ? C38 C39 1.38(2) . ? C39 C40 1.36(2) . ? C40 C41 1.41(2) . ? C41 C42 1.35(2) . ? C43 C48 1.39(2) . ? C43 C44 1.37(2) . ? C44 C45 1.38(3) . ? C45 C46 1.31(3) . ? C46 C47 1.36(2) . ? C47 C48 1.41(2) . ? C49 C54 1.44(2) . ? C49 C50 1.44(2) . ? C50 C51 1.40(2) . ? C50 C55 1.55(2) . ? C51 C52 1.38(2) . ? C52 C53 1.27(2) . ? C52 C61 1.621(19) . ? C53 C54 1.41(2) . ? C54 C67 1.49(2) . ? C55 C56 1.27(3) . ? C55 C60 1.38(2) . ? C56 C57 1.48(3) . ? C57 C58 1.42(4) . ? C58 C59 1.32(4) . ? C59 C60 1.34(3) . ? C61 C66 1.50(3) . ? C61 C62 1.43(2) . ? C62 C63 1.31(2) . ? C63 C64 1.25(2) . ? C64 C65 1.38(3) . ? C65 C66 1.41(2) . ? C67 C68 1.380(19) . ? C67 C72 1.40(2) . ? C68 C69 1.43(2) . ? C69 C70 1.36(3) . ? C70 C71 1.35(2) . ? C71 C72 1.36(2) . ? C73 C74 1.394(19) . ? C73 C78 1.481(17) . ? C74 C75 1.38(2) . ? C74 C79 1.495(17) . ? C75 C76 1.432(19) . ? C76 C77 1.435(18) . ? C76 C85 1.43(2) . ? C77 C78 1.396(18) . ? C78 C91 1.499(17) . ? C79 C80 1.34(2) . ? C79 C84 1.418(17) . ? C80 C81 1.45(2) . ? C81 C82 1.41(3) . ? C82 C83 1.23(3) . ? C83 C84 1.43(2) . ? C85 C90 1.387(18) . ? C85 C86 1.46(2) . ? C86 C87 1.31(2) . ? C87 C88 1.42(2) . ? C88 C89 1.45(3) . ? C89 C90 1.35(2) . ? C91 C92 1.43(2) . ? C91 C96 1.361(19) . ? C92 C93 1.373(18) . ? C93 C94 1.36(2) . ? C94 C95 1.34(2) . ? C95 C96 1.385(17) . ? C97 C103 1.34(4) . ? C97 C102 1.45(5) . ? C97 C98 1.56(6) . ? C98 C99 1.47(10) . ? C99 C109 1.78(10) . ? C99 C100 1.64(10) . ? C100 C101 1.40(7) . ? C101 C115 1.83(6) . ? C101 C102 1.36(4) . ? C103 C108 1.32(3) . ? C103 C104 1.68(4) . ? C104 C105 1.36(3) . ? C105 C106 1.17(4) . ? C106 C107 1.80(5) . ? C107 C108 1.36(3) . ? C109 C114 1.42(4) . ? C109 C110 1.41(5) . ? C110 C111 1.08(6) . ? C111 C112 1.09(7) . ? C112 C113 2.02(8) . ? C113 C114 1.26(4) . ? C115 C116 1.38(9) . ? C115 C120 1.54(6) . ? C116 C117 1.43(9) . ? C117 C118 1.63(6) . ? C118 C119 1.26(4) . ? C119 C120 1.38(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Pb1 C25 95.8(5) . . ? C73 Pb2 C49 92.7(6) . . ? C6 C1 C2 112.1(12) . . ? C6 C1 Pb1 120.2(10) . . ? C2 C1 Pb1 120.0(11) . . ? C3 C2 C1 130.0(13) . . ? C3 C2 C7 113.7(13) . . ? C1 C2 C7 116.1(13) . . ? C2 C3 C4 112.3(12) . . ? C5 C4 C13 119.6(13) . . ? C5 C4 C3 122.9(13) . . ? C13 C4 C3 116.8(14) . . ? C4 C5 C6 117.4(13) . . ? C1 C6 C5 124.6(12) . . ? C1 C6 C19 119.3(12) . . ? C5 C6 C19 116.0(12) . . ? C12 C7 C8 120.2(16) . . ? C12 C7 C2 121.7(14) . . ? C8 C7 C2 117.9(13) . . ? C9 C8 C7 119.9(18) . . ? C10 