# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_coden_Cambridge 182 _publ_requested_journal Chem.Commun. _publ_contact_author_name 'Prof. Dr. Matthias Driess' _publ_contact_author_address ; Technische Universitat Berlin Institute of Chemistry: Metalorganics and Inorganic Materials Sekretariat C2; Strasse des 17. Juni 135 D-10623 Berlin ; _publ_contact_author_email matthias.driess@tu-berlin.de _publ_contact_author_phone +49(0)30-314-29731 _publ_contact_author_fax +49(0)30-314-29732 _publ_section_title ; A new type of heteroleptic complexes of divalent lead and synthesis of the P-plumbyleniophosphasilene, R2Si=P?Pb(L): (L = B-diketiminate) ; loop_ _publ_author_name _publ_author_address 'Shenglai Yao.' ;Technische Universitat Berlin Institute of Chemistry: Metalorganics and Inorganic Materials Sekretariat C2; Strasse des 17. Juni 135 D-10623 Berlin ; 'Block, S.' ;Technische Universitat Berlin Institute of Chemistry: Metalorganics and Inorganic Materials Sekretariat C2; Strasse des 17. Juni 135 D-10623 Berlin ; 'Brym, M.' ;Technische Universitat Berlin Institute of Chemistry: Metalorganics and Inorganic Materials Sekretariat C2; Strasse des 17. Juni 135 D-10623 Berlin ; 'Driess, M.' ;Technische Universitat Berlin Institute of Chemistry: Metalorganics and Inorganic Materials Sekretariat C2; Strasse des 17. Juni 135 D-10623 Berlin ; data_Pb-OR _database_code_depnum_ccdc_archive 'CCDC 654313' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H124 N4 O2 Pb2' _chemical_formula_weight 1660.27 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.6849(6) _cell_length_b 10.9636(4) _cell_length_c 36.7625(12) _cell_angle_alpha 90.00 _cell_angle_beta 91.3040(10) _cell_angle_gamma 90.00 _cell_volume 7931.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.390 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3392 _exptl_absorpt_coefficient_mu 4.287 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2789 _exptl_absorpt_correction_T_max 0.4137 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _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 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 47359 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13905 _reflns_number_gt 10622 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-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^)+(0.0554P)^2^+8.3919P] 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 13905 _refine_ls_number_parameters 879 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.1029 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.035 _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 0.056433(13) -0.17959(3) 0.364340(7) 0.03908(9) Uani 1 1 d . . . O1 O -0.0153(2) -0.1759(5) 0.40994(13) 0.0453(12) Uani 1 1 d . . . N1 N 0.0243(3) -0.3647(6) 0.33984(16) 0.0433(15) Uani 1 1 d . . . C1 C 0.0176(4) -0.5863(8) 0.3325(2) 0.054(2) Uani 1 1 d . . . H1A H -0.0307 -0.5969 0.3376 0.081 Uiso 1 1 calc R . . H1B H 0.0430 -0.6575 0.3415 0.081 Uiso 1 1 calc R . . H1C H 0.0234 -0.5783 0.3062 0.081 Uiso 1 1 calc R . . Pb2 Pb 0.472386(12) 0.37604(2) 0.382324(7) 0.03357(8) Uani 1 1 d . . . O2 O 0.5801(2) 0.4023(5) 0.36530(12) 0.0392(11) Uani 1 1 d . . . N2 N 0.1347(3) -0.2946(6) 0.39603(15) 0.0387(14) Uani 1 1 d . . . C2 C 0.0434(3) -0.4748(8) 0.35113(19) 0.0449(19) Uani 1 1 d . . . N3 N 0.4229(3) 0.2211(5) 0.34805(14) 0.0335(12) Uani 1 1 d . . . C3 C 0.0870(4) -0.4936(7) 0.38229(18) 0.0429(17) Uani 1 1 d . . . H3 H 0.0854 -0.5735 0.3922 0.052 Uiso 1 1 calc R . . N4 N 0.4990(3) 0.2200(5) 0.42216(14) 0.0333(12) Uani 1 1 d . . . C4 C 0.1316(3) -0.4144(7) 0.40068(19) 0.0408(17) Uani 1 1 d . . . C5 C 0.1807(4) -0.4752(8) 0.4278(2) 0.052(2) Uani 1 1 d . . . H5A H 0.2245 -0.4886 0.4162 0.078 Uiso 1 1 calc R . . H5B H 0.1619 -0.5537 0.4354 0.078 Uiso 1 1 calc R . . H5C H 0.1872 -0.4225 0.4491 0.078 Uiso 1 1 calc R . . C6 C -0.0143(4) -0.3562(8) 0.30541(19) 0.0458(19) Uani 1 1 d . . . C7 C -0.0857(4) -0.3600(8) 0.3047(2) 0.0495(19) Uani 1 1 d . . . C8 C -0.1196(4) -0.3606(9) 0.2704(2) 0.061(2) Uani 1 1 d . . . H8 H -0.1678 -0.3661 0.2691 0.073 Uiso 1 1 calc R . . C9 C -0.0841(5) -0.3534(10) 0.2394(2) 0.068(3) Uani 1 1 d . . . H9 H -0.1075 -0.3571 0.2165 0.082 Uiso 1 1 calc R . . C10 C -0.0142(5) -0.3409(10) 0.2404(2) 0.071(3) Uani 1 1 d . . . H10 H 0.0093 -0.3312 0.2183 0.085 Uiso 1 1 calc R . . C11 C 0.0220(4) -0.3422(8) 0.2730(2) 0.052(2) Uani 1 1 d . . . C12 C 0.0994(4) -0.3274(9) 0.2728(2) 0.057(2) Uani 1 1 d . . . H12 H 0.1160 -0.3176 0.2986 0.068 Uiso 1 1 calc R . . C13 C 0.1322(5) -0.4416(11) 0.2573(3) 0.085(3) Uani 1 1 d . . . H13A H 0.1162 -0.5136 0.2703 0.127 Uiso 1 1 calc R . . H13B H 0.1817 -0.4355 0.2601 0.127 Uiso 1 1 calc R . . H13C H 0.1199 -0.4489 0.2314 0.127 Uiso 1 1 calc R . . C14 C 0.1196(5) -0.2141(11) 0.2517(3) 0.086(3) Uani 1 1 d . . . H14A H 0.1072 -0.2248 0.2260 0.130 Uiso 1 1 calc R . . H14B H 0.1688 -0.2017 0.2543 0.130 Uiso 1 1 calc R . . H14C H 0.0958 -0.1430 0.2613 0.130 Uiso 1 1 calc R . . C15 C -0.1273(4) -0.3607(9) 0.3387(2) 0.061(2) Uani 1 1 d . . . H15 H -0.0954 -0.3567 0.3602 0.073 Uiso 1 1 calc R . . C16 C -0.1736(5) -0.2499(11) 0.3397(3) 0.078(3) Uani 1 1 d . . . H16A H -0.1462 -0.1755 0.3385 0.117 Uiso 1 1 calc R . . H16B H -0.1989 -0.2504 0.3623 0.117 Uiso 1 1 calc R . . H16C H -0.2056 -0.2524 0.3189 0.117 Uiso 1 1 calc R . . C17 C -0.1688(5) -0.4803(11) 0.3412(3) 0.083(3) Uani 1 1 d . . . H17A H -0.2005 -0.4859 0.3204 0.124 Uiso 1 1 calc R . . H17B H -0.1943 -0.4805 0.3638 0.124 Uiso 1 1 calc R . . H17C H -0.1378 -0.5502 0.3411 0.124 Uiso 1 1 calc R . . C18 C 0.1973(3) -0.2310(7) 0.40722(19) 0.0395(16) Uani 1 1 d . . . C19 C 0.2558(3) -0.2476(7) 0.3864(2) 0.0434(17) Uani 1 1 d . . . C20 C 0.3146(4) -0.1846(9) 0.3969(2) 0.058(2) Uani 1 1 d . . . H20 H 0.3552 -0.1969 0.3839 0.069 Uiso 1 1 calc R . . C21 C 0.3149(4) -0.1048(9) 0.4258(3) 0.064(3) Uani 1 1 d . . . H21 H 0.3551 -0.0613 0.4322 0.077 Uiso 1 1 calc R . . C22 C 0.2564(4) -0.0879(8) 0.4456(2) 0.057(2) Uani 1 1 d . . . H22 H 0.2571 -0.0323 0.4654 0.068 Uiso 1 1 calc R . . C23 C 0.1964(4) -0.1514(7) 0.4370(2) 0.0469(19) Uani 1 1 d . . . C24 C 0.1354(4) -0.1333(8) 0.4605(2) 0.054(2) Uani 1 1 d . . . H24 H 0.0941 -0.1595 0.4462 0.065 Uiso 1 1 calc R . . C25 C 0.1407(5) -0.2118(12) 0.4952(3) 0.085(4) Uani 1 1 d . . . H25A H 0.1438 -0.2980 0.4885 0.128 Uiso 1 1 calc R . . H25B H 0.1004 -0.1988 0.5098 0.128 Uiso 1 1 calc R . . H25C H 0.1814 -0.1883 0.5094 0.128 Uiso 1 1 calc R . . C26 C 0.1253(5) 0.0020(10) 0.4724(3) 0.084(4) Uani 1 1 d . . . H26A H 0.1635 0.0271 0.4883 0.126 Uiso 1 1 calc R . . H26B H 0.0828 0.0094 0.4856 0.126 Uiso 1 1 calc R . . H26C H 0.1234 0.0545 0.4509 0.126 Uiso 1 1 calc R . . C27 C 0.2585(4) -0.3319(8) 0.3536(2) 0.053(2) Uani 1 1 d . . . H27 H 0.2148 -0.3782 0.3518 0.063 Uiso 1 1 calc R . . C28 C 0.3172(5) -0.4240(10) 0.3572(3) 0.079(3) Uani 1 1 d . . . H28A H 0.3604 -0.3823 0.3533 0.118 Uiso 1 1 calc R . . H28B H 0.3109 -0.4885 0.3390 0.118 Uiso 1 1 calc R . . H28C H 0.3176 -0.4601 0.3816 0.118 Uiso 1 1 calc R . . C29 C 0.2666(5) -0.2581(10) 0.3186(2) 0.075(3) Uani 1 1 d . . . H29A H 0.2304 -0.1968 0.3167 0.113 Uiso 1 1 calc R . . H29B H 0.2635 -0.3129 0.2976 0.113 Uiso 1 1 calc R . . H29C H 0.3109 -0.2174 0.3192 0.113 Uiso 1 1 calc R . . C30 C -0.0790(3) -0.1478(7) 0.41747(18) 0.0393(17) Uani 1 1 d . . . C31 C -0.1183(4) -0.2352(8) 0.4379(2) 0.0462(18) Uani 1 1 d . . . C32 C -0.1867(4) -0.2138(8) 0.4420(2) 0.052(2) Uani 1 1 d . . . H32 H -0.2132 -0.2730 0.4542 0.063 Uiso 1 1 calc R . . C33 C -0.2180(4) -0.1091(9) 0.4290(2) 0.055(2) Uani 1 1 d . . . H33 H -0.2657 -0.0989 0.4309 0.067 Uiso 1 1 calc R . . C34 C -0.1792(4) -0.0201(9) 0.4133(2) 0.054(2) Uani 1 1 d . . . H34 H -0.1997 0.0549 0.4062 0.065 Uiso 1 1 calc R . . C35 C -0.1100(3) -0.0385(7) 0.4076(2) 0.0436(18) Uani 1 1 d . . . C36 C -0.0848(4) -0.3454(8) 0.4573(2) 0.050(2) Uani 1 1 d . . . C37 C -0.0295(6) -0.2990(10) 0.4835(3) 0.095(4) Uani 1 1 d . . . H37A H -0.0114 -0.3672 0.4979 0.143 Uiso 1 1 calc R . . H37B H -0.0487 -0.2377 0.4997 0.143 Uiso 1 1 calc R . . H37C H 0.0071 -0.2622 0.4696 0.143 Uiso 1 1 calc R . . C38 C -0.1350(6) -0.4160(11) 0.4799(4) 0.101(4) Uani 1 1 d . . . H38A H -0.1695 -0.4534 0.4639 0.151 Uiso 1 1 calc R . . H38B H -0.1570 -0.3604 0.4969 0.151 Uiso 1 1 calc R . . H38C H -0.1109 -0.4799 0.4937 0.151 Uiso 1 1 calc R . . C39 C -0.0556(6) -0.4363(10) 0.4312(3) 0.083(3) Uani 1 1 d . . . H39A H -0.0412 -0.5095 0.4446 0.125 Uiso 1 1 calc R . . H39B H -0.0163 -0.4001 0.4193 0.125 Uiso 1 1 calc R . . H39C H -0.0902 -0.4583 0.4128 0.125 Uiso 1 1 calc R . . C40 C -0.0724(4) 0.0754(8) 0.3925(2) 0.053(2) Uani 1 1 d . . . C41 C -0.1093(4) 0.1978(8) 0.3985(3) 0.063(2) Uani 1 1 