# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email wjzheng@fudan.edu.cn _publ_contact_author_name 'Wenjun Zheng' _publ_author_name 'Wenjun Zheng' # Attachment '- complex5a.cif' data_5a _database_code_depnum_ccdc_archive 'CCDC 823608' #TrackingRef '- complex5a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H80 N4 Pb2 Si2' _chemical_formula_weight 1231.76 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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.444(4) _cell_length_b 18.724(6) _cell_length_c 12.638(4) _cell_angle_alpha 90.00 _cell_angle_beta 116.420(4) _cell_angle_gamma 90.00 _cell_volume 2637.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 926 _cell_measurement_theta_min 3.270 _cell_measurement_theta_max 26.750 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.551 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_absorpt_coefficient_mu 6.457 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3583 _exptl_absorpt_correction_T_max 0.4442 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11715 _diffrn_reflns_av_R_equivalents 0.0350 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5195 _reflns_number_gt 4027 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^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 5195 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0259 _refine_ls_wR_factor_ref 0.0593 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 0.944 _refine_ls_restrained_S_all 0.944 _refine_ls_shift/su_max 0.004 _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 1.007798(14) 0.074020(8) 1.083742(13) 0.03179(6) Uani 1 1 d . . . Si1 Si 0.76044(10) 0.04756(6) 0.88071(10) 0.0302(2) Uani 1 1 d . . . N1 N 0.8158(3) 0.05116(17) 1.0311(3) 0.0301(7) Uani 1 1 d . . . N2 N 0.8989(3) 0.05251(16) 0.8738(3) 0.0270(7) Uani 1 1 d . . . C1 C 0.7560(3) 0.0651(2) 1.1036(3) 0.0291(9) Uani 1 1 d . . . C2 C 0.7129(4) 0.0086(2) 1.1479(3) 0.0329(9) Uani 1 1 d . . . C3 C 0.6583(4) 0.0239(3) 1.2201(4) 0.0418(11) Uani 1 1 d . . . H3A H 0.6277 -0.0135 1.2471 0.050 Uiso 1 1 calc R . . C4 C 0.6481(4) 0.0923(3) 1.2529(4) 0.0507(13) Uani 1 1 d . . . H4A H 0.6125 0.1010 1.3026 0.061 Uiso 1 1 calc R . . C5 C 0.6908(4) 0.1474(3) 1.2119(4) 0.0469(12) Uani 1 1 d . . . H5A H 0.6845 0.1937 1.2351 0.056 Uiso 1 1 calc R . . C6 C 0.7436(4) 0.1362(2) 1.1360(4) 0.0359(10) Uani 1 1 d . . . C7 C 0.7851(4) 0.2008(2) 1.0909(4) 0.0451(11) Uani 1 1 d . . . H7A H 0.8113 0.1838 1.0328 0.054 Uiso 1 1 calc R . . C8 C 0.6825(5) 0.2541(3) 1.0285(5) 0.0642(15) Uani 1 1 d . . . H8A H 0.6166 0.2303 0.9657 0.096 Uiso 1 1 calc R . . H8B H 0.7099 0.2926 0.9966 0.096 Uiso 1 1 calc R . . H8C H 0.6566 0.2727 1.0842 0.096 Uiso 1 1 calc R . . C9 C 0.8922(5) 0.2377(3) 1.1906(6) 0.0735(17) Uani 1 1 d . . . H9A H 0.9560 0.2039 1.2281 0.110 Uiso 1 1 calc R . . H9B H 0.8682 0.2563 1.2477 0.110 Uiso 1 1 calc R . . H9C H 0.9196 0.2762 1.1585 0.110 Uiso 1 1 calc R . . C10 C 0.7243(4) -0.0697(2) 1.1201(4) 0.0383(10) Uani 1 1 d . . . H10A H 0.7650 -0.0713 1.0692 0.046 Uiso 1 1 calc R . . C11 C 0.6022(5) -0.1066(3) 1.0546(5) 0.0653(15) Uani 1 1 d . . . H11A H 0.5543 -0.0811 0.9831 0.098 Uiso 1 1 calc R . . H11B H 0.5618 -0.1072 1.1040 0.098 Uiso 1 1 calc R . . H11C H 0.6140 -0.1548 1.0357 0.098 Uiso 1 1 calc R . . C12 C 0.8005(5) -0.1107(3) 1.2328(4) 0.0573(14) Uani 1 1 d . . . H12A H 0.8771 -0.0878 1.2736 0.086 Uiso 1 1 calc R . . H12B H 0.8119 -0.1588 1.2131 0.086 Uiso 1 1 calc R . . H12C H 0.7607 -0.1116 1.2827 0.086 Uiso 1 1 calc R . . C13 C 0.6573(4) 0.1217(3) 0.7952(4) 0.0522(13) Uani 1 1 d . . . H13A H 0.5843 0.1019 0.7355 0.078 Uiso 1 1 calc R . . H13B H 0.6953 0.1503 0.7585 0.078 Uiso 1 1 calc R . . H13C H 0.6393 0.1509 0.8477 0.078 Uiso 1 1 calc R . . C14 C 0.6718(4) -0.0358(3) 0.8165(4) 0.0450(11) Uani 1 1 d . . . H14A H 0.5960 -0.0235 0.7520 0.067 Uiso 1 1 calc R . . H14B H 0.6583 -0.0604 0.8762 0.067 Uiso 1 1 calc R . . H14C H 0.7156 -0.0663 0.7883 0.067 Uiso 1 1 calc R . . C15 C 0.9010(4) 0.0941(2) 0.7763(3) 0.0323(9) Uani 1 1 d . . . C16 C 0.8666(4) 0.0609(2) 0.6632(4) 0.0404(11) Uani 1 1 d . . . C17 C 0.8675(4) 0.1015(3) 0.5712(4) 0.0508(12) Uani 1 1 d . . . H17A H 0.8472 0.0796 0.4987 0.061 Uiso 1 1 calc R . . C18 C 0.8976(4) 0.1730(3) 0.5839(4) 0.0549(14) Uani 1 1 d . . . H18A H 0.8972 0.1990 0.5210 0.066 Uiso 1 1 calc R . . C19 C 0.9275(4) 0.2045(3) 0.6892(5) 0.0503(13) Uani 1 1 d . . . H19A H 0.9478 0.2527 0.6976 0.060 Uiso 1 1 calc R . . C20 C 0.9293(4) 0.1678(2) 0.7869(4) 0.0379(10) Uani 1 1 d . . . C21 C 0.9644(4) 0.2116(2) 0.9003(4) 0.0427(11) Uani 1 1 d . . . H21A H 0.9386 0.1842 0.9509 0.051 Uiso 1 1 calc R . . C22 C 1.0989(5) 0.2211(3) 0.9686(5) 0.0722(17) Uani 1 1 d . . . H22A H 1.1374 0.1753 0.9825 0.108 Uiso 1 1 calc R . . H22B H 1.1174 0.2438 1.0429 0.108 Uiso 1 1 calc R . . H22C H 1.1272 0.2503 0.9238 0.108 Uiso 1 1 calc R . . C23 C 0.9001(6) 0.2849(3) 0.8779(6) 0.084(2) Uani 1 1 d . . . H23A H 0.9251 0.3097 0.9516 0.125 Uiso 1 1 calc R . . H23B H 0.8149 0.2776 0.8426 0.125 Uiso 1 1 calc R . . H23C H 0.9205 0.3128 0.8257 0.125 Uiso 1 1 calc R . . C24 C 0.8305(5) -0.0167(3) 0.6369(4) 0.0496(12) Uani 1 1 d . . . H24A H 0.8267 -0.0370 0.7066 0.059 Uiso 1 1 calc R . . C25 C 0.9257(7) -0.0581(3) 0.6172(6) 0.0785(19) Uani 1 1 d . . . H25A H 1.0022 -0.0523 0.6846 0.118 Uiso 1 1 calc R . . H25B H 0.9301 -0.0402 0.5480 0.118 Uiso 1 1 calc R . . H25C H 0.9048 -0.1078 0.6066 0.118 Uiso 1 1 calc R . . C26 C 0.7062(5) -0.0245(3) 0.5328(4) 0.0743(18) Uani 1 1 d . . . H26A H 0.6488 0.0016 0.5489 0.111 Uiso 1 1 calc R . . H26B H 0.6842 -0.0741 0.5215 0.111 Uiso 1 1 calc R . . H26C H 0.7077 -0.0060 0.4626 0.111 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 0.03062(9) 0.02646(8) 0.03651(9) -0.00287(8) 0.01331(7) -0.00135(8) Si1 0.0280(6) 0.0309(6) 0.0309(6) 0.0010(5) 0.0124(5) 0.0015(5) N1 0.0309(19) 0.0316(18) 0.0312(17) -0.0018(14) 0.0169(15) -0.0006(14) N2 0.0292(18) 0.0235(16) 0.0300(17) 0.0026(13) 0.0147(15) -0.0028(13) C1 0.025(2) 0.036(2) 0.0257(19) -0.0031(17) 0.0101(16) -0.0002(17) C2 0.028(2) 0.040(2) 0.030(2) 0.0062(18) 0.0116(18) 0.0043(19) C3 0.039(3) 0.056(3) 0.034(2) 0.008(2) 0.019(2) 0.002(2) C4 0.044(3) 0.077(4) 0.037(2) -0.004(2) 0.023(2) 0.011(3) C5 0.050(3) 0.049(3) 0.043(3) -0.012(2) 0.022(2) 0.003(2) C6 0.030(2) 0.040(3) 0.036(2) -0.0038(19) 0.0130(19) 0.0018(19) C7 0.045(3) 0.031(2) 0.061(3) -0.009(2) 0.025(2) 0.002(2) C8 0.076(4) 0.044(3) 0.084(4) 0.007(3) 0.046(3) 0.015(3) C9 0.055(4) 0.058(4) 0.100(5) -0.023(3) 0.027(3) -0.016(3) C10 0.045(3) 0.033(2) 0.042(2) 0.005(2) 0.024(2) 0.000(2) C11 0.060(4) 0.055(3) 0.069(4) 0.000(3) 0.018(3) -0.011(3) C12 0.051(3) 0.057(3) 0.064(3) 0.020(3) 0.025(3) 0.009(3) C13 0.041(3) 0.061(3) 0.054(3) 0.009(3) 0.020(2) 0.014(2) C14 0.031(3) 0.058(3) 0.042(3) -0.005(2) 0.013(2) -0.011(2) C15 0.030(2) 0.035(2) 0.034(2) 0.0065(17) 0.0152(18) 0.0030(18) C16 0.035(3) 0.050(3) 0.034(2) 0.007(2) 0.0132(19) -0.001(2) C17 0.053(3) 0.067(3) 0.032(2) 0.010(2) 0.018(2) -0.005(3) C18 0.051(3) 0.067(4) 0.050(3) 0.027(3) 0.025(3) 0.003(3) C19 0.051(3) 0.038(3) 0.065(3) 0.020(2) 0.030(3) 0.001(2) C20 0.039(3) 0.031(2) 0.046(3) 0.009(2) 0.021(2) 0.0039(19) C21 0.057(3) 0.026(2) 0.052(3) 0.012(2) 0.031(3) 0.006(2) C22 0.080(4) 0.070(4) 0.065(4) -0.018(3) 0.031(3) -0.029(3) C23 0.132(6) 0.032(3) 0.111(5) 0.013(3) 0.077(5) 0.016(3) C24 0.067(3) 0.051(3) 0.028(2) -0.001(2) 0.019(2) -0.011(3) C25 0.119(6) 0.066(4) 0.069(4) -0.012(3) 0.058(4) 0.000(4) C26 0.077(4) 0.087(4) 0.039(3) -0.002(3) 0.008(3) -0.036(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 2.218(3) . ? Pb1 N2 2.417(3) . ? Pb1 N2 2.587(3) 3_757 ? Pb1 Si1 3.0457(14) . ? Pb1 Pb1 3.4404(9) 3_757 ? Si1 N1 1.711(3) . ? Si1 N2 1.766(3) . ? Si1 C13 1.873(5) . ? Si1 C14 1.875(5) . ? N1 C1 1.438(5) . ? N2 C15 1.468(5) . ? N2 Pb1 2.587(3) 3_757 ? C1 C2 1.409(5) . ? C1 C6 1.423(5) . ? C2 C3 1.389(6) . ? C2 C10 1.529(6) . ? C3 C4 1.368(7) . ? C3 H3A 0.9300 . ? C4 C5 1.364(7) . ? C4 H4A 0.9300 . ? C5 C6 1.399(6) . ? C5 H5A 0.9300 . ? C6 C7 1.522(6) . ? C7 C9 1.532(7) . ? C7 C8 1.534(7) . ? C7 H7A 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 C12 1.523(6) . ? C10 C11 1.534(7) . ? C10 H10A 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.415(5) . ? C15 C16 1.437(6) . ? C16 C17 1.394(6) . ? C16 C24 1.515(6) . ? C17 C18 1.381(7) . ? C17 H17A 0.9300 . ? C18 C19 1.348(7) . ? C18 H18A 0.9300 . ? C19 C20 1.404(6) . ? C19 H19A 0.9300 . ? C20 C21 1.536(6) . ? C21 C22 1.514(7) . ? C21 C23 1.550(6) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C25 1.525(8) . ? C24 C26 1.527(7) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 N2 68.62(11) . . ? N1 Pb1 N2 102.11(11) . 3_757 ? N2 Pb1 N2 93.21(10) . 3_757 ? N1 Pb1 Si1 33.48(8) . . ? N2 Pb1 Si1 35.41(8) . . ? N2 Pb1 Si1 102.59(7) 3_757 . ? N1 Pb1 Pb1 84.36(8) . 3_757 ? N2 Pb1 Pb1 48.67(7) . 3_757 ? N2 Pb1 Pb1 44.54(7) 3_757 3_757 ? Si1 Pb1 Pb1 65.88(3) . 3_757 ? N1 Si1 N2 97.68(16) . . ? N1 Si1 C13 116.5(2) . . ? N2 Si1 C13 111.45(19) . . ? N1 Si1 C14 112.48(19) . . ? N2 Si1 C14 114.91(19) . . ? C13 Si1 C14 104.3(2) . . ? N1 Si1 Pb1 45.66(11) . . ? N2 Si1 Pb1 52.46(11) . . ? C13 Si1 Pb1 122.82(17) . . ? C14 Si1 Pb1 132.81(16) . . ? C1 N1 Si1 130.4(3) . . ? C1 N1 Pb1 124.6(2) . . ? Si1 N1 Pb1 100.86(15) . . ? C15 N2 Si1 116.9(3) . . ? C15 N2 Pb1 128.5(2) . . ? Si1 N2 Pb1 92.13(13) . . ? C15 N2 Pb1 119.1(2) . 3_757 ? Si1 N2 Pb1 107.42(14) . 3_757 ? Pb1 N2 Pb1 86.79(10) . 3_757 ? C2 C1 C6 118.6(4) . . ? C2 C1 N1 120.9(3) . . ? C6 C1 N1 120.4(3) . . ? C3 C2 C1 119.4(4) . . ? C3 C2 C10 118.1(4) . . ? C1 C2 C10 122.5(4) . . ? C4 C3 C2 122.0(4) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C5 C4 C3 119.3(4) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C6 121.9(4) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 118.8(4) . . ? C5 C6 C7 118.7(4) . . ? C1 C6 C7 122.6(4) . . ? C6 C7 C9 111.5(4) . . ? C6 C7 C8 111.4(4) . . ? C9 C7 C8 110.5(4) . . ? C6 C7 H7A 107.7 . . ? C9 C7 H7A 107.7 . . ? C8 C7 H7A 107.7 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C2 110.6(4) . . ? C12 C10 C11 109.4(4) . . ? C2 C10 C11 112.7(4) . . ? C12 C10 H10A 108.0 . . ? C2 C10 H10A 108.0 . . ? C11 C10 H10A 108.