Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'John Nixon' 'Mahmoud M Al-Ktaifani' 'Peter B Hitchcock' 'Michael Franz Lappert' 'Philip Uiterweerd' _publ_contact_author_name 'John Nixon' _publ_contact_author_address ; Department of Chemistry University of Sussex School of Life Sciences BRIGHTON Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email J.NIXON@SUSSEX.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Specific insertion reactions of a germylene, stannylene and plumbylene into the unique P-P bond of the hexaphospha-pentaprismane cage, P6C4tBu4: Crystal and Molecular structures of P6C4tBu4ER2 (E = Ge, Sn, R = N(SiMe3)2; E = Pb, R = (C6H3(NMe2)2 -2,6) ; _publ_requested_category FM data_c855 _database_code_depnum_ccdc_archive 'CCDC 674809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H33 N4 Pb' _chemical_formula_weight 572.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M ' P2(1)/c ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.714(4) _cell_length_b 10.324(3) _cell_length_c 17.259(5) _cell_angle_alpha 90.00 _cell_angle_beta 109.372(4) _cell_angle_gamma 90.00 _cell_volume 2305.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 1200 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1124 _exptl_absorpt_coefficient_mu 7.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 1.67 _exptl_absorpt_correction_T_max 27.26 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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 (AXS Bruker)' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14598 _diffrn_reflns_av_R_equivalents 0.0494 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 28.71 _reflns_number_total 5471 _reflns_number_gt 4226 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick,1997)' _computing_molecular_graphics 'ORTEP3 for Windows (L. J. Farrugia, 1997)' _computing_publication_material 'WINGX (L.J. Farrugia,1999)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0554P)^2^+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 5471 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0365 _refine_ls_wR_factor_ref 0.0962 _refine_ls_wR_factor_gt 0.0837 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _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 0.2351(4) 0.0014(5) 0.3073(3) 0.0282(11) Uani 1 1 d . . . C2 C 0.2231(4) 0.1334(5) 0.3247(3) 0.0310(11) Uani 1 1 d . . . C3 C 0.2815(5) 0.1816(6) 0.4030(4) 0.0397(13) Uani 1 1 d . . . H3 H 0.2773 0.2699 0.4149 0.048 Uiso 1 1 calc R . . C4 C 0.3443(5) 0.1011(6) 0.4621(4) 0.0440(14) Uani 1 1 d . . . H4 H 0.3831 0.1352 0.5137 0.053 Uiso 1 1 calc R . . C5 C 0.3510(5) -0.0298(6) 0.4466(3) 0.0399(13) Uani 1 1 d . . . H5 H 0.3920 -0.0858 0.4874 0.048 Uiso 1 1 calc R . . C6 C 0.2957(4) -0.0754(5) 0.3695(3) 0.0307(11) Uani 1 1 d . . . C7 C 0.3145(4) -0.1554(4) 0.1503(3) 0.0294(11) Uani 1 1 d . . . C8 C 0.3141(4) -0.0382(5) 0.1100(3) 0.0302(11) Uani 1 1 d . . . C9 C 0.3916(5) -0.0021(5) 0.0802(3) 0.0381(13) Uani 1 1 d . . . H9 H 0.3899 0.0787 0.0547 0.046 Uiso 1 1 calc R . . C10 C 0.4725(5) -0.0884(6) 0.0887(4) 0.0429(14) Uani 1 1 d . . . H10 H 0.5271 -0.0650 0.0700 0.051 Uiso 1 1 calc R . . C11 C 0.4730(4) -0.2072(6) 0.1242(3) 0.0394(13) Uani 1 1 d . . . H11 H 0.5278 -0.2646 0.1289 0.047 Uiso 1 1 calc R . . C12 C 0.3934(4) -0.2450(5) 0.1537(3) 0.0329(12) Uani 1 1 d . . . C13 C 0.0565(6) 0.1623(6) 0.2136(5) 0.061(2) Uani 1 1 d . . . H13A H 0.0679 0.0868 0.1842 0.091 Uiso 1 1 calc R . . H13B H 0.0197 0.2278 0.1745 0.091 Uiso 1 1 calc R . . H13C H 0.0158 0.1378 0.2477 0.091 Uiso 1 1 calc R . . C14 C 0.1509(7) 0.3509(5) 0.2849(5) 0.062(2) Uani 1 1 d . . . H14A H 0.1232 0.3594 0.3296 0.093 Uiso 1 1 calc R . . H14B H 0.1065 0.3966 0.2370 0.093 Uiso 1 1 calc R . . H14C H 0.2198 0.3877 0.3012 0.093 Uiso 1 1 calc R . . C15 C 0.4012(4) -0.2642(5) 0.3657(3) 0.0404(13) Uani 1 1 d . . . H15A H 0.4362 -0.2167 0.3341 0.061 Uiso 1 1 calc R . . H15B H 0.3978 -0.3552 0.3510 0.061 Uiso 1 1 calc R . . H15C H 0.4391 -0.2545 0.4238 0.061 Uiso 1 1 calc R . . C16 C 0.2406(5) -0.2915(6) 0.3919(4) 0.0463(15) Uani 1 1 d . . . H16A H 0.2364 -0.3807 0.3735 0.069 Uiso 1 1 calc R . . H16B H 0.1713 -0.2573 0.3808 0.069 Uiso 1 1 calc R . . H16C H 0.2777 -0.2876 0.4505 0.069 Uiso 1 1 calc R . . C17 C 0.4790(6) -0.4560(6) 0.1938(4) 0.0547(18) Uani 1 1 d . . . H17A H 0.4697 -0.5353 0.2206 0.082 Uiso 1 1 calc R . . H17B H 0.5437 -0.4155 0.2258 0.082 Uiso 1 1 calc R . . H17C H 0.4806 -0.4758 0.1393 0.082 Uiso 1 1 calc R . . C18 C 0.2977(6) -0.4317(6) 0.1771(5) 0.0612(19) Uani 1 1 d . . . H18A H 0.2640 -0.3908 0.2120 0.092 Uiso 1 1 calc R . . H18B H 0.3103 -0.5222 0.1920 0.092 Uiso 1 1 calc R . . H18C H 0.2536 -0.4250 0.1202 0.092 Uiso 1 1 calc R . . C19 C 0.1490(5) 0.0328(6) 0.0173(4) 0.0489(15) Uani 1 1 d . . . H19A H 0.1801 0.0643 -0.0221 0.073 Uiso 1 1 calc R . . H19B H 0.0882 0.0840 0.0132 0.073 Uiso 1 1 calc R . . H19C H 0.1294 -0.0572 0.0058 0.073 Uiso 1 1 calc R . . C20 C 0.2521(6) 