d . . . H41A H -0.0799 0.2652 0.3912 0.095 Uiso 1 1 calc R . . H41B H -0.1200 0.2065 0.4243 0.095 Uiso 1 1 calc R . . H41C H -0.1514 0.1995 0.3838 0.095 Uiso 1 1 calc R . . C42 C -0.0654(4) 0.0625(10) 0.3520(2) 0.065(2) Uani 1 1 d . . . H42A H -0.0349 0.1259 0.3431 0.097 Uiso 1 1 calc R . . H42B H -0.1101 0.0710 0.3400 0.097 Uiso 1 1 calc R . . H42C H -0.0466 -0.0180 0.3465 0.097 Uiso 1 1 calc R . . C43 C -0.0025(4) 0.0956(8) 0.4117(2) 0.054(2) Uani 1 1 d . . . H43A H 0.0259 0.0232 0.4084 0.081 Uiso 1 1 calc R . . H43B H -0.0089 0.1098 0.4377 0.081 Uiso 1 1 calc R . . H43C H 0.0198 0.1666 0.4010 0.081 Uiso 1 1 calc R . . C44 C 0.4176(4) 0.0157(7) 0.32118(18) 0.0414(17) Uani 1 1 d . . . H44A H 0.3687 -0.0005 0.3221 0.062 Uiso 1 1 calc R . . H44B H 0.4427 -0.0609 0.3242 0.062 Uiso 1 1 calc R . . H44C H 0.4283 0.0522 0.2976 0.062 Uiso 1 1 calc R . . C45 C 0.4379(3) 0.1027(6) 0.35138(18) 0.0369(16) Uani 1 1 d . . . C46 C 0.4715(3) 0.0502(6) 0.38116(19) 0.0385(16) Uani 1 1 d . . . H46 H 0.4827 -0.0333 0.3781 0.046 Uiso 1 1 calc R . . C47 C 0.4916(3) 0.1000(7) 0.41508(18) 0.0376(16) Uani 1 1 d . . . C48 C 0.5046(4) 0.0101(7) 0.4461(2) 0.0476(18) Uani 1 1 d . . . H48A H 0.5407 0.0415 0.4623 0.071 Uiso 1 1 calc R . . H48B H 0.5184 -0.0688 0.4361 0.071 Uiso 1 1 calc R . . H48C H 0.4629 -0.0004 0.4599 0.071 Uiso 1 1 calc R . . C49 C 0.3722(3) 0.2585(7) 0.32146(18) 0.0361(15) Uani 1 1 d . . . C50 C 0.3906(4) 0.3298(7) 0.29177(19) 0.0385(16) Uani 1 1 d . . . C51 C 0.3398(4) 0.3679(7) 0.2669(2) 0.0412(16) Uani 1 1 d . . . H51 H 0.3519 0.4145 0.2462 0.049 Uiso 1 1 calc R . . C52 C 0.2730(4) 0.3390(7) 0.2720(2) 0.0445(18) Uani 1 1 d . . . H52 H 0.2391 0.3655 0.2549 0.053 Uiso 1 1 calc R . . C53 C 0.2549(4) 0.2712(7) 0.3019(2) 0.0457(18) Uani 1 1 d . . . H53 H 0.2083 0.2533 0.3055 0.055 Uiso 1 1 calc R . . C54 C 0.3030(3) 0.2287(7) 0.32700(19) 0.0375(16) Uani 1 1 d . . . C55 C 0.2797(4) 0.1581(8) 0.3604(2) 0.0475(19) Uani 1 1 d . . . H55 H 0.3191 0.1092 0.3700 0.057 Uiso 1 1 calc R . . C56 C 0.2589(5) 0.2466(9) 0.3900(2) 0.066(2) Uani 1 1 d . . . H56A H 0.2186 0.2922 0.3818 0.099 Uiso 1 1 calc R . . H56B H 0.2962 0.3036 0.3952 0.099 Uiso 1 1 calc R . . H56C H 0.2485 0.2010 0.4121 0.099 Uiso 1 1 calc R . . C57 C 0.2215(4) 0.0699(9) 0.3513(2) 0.062(2) Uani 1 1 d . . . H57A H 0.2153 0.0139 0.3718 0.093 Uiso 1 1 calc R . . H57B H 0.2323 0.0232 0.3295 0.093 Uiso 1 1 calc R . . H57C H 0.1795 0.1162 0.3469 0.093 Uiso 1 1 calc R . . C58 C 0.4638(3) 0.3657(7) 0.28366(19) 0.0403(16) Uani 1 1 d . . . H58 H 0.4932 0.3378 0.3046 0.048 Uiso 1 1 calc R . . C59 C 0.4718(4) 0.5011(8) 0.2805(2) 0.058(2) Uani 1 1 d . . . H59A H 0.4429 0.5313 0.2604 0.087 Uiso 1 1 calc R . . H59B H 0.5194 0.5206 0.2757 0.087 Uiso 1 1 calc R . . H59C H 0.4585 0.5399 0.3032 0.087 Uiso 1 1 calc R . . C60 C 0.4888(4) 0.3032(9) 0.2497(2) 0.058(2) Uani 1 1 d . . . H60A H 0.4798 0.2155 0.2512 0.087 Uiso 1 1 calc R . . H60B H 0.5378 0.3167 0.2477 0.087 Uiso 1 1 calc R . . H60C H 0.4651 0.3371 0.2283 0.087 Uiso 1 1 calc R . . C61 C 0.5125(3) 0.2621(7) 0.45869(18) 0.0374(16) Uani 1 1 d . . . C62 C 0.4579(3) 0.2806(7) 0.48205(18) 0.0385(16) Uani 1 1 d . . . C63 C 0.4713(4) 0.3215(8) 0.5172(2) 0.055(2) Uani 1 1 d . . . H63 H 0.4347 0.3371 0.5329 0.066 Uiso 1 1 calc R . . C64 C 0.5381(4) 0.3398(8) 0.5297(2) 0.054(2) Uani 1 1 d . . . H64 H 0.5471 0.3640 0.5541 0.064 Uiso 1 1 calc R . . C65 C 0.5904(4) 0.3224(8) 0.5063(2) 0.050(2) Uani 1 1 d . . . H65 H 0.6357 0.3361 0.5148 0.060 Uiso 1 1 calc R . . C66 C 0.5794(3) 0.2853(7) 0.47048(19) 0.0386(16) Uani 1 1 d . . . C67 C 0.6392(3) 0.2716(7) 0.44562(19) 0.0427(17) Uani 1 1 d . . . H67 H 0.6217 0.2857 0.4202 0.051 Uiso 1 1 calc R . . C68 C 0.6689(5) 0.1430(8) 0.4468(3) 0.069(3) Uani 1 1 d . . . H68A H 0.6789 0.1199 0.4721 0.103 Uiso 1 1 calc R . . H68B H 0.7109 0.1410 0.4329 0.103 Uiso 1 1 calc R . . H68C H 0.6360 0.0856 0.4360 0.103 Uiso 1 1 calc R . . C69 C 0.6957(4) 0.3633(8) 0.4526(2) 0.056(2) Uani 1 1 d . . . H69A H 0.6769 0.4460 0.4520 0.084 Uiso 1 1 calc R . . H69B H 0.7299 0.3552 0.4338 0.084 Uiso 1 1 calc R . . H69C H 0.7169 0.3479 0.4765 0.084 Uiso 1 1 calc R . . C70 C 0.3838(4) 0.2596(7) 0.46999(19) 0.0436(17) Uani 1 1 d . . . H70 H 0.3834 0.2249 0.4448 0.052 Uiso 1 1 calc R . . C71 C 0.3492(4) 0.1673(9) 0.4951(2) 0.059(2) Uani 1 1 d . . . H71A H 0.3715 0.0878 0.4930 0.089 Uiso 1 1 calc R . . H71B H 0.3011 0.1597 0.4880 0.089 Uiso 1 1 calc R . . H71C H 0.3531 0.1958 0.5203 0.089 Uiso 1 1 calc R . . C72 C 0.3442(4) 0.3792(9) 0.4690(2) 0.062(2) Uani 1 1 d . . . H72A H 0.3435 0.4142 0.4935 0.092 Uiso 1 1 calc R . . H72B H 0.2975 0.3636 0.4604 0.092 Uiso 1 1 calc R . . H72C H 0.3661 0.4365 0.4525 0.092 Uiso 1 1 calc R . . C73 C 0.6129(3) 0.4498(6) 0.33635(17) 0.0334(15) Uani 1 1 d . . . C74 C 0.6197(3) 0.5790(7) 0.33209(18) 0.0363(15) Uani 1 1 d . . . C75 C 0.6467(3) 0.6215(7) 0.29984(19) 0.0400(16) Uani 1 1 d . . . H75 H 0.6507 0.7071 0.2965 0.048 Uiso 1 1 calc R . . C76 C 0.6678(3) 0.5456(8) 0.27267(18) 0.0433(18) Uani 1 1 d . . . H76 H 0.6822 0.5782 0.2502 0.052 Uiso 1 1 calc R . . C77 C 0.6677(3) 0.4214(8) 0.27849(18) 0.0426(17) Uani 1 1 d . . . H77 H 0.6853 0.3691 0.2604 0.051 Uiso 1 1 calc R . . C78 C 0.6428(3) 0.3706(7) 0.30995(18) 0.0357(15) Uani 1 1 d . . . C79 C 0.6583(3) 0.2350(7) 0.31858(18) 0.0396(16) Uani 1 1 d . . . C80 C 0.6911(4) 0.1674(9) 0.2876(2) 0.061(2) Uani 1 1 d . . . H80A H 0.7332 0.2087 0.2811 0.092 Uiso 1 1 calc R . . H80B H 0.6598 0.1661 0.2664 0.092 Uiso 1 1 calc R . . H80C H 0.7013 0.0835 0.2952 0.092 Uiso 1 1 calc R . . C81 C 0.7088(4) 0.2318(8) 0.3506(2) 0.053(2) Uani 1 1 d . . . H81A H 0.7218 0.1471 0.3557 0.079 Uiso 1 1 calc R . . H81B H 0.6878 0.2674 0.3720 0.079 Uiso 1 1 calc R . . H81C H 0.7494 0.2789 0.3445 0.079 Uiso 1 1 calc R . . C82 C 0.5951(4) 0.1592(7) 0.3286(3) 0.057(2) Uani 1 1 d . . . H82A H 0.5644 0.1526 0.3073 0.085 Uiso 1 1 calc R . . H82B H 0.5714 0.1997 0.3484 0.085 Uiso 1 1 calc R . . H82C H 0.6094 0.0775 0.3364 0.085 Uiso 1 1 calc R . . C83 C 0.6020(4) 0.6729(7) 0.3619(2) 0.0421(17) Uani 1 1 d . . . C84 C 0.5252(4) 0.6885(8) 0.3651(3) 0.066(3) Uani 1 1 d . . . H84A H 0.5040 0.6085 0.3683 0.100 Uiso 1 1 calc R . . H84B H 0.5068 0.7269 0.3429 0.100 Uiso 1 1 calc R . . H84C H 0.5156 0.7402 0.3861 0.100 Uiso 1 1 calc R . . C85 C 0.6306(4) 0.8008(8) 0.3538(2) 0.056(2) Uani 1 1 d . . . H85A H 0.6105 0.8310 0.3308 0.085 Uiso 1 1 calc R . . H85B H 0.6801 0.7960 0.3517 0.085 Uiso 1 1 calc R . . H85C H 0.6194 0.8566 0.3735 0.085 Uiso 1 1 calc R . . C86 C 0.6338(5) 0.6321(8) 0.3980(2) 0.064(2) Uani 1 1 d . . . H86A H 0.6231 0.6916 0.4170 0.096 Uiso 1 1 calc R . . H86B H 0.6832 0.6264 0.3958 0.096 Uiso 1 1 calc R . . H86C H 0.6155 0.5521 0.4046 0.096 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 0.03786(15) 0.03929(17) 0.04026(15) 0.00280(12) 0.00423(10) 0.00189(12) O1 0.033(3) 0.055(4) 0.048(3) 0.009(2) 0.006(2) 0.006(2) N1 0.042(3) 0.043(4) 0.045(3) -0.010(3) -0.003(3) -0.002(3) C1 0.062(5) 0.042(5) 0.059(5) -0.006(4) -0.007(4) -0.009(4) Pb2 0.03413(14) 0.03041(15) 0.03628(14) -0.00055(11) 0.00325(9) 0.00098(11) O2 0.038(2) 0.042(3) 0.038(3) 0.004(2) 0.0008(19) 0.000(2) N2 0.035(3) 0.043(4) 0.037(3) 0.000(3) 0.003(2) -0.002(3) C2 0.037(4) 0.060(6) 0.037(4) 0.003(4) -0.008(3) -0.003(4) N3 0.032(3) 0.035(3) 0.033(3) 0.002(2) -0.003(2) 0.005(2) C3 0.045(4) 0.045(5) 0.039(4) 0.009(3) 0.004(3) 0.000(3) N4 0.037(3) 0.034(3) 0.029(3) 0.000(2) 0.000(2) 0.001(2) C4 0.039(4) 0.043(5) 0.041(4) 0.000(3) 0.003(3) 0.003(3) C5 0.047(4) 0.054(6) 0.055(5) 0.012(4) 0.000(3) 0.005(4) C6 0.046(4) 0.052(5) 0.039(4) -0.007(3) -0.003(3) 0.004(4) C7 0.043(4) 0.055(6) 0.051(4) -0.004(4) -0.004(3) 0.001(4) C8 0.050(5) 0.072(7) 0.061(5) -0.008(5) -0.011(4) 0.008(4) C9 0.068(6) 0.102(9) 0.034(4) -0.006(4) -0.010(4) 0.028(5) C10 0.062(6) 0.107(9) 0.044(5) 0.001(5) 0.001(4) 0.033(5) C11 0.051(5) 0.062(6) 0.042(4) -0.001(4) 0.001(3) 0.014(4) C12 0.049(5) 0.079(7) 0.043(4) 0.010(4) 0.011(3) 0.012(4) C13 0.061(6) 0.088(9) 0.105(8) 0.009(7) 0.020(5) 0.030(6) C14 0.070(7) 0.100(10) 0.090(8) 0.022(7) 0.004(5) 0.012(6) C15 0.046(5) 0.088(8) 0.049(5) 0.001(4) -0.002(4) -0.001(5) C16 0.055(5) 0.107(9) 0.072(6) -0.016(6) 0.006(4) 0.003(6) C17 0.059(6) 0.110(10) 0.080(7) 0.028(6) 0.002(5) -0.021(6) C18 0.027(3) 0.040(4) 0.052(4) 0.006(3) 0.001(3) 0.002(3) C19 0.036(4) 0.041(5) 0.053(4) -0.002(3) 0.008(3) 0.000(3) C20 0.042(4) 0.061(6) 0.069(6) 0.002(5) 0.001(4) -0.007(4) C21 0.043(5) 0.078(7) 0.071(6) 0.002(5) -0.007(4) -0.017(4) C22 0.059(5) 0.053(6) 0.057(5) -0.005(4) -0.011(4) -0.008(4) C23 0.044(4) 0.049(5) 0.048(4) 0.000(3) -0.005(3) 0.007(3) C24 0.052(5) 0.066(6) 0.043(4) -0.007(4) -0.004(3) 0.003(4) C25 0.073(7) 0.128(11) 