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C16 117.9(4) . . ? C20 C15 N2 122.3(4) . . ? C16 C15 N2 119.7(3) . . ? C17 C16 C15 119.0(4) . . ? C17 C16 C24 116.8(4) . . ? C15 C16 C24 124.2(4) . . ? C18 C17 C16 122.3(5) . . ? C18 C17 H17A 118.8 . . ? C16 C17 H17A 118.8 . . ? C19 C18 C17 118.7(4) . . ? C19 C18 H18A 120.6 . . ? C17 C18 H18A 120.6 . . ? C18 C19 C20 122.9(4) . . ? C18 C19 H19A 118.5 . . ? C20 C19 H19A 118.5 . . ? C19 C20 C15 119.2(4) . . ? C19 C20 C21 116.4(4) . . ? C15 C20 C21 124.4(4) . . ? C22 C21 C20 112.3(4) . . ? C22 C21 C23 110.5(4) . . ? C20 C21 C23 113.2(4) . . ? C22 C21 H21A 106.8 . . ? C20 C21 H21A 106.8 . . ? C23 C21 H21A 106.8 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C16 C24 C25 110.4(4) . . ? C16 C24 C26 111.6(4) . . ? C25 C24 C26 111.9(5) . . ? C16 C24 H24A 107.6 . . ? C25 C24 H24A 107.6 . . ? C26 C24 H24A 107.6 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.168 _refine_diff_density_min -0.775 _refine_diff_density_rms 0.105 data_4 _database_code_depnum_ccdc_archive 'CCDC 823609' #TrackingRef '- complex4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H40 N2 Si Sn' _chemical_formula_weight 527.38 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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pna2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z+1/2' _cell_length_a 17.83(4) _cell_length_b 8.55(2) _cell_length_c 36.69(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5595(22) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 966 _cell_measurement_theta_min 2.540 _cell_measurement_theta_max 23.000 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.252 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2192 _exptl_absorpt_coefficient_mu 0.970 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8448 _exptl_absorpt_correction_T_max 0.8843 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 7.74 _diffrn_reflns_number 18142 _diffrn_reflns_av_R_equivalents 0.0626 _diffrn_reflns_av_sigmaI/netI 0.0731 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7707 _reflns_number_gt 5035 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Some atoms have poor thermal parameters. ISOR was used to restrain atoms C41 N2 C3 C27 and C46. ; _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^)+(0.1060P)^2^+7.7189P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00(17) _refine_ls_number_reflns 7707 _refine_ls_number_parameters 561 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.1125 _refine_ls_R_factor_gt 0.0762 _refine_ls_wR_factor_ref 0.2050 _refine_ls_wR_factor_gt 0.1880 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.047 _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 Sn1 Sn 0.19100(5) 1.13079(12) 0.26809(4) 0.0711(4) Uani 1 1 d . . . Si1 Si 0.3073(2) 0.9133(4) 0.25230(12) 0.0540(11) Uani 1 1 d . . . N1 N 0.3054(7) 1.1095(11) 0.2626(4) 0.063(3) Uani 1 1 d . . . N2 N 0.2108(6) 0.9040(9) 0.2530(3) 0.041(3) Uani 1 1 d U . . C1 C 0.3502(7) 0.8687(16) 0.2070(5) 0.070(5) Uani 1 1 d . . . H1A H 0.3321 0.9419 0.1892 0.105 Uiso 1 1 calc R . . H1B H 0.3368 0.7645 0.1997 0.105 Uiso 1 1 calc R . . H1C H 0.4038 0.8769 0.2087 0.105 Uiso 1 1 calc R . . C2 C 0.3512(12) 0.787(2) 0.2851(6) 0.106(8) Uani 1 1 d . . . H2A H 0.4030 0.8156 0.2877 0.158 Uiso 1 1 calc R . . H2B H 0.3476 0.6808 0.2771 0.158 Uiso 1 1 calc R . . H2C H 0.3264 0.7982 0.3082 0.158 Uiso 1 1 calc R . . C3 C 0.3628(6) 1.2291(13) 0.2629(4) 0.040(3) Uani 1 1 d U . . C4 C 0.3991(10) 1.2642(17) 0.2931(5) 0.062(5) Uani 1 1 d . . . C5 C 0.4603(7) 1.3767(19) 0.2904(5) 0.061(4) Uani 1 1 d . . . H5 H 0.4937 1.3855 0.3097 0.073 Uiso 1 1 calc R . . C6 C 0.4696(8) 1.460(2) 0.2635(7) 0.081(6) Uani 1 1 d . . . H6 H 0.5039 1.5420 0.2644 0.098 Uiso 1 1 calc R . . C7 C 0.4299(9) 1.4327(16) 0.2325(5) 0.064(5) Uani 1 1 d . . . H7 H 0.4413 1.4892 0.2115 0.077 Uiso 1 1 calc R . . C8 C 0.3711(8) 1.3191(14) 0.2314(4) 0.049(4) Uani 1 1 d . . . C9 C 0.3893(9) 1.183(2) 0.3284(5) 0.068(4) Uani 1 1 d . . . H9 H 0.3618 1.0871 0.3222 0.082 Uiso 1 1 calc R . . C10 C 0.3398(11) 1.265(3) 0.3558(5) 0.095(7) Uani 1 1 d . . . H10A H 0.3226 1.1906 0.3736 0.142 Uiso 1 1 calc R . . H10B H 0.2975 1.3097 0.3435 0.142 Uiso 1 1 calc R . . H10C H 0.3679 1.3457 0.3677 0.142 Uiso 1 1 calc R . . C11 C 0.4593(8) 1.125(2) 0.3485(6) 0.095(6) Uani 1 1 d . . . H11A H 0.4917 1.2118 0.3537 0.142 Uiso 1 1 calc R . . H11B H 0.4855 1.0506 0.3336 0.142 Uiso 1 1 calc R . . H11C H 0.4447 1.0756 0.3710 0.142 Uiso 1 1 calc R . . C12 C 0.3273(12) 1.297(2) 0.1968(6) 0.087(6) Uani 1 1 d . . . H12 H 0.3039 1.1939 0.1993 0.105 Uiso 1 1 calc R . . C13 C 0.3749(14) 1.286(3) 0.1614(6) 0.119(9) Uani 1 1 d . . . H13A H 0.3465 1.2335 0.1429 0.178 Uiso 1 1 calc R . . H13B H 0.4200 1.2283 0.1663 0.178 Uiso 1 1 calc R . . H13C H 0.3876 1.3893 0.1533 0.178 Uiso 1 1 calc R . . C14 C 0.2642(14) 1.407(2) 0.1957(8) 0.139(10) Uani 1 1 d . . . H14A H 0.2441 1.4198 0.2198 0.208 Uiso 1 1 calc R . . H14B H 0.2260 1.3671 0.1798 0.208 Uiso 1 1 calc R . . H14C H 0.2813 1.5064 0.1868 0.208 Uiso 1 1 calc R . . C15 C 0.1621(9) 0.7823(14) 0.2455(5) 0.056(4) Uani 1 1 d . . . C16 C 0.1376(7) 0.6787(17) 0.2728(4) 0.051(4) Uani 1 1 d . . . C17 C 0.0856(8) 0.5607(17) 0.2657(6) 0.065(4) Uani 1 1 d . . . H17 H 0.0657 0.4995 0.2843 0.078 Uiso 1 1 calc R . . C18 C 0.0653(9) 0.539(2) 0.2300(7) 0.082(6) Uani 1 1 d . . . H18 H 0.0364 0.4527 0.2238 0.098 Uiso 1 1 calc R . . C19 C 0.0843(7) 0.6329(16) 0.2055(4) 0.045(3) Uani 1 1 d . . . H19 H 0.0641 0.6170 0.1824 0.054 Uiso 1 1 calc R . . C20 C 0.1309(7) 0.7533(14) 0.2095(4) 0.040(4) Uani 1 1 d . . . C21 C 0.1616(10) 0.7053(17) 0.3129(5) 0.071(5) Uani 1 1 d . . . H21 H 0.2014 0.7841 0.3134 0.085 Uiso 1 1 calc R . . C22 C 0.1902(13) 0.560(3) 0.3298(6) 0.122(9) Uani 1 1 d . . . H22A H 0.1642 0.4713 0.3198 0.183 Uiso 1 1 calc R . . H22B H 0.1820 0.5634 0.3557 0.183 Uiso 1 1 calc R . . H22C H 0.2429 0.5496 0.3250 0.183 Uiso 1 1 calc R . . C23 C 0.0848(15) 0.779(4) 0.3336(7) 0.144(11) Uani 1 1 d . . . H23A H 0.0959 0.7989 0.3588 0.215 Uiso 1 1 calc R . . H23B H 0.0444 0.7054 0.3319 0.215 Uiso 1 1 calc R . . H23C H 0.0706 0.8751 0.3220 0.215 Uiso 1 1 calc R . . C24 C 0.1535(9) 0.865(2) 0.1786(6) 0.085(6) Uani 1 1 d . . . H24 H 0.2001 0.9154 0.1863 0.102 Uiso 1 1 calc R . . C25 C 0.1716(14) 0.780(3) 0.1416(5) 0.107(8) Uani 1 1 d . . . H25A H 0.1325 0.7060 0.1362 0.160 Uiso 1 1 calc R . . H25B H 0.2186 0.7254 0.1437 0.160 Uiso 1 1 calc R . . H25C H 0.1748 0.8554 0.1224 0.160 Uiso 1 1 calc R . . C26 C 0.0975(13) 0.991(3) 0.1739(6) 0.115(8) Uani 1 1 d . . . H26A H 0.0509 0.9473 0.1657 0.173 Uiso 1 1 calc R . . H26B H 0.1154 1.0649 0.1561 0.173 Uiso 1 1 calc R . . H26C H 0.0900 1.0436 0.1968 0.173 Uiso 1 1 calc R . . Sn2 Sn 1.05489(5) 0.61818(12) 0.49033(3) 0.0754(4) Uani 1 1 d . . . Si2 Si 0.93735(19) 0.3864(4) 0.50016(11) 0.0456(10) Uani 1 1 d . . . N3 N 1.0375(5) 0.3806(10) 0.5011(3) 0.042(3) Uani 1 1 d . . . N4 N 0.9382(4) 0.5900(9) 0.4920(4) 0.040(2) Uani 1 1 d . . . C27 C 0.8922(8) 0.3245(19) 0.5395(5) 0.069(4) Uani 1 1 d U . . H27A H 0.9159 0.3707 0.5604 0.104 Uiso 1 1 calc R . . H27B H 0.8952 0.2126 0.5412 0.104 Uiso 1 1 calc R . . H27C H 0.8405 0.3558 0.5386 0.104 Uiso 1 1 calc R . . C28 C 0.8966(7) 0.2725(17) 0.4618(5) 0.064(5) Uani 1 1 d . . . H28A H 0.9239 0.2948 0.4398 0.096 Uiso 1 1 calc R . . H28B H 0.8449 0.3012 0.4586 0.096 Uiso 1 1 calc R . . H28C H 0.8999 0.1629 0.4671 0.096 Uiso 1 1 calc R . . C29 C 1.0892(7) 0.2604(13) 0.5087(4) 0.032(3) Uani 1 1 d . . . C30 C 1.1083(10) 0.2266(19) 0.5422(5) 0.062(5) Uani 1 1 d . . . C31 C 1.1640(11) 0.109(2) 0.5526(7) 0.097(7) Uani 1 1 d . . . H31 H 1.1810 0.0924 0.5763 0.116 Uiso 1 1 calc R . . C32 C 1.1894(9) 0.0197(19) 0.5202(6) 0.079(6) Uani 1 1 d . . . H32 H 1.2216 -0.0646 0.5236 0.095 Uiso 1 1 calc R . . C33 C 1.1680(6) 0.0553(16) 0.4862(5) 0.067(5) Uani 1 1 d . . . H33 H 1.1883 -0.0023 0.4671 0.080 Uiso 1 1 calc R . . C34 C 1.1175(9) 0.1731(16) 0.4779(5) 0.065(5) Uani 1 1 d . . . C35 C 1.0869(8) 0.3299(19) 0.5749(4) 0.061(4) Uani 1 1 d . . . H35 H 1.0421 0.3889 0.5679 0.074 Uiso 1 1 calc R . . C36 C 1.0679(14) 0.241(3) 0.6074(6) 0.107(8) Uani 1 1 d . . . H36A H 1.0357 0.1558 0.6009 0.161 Uiso 1 1 calc R . . H36B H 1.0424 0.3081 0.6244 0.161 Uiso 1 1 calc R . . H36C H 1.1129 0.2016 0.6184 0.161 Uiso 1 1 calc R . . C37 C 1.1476(12) 0.451(3) 0.5855(6) 0.116(8) Uani 1 1 d . . . H37A H 1.1242 0.5397 0.5967 0.174 Uiso 1 1 calc R . . H37B H 1.1742 0.4831 0.5641 0.174 Uiso 1 1 calc R . . H37C H 1.1821 0.4040 0.6024 0.174 Uiso 1 1 calc R . . C38 C 1.0998(9) 0.208(2) 0.4391(5) 0.074(5) Uani 1 1 d U . . H38 H 1.0539 0.2708 0.4394 0.089 Uiso 1 1 calc R . . C39 C 1.1510(13) 0.291(4) 0.4194(6) 0.130(10) Uani 1 1 d U . . H39A H 1.1388 0.4001 0.4204 0.195 Uiso 1 1 calc R . . H39B H 1.1500 0.2564 0.3945 0.195 Uiso 1 1 calc R . . H39C H 1.2001 0.2746 0.4293 0.195 Uiso 1 1 calc R . . C40 C 1.0815(13) 0.062(3) 0.4176(7) 0.124(9) Uani 1 1 d . . . H40A H 1.0585 0.0903 0.3949 0.186 Uiso 1 1 calc R . . H40B H 1.0476 -0.0024 0.4314 0.186 Uiso 1 1 calc R . . H40C H 1.1268 0.0045 0.4129 0.186 Uiso 1 1 calc R . . C41 C 0.8846(6) 0.7021(11) 0.4936(4) 0.040(3) Uani 1 1 d U . . C42 C 0.8422(7) 0.7489(16) 0.4618(5) 0.049(4) Uani 1 1 d . . . C43 C 0.7936(7) 0.8689(19) 0.4646(7) 0.083(6) Uani 1 1 d . . . H43 H 0.7699 0.9086 0.4440 0.100 Uiso 1 1 calc R . . C44 C 0.7800(8) 0.9307(18) 0.4981(6) 0.069(5) Uani 1 1 d . . . H44 H 0.7421 1.0045 0.5006 0.083 Uiso 1 1 calc R . . C45 C 0.8213(8) 0.8868(16) 0.5288(5) 0.059(4) Uani 1 1 d . . . H45 H 0.8161 0.9412 0.5506 0.070 Uiso 1 1 calc R . . C46 C 0.8664(8) 0.7706(15) 0.5265(4) 0.047(4) Uani 1 1 d U . . C47 C 0.8623(8) 0.682(2) 0.4248(5) 0.067(4) Uani 1 1 d . . . H47 H 0.8912 