0.1810(6) 0.1208(4) 0.0492(16) Uani 1 1 d . . . H20A H 0.3017 0.1875 0.1758 0.074 Uiso 1 1 calc R . . H20B H 0.1905 0.2298 0.1177 0.074 Uiso 1 1 calc R . . H20C H 0.2823 0.2158 0.0817 0.074 Uiso 1 1 calc R . . C21 C 0.0701(6) 0.5148(7) 0.9596(4) 0.0571(18) Uani 1 1 d . . . H21 H 0.1177 0.5253 0.9315 0.069 Uiso 1 1 calc R . . C22 C 0.0238(6) 0.3983(6) 0.9589(5) 0.0577(19) Uani 1 1 d . . . H22 H 0.0404 0.3279 0.9310 0.069 Uiso 1 1 calc R . . C23 C 0.0472(7) 0.6173(6) 1.0013(5) 0.065(2) Uani 1 1 d . . . H23 H 0.0799 0.6977 1.0026 0.078 Uiso 1 1 calc R . . N1 N 0.1554(4) 0.2139(4) 0.2649(3) 0.0437(12) Uani 1 1 d . . . N2 N 0.2958(3) -0.2131(4) 0.3476(3) 0.0318(10) Uani 1 1 d . . . N3 N 0.3939(4) -0.3681(4) 0.1874(3) 0.0441(12) Uani 1 1 d . . . N4 N 0.2245(4) 0.0442(4) 0.1013(3) 0.0335(10) Uani 1 1 d . . . Pb1 Pb 0.173801(15) -0.139542(18) 0.196400(12) 0.03102(8) 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 0.030(3) 0.032(3) 0.025(3) -0.001(2) 0.012(2) 0.001(2) C2 0.030(3) 0.034(3) 0.034(3) 0.001(2) 0.016(2) 0.000(2) C3 0.041(3) 0.037(3) 0.046(3) -0.014(3) 0.021(3) -0.008(3) C4 0.039(3) 0.052(3) 0.036(3) -0.013(3) 0.006(3) -0.002(3) C5 0.037(3) 0.052(3) 0.028(3) -0.002(3) 0.007(2) 0.004(3) C6 0.029(3) 0.036(3) 0.031(3) -0.006(2) 0.015(2) 0.001(2) C7 0.032(3) 0.032(3) 0.027(3) -0.003(2) 0.014(2) -0.002(2) C8 0.035(3) 0.033(2) 0.026(3) -0.006(2) 0.013(2) -0.004(2) C9 0.045(4) 0.038(3) 0.037(3) -0.003(2) 0.021(3) -0.007(3) C10 0.038(3) 0.056(3) 0.041(3) -0.007(3) 0.022(3) -0.007(3) C11 0.030(3) 0.051(3) 0.038(3) -0.009(3) 0.012(2) 0.005(3) C12 0.036(3) 0.035(3) 0.029(3) -0.007(2) 0.011(2) 0.000(2) C13 0.055(5) 0.058(4) 0.062(5) 0.005(3) 0.010(4) 0.019(4) C14 0.091(6) 0.036(3) 0.065(5) 0.005(3) 0.034(5) 0.014(4) C15 0.039(3) 0.041(3) 0.039(3) 0.003(3) 0.009(3) 0.014(3) C16 0.053(4) 0.046(3) 0.047(4) 0.006(3) 0.026(3) -0.006(3) C17 0.065(5) 0.058(4) 0.043(4) 0.008(3) 0.021(3) 0.026(4) C18 0.076(5) 0.034(3) 0.083(5) 0.002(3) 0.040(4) -0.002(3) C19 0.047(4) 0.059(4) 0.039(3) 0.010(3) 0.012(3) 0.006(3) C20 0.065(5) 0.033(3) 0.055(4) -0.003(3) 0.026(4) -0.003(3) C21 0.052(4) 0.064(4) 0.064(5) -0.008(4) 0.030(4) -0.009(4) C22 0.068(5) 0.045(4) 0.068(5) -0.012(3) 0.032(4) 0.000(3) C23 0.086(6) 0.041(4) 0.080(6) -0.009(3) 0.043(5) -0.019(4) N1 0.057(3) 0.035(3) 0.041(3) 0.004(2) 0.018(3) 0.013(2) N2 0.034(3) 0.033(2) 0.030(2) 0.0044(18) 0.0118(19) 0.004(2) N3 0.053(3) 0.039(3) 0.045(3) 0.001(2) 0.023(3) 0.011(2) N4 0.039(3) 0.032(2) 0.031(2) 0.0030(18) 0.013(2) 0.001(2) Pb1 0.02859(12) 0.03469(12) 0.03205(12) -0.00530(9) 0.01311(8) -0.00330(9) _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 C6 1.372(7) . ? C1 C2 1.416(7) . ? C1 Pb1 2.328(5) . ? C2 N1 1.408(7) . ? C2 C3 1.413(8) . ? C3 C4 1.375(9) . ? C4 C5 1.387(8) . ? C5 C6 1.377(7) . ? C6 N2 1.471(7) . ? C7 C8 1.393(7) . ? C7 C12 1.410(7) . ? C7 Pb1 2.325(5) . ? C8 C9 1.378(7) . ? C8 N4 1.460(7) . ? C9 C10 1.391(8) . ? C10 C11 1.370(9) . ? C11 C12 1.405(7) . ? C12 N3 1.396(7) . ? C13 N1 1.453(9) . ? C14 N1 1.462(7) . ? C15 N2 1.471(7) . ? C16 N2 1.484(6) . ? C17 N3 1.453(8) . ? C18 N3 1.431(8) . ? C19 N4 1.480(7) . ? C20 N4 1.472(7) . ? C21 C22 1.358(9) . ? C21 C23 1.374(9) . ? C22 C23 1.375(10) 3_567 ? C23 C22 1.375(10) 3_567 ? N2 Pb1 2.699(4) . ? N4 Pb1 2.744(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C6 C1 C2 118.2(5) . . ? C6 C1 Pb1 104.0(3) . . ? C2 C1 Pb1 137.8(4) . . ? N1 C2 C3 121.3(5) . . ? N1 C2 C1 120.5(5) . . ? C3 C2 C1 118.3(5) . . ? C4 C3 C2 120.9(5) . . ? C3 C4 C5 120.7(6) . . ? C6 C5 C4 118.0(6) . . ? C1 C6 C5 123.7(5) . . ? C1 C6 N2 114.2(4) . . ? C5 C6 N2 122.1(5) . . ? C8 C7 C12 117.8(5) . . ? C8 C7 Pb1 104.1(3) . . ? C12 C7 Pb1 138.1(4) . . ? C9 C8 C7 123.0(5) . . ? C9 C8 N4 122.1(5) . . ? C7 C8 N4 114.9(4) . . ? C8 C9 C10 118.3(5) . . ? C11 C10 C9 120.4(5) . . ? C10 C11 C12 121.4(5) . . ? N3 C12 C11 120.4(5) . . ? N3 C12 C7 120.9(5) . . ? C11 C12 C7 118.7(5) . . ? C22 C21 C23 120.0(6) . . ? C21 C22 C23 120.3(6) . 3_567 ? C21 C23 C22 119.7(6) . 3_567 ? C2 N1 C13 119.1(5) . . ? C2 N1 C14 117.9(5) . . ? C13 N1 C14 113.2(6) . . ? C15 N2 C6 112.2(4) . . ? C15 N2 C16 109.2(4) . . ? C6 N2 C16 110.4(4) . . ? C15 N2 Pb1 123.8(3) . . ? C6 N2 Pb1 85.6(3) . . ? C16 N2 Pb1 113.2(4) . . ? C12 N3 C18 119.2(5) . . ? C12 N3 C17 119.6(5) . . ? C18 N3 C17 114.0(5) . . ? C8 N4 C20 113.1(5) . . ? C8 N4 C19 110.2(4) . . ? C20 N4 C19 110.0(5) . . ? C8 N4 Pb1 84.7(3) . . ? C20 N4 Pb1 128.6(3) . . ? C19 N4 Pb1 107.3(3) . . ? C7 Pb1 C1 102.19(17) . . ? C7 Pb1 N2 89.55(16) . . ? C1 Pb1 N2 56.11(15) . . ? C7 Pb1 N4 55.94(15) . . ? C1 Pb1 N4 88.03(15) . . ? N2 Pb1 N4 124.99(13) . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 28.71 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.418 _refine_diff_density_min -2.902 _refine_diff_density_rms 0.207 # Attachment 'feb3601.cif' data_feb3601 _database_code_depnum_ccdc_archive 'CCDC 674810' _audit_creation_date 2001-03-09T09:53:23-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H72 Ge N2 P6 Si4' _chemical_formula_sum 'C32 H72 Ge N2 P6 Si4' _chemical_formula_weight 855.