0.055(6) 0.017(6) 0.008(5) 0.017(6) C26 0.074(6) 0.087(8) 0.090(7) -0.047(6) -0.016(5) 0.028(6) C27 0.047(4) 0.053(5) 0.058(5) -0.011(4) 0.011(4) -0.004(4) C28 0.068(6) 0.065(7) 0.104(8) -0.018(6) 0.018(5) 0.010(5) C29 0.097(8) 0.070(7) 0.058(5) -0.010(5) 0.009(5) -0.010(6) C30 0.040(4) 0.042(5) 0.036(4) 0.001(3) -0.003(3) 0.003(3) C31 0.044(4) 0.045(5) 0.050(4) 0.002(4) 0.008(3) 0.002(3) C32 0.043(4) 0.055(6) 0.059(5) 0.001(4) 0.013(4) -0.005(4) C33 0.033(4) 0.071(7) 0.063(5) -0.003(4) 0.013(3) 0.004(4) C34 0.046(4) 0.067(6) 0.050(5) 0.003(4) 0.006(4) 0.016(4) C35 0.036(4) 0.047(5) 0.047(4) 0.016(3) 0.002(3) 0.001(3) C36 0.044(4) 0.056(6) 0.050(4) 0.009(4) 0.010(3) 0.003(4) C37 0.124(10) 0.068(8) 0.092(8) 0.034(6) -0.041(7) -0.001(7) C38 0.088(8) 0.079(8) 0.137(10) 0.063(8) 0.047(7) 0.023(6) C39 0.125(9) 0.068(7) 0.058(6) 0.018(5) 0.027(6) 0.038(7) C40 0.054(5) 0.054(5) 0.052(5) 0.012(4) 0.002(4) 0.015(4) C41 0.060(5) 0.050(6) 0.079(6) 0.015(5) 0.006(4) 0.009(4) C42 0.063(5) 0.078(7) 0.054(5) 0.012(5) 0.002(4) -0.001(5) C43 0.054(5) 0.050(6) 0.058(5) 0.004(4) 0.004(4) -0.002(4) C44 0.049(4) 0.035(4) 0.040(4) -0.001(3) 0.000(3) 0.004(3) C45 0.038(4) 0.036(5) 0.037(4) -0.004(3) 0.006(3) 0.004(3) C46 0.047(4) 0.010(3) 0.058(4) 0.002(3) 0.003(3) 0.004(3) C47 0.038(4) 0.036(5) 0.039(4) 0.004(3) 0.002(3) 0.000(3) C48 0.058(5) 0.039(5) 0.046(4) 0.005(3) -0.007(3) 0.001(4) C49 0.035(4) 0.033(4) 0.040(4) -0.002(3) -0.002(3) 0.005(3) C50 0.045(4) 0.028(4) 0.042(4) -0.009(3) -0.003(3) 0.000(3) C51 0.045(4) 0.032(4) 0.045(4) 0.001(3) -0.006(3) 0.002(3) C52 0.044(4) 0.042(5) 0.047(4) 0.000(3) -0.007(3) 0.008(3) C53 0.036(4) 0.045(5) 0.056(5) -0.005(4) -0.002(3) -0.003(3) C54 0.032(4) 0.036(4) 0.044(4) -0.001(3) -0.002(3) -0.001(3) C55 0.042(4) 0.051(5) 0.049(4) 0.006(4) 0.000(3) -0.007(3) C56 0.080(6) 0.066(7) 0.054(5) 0.004(4) 0.019(4) -0.005(5) C57 0.063(5) 0.059(6) 0.064(5) 0.017(5) -0.011(4) -0.019(5) C58 0.039(4) 0.042(4) 0.040(4) 0.002(3) -0.005(3) -0.004(3) C59 0.054(5) 0.046(5) 0.072(6) 0.015(4) -0.009(4) -0.009(4) C60 0.046(5) 0.073(7) 0.055(5) -0.013(4) 0.001(4) -0.009(4) C61 0.044(4) 0.030(4) 0.038(4) -0.003(3) 0.003(3) 0.001(3) C62 0.040(4) 0.036(4) 0.040(4) 0.002(3) 0.005(3) -0.004(3) C63 0.056(5) 0.062(6) 0.048(4) -0.015(4) 0.016(4) -0.021(4) C64 0.066(5) 0.059(6) 0.037(4) -0.011(4) 0.002(4) -0.003(4) C65 0.048(4) 0.064(6) 0.038(4) -0.002(4) -0.002(3) -0.011(4) C66 0.039(4) 0.036(4) 0.040(4) 0.002(3) -0.006(3) 0.000(3) C67 0.036(4) 0.053(5) 0.040(4) -0.004(3) 0.004(3) -0.002(3) C68 0.065(6) 0.049(6) 0.092(7) -0.005(5) 0.013(5) 0.001(5) C69 0.049(5) 0.064(6) 0.055(5) 0.001(4) 0.004(4) -0.009(4) C70 0.041(4) 0.049(5) 0.041(4) -0.005(3) 0.005(3) -0.004(3) C71 0.049(5) 0.069(6) 0.060(5) -0.001(4) 0.007(4) -0.019(4) C72 0.047(5) 0.070(7) 0.067(6) -0.013(5) 0.001(4) 0.006(4) C73 0.032(3) 0.032(4) 0.035(3) 0.000(3) -0.005(3) 0.000(3) C74 0.027(3) 0.045(4) 0.036(4) 0.000(3) 0.001(3) -0.003(3) C75 0.037(4) 0.036(4) 0.047(4) 0.011(3) -0.003(3) -0.003(3) C76 0.043(4) 0.056(6) 0.030(4) 0.004(3) 0.001(3) -0.010(4) C77 0.040(4) 0.051(5) 0.037(4) -0.006(3) 0.002(3) -0.003(3) C78 0.024(3) 0.041(4) 0.042(4) -0.001(3) 0.002(3) -0.003(3) C79 0.038(4) 0.044(5) 0.037(4) -0.002(3) 0.003(3) 0.002(3) C80 0.060(5) 0.055(6) 0.068(6) -0.012(4) 0.016(4) 0.006(4) C81 0.048(4) 0.051(5) 0.058(5) 0.000(4) -0.007(4) 0.011(4) C82 0.051(5) 0.032(5) 0.088(6) 0.006(4) 0.010(4) 0.000(4) C83 0.043(4) 0.040(4) 0.044(4) -0.004(3) 0.008(3) -0.003(3) C84 0.061(5) 0.037(5) 0.103(7) -0.009(5) 0.033(5) -0.005(4) C85 0.062(5) 0.049(6) 0.058(5) -0.004(4) 0.004(4) -0.008(4) C86 0.106(7) 0.045(5) 0.042(4) -0.009(4) 0.007(4) -0.005(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 Pb1 O1 2.216(5) . ? Pb1 N2 2.289(6) . ? Pb1 N1 2.303(6) . ? O1 C30 1.327(8) . ? N1 C2 1.328(10) . ? N1 C6 1.465(9) . ? C1 C2 1.485(11) . ? Pb2 O2 2.242(5) . ? Pb2 N4 2.305(5) . ? Pb2 N3 2.316(6) . ? O2 C73 1.361(8) . ? N2 C4 1.326(10) . ? N2 C18 1.467(9) . ? C2 C3 1.431(10) . ? N3 C45 1.337(9) . ? N3 C49 1.441(8) . ? C3 C4 1.398(10) . ? N4 C47 1.349(9) . ? N4 C61 1.439(8) . ? C4 C5 1.525(10) . ? C6 C7 1.405(10) . ? C6 C11 1.411(11) . ? C7 C8 1.415(11) . ? C7 C15 1.510(11) . ? C8 C9 1.354(12) . ? C9 C10 1.382(13) . ? C10 C11 1.382(11) . ? C11 C12 1.531(11) . ? C12 C14 1.522(14) . ? C12 C13 1.526(13) . ? C15 C16 1.519(14) . ? C15 C17 1.549(14) . ? C18 C23 1.400(11) . ? C18 C19 1.409(10) . ? C19 C20 1.395(11) . ? C19 C27 1.520(11) . ? C20 C21 1.376(13) . ? C21 C22 1.388(12) . ? C22 C23 1.402(11) . ? C23 C24 1.507(11) . ? C24 C25 1.540(12) . ? C24 C26 1.562(13) . ? C27 C29 1.532(12) . ? C27 C28 1.537(12) . ? C30 C35 1.388(10) . ? C30 C31 1.452(10) . ? C31 C32 1.377(10) . ? C31 C36 1.545(11) . ? C32 C33 1.383(12) . ? C33 C34 1.373(12) . ? C34 C35 1.399(10) . ? C35 C40 1.561(11) . ? C36 C39 1.506(12) . ? C36 C38 1.518(12) . ? C36 C37 1.523(13) . ? C40 C42 1.507(11) . ? C40 C41 1.544(12) . ? C40 C43 1.546(11) . ? C44 C45 1.510(9) . ? C45 C46 1.390(10) . ? C46 C47 1.409(10) . ? C47 C48 1.525(10) . ? C49 C50 1.397(10) . ? C49 C54 1.419(9) . ? C50 C51 1.404(10) . ? C50 C58 1.530(10) . ? C51 C52 1.369(10) . ? C52 C53 1.382(11) . ? C53 C54 1.387(10) . ? C54 C55 1.531(10) . ? C55 C56 1.521(12) . ? C55 C57 1.530(11) . ? C58 C59 1.498(11) . ? C58 C60 1.516(11) . ? C61 C66 1.399(10) . ? C61 C62 1.406(9) . ? C62 C63 1.387(10) . ? C62 C70 1.533(10) . ? C63 C64 1.396(11) . ? C64 C65 1.370(11) . ? C65 C66 1.389(10) . ? C66 C67 1.515(10) . ? C67 C69 1.517(11) . ? C67 C68 1.527(12) . ? C70 C72 1.526(12) . ? C70 C71 1.538(11) . ? C73 C74 1.432(10) . ? C73 C78 1.438(9) . ? C74 C75 1.391(9) . ? C74 C83 1.550(10) . ? C75 C76 1.371(10) . ? C76 C77 1.378(11) . ? C77 C78 1.383(10) . ? C78 C79 1.549(11) . ? C79 C80 1.515(10) . ? C79 C81 1.523(10) . ? C79 C82 1.549(10) . ? C83 C86 1.521(11) . ? C83 C84 1.529(11) . ? C83 C85 1.543(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 N2 93.31(18) . . ? O1 Pb1 N1 97.9(2) . . ? N2 Pb1 N1 83.6(2) . . ? C30 O1 Pb1 141.6(4) . . ? C2 N1 C6 117.8(6) . . ? C2 N1 Pb1 127.3(5) . . ? C6 N1 Pb1 114.5(5) . . ? O2 Pb2 N4 93.99(18) . . ? O2 Pb2 N3 109.31(18) . . ? N4 Pb2 N3 83.58(19) . . ? C73 O2 Pb2 137.4(4) . . ? C4 N2 C18 118.4(6) . . ? C4 N2 Pb1 125.4(5) . . ? C18 N2 Pb1 115.6(4) . . ? N1 C2 C3 122.8(7) . . ? N1 C2 C1 120.9(6) . . ? C3 C2 C1 116.3(7) . . ? C45 N3 C49 119.1(6) . . ? C45 N3 Pb2 125.0(4) . . ? C49 N3 Pb2 115.9(4) . . ? C4 C3 C2 131.1(7) . . ? C47 N4 C61 120.7(6) . . ? C47 N4 Pb2 125.4(4) . . ? C61 N4 Pb2 112.9(4) . . ? N2 C4 C3 125.6(7) . . ? N2 C4 C5 119.2(7) . . ? C3 C4 C5 115.2(7) . . ? C7 C6 C11 120.9(7) . . ? C7 C6 N1 120.8(7) . . ? C11 C6 N1 118.2(7) . . ? C6 C7 C8 117.9(7) . . ? C6 C7 C15 123.2(7) . . ? C8 C7 C15 118.9(7) . . ? C9 C8 C7 120.6(8) . . ? C8 C9 C10 121.0(8) . . ? C9 C10 C11 121.1(8) . . ? C10 C11 C6 118.2(8) . . ? C10 C11 C12 119.2(7) . . ? C6 C11 C12 122.6(7) . . ? C14 C12 C13 111.1(8) . . ? C14 C12 C11 111.1(7) . . ? C13 C12 C11 110.2(8) . . ? C7 C15 C16 110.7(8) . . ? C7 C15 C17 110.5(8) . . ? C16 C15 C17 111.0(8) . . ? C23 C18 C19 122.0(7) . . ? C23 C18 N2 119.3(6) . . ? C19 C18 N2 118.6(7) . . ? C20 C19 C18 118.0(7) . . ? C20 C19 C27 118.4(7) . . ? C18 C19 C27 123.6(7) . . ? C21 C20 C19 121.1(8) . . ? C20 C21 C22 120.2(8) . . ? C21 C22 C23 121.2(8) . . ? C18 C23 C22 117.5(7) . . ? C18 C23 C24 123.7(7) . . ? C22 C23 C24 118.8(7) . . ? C23 C24 C25 111.2(7) . . ? C23 C24 C26 113.2(8) . . ? C25 C24 C26 107.7(8) . . ? C19 C27 C29 110.5(7) . . ? C19 C27 C28 111.9(7) . . ? C29 C27 C28 109.1(8) . . ? O1 C30 C35 124.0(7) . . ? O1 C30 C31 118.2(6) . . ? C35 C30 C31 117.8(6) . . ? C32 C31 C30 118.6(7) . . ? C32 C31 C36 119.4(7) . . ? C30 C31 C36 121.9(6) . . ? C31 C32 C33 122.1(8) . . ? C34 C33 C32 119.2(7) . . ? C33 C34 C35 120.9(8) . . ? C30 C35 C34 120.7(7) . . ? C30 C35 C40 125.0(6) . . ? C34 C35 C40 114.2(7) . . ? C39 C36 C38 105.9(9) . . ? C39 C36 C37 110.2(9) . . ? C38 C36 C37 106.8(9) . . ? C39 C36 C31 112.9(7) . . ? C38 C36 C31 112.1(7) . . ? C37 C36 C31 108.8(7) . . ? C42 C40 C41 106.0(7) . . ? C42 C40 C43 111.3(7) . . ? C41 C40 C43 103.2(7) . . ? C42 C40 C35 109.3(8) . . ? C41 C40 C35 114.6(7) . . ? C43 C40 C35 112.1(6) . . ? N3 C45 C46 125.0(6) . . ? N3 C45 C44 119.4(6) . . ? C46 C45 C44 115.5(6) . . ? C45 C46 C47 131.0(6) . . ? N4 C47 C46 125.1(6) . . ? N4 C47 C48 118.1(6) . . ? C46 C47 C48 116.8(6) . . ? C50 C49 C54 120.5(6) . . ? C50 C49 N3 120.1(6) . . ? C54 C49 N3 119.3(6) . . ? C49 C50 C51 118.8(7) . . ? C49 C50 C58 123.9(6) . . ? C51 C50 C58 117.2(6) . . ? C52 C51 C50 121.0(7) . . ? C51 C52 C53 119.9(7) . . ? C52 C53 C54 121.8(7) . . ? C53 C54 C49 118.0(7) . . ? C53 C54 C55 119.4(6) . . ? C49 C54 C55 122.5(6) . . ? C56 C55 C57 110.3(7) . . ? C56 