0.5859 0.4284 0.081 Uiso 1 1 calc R . . C48 C 0.7981(13) 0.648(3) 0.4024(5) 0.126(9) Uani 1 1 d . . . H48A H 0.7694 0.5656 0.4134 0.190 Uiso 1 1 calc R . . H48B H 0.8147 0.6150 0.3787 0.190 Uiso 1 1 calc R . . H48C H 0.7676 0.7397 0.4001 0.190 Uiso 1 1 calc R . . C49 C 0.912(2) 0.803(4) 0.4056(8) 0.21(2) Uani 1 1 d . . . H49A H 0.8850 0.8991 0.4030 0.321 Uiso 1 1 calc R . . H49B H 0.9258 0.7641 0.3820 0.321 Uiso 1 1 calc R . . H49C H 0.9564 0.8203 0.4198 0.321 Uiso 1 1 calc R . . C50 C 0.9094(10) 0.7377(17) 0.5619(5) 0.063(5) Uani 1 1 d . . . H50 H 0.9394 0.6437 0.5574 0.075 Uiso 1 1 calc R . . C51 C 0.9623(12) 0.860(2) 0.5735(6) 0.103(7) Uani 1 1 d . . . H51A H 0.9895 0.8971 0.5527 0.155 Uiso 1 1 calc R . . H51B H 0.9968 0.8167 0.5909 0.155 Uiso 1 1 calc R . . H51C H 0.9352 0.9444 0.5844 0.155 Uiso 1 1 calc R . . C52 C 0.8485(14) 0.690(3) 0.5938(7) 0.121(8) Uani 1 1 d . . . H52A H 0.8733 0.6868 0.6170 0.181 Uiso 1 1 calc R . . H52B H 0.8274 0.5897 0.5884 0.181 Uiso 1 1 calc R . . H52C H 0.8092 0.7671 0.5945 0.181 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 Sn1 0.0514(5) 0.0555(6) 0.1066(10) -0.0098(7) 0.0006(6) 0.0043(5) Si1 0.0477(19) 0.0442(19) 0.070(3) -0.0024(18) -0.015(2) 0.0020(17) N1 0.077(7) 0.052(6) 0.062(9) -0.011(7) -0.002(7) -0.007(6) N2 0.055(5) 0.011(4) 0.058(7) -0.009(4) 0.005(4) -0.004(4) C1 0.044(7) 0.045(8) 0.121(15) -0.003(9) -0.002(8) 0.014(7) C2 0.123(16) 0.094(13) 0.100(16) -0.005(12) -0.046(13) 0.068(13) C3 0.029(5) 0.028(5) 0.064(8) 0.003(6) 0.005(5) -0.012(4) C4 0.072(11) 0.047(9) 0.066(13) -0.009(8) -0.035(10) 0.006(7) C5 0.030(7) 0.069(10) 0.084(13) 0.001(10) -0.019(7) 0.007(7) C6 0.048(8) 0.064(11) 0.133(19) -0.034(13) -0.002(12) -0.002(8) C7 0.067(10) 0.037(7) 0.090(14) 0.009(7) 0.009(9) -0.020(7) C8 0.053(8) 0.025(6) 0.068(11) 0.003(7) -0.003(7) -0.001(6) C9 0.075(10) 0.076(11) 0.053(11) -0.027(10) -0.015(9) 0.011(9) C10 0.081(12) 0.128(18) 0.075(15) 0.022(12) 0.022(10) 0.047(12) C11 0.046(9) 0.132(16) 0.105(16) 0.010(13) -0.005(8) 0.018(10) C12 0.109(15) 0.059(10) 0.094(17) 0.012(11) -0.012(13) 0.015(11) C13 0.15(2) 0.134(19) 0.071(16) 0.013(14) -0.011(15) -0.049(17) C14 0.15(2) 0.107(17) 0.16(3) -0.002(16) -0.079(19) 0.035(16) C15 0.088(11) 0.013(5) 0.068(12) 0.000(7) 0.005(10) 0.011(6) C16 0.051(7) 0.061(9) 0.040(10) -0.020(8) -0.010(7) 0.012(6) C17 0.075(10) 0.057(8) 0.063(12) 0.010(10) 0.014(10) -0.034(7) C18 0.055(10) 0.078(12) 0.113(19) -0.019(13) 0.027(11) -0.004(9) C19 0.038(6) 0.063(8) 0.034(8) -0.001(7) -0.027(6) 0.001(7) C20 0.025(6) 0.048(8) 0.048(11) 0.005(7) -0.018(6) -0.009(5) C21 0.100(13) 0.033(7) 0.079(14) 0.010(9) 0.018(10) 0.012(8) C22 0.18(2) 0.106(16) 0.083(17) 0.034(13) -0.065(15) -0.027(15) C23 0.14(2) 0.21(3) 0.081(19) -0.070(18) 0.006(16) 0.04(2) C24 0.052(9) 0.087(12) 0.115(17) 0.022(12) -0.019(9) -0.007(9) C25 0.117(17) 0.17(2) 0.033(12) 0.008(12) -0.001(12) 0.006(16) C26 0.126(18) 0.127(19) 0.094(16) 0.048(14) -0.006(13) 0.007(15) Sn2 0.0492(5) 0.0535(6) 0.1235(12) 0.0101(8) -0.0008(6) -0.0007(5) Si2 0.0356(15) 0.0433(17) 0.058(3) -0.0003(19) -0.0174(18) 0.0054(16) N3 0.030(4) 0.021(4) 0.075(9) 0.011(5) -0.009(5) -0.009(4) N4 0.019(4) 0.030(4) 0.073(8) 0.002(6) -0.006(5) -0.014(4) C27 0.056(7) 0.070(8) 0.082(9) -0.014(7) -0.017(6) 0.019(6) C28 0.032(7) 0.062(9) 0.098(14) 0.018(9) -0.018(7) 0.012(6) C29 0.018(5) 0.034(7) 0.045(10) 0.000(6) 0.009(6) -0.015(5) C30 0.085(12) 0.056(10) 0.044(12) 0.001(8) -0.002(9) -0.045(9) C31 0.080(12) 0.101(15) 0.108(17) 0.032(14) 0.013(12) 0.034(12) C32 0.073(11) 0.051(9) 0.113(16) 0.005(9) -0.044(11) 0.038(8) C33 0.030(6) 0.063(8) 0.107(15) -0.030(10) -0.031(8) 0.016(6) C34 0.066(9) 0.041(8) 0.088(15) 0.004(8) 0.004(9) 0.008(7) C35 0.052(8) 0.089(11) 0.043(10) -0.001(9) -0.012(7) 0.000(8) C36 0.125(19) 0.136(19) 0.061(17) -0.015(13) 0.005(14) 0.003(15) C37 0.122(17) 0.123(17) 0.104(17) -0.039(14) 0.016(13) -0.074(15) C38 0.056(9) 0.106(13) 0.060(13) -0.020(10) -0.006(8) 0.042(9) C39 0.089(15) 0.25(3) 0.054(15) 0.006(16) 0.007(11) 0.014(16) C40 0.141(19) 0.105(16) 0.13(2) -0.068(15) -0.039(16) 0.010(15) C41 0.052(6) 0.009(4) 0.057(7) 0.007(6) 0.008(6) -0.007(4) C42 0.019(6) 0.070(10) 0.058(12) 0.017(7) 0.015(7) 0.004(6) C43 0.022(7) 0.068(10) 0.16(2) 0.007(12) -0.003(9) 0.010(7) C44 0.038(7) 0.062(9) 0.108(16) -0.029(11) -0.007(9) -0.002(6) C45 0.050(8) 0.052(9) 0.074(12) -0.023(8) 0.013(8) -0.030(7) C46 0.048(6) 0.028(6) 0.065(8) -0.013(6) -0.003(6) -0.008(5) C47 0.059(9) 0.079(11) 0.063(12) 0.015(10) -0.005(9) 0.013(8) C48 0.113(17) 0.21(3) 0.055(14) -0.009(15) 0.003(12) -0.032(18) C49 0.33(5) 0.16(3) 0.15(3) -0.04(2) 0.06(3) -0.15(3) C50 0.071(10) 0.047(9) 0.070(13) -0.014(8) 0.004(9) 0.018(8) C51 0.113(16) 0.099(15) 0.098(17) -0.011(12) -0.029(13) 0.006(13) C52 0.114(17) 0.13(2) 0.11(2) -0.036(17) -0.004(15) 0.009(16) _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 Sn1 N2 2.048(9) . ? Sn1 N1 2.059(14) . ? Sn1 Si1 2.845(6) . ? Si1 N1 1.721(11) . ? Si1 N2 1.723(12) . ? Si1 C2 1.796(18) . ? Si1 C1 1.870(19) . ? N1 C3 1.447(15) . ? N2 C15 1.383(18) . ? C3 C4 1.32(2) . ? C3 C8 1.40(2) . ? C4 C5 1.46(2) . ? C4 C9 1.48(3) . ? C5 C6 1.23(2) . ? C6 C7 1.36(3) . ? C7 C8 1.43(2) . ? C8 C12 1.50(3) . ? C9 C10 1.51(2) . ? C9 C11 1.53(2) . ? C12 C14 1.47(3) . ? C12 C13 1.56(3) . ? C15 C16 1.41(2) . ? C15 C20 1.45(2) . ? C16 C17 1.395(19) . ? C16 C21 1.55(2) . ? C17 C18 1.37(3) . ? C18 C19 1.25(2) . ? C19 C20 1.331(18) . ? C20 C24 1.54(2) . ? C21 C22 1.48(3) . ? C21 C23 1.69(3) . ? C24 C26 1.48(2) . ? C24 C25 1.57(3) . ? Sn2 N3 2.094(9) . ? Sn2 N4 2.096(9) . ? Sn2 Si2 2.907(6) . ? Si2 C27 1.735(18) . ? Si2 N4 1.766(9) . ? Si2 N3 1.786(10) . ? Si2 C28 1.861(16) . ? N3 C29 1.408(15) . ? N4 C41 1.355(14) . ? C29 C30 1.31(2) . ? C29 C34 1.45(2) . ? C30 C31 1.46(3) . ? C30 C35 1.54(2) . ? C31 C32 1.48(3) . ? C32 C33 1.34(2) . ? C33 C34 1.385(19) . ? C34 C38 1.49(2) . ? C35 C36 1.45(3) . ? C35 C37 1.55(2) . ? C38 C39 1.36(3) . ? C38 C40 1.51(3) . ? C41 C46 1.38(2) . ? C41 C42 1.45(2) . ? C42 C43 1.347(19) . ? C42 C47 1.52(2) . ? C43 C44 1.36(3) . ? C44 C45 1.40(2) . ? C45 C46 1.280(19) . ? C46 C50 1.54(2) . ? C47 C48 1.44(3) . ? C47 C49 1.53(3) . ? C50 C51 1.47(2) . ? C50 C52 1.64(3) . ? 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 Sn1 N1 73.7(4) . . ? N2 Sn1 Si1 36.9(3) . . ? N1 Sn1 Si1 36.9(3) . . ? N1 Si1 N2 91.3(5) . . ? N1 Si1 C2 116.4(9) . . ? N2 Si1 C2 113.5(9) . . ? N1 Si1 C1 113.7(7) . . ? N2 Si1 C1 114.3(6) . . ? C2 Si1 C1 107.2(9) . . ? N1 Si1 Sn1 45.9(5) . . ? N2 Si1 Sn1 45.5(3) . . ? C2 Si1 Sn1 125.0(7) . . ? C1 Si1 Sn1 127.8(5) . . ? C3 N1 Si1 132.7(10) . . ? C3 N1 Sn1 129.6(8) . . ? Si1 N1 Sn1 97.3(6) . . ? C15 N2 Si1 131.2(9) . . ? C15 N2 Sn1 131.2(9) . . ? Si1 N2 Sn1 97.6(4) . . ? C4 C3 C8 121.2(12) . . ? C4 C3 N1 121.0(14) . . ? C8 C3 N1 117.2(13) . . ? C3 C4 C5 117.4(17) . . ? C3 C4 C9 124.7(15) . . ? C5 C4 C9 117.3(15) . . ? C6 C5 C4 122.7(16) . . ? C5 C6 C7 120.0(16) . . ? C6 C7 C8 121.5(16) . . ? C3 C8 C7 115.3(13) . . ? C3 C8 C12 125.1(14) . . ? C7 C8 C12 119.4(15) . . ? C4 C9 C10 115.6(15) . . ? C4 C9 C11 118.5(15) . . ? C10 C9 C11 107.8(15) . . ? C14 C12 C8 110.0(18) . . ? C14 C12 C13 116(2) . . ? C8 C12 C13 115.4(17) . . ? N2 C15 C16 121.7(15) . . ? N2 C15 C20 123.3(14) . . ? C16 C15 C20 115.0(13) . . ? C17 C16 C15 121.8(15) . . ? C17 C16 C21 117.8(15) . . ? C15 C16 C21 120.0(13) . . ? C18 C17 C16 116.8(16) . . ? C19 C18 C17 122.0(17) . . ? C18 C19 C20 125.8(16) . . ? C19 C20 C15 118.1(14) . . ? C19 C20 C24 124.2(14) . . ? C15 C20 C24 117.7(12) . . ? C22 C21 C16 111.7(15) . . ? C22 C21 C23 113.8(19) . . ? C16 C21 C23 105.0(15) . . ? C26 C24 C20 111.2(16) . . ? C26 C24 C25 112.1(17) . . ? C20 C24 C25 113.8(16) . . ? N3 Sn2 N4 74.6(3) . . ? N3 Sn2 Si2 37.6(3) . . ? N4 Sn2 Si2 37.1(2) . . ? C27 Si2 N4 116.4(7) . . ? C27 Si2 N3 116.0(6) . . ? N4 Si2 N3 91.3(4) . . ? C27 Si2 C28 106.7(8) . . ? N4 Si2 C28 113.1(6) . . ? N3 Si2 C28 113.0(6) . . ? C27 Si2 Sn2 130.2(6) . . ? N4 Si2 Sn2 45.6(3) . . ? N3 Si2 Sn2 45.7(3) . . ? C28 Si2 Sn2 123.0(5) . . ? C29 N3 Si2 132.8(7) . . ? C29 N3 Sn2 130.4(7) . . ? Si2 N3 Sn2 96.7(4) . . ? C41 N4 Si2 133.2(7) . . ? C41 N4 Sn2 128.3(6) . . ? Si2 N4 Sn2 97.3(4) . . ? C30 C29 N3 121.1(14) . . ? C30 C29 C34 122.0(14) . . ? N3 C29 C34 116.9(13) . . ? C29 C30 C31 124.9(18) . . ? C29 C30 C35 122.8(16) . . ? C31 C30 C35 111.1(17) . . ? C30 C31 C32 110.6(18) . . ? C33 C32 C31 122.9(14) . . ? C32 C33 C34 123.7(16) . . ? C33 C34 C29 115.6(15) . . ? C33 C34 C38 119.6(15) . . ? C29 C34 C38 124.7(13) . . ? C36 C35 C30 113.5(16) . . ? C36 C35 C37 107.8(16) . . ? C30 C35 C37 114.0(14) . . ? C39 C38 C34 118.0(17) . . ? C39 C38 C40 107(2) . . ? C34 C38 C40 112.2(18) . . ? N4 C41 C46 120.2(14) . . ? N4 C41 C42 122.1(13) . . ? C46 C41 C42 117.6(12) . . ? C43 C42 C41 119.1(17) . . ? C43 C42 C47 120.4(17) . . ? C41 C42 C47 119.6(12) . . ? C42 C43 C44 119(2) . . ? C43 C44 C45 122.0(15) . . ? C46 C45 C44 119.1(16) . . ? C45 C46 C41 122.3(15) . . ? C45 C46 C50 113.6(14) . . ? C41 C46 C50 123.0(13) . . ? C48 C47 C42 113.7(15) . . ? C48 C47 C49 110(2) . . ? C42 C47 C49 107.2(17) . . ? C51 C50 C46 115.8(15) . . ? C51 C50 C52 113.2(18) . . ? C46 C50 C52 108.4(15) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.142 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.097 # Attachment '- complex6.cif' data_a00413c _database_code_depnum_ccdc_archive 'CCDC 823610' #TrackingRef '- complex6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H90 Ge2 N4 O3 Si2' _chemical_formula_weight 1068.68 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' Ge Ge 0.1547 1.8001 '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' O O 0.0106 0.0060 '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/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y, -z+1/2' '-x, -y, -z' 'x-1/2, -y, z-1/2' _cell_length_a 13.449(4) _cell_length_b 10.478(4) _cell_length_c 21.692(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.705(5) _cell_angle_gamma 90.00 _cell_volume 3056.