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 18.0331(4) _cell_length_b 18.1166(5) _cell_length_c 24.3208(7) _cell_angle_alpha 82.831(2) _cell_angle_beta 69.414(2) _cell_angle_gamma 65.093(2) _cell_volume 6743.9(3) _cell_formula_units_Z 6 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 29464 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.05 _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2736 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.026 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.838 _exptl_absorpt_correction_T_max 0.931 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 46958 _diffrn_reflns_av_R_equivalents 0.0634 _diffrn_reflns_av_unetI/netI 0.0966 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 23675 _reflns_number_gt 16354 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; ******* I have looked for any higher symmetry space group that might relate the three molecules but could not find one. If anyone can point out a matrix transformation that could produce a higher symmetry space group I will be happy to re-refine the structure. ******* 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^)+(0.0221P)^2^+12.4804P] 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_number_reflns 23675 _refine_ls_number_parameters 1222 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0919 _refine_ls_R_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.1072 _refine_ls_wR_factor_gt 0.0926 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.421 _refine_diff_density_min -0.428 _refine_diff_density_rms 0.092 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ge Ge 0.24025(3) 0.57652(3) 0.191929(19) 0.01768(11) Uani 1 1 d . A 1 P1 P 0.07550(7) 0.55404(7) 0.39152(5) 0.0220(3) Uani 1 1 d . A 1 P2 P 0.14347(7) 0.68358(7) 0.31571(5) 0.0209(3) Uani 1 1 d . A 1 P3 P 0.10093(7) 0.62510(7) 0.26672(5) 0.0198(3) Uani 1 1 d . A 1 P4 P 0.21020(7) 0.58249(7) 0.39516(5) 0.0222(3) Uani 1 1 d . A 1 P5 P 0.22280(7) 0.45745(7) 0.30766(5) 0.0213(3) Uani 1 1 d . A 1 P6 P 0.30942(7) 0.51920(7) 0.26505(5) 0.0204(3) Uani 1 1 d . A 1 Si1 Si 0.18635(8) 0.76836(7) 0.15788(6) 0.0242(3) Uani 1 1 d . A 1 Si2 Si 0.36386(8) 0.64537(8) 0.09537(6) 0.0255(3) Uani 1 1 d . A 1 Si3 Si 0.33464(7) 0.39091(7) 0.13699(5) 0.0234(3) Uani 1 1 d . A 1 Si4 Si 0.20948(8) 0.52152(8) 0.08689(5) 0.0233(3) Uani 1 1 d . A 1 N1 N 0.2606(2) 0.6641(2) 0.14893(15) 0.0211(8) Uani 1 1 d . A 1 N2 N 0.2638(2) 0.4956(2) 0.13955(14) 0.0186(8) Uani 1 1 d . A 1 C1 C 0.0980(3) 0.6465(3) 0.39014(18) 0.0223(10) Uani 1 1 d . A 1 C2 C 0.1068(2) 0.5324(3) 0.31112(18) 0.0199(10) Uani 1 1 d . A 1 C3 C 0.1934(3) 0.4905(3) 0.38519(19) 0.0220(10) Uani 1 1 d . A 1 C4 C 0.2574(2) 0.6081(2) 0.31652(18) 0.0191(9) Uani 1 1 d . A 1 C5 C 0.0252(3) 0.7130(3) 0.43709(19) 0.0248(10) Uani 1 1 d . A 1 C6 C -0.0581(3) 0.7425(3) 0.4228(2) 0.0361(13) Uani 1 1 d . A 1 H6A H -0.0731 0.6965 0.4228 0.054 Uiso 1 1 calc R A 1 H6B H -0.0499 0.7668 0.384 0.054 Uiso 1 1 calc R A 1 H6C H -0.105 0.7834 0.4524 0.054 Uiso 1 1 calc R A 1 C7 C 0.0124(3) 0.6752(3) 0.49800(19) 0.0327(12) Uani 1 1 d . A 1 H7A H 0.0661 0.6567 0.5073 0.049 Uiso 1 1 calc R A 1 H7B H -0.0021 0.6288 0.498 0.049 Uiso 1 1 calc R A 1 H7C H -0.0348 0.7161 0.5275 0.049 Uiso 1 1 calc R A 1 C8 C 0.0490(3) 0.7843(3) 0.4377(2) 0.0310(11) Uani 1 1 d . A 1 H8A H 0.1026 0.7647 0.4472 0.046 Uiso 1 1 calc R A 1 H8B H 0.0021 0.8251 0.4674 0.046 Uiso 1 1 calc R A 1 H8C H 0.0576 0.8088 0.399 0.046 Uiso 1 1 calc R A 1 C9 C 0.0471(3) 0.4949(3) 0.30116(19) 0.0216(10) Uani 1 1 d . A 1 C10 C 0.0568(3) 0.4146(3) 0.3328(2) 0.0338(12) Uani 1 1 d . A 1 H10A H 0.0424 0.4236 0.3748 0.051 Uiso 1 1 calc R A 1 H10B H 0.1168 0.3746 0.3167 0.051 Uiso 1 1 calc R A 1 H10C H 0.0175 0.3943 0.327 0.051 Uiso 1 1 calc R A 1 C11 C -0.0485(3) 0.5554(3) 0.3254(2) 0.0341(12) Uani 1 1 d . A 1 H11A H -0.056 0.6073 0.3057 0.051 Uiso 1 1 calc R A 1 H11B H -0.0648 0.564 0.3678 0.051 Uiso 1 1 calc R A 1 H11C H -0.0854 0.5332 0.3182 0.051 Uiso 1 1 calc R A 1 C12 C 0.0696(3) 0.4799(3) 0.23561(19) 0.0312(11) Uani 1 1 d . A 1 H12A H 0.0636 0.531 0.2149 0.047 Uiso 1 1 calc R A 1 H12B H 0.0301 0.4595 0.2302 0.047 Uiso 1 1 calc R A 1 H12C H 0.1294 0.4396 0.2198 0.047 Uiso 1 1 calc R A 1 C13 C 0.2201(3) 0.4218(3) 0.42887(19) 0.0270(11) Uani 1 1 d . A 1 C14 C 0.1749(3) 0.4557(3) 0.4925(2) 0.0431(14) Uani 1 1 d . A 1 H14A H 0.1904 0.5 0.4966 0.065 Uiso 1 1 calc R A 1 H14B H 0.1935 0.4123 0.5193 0.065 Uiso 1 1 calc R A 1 H14C H 0.1119 0.4765 0.5021 0.065 Uiso 1 1 calc R A 1 C15 C 0.3185(3) 0.3902(3) 0.4145(2) 0.0344(12) Uani 1 1 d . A 1 H15A H 0.3333 0.4353 0.4178 0.052 Uiso 1 1 calc R A 1 H15B H 0.3481 0.3671 0.3744 0.052 Uiso 1 1 calc R A 1 H15C H 0.3368 0.3481 0.4422 0.052 Uiso 1 1 calc R A 1 C16 C 0.1953(3) 0.3532(3) 0.4241(2) 0.0335(12) Uani 