C55 C54 110.0(7) . . ? C57 C55 C54 112.4(6) . . ? C59 C58 C60 110.3(7) . . ? C59 C58 C50 111.8(6) . . ? C60 C58 C50 111.7(6) . . ? C66 C61 C62 120.8(6) . . ? C66 C61 N4 120.0(6) . . ? C62 C61 N4 119.3(6) . . ? C63 C62 C61 118.9(6) . . ? C63 C62 C70 118.6(6) . . ? C61 C62 C70 122.5(6) . . ? C62 C63 C64 120.7(7) . . ? C65 C64 C63 119.3(7) . . ? C64 C65 C66 122.1(7) . . ? C65 C66 C61 118.2(7) . . ? C65 C66 C67 119.6(6) . . ? C61 C66 C67 122.3(6) . . ? C66 C67 C69 114.2(6) . . ? C66 C67 C68 112.2(7) . . ? C69 C67 C68 109.1(7) . . ? C72 C70 C62 111.1(7) . . ? C72 C70 C71 110.3(7) . . ? C62 C70 C71 110.9(6) . . ? O2 C73 C74 120.7(6) . . ? O2 C73 C78 120.4(6) . . ? C74 C73 C78 118.8(6) . . ? C75 C74 C73 117.6(7) . . ? C75 C74 C83 118.5(7) . . ? C73 C74 C83 123.8(6) . . ? C76 C75 C74 123.0(7) . . ? C75 C76 C77 119.0(7) . . ? C76 C77 C78 121.9(7) . . ? C77 C78 C73 118.7(7) . . ? C77 C78 C79 119.0(6) . . ? C73 C78 C79 121.5(6) . . ? C80 C79 C81 106.8(6) . . ? C80 C79 C78 113.6(6) . . ? C81 C79 C78 107.6(6) . . ? C80 C79 C82 105.9(7) . . ? C81 C79 C82 108.5(6) . . ? C78 C79 C82 114.1(6) . . ? C86 C83 C84 110.8(7) . . ? C86 C83 C85 107.0(7) . . ? C84 C83 C85 106.1(7) . . ? C86 C83 C74 109.1(6) . . ? C84 C83 C74 111.5(6) . . ? C85 C83 C74 112.1(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.213 _refine_diff_density_min -1.600 _refine_diff_density_rms 0.133 # Attachment '2b.CIF' data_Pb-NTMS2 _database_code_depnum_ccdc_archive 'CCDC 654314' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H66 N3 Pb Si2' _chemical_formula_weight 828.31 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9877(7) _cell_length_b 12.6789(8) _cell_length_c 15.1520(10) _cell_angle_alpha 76.037(2) _cell_angle_beta 89.319(2) _cell_angle_gamma 65.115(2) _cell_volume 2016.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour yellow _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.364 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 4.270 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2800 _exptl_absorpt_correction_T_max 0.2800 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12160 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0662 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6989 _reflns_number_gt 5838 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-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^)+(0.1345P)^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 6989 _refine_ls_number_parameters 414 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0713 _refine_ls_R_factor_gt 0.0586 _refine_ls_wR_factor_ref 0.1809 _refine_ls_wR_factor_gt 0.1674 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 0.73553(3) 0.51735(3) 0.67129(2) 0.03694(16) Uani 1 1 d . . . Si1 Si 0.7004(3) 0.7618(2) 0.77166(19) 0.0420(6) Uani 1 1 d . . . N1 N 0.7478(8) 0.6851(7) 0.6890(5) 0.0393(17) Uani 1 1 d . . . C1 C 0.4758(9) 0.4434(10) 0.8892(8) 0.050(2) Uani 1 1 d . . . H1A H 0.4105 0.5259 0.8764 0.075 Uiso 1 1 calc R . . H1B H 0.4979 0.4106 0.9553 0.075 Uiso 1 1 calc R . . H1C H 0.4461 0.3933 0.8656 0.075 Uiso 1 1 calc R . . Si2 Si 0.7827(3) 0.7522(2) 0.58430(19) 0.0423(6) Uani 1 1 d . . . N2 N 0.5764(7) 0.4996(7) 0.7545(5) 0.0395(17) Uani 1 1 d . . . C2 C 0.5877(9) 0.4442(8) 0.8434(7) 0.041(2) Uani 1 1 d . . . N3 N 0.8594(7) 0.3796(7) 0.8011(5) 0.0363(16) Uani 1 1 d . . . C3 C 0.7003(8) 0.3814(7) 0.9015(6) 0.0358(19) Uani 1 1 d . . . H3 H 0.6904 0.3579 0.9644 0.043 Uiso 1 1 calc R . . C4 C 0.8232(9) 0.3481(8) 0.8825(7) 0.039(2) Uani 1 1 d . . . C5 C 0.9169(9) 0.2616(12) 0.9627(7) 0.055(3) Uani 1 1 d . . . H5A H 0.9865 0.2828 0.9641 0.082 Uiso 1 1 calc R . . H5B H 0.9469 0.1793 0.9563 0.082 Uiso 1 1 calc R . . H5C H 0.8779 0.2668 1.0197 0.082 Uiso 1 1 calc R . . C6 C 0.4679(9) 0.5222(8) 0.6970(7) 0.041(2) Uani 1 1 d . . . C7 C 0.3707(10) 0.6410(9) 0.6702(7) 0.047(2) Uani 1 1 d . . . C8 C 0.2680(10) 0.6566(10) 0.6151(7) 0.050(2) Uani 1 1 d . . . H8 H 0.2002 0.7339 0.5966 0.059 Uiso 1 1 calc R . . C9 C 0.2639(11) 0.5626(12) 0.5875(8) 0.059(3) Uani 1 1 d . . . H9 H 0.1925 0.5769 0.5510 0.070 Uiso 1 1 calc R . . C10 C 0.3590(10) 0.4488(11) 0.6106(8) 0.051(2) Uani 1 1 d . . . H10 H 0.3544 0.3857 0.5898 0.061 Uiso 1 1 calc R . . C11 C 0.4680(11) 0.4270(11) 0.6682(8) 0.055(3) Uani 1 1 d . . . C12 C 0.5727(10) 0.3020(11) 0.6899(10) 0.060(3) Uani 1 1 d . . . H12 H 0.6473 0.3086 0.7117 0.072 Uiso 1 1 calc R . . C13 C 0.5509(17) 0.2125(14) 0.7662(14) 0.103(6) Uani 1 1 d . . . H13A H 0.5261 0.2467 0.8187 0.154 Uiso 1 1 calc R . . H13B H 0.6272 0.1379 0.7846 0.154 Uiso 1 1 calc R . . H13C H 0.4853 0.1951 0.7446 0.154 Uiso 1 1 calc R . . C14 C 0.6044(19) 0.2532(19) 0.6059(14) 0.107(6) Uani 1 1 d . . . H14A H 0.5382 0.2347 0.5872 0.160 Uiso 1 1 calc R . . H14B H 0.6822 0.1798 0.6205 0.160 Uiso 1 1 calc R . . H14C H 0.6133 0.3137 0.5559 0.160 Uiso 1 1 calc R . . C15 C 0.3712(10) 0.7456(9) 0.6969(8) 0.051(2) Uani 1 1 d . . . H15 H 0.4587 0.7253 0.7165 0.061 Uiso 1 1 calc R . . C16 C 0.3233(12) 0.8612(11) 0.6164(10) 0.063(3) Uani 1 1 d . . . H16A H 0.3489 0.8393 0.5592 0.095 Uiso 1 1 calc R . . H16B H 0.3578 0.9152 0.6271 0.095 Uiso 1 1 calc R . . H16C H 0.2329 0.9020 0.6122 0.095 Uiso 1 1 calc R . . C17 C 0.2954(17) 0.7744(13) 0.7772(10) 0.083(4) Uani 1 1 d . . . H17A H 0.3079 0.8369 0.7972 0.124 Uiso 1 1 calc R . . H17B H 0.3222 0.7016 0.8279 0.124 Uiso 1 1 calc R . . H17C H 0.2075 0.8032 0.7578 0.124 Uiso 1 1 calc R . . C18 C 0.9888(9) 0.3145(9) 0.7846(7) 0.045(2) Uani 1 1 d . . . C19 C 1.0177(9) 0.2162(9) 0.7473(8) 0.047(2) Uani 1 1 d . . . C20 C 1.1401(11) 0.1587(10) 0.7293(9) 0.056(3) Uani 1 1 d . . . H20 H 1.1624 0.0907 0.7054 0.067 Uiso 1 1 calc R . . C21 C 1.2289(9) 0.1936(12) 0.7439(9) 0.063(3) Uani 1 1 d . . . H21 H 1.3110 0.1521 0.7298 0.075 Uiso 1 1 calc R . . C22 C 1.1959(9) 0.2926(10) 0.7802(7) 0.049(2) Uani 1 1 d . . . H22 H 1.2574 0.3176 0.7919 0.059 Uiso 1 1 calc R . . C23 C 1.0778(9) 0.3551(9) 0.7996(7) 0.044(2) Uani 1 1 d . . . C24 C 1.0524(10) 0.4615(10) 0.8391(7) 0.047(2) Uani 1 1 d . . . H24 H 0.9625 0.4992 0.8474 0.056 Uiso 1 1 calc R . . C25 C 1.0841(12) 0.5583(11) 0.7752(9) 0.060(3) Uani 1 1 d . . . H25A H 1.1693 0.5207 0.7601 0.090 Uiso 1 1 calc R . . H25B H 1.0755 0.6204 0.8062 0.090 Uiso 1 1 calc R . . H25C H 1.0275 0.5951 0.7190 0.090 Uiso 1 1 calc R . . C26 C 1.1266(13) 0.4210(13) 0.9325(9) 0.067(3) Uani 1 1 d . . . H26A H 1.2134 0.4022 0.9240 0.100 Uiso 1 1 calc R . . H26B H 1.1206 0.3491 0.9698 0.100 Uiso 1 1 calc R . . H26C H 1.0931 0.4857 0.9635 0.100 Uiso 1 1 calc R . . C27 C 0.9278(10) 0.1684(10) 0.7267(10) 0.061(3) Uani 1 1 d . . . H27 H 0.8421 0.2321 0.7252 0.074 Uiso 1 1 calc R . . C28 C 0.9407(16) 0.1373(17) 0.6339(12) 0.088(5) Uani 1 1 d . . . H28A H 0.9368 0.2067 0.5860 0.132 Uiso 1 1 calc R . . H28B H 0.8734 0.1174 0.6201 0.132 Uiso 1 1 calc R . . H28C H 1.0203 0.0682 0.6364 0.132 Uiso 1 1 calc R . . C29 C 0.944(2) 0.0562(19) 0.8036(13) 0.107(7) Uani 1 1 d . . . H29A H 0.8796 0.0313 0.7933 0.160 Uiso 1 1 calc R . . H29B H 0.9385 0.0757 0.8627 0.160 Uiso 1 1 calc R . . H29C H 1.0256 -0.0095 0.8035 0.160 Uiso 1 1 calc R . . C30 C 0.6484(10) 0.6789(9) 0.8705(7) 0.046(2) Uani 1 1 d . . . H30A H 0.5745 0.6731 0.8499 0.069 Uiso 1 1 calc R . . H30B H 0.6290 0.7224 0.9182 0.069 Uiso 1 1 calc R . . H30C H 0.7144 0.5978 0.8952 0.069 Uiso 1 1 calc R . . C31 C 0.8259(10) 0.7882(12) 0.8256(8) 0.054(3) Uani 1 1 d . . . H31A H 0.8898 0.7110 0.8612 0.081 Uiso 1 1 calc R . . H31B H 0.7896 0.8413 0.8658 0.081 Uiso 1 1 calc R . . H31C H 0.8629 0.8259 0.7774 0.081 Uiso 1 1 calc R . . C32 C 0.5698(12) 0.9153(10) 0.7262(9) 0.056(3) Uani 1 1 d . . . H32A H 0.5938 0.9603 0.6733 0.084 Uiso 1 1 calc R . . H32B H 0.5511 0.9587 0.7740 0.084 Uiso 1 1 calc R . . H32C H 0.4965 0.9071 0.7076 0.084 Uiso 1 1 calc R . . C33 C 0.8541(13) 0.8571(11) 0.5917(10) 0.063(3) Uani 1 1 d . . . H33A H 0.7941 0.9261 0.6112 0.094 Uiso 1 1 calc R . . H33B H 0.8776 0.8855 0.5316 0.094 Uiso 1 1 calc R . . H33C H 0.9276 0.8143 0.6361 0.094 Uiso 1 1 calc R . . C34 C 0.6432(11) 0.8377(12) 0.4998(9) 0.061(3) Uani 1 1 d . . . H34A H 0.5988 0.7880 0.4999 0.092 Uiso 1 1 calc R . . H34B H 0.6683 0.8586 0.4387 0.092 Uiso 1 1 calc R . . H34C H 0.5888 0.9116 0.5164 0.092 Uiso 1 1 calc R . . C35 C 0.8958(9) 0.6377(10) 0.5300(8) 0.048(2) Uani 1 1 d . . . H35A H 0.9620 0.5762 0.5764 0.072 Uiso 1 1 calc R . . H35B H 0.9313 0.6773 0.4819 0.072 Uiso 1 1 calc R . . H35C H 0.8533 0.5997 0.5034 0.072 Uiso 1 1 calc R . . C36 C 1.2424(15) -0.0177(18) 0.9741(12) 0.088(5) Uani 1 1 d . . . H36A H 1.2234 -0.0148 1.0368 0.132 Uiso 1 1 calc R . . H36B H 1.2187 -0.0757 0.9567 0.132 Uiso 1 1 calc R . . H36C H 1.1962 0.0622 0.9324 0.132 Uiso 1 1 calc R . . C37 C 1.3809(12) -0.0567(13) 