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 939 _cell_measurement_theta_min 2.630 _cell_measurement_theta_max 25.280 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1140 _exptl_absorpt_coefficient_mu 1.064 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7769 _exptl_absorpt_correction_T_max 0.8654 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12377 _diffrn_reflns_av_R_equivalents 0.0605 _diffrn_reflns_av_sigmaI/netI 0.0708 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5382 _reflns_number_gt 2458 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1434P)^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 5382 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1385 _refine_ls_R_factor_gt 0.0739 _refine_ls_wR_factor_ref 0.2310 _refine_ls_wR_factor_gt 0.1946 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.23345(4) 0.07635(8) 0.19089(3) 0.0870(4) Uani 1 1 d . . . Si1 Si 0.20589(12) 0.0561(2) 0.07331(7) 0.0995(8) Uani 1 1 d . . . N1 N 0.3048(3) 0.0985(5) 0.12117(19) 0.0722(13) Uani 1 1 d . . . N2 N 0.1340(3) 0.0299(6) 0.1384(2) 0.0864(16) Uani 1 1 d . . . O1 O 0.2500 0.1952(11) 0.2500 0.192(4) Uani 1 2 d S . . O2 O 0.2500 -0.0528(8) 0.2500 0.146(3) Uani 1 2 d S . . C1 C 0.1559(6) 0.1863(11) 0.0222(4) 0.169(4) Uani 1 1 d . . . H1A H 0.1523 0.1563 -0.0195 0.253 Uiso 1 1 calc R . . H1B H 0.1992 0.2590 0.0246 0.253 Uiso 1 1 calc R . . H1C H 0.0907 0.2101 0.0356 0.253 Uiso 1 1 calc R . . C2 C 0.2324(7) -0.0870(10) 0.0248(4) 0.170(5) Uani 1 1 d . . . H2A H 0.2155 -0.0688 -0.0174 0.255 Uiso 1 1 calc R . . H2B H 0.1936 -0.1579 0.0388 0.255 Uiso 1 1 calc R . . H2C H 0.3018 -0.1078 0.0280 0.255 Uiso 1 1 calc R . . C3 C 0.0353(4) -0.0108(7) 0.1482(2) 0.0658(15) Uani 1 1 d . . . C4 C -0.0390(4) 0.0802(7) 0.1590(3) 0.0715(16) Uani 1 1 d . . . C5 C -0.1350(4) 0.0375(8) 0.1683(3) 0.092(2) Uani 1 1 d . . . H5A H -0.1849 0.0973 0.1747 0.111 Uiso 1 1 calc R . . C6 C -0.1590(5) -0.0869(9) 0.1683(4) 0.101(2) Uani 1 1 d . . . H6A H -0.2241 -0.1124 0.1753 0.121 Uiso 1 1 calc R . . C7 C -0.0868(5) -0.1754(7) 0.1581(3) 0.090(2) Uani 1 1 d . . . H7A H -0.1032 -0.2616 0.1578 0.108 Uiso 1 1 calc R . . C8 C 0.0117(4) -0.1387(8) 0.1481(3) 0.0787(18) Uani 1 1 d . . . C9 C 0.0882(6) -0.2446(8) 0.1389(4) 0.110(2) Uani 1 1 d . . . H9A H 0.1516 -0.2031 0.1295 0.132 Uiso 1 1 calc R . . C10 C 0.1039(7) -0.3198(10) 0.1987(5) 0.176(5) Uani 1 1 d . . . H10A H 0.1235 -0.2625 0.2311 0.264 Uiso 1 1 calc R . . H10B H 0.1549 -0.3826 0.1929 0.264 Uiso 1 1 calc R . . H10C H 0.0430 -0.3616 0.2095 0.264 Uiso 1 1 calc R . . C11 C 0.0625(7) -0.3291(9) 0.0850(5) 0.154(4) Uani 1 1 d . . . H11A H 0.0566 -0.2783 0.0484 0.231 Uiso 1 1 calc R . . H11B H 0.0005 -0.3714 0.0925 0.231 Uiso 1 1 calc R . . H11C H 0.1139 -0.3916 0.0799 0.231 Uiso 1 1 calc R . . C12 C -0.0178(5) 0.2207(8) 0.1620(3) 0.103(2) Uani 1 1 d . . . H12A H 0.0520 0.2338 0.1511 0.124 Uiso 1 1 calc R . . C13 C -0.0833(8) 0.2981(9) 0.1156(5) 0.158(4) Uani 1 1 d . . . H13A H -0.0742 0.2656 0.0747 0.237 Uiso 1 1 calc R . . H13B H -0.0643 0.3864 0.1170 0.237 Uiso 1 1 calc R . . H13C H -0.1520 0.2902 0.1266 0.237 Uiso 1 1 calc R . . C14 C -0.0329(7) 0.2742(8) 0.2270(4) 0.134(3) Uani 1 1 d . . . H14A H 0.0085 0.2284 0.2558 0.201 Uiso 1 1 calc R . . H14B H -0.1013 0.2647 0.2382 0.201 Uiso 1 1 calc R . . H14C H -0.0153 0.3630 0.2277 0.201 Uiso 1 1 calc R . . C15 C 0.4025(4) 0.1445(7) 0.1115(2) 0.0698(16) Uani 1 1 d . . . C16 C 0.4831(4) 0.0567(7) 0.1114(2) 0.0701(17) Uani 1 1 d . . . C17 C 0.5767(4) 0.1073(8) 0.1035(3) 0.085(2) Uani 1 1 d . . . H17A H 0.6308 0.0521 0.1044 0.102 Uiso 1 1 calc R . . C18 C 0.5940(5) 0.2339(9) 0.0945(3) 0.102(2) Uani 1 1 d . . . H18A H 0.6584 0.2633 0.0884 0.123 Uiso 1 1 calc R . . C19 C 0.5158(5) 0.3176(7) 0.0944(3) 0.099(2) Uani 1 1 d . . . H19A H 0.5274 0.4041 0.0881 0.119 Uiso 1 1 calc R . . C20 C 0.4196(4) 0.2751(8) 0.1035(3) 0.0844(19) Uani 1 1 d . . . C21 C 0.3371(6) 0.3761(8) 0.1049(4) 0.120(3) Uani 1 1 d . . . H21A H 0.2739 0.3305 0.1091 0.144 Uiso 1 1 calc R . . C22 C 0.3313(9) 0.4493(10) 0.0452(6) 0.176(5) Uani 1 1 d . . . H22A H 0.3208 0.3910 0.0116 0.264 Uiso 1 1 calc R . . H22B H 0.3924 0.4949 0.0393 0.264 Uiso 1 1 calc R . . H22C H 0.2771 0.5088 0.0467 0.264 Uiso 1 1 calc R . . C23 C 0.3502(7) 0.4605(10) 0.1625(5) 0.175(5) Uani 1 1 d . . . H23A H 0.2976 0.5224 0.1637 0.263 Uiso 1 1 calc R . . H23B H 0.4131 0.5035 0.1609 0.263 Uiso 1 1 calc R . . H23C H 0.3480 0.4081 0.1988 0.263 Uiso 1 1 calc R . . C24 C 0.4709(5) -0.0825(8) 0.1205(3) 0.090(2) Uani 1 1 d . . . H24A H 0.3997 -0.1023 0.1189 0.109 Uiso 1 1 calc R . . C25 C 0.5116(8) -0.1223(10) 0.1832(4) 0.148(4) Uani 1 1 d . . . H25A H 0.4787 -0.0747 0.2148 0.222 Uiso 1 1 calc R . . H25B H 0.5817 -0.1054 0.1853 0.222 Uiso 1 1 calc R . . H25C H 0.5001 -0.2118 0.1893 0.222 Uiso 1 1 calc R . . C26 C 0.5215(7) -0.1584(8) 0.0711(4) 0.126(3) Uani 1 1 d . . . H26A H 0.4956 -0.1337 0.0314 0.189 Uiso 1 1 calc R . . H26B H 0.5094 -0.2477 0.0776 0.189 Uiso 1 1 calc R . . H26C H 0.5917 -0.1424 0.0728 0.189 Uiso 1 1 calc R . . C27 C 0.714(2) 0.525(3) 0.1985(19) 0.31(2) Uani 1 1 d . . . C28 C 0.663(4) 0.574(5) 0.185(2) 0.193(18) Uani 0.50 1 d P . . C29 C 0.715(2) 0.572(3) 0.1278(19) 0.195(16) Uani 0.50 1 d P . . O3 O 0.7771(17) 0.5634(16) 0.2207(9) 0.158(7) Uani 0.50 1 d P . . 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 Ge1 0.0413(4) 0.1728(9) 0.0470(4) 0.0051(4) 0.0018(2) -0.0067(4) Si1 0.0501(9) 0.206(2) 0.0428(9) -0.0044(11) 0.0022(7) -0.0300(11) N1 0.041(2) 0.130(4) 0.046(2) 0.004(2) 0.0038(18) -0.009(2) N2 0.050(3) 0.159(5) 0.050(3) -0.008(3) 0.002(2) -0.015(3) O1 0.133(7) 0.287(12) 0.157(8) 0.000 0.097(6) 0.000 O2 0.084(5) 0.182(8) 0.172(9) 0.000 0.002(5) 0.000 C1 0.102(6) 0.324(14) 0.080(6) 0.075(7) -0.024(4) -0.029(7) C2 0.122(7) 0.291(13) 0.098(6) -0.092(7) 0.049(5) -0.084(7) C3 0.038(3) 0.108(5) 0.052(3) 0.002(3) 0.000(2) -0.010(3) C4 0.054(3) 0.093(5) 0.068(4) 0.004(3) 0.002(3) -0.005(3) C5 0.050(4) 0.121(6) 0.105(5) -0.001(4) 0.003(3) 0.014(4) C6 0.046(3) 0.133(7) 0.124(6) 0.011(5) 0.001(4) -0.021(4) C7 0.082(5) 0.092(5) 0.097(5) 0.006(4) 0.002(4) -0.017(4) C8 0.058(4) 0.115(6) 0.063(4) 0.002(4) -0.001(3) 0.017(4) C9 0.102(5) 0.132(7) 0.097(6) 0.001(5) 0.011(4) 0.025(5) C10 0.163(9) 0.214(11) 0.151(9) 0.058(8) 0.021(7) 0.105(8) C11 0.157(9) 0.144(8) 0.160(9) -0.043(7) 0.011(7) 0.038(6) C12 0.078(4) 0.133(7) 0.098(5) -0.008(5) -0.006(4) -0.004(4) C13 0.189(10) 0.129(8) 0.155(9) 0.034(6) -0.061(7) -0.021(7) C14 0.138(7) 0.155(8) 0.108(7) -0.037(6) -0.003(5) 0.010(6) C15 0.051(3) 0.114(5) 0.044(3) -0.004(3) 0.011(2) -0.008(3) C16 0.047(3) 0.116(6) 0.048(3) -0.009(3) 0.009(2) -0.005(3) C17 0.050(3) 0.137(7) 0.069(4) -0.019(4) 0.000(3) 0.006(4) C18 0.054(4) 0.142(7) 0.112(6) -0.041(5) 0.018(3) -0.025(4) C19 0.083(5) 0.103(6) 0.111(6) -0.016(4) 0.020(4) -0.019(4) C20 0.064(4) 0.123(6) 0.067(4) -0.014(4) 0.008(3) 0.007(4) C21 0.098(6) 0.119(7) 0.144(8) -0.004(6) 0.022(5) 0.019(5) C22 0.168(10) 0.165(10) 0.195(12) 0.067(8) 0.015(9) 0.048(7) C23 0.137(8) 0.197(11) 0.193(11) -0.085(9) 0.004(7) 0.062(7) C24 0.070(4) 0.125(7) 0.076(5) 0.005(4) 0.003(3) 0.000(4) C25 0.174(9) 0.191(9) 0.079(6) 0.025(6) 0.013(6) 0.037(7) C26 0.159(8) 0.124(6) 0.095(6) -0.005(5) 0.019(5) 0.005(6) C27 0.24(4) 0.19(3) 0.51(7) -0.03(2) 0.14(4) -0.07(2) C28 0.20(4) 0.21(4) 0.17(3) 0.03(3) -0.05(3) 0.03(2) C29 0.16(2) 0.106(17) 0.32(5) 0.07(2) -0.09(3) -0.052(15) O3 0.173(19) 0.108(11) 0.191(18) 0.046(9) -0.028(13) -0.050(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.799(8) . ? Ge1 N2 1.812(4) . ? Ge1 N1 1.816(4) . ? Ge1 O2 1.875(6) . ? Ge1 Si1 2.5816(19) . ? Ge1 Ge1 2.5972(14) 2 ? Si1 N1 1.735(4) . ? Si1 N2 1.744(5) . ? Si1 C2 1.869(8) . ? Si1 C1 1.876(9) . ? N1 C15 1.418(6) . ? N2 C3 1.412(6) . ? O1 Ge1 1.799(8) 2 ? O2 Ge1 1.875(6) 2 ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 C8 1.377(8) . ? C3 C4 1.404(8) . ? C4 C5 1.384(8) . ? C4 C12 1.501(9) . ? C5 C6 1.343(9) . ? C5 H5A 0.9300 . ? C6 C7 1.363(9) . ? C6 H6A 0.9300 . ? C7 C8 1.399(8) . ? C7 H7A 0.9300 . ? C8 C9 1.528(9) . ? C9 C11 1.503(10) . ? C9 C10 1.530(11) . ? C9 H9A 0.9800 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C14 1.534(10) . ? C12 C13 1.556(10) . ? C12 H12A 0.9800 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.399(8) . ? C15 C16 1.420(8) . ? C16 C17 1.378(8) . ? C16 C24 1.481(8) . ? C17 C18 1.361(9) . ? C17 H17A 0.9300 . ? C18 C19 1.370(9) . ? C18 H18A 0.9300 . ? C19 C20 1.384(8) . ? C19 H19A 0.9300 . ? C20 C21 1.535(9) . ? C21 C22 1.506(12) . ? C21 C23 1.540(12) . ? C21 H21A 0.9800 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 C26 1.503(9) . ? C24 C25 1.520(10) . ? C24 H24A 0.9800 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 0.89(5) . ? C27 O3 1.05(3) . ? C27 C29 1.61(5) . ? C27 O3 1.80(4) 2_655 ? C28 C29 1.44(6) . ? C28 O3 1.71(6) . ? O3 O3 1.47(4) 2_655 ? O3 C27 1.80(4) 2_655 ? 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 Ge1 N2 135.8(2) . . ? O1 Ge1 N1 116.3(2) . . ? N2 Ge1 N1 84.54(19) . . ? O1 Ge1 O2 90.0(3) . . ? N2 Ge1 O2 108.4(2) . . ? N1 Ge1 O2 127.02(18) . . ? O1 Ge1 Si1 140.9(3) . . ? N2 Ge1 Si1 42.41(14) . . ? N1 Ge1 Si1 42.15(13) . . ? O2 Ge1 Si1 129.1(2) . . ? O1 Ge1 Ge1 43.8(3) . 2 ? N2 Ge1 Ge1 137.41(15) . 2 ? N1 Ge1 Ge1 137.42(13) . 2 ? O2 Ge1 Ge1 46.17(19) . 2 ? Si1 Ge1 Ge1 175.03(6) . 2 ? N1 Si1 N2 89.1(2) . . ? N1 Si1 C2 113.1(4) . . ? N2 Si1 C2 116.2(3) . . ? N1 Si1 C1 115.7(4) . . ? N2 Si1 C1 113.2(3) . . ? C2 Si1 C1 108.7(5) . . ? N1 Si1 Ge1 44.61(14) . . ? N2 Si1 Ge1 44.50(15) . . ? C2 Si1 Ge1 126.6(3) . . ? C1 Si1 Ge1 124.7(3) . . ? C15 N1 Si1 134.7(3) . . ? C15 N1 Ge1 131.8(3) . . ? Si1 N1 Ge1 93.24(19) . . ? C3 N2 Si1 134.5(4) . . ? C3 N2 Ge1 132.4(3) . . ? Si1 N2 Ge1 93.1(2) . . ? Ge1 O1 Ge1 92.4(6) 2 . ? Ge1 O2 Ge1 87.7(4) 2 . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C8 C3 C4 119.8(5) . . ? C8 C3 N2 120.7(6) . . ? C4 C3 N2 119.4(6) . . ? C5 C4 C3 118.2(6) . . ? C5 C4 C12 119.2(6) . . ? C3 C4 C12 122.6(5) . . ? C6 C5 C4 122.6(6) . . ? C6 C5 H5A 118.7 . . ? C4 C5 H5A 118.7 . . ? C5 C6 C7 119.2(6) . . ? C5 C6 H6A 120.4 . . ? C7 C6 H6A 120.4 . . ? C6 C7 C8 121.1(7) . . ? C6 C7 H7A 119.4 . . ? C8 C7 H7A 119.4 . . ? C3 C8 C7 119.0(6) . . ? C3 C8 C9 123.5(6) . . ? C7 C8 C9 117.5(7) . . ? C11 C9 C8 112.4(7) . . ? C11 C9 C10 112.6(8) . . ? C8 C9 C10 110.4(6) . . ? C11 C9 H9A 107.0 . . ? C8 C9 H9A 107.0 . . ? C10 C9 H9A 107.0 . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C4 C12 C14 111.7(7) . . ? C4 C12 C13 112.2(6) . . ? C14 C12 C13 108.8(7) . . ? C4 C12 H12A 108.0 . . ? C14 C12 H12A 108.0 . . ? C13 C12 H12A 108.0 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 N1 120.3(6) . . ? C20 C15 C16 120.4(5) . . ? N1 C15 C16 119.3(6) . . ? C17 C16 C15 116.7(7) . . ? C17 C16 C24 119.8(6) . . ? C15 C16 C24 123.5(5) . . ? C18 C17 C16 123.4(6) . . ? C18 C17 H17A 118.3 . . ? C16 C17 H17A 118.3 . . ? C17 C18 C19 119.4(6) . . ? C17 C18 H18A 120.3 . . ? C19 C18 H18A 120.3 . . ? C18 C19 C20 120.8(7) . . ? C18 C19 H19A 119.6 . . ? C20 C19 H19A 119.6 . . ? C19 C20 C15 119.2(6) . . ? C19 C20 C21 117.3(7) . . ? C15 C20 C21 123.5(6) . . ? C22 C21 C20 111.4(7) . . ? C22 C21 C23 114.2(9) . . ? C20 C21 C23 109.6(7) . . ? C22 C21 H21A 107.1 . . ? C20 C21 H21A 107.1 . . ? C23 C21 H21A 107.1 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C16 C24 C26 112.0(6) . . ? C16 C24 C25 110.5(7) . . ? C26 C24 C25 109.4(7) . . ? C16 C24 H24A 108.3 . . ? C26 C24 H24A 108.3 . . ? C25 C24 H24A 108.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 O3 122(7) . . ? C28 C27 C29 63(5) . . ? O3 C27 C29 108(3) . . ? C28 C27 O3 103(6) . 2_655 ? O3 C27 O3 55(3) . 2_655 ? C29 C27 O3 149(3) . 2_655 ? C27 C28 C29 84(6) . . ? C27 C28 O3 31(4) . . ? C29 C28 O3 87(3) . . ? C28 C29 C27 33(2) . . ? C27 O3 O3 89(3) . 2_655 ? C27 O3 C28 26(3) . . ? O3 O3 C28 86(3) 2_655 . ? C27 O3 C27 114(3) . 2_655 ? O3 O3 C27 35.7(11) 2_655 2_655 ? C28 O3 C27 120(3) . 2_655 ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.206 _refine_diff_density_min -0.508 _refine_diff_density_rms 0.084 data_110721cm _database_code_depnum_ccdc_archive 'CCDC 838183' #TrackingRef 'C36 H44 N2 Pb Si.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H44 N2 Pb Si' _chemical_formula_weight 740.01 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 Tetragonal _symmetry_space_group_name_H-M P4(3)2(1)2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+3/4' 'y+1/2, -x+1/2, z+1/4' '-x+1/2, y+1/2, -z+3/4' 'x+1/2, -y+1/2, -z+1/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.4575(10) _cell_length_b 12.4575(10) _cell_length_c 43.426(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6739.2(13) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 7046 _cell_measurement_theta_min 2.157 _cell_measurement_theta_max 21.846 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.459 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 5.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1947 _exptl_absorpt_correction_T_max 0.3026 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 38768 _diffrn_reflns_av_R_equivalents 0.1244 _diffrn_reflns_av_sigmaI/netI 0.0976 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 55 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 27.00 _reflns_number_total 7339 _reflns_number_gt 5414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0415P)^2^+13.6902P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.032(12) _refine_ls_number_reflns 7339 _refine_ls_number_parameters 369 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0946 _refine_ls_R_factor_gt 0.0618 _refine_ls_wR_factor_ref 0.1233 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6739(14) -0.2359(13) 0.0533(4) 0.101(5) Uani 1 1 d . . . H1A H 0.6571 -0.2823 0.0702 0.152 Uiso 1 1 calc R . . H1B H 0.7460 -0.2097 0.0554 0.152 Uiso 1 1 calc R . . H1C H 0.6675 -0.2752 0.0343 0.152 Uiso 1 1 calc R . . C2 C 0.5970(11) -0.1426(9) 0.0529(2) 0.058(3) Uani 1 1 d . . . H2 H 0.5980 -0.1104 0.0735 0.069 Uiso 1 1 calc R . . C3 C 0.4832(11) -0.1808(12) 0.0468(3) 0.081(4) Uani 1 1 d . . . H3A H 0.4817 -0.2215 0.0280 0.121 Uiso 1 1 calc R . . H3B H 0.4365 -0.1199 0.0449 0.121 Uiso 1 1 calc R . . H3C H 0.4596 -0.2251 0.0635 0.121 Uiso 1 1 calc R . . C4 C 0.6320(9) -0.0546(9) 0.0298(2) 0.049(3) Uani 1 1 d . . . C5 C 0.6300(10) -0.0793(10) -0.0017(3) 0.064(4) Uani 1 1 d . . . H5 H 0.6085 -0.1473 -0.0081 0.076 Uiso 1 1 calc R . . C6 C 0.6590(13) -0.0056(13) -0.0231(3) 0.086(5) Uani 1 1 d . . . H6 H 0.6541 -0.0215 -0.0439 0.104 Uiso 1 1 calc R . . C7 C 0.6955(11) 0.0926(13) -0.0136(2) 0.074(4) Uani 1 1 d . . . H7 H 0.7158 0.1424 -0.0285 0.089 Uiso 1 1 calc R . . C8 C 0.7037(9) 0.1214(9) 0.0173(2) 0.046(2) Uani 1 1 d . . . C9 C 0.6733(8) 0.0452(9) 0.0396(2) 0.040(3) Uani 1 1 d . . . C10 C 0.7462(9) 0.2315(9) 0.0250(2) 0.051(3) Uani 1 1 d . . . H10 H 0.7576 0.2316 0.0473 0.061 Uiso 1 1 calc R . . C11 C 0.8553(11) 0.2549(11) 0.0108(3) 0.076(4) Uani 1 1 d . . . H11A H 0.9060 0.2018 0.0175 0.114 Uiso 1 1 calc R . . H11B H 0.8791 0.3248 0.0172 0.114 Uiso 1 1 calc R . . H11C H 0.8495 0.2530 -0.0112 0.114 Uiso 1 1 calc R . . C12 C 0.6668(12) 0.3185(11) 0.0189(3) 0.087(5) Uani 1 1 d . . . H12A H 0.6532 0.3229 -0.0028 0.130 Uiso 1 1 calc R . . H12B H 0.6951 0.3857 0.0261 0.130 Uiso 1 1 calc R . . H12C H 0.6011 0.3029 0.0296 0.130 Uiso 1 1 calc R . . C13 C 0.9354(15) 0.4235(16) 0.0876(3) 0.130(8) Uani 1 1 d . . . H13A H 0.9273 0.4379 0.0660 0.195 Uiso 1 1 calc R . . H13B H 0.9892 0.3692 0.0905 0.195 Uiso 1 1 calc R . . H13C H 0.9569 0.4880 0.0980 0.195 Uiso 1 1 calc R . . C14 C 0.8290(10) 0.3843(10) 0.1007(2) 0.061(3) Uani 1 1 d . . . H14 H 0.8060 0.3250 0.0875 0.073 Uiso 1 1 calc R . . C15 C 0.7471(16) 0.4652(11) 0.0982(4) 0.129(8) Uani 1 1 d . . . H15A H 0.6837 0.4418 0.1088 0.194 Uiso 1 1 calc R . . H15B H 0.7305 0.4768 0.0768 0.194 Uiso 1 1 calc R . . H15C H 0.7724 0.5309 0.1071 0.194 Uiso 1 1 calc R . . C16 C 0.8417(9) 0.3368(9) 0.1328(2) 0.042(2) Uani 1 1 d . . . C17 C 0.8808(9) 0.4026(10) 0.1557(3) 0.059(3) Uani 1 1 d . . . H17 H 0.8988 0.4727 0.1503 0.070 Uiso 1 1 calc R . . C18 C 0.8952(10) 0.3725(10) 0.1856(3) 0.054(3) Uani 1 1 d . . . H18 H 0.9225 0.4197 0.2002 0.064 Uiso 1 1 calc R . . C19 C 0.8674(9) 0.2693(12) 0.1931(2) 0.057(3) Uani 1 1 d . . . H19 H 0.8770 0.2466 0.2133 0.069 Uiso 1 1 calc R . . C20 C 0.8263(8) 0.1984(9) 0.1722(2) 0.042(3) Uani 1 1 d . . . C21 C 0.8089(7) 0.2306(8) 0.14101(19) 0.035(2) Uani 1 1 d . . . C22 C 0.7968(11) 0.0855(10) 0.1821(2) 0.062(4) Uani 1 1 d . . . H22 H 0.7561 0.0527 0.1652 0.075 Uiso 1 1 calc R . . C23 C 0.8899(19) 0.0176(13) 0.1879(4) 0.131(7) Uani 1 1 d . . . H23A H 0.9397 0.0239 0.1712 0.197 Uiso 1 1 calc R . . H23B H 0.8672 -0.0558 0.1898 0.197 Uiso 1 1 calc R . . H23C H 0.9241 0.0398 0.2067 0.197 Uiso 1 1 calc R . . C24 C 0.7246(15) 0.0879(15) 0.2101(3) 0.117(6) Uani 1 1 d . . . H24A H 0.7092 0.0158 0.2165 0.176 Uiso 1 1 calc R . . H24B H 0.6587 0.1239 0.2050 0.176 Uiso 1 1 calc R . . H24C H 0.7599 0.1256 0.2265 0.176 Uiso 1 1 calc R . . C25 C 0.7684(9) -0.0782(8) 0.1178(2) 0.041(3) Uani 1 1 d . . . C26 C 0.6735(9) -0.1086(10) 0.1312(2) 0.051(3) Uani 1 1 d . . . H26 H 0.6153 -0.0623 0.1296 0.061 Uiso 1 1 calc R . . C27 C 0.6591(12) -0.2030(11) 0.1469(3) 0.068(4) Uani 1 1 d . . . H27 H 0.5939 -0.2187 0.1563 0.082 Uiso 1 1 calc R . . C28 C 0.7436(18) -0.2743(13) 0.1484(3) 0.094(6) Uani 1 1 d . . . H28 H 0.7351 -0.3389 0.1588 0.113 Uiso 1 1 calc R . . C29 C 0.8379(16) -0.2518(11) 0.1350(3) 0.086(5) Uani 1 1 d . . . H29 H 0.8933 -0.3018 0.1356 0.103 Uiso 1 1 calc R . . C30 C 0.8531(10) -0.1525(9) 0.1202(3) 0.055(3) Uani 1 1 d . . . H30 H 0.9198 -0.1359 0.1118 0.066 Uiso 1 1 calc R . . C31 C 0.9188(8) 0.0501(8) 0.0780(2) 0.039(2) Uani 1 1 d . . . C32 C 0.9991(9) 0.1236(12) 0.0844(3) 0.072(4) Uani 1 1 d . . . H32 H 0.9870 0.1762 0.0992 0.086 Uiso 1 1 calc R . . C33 C 1.0933(11) 0.1212(14) 0.0699(3) 0.098(6) Uani 1 1 d . . . H33 H 1.1461 0.1703 0.0754 0.118 Uiso 1 1 calc R . . C34 C 1.1142(12) 0.0485(15) 0.0473(3) 0.100(6) Uani 1 1 d . . . H34 H 1.1808 0.0468 0.0376 0.120 Uiso 1 1 calc R . . C35 C 1.0358(12) -0.0211(13) 0.0392(3) 0.085(5) Uani 1 1 d . . . H35 H 1.0482 -0.0709 0.0236 0.102 Uiso 1 1 calc R . . C36 C 0.9381(10) -0.0190(11) 0.0538(3) 0.066(4) Uani 1 1 d . . . H36 H 0.8839 -0.0649 0.0472 0.079 Uiso 1 1 calc R . . N1 N 0.6795(7) 0.0708(6) 0.07145(16) 0.0365(19) Uani 1 1 d . . . N2 N 0.7595(6) 0.1644(7) 0.11920(15) 0.0339(18) Uani 1 1 d . . . Pb1 Pb 0.60756(3) 0.21225(3) 0.093984(9) 0.04267(12) Uani 1 1 d . . . Si1 Si 0.7830(2) 0.0535(2) 0.09693(6) 0.0337(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.100(14) 0.081(13) 0.123(13) 0.015(10) -0.015(10) -0.004(10) C2 0.073(9) 0.056(9) 0.044(6) -0.017(5) -0.005(6) -0.016(7) C3 0.069(10) 0.080(11) 0.094(10) -0.011(8) 0.005(8) -0.015(8) C4 0.053(8) 0.051(7) 0.042(5) -0.003(5) -0.001(5) -0.007(6) C5 0.073(10) 0.058(9) 0.059(7) -0.028(6) 0.001(6) -0.017(7) C6 0.137(15) 0.089(12) 0.033(6) -0.021(7) 0.005(7) -0.006(10) C7 0.077(10) 0.100(12) 0.046(6) 0.002(7) 0.002(6) -0.016(9) C8 0.041(7) 0.054(8) 0.043(5) -0.002(5) -0.012(5) 0.002(6) C9 0.021(6) 0.059(8) 0.039(5) -0.013(5) -0.004(4) 0.002(5) C10 0.066(8) 0.057(8) 0.030(5) 0.000(5) 0.008(5) -0.007(6) C11 0.079(11) 0.061(10) 0.088(9) -0.001(7) 0.006(8) -0.018(7) C12 0.083(11) 0.050(9) 0.128(12) 0.017(8) 0.003(9) 0.012(8) C13 0.154(18) 0.157(19) 0.080(10) 0.011(10) -0.004(10) -0.088(15) C14 0.072(9) 0.051(8) 0.058(7) -0.010(6) -0.018(6) -0.020(7) C15 0.19(2) 0.038(9) 0.163(15) 0.020(10) -0.100(15) -0.016(10) C16 0.041(7) 0.034(6) 0.051(6) -0.002(5) -0.010(5) -0.005(5) C17 0.048(7) 0.053(7) 0.075(7) -0.012(7) -0.013(7) -0.005(6) C18 0.041(7) 0.058(9) 0.061(7) -0.031(6) -0.007(6) 0.006(6) C19 0.036(7) 0.093(11) 0.043(6) -0.011(6) -0.002(5) 0.009(6) C20 0.043(7) 0.041(7) 0.041(5) -0.012(5) -0.005(4) 