1 1 d . A 1 H16A H 0.1324 0.3744 0.4335 0.05 Uiso 1 1 calc R A 1 H16B H 0.2132 0.3109 0.4518 0.05 Uiso 1 1 calc R A 1 H16C H 0.2244 0.33 0.384 0.05 Uiso 1 1 calc R A 1 C17 C 0.3239(3) 0.6457(3) 0.31273(19) 0.0263(11) Uani 1 1 d . A 1 C18 C 0.3967(3) 0.5842(3) 0.3349(2) 0.0321(12) Uani 1 1 d . A 1 H18A H 0.3716 0.571 0.3756 0.048 Uiso 1 1 calc R A 1 H18B H 0.4372 0.6081 0.3331 0.048 Uiso 1 1 calc R A 1 H18C H 0.4277 0.5345 0.3102 0.048 Uiso 1 1 calc R A 1 C19 C 0.2795(3) 0.7239(3) 0.3506(2) 0.0368(12) Uani 1 1 d . A 1 H19A H 0.233 0.7641 0.3372 0.055 Uiso 1 1 calc R A 1 H19B H 0.3221 0.7459 0.3472 0.055 Uiso 1 1 calc R A 1 H19C H 0.2551 0.7118 0.3918 0.055 Uiso 1 1 calc R A 1 C20 C 0.3648(3) 0.6654(3) 0.2494(2) 0.0331(12) Uani 1 1 d . A 1 H20A H 0.3193 0.7049 0.2347 0.05 Uiso 1 1 calc R A 1 H20B H 0.3956 0.6155 0.2249 0.05 Uiso 1 1 calc R A 1 H20C H 0.4057 0.6885 0.2479 0.05 Uiso 1 1 calc R A 1 C21 C 0.0684(3) 0.7919(3) 0.1936(2) 0.0285(11) Uani 1 1 d . A 1 H21A H 0.0583 0.7697 0.2331 0.043 Uiso 1 1 calc R A 1 H21B H 0.0499 0.7672 0.1701 0.043 Uiso 1 1 calc R A 1 H21C H 0.0351 0.851 0.1963 0.043 Uiso 1 1 calc R A 1 C22 C 0.2076(3) 0.8327(3) 0.1998(2) 0.0345(12) Uani 1 1 d . A 1 H22A H 0.2688 0.8238 0.1835 0.052 Uiso 1 1 calc R A 1 H22B H 0.194 0.8177 0.2412 0.052 Uiso 1 1 calc R A 1 H22C H 0.1712 0.8902 0.1968 0.052 Uiso 1 1 calc R A 1 C23 C 0.1927(3) 0.8149(3) 0.0839(2) 0.0402(13) Uani 1 1 d . A 1 H23A H 0.253 0.8058 0.0615 0.06 Uiso 1 1 calc R A 1 H23B H 0.1567 0.8736 0.0889 0.06 Uiso 1 1 calc R A 1 H23C H 0.1718 0.7897 0.0626 0.06 Uiso 1 1 calc R A 1 C24 C 0.4109(3) 0.7168(3) 0.1022(2) 0.0315(11) Uani 1 1 d . A 1 H24A H 0.3708 0.773 0.0994 0.047 Uiso 1 1 calc R A 1 H24B H 0.4665 0.7049 0.0705 0.047 Uiso 1 1 calc R A 1 H24C H 0.4201 0.71 0.1402 0.047 Uiso 1 1 calc R A 1 C25 C 0.3632(3) 0.6566(3) 0.0173(2) 0.0386(13) Uani 1 1 d . A 1 H25A H 0.3707 0.7063 0.0012 0.058 Uiso 1 1 calc R A 1 H25B H 0.3078 0.6598 0.0167 0.058 Uiso 1 1 calc R A 1 H25C H 0.4107 0.6094 -0.0067 0.058 Uiso 1 1 calc R A 1 C26 C 0.4445(3) 0.5420(3) 0.1011(2) 0.0336(12) Uani 1 1 d . A 1 H26A H 0.4234 0.5015 0.0978 0.05 Uiso 1 1 calc R A 1 H26B H 0.4533 0.5373 0.1391 0.05 Uiso 1 1 calc R A 1 H26C H 0.4996 0.5324 0.0694 0.05 Uiso 1 1 calc R A 1 C27 C 0.4188(3) 0.3630(3) 0.1728(2) 0.0330(12) Uani 1 1 d . A 1 H27A H 0.3905 0.3797 0.2145 0.049 Uiso 1 1 calc R A 1 H27B H 0.4572 0.3908 0.1535 0.049 Uiso 1 1 calc R A 1 H27C H 0.4527 0.304 0.1693 0.049 Uiso 1 1 calc R A 1 C28 C 0.3981(3) 0.3561(3) 0.0589(2) 0.0377(13) Uani 1 1 d . A 1 H28A H 0.3583 0.3686 0.0368 0.057 Uiso 1 1 calc R A 1 H28B H 0.4326 0.2973 0.0572 0.057 Uiso 1 1 calc R A 1 H28C H 0.4367 0.3843 0.0417 0.057 Uiso 1 1 calc R A 1 C29 C 0.2794(3) 0.3212(3) 0.1704(2) 0.0347(12) Uani 1 1 d . A 1 H29A H 0.245 0.3374 0.2117 0.052 Uiso 1 1 calc R A 1 H29B H 0.323 0.2652 0.1681 0.052 Uiso 1 1 calc R A 1 H29C H 0.2412 0.3242 0.149 0.052 Uiso 1 1 calc R A 1 C30 C 0.2816(3) 0.5227(3) 0.00918(19) 0.0355(12) Uani 1 1 d . A 1 H30A H 0.2918 0.4761 -0.0132 0.053 Uiso 1 1 calc R A 1 H30B H 0.3371 0.5195 0.0095 0.053 Uiso 1 1 calc R A 1 H30C H 0.2535 0.5733 -0.0091 0.053 Uiso 1 1 calc R A 1 C31 C 0.1629(3) 0.4481(3) 0.0838(2) 0.0290(11) Uani 1 1 d . A 1 H31A H 0.2092 0.3932 0.0748 0.043 Uiso 1 1 calc R A 1 H31B H 0.1359 0.4639 0.0531 0.043 Uiso 1 1 calc R A 1 H31C H 0.1192 0.4487 0.1219 0.043 Uiso 1 1 calc R A 1 C32 C 0.1172(3) 0.6233(3) 0.1037(2) 0.0344(12) Uani 1 1 d . A 1 H32A H 0.1383 0.6643 0.1057 0.052 Uiso 1 1 calc R A 1 H32B H 0.0739 0.6222 0.1416 0.052 Uiso 1 1 calc R A 1 H32C H 0.0908 0.637 0.0728 0.052 Uiso 1 1 calc R A 1 Ge1B Ge 0.55399(3) -0.07621(3) 0.280611(19) 0.01730(11) Uani 1 1 d . B 2 P1B P 0.58259(7) -0.07601(7) 0.07769(5) 0.0195(2) Uani 1 1 d . B 2 P2B P 0.68099(7) -0.19267(7) 0.16180(5) 0.0197(3) Uani 1 1 d . B 2 P3B P 0.54027(7) -0.13783(7) 0.20528(5) 0.0185(2) Uani 1 1 d . B 2 P4B P 0.73763(7) -0.09210(7) 0.08161(5) 0.0208(3) Uani 1 1 d . B 2 P5B P 0.55246(7) 0.03107(7) 0.16096(5) 0.0183(2) Uani 1 1 d . B 2 P6B P 0.64474(7) -0.01999(7) 0.20917(5) 0.0189(2) Uani 1 1 d . B 2 Si1B Si 0.63008(8) -0.26396(8) 0.32381(6) 0.0268(3) Uani 1 1 d . B 2 Si2B Si 0.62948(8) -0.13104(8) 0.38511(5) 0.0264(3) Uani 1 1 d . B 2 Si3B Si 0.43644(8) 0.11447(8) 0.32354(5) 0.0266(3) Uani 1 1 d . B 2 Si4B Si 0.36852(8) -0.01147(8) 0.37717(5) 0.0280(3) Uani 1 1 d . B 2 N1B N 0.6030(2) -0.1579(2) 0.32913(15) 0.0207(8) Uani 1 1 d . B 2 N2B N 0.4548(2) 0.0098(2) 0.32625(15) 0.0209(8) Uani 1 1 d . B 2 C1B C 0.6826(3) -0.1624(2) 0.08471(18) 0.0199(10) Uani 1 1 d . B 2 C2B C 0.5117(2) -0.0500(3) 0.15678(18) 0.0191(9) Uani 1 1 d . B 2 C3B C 0.6320(2) -0.0050(3) 0.08533(18) 0.0195(9) Uani 1 1 d . B 2 C4B C 0.7243(2) -0.1115(3) 0.16174(17) 0.0191(9) Uani 1 1 d . B 2 C5B C 0.7209(3) -0.2341(3) 0.04021(19) 0.0246(10) Uani 1 1 d . B 2 C6B C 0.6620(3) -0.2802(3) 0.0588(2) 0.0359(12) Uani 1 1 d . B 2 H6B1 H 0.6033 -0.2429 0.0599 0.054 Uiso 1 1 calc R B 