0.9684(10) 0.070(3) Uani 1 1 d . . . H37A H 1.4261 -0.1414 1.0044 0.084 Uiso 1 1 calc R . . H37B H 1.3981 -0.0533 0.9040 0.084 Uiso 1 1 calc R . . C38 C 1.4295(12) 0.0189(13) 1.0026(9) 0.067(3) Uani 1 1 d . . . H38A H 1.4121 0.0154 1.0670 0.080 Uiso 1 1 calc R . . H38B H 1.3838 0.1036 0.9666 0.080 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 0.0405(2) 0.0304(2) 0.0407(2) -0.01383(14) 0.00896(14) -0.01363(15) Si1 0.0467(14) 0.0343(13) 0.0457(14) -0.0163(12) 0.0078(11) -0.0150(12) N1 0.052(5) 0.031(4) 0.040(4) -0.012(3) 0.012(3) -0.021(4) C1 0.040(5) 0.044(6) 0.055(6) -0.012(5) 0.015(4) -0.009(4) Si2 0.0454(14) 0.0321(13) 0.0483(15) -0.0124(11) 0.0097(11) -0.0148(11) N2 0.038(4) 0.037(4) 0.038(4) -0.008(3) -0.001(3) -0.012(3) C2 0.039(5) 0.029(4) 0.050(5) -0.019(4) 0.013(4) -0.006(4) N3 0.035(4) 0.030(4) 0.046(4) -0.015(3) 0.013(3) -0.014(3) C3 0.042(5) 0.021(4) 0.043(5) -0.012(4) 0.011(4) -0.010(4) C4 0.049(5) 0.022(4) 0.049(5) -0.011(4) 0.003(4) -0.017(4) C5 0.037(5) 0.067(7) 0.042(5) -0.003(5) 0.000(4) -0.012(5) C6 0.044(5) 0.026(4) 0.046(5) -0.013(4) 0.011(4) -0.008(4) C7 0.052(6) 0.037(5) 0.047(5) -0.007(4) 0.013(4) -0.017(5) C8 0.043(5) 0.041(5) 0.050(6) -0.008(5) 0.010(4) -0.007(4) C9 0.047(6) 0.070(8) 0.058(7) -0.014(6) 0.000(5) -0.025(6) C10 0.050(6) 0.049(6) 0.054(6) -0.015(5) 0.005(5) -0.022(5) C11 0.064(7) 0.050(6) 0.065(7) -0.025(6) 0.034(6) -0.032(6) C12 0.042(6) 0.046(6) 0.095(9) -0.033(6) 0.003(6) -0.015(5) C13 0.094(12) 0.047(8) 0.121(14) 0.003(9) 0.031(10) -0.002(8) C14 0.104(13) 0.111(15) 0.124(15) -0.078(13) 0.055(11) -0.039(11) C15 0.048(6) 0.034(5) 0.063(7) -0.012(5) 0.006(5) -0.011(4) C16 0.063(7) 0.046(6) 0.080(8) -0.015(6) 0.007(6) -0.023(6) C17 0.125(13) 0.051(7) 0.080(9) -0.037(7) 0.034(9) -0.036(8) C18 0.037(5) 0.038(5) 0.047(5) -0.003(4) 0.006(4) -0.008(4) C19 0.039(5) 0.038(5) 0.063(6) -0.021(5) 0.001(4) -0.010(4) C20 0.052(6) 0.034(5) 0.071(7) -0.022(5) 0.004(5) -0.004(5) C21 0.025(5) 0.071(8) 0.085(8) -0.032(7) 0.012(5) -0.007(5) C22 0.037(5) 0.054(6) 0.051(6) -0.008(5) -0.001(4) -0.018(5) C23 0.043(5) 0.040(5) 0.044(5) -0.011(4) 0.006(4) -0.015(4) C24 0.041(5) 0.049(6) 0.048(6) -0.012(5) 0.000(4) -0.018(5) C25 0.061(7) 0.043(6) 0.063(7) -0.009(5) 0.006(5) -0.013(5) C26 0.074(8) 0.060(8) 0.061(7) -0.016(6) 0.002(6) -0.024(7) C27 0.039(5) 0.043(6) 0.108(10) -0.041(6) 0.015(6) -0.012(5) C28 0.085(10) 0.099(12) 0.102(12) -0.036(10) -0.002(9) -0.055(10) C29 0.145(17) 0.118(15) 0.117(14) -0.047(12) 0.049(13) -0.105(15) C30 0.055(6) 0.040(5) 0.045(5) -0.016(4) 0.010(4) -0.020(5) C31 0.052(6) 0.062(7) 0.056(6) -0.026(6) 0.010(5) -0.027(6) C32 0.072(7) 0.035(5) 0.063(7) -0.026(5) 0.014(6) -0.019(5) C33 0.082(9) 0.045(6) 0.074(8) -0.021(6) 0.016(7) -0.036(6) C34 0.051(6) 0.058(7) 0.061(7) -0.023(6) 0.008(5) -0.006(5) C35 0.042(5) 0.041(5) 0.059(6) -0.014(5) 0.018(4) -0.015(4) C36 0.077(9) 0.106(13) 0.086(10) -0.026(10) 0.024(8) -0.045(9) C37 0.063(7) 0.069(8) 0.065(8) -0.021(7) 0.012(6) -0.015(7) C38 0.066(8) 0.067(8) 0.061(7) -0.023(6) 0.015(6) -0.019(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 N1 2.271(8) . ? Pb1 N3 2.314(8) . ? Pb1 N2 2.334(8) . ? Pb1 Si2 3.229(3) . ? Si1 N1 1.715(8) . ? Si1 C30 1.873(10) . ? Si1 C32 1.878(12) . ? Si1 C31 1.905(11) . ? N1 Si2 1.746(8) . ? C1 C2 1.506(14) . ? Si2 C34 1.862(12) . ? Si2 C35 1.875(11) . ? Si2 C33 1.883(12) . ? N2 C2 1.338(13) . ? N2 C6 1.459(13) . ? C2 C3 1.420(13) . ? N3 C4 1.329(13) . ? N3 C18 1.471(12) . ? C3 C4 1.399(14) . ? C4 C5 1.515(13) . ? C6 C11 1.378(16) . ? C6 C7 1.425(14) . ? C7 C8 1.412(16) . ? C7 C15 1.478(16) . ? C8 C9 1.374(18) . ? C9 C10 1.373(17) . ? C10 C11 1.467(17) . ? C11 C12 1.510(16) . ? C12 C13 1.52(2) . ? C12 C14 1.52(2) . ? C15 C17 1.533(18) . ? C15 C16 1.552(16) . ? C18 C19 1.402(15) . ? C18 C23 1.407(15) . ? C19 C20 1.394(16) . ? C19 C27 1.509(15) . ? C20 C21 1.352(18) . ? C21 C22 1.396(18) . ? C22 C23 1.370(15) . ? C23 C24 1.519(15) . ? C24 C26 1.535(16) . ? C24 C25 1.548(16) . ? C27 C28 1.54(2) . ? C27 C29 1.54(2) . ? C36 C37 1.53(2) . ? C37 C38 1.50(2) . ? C38 C38 1.56(3) 2_857 ? 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 N1 Pb1 N3 99.2(3) . . ? N1 Pb1 N2 106.6(3) . . ? N3 Pb1 N2 83.2(3) . . ? N1 Pb1 Si2 31.3(2) . . ? N3 Pb1 Si2 118.37(19) . . ? N2 Pb1 Si2 129.9(2) . . ? N1 Si1 C30 112.3(4) . . ? N1 Si1 C32 112.3(5) . . ? C30 Si1 C32 107.6(5) . . ? N1 Si1 C31 114.2(5) . . ? C30 Si1 C31 104.4(5) . . ? C32 Si1 C31 105.5(6) . . ? Si1 N1 Si2 120.7(5) . . ? Si1 N1 Pb1 131.5(4) . . ? Si2 N1 Pb1 106.3(4) . . ? N1 Si2 C34 111.5(5) . . ? N1 Si2 C35 112.0(4) . . ? C34 Si2 C35 105.3(6) . . ? N1 Si2 C33 114.3(5) . . ? C34 Si2 C33 107.8(6) . . ? C35 Si2 C33 105.4(6) . . ? N1 Si2 Pb1 42.5(3) . . ? C34 Si2 Pb1 98.5(5) . . ? C35 Si2 Pb1 77.9(3) . . ? C33 Si2 Pb1 151.2(4) . . ? C2 N2 C6 118.5(8) . . ? C2 N2 Pb1 125.9(6) . . ? C6 N2 Pb1 113.3(6) . . ? N2 C2 C3 125.3(9) . . ? N2 C2 C1 120.2(9) . . ? C3 C2 C1 114.5(9) . . ? C4 N3 C18 119.4(8) . . ? C4 N3 Pb1 127.0(6) . . ? C18 N3 Pb1 113.2(6) . . ? C4 C3 C2 131.4(9) . . ? N3 C4 C3 125.2(9) . . ? N3 C4 C5 120.7(9) . . ? C3 C4 C5 113.9(9) . . ? C11 C6 C7 123.5(10) . . ? C11 C6 N2 117.4(9) . . ? C7 C6 N2 119.1(9) . . ? C8 C7 C6 116.2(10) . . ? C8 C7 C15 119.4(10) . . ? C6 C7 C15 124.5(10) . . ? C9 C8 C7 121.6(10) . . ? C10 C9 C8 122.5(10) . . ? C9 C10 C11 118.4(11) . . ? C6 C11 C10 117.7(11) . . ? C6 C11 C12 125.1(11) . . ? C10 C11 C12 117.1(10) . . ? C11 C12 C13 113.4(11) . . ? C11 C12 C14 112.5(13) . . ? C13 C12 C14 110.2(14) . . ? C7 C15 C17 113.0(10) . . ? C7 C15 C16 112.6(10) . . ? C17 C15 C16 108.3(10) . . ? C19 C18 C23 121.5(9) . . ? C19 C18 N3 117.4(9) . . ? C23 C18 N3 121.0(10) . . ? C20 C19 C18 116.3(10) . . ? C20 C19 C27 118.6(10) . . ? C18 C19 C27 125.1(10) . . ? C21 C20 C19 124.2(11) . . ? C20 C21 C22 117.6(10) . . ? C23 C22 C21 122.3(10) . . ? C22 C23 C18 118.1(10) . . ? C22 C23 C24 117.7(9) . . ? C18 C23 C24 124.2(9) . . ? C23 C24 C26 111.2(9) . . ? C23 C24 C25 112.2(9) . . ? C26 C24 C25 108.4(10) . . ? C19 C27 C28 112.8(11) . . ? C19 C27 C29 110.1(12) . . ? C28 C27 C29 109.7(13) . . ? C38 C37 C36 113.9(13) . . ? C37 C38 C38 114.9(15) . 2_857 ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 2.837 _refine_diff_density_min -2.401 _refine_diff_density_rms 0.223 # Attachment '2c.CIF' data_Pb-PTMS2 _database_code_depnum_ccdc_archive 'CCDC 654315' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C35 H59 N2 P Pb Si2' _chemical_formula_weight 802.18 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_int_tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5295(3) _cell_length_b 10.2387(3) _cell_length_c 21.1917(6) _cell_angle_alpha 90.1280(10) _cell_angle_beta 90.4550(10) _cell_angle_gamma 109.5890(10) _cell_volume 1947.91(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description rod _exptl_crystal_colour orange _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.368 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 4.457 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2336 _exptl_absorpt_correction_T_max 0.5742 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Siemens SMART CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11779 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0489 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 0.96 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6757 _reflns_number_gt 5862 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-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^)+(0.0895P)^2^+3.6958P] 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 6757 _refine_ls_number_parameters 386 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.1361 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 0.73956(3) 0.69075(3) 0.742647(12) 0.03621(12) Uani 1 1 d . . . P1 P 0.4592(2) 0.6962(2) 0.75856(10) 0.0404(4) Uani 1 1 d . . . Si1 Si 0.3821(2) 0.5094(2) 0.82226(11) 0.0445(5) Uani 1 1 d . . . N1 N 0.8578(6) 0.8582(6) 0.8201(3) 0.0347(12) Uani 1 1 d . . . C1 C 1.0961(9) 1.0187(9) 0.8626(4) 0.0499(19) Uani 1 1 d . . . H1A H 1.0626 1.0945 0.8768 0.075 Uiso 1 1 calc R . . H1B H 1.1989 1.0569 0.8478 0.075 Uiso 1 1 calc R . . H1C H 1.0913 0.9555 0.8978 0.075 Uiso 1 1 calc R . . Si2 Si 0.3182(2) 0.6086(2) 0.67282(11) 0.0456(5) Uani 1 1 d . . . N2 N 0.8473(7) 0.8784(6) 0.6767(3) 0.0365(13) Uani 1 1 d . . . C2 C 0.9951(9) 0.9395(8) 0.8087(4) 0.0430(17) Uani 1 1 d . . . C3 C 1.0611(9) 0.9646(8) 0.7477(4) 0.0430(17) Uani 1 1 d . . . H3 H 1.1669 0.9961 0.7474 0.052 Uiso 1 1 calc R . . C4 C 0.9920(9) 0.9492(8) 0.6884(4) 0.0428(17) Uani 1 1 d . . . C5 C 1.0923(10) 1.0241(10) 0.6353(4) 0.054(2) Uani 1 1 d . . . H5A H 1.0830 0.9601 0.5999 0.081 Uiso 1 1 calc R . . H5B H 1.1959 1.0582 