0.001(5) C21 0.023(6) 0.042(6) 0.042(5) -0.016(4) -0.007(4) 0.000(4) C22 0.086(10) 0.063(9) 0.038(6) 0.002(5) -0.019(6) -0.019(8) C23 0.18(2) 0.058(12) 0.159(17) -0.007(11) -0.013(16) 0.001(14) C24 0.138(17) 0.131(16) 0.082(9) 0.042(10) 0.008(10) -0.037(13) C25 0.054(8) 0.035(7) 0.035(5) -0.005(4) -0.001(5) 0.000(5) C26 0.050(7) 0.047(7) 0.056(6) -0.002(6) 0.004(5) 0.004(6) C27 0.080(10) 0.065(10) 0.059(7) 0.007(7) -0.007(6) -0.021(8) C28 0.159(19) 0.057(10) 0.066(9) 0.014(7) -0.007(10) -0.002(11) C29 0.119(15) 0.047(10) 0.092(10) 0.006(8) -0.015(10) 0.029(9) C30 0.056(9) 0.033(7) 0.076(8) 0.000(6) 0.011(6) 0.005(5) C31 0.030(6) 0.049(7) 0.038(5) -0.005(4) -0.003(4) 0.003(5) C32 0.023(6) 0.109(12) 0.083(8) -0.044(8) 0.009(6) -0.027(7) C33 0.035(8) 0.140(16) 0.119(11) -0.058(11) 0.009(8) -0.027(9) C34 0.047(9) 0.161(17) 0.091(9) -0.057(10) 0.030(8) -0.023(10) C35 0.072(11) 0.117(14) 0.065(8) -0.040(8) 0.007(7) -0.023(9) C36 0.036(7) 0.071(10) 0.092(9) -0.035(7) 0.022(6) -0.005(6) N1 0.041(5) 0.027(5) 0.042(4) -0.008(3) -0.001(4) 0.002(3) N2 0.013(4) 0.048(5) 0.041(4) -0.008(4) -0.005(3) 0.004(3) Pb1 0.0307(2) 0.0447(3) 0.05261(19) -0.0123(2) -0.00599(19) 0.00572(19) Si1 0.0277(14) 0.0337(15) 0.0398(13) -0.0070(11) -0.0008(13) 0.0026(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.506(19) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.519(17) . ? C2 C4 1.551(15) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.403(14) . ? C4 C9 1.412(14) . ? C5 C6 1.353(17) . ? C5 H5 0.9300 . ? C6 C7 1.369(18) . ? C6 H6 0.9300 . ? C7 C8 1.394(14) . ? C7 H7 0.9300 . ? C8 C9 1.406(14) . ? C8 C10 1.508(15) . ? C9 N1 1.423(11) . ? C10 C12 1.490(16) . ? C10 C11 1.520(16) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.524(19) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.44(2) . ? C14 C16 1.523(15) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.377(14) . ? C16 C21 1.429(14) . ? C17 C18 1.363(15) . ? C17 H17 0.9300 . ? C18 C19 1.371(17) . ? C18 H18 0.9300 . ? C19 C20 1.365(14) . ? C19 H19 0.9300 . ? C20 C21 1.428(12) . ? C20 C22 1.516(16) . ? C21 N2 1.398(11) . ? C22 C23 1.46(2) . ? C22 C24 1.512(18) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.372(14) . ? C25 C30 1.407(15) . ? C25 Si1 1.883(10) . ? C26 C27 1.370(16) . ? C26 H26 0.9300 . ? C27 C28 1.38(2) . ? C27 H27 0.9300 . ? C28 C29 1.34(2) . ? C28 H28 0.9300 . ? C29 C30 1.408(18) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.382(14) . ? C31 C32 1.384(14) . ? C31 Si1 1.881(10) . ? C32 C33 1.332(16) . ? C32 H32 0.9300 . ? C33 C34 1.362(18) . ? C33 H33 0.9300 . ? C34 C35 1.353(19) . ? C34 H34 0.9300 . ? C35 C36 1.371(17) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? N1 Si1 1.712(8) . ? N1 Pb1 2.206(8) . ? N2 Si1 1.711(8) . ? N2 Pb1 2.267(7) . ? Pb1 Si1 2.950(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C1 C2 C3 110.7(11) . . ? C1 C2 C4 111.9(11) . . ? C3 C2 C4 111.7(10) . . ? C1 C2 H2 107.5 . . ? C3 C2 H2 107.5 . . ? C4 C2 H2 107.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 119.6(10) . . ? C5 C4 C2 118.2(10) . . ? C9 C4 C2 122.0(9) . . ? C6 C5 C4 120.9(11) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C7 119.3(11) . . ? C5 C6 H6 120.3 . . ? C7 C6 H6 120.3 . . ? C6 C7 C8 122.9(12) . . ? C6 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? C7 C8 C9 117.9(11) . . ? C7 C8 C10 118.3(10) . . ? C9 C8 C10 123.8(8) . . ? C8 C9 C4 119.1(9) . . ? C8 C9 N1 120.2(9) . . ? C4 C9 N1 120.7(9) . . ? C12 C10 C8 112.9(10) . . ? C12 C10 C11 112.4(11) . . ? C8 C10 C11 113.5(10) . . ? C12 C10 H10 105.7 . . ? C8 C10 H10 105.7 . . ? C11 C10 H10 105.7 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C16 114.6(12) . . ? C15 C14 C13 111.4(14) . . ? C16 C14 C13 112.2(11) . . ? C15 C14 H14 106.0 . . ? C16 C14 H14 106.0 . . ? C13 C14 H14 106.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 C21 118.3(9) . . ? C17 C16 C14 117.7(10) . . ? C21 C16 C14 123.9(9) . . ? C18 C17 C16 124.7(12) . . ? C18 C17 H17 117.7 . . ? C16 C17 H17 117.7 . . ? C17 C18 C19 116.8(10) . . ? C17 C18 H18 121.6 . . ? C19 C18 H18 121.6 . . ? C20 C19 C18 123.0(10) . . ? C20 C19 H19 118.5 . . ? C18 C19 H19 118.5 . . ? C19 C20 C21 120.3(11) . . ? C19 C20 C22 120.2(10) . . ? C21 C20 C22 119.5(9) . . ? N2 C21 C20 122.9(9) . . ? N2 C21 C16 120.2(8) . . ? C20 C21 C16 116.8(8) . . ? C23 C22 C24 110.2(12) . . ? C23 C22 C20 113.3(13) . . ? C24 C22 C20 110.7(11) . . ? C23 C22 H22 107.5 . . ? C24 C22 H22 107.5 . . ? C20 C22 H22 107.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 115.6(10) . . ? C26 C25 Si1 121.9(9) . . ? C30 C25 Si1 122.5(9) . . ? C27 C26 C25 124.1(12) . . ? C27 C26 H26 117.9 . . ? C25 C26 H26 117.9 . . ? C26 C27 C28 118.5(13) . . ? C26 C27 H27 120.8 . . ? C28 C27 H27 120.8 . . ? C29 C28 C27 120.9(14) . . ? C29 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C28 C29 C30 120.0(14) . . ? C28 C29 H29 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 C29 120.7(12) . . ? C25 C30 H30 119.6 . . ? C29 C30 H30 119.6 . . ? C36 C31 C32 116.0(10) . . ? C36 C31 Si1 120.2(8) . . ? C32 C31 Si1 123.2(8) . . ? C33 C32 C31 121.8(12) . . ? C33 C32 H32 119.1 . . ? C31 C32 H32 119.1 . . ? C32 C33 C34 121.7(14) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C35 C34 C33 118.3(13) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C34 C35 C36 120.6(13) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 121.2(12) . . ? C35 C36 H36 119.4 . . ? C31 C36 H36 119.4 . . ? C9 N1 Si1 129.9(7) . . ? C9 N1 Pb1 126.0(6) . . ? Si1 N1 Pb1 96.9(3) . . ? C21 N2 Si1 141.6(7) . . ? C21 N2 Pb1 122.6(6) . . ? Si1 N2 Pb1 94.7(3) . . ? N1 Pb1 N2 70.4(3) . . ? N1 Pb1 Si1 35.2(2) . . ? N2 Pb1 Si1 35.3(2) . . ? N2 Si1 N1 97.8(4) . . ? N2 Si1 C31 114.7(4) . . ? N1 Si1 C31 113.4(4) . . ? N2 Si1 C25 114.5(4) . . ? N1 Si1 C25 110.4(4) . . ? C31 Si1 C25 106.1(5) . . ? N2 Si1 Pb1 50.0(2) . . ? N1 Si1 Pb1 48.0(3) . . ? C31 Si1 Pb1 131.5(3) . . ? C25 Si1 Pb1 122.3(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C4 C5 66.5(15) . . . . ? C3 C2 C4 C5 -58.2(15) . . . . ? C1 C2 C4 C9 -108.4(13) . . . . ? C3 C2 C4 C9 126.9(11) . . . . ? C9 C4 C5 C6 -5.4(19) . . . . ? C2 C4 C5 C6 179.6(13) . . . . ? C4 C5 C6 C7 3(2) . . . . ? C5 C6 C7 C8 -1(2) . . . . ? C6 C7 C8 C9 0(2) . . . . ? C6 C7 C8 C10 179.3(13) . . . . ? C7 C8 C9 C4 -2.6(16) . . . . ? C10 C8 C9 C4 178.5(10) . . . . ? C7 C8 C9 N1 -179.7(11) . . . . ? C10 C8 C9 N1 1.4(16) . . . . ? C5 C4 C9 C8 5.1(16) . . . . ? C2 C4 C9 C8 179.9(10) . . . . ? C5 C4 C9 N1 -177.9(10) . . . . ? C2 C4 C9 N1 -3.1(16) . . . . ? C7 C8 C10 C12 74.6(15) . . . . ? C9 C8 C10 C12 -106.5(12) . . . . ? C7 C8 C10 C11 -54.9(14) . . . . ? C9 C8 C10 C11 124.1(11) . . . . ? C15 C14 C16 C17 -67.9(15) . . . . ? C13 C14 C16 C17 60.4(16) . . . . ? C15 C14 C16 C21 108.0(13) . . . . ? C13 C14 C16 C21 -123.7(13) . . . . ? C21 C16 C17 C18 2.9(17) . . . . ? C14 C16 C17 C18 179.0(11) . . . . ? C16 C17 C18 C19 -0.6(18) . . . . ? C17 C18 C19 C20 -0.5(17) . . . . ? C18 C19 C20 C21 -0.8(17) . . . . ? C18 C19 C20 C22 -179.7(11) . . . . ? C19 C20 C21 N2 -175.0(9) . . . . ? C22 C20 C21 N2 3.9(15) . . . . ? C19 C20 C21 C16 3.1(14) . . . . ? C22 C20 C21 C16 -178.0(10) . . . . ? C17 C16 C21 N2 174.1(9) . . . . ? C14 C16 C21 N2 -1.7(15) . . . . ? C17 C16 C21 C20 -4.1(14) . . . . ? C14 C16 C21 C20 -179.9(10) . . . . ? C19 C20 C22 C23 -72.6(15) . . . . ? C21 C20 C22 C23 108.5(13) . . . . ? C19 C20 C22 C24 51.7(16) . . . . ? C21 C20 C22 C24 -127.2(11) . . . . ? C30 C25 C26 C27 1.7(15) . . . . ? Si1 C25 C26 C27 -179.4(9) . . . . ? C25 C26 C27 C28 -2.5(18) . . . . ? C26 C27 C28 C29 0(2) . . . . ? C27 C28 C29 C30 2(2) . . . . ? C26 C25 C30 C29 1.1(16) . . . . ? Si1 C25 C30 C29 -177.8(9) . . . . ? C28 C29 C30 C25 -3(2) . . . . ? C36 C31 C32 C33 -6(2) . . . . ? Si1 C31 C32 C33 -177.8(12) . . . . ? C31 C32 C33 C34 2(3) . . . . ? C32 C33 C34 C35 1(3) . . . . ? C33 C34 C35 C36 -1(3) . . . . ? C34 C35 C36 C31 -3(2) . . . . ? C32 C31 C36 C35 6.5(19) . . . . ? Si1 C31 C36 C35 178.6(11) . . . . ? C8 C9 N1 Si1 -90.3(11) . . . . ? C4 C9 N1 Si1 92.7(11) . . . . ? C8 C9 N1 Pb1 53.0(12) . . . . ? C4 C9 N1 Pb1 -124.0(9) . . . . ? C20 C21 N2 Si1 -74.2(14) . . . . ? C16 C21 N2 Si1 107.8(12) . . . . ? C20 C21 N2 Pb1 121.1(9) . . . . ? C16 C21 N2 Pb1 -56.9(11) . . . . ? C9 N1 Pb1 N2 -149.1(8) . . . . ? Si1 N1 Pb1 N2 3.4(3) . . . . ? C9 N1 Pb1 Si1 -152.5(9) . . . . ? C21 N2 Pb1 N1 167.2(8) . . . . ? Si1 N2 Pb1 N1 -3.4(3) . . . . ? C21 N2 Pb1 Si1 170.5(9) . . . . ? C21 N2 Si1 N1 -163.0(11) . . . . ? Pb1 N2 Si1 N1 4.1(4) . . . . ? C21 N2 Si1 C31 -42.7(12) . . . . ? Pb1 N2 Si1 C31 124.4(4) . . . . ? C21 N2 Si1 C25 80.4(12) . . . . ? Pb1 N2 Si1 C25 -112.5(4) . . . . ? C21 N2 Si1 Pb1 -167.1(12) . . . . ? C9 N1 Si1 N2 146.6(9) . . . . ? Pb1 N1 Si1 N2 -4.2(4) . . . . ? C9 N1 Si1 C31 25.3(10) . . . . ? Pb1 N1 Si1 C31 -125.5(4) . . . . ? C9 N1 Si1 C25 -93.6(9) . . . . ? Pb1 N1 Si1 C25 115.6(4) . . . . ? C9 N1 Si1 Pb1 150.8(10) . . . . ? C36 C31 Si1 N2 -163.7(9) . . . . ? C32 C31 Si1 N2 7.8(12) . . . . ? C36 C31 Si1 N1 -52.4(11) . . . . ? C32 C31 Si1 N1 119.0(10) . . . . ? C36 C31 Si1 C25 68.9(10) . . . . ? C32 C31 Si1 C25 -119.7(10) . . . . ? C36 C31 Si1 Pb1 -106.2(10) . . . . ? C32 C31 Si1 Pb1 65.3(11) . . . . ? C26 C25 Si1 N2 60.2(9) . . . . ? C30 C25 Si1 N2 -121.0(8) . . . . ? C26 C25 Si1 N1 -49.0(9) . . . . ? C30 C25 Si1 N1 129.9(8) . . . . ? C26 C25 Si1 C31 -172.2(8) . . . . ? C30 C25 Si1 C31 6.6(9) . . . . ? C26 C25 Si1 Pb1 3.4(9) . . . . ? C30 C25 Si1 Pb1 -177.8(7) . . . . ? N1 Pb1 Si1 N2 174.5(5) . . . . ? N2 Pb1 Si1 N1 -174.5(5) . . . . ? N1 Pb1 Si1 C31 85.3(5) . . . . ? N2 Pb1 Si1 C31 -89.3(5) . . . . ? N1 Pb1 Si1 C25 -89.1(5) . . . . ? N2 Pb1 Si1 C25 96.4(5) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.432 _refine_diff_density_min -1.313 _refine_diff_density_rms 0.133 data_3b _database_code_depnum_ccdc_archive 'CCDC 838184' #TrackingRef '- complex3b.