2 H6B2 H 0.6605 -0.3022 0.0979 0.054 Uiso 1 1 calc R B 2 H6B3 H 0.6846 -0.3249 0.0305 0.054 Uiso 1 1 calc R B 2 C7B C 0.7275(3) -0.2025(3) -0.02210(19) 0.0370(13) Uani 1 1 d . B 2 H7B1 H 0.6698 -0.1649 -0.0228 0.055 Uiso 1 1 calc R B 2 H7B2 H 0.7507 -0.2485 -0.0495 0.055 Uiso 1 1 calc R B 2 H7B3 H 0.7662 -0.174 -0.0338 0.055 Uiso 1 1 calc R B 2 C8B C 0.8125(3) -0.2924(3) 0.0387(2) 0.0335(12) Uani 1 1 d . B 2 H8B1 H 0.8503 -0.2631 0.0268 0.05 Uiso 1 1 calc R B 2 H8B2 H 0.835 -0.3372 0.0104 0.05 Uiso 1 1 calc R B 2 H8B3 H 0.8108 -0.3144 0.0778 0.05 Uiso 1 1 calc R B 2 C9B C 0.4132(2) -0.0171(3) 0.16221(18) 0.0215(10) Uani 1 1 d . B 2 C10B C 0.3882(3) 0.0583(3) 0.1241(2) 0.0293(11) Uani 1 1 d . B 2 H10D H 0.4249 0.0439 0.083 0.044 Uiso 1 1 calc R B 2 H10E H 0.3964 0.102 0.1377 0.044 Uiso 1 1 calc R B 2 H10F H 0.3273 0.0767 0.1273 0.044 Uiso 1 1 calc R B 2 C11B C 0.3968(3) -0.0834(3) 0.1412(2) 0.0288(11) Uani 1 1 d . B 2 H11D H 0.434 -0.0993 0.1004 0.043 Uiso 1 1 calc R B 2 H11E H 0.3359 -0.0623 0.1438 0.043 Uiso 1 1 calc R B 2 H11F H 0.4099 -0.1308 0.166 0.043 Uiso 1 1 calc R B 2 C12B C 0.3550(3) 0.0070(3) 0.22568(19) 0.0305(11) Uani 1 1 d . B 2 H12D H 0.3649 0.0494 0.2395 0.046 Uiso 1 1 calc R B 2 H12E H 0.3684 -0.0407 0.2503 0.046 Uiso 1 1 calc R B 2 H12F H 0.2942 0.0276 0.2281 0.046 Uiso 1 1 calc R B 2 C13B C 0.6419(3) 0.0633(3) 0.04148(18) 0.0227(10) Uani 1 1 d . B 2 C14B C 0.7004(3) 0.0259(3) -0.02025(19) 0.0285(11) Uani 1 1 d . B 2 H14D H 0.7574 -0.0128 -0.0189 0.043 Uiso 1 1 calc R B 2 H14E H 0.7071 0.0691 -0.0475 0.043 Uiso 1 1 calc R B 2 H14F H 0.6739 -0.0026 -0.0338 0.043 Uiso 1 1 calc R B 2 C15B C 0.6834(3) 0.1066(3) 0.0633(2) 0.0373(12) Uani 1 1 d . B 2 H15D H 0.7396 0.0671 0.0656 0.056 Uiso 1 1 calc R B 2 H15E H 0.6454 0.1312 0.1023 0.056 Uiso 1 1 calc R B 2 H15F H 0.6919 0.1492 0.036 0.056 Uiso 1 1 calc R B 2 C16B C 0.5542(3) 0.1235(3) 0.0375(2) 0.0361(13) Uani 1 1 d . B 2 H16D H 0.5286 0.0948 0.0233 0.054 Uiso 1 1 calc R B 2 H16E H 0.5621 0.1663 0.0101 0.054 Uiso 1 1 calc R B 2 H16F H 0.5155 0.148 0.0764 0.054 Uiso 1 1 calc R B 2 C17B C 0.8146(3) -0.1425(3) 0.17136(19) 0.0238(10) Uani 1 1 d . B 2 C18B C 0.8527(3) -0.0784(3) 0.1498(2) 0.0323(12) Uani 1 1 d . B 2 H18D H 0.8593 -0.0686 0.1081 0.048 Uiso 1 1 calc R B 2 H18E H 0.9095 -0.0981 0.1549 0.048 Uiso 1 1 calc R B 2 H18F H 0.8136 -0.0275 0.1726 0.048 Uiso 1 1 calc R B 2 C19B C 0.8792(3) -0.2235(3) 0.1371(2) 0.0308(12) Uani 1 1 d . B 2 H19D H 0.8869 -0.2159 0.0952 0.046 Uiso 1 1 calc R B 2 H19E H 0.8566 -0.2655 0.1515 0.046 Uiso 1 1 calc R B 2 H19F H 0.9352 -0.2406 0.1429 0.046 Uiso 1 1 calc R B 2 C20B C 0.8043(3) -0.1563(3) 0.23653(19) 0.0281(11) Uani 1 1 d . B 2 H20D H 0.7798 -0.197 0.2509 0.042 Uiso 1 1 calc R B 2 H20E H 0.7654 -0.105 0.2589 0.042 Uiso 1 1 calc R B 2 H20F H 0.8611 -0.1758 0.2415 0.042 Uiso 1 1 calc R B 2 C21B C 0.5658(3) -0.2946(3) 0.2928(2) 0.0404(13) Uani 1 1 d . B 2 H21D H 0.5038 -0.2636 0.313 0.061 Uiso 1 1 calc R B 2 H21E H 0.58 -0.3529 0.2984 0.061 Uiso 1 1 calc R B 2 H21F H 0.5797 -0.2834 0.2508 0.061 Uiso 1 1 calc R B 2 C22B C 0.7455(3) -0.3273(3) 0.2813(2) 0.0384(13) Uani 1 1 d . B 2 H22D H 0.7838 -0.3146 0.2952 0.058 Uiso 1 1 calc R B 2 H22E H 0.7564 -0.3153 0.2395 0.058 Uiso 1 1 calc R B 2 H22F H 0.7568 -0.3851 0.2869 0.058 Uiso 1 1 calc R B 2 C23B C 0.6127(3) -0.3071(3) 0.3991(2) 0.0425(14) Uani 1 1 d . B 2 H23D H 0.553 -0.2767 0.4242 0.064 Uiso 1 1 calc R B 2 H23E H 0.6529 -0.3029 0.4159 0.064 Uiso 1 1 calc R B 2 H23F H 0.6233 -0.3645 0.3966 0.064 Uiso 1 1 calc R B 2 C24B C 0.7436(3) -0.1966(3) 0.3839(2) 0.0386(13) Uani 1 1 d . B 2 H24D H 0.7519 -0.2538 0.3873 0.058 Uiso 1 1 calc R B 2 H24E H 0.7533 -0.1805 0.4169 0.058 Uiso 1 1 calc R B 2 H24F H 0.7848 -0.1895 0.3469 0.058 Uiso 1 1 calc R B 2 C25B C 0.5574(3) -0.1388(3) 0.4610(2) 0.0415(14) Uani 1 1 d . B 2 H25D H 0.5904 -0.185 0.4806 0.062 Uiso 1 1 calc R B 2 H25E H 0.5084 -0.1471 0.4585 0.062 Uiso 1 1 calc R B 2 H25F H 0.5358 -0.0885 0.4836 0.062 Uiso 1 1 calc R B 2 C26B C 0.6214(3) -0.0248(3) 0.3785(2) 0.0329(12) Uani 1 1 d . B 2 H26D H 0.6584 -0.018 0.3393 0.049 Uiso 1 1 calc R B 2 H26E H 0.6405 -0.0135 0.4083 0.049 Uiso 1 1 calc R B 2 H26F H 0.5612 0.013 0.3842 0.049 Uiso 1 1 calc R B 2 C27B C 0.5310(3) 0.1423(3) 0.2914(2) 0.0367(12) Uani 1 1 d . B 2 H27D H 0.5616 0.1218 0.2506 0.055 Uiso 1 1 calc R B 2 H27E H 0.5704 0.1181 0.3143 0.055 Uiso 1 1 calc R B 2 H27F H 0.5108 0.2017 0.2924 0.055 Uiso 1 1 calc R B 2 C28B C 0.3866(3) 0.1581(3) 0.4002(2) 0.0419(14) Uani 1 1 d . B 2 H28D H 0.3356 0.1461 0.421 0.063 Uiso 1 1 calc R B 2 H28E H 0.3691 0.2171 0.3989 0.063 Uiso 1 1 calc R B 2 H28F H 0.429 0.1337 0.4208 0.063 Uiso 1 1 calc R B 2 C29B C 0.3609(3) 0.1787(3) 0.2831(2) 0.0379(13) Uani 1 1 d . B 2 H29D H 0.3083 0.1682 0.2973 0.057 Uiso 1 1 calc R B 2 H29E H 0.3893 0.1652 0.241 0.057 Uiso 1 1 calc R B 2 H29F H 0.3455 0.2363 0.2898 0.057 Uiso 1 1 calc R B 2 C30B C 0.3591(3) -0.0043(3) 0.4561(2) 