C9 C8 118.4(19) . . ? C9 C10 C11 124(2) . . ? C10 C11 C12 118(2) . . ? C7 C12 C11 120.1(19) . . ? C14 C13 C18 111.0(18) . . ? C14 C13 C4 127.2(15) . . ? C18 C13 C4 120.3(15) . . ? C13 C14 C15 127.3(19) . . ? C16 C15 C14 115(2) . . ? C17 C16 C15 127.7(19) . . ? C16 C17 C18 116.0(19) . . ? C17 C18 C13 122.5(19) . . ? C24 C19 C20 117.8(15) . . ? C24 C19 C6 120.5(14) . . ? C20 C19 C6 121.7(13) . . ? C21 C20 C19 122.3(15) . . ? C22 C21 C20 116.5(15) . . ? C21 C22 C23 121.1(17) . . ? C22 C23 C24 122.5(17) . . ? C19 C24 C23 119.7(18) . . ? C30 C25 C26 120.4(11) . . ? C30 C25 Pb1 115.9(10) . . ? C26 C25 Pb1 122.0(9) . . ? C27 C26 C25 119.2(11) . . ? C27 C26 C31 120.6(10) . . ? C25 C26 C31 120.1(10) . . ? C26 C27 C28 124.1(10) . . ? C29 C28 C27 116.1(11) . . ? C29 C28 C37 122.4(12) . . ? C27 C28 C37 121.5(10) . . ? C28 C29 C30 122.3(12) . . ? C25 C30 C29 117.6(12) . . ? C25 C30 C43 123.4(12) . . ? C29 C30 C43 118.8(11) . . ? C36 C31 C32 117.8(12) . . ? C36 C31 C26 119.8(11) . . ? C32 C31 C26 122.3(11) . . ? C31 C32 C33 123.4(13) . . ? C32 C33 C34 118.5(13) . . ? C35 C34 C33 118.5(12) . . ? C34 C35 C36 122.9(13) . . ? C31 C36 C35 118.8(12) . . ? C38 C37 C42 120.0(14) . . ? C38 C37 C28 119.4(13) . . ? C42 C37 C28 120.0(14) . . ? C39 C38 C37 117.4(15) . . ? C38 C39 C40 122.2(17) . . ? C41 C40 C39 119.9(15) . . ? C42 C41 C40 119.7(14) . . ? C41 C42 C37 120.6(15) . . ? C48 C43 C44 116.7(17) . . ? C48 C43 C30 121.1(13) . . ? C44 C43 C30 122.2(15) . . ? C43 C44 C45 119(2) . . ? C46 C45 C44 124.7(19) . . ? C45 C46 C47 119.4(16) . . ? C46 C47 C48 117.9(18) . . ? C43 C48 C47 122.5(17) . . ? C54 C49 C50 115.3(13) . . ? C54 C49 Pb2 121.4(12) . . ? C50 C49 Pb2 119.6(11) . . ? C51 C50 C49 120.7(14) . . ? C51 C50 C55 120.0(13) . . ? C49 C50 C55 119.3(14) . . ? C52 C51 C50 119.1(13) . . ? C51 C52 C53 122.4(13) . . ? C51 C52 C61 114.8(17) . . ? C53 C52 C61 122.5(18) . . ? C52 C53 C54 122.3(15) . . ? C53 C54 C49 119.4(15) . . ? C53 C54 C67 122.1(13) . . ? C49 C54 C67 118.3(13) . . ? C56 C55 C60 122.8(17) . . ? C56 C55 C50 120.0(16) . . ? C60 C55 C50 117.2(14) . . ? C57 C56 C55 117(2) . . ? C56 C57 C58 121(2) . . ? C59 C58 C57 114(2) . . ? C60 C59 C58 126(2) . . ? C59 C60 C55 119(2) . . ? C66 C61 C62 123.3(13) . . ? C66 C61 C52 111.2(13) . . ? C62 C61 C52 124.8(15) . . ? C63 C62 C61 111.1(17) . . ? C62 C63 C64 132.1(17) . . ? C65 C64 C63 118.8(14) . . ? C64 C65 C66 121.8(19) . . ? C61 C66 C65 111.8(18) . . ? C68 C67 C72 