0.6503 0.081 Uiso 1 1 calc R . . H5C H 1.0629 1.1026 0.6215 0.081 Uiso 1 1 calc R . . C6 C 0.8031(8) 0.8480(8) 0.8837(3) 0.0374(15) Uani 1 1 d . . . C7 C 0.7067(9) 0.9207(8) 0.9004(4) 0.0399(16) Uani 1 1 d . . . C8 C 0.6574(10) 0.9108(9) 0.9622(4) 0.0488(19) Uani 1 1 d . . . H8 H 0.5939 0.9606 0.9745 0.059 Uiso 1 1 calc R . . C9 C 0.6977(11) 0.8312(10) 1.0062(4) 0.056(2) Uani 1 1 d . . . H9 H 0.6626 0.8263 1.0483 0.067 Uiso 1 1 calc R . . C10 C 0.7905(9) 0.7578(9) 0.9885(4) 0.0472(19) Uani 1 1 d . . . H10 H 0.8170 0.7017 1.0188 0.057 Uiso 1 1 calc R . . C11 C 0.8455(9) 0.7644(8) 0.9274(4) 0.0416(17) Uani 1 1 d . . . C12 C 0.9420(9) 0.6793(8) 0.9103(4) 0.0439(17) Uani 1 1 d . . . H12 H 0.9866 0.7101 0.8681 0.053 Uiso 1 1 calc R . . C13 C 1.0693(11) 0.6986(13) 0.9582(5) 0.068(3) Uani 1 1 d . . . H13A H 1.0278 0.6604 0.9990 0.102 Uiso 1 1 calc R . . H13B H 1.1257 0.7976 0.9631 0.102 Uiso 1 1 calc R . . H13C H 1.1355 0.6501 0.9431 0.102 Uiso 1 1 calc R . . C14 C 0.8472(11) 0.5254(10) 0.9056(5) 0.059(2) Uani 1 1 d . . . H14A H 0.8040 0.4928 0.9468 0.088 Uiso 1 1 calc R . . H14B H 0.9100 0.4717 0.8924 0.088 Uiso 1 1 calc R . . H14C H 0.7672 0.5134 0.8745 0.088 Uiso 1 1 calc R . . C15 C 0.6623(10) 1.0118(8) 0.8533(4) 0.0466(18) Uani 1 1 d . . . H15 H 0.6664 0.9721 0.8104 0.056 Uiso 1 1 calc R . . C16 C 0.7745(14) 1.1586(10) 0.8537(6) 0.079(3) Uani 1 1 d . . . H16A H 0.7392 1.2171 0.8256 0.118 Uiso 1 1 calc R . . H16B H 0.8711 1.1566 0.8391 0.118 Uiso 1 1 calc R . . H16C H 0.7852 1.1964 0.8967 0.118 Uiso 1 1 calc R . . C17 C 0.5048(11) 1.0130(11) 0.8616(5) 0.060(2) Uani 1 1 d . . . H17A H 0.4358 0.9175 0.8639 0.091 Uiso 1 1 calc R . . H17B H 0.4775 1.0598 0.8256 0.091 Uiso 1 1 calc R . . H17C H 0.4993 1.0624 0.9006 0.091 Uiso 1 1 calc R . . C18 C 0.7873(8) 0.8999(9) 0.6172(4) 0.0427(17) Uani 1 1 d . . . C19 C 0.7277(9) 1.0074(8) 0.6126(4) 0.0433(17) Uani 1 1 d . . . C20 C 0.6783(10) 1.0350(10) 0.5535(4) 0.053(2) Uani 1 1 d . . . H20 H 0.6436 1.1113 0.5489 0.063 Uiso 1 1 calc R . . C21 C 0.6791(9) 0.9519(10) 0.5011(4) 0.053(2) Uani 1 1 d . . . H21 H 0.6443 0.9710 0.4612 0.064 Uiso 1 1 calc R . . C22 C 0.7306(9) 0.8425(9) 0.5080(4) 0.0462(18) Uani 1 1 d . . . H22 H 0.7275 0.7841 0.4727 0.055 Uiso 1 1 calc R . . C23 C 0.7874(8) 0.8147(9) 0.5654(4) 0.0436(17) Uani 1 1 d . . . C24 C 0.8452(10) 0.6918(9) 0.5696(4) 0.0490(19) Uani 1 1 d . . . H24 H 0.8945 0.6966 0.6118 0.059 Uiso 1 1 calc R . . C25 C 0.7212(14) 0.5553(12) 0.5653(6) 0.079(3) Uani 1 1 d . . . H25A H 0.6500 0.5493 0.5992 0.118 Uiso 1 1 calc R . . H25B H 0.7621 0.4798 0.5696 0.118 Uiso 1 1 calc R . . H25C H 0.6705 0.5477 0.5244 0.118 Uiso 1 1 calc R . . C26 C 0.9625(12) 0.6981(12) 0.5187(5) 0.067(3) Uani 1 1 d . . . H26A H 1.0099 0.6288 0.5280 0.100 Uiso 1 1 calc R . . H26B H 1.0382 0.7906 0.5187 0.100 Uiso 1 1 calc R . . H26C H 0.9138 0.6787 0.4772 0.100 Uiso 1 1 calc R . . C27 C 0.7254(10) 1.1014(8) 0.6684(4) 0.0500(19) Uani 1 1 d . . . H27 H 0.7528 1.0582 0.7067 0.060 Uiso 1 1 calc R . . C28 C 0.8406(16) 1.2436(13) 0.6625(8) 0.096(4) Uani 1 1 d . . . H28A H 0.8270 1.2844 0.6221 0.145 Uiso 1 1 calc R . . H28B H 0.9404 1.2361 0.6645 0.145 Uiso 1 1 calc R . . H28C H 0.8292 1.3026 0.6972 0.145 Uiso 1 1 calc R . . C29 C 0.5728(13) 1.1095(13) 0.6799(6) 0.076(3) Uani 1 1 d . . . H29A H 0.5761 1.1672 0.7172 0.115 Uiso 1 1 calc R . . H29B H 0.5022 1.0161 0.6869 0.115 Uiso 1 1 calc R . . H29C H 0.5408 1.1505 0.6431 0.115 Uiso 1 1 calc R . . C30 C 0.4562(12) 0.3655(10) 0.8033(5) 0.065(3) Uani 1 1 d . . . H30A H 0.5621 0.4049 0.7929 0.098 Uiso 1 1 calc R . . H30B H 0.4011 0.3119 0.7672 0.098 Uiso 1 1 calc R . . H30C H 0.4441 0.3046 0.8399 0.098 Uiso 1 1 calc R . . C31 C 0.4418(10) 0.5668(11) 0.9049(5) 0.059(2) Uani 1 1 d . . . H31A H 0.3959 0.6347 0.9183 0.088 Uiso 1 1 calc R . . H31B H 0.5504 0.6092 0.9068 0.088 Uiso 1 1 calc R . . H31C H 0.4102 0.4865 0.9330 0.088 Uiso 1 1 calc R . . C32 C 0.1730(10) 0.4311(10) 0.8242(5) 0.059(2) Uani 1 1 d . . . H32A H 0.1437 0.3640 0.8587 0.089 Uiso 1 1 calc R . . H32B H 0.1364 0.3842 0.7840 0.089 Uiso 1 1 calc R . . H32C H 0.1300 0.5045 0.8310 0.089 Uiso 1 1 calc R . . C33 C 0.3021(12) 0.4259(10) 0.6498(5) 0.063(2) Uani 1 1 d . . . H33A H 0.2417 0.3992 0.6112 0.094 Uiso 1 1 calc R . . H33B H 0.2545 0.3623 0.6839 0.094 Uiso 1 1 calc R . . H33C H 0.4016 0.4212 0.6423 0.094 Uiso 1 1 calc R . . C34 C 0.1267(10) 0.6149(12) 0.6873(5) 0.066(3) Uani 1 1 d . . . H34A H 0.1332 0.7103 0.6973 0.099 Uiso 1 1 calc R . . H34B H 0.0818 0.5544 0.7227 0.099 Uiso 1 1 calc R . . H34C H 0.0649 0.5834 0.6493 0.099 Uiso 1 1 calc R . . C35 C 0.3856(10) 0.7203(12) 0.6025(5) 0.063(2) Uani 1 1 d . . . H35A H 0.4912 0.7338 0.5959 0.094 Uiso 1 1 calc R . . H35B H 0.3730 0.8104 0.6093 0.094 Uiso 1 1 calc R . . H35C H 0.3279 0.6754 0.5651 0.094 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 0.03770(17) 0.03377(17) 0.03568(17) -0.00240(10) -0.00132(10) 0.01008(11) P1 0.0382(10) 0.0356(9) 0.0437(11) -0.0037(8) -0.0036(8) 0.0077(8) Si1 0.0387(11) 0.0424(11) 0.0469(12) 0.0014(9) 0.0021(9) 0.0063(9) N1 0.035(3) 0.038(3) 0.031(3) -0.001(2) -0.003(2) 0.011(3) C1 0.040(4) 0.052(5) 0.048(5) 0.005(4) -0.005(3) 0.003(4) Si2 0.0401(11) 0.0449(12) 0.0483(12) -0.0036(9) -0.0072(9) 0.0097(9) N2 0.040(3) 0.036(3) 0.031(3) 0.000(2) 0.003(2) 0.009(3) C2 0.043(4) 0.043(4) 0.043(4) -0.005(3) -0.010(3) 0.016(3) C3 0.046(4) 0.043(4) 0.034(4) 0.004(3) 0.000(3) 0.006(3) C4 0.039(4) 0.046(4) 0.043(4) -0.004(3) 0.001(3) 0.014(3) C5 0.046(5) 0.059(5) 0.047(5) 0.008(4) 0.003(4) 0.004(4) C6 0.036(4) 0.037(4) 0.035(4) -0.006(3) -0.005(3) 0.006(3) C7 0.044(4) 0.039(4) 0.033(4) -0.006(3) 0.000(3) 0.009(3) C8 0.060(5) 0.049(5) 0.042(4) -0.014(4) 0.003(4) 0.025(4) C9 0.063(5) 0.069(6) 0.033(4) -0.008(4) 0.007(4) 0.017(5) C10 0.051(5) 0.052(5) 0.035(4) 0.009(3) -0.004(3) 0.013(4) C11 0.041(4) 0.040(4) 0.041(4) -0.012(3) -0.004(3) 0.010(3) C12 0.046(4) 0.048(4) 0.041(4) 0.002(3) -0.001(3) 0.020(4) C13 0.061(6) 0.094(8) 0.059(6) 0.010(5) -0.009(5) 0.038(6) C14 0.062(6) 0.052(5) 0.068(6) 0.002(4) 0.005(5) 0.028(4) C15 0.057(5) 0.044(4) 0.045(4) -0.004(3) -0.001(4) 0.025(4) C16 0.093(8) 0.040(5) 0.093(8) 0.006(5) -0.031(7) 0.010(5) C17 0.066(6) 0.069(6) 0.057(6) 0.004(5) 0.008(4) 0.037(5) C18 0.037(4) 0.051(4) 0.039(4) -0.003(3) -0.004(3) 0.012(3) C19 0.041(4) 0.040(4) 0.042(4) 0.007(3) 0.002(3) 0.005(3) C20 0.046(4) 0.066(6) 0.050(5) 0.020(4) 0.005(4) 0.023(4) C21 0.039(4) 0.076(6) 0.041(4) 0.007(4) 0.001(3) 0.014(4) C22 0.047(4) 0.060(5) 0.032(4) -0.001(3) 0.001(3) 0.019(4) C23 0.037(4) 0.055(5) 0.036(4) -0.002(3) 0.000(3) 0.012(3) C24 0.058(5) 0.056(5) 0.037(4) -0.004(4) 0.000(4) 0.025(4) C25 0.084(8) 0.067(7) 0.091(9) 0.021(6) 0.011(6) 0.033(6) C26 0.065(6) 0.082(7) 0.063(6) -0.010(5) -0.004(5) 0.038(6) C27 0.058(5) 0.039(4) 0.049(5) -0.002(3) -0.002(4) 0.012(4) C28 0.094(9) 0.061(7) 0.124(12) -0.018(7) 0.009(8) 0.013(7) C29 0.074(7) 0.089(8) 0.070(7) -0.018(6) -0.002(5) 0.031(6) C30 0.067(6) 0.047(5) 0.078(7) 0.013(5) 0.002(5) 0.016(5) C31 0.046(5) 0.063(6) 0.056(5) 0.007(4) 0.002(4) 0.003(4) C32 0.049(5) 0.055(5) 0.059(6) 0.003(4) 0.000(4) -0.001(4) C33 0.069(6) 0.048(5) 0.064(6) -0.015(4) -0.013(5) 0.009(4) C34 0.045(5) 0.079(7) 0.078(7) 0.006(5) -0.008(5) 0.025(5) C35 0.045(5) 0.084(7) 0.050(5) 0.007(5) -0.002(4) 0.009(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 Pb1 N2 2.325(6) . ? Pb1 N1 2.359(6) . ? Pb1 P1 2.715(2) . ? P1 Si2 2.248(3) . ? P1 Si1 2.260(3) . ? Si1 C31 1.869(10) . ? Si1 C30 1.879(10) . ? Si1 C32 1.883(9) . ? N1 C2 1.318(10) . ? N1 C6 1.441(9) . ? C1 C2 1.532(11) . ? Si2 C35 1.864(10) . ? Si2 C34 1.876(10) . ? Si2 C33 1.889(10) . ? N2 C4 1.346(10) . ? N2 C18 1.428(10) . ? C2 C3 1.427(11) . ? C3 C4 1.398(11) . ? C4 C5 1.516(11) . ? C6 C11 1.408(11) . ? C6 C7 1.409(11) . ? C7 C8 1.389(11) . ? C7 C15 1.518(11) . ? C8 C9 1.374(13) . ? C9 C10 1.392(13) . ? C10 C11 1.394(11) . ? C11 C12 1.509(11) . ? C12 C14 1.533(12) . ? C12 C13 1.536(12) . ? C15 C17 1.517(12) . ? C15 C16 1.524(13) . ? C18 C23 1.400(11) . ? C18 C19 1.401(12) . ? C19 C20 1.397(12) . ? C19 C27 1.527(12) . ? C20 C21 1.400(13) . ? C21 C22 1.373(13) . ? C22 C23 1.397(11) . ? C23 C24 1.536(12) . ? C24 C25 1.499(15) . ? C24 C26 1.545(13) . ? C27 C28 1.507(15) . ? C27 C29 1.506(14) . ? 