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H52 Ge N2 O Si' _chemical_formula_weight 677.52 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 '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 10.8195(15) _cell_length_b 18.818(3) _cell_length_c 19.240(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.039(2) _cell_angle_gamma 90.00 _cell_volume 3816.1(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 3631 _cell_measurement_theta_min 2.214 _cell_measurement_theta_max 23.074 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.179 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 0.865 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7516 _exptl_absorpt_correction_T_max 0.9340 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19903 _diffrn_reflns_av_R_equivalents 0.0437 _diffrn_reflns_av_sigmaI/netI 0.0618 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 25.50 _reflns_number_total 7076 _reflns_number_gt 4705 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.Hydrogen atoms attached to anisotropically refined atoms were placed in geometrically idealized positions and refined using a fiding model [0.930(aromatic CH)U~iso~(H) = 1.2U~eq~(C) and 0.970\%A(methyl CH~3~), U~iso~(H) = 1.5U~eq~(C)]. the C-C bonds of the THF molecule were refined in 1.467~1.483 ? distance restraint. In total three geometric restraints were used in modeling the solvent. ; _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^)+(0.0757P)^2^+0.4521P] 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 7076 _refine_ls_number_parameters 414 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0888 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1495 _refine_ls_wR_factor_gt 0.1317 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.032 _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 C1 C -0.0604(6) 0.6238(4) 0.3766(3) 0.129(3) Uani 1 1 d . . . H1A H -0.0390 0.5947 0.4186 0.194 Uiso 1 1 calc R . . H1B H -0.1469 0.6392 0.3695 0.194 Uiso 1 1 calc R . . H1C H -0.0055 0.6645 0.3822 0.194 Uiso 1 1 calc R . . C2 C -0.0442(4) 0.5811(2) 0.3124(2) 0.0692(12) Uani 1 1 d . . . H2 H -0.0707 0.6116 0.2704 0.083 Uiso 1 1 calc R . . C3 C -0.1292(6) 0.5147(3) 0.3000(4) 0.140(3) Uani 1 1 d . . . H3A H -0.1158 0.4895 0.2590 0.210 Uiso 1 1 calc R . . H3B H -0.2165 0.5288 0.2922 0.210 Uiso 1 1 calc R . . H3C H -0.1083 0.4845 0.3412 0.210 Uiso 1 1 calc R . . C4 C 0.0922(4) 0.56136(18) 0.31702(18) 0.0519(9) Uani 1 1 d . . . C5 C 0.1509(5) 0.5131(2) 0.3677(2) 0.0650(11) Uani 1 1 d . . . H5 H 0.1056 0.4949 0.3994 0.078 Uiso 1 1 calc R . . C6 C 0.2735(5) 0.4909(2) 0.3731(2) 0.0695(12) Uani 1 1 d . . . H6 H 0.3108 0.4585 0.4081 0.083 Uiso 1 1 calc R . . C7 C 0.3394(4) 0.51731(19) 0.3261(2) 0.0646(11) Uani 1 1 d . . . H7 H 0.4219 0.5016 0.3289 0.077 Uiso 1 1 calc R . . C8 C 0.2876(4) 0.56669(18) 0.27455(19) 0.0506(9) Uani 1 1 d . . . C9 C 0.1619(3) 0.59007(16) 0.27001(17) 0.0433(8) Uani 1 1 d . . . C10 C 0.3658(4) 0.5904(2) 0.2223(2) 0.0639(11) Uani 1 1 d . . . H10 H 0.3225 0.6312 0.1960 0.077 Uiso 1 1 calc R . . C11 C 0.4991(5) 0.6142(3) 0.2585(3) 0.1022(17) Uani 1 1 d . . . H11A H 0.4943 0.6511 0.2924 0.153 Uiso 1 1 calc R . . H11B H 0.5414 0.6321 0.2233 0.153 Uiso 1 1 calc R . . H11C H 0.5457 0.5746 0.2828 0.153 Uiso 1 1 calc R . . C12 C 0.3703(6) 0.5320(3) 0.1682(3) 0.1018(17) Uani 1 1 d . . . H12A H 0.4129 0.4911 0.1923 0.153 Uiso 1 1 calc R . . H12B H 0.4154 0.5488 0.1338 0.153 Uiso 1 1 calc R . . H12C H 0.2854 0.5192 0.1444 0.153 Uiso 1 1 calc R . . C13 C 0.3267(6) 0.6945(3) 0.0252(3) 0.127(2) Uani 1 1 d . . . H13A H 0.2530 0.6646 0.0136 0.191 Uiso 1 1 calc R . . H13B H 0.3996 0.6662 0.0457 0.191 Uiso 1 1 calc R . . H13C H 0.3394 0.7171 -0.0174 0.191 Uiso 1 1 calc R . . C14 C 0.3075(4) 0.7515(2) 0.0791(2) 0.0753(13) Uani 1 1 d . . . H14 H 0.2955 0.7267 0.1219 0.090 Uiso 1 1 calc R . . C15 C 0.4260(5) 0.7973(3) 0.1011(3) 0.116(2) Uani 1 1 d . . . H15A H 0.4374 0.8247 0.0609 0.174 Uiso 1 1 calc R . . H15B H 0.4986 0.7674 0.1173 0.174 Uiso 1 1 calc R . . H15C H 0.4168 0.8288 0.1389 0.174 Uiso 1 1 calc R . . C16 C 0.1896(4) 0.7941(2) 0.05063(18) 0.0529(9) Uani 1 1 d . . . C17 C 0.1914(4) 0.8421(2) -0.0050(2) 0.0652(11) Uani 1 1 d . . . H17 H 0.2637 0.8454 -0.0233 0.078 Uiso 1 1 calc R . . C18 C 0.0898(5) 0.8839(2) -0.0325(2) 0.0650(11) Uani 1 1 d . . . H18 H 0.0929 0.9153 -0.0694 0.078 Uiso 1 1 calc R . . C19 C -0.0165(4) 0.8797(2) -0.0062(2) 0.0601(10) Uani 1 1 d . . . H19 H -0.0850 0.9091 -0.0248 0.072 Uiso 1 1 calc R . . C20 C -0.0249(3) 0.83213(19) 0.04811(18) 0.0480(8) Uani 1 1 d . . . C21 C 0.0792(3) 0.78897(17) 0.07680(16) 0.0425(8) Uani 1 1 d . . . C22 C -0.1444(4) 0.8307(2) 0.0754(2) 0.0648(11) Uani 1 1 d . . . H22 H -0.1416 0.7883 0.1052 0.078 Uiso 1 1 calc R . . C23 C -0.2631(5) 0.8252(4) 0.0142(3) 0.137(3) Uani 1 1 d . . . H23A H -0.2683 0.8662 -0.0159 0.205 Uiso 1 1 calc R . . H23B H -0.3373 0.8227 0.0336 0.205 Uiso 1 1 calc R . . H23C H -0.2577 0.7831 -0.0132 0.205 Uiso 1 1 calc R . . C24 C -0.1521(6) 0.8950(3) 0.1220(3) 0.119(2) Uani 1 1 d . . . H24A H -0.0797 0.8957 0.1615 0.178 Uiso 1 1 calc R . . H24B H -0.2282 0.8925 0.1395 0.178 Uiso 1 1 calc R . . H24C H -0.1531 0.9376 0.0943 0.178 Uiso 1 1 calc R . . C25 C -0.0296(3) 0.77076(18) 0.26084(18) 0.0459(8) Uani 1 1 d . . . C26 C -0.1534(4) 0.7486(2) 0.2387(2) 0.0597(10) Uani 1 1 d . . . H26 H -0.1724 0.7133 0.2041 0.072 Uiso 1 1 calc R . . C27 C -0.2512(4) 0.7768(3) 0.2660(3) 0.0807(14) Uani 1 1 d . . . H27 H -0.3340 0.7606 0.2502 0.097 Uiso 1 1 calc R . . C28 C -0.2233(5) 0.8290(3) 0.3165(3) 0.1053(19) Uani 1 1 d . . . H28 H -0.2881 0.8487 0.3349 0.126 Uiso 1 1 calc R . . C29 C -0.1034(5) 0.8523(3) 0.3401(3) 0.1030(19) Uani 1 1 d . . . H29 H -0.0858 0.8878 0.3746 0.124 Uiso 1 1 calc R . . C30 C -0.0062(4) 0.8231(2) 0.3127(2) 0.0745(13) Uani 1 1 d . . . H30 H 0.0764 0.8392 0.3296 0.089 Uiso 1 1 calc R . . C31 C 0.2484(3) 0.77818(17) 0.27243(17) 0.0408(8) Uani 1 1 d . . . C32 C 0.2808(4) 0.8453(2) 0.2534(2) 0.0620(11) Uani 1 1 d . . . H32 H 0.2348 0.8653 0.2112 0.074 Uiso 1 1 calc R . . C33 C 0.3784(4) 0.8836(2) 0.2945(3) 0.0768(13) Uani 1 1 d . . . H33 H 0.3962 0.9291 0.2807 0.092 Uiso 1 1 calc R . . C34 C 0.4497(4) 0.8545(2) 0.3559(3) 0.0724(12) Uani 1 1 d . . . H34 H 0.5168 0.8800 0.3834 0.087 Uiso 1 1 calc R . . C35 C 0.4217(4) 0.7877(2) 0.3766(2) 0.0720(12) Uani 1 1 d . . . H35 H 0.4692 0.7678 0.4184 0.086 Uiso 1 1 calc R . . C36 C 0.3217(4) 0.75005(19) 0.3346(2) 0.0578(10) Uani 1 1 d . . . H36 H 0.3035 0.7047 0.3487 0.069 Uiso 1 1 calc R . . C37 C 0.7567(10) 0.6324(6) 0.0321(6) 0.256(7) Uani 1 1 d D . . H37A H 0.8064 0.6403 -0.0033 0.307 Uiso 1 1 calc R . . H37B H 0.7102 0.6755 0.0372 0.307 Uiso 1 1 calc R . . C38 C 0.6689(11) 0.5716(7) 0.0116(8) 0.321(10) Uani 1 1 d D . . H38A H 0.6029 0.5700 0.0384 0.386 Uiso 1 1 calc R . . H38B H 0.6316 0.5700 -0.0392 0.386 Uiso 1 1 calc R . . C39 C 0.7664(16) 0.5170(6) 0.0343(7) 0.305(9) Uani 1 1 d D . . H39A H 0.8369 0.5207 0.0110 0.366 Uiso 1 1 calc R . . H39B H 0.7330 0.4690 0.0310 0.366 Uiso 1 1 calc R . . C40 C 0.7947(13) 0.5460(7) 0.1079(5) 0.262(7) Uani 1 1 d D . . H40A H 0.7198 0.5465 0.1277 0.314 Uiso 1 1 calc R . . H40B H 0.8615 0.5193 0.1393 0.314 Uiso 1 1 calc R . . Ge1 Ge 0.07707(4) 0.63809(2) 0.11865(2) 0.05311(16) Uani 1 1 d . . . N1 N 0.0722(3) 0.73752(14) 0.13069(13) 0.0421(7) Uani 1 1 d . . . N2 N 0.1075(3) 0.64245(13) 0.21907(15) 0.0445(7) Uani 1 1 d . . . O1 O 0.8331(5) 0.6128(3) 0.0963(3) 0.1496(17) Uani 1 1 d . . . Si1 Si 0.10130(9) 0.73402(5) 0.22251(5) 0.0382(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.134(6) 0.190(7) 0.078(4) 0.015(4) 0.054(4) 0.060(5) C2 0.071(3) 0.072(3) 0.070(3) 0.021(2) 0.028(2) -0.005(2) C3 0.087(4) 0.120(5) 0.206(8) 0.039(5) 0.019(5) -0.033(4) C4 0.070(3) 0.0408(19) 0.044(2) 0.0002(16) 0.0109(19) -0.0068(18) C5 0.096(4) 0.047(2) 0.050(2) 0.0061(18) 0.011(2) -0.012(2) C6 0.101(4) 0.043(2) 0.051(2) 0.0081(18) -0.009(2) 0.004(2) C7 0.075(3) 0.043(2) 0.065(3) -0.0007(19) -0.008(2) 0.011(2) C8 0.060(2) 0.0368(18) 0.051(2) -0.0057(16) 0.0033(18) 0.0022(17) C9 0.058(2) 0.0300(16) 0.0375(18) -0.0034(14) 0.0014(17) 0.0000(16) C10 0.055(2) 0.063(3) 0.071(3) 0.007(2) 0.010(2) 0.012(2) C11 0.070(3) 0.128(5) 0.111(4) -0.007(4) 0.026(3) -0.012(3) C12 0.112(4) 0.116(4) 0.084(4) -0.024(3) 0.036(3) 0.008(3) C13 0.150(6) 0.112(5) 0.144(5) 0.016(4) 0.083(5) 0.060(4) C14 0.063(3) 0.099(3) 0.074(3) 0.026(3) 0.035(2) 0.020(3) C15 0.057(3) 0.176(6) 0.116(5) 0.029(4) 0.021(3) 0.005(4) C16 0.061(2) 0.059(2) 0.0396(19) -0.0001(17) 0.0140(18) 0.0024(19) C17 0.077(3) 0.076(3) 0.048(2) 0.003(2) 0.024(2) -0.005(2) C18 0.084(3) 0.064(3) 0.043(2) 0.0123(19) 0.008(2) -0.006(2) C19 0.069(3) 0.054(2) 0.048(2) 0.0128(18) -0.005(2) 0.006(2) C20 0.053(2) 0.0453(19) 0.0423(19) 0.0043(16) 0.0033(17) 0.0008(18) C21 0.049(2) 0.0468(19) 0.0297(17) 0.0017(14) 0.0056(16) 0.0018(16) C22 0.049(2) 0.067(3) 0.076(3) 0.019(2) 0.010(2) 0.012(2) C23 0.052(3) 0.214(7) 0.128(5) 0.065(5) -0.010(3) -0.010(4) C24 0.146(5) 0.070(3) 0.170(6) 0.005(4) 0.097(5) 0.026(3) C25 0.047(2) 0.048(2) 0.045(2) -0.0006(16) 0.0165(17) 0.0018(17) C26 0.053(2) 0.064(2) 0.065(3) 0.000(2) 0.019(2) -0.001(2) C27 0.046(3) 0.107(4) 0.093(4) 0.003(3) 0.023(3) 0.001(3) C28 0.073(4) 0.136(5) 0.122(5) -0.030(4) 0.056(4) 0.013(4) C29 0.083(4) 0.123(5) 0.114(4) -0.057(4) 0.045(3) 0.000(3) C30 0.066(3) 0.085(3) 0.081(3) -0.026(3) 0.034(2) -0.001(2) C31 0.0421(19) 0.0395(18) 0.0422(18) 0.0034(15) 0.0124(16) 0.0056(15) C32 0.059(3) 0.059(2) 0.064(3) 0.0188(19) 0.006(2) -0.008(2) C33 0.070(3) 0.066(3) 0.092(3) 0.010(3) 0.012(3) -0.025(2) C34 0.049(2) 0.077(3) 0.089(3) -0.018(3) 0.009(2) -0.012(2) C35 0.072(3) 0.069(3) 0.062(3) -0.004(2) -0.013(2) 0.002(2) C36 0.065(3) 0.046(2) 0.055(2) 0.0060(17) -0.003(2) -0.0032(19) C37 0.199(11) 0.262(14) 0.246(12) 0.150(11) -0.079(9) 0.003(9) C38 0.200(11) 0.265(15) 0.39(2) -0.175(15) -0.159(12) 0.009(11) C39 0.45(2) 0.155(10) 0.249(14) -0.083(10) -0.056(15) 0.074(11) C40 0.368(18) 0.245(13) 0.151(9) 