115.5(13) . . ? C68 C67 C54 122.7(13) . . ? C72 C67 C54 121.7(13) . . ? C67 C68 C69 122.5(16) . . ? C70 C69 C68 115.2(15) . . ? C69 C70 C71 125.2(17) . . ? C72 C71 C70 117.1(17) . . ? C71 C72 C67 124.3(14) . . ? C74 C73 C78 116.9(10) . . ? C74 C73 Pb2 121.3(9) . . ? C78 C73 Pb2 121.3(10) . . ? C75 C74 C73 123.7(12) . . ? C75 C74 C79 119.4(12) . . ? C73 C74 C79 116.9(11) . . ? C74 C75 C76 121.4(12) . . ? C75 C76 C77 114.4(11) . . ? C75 C76 C85 122.7(11) . . ? C77 C76 C85 122.8(11) . . ? C76 C77 C78 125.1(11) . . ? C73 C78 C77 117.1(10) . . ? C73 C78 C91 121.5(11) . . ? C77 C78 C91 121.3(11) . . ? C80 C79 C84 118.8(14) . . ? C80 C79 C74 120.4(13) . . ? C84 C79 C74 120.6(12) . . ? C79 C80 C81 119.6(17) . . ? C82 C81 C80 119.2(16) . . ? C83 C82 C81 119.9(17) . . ? C82 C83 C84 124(2) . . ? C79 C84 C83 118.0(15) . . ? C90 C85 C86 116.4(13) . . ? C90 C85 C76 121.5(13) . . ? C86 C85 C76 122.0(13) . . ? C87 C86 C85 124.0(16) . . ? C88 C87 C86 120.8(17) . . ? C87 C88 C89 114.6(16) . . ? C90 C89 C88 124.5(15) . . ? C89 C90 C85 119.4(15) . . ? C92 C91 C96 117.7(12) . . ? C92 C91 C78 119.2(12) . . ? C96 C91 C78 123.2(13) . . ? C91 C92 C93 116.0(13) . . ? C94 C93 C92 125.0(15) . . ? C95 C94 C93 118.9(13) . . ? C94 C95 C96 118.8(13) . . ? C91 C96 C95 123.4(13) . . ? C103 C97 C102 130(3) . . ? C103 C97 C98 106(3) . . ? C102 C97 C98 122(4) . . ? C97 C98 C99 94(5) . . ? C109 C99 C100 104(7) . . ? C109 C99 C98 108(7) . . ? C100 C99 C98 135(8) . . ? C101 C100 C99 102(6) . . ? C115 C101 C102 123(3) . . ? C115 C101 C100 114(4) . . ? C102 C101 C100 123(4) . . ? C97 C102 C101 128(3) . . ? C97 C103 C108 129(3) . . ? C97 C103 C104 120(3) . . ? C108 C103 C104 108(2) . . ? C105 C104 C103 118(3) . . ? C106 C105 C104 128(4) . . ? C105 C106 C107 121(3) . . ? C108 C107 C106 103(2) . . ? C103 C108 C107 141(3) . . ? C99 C109 C114 120(5) . . ? C99 C109 C110 117(5) . . ? C114 C109 C110 121(3) . . ? C109 C110 C111 128(6) . . ? C112 C111 C110 113(9) . . ? C111 C112 C113 130(7) . . ? C114 C113 C112 96(4) . . ? C113 C114 C109 123(4) . . ? C116 C115 C120 154(7) . . ? C116 C115 C101 100(6) . . ? C120 C115 C101 105(4) . . ? C115 C116 C117 85(8) . . ? C118 C117 C116 130(6) . . ? C119 C118 C117 113(3) . . ? C118 C119 C120 128(3) . . ? C115 C120 C119 99(3) . . ? _diffrn_measured_fraction_theta_max 0.820 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.820 _refine_diff_density_max 1.955 _refine_diff_density_min -1.061 _refine_diff_density_rms 0.092