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 N2 Pb1 N1 81.2(2) . . ? N2 Pb1 P1 103.18(16) . . ? N1 Pb1 P1 97.32(15) . . ? Si2 P1 Si1 99.45(11) . . ? Si2 P1 Pb1 110.25(10) . . ? Si1 P1 Pb1 96.00(9) . . ? C31 Si1 C30 107.0(5) . . ? C31 Si1 C32 105.7(4) . . ? C30 Si1 C32 107.2(5) . . ? C31 Si1 P1 108.5(3) . . ? C30 Si1 P1 115.7(3) . . ? C32 Si1 P1 112.1(3) . . ? C2 N1 C6 119.0(6) . . ? C2 N1 Pb1 117.2(5) . . ? C6 N1 Pb1 121.5(4) . . ? C35 Si2 C34 104.8(5) . . ? C35 Si2 C33 107.4(5) . . ? C34 Si2 C33 108.7(5) . . ? C35 Si2 P1 111.3(3) . . ? C34 Si2 P1 107.9(4) . . ? C33 Si2 P1 116.1(3) . . ? C4 N2 C18 117.5(6) . . ? C4 N2 Pb1 115.4(5) . . ? C18 N2 Pb1 124.9(5) . . ? N1 C2 C3 124.9(7) . . ? N1 C2 C1 120.4(7) . . ? C3 C2 C1 114.7(7) . . ? C4 C3 C2 129.1(8) . . ? N2 C4 C3 125.2(7) . . ? N2 C4 C5 120.0(7) . . ? C3 C4 C5 114.8(7) . . ? C11 C6 C7 121.7(7) . . ? C11 C6 N1 119.3(7) . . ? C7 C6 N1 119.0(7) . . ? C8 C7 C6 117.8(7) . . ? C8 C7 C15 120.6(7) . . ? C6 C7 C15 121.5(7) . . ? C9 C8 C7 122.0(8) . . ? C8 C9 C10 119.3(8) . . ? C9 C10 C11 121.7(8) . . ? C10 C11 C6 117.5(7) . . ? C10 C11 C12 119.4(7) . . ? C6 C11 C12 123.1(7) . . ? C11 C12 C14 110.2(7) . . ? C11 C12 C13 112.0(7) . . ? C14 C12 C13 109.8(8) . . ? C7 C15 C17 113.8(7) . . ? C7 C15 C16 111.1(7) . . ? C17 C15 C16 111.1(8) . . ? C23 C18 C19 121.4(7) . . ? C23 C18 N2 120.6(7) . . ? C19 C18 N2 118.0(7) . . ? C20 C19 C18 118.2(8) . . ? C20 C19 C27 119.1(8) . . ? C18 C19 C27 122.5(7) . . ? C19 C20 C21 121.0(8) . . ? C22 C21 C20 119.2(8) . . ? C21 C22 C23 121.8(8) . . ? C22 C23 C18 118.2(8) . . ? C22 C23 C24 119.0(7) . . ? C18 C23 C24 122.8(7) . . ? C25 C24 C23 112.0(8) . . ? C25 C24 C26 109.6(8) . . ? C23 C24 C26 112.3(7) . . ? C28 C27 C29 111.5(9) . . ? C28 C27 C19 112.3(8) . . ? C29 C27 C19 112.6(8) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.713 _refine_diff_density_min -1.206 _refine_diff_density_rms 0.161 # Attachment '3.CIF' data_block33 _database_code_depnum_ccdc_archive 'CCDC 654316' _audit_creation_method ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C63 H99 N2 P Pb Si2' _chemical_formula_weight 1178.78 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 P21/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 12.4953(2) _cell_length_b 18.9054(3) _cell_length_c 14.3412(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.2604(17) _cell_angle_gamma 90.00 _cell_volume 3198.18(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 14147 _cell_measurement_theta_min 3.1155 _cell_measurement_theta_max 30.1715 _exptl_crystal_description drop _exptl_crystal_colour pink _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1232 _exptl_absorpt_coefficient_mu 2.736 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.3303 _exptl_absorpt_correction_T_max 0.5146 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur S Sapphire' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17579 _diffrn_reflns_av_R_equivalents 0.0205 _diffrn_reflns_av_sigmaI/netI 0.0294 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.13 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5751 _reflns_number_gt 5002 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.10 (release 13-04-2006 CrysAlis171 .NET) (compiled Apr 13 2006,12:24:59) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-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^)+(0.0331P)^2^+0.5054P] 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 5751 _refine_ls_number_parameters 443 _refine_ls_number_restraints 188 _refine_ls_R_factor_all 0.0301 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0616 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.191 _refine_ls_restrained_S_all 1.282 _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 0.670352(14) 0.2500 0.372083(12) 0.02936(7) Uani 1 2 d S . . P1 P 0.68525(9) 0.2500 0.19055(8) 0.0279(2) Uani 1 2 d S B . Si1 Si 0.51168(10) 0.2500 0.11324(8) 0.0232(2) Uani 1 2 d S . . N1 N 0.8178(2) 0.33216(14) 0.44330(18) 0.0320(6) Uani 1 1 d . . . C1 C 0.9963(3) 0.3771(2) 0.5597(3) 0.0624(12) Uani 1 1 d . . . H1A H 0.9797 0.4196 0.5182 0.094 Uiso 1 1 calc R . . H1B H 1.0756 0.3635 0.5734 0.094 Uiso 1 1 calc R . . H1C H 0.9830 0.3870 0.6221 0.094 Uiso 1 1 calc R . . C2 C 0.9197(3) 0.31731(18) 0.5065(2) 0.0351(8) Uani 1 1 d . . . C3 C 0.9657(4) 0.2500 0.5328(3) 0.0368(11) Uani 1 2 d S . . H3 H 1.0418 0.2500 0.5763 0.055 Uiso 1 2 calc SR . . C4 C 0.7800(3) 0.40413(19) 0.4335(3) 0.0406(9) Uani 1 1 d . . . C5 C 0.7959(3) 0.44746(19) 0.3599(3) 0.0456(9) Uani 1 1 d . . . C6 C 0.7590(3) 0.5175(2) 0.3536(3) 0.0612(12) Uani 1 1 d . . . H6 H 0.7699 0.5477 0.3046 0.092 Uiso 1 1 calc R . . C7 C 0.7065(4) 0.5434(3) 0.4184(4) 0.0745(15) Uani 1 1 d . . . H7 H 0.6817 0.5912 0.4134 0.112 Uiso 1 1 calc R . . C8 C 0.6906(4) 0.5001(3) 0.4894(4) 0.0705(14) Uani 1 1 d . . . H8 H 0.6551 0.5187 0.5333 0.106 Uiso 1 1 calc R . . C9 C 0.7250(3) 0.4297(2) 0.4988(3) 0.0546(11) Uani 1 1 d . . . C10 C 0.8520(3) 0.4201(2) 0.2875(3) 0.0496(9) Uani 1 1 d . . . H10 H 0.8544 0.3673 0.2923 0.074 Uiso 1 1 calc R . . C11 C 0.7837(5) 0.4393(3) 0.1822(4) 0.0836(15) Uani 1 1 d . . . H11A H 0.7057 0.4224 0.1672 0.125 Uiso 1 1 calc R . . H11B H 0.8177 0.4172 0.1369 0.125 Uiso 1 1 calc R . . H11C H 0.7834 0.4908 0.1743 0.125 Uiso 1 1 calc R . . C12 C 0.9719(4) 0.4458(4) 0.3098(5) 0.108(2) Uani 1 1 d . . . H12A H 0.9718 0.4973 0.3022 0.162 Uiso 1 1 calc R . . H12B H 1.0053 0.4237 0.2641 0.162 Uiso 1 1 calc R . . H12C H 1.0165 0.4331 0.3778 0.162 Uiso 1 1 calc R . . C13 C 0.7045(3) 0.3834(3) 0.5774(3) 0.0633(12) Uani 1 1 d . . . H13 H 0.7395 0.3362 0.5751 0.095 Uiso 1 1 calc R . . C14 C 0.5772(4) 0.3721(3) 0.5580(4) 0.0889(18) Uani 1 1 d . . . H14A H 0.5430 0.4165 0.5696 0.133 Uiso 1 1 calc R . . H14B H 0.5667 0.3355 0.6026 0.133 Uiso 1 1 calc R . . H14C H 0.5407 0.3571 0.4893 0.133 Uiso 1 1 calc R . . C15 C 0.7598(5) 0.4141(4) 0.6816(4) 0.108(2) Uani 1 1 d . . . H15A H 0.8413 0.4200 0.6946 0.161 Uiso 1 1 calc R . . H15B H 0.7475 0.3817 0.7305 0.161 Uiso 1 1 calc R . . H15C H 0.7257 0.4601 0.6862 0.161 Uiso 1 1 calc R . . C16 C 0.4055(3) 0.2500 0.1820(3) 0.0275(9) Uani 1 2 d S . . C17 C 0.3698(3) 0.31428(19) 0.2123(2) 0.0366(8) Uani 1 1 d . . . C18 C 0.3052(3) 0.3124(3) 0.2749(3) 0.0563(11) Uani 1 1 d . A . H18 H 0.2825 0.3558 0.2960 0.085 Uiso 1 1 calc R . . C19 C 0.2731(5) 0.2500 0.3071(4) 0.070(2) Uani 1 2 d S . . C20 C 0.3990(3) 0.38491(19) 0.1787(3) 0.0442(9) Uani 1 1 d . B . H20 H 0.4350 0.3755 0.1272 0.066 Uiso 1 1 calc R . . C21 C 0.4849(3) 0.4262(2) 0.2617(3) 0.0609(11) Uani 1 1 d . . . H21A H 0.4528 0.4359 0.3142 0.091 Uiso 1 1 calc R B . H21B H 0.5027 0.4709 0.2356 0.091 Uiso 1 1 calc R . . H21C H 0.5543 0.3982 0.2885 0.091 Uiso 1 1 calc R . . C22 C 0.2942(4) 0.4316(2) 0.1305(3) 0.0700(13) Uani 1 1 d . . . H22A H 0.2398 0.4056 0.0761 0.105 Uiso 1 1 calc R B . H22B H 0.3174 0.4749 0.1049 0.105 Uiso 1 1 calc R . . H22C H 0.2585 0.4439 0.1798 0.105 Uiso 1 1 calc R . . C23 C 0.2029(7) 0.2685(5) 0.3774(6) 0.058(4) Uani 0.50 1 d P A -1 H23 H 0.2071 0.3211 0.3729 0.087 Uiso 0.50 1 calc PR A -1 C24 C 0.2635(9) 0.2625(15) 0.4736(7) 0.098(8) Uani 0.50 1 d P A -1 H24A H 0.2122 0.2551 0.5117 0.148 Uiso 0.50 1 calc PR A -1 H24B H 0.3074 0.3058 0.4961 0.148 Uiso 0.50 1 calc PR A -1 H24C H 0.3153 0.2221 0.4832 0.148 Uiso 0.50 1 calc PR A -1 C25 C 0.0877(8) 0.2618(16) 0.3299(7) 0.101(8) Uani 0.50 1 d P A -1 H25A H 0.0520 0.2428 0.3760 0.152 Uiso 0.50 1 calc PR A -1 H25B H 0.0740 0.2296 0.2736 0.152 Uiso 0.50 1 calc PR A -1 H25C H 0.0553 0.3083 0.3064 0.152 Uiso 0.50 1 calc PR A -1 Si2 Si 0.45464(14) 0.2531(7) -0.06476(11) 0.0365(8) Uani 0.50 1 d PD B -2 C26 C 0.2902(5) 0.2533(10) -0.1198(4) 0.0568(16) Uani 0.50 1 d PDU B -2 C27 C 0.2439(7) 0.2672(7) -0.2312(5) 0.069(4) Uani 0.50 1 d PDU B -2 H27A H 0.1615 0.2609 -0.2549 0.104 Uiso 0.50 1 calc PR B -2 H27B H 0.2784 0.2338 -0.2653 0.104 Uiso 0.50 1 calc PR B -2 H27C H 0.2623 0.3157 -0.2446 0.104 Uiso 0.50 1 calc PR B -2 C28 C 0.2453(9) 0.3274(6) -0.1080(7) 0.070(3) Uani 0.50 1 d PDU B -2 H28A H 0.2659 0.3608 -0.1515 0.106 Uiso 0.50 1 calc PR B -2 H28B H 0.2787 0.3430 -0.0393 0.106 Uiso 0.50 1 calc PR B -2 H28C H 0.1626 0.3258 -0.1256 0.106 Uiso 0.50 1 calc PR B -2 C28A C 0.2362(8) 0.2024(6) -0.0646(7) 0.068(3) Uani 0.50 1 d PDU B -2 H28D H 0.1538 0.2020 -0.0969 0.103 Uiso 0.50 1 calc PR B -2 H28E H 0.2542 0.2181 0.0040 0.103 Uiso 0.50 1 calc PR B -2 H28F H 0.2662 0.1546 -0.0658 0.103 Uiso 0.50 1 calc PR B -2 C29 C 0.5222(11) 0.3365(6) -0.0997(9) 0.045(4) Uani 0.50 1 d PDU B -2 C30 C 0.5089(9) 0.4009(5) -0.0392(7) 0.057(2) Uani 0.50 1 d PDU B -2 H30A H 0.5356 0.4434 -0.0639 0.085 Uiso 0.50 1 calc PR B -2 H30B H 0.5537 0.3937 0.0304 0.085 Uiso 0.50 1 calc PR B -2 H30C H 0.4288 0.4067 -0.0456 0.085 Uiso 0.50 1 calc PR B -2 C31 C 0.6521(9) 0.3278(7) -0.0750(7) 0.057(3) Uani 0.50 1 d PDU B -2 H31A H 0.6851 0.3730 -0.0852 0.085 Uiso 0.50 1 calc PR B -2 H31B H 0.6671 0.2918 -0.1183 0.085 Uiso 0.50 1 calc PR B -2 H31C H 0.6861 0.3131 -0.0060 0.085 Uiso 0.50 1 calc PR B -2 C32 C 0.4701(13) 0.3539(9) -0.2115(8) 0.070(3) Uani 0.50 1 d PDU B -2 H32A H 0.3878 0.3592 -0.2290 0.105 Uiso 0.50 1 calc PR B -2 H32B H 