0.0428(14) Uani 1 1 d . B 2 H30D H 0.3092 0.0455 0.4747 0.064 Uiso 1 1 calc R B 2 H30E H 0.4121 -0.0031 0.4577 0.064 Uiso 1 1 calc R B 2 H30F H 0.351 -0.0517 0.4769 0.064 Uiso 1 1 calc R B 2 C31B C 0.2585(3) 0.0604(3) 0.3743(2) 0.0414(14) Uani 1 1 d . B 2 H31D H 0.2491 0.1164 0.3811 0.062 Uiso 1 1 calc R B 2 H31E H 0.2139 0.0468 0.4048 0.062 Uiso 1 1 calc R B 2 H31F H 0.2552 0.0556 0.3357 0.062 Uiso 1 1 calc R B 2 C32B C 0.3814(3) -0.1160(3) 0.3641(2) 0.0368(12) Uani 1 1 d . B 2 H32D H 0.3868 -0.1222 0.3232 0.055 Uiso 1 1 calc R B 2 H32E H 0.3305 -0.1247 0.3905 0.055 Uiso 1 1 calc R B 2 H32F H 0.4335 -0.1561 0.3717 0.055 Uiso 1 1 calc R B 2 Ge1C Ge -0.18881(3) 1.23051(3) 0.325413(19) 0.01726(11) Uani 1 1 d . C 3 P1C P -0.18258(7) 1.30119(8) 0.12816(5) 0.0263(3) Uani 1 1 d . C 3 P2C P -0.07389(7) 1.15093(7) 0.19057(5) 0.0223(3) Uani 1 1 d . C 3 P3C P -0.21259(7) 1.20043(7) 0.24127(5) 0.0205(3) Uani 1 1 d . C 3 P4C P -0.02216(7) 1.26867(8) 0.13053(5) 0.0253(3) Uani 1 1 d . C 3 P5C P -0.20125(7) 1.37275(7) 0.22703(5) 0.0238(3) Uani 1 1 d . C 3 P6C P -0.10049(7) 1.29810(7) 0.26547(5) 0.0211(3) Uani 1 1 d . C 3 Si1C Si -0.11537(8) 1.03348(8) 0.34077(6) 0.0270(3) Uani 1 1 d . C 3 Si2C Si -0.09886(8) 1.13692(8) 0.41807(6) 0.0273(3) Uani 1 1 d . C 3 Si3C Si -0.30373(8) 1.40641(8) 0.39695(6) 0.0289(3) Uani 1 1 d . C 3 Si4C Si -0.36557(7) 1.27344(8) 0.42972(6) 0.0265(3) Uani 1 1 d . C 3 N1C N -0.1363(2) 1.1328(2) 0.36085(15) 0.0193(8) Uani 1 1 d . C 3 N2C N -0.2832(2) 1.3044(2) 0.38334(15) 0.0210(8) Uani 1 1 d . C 3 C1C C -0.0808(3) 1.2074(3) 0.12088(18) 0.0258(11) Uani 1 1 d . C 3 C2C C -0.2456(2) 1.3027(3) 0.20847(18) 0.0222(10) Uani 1 1 d . C 3 C3C C -0.1288(3) 1.3593(3) 0.14839(19) 0.0257(11) Uani 1 1 d . C 3 C4C C -0.0272(2) 1.2216(3) 0.20467(18) 0.0212(10) Uani 1 1 d . C 3 C5C C -0.0494(3) 1.1543(3) 0.0653(2) 0.0337(12) Uani 1 1 d . C 3 C6C C -0.1148(3) 1.1178(3) 0.0720(2) 0.0451(14) Uani 1 1 d . C 3 H6C1 H -0.1725 1.1618 0.0782 0.068 Uiso 1 1 calc R C 3 H6C2 H -0.1164 1.0822 0.1058 0.068 Uiso 1 1 calc R C 3 H6C3 H -0.0974 1.0862 0.0364 0.068 Uiso 1 1 calc R C 3 C7C C -0.0450(4) 1.2076(4) 0.0103(2) 0.0475(15) Uani 1 1 d . C 3 H7C1 H -0.0029 1.2308 0.0054 0.071 Uiso 1 1 calc R C 3 H7C2 H -0.1022 1.2517 0.0152 0.071 Uiso 1 1 calc R C 3 H7C3 H -0.027 1.1741 -0.0245 0.071 Uiso 1 1 calc R C 3 C8C C 0.0410(3) 1.0863(3) 0.0555(2) 0.0475(15) Uani 1 1 d . C 3 H8C1 H 0.0824 1.1101 0.0512 0.071 Uiso 1 1 calc R C 3 H8C2 H 0.0586 1.0546 0.0198 0.071 Uiso 1 1 calc R C 3 H8C3 H 0.0398 1.0505 0.0892 0.071 Uiso 1 1 calc R C 3 C9C C -0.3464(3) 1.3387(3) 0.2177(2) 0.0293(11) Uani 1 1 d . C 3 C10C C -0.3788(3) 1.4263(3) 0.1965(2) 0.0400(13) Uani 1 1 d . C 3 H10G H -0.3458 1.4276 0.1549 0.06 Uiso 1 1 calc R C 3 H10H H -0.3708 1.4613 0.2196 0.06 Uiso 1 1 calc R C 3 H10I H -0.4405 1.446 0.2014 0.06 Uiso 1 1 calc R C 3 C11C C -0.3621(3) 1.2854(3) 0.1826(2) 0.0391(13) Uani 1 1 d . C 3 H11G H -0.3287 1.2851 0.1409 0.059 Uiso 1 1 calc R C 3 H11H H -0.424 1.3074 0.1875 0.059 Uiso 1 1 calc R C 3 H11I H -0.3437 1.2297 0.1968 0.059 Uiso 1 1 calc R C 3 C12C C -0.3986(3) 1.3383(3) 0.2823(2) 0.0338(12) Uani 1 1 d . C 3 H12G H -0.3894 1.3725 0.3052 0.051 Uiso 1 1 calc R C 3 H12H H -0.3796 1.2824 0.2963 0.051 Uiso 1 1 calc R C 3 H12I H -0.4603 1.3596 0.287 0.051 Uiso 1 1 calc R C 3 C13C C -0.1235(3) 1.4388(3) 0.1180(2) 0.0341(12) Uani 1 1 d . C 3 C14C C -0.0749(3) 1.4227(4) 0.0517(2) 0.0503(16) Uani 1 1 d . C 3 H14G H -0.1063 1.4049 0.0343 0.075 Uiso 1 1 calc R C 3 H14H H -0.0164 1.3801 0.0453 0.075 Uiso 1 1 calc R C 3 H14I H -0.071 1.4728 0.0332 0.075 Uiso 1 1 calc R C 3 C15C C -0.0754(3) 1.4670(3) 0.1458(2) 0.0464(14) Uani 1 1 d . C 3 H15G H -0.1069 1.477 0.1881 0.07 Uiso 1 1 calc R C 3 H15H H -0.0717 1.5173 0.1277 0.07 Uiso 1 1 calc R C 3 H15I H -0.0168 1.4247 0.1396 0.07 Uiso 1 1 calc R C 3 C16C C -0.2140(3) 1.5066(3) 0.1264(2) 0.0438(14) Uani 1 1 d . C 3 H16G H -0.2451 1.4892 0.1085 0.066 Uiso 1 1 calc R C 3 H16H H -0.2085 1.556 0.1076 0.066 Uiso 1 1 calc R C 3 H16I H -0.2463 1.518 0.1684 0.066 Uiso 1 1 calc R C 3 C17C C 0.0674(3) 1.1780(3) 0.2093(2) 0.0269(11) Uani 1 1 d . C 3 C18C C 0.1084(3) 1.2397(3) 0.2001(2) 0.0373(13) Uani 1 1 d . C 3 H18G H 0.0714 1.2843 0.2294 0.056 Uiso 1 1 calc R C 3 H18H H 0.1141 1.2615 0.1606 0.056 Uiso 1 1 calc R C 3 H18I H 0.1658 1.2126 0.2045 0.056 Uiso 1 1 calc R C 3 C19C C 0.1259(3) 1.1086(3) 0.1633(2) 0.0364(13) Uani 1 1 d . C 3 H19G H 0.1002 1.069 0.1689 0.055 Uiso 1 1 calc R C 3 H19H H 0.1832 1.0817 0.1679 0.055 Uiso 1 1 calc R C 3 H19I H 0.1317 1.1307 0.1239 0.055 Uiso 1 1 calc R C 3 C20C C 0.0631(3) 1.1419(3) 0.2704(2) 0.0349(13) Uani 1 1 d . C 3 H20G H 0.037 1.1025 0.277 0.052 Uiso 1 1 calc R C 3 H20H H 0.0278 1.1856 0.3004 0.052 Uiso 1 1 calc R C 3 H20I H 0.1218 1.1146 0.2726 0.052 Uiso 1 1 calc R C 3 C21C C -0.1764(3) 1.0230(3) 0.2965(2) 0.0377(12) Uani 1 1 d . C 3 H21G H -0.2387 1.0536 0.316 0.057 Uiso 1 1 calc R C 3 H21H H -0.1641 0.9654 0.2929 