0.057(9) 0.014(10) -0.153(12) Ge1 0.0656(3) 0.0485(2) 0.0432(2) -0.00470(17) 0.00795(19) 0.0037(2) N1 0.0486(17) 0.0420(15) 0.0361(15) 0.0018(12) 0.0101(13) 0.0061(13) N2 0.0537(18) 0.0369(15) 0.0426(16) 0.0025(12) 0.0100(14) 0.0012(13) O1 0.171(5) 0.122(4) 0.138(4) -0.011(3) -0.002(4) -0.034(4) Si1 0.0408(5) 0.0379(5) 0.0360(5) 0.0028(4) 0.0090(4) 0.0032(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.516(6) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C4 1.505(5) . ? C2 C3 1.537(7) . ? C2 H2 0.9800 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.378(5) . ? C4 C9 1.410(5) . ? C5 C6 1.372(6) . ? C5 H5 0.9300 . ? C6 C7 1.366(6) . ? C6 H6 0.9300 . ? C7 C8 1.382(5) . ? C7 H7 0.9300 . ? C8 C9 1.413(5) . ? C8 C10 1.519(5) . ? C9 N2 1.421(4) . ? C10 C11 1.521(6) . ? C10 C12 1.522(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.539(7) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C16 1.501(5) . ? C14 C15 1.524(7) . ? C14 H14 0.9800 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C21 1.400(5) . ? C16 C17 1.404(5) . ? C17 C18 1.358(6) . ? C17 H17 0.9300 . ? C18 C19 1.360(6) . ? C18 H18 0.9300 . ? C19 C20 1.394(5) . ? C19 H19 0.9300 . ? C20 C21 1.397(5) . ? C20 C22 1.501(5) . ? C21 N1 1.433(4) . ? C22 C24 1.519(7) . ? C22 C23 1.537(6) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.376(5) . ? C25 C30 1.385(5) . ? C25 Si1 1.870(3) . ? C26 C27 1.388(6) . ? C26 H26 0.9300 . ? C27 C28 1.366(7) . ? C27 H27 0.9300 . ? C28 C29 1.348(7) . ? C28 H28 0.9300 . ? C29 C30 1.391(6) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C36 1.383(5) . ? C31 C32 1.383(5) . ? C31 Si1 1.859(4) . ? C32 C33 1.372(6) . ? C32 H32 0.9300 . ? C33 C34 1.370(6) . ? C33 H33 0.9300 . ? C34 C35 1.374(6) . ? C34 H34 0.9300 . ? C35 C36 1.389(5) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O1 1.372(9) . ? C37 C38 1.483(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.467(8) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.483(8) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 O1 1.358(9) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? Ge1 N2 1.887(3) . ? Ge1 N1 1.888(3) . ? Ge1 Si1 2.6616(10) . ? N1 Si1 1.724(3) . ? N2 Si1 1.726(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C4 C2 C1 112.0(4) . . ? C4 C2 C3 110.7(4) . . ? C1 C2 C3 112.4(4) . . ? C4 C2 H2 107.1 . . ? C1 C2 H2 107.1 . . ? C3 C2 H2 107.1 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C9 118.6(4) . . ? C5 C4 C2 119.6(4) . . ? C9 C4 C2 121.8(3) . . ? C6 C5 C4 122.6(4) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C7 C6 C5 118.6(4) . . ? C7 C6 H6 120.7 . . ? C5 C6 H6 120.7 . . ? C6 C7 C8 122.2(4) . . ? C6 C7 H7 118.9 . . ? C8 C7 H7 118.9 . . ? C7 C8 C9 118.8(4) . . ? C7 C8 C10 118.4(4) . . ? C9 C8 C10 122.7(3) . . ? C4 C9 C8 119.2(3) . . ? C4 C9 N2 120.7(3) . . ? C8 C9 N2 120.1(3) . . ? C8 C10 C11 113.3(4) . . ? C8 C10 C12 110.4(4) . . ? C11 C10 C12 110.7(4) . . ? C8 C10 H10 107.4 . . ? C11 C10 H10 107.4 . . ? C12 C10 H10 107.4 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C16 C14 C15 113.1(4) . . ? C16 C14 C13 111.0(4) . . ? C15 C14 C13 110.4(4) . . ? C16 C14 H14 107.4 . . ? C15 C14 H14 107.4 . . ? C13 C14 H14 107.4 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 118.6(4) . . ? C21 C16 C14 123.7(3) . . ? C17 C16 C14 117.7(4) . . ? C18 C17 C16 121.3(4) . . ? C18 C17 H17 119.3 . . ? C16 C17 H17 119.3 . . ? C17 C18 C19 119.9(4) . . ? C17 C18 H18 120.0 . . ? C19 C18 H18 120.0 . . ? C18 C19 C20 121.4(4) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 119.1(3) . . ? C19 C20 C22 118.7(3) . . ? C21 C20 C22 122.2(3) . . ? C20 C21 C16 119.6(3) . . ? C20 C21 N1 120.6(3) . . ? C16 C21 N1 119.7(3) . . ? C20 C22 C24 111.0(4) . . ? C20 C22 C23 111.7(4) . . ? C24 C22 C23 111.0(5) . . ? C20 C22 H22 107.6 . . ? C24 C22 H22 107.6 . . ? C23 C22 H22 107.6 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 116.4(3) . . ? C26 C25 Si1 122.5(3) . . ? C30 C25 Si1 121.1(3) . . ? C25 C26 C27 122.6(4) . . ? C25 C26 H26 118.7 . . ? C27 C26 H26 118.7 . . ? C28 C27 C26 118.6(4) . . ? C28 C27 H27 120.7 . . ? C26 C27 H27 120.7 . . ? C29 C28 C27 121.1(4) . . ? C29 C28 H28 119.5 . . ? C27 C28 H28 119.5 . . ? C28 C29 C30 119.7(5) . . ? C28 C29 H29 120.2 . . ? C30 C29 H29 120.2 . . ? C25 C30 C29 121.6(4) . . ? C25 C30 H30 119.2 . . ? C29 C30 H30 119.2 . . ? C36 C31 C32 116.7(3) . . ? C36 C31 Si1 122.2(3) . . ? C32 C31 Si1 120.7(3) . . ? C33 C32 C31 122.3(4) . . ? C33 C32 H32 118.8 . . ? C31 C32 H32 118.8 . . ? C34 C33 C32 119.9(4) . . ? C34 C33 H33 120.1 . . ? C32 C33 H33 120.1 . . ? C33 C34 C35 119.8(4) . . ? C33 C34 H34 120.1 . . ? C35 C34 H34 120.1 . . ? C34 C35 C36 119.4(4) . . ? C34 C35 H35 120.3 . . ? C36 C35 H35 120.3 . . ? C31 C36 C35 121.8(4) . . ? C31 C36 H36 119.1 . . ? C35 C36 H36 119.1 . . ? O1 C37 C38 104.5(7) . . ? O1 C37 H37A 110.8 . . ? C38 C37 H37A 110.8 . . ? O1 C37 H37B 110.8 . . ? C38 C37 H37B 110.8 . . ? H37A C37 H37B 108.9 . . ? C39 C38 C37 95.0(9) . . ? C39 C38 H38A 112.7 . . ? C37 C38 H38A 112.7 . . ? C39 C38 H38B 112.7 . . ? C37 C38 H38B 112.7 . . ? H38A C38 H38B 110.2 . . ? C38 C39 C40 90.3(9) . . ? C38 C39 H39A 113.6 . . ? C40 C39 H39A 113.6 . . ? C38 C39 H39B 113.6 . . ? C40 C39 H39B 113.6 . . ? H39A C39 H39B 110.9 . . ? O1 C40 C39 100.9(8) . . ? O1 C40 H40A 111.6 . . ? C39 C40 H40A 111.6 . . ? O1 C40 H40B 111.6 . . ? C39 C40 H40B 111.6 . . ? H40A C40 H40B 109.4 . . ? N2 Ge1 N1 80.47(11) . . ? N2 Ge1 Si1 40.27(8) . . ? N1 Ge1 Si1 40.21(8) . . ? C21 N1 Si1 137.7(2) . . ? C21 N1 Ge1 125.0(2) . . ? Si1 N1 Ge1 94.83(12) . . ? C9 N2 Si1 132.8(2) . . ? C9 N2 Ge1 128.7(2) . . ? Si1 N2 Ge1 94.79(12) . . ? C40 O1 C37 104.6(7) . . ? N1 Si1 N2 89.91(13) . . ? N1 Si1 C31 116.71(14) . . ? N2 Si1 C31 115.45(15) . . ? N1 Si1 C25 114.22(14) . . ? N2 Si1 C25 115.06(15) . . ? C31 Si1 C25 105.50(15) . . ? N1 Si1 Ge1 44.96(9) . . ? N2 Si1 Ge1 44.95(9) . . ? C31 Si1 Ge1 128.23(10) . . ? C25 Si1 Ge1 126.27(12) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C4 C5 68.7(5) . . . . ? C3 C2 C4 C5 -57.6(5) . . . . ? C1 C2 C4 C9 -112.3(4) . . . . ? C3 C2 C4 C9 121.4(4) . . . . ? C9 C4 C5 C6 -1.4(6) . . . . ? C2 C4 C5 C6 177.6(4) . . . . ? C4 C5 C6 C7 -0.5(6) . . . . ? C5 C6 C7 C8 1.4(6) . . . . ? C6 C7 C8 C9 -0.5(6) . . . . ? C6 C7 C8 C10 -177.1(3) . . . . ? C5 C4 C9 C8 2.3(5) . . . . ? C2 C4 C9 C8 -176.7(3) . . . . ? C5 C4 C9 N2 -177.1(3) . . . . ? C2 C4 C9 N2 4.0(5) . . . . ? C7 C8 C9 C4 -1.4(5) . . . . ? C10 C8 C9 C4 175.0(3) . . . . ? C7 C8 C9 N2 178.0(3) . . . . ? C10 C8 C9 N2 -5.6(5) . . . . ? C7 C8 C10 C11 -51.1(5) . . . . ? C9 C8 C10 C11 132.5(4) . . . . ? C7 C8 C10 C12 73.8(5) . . . . ? C9 C8 C10 C12 -102.7(4) . . . . ? C15 C14 C16 C21 -126.5(4) . . . . ? C13 C14 C16 C21 108.8(4) . . . . ? C15 C14 C16 C17 53.0(5) . . . . ? C13 C14 C16 C17 -71.7(5) . . . . ? C21 C16 C17 C18 1.1(6) . . . . ? C14 C16 C17 C18 -178.4(4) . . . . ? C16 C17 C18 C19 0.0(7) . . . . ? C17 C18 C19 C20 -1.2(6) . . . . ? C18 C19 C20 C21 1.2(6) . . . . ? C18 C19 C20 C22 179.3(4) . . . . ? C19 C20 C21 C16 0.0(5) . . . . ? C22 C20 C21 C16 -178.1(3) . . . . ? C19 C20 C21 N1 -177.5(3) . . . . ? C22 C20 C21 N1 4.5(5) . . . . ? C17 C16 C21 C20 -1.1(5) . . . . ? C14 C16 C21 C20 178.4(4) . . . . ? C17 C16 C21 N1 176.4(3) . . . . ? C14 C16 C21 N1 -4.1(5) . . . . ? C19 C20 C22 C24 -74.5(5) . . . . ? C21 C20 C22 C24 103.6(5) . . . . ? C19 C20 C22 C23 50.0(6) . . . . ? C21 C20 C22 C23 -131.9(5) . . . . ? C30 C25 C26 C27 0.3(6) . . . . ? Si1 C25 C26 C27 -178.6(3) . . . . ? C25 C26 C27 C28 0.4(7) . . . . ? C26 C27 C28 C29 -0.6(9) . . . . ? C27 C28 C29 C30 0.1(10) . . . . ? C26 C25 C30 C29 -0.8(7) . . . . ? Si1 C25 C30 C29 178.1(4) . . . . ? C28 C29 C30 C25 0.6(9) . . . . ? C36 C31 C32 C33 -1.6(6) . . . . ? Si1 C31 C32 C33 170.8(3) . . . . ? C31 C32 C33 C34 1.7(7) . . . . ? C32 C33 C34 C35 -1.1(7) . . . . ? C33 C34 C35 C36 0.5(7) . . . . ? C32 C31 C36 C35 1.0(6) . . . . ? Si1 C31 C36 C35 -171.3(3) . . . . ? C34 C35 C36 C31 -0.5(6) . . . . ? O1 C37 C38 C39 -41.2(14) . . . . ? C37 C38 C39 C40 58.5(13) . . . . ? C38 C39 C40 O1 -61.3(13) . . . . ? C20 C21 N1 Si1 -89.5(4) . . . . ? C16 C21 N1 Si1 93.0(4) . . . . ? C20 C21 N1 Ge1 113.2(3) . . . . ? C16 C21 N1 Ge1 -64.2(4) . . . . ? N2 Ge1 N1 C21 165.1(3) . . . . ? Si1 Ge1 N1 C21 164.9(3) . . . . ? N2 Ge1 N1 Si1 0.22(12) . . . . ? C4 C9 N2 Si1 88.2(4) . . . . ? C8 C9 N2 Si1 -91.1(4) . . . . ? C4 C9 N2 Ge1 -119.1(3) . . . . ? C8 C9 N2 Ge1 61.6(4) . . . . ? N1 Ge1 N2 C9 -160.5(3) . . . . ? Si1 Ge1 N2 C9 -160.3(4) . . . . ? N1 Ge1 N2 Si1 -0.22(12) . . . . ? C39 C40 O1 C37 36.9(13) . . . . ? C38 C37 O1 C40 2.7(14) . . . . ? C21 N1 Si1 N2 -161.7(3) . . . . ? Ge1 N1 Si1 N2 -0.24(13) . . . . ? C21 N1 Si1 C31 -43.0(4) . . . . ? Ge1 N1 Si1 C31 118.46(14) . . . . ? C21 N1 Si1 C25 80.7(4) . . . . ? Ge1 N1 Si1 C25 -117.88(15) . . . . ? C21 N1 Si1 Ge1 -161.4(4) . . . . ? C9 N2 Si1 N1 159.2(3) . . . . ? Ge1 N2 Si1 N1 0.24(13) . . . . ? C9 N2 Si1 C31 39.4(4) . . . . ? Ge1 N2 Si1 C31 -119.56(14) . . . . ? C9 N2 Si1 C25 -83.9(3) . . . . ? Ge1 N2 Si1 C25 117.13(15) . . . . ? C9 N2 Si1 Ge1 159.0(4) . . . . ? C36 C31 Si1 N1 -142.3(3) . . . . ? C32 C31 Si1 N1 45.6(3) . . . . ? C36 C31 Si1 N2 -38.6(3) . . . . ? C32 C31 Si1 N2 149.4(3) . . . . ? C36 C31 Si1 C25 89.7(3) . . . . ? C32 C31 Si1 C25 -82.4(3) . . . . ? C36 C31 Si1 Ge1 -90.0(3) . . . . ? C32 C31 Si1 Ge1 97.9(3) . . . . ? C26 C25 Si1 N1 52.7(3) . . . . ? C30 C25 Si1 N1 -126.2(3) . . . . ? C26 C25 Si1 N2 -49.3(4) . . . . ? C30 C25 Si1 N2 131.8(3) . . . . ? C26 C25 Si1 C31 -177.8(3) . . . . ? C30 C25 Si1 C31 3.3(4) . . . . ? C26 C25 Si1 Ge1 1.9(4) . . . . ? C30 C25 Si1 Ge1 -177.0(3) . . . . ? N2 Ge1 Si1 N1 -179.66(19) . . . . ? N1 Ge1 Si1 N2 179.66(19) . . . . ? N2 Ge1 Si1 C31 89.15(19) . . . . ? N1 Ge1 Si1 C31 -91.20(18) . . . . ? N2 Ge1 Si1 C25 -90.50(19) . . . . ? N1 Ge1 Si1 C25 89.16(18) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.532 _refine_diff_density_min -0.330 _refine_diff_density_rms 0.057