0.4869 0.3155 -0.2504 0.105 Uiso 0.50 1 calc PR B -2 H32C H 0.5027 0.3982 -0.2256 0.105 Uiso 0.50 1 calc PR B -2 C29A C 0.5123(12) 0.1670(8) -0.1037(10) 0.062(5) Uani 0.50 1 d PDU B -2 C30A C 0.4430(11) 0.1011(6) -0.0950(8) 0.078(3) Uani 0.50 1 d PDU B -2 H30D H 0.4735 0.0593 -0.1180 0.118 Uiso 0.50 1 calc PR B -2 H30E H 0.3635 0.1077 -0.1357 0.118 Uiso 0.50 1 calc PR B -2 H30F H 0.4481 0.0944 -0.0259 0.118 Uiso 0.50 1 calc PR B -2 C31A C 0.6360(10) 0.1520(7) -0.0387(8) 0.068(3) Uani 0.50 1 d PDU B -2 H31D H 0.6646 0.1109 -0.0648 0.102 Uiso 0.50 1 calc PR B -2 H31E H 0.6387 0.1423 0.0292 0.102 Uiso 0.50 1 calc PR B -2 H31F H 0.6831 0.1933 -0.0392 0.102 Uiso 0.50 1 calc PR B -2 C32A C 0.5135(12) 0.1706(8) -0.2128(8) 0.070(3) Uani 0.50 1 d PDU B -2 H32D H 0.5672 0.2071 -0.2177 0.105 Uiso 0.50 1 calc PR B -2 H32E H 0.4374 0.1824 -0.2574 0.105 Uiso 0.50 1 calc PR B -2 H32F H 0.5367 0.1247 -0.2314 0.105 Uiso 0.50 1 calc PR B -2 C33 C 0.9649(11) 0.3948(12) -0.0239(13) 0.380(14) Uani 0.50 1 d PDU C -3 C34 C 0.9875(13) 0.3563(12) 0.0578(12) 0.393(14) Uani 0.50 1 d PDU C -3 H34 H 1.0114 0.3804 0.1194 0.589 Uiso 0.50 1 calc PR C -3 C35 C 0.9790(13) 0.2873(13) 0.0589(12) 0.384(14) Uani 0.50 1 d PDU C -3 H35 H 0.9917 0.2654 0.1213 0.576 Uiso 0.50 1 calc PR C -3 C36 C 0.9543(10) 0.2458(13) -0.0187(12) 0.341(14) Uani 0.50 1 d PDU C -3 H36 H 0.9522 0.1956 -0.0161 0.511 Uiso 0.50 1 calc PR C -3 C37 C 0.9319(15) 0.2845(13) -0.1040(12) 0.436(15) Uani 0.50 1 d PDU C -3 H37 H 0.9103 0.2598 -0.1651 0.654 Uiso 0.50 1 calc PR C -3 C38 C 0.9389(15) 0.3551(12) -0.1058(12) 0.436(15) Uani 0.50 1 d PDU C -3 H38 H 0.9248 0.3780 -0.1677 0.654 Uiso 0.50 1 calc PR C -3 C39 C 0.9750(14) 0.4594(12) -0.0226(14) 0.382(15) Uani 0.50 1 d PDU C -3 H39A H 0.9552 0.4771 -0.0904 0.572 Uiso 0.50 1 calc PR C -3 H39B H 1.0537 0.4722 0.0144 0.572 Uiso 0.50 1 calc PR C -3 H39C H 0.9244 0.4806 0.0094 0.572 Uiso 0.50 1 calc PR C -3 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 0.02178(10) 0.04337(12) 0.02235(10) 0.000 0.00647(6) 0.000 P1 0.0237(6) 0.0350(7) 0.0254(6) 0.000 0.0087(5) 0.000 Si1 0.0240(6) 0.0262(6) 0.0192(6) 0.000 0.0070(5) 0.000 N1 0.0274(14) 0.0383(16) 0.0281(14) -0.0082(12) 0.0060(12) 0.0007(12) C1 0.040(2) 0.059(3) 0.067(3) -0.023(2) -0.013(2) -0.0014(19) C2 0.0278(18) 0.046(2) 0.0290(17) -0.0085(15) 0.0067(14) -0.0020(15) C3 0.021(2) 0.052(3) 0.032(3) 0.000 0.0015(19) 0.000 C4 0.0292(18) 0.042(2) 0.041(2) -0.0159(17) -0.0015(15) 0.0034(15) C5 0.034(2) 0.039(2) 0.049(2) -0.0121(17) -0.0056(16) -0.0011(16) C6 0.045(2) 0.045(2) 0.074(3) -0.007(2) -0.007(2) -0.0008(19) C7 0.056(3) 0.052(3) 0.094(4) -0.028(3) -0.004(3) 0.019(2) C8 0.056(3) 0.067(3) 0.079(3) -0.028(3) 0.009(2) 0.021(2) C9 0.038(2) 0.062(3) 0.055(3) -0.025(2) 0.0030(18) 0.0127(19) C10 0.055(2) 0.041(2) 0.050(2) -0.0071(18) 0.0125(19) -0.0122(18) C11 0.098(4) 0.089(4) 0.064(3) 0.015(3) 0.026(3) -0.009(3) C12 0.058(3) 0.153(6) 0.118(5) -0.075(4) 0.035(3) -0.023(4) C13 0.053(3) 0.097(4) 0.041(2) -0.021(2) 0.016(2) 0.016(2) C14 0.064(3) 0.147(5) 0.064(3) -0.015(3) 0.032(3) 0.014(3) C15 0.106(5) 0.151(6) 0.057(3) -0.036(4) 0.016(3) 0.010(4) C16 0.020(2) 0.040(3) 0.021(2) 0.000 0.0048(17) 0.000 C17 0.0290(17) 0.049(2) 0.0294(18) -0.0045(15) 0.0071(14) 0.0087(16) C18 0.041(2) 0.089(3) 0.044(2) -0.014(2) 0.0219(19) 0.014(2) C19 0.038(3) 0.143(7) 0.038(3) 0.000 0.023(3) 0.000 C20 0.041(2) 0.042(2) 0.045(2) -0.0086(17) 0.0073(17) 0.0133(16) C21 0.046(2) 0.056(3) 0.066(3) -0.013(2) 0.000(2) 0.007(2) C22 0.059(3) 0.054(3) 0.073(3) -0.017(2) -0.010(2) 0.023(2) C23 0.063(5) 0.072(11) 0.059(5) 0.009(4) 0.048(4) 0.002(4) C24 0.129(9) 0.12(2) 0.085(7) -0.056(12) 0.087(7) -0.066(14) C25 0.081(6) 0.15(2) 0.107(7) 0.070(13) 0.074(6) 0.062(13) Si2 0.0380(8) 0.051(2) 0.0194(7) -0.007(3) 0.0079(6) 0.015(3) C26 0.039(3) 0.100(5) 0.023(3) -0.008(9) -0.002(2) -0.005(9) C27 0.058(5) 0.100(14) 0.034(3) 0.007(4) -0.006(3) 0.004(5) C28 0.048(6) 0.124(7) 0.033(5) 0.009(5) 0.004(4) 0.028(6) C28A 0.035(5) 0.128(8) 0.033(5) -0.003(5) -0.001(4) -0.018(5) C29 0.062(6) 0.049(8) 0.034(6) 0.020(6) 0.027(7) 0.007(7) C30 0.083(7) 0.046(5) 0.048(5) 0.015(4) 0.031(5) 0.001(4) C31 0.066(5) 0.078(7) 0.040(5) 0.014(5) 0.035(4) -0.005(5) C32 0.094(8) 0.088(10) 0.037(4) 0.029(5) 0.033(5) 0.020(7) C29A 0.070(7) 0.077(11) 0.036(6) -0.017(8) 0.013(7) 0.002(7) C30A 0.109(8) 0.078(7) 0.052(6) -0.033(5) 0.031(6) -0.013(6) C31A 0.075(6) 0.085(9) 0.048(5) -0.018(6) 0.027(5) 0.030(5) C32A 0.086(10) 0.083(10) 0.044(5) -0.023(5) 0.025(5) 0.012(7) C33 0.067(10) 0.87(4) 0.222(14) -0.068(16) 0.078(13) 0.016(19) C34 0.107(12) 0.81(4) 0.245(13) -0.069(16) 0.041(14) 0.01(2) C35 0.114(11) 0.80(4) 0.210(11) -0.130(17) 0.020(12) 0.02(2) C36 0.049(7) 0.87(4) 0.112(10) -0.099(17) 0.045(8) -0.02(2) C37 0.214(14) 0.85(4) 0.215(11) -0.030(18) 0.026(14) -0.03(2) C38 0.185(15) 0.84(4) 0.248(14) -0.076(17) 0.029(16) -0.01(2) C39 0.110(19) 0.84(4) 0.131(16) -0.041(17) -0.047(13) 0.16(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 N1 2.368(3) . ? Pb1 N1 2.368(3) 4_565 ? Pb1 P1 2.6706(11) . ? P1 Si1 2.0849(16) . ? Si1 C16 1.897(4) . ? Si1 Si2 2.4140(19) 4_565 ? Si1 Si2 2.4140(19) . ? N1 C2 1.327(4) . ? N1 C4 1.432(4) . ? C1 C2 1.515(5) . ? C2 C3 1.396(4) . ? C3 C2 1.396(4) 4_565 ? C4 C5 1.400(5) . ? C4 C9 1.417(5) . ? C5 C6 1.394(5) . ? C5 C10 1.523(5) . ? C6 C7 1.391(6) . ? C7 C8 1.372(7) . ? C8 C9 1.393(6) . ? C9 C13 1.514(6) . ? C10 C12 1.505(6) . ? C10 C11 1.514(6) . ? C13 C14 1.536(6) . ? C13 C15 1.538(6) . ? C16 C17 1.411(4) . ? C16 C17 1.411(4) 4_565 ? C17 C18 1.391(5) . ? C17 C20 1.504(5) . ? C18 C19 1.375(5) . ? C19 C18 1.375(5) 4_565 ? C19 C23 1.578(8) . ? C19 C23 1.578(8) 4_565 ? C20 C21 1.528(5) . ? C20 C22 1.541(5) . ? C23 C24 1.341(12) . ? C23 C25 1.380(13) . ? Si2 C29 1.931(11) . ? Si2 C29A 1.935(12) . ? Si2 C26 1.943(6) . ? C26 C27 1.531(8) . ? C26 C28A 1.536(11) . ? C26 C28 1.540(14) . ? C29 C30 1.536(12) . ? C29 C31 1.551(12) . ? C29 C32 1.553(11) . ? C29A C31A 1.546(12) . ? C29A C30A 1.546(13) . ? C29A C32A 1.572(12) . ? C33 C39 1.228(18) . ? C33 C34 1.329(10) . ? C33 C38 1.341(10) . ? C34 C35 1.310(10) . ? C35 C36 1.313(10) . ? C36 C37 1.372(10) . ? C37 C38 1.339(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 N1 Pb1 N1 81.96(13) . 4_565 ? N1 Pb1 P1 97.23(6) . . ? N1 Pb1 P1 97.23(6) 4_565 . ? Si1 P1 Pb1 97.10(5) . . ? C16 Si1 P1 120.47(14) . . ? C16 Si1 Si2 122.45(14) . 4_565 ? P1 Si1 Si2 117.05(7) . 4_565 ? C16 Si1 Si2 122.45(14) . . ? P1 Si1 Si2 117.05(7) . . ? Si2 Si1 Si2 2.8(6) 4_565 . ? C2 N1 C4 118.7(3) . . ? C2 N1 Pb1 126.2(2) . . ? C4 N1 Pb1 113.32(19) . . ? N1 C2 C3 126.5(3) . . ? N1 C2 C1 119.4(3) . . ? C3 C2 C1 114.2(3) . . ? C2 C3 C2 131.4(4) . 4_565 ? C5 C4 C9 121.3(3) . . ? C5 C4 N1 120.4(3) . . ? C9 C4 N1 118.3(3) . . ? C6 C5 C4 118.6(4) . . ? C6 C5 C10 119.7(4) . . ? C4 C5 C10 121.8(3) . . ? C7 C6 C5 120.7(5) . . ? C8 C7 C6 120.1(4) . . ? C7 C8 C9 121.8(4) . . ? C8 C9 C4 117.6(4) . . ? C8 C9 C13 120.2(4) . . ? C4 C9 C13 122.3(4) . . ? C12 C10 C11 109.2(4) . . ? C12 C10 C5 113.3(3) . . ? C11 C10 C5 111.3(4) . . ? C9 C13 C14 111.4(4) . . ? C9 C13 C15 111.9(4) . . ? C14 C13 C15 109.6(4) . . ? C17 C16 C17 118.9(4) . 4_565 ? C17 C16 Si1 120.41(19) . . ? C17 C16 Si1 120.41(19) 4_565 . ? C18 C17 C16 119.1(3) . . ? C18 C17 C20 118.8(3) . . ? C16 C17 C20 122.1(3) . . ? C19 C18 C17 122.3(4) . . ? C18 C19 C18 118.3(5) . 4_565 ? C18 C19 C23 108.1(4) . . ? C18 C19 C23 133.7(4) 4_565 . ? C18 C19 C23 133.7(4) . 4_565 ? C18 C19 C23 108.1(4) 4_565 4_565 ? C23 C19 C23 25.6(7) . 4_565 ? C17 C20 C21 112.7(3) . . ? C17 C20 C22 113.1(3) . . ? C21 C20 C22 109.4(3) . . ? C24 C23 C25 130.0(7) . . ? C24 C23 C19 113.2(8) . . ? C25 C23 C19 111.9(8) . . ? C29 Si2 C29A 112.0(3) . . ? C29 Si2 C26 112.8(8) . . ? C29A Si2 C26 109.2(8) . . ? C29 Si2 Si1 107.0(5) . . ? C29A Si2 Si1 106.1(6) . . ? C26 Si2 Si1 109.48(17) . . ? C27 C26 C28A 124.5(9) . . ? C27 C26 C28 86.2(10) . . ? C28A C26 C28 106.0(8) . . ? C27 C26 Si2 114.1(5) . . ? C28A C26 Si2 112.0(7) . . ? C28 C26 Si2 109.4(9) . . ? C30 C29 C31 104.8(9) . . ? C30 C29 C32 109.1(9) . . ? C31 C29 C32 108.0(9) . . ? C30 C29 Si2 111.2(8) . . ? C31 C29 Si2 111.6(8) . . ? C32 C29 Si2 111.8(10) . . ? C31A C29A C30A 106.2(11) . . ? C31A C29A C32A 105.8(11) . . ? C30A C29A C32A 107.7(10) . . ? C31A C29A Si2 111.9(9) . . ? C30A C29A Si2 112.6(10) . . ? C32A C29A Si2 112.2(10) . . ? C39 C33 C34 122.7(13) . . ? C39 C33 C38 124.4(13) . . ? C34 C33 C38 112.7(10) . . ? C35 C34 C33 124.2(11) . . ? C34 C35 C36 125.6(11) . . ? C35 C36 C37 111.1(10) . . ? C38 C37 C36 123.6(11) . . ? C37 C38 C33 122.7(11) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.645 _refine_diff_density_min -0.674 _refine_diff_density_rms 0.067