0.057 Uiso 1 1 calc R C 3 H21I H -0.1585 1.0445 0.2573 0.057 Uiso 1 1 calc R C 3 C22C C -0.0003(3) 0.9720(3) 0.2971(2) 0.0407(13) Uani 1 1 d . C 3 H22G H 0.0378 0.9735 0.317 0.061 Uiso 1 1 calc R C 3 H22H H 0.0138 0.9947 0.2579 0.061 Uiso 1 1 calc R C 3 H22I H 0.0081 0.9156 0.2934 0.061 Uiso 1 1 calc R C 3 C23C C -0.1430(3) 0.9753(3) 0.4086(2) 0.0415(13) Uani 1 1 d . C 3 H23G H -0.1132 0.9777 0.4347 0.062 Uiso 1 1 calc R C 3 H23H H -0.1246 0.9184 0.3977 0.062 Uiso 1 1 calc R C 3 H23I H -0.2058 0.9994 0.429 0.062 Uiso 1 1 calc R C 3 C24C C 0.0146(3) 1.0604(3) 0.4091(2) 0.0402(13) Uani 1 1 d . C 3 H24G H 0.0179 1.0054 0.4068 0.06 Uiso 1 1 calc R C 3 H24H H 0.0301 1.065 0.4429 0.06 Uiso 1 1 calc R C 3 H24I H 0.0549 1.0709 0.373 0.06 Uiso 1 1 calc R C 3 C25C C -0.1637(3) 1.1147(3) 0.4923(2) 0.0418(14) Uani 1 1 d . C 3 H25G H -0.1293 1.0615 0.5047 0.063 Uiso 1 1 calc R C 3 H25H H -0.2168 1.1142 0.4903 0.063 Uiso 1 1 calc R C 3 H25I H -0.1789 1.1569 0.5208 0.063 Uiso 1 1 calc R C 3 C26C C -0.1002(3) 1.2389(3) 0.4227(2) 0.0375(13) Uani 1 1 d . C 3 H26G H -0.0666 1.252 0.3844 0.056 Uiso 1 1 calc R C 3 H26H H -0.0746 1.2389 0.4522 0.056 Uiso 1 1 calc R C 3 H26I H -0.1602 1.2798 0.434 0.056 Uiso 1 1 calc R C 3 C27C C -0.2102(3) 1.4367(3) 0.3709(2) 0.0357(12) Uani 1 1 d . C 3 H27G H -0.1822 1.4265 0.3284 0.053 Uiso 1 1 calc R C 3 H27H H -0.1683 1.4047 0.3908 0.053 Uiso 1 1 calc R C 3 H27I H -0.231 1.4947 0.3798 0.053 Uiso 1 1 calc R C 3 C28C C -0.3476(3) 1.4304(3) 0.4779(2) 0.0426(13) Uani 1 1 d . C 3 H28G H -0.3978 1.4165 0.4962 0.064 Uiso 1 1 calc R C 3 H28H H -0.3654 1.4886 0.4844 0.064 Uiso 1 1 calc R C 3 H28I H -0.3026 1.3986 0.4955 0.064 Uiso 1 1 calc R C 3 C29C C -0.3865(3) 1.4833(3) 0.3657(2) 0.0430(14) Uani 1 1 d . C 3 H29G H -0.438 1.4713 0.378 0.065 Uiso 1 1 calc R C 3 H29H H -0.362 1.4808 0.3227 0.065 Uiso 1 1 calc R C 3 H29I H -0.4025 1.538 0.3801 0.065 Uiso 1 1 calc R C 3 C30C C -0.3658(3) 1.2595(3) 0.5077(2) 0.0439(14) Uani 1 1 d . C 3 H30G H -0.4126 1.3068 0.5319 0.066 Uiso 1 1 calc R C 3 H30H H -0.31 1.2542 0.5088 0.066 Uiso 1 1 calc R C 3 H30I H -0.3751 1.2102 0.5229 0.066 Uiso 1 1 calc R C 3 C31C C -0.4781(3) 1.3489(3) 0.4362(2) 0.0382(13) Uani 1 1 d . C 3 H31G H -0.4875 1.4015 0.4505 0.057 Uiso 1 1 calc R C 3 H31H H -0.5201 1.3294 0.4638 0.057 Uiso 1 1 calc R C 3 H31I H -0.4854 1.3555 0.3975 0.057 Uiso 1 1 calc R C 3 C32C C -0.3547(3) 1.1765(3) 0.4024(2) 0.0340(12) Uani 1 1 d . C 3 H32G H -0.2966 1.1345 0.3981 0.051 Uiso 1 1 calc R C 3 H32H H -0.3637 1.1851 0.3643 0.051 Uiso 1 1 calc R C 3 H32I H -0.3981 1.159 0.4305 0.051 Uiso 1 1 calc R C 3 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge 0.0181(2) 0.0173(2) 0.0197(2) 0.00079(19) -0.00685(18) -0.00874(19) P1 0.0209(5) 0.0241(6) 0.0219(6) 0.0013(5) -0.0066(5) -0.0105(5) P2 0.0221(6) 0.0208(6) 0.0220(6) -0.0002(5) -0.0078(5) -0.0101(5) P3 0.0177(5) 0.0220(6) 0.0210(6) 0.0010(5) -0.0074(5) -0.0088(5) P4 0.0224(6) 0.0241(6) 0.0224(6) 0.0006(5) -0.0089(5) -0.0103(5) P5 0.0200(5) 0.0211(6) 0.0240(6) 0.0018(5) -0.0073(5) -0.0096(5) P6 0.0189(5) 0.0214(6) 0.0223(6) 0.0003(5) -0.0071(5) -0.0090(5) Si1 0.0248(6) 0.0183(7) 0.0287(7) 0.0021(5) -0.0077(5) -0.0094(5) Si2 0.0244(6) 0.0239(7) 0.0267(7) 0.0002(6) -0.0024(5) -0.0133(5) Si3 0.0246(6) 0.0175(7) 0.0305(7) -0.0013(5) -0.0127(5) -0.0073(5) Si4 0.0263(6) 0.0219(7) 0.0249(7) -0.0005(5) -0.0130(5) -0.0087(5) N1 0.0228(18) 0.0171(19) 0.023(2) 0.0029(16) -0.0047(15) -0.0108(16) N2 0.0228(18) 0.0144(19) 0.0191(19) -0.0005(15) -0.0073(15) -0.0075(15) C1 0.024(2) 0.026(3) 0.021(2) -0.001(2) -0.0072(19) -0.013(2) C2 0.021(2) 0.023(2) 0.020(2) 0.0054(19) -0.0066(18) -0.0140(19) C3 0.023(2) 0.020(2) 0.028(3) 0.003(2) -0.0114(19) -0.0115(19) C4 0.020(2) 0.017(2) 0.024(2) -0.0025(19) -0.0075(18) -0.0099(18) C5 0.023(2) 0.027(3) 0.023(2) -0.003(2) -0.0056(19) -0.008(2) C6 0.025(2) 0.035(3) 0.045(3) -0.015(2) -0.012(2) -0.004(2) C7 0.036(3) 0.036(3) 0.027(3) -0.001(2) -0.004(2) -0.020(2) C8 0.039(3) 0.022(3) 0.031(3) -0.003(2) -0.010(2) -0.012(2) C9 0.023(2) 0.021(2) 0.027(3) 0.0001(19) -0.0070(19) -0.0151(19) C10 0.039(3) 0.035(3) 0.039(3) 0.005(2) -0.012(2) -0.029(2) C11 0.022(2) 0.044(3) 0.041(3) -0.004(2) -0.006(2) -0.019(2) C12 0.034(3) 0.038(3) 0.033(3) -0.004(2) -0.011(2) -0.024(2) C13 0.026(2) 0.027(3) 0.026(3) 0.007(2) -0.008(2) -0.011(2) C14 0.055(3) 0.038(3) 0.030(3) 0.008(2) -0.014(3) -0.015(3) C15 0.033(3) 0.030(3) 0.046(3) 0.010(2) -0.022(2) -0.013(2) C16 0.032(3) 0.028(3) 0.042(3) 0.014(2) -0.015(2) -0.015(2) C17 0.028(2) 0.031(3) 0.027(3) -0.002(2) -0.010(2) -0.016(2) C18 0.027(2) 0.039(3) 0.040(3) 0.002(2) -0.016(2) -0.018(2) C19 0.039(3) 0.041(3) 0.043(3) -0.002(3) -0.015(2) -0.026(2) C20 0.031(2) 0.039(3) 0.037(3) 0.003(2) -0.009(2) -0.024(2) C21 0.027(2) 0.023(3) 0.036(3) 0.002(2) -0.013(2) -0.009(2) C22 0.031(3) 0.021(3) 0.048(3) -0.002(2) -0.006(2) -0.012(2) C23 0.044(3) 0.028(3) 0.041(3) 0.009(2) -0.013(2) -0.010(2) C24 0.033(2) 0.033(3) 0.031(3) 0.001(2) -0.002(2) -0.023(2) C25 0.045(3) 0.037(3) 0.035(3) -0.002(2) -0.005(2) -0.024(3) C26 0.028(2) 0.028(3) 0.041(3) -0.002(2) -0.005(2) -0.013(2) C27 0.030(2) 0.023(3) 0.045(3) 0.002(2) -0.019(2) -0.004(2) C28 0.037(3) 0.031(3) 0.036(3) -0.007(2) -0.014(2) -0.003(2) C29 0.041(3) 0.021(3) 0.049(3) 0.004(2) -0.025(2) -0.012(2) C30 0.052(3) 0.036(3) 0.025(3) 0.005(2) -0.013(2) -0.024(3) C31 0.030(2) 0.031(3) 0.034(3) 0.000(2) -0.018(2) -0.013(2) C32 0.036(3) 0.028(3) 0.039(3) -0.001(2) -0.024(2) -0.003(2) Ge1B 0.0197(2) 0.0175(2) 0.0174(2) 0.00350(19) -0.00788(18) -0.00941(19) P1B 0.0228(6) 0.0194(6) 0.0185(6) 0.0028(5) -0.0092(5) -0.0095(5) P2B 0.0216(5) 0.0174(6) 0.0204(6) 0.0021(5) -0.0081(5) -0.0079(5) P3B 0.0214(5) 0.0183(6) 0.0199(6) 0.0035(5) -0.0092(5) -0.0106(5) P4B 0.0200(5) 0.0223(6) 0.0201(6) 0.0025(5) -0.0058(5) -0.0098(5) P5B 0.0213(5) 0.0161(6) 0.0185(6) 0.0022(5) -0.0074(5) -0.0084(5) P6B 0.0194(5) 0.0202(6) 0.0197(6) 0.0015(5) -0.0073(5) -0.0101(5) Si1B 0.0333(7) 0.0205(7) 0.0304(7) 0.0082(6) -0.0155(6) -0.0124(6) Si2B 0.0311(7) 0.0293(7) 0.0254(7) 0.0061(6) -0.0167(6) -0.0139(6) Si3B 0.0346(7) 0.0190(7) 0.0239(7) 0.0005(5) -0.0105(6) -0.0082(6) Si4B 0.0250(6) 0.0321(8) 0.0222(7) 0.0021(6) -0.0034(5) -0.0111(6) N1B 0.0253(18) 0.020(2) 0.0194(19) 0.0066(16) -0.0100(15) -0.0107(16) N2B 0.0223(18) 0.021(2) 0.020(2) 0.0041(16) -0.0062(15) -0.0111(16) C1B 0.023(2) 0.016(2) 0.023(2) 0.0023(19) -0.0079(19) -0.0102(19) C2B 0.022(2) 0.020(2) 0.021(2) 0.0032(19) -0.0108(18) -0.0117(19) C3B 0.021(2) 0.021(2) 0.019(2) 0.0003(19) -0.0072(18) -0.0100(19) C4B 0.020(2) 0.020(2) 0.018(2) 0.0019(18) -0.0072(18) -0.0080(18) C5B 0.029(2) 0.020(2) 0.023(2) 0.000(2) -0.009(2) -0.009(2) C6B 0.047(3) 0.029(3) 0.036(3) -0.001(2) -0.013(2) -0.020(2) C7B 0.051(3) 0.031(3) 0.019(3) -0.004(2) -0.006(2) -0.010(2) C8B 0.033(3) 0.027(3) 0.034(3) -0.008(2) -0.006(2) -0.008(2) C9B 0.020(2) 0.027(3) 0.021(2) 0.003(2) -0.0120(18) -0.0091(19) C10B 0.021(2) 0.031(3) 0.036(3) 0.011(2) -0.014(2) -0.009(2) C11B 0.030(2) 0.037(3) 0.032(3) 0.007(2) -0.017(2) -0.020(2) C12B 0.021(2) 0.041(3) 0.028(3) 0.000(2) -0.006(2) -0.012(2) C13B 0.029(2) 0.022(2) 0.020(2) 0.0072(19) -0.0079(19) -0.014(2) C14B 0.031(2) 0.031(3) 0.024(3) 0.008(2) -0.007(2) -0.016(2) C15B 0.067(3) 0.032(3) 0.032(3) 0.008(2) -0.020(3) -0.036(3) C16B 0.043(3) 0.025(3) 0.029(3) 0.012(2) -0.010(2) -0.009(2) C17B 0.019(2) 0.026(3) 0.026(3) 0.000(2) -0.0095(19) -0.0073(19) C18B 0.023(2) 0.042(3) 0.038(3) 0.008(2) -0.012(2) -0.019(2) C19B 0.017(2) 0.029(3) 0.042(3) -0.002(2) -0.010(2) -0.004(2) C20B 0.024(2) 0.032(3) 0.032(3) 0.003(2) -0.016(2) -0.011(2) C21B 0.057(3) 0.027(3) 0.052(3) 0.012(3) -0.031(3) -0.022(3) C22B 0.042(3) 0.025(3) 0.044(3) 0.005(2) -0.020(2) -0.007(2) C23B 0.058(3) 0.036(3) 0.039(3) 0.018(3) -0.022(3) -0.025(3) C24B 0.042(3) 0.043(3) 0.040(3) 0.013(3) -0.028(2) -0.018(3) C25B 0.048(3) 0.043(3) 0.028(3) 0.002(2) -0.014(2) -0.014(3) C26B 0.043(3) 0.034(3) 0.035(3) 0.001(2) -0.020(2) -0.022(2) C27B 0.046(3) 0.024(3) 0.039(3) -0.001(2) -0.012(2) -0.014(2) C28B 0.059(3) 0.027(3) 0.032(3) -0.006(2) -0.016(3) -0.007(3) C29B 0.043(3) 0.026(3) 0.037(3) 0.005(2) -0.016(2) -0.006(2) C30B 0.043(3) 0.050(4) 0.027(3) 0.007(3) -0.005(2) -0.017(3) C31B 0.024(2) 0.052(4) 0.037(3) 0.007(3) -0.002(2) -0.013(2) C32B 0.039(3) 0.041(3) 0.032(3) 0.008(2) -0.008(2) -0.023(2) Ge1C 0.0171(2) 0.0171(2) 0.0185(2) 0.00228(19) -0.00658(18) -0.00772(19) P1C 0.0264(6) 0.0363(7) 0.0223(6) 0.0073(5) -0.0116(5) -0.0171(6) P2C 0.0203(5) 0.0261(7) 0.0214(6) 0.0009(5) -0.0058(5) -0.0111(5) P3C 0.0192(5) 0.0251(6) 0.0209(6) 0.0029(5) -0.0078(5) -0.0119(5) P4C 0.0234(6) 0.0332(7) 0.0224(7) 0.0051(5) -0.0070(5) -0.0159(5) P5C 0.0241(6) 0.0238(6) 0.0259(7) 0.0071(5) -0.0117(5) -0.0110(5) P6C 0.0215(5) 0.0241(6) 0.0231(6) 0.0044(5) -0.0098(5) -0.0133(5) Si1C 0.0276(6) 0.0177(7) 0.0327(8) -0.0006(6) -0.0083(6) -0.0073(5) Si2C 0.0315(7) 0.0260(7) 0.0261(7) 0.0044(6) -0.0152(6) -0.0097(6) Si3C 0.0295(7) 0.0199(7) 0.0346(8) -0.0025(6) -0.0096(6) -0.0076(6) Si4C 0.0193(6) 0.0273(7) 0.0276(7) 0.0032(6) -0.0045(5) -0.0079(5) N1C 0.0204(17) 0.0129(18) 0.025(2) -0.0001(15) -0.0093(15) -0.0056(15) N2C 0.0212(18) 0.0153(19) 0.025(2) -0.0016(16) -0.0067(16) -0.0059(15) C1C 0.021(2) 0.038(3) 0.020(2) 0.003(2) -0.0054(19) -0.016(2) C2C 0.019(2) 0.031(3) 0.021(2) 0.007(2) -0.0087(18) -0.014(2) C3C 0.028(2) 0.028(3) 0.026(3) 0.011(2) -0.013(2) -0.016(2) C4C 0.018(2) 0.030(3) 0.019(2) 0.006(2) -0.0073(18) -0.0147(19) C5C 0.033(3) 0.050(3) 0.023(3) -0.001(2) -0.008(2) -0.023(2) C6C 0.051(3) 0.054(4) 0.039(3) -0.011(3) -0.008(3) -0.032(3) C7C 0.059(3) 0.074(4) 0.018(3) -0.001(3) -0.004(2) -0.041(3) C8C 0.044(3) 0.055(4) 0.034(3) -0.016(3) -0.004(2) -0.014(3) C9C 0.021(2) 0.039(3) 0.029(3) 0.008(2) -0.012(2) -0.011(2) C10C 0.031(3) 0.043(3) 0.046(3) 0.016(3) -0.021(2) -0.011(2) C11C 0.028(2) 0.061(4) 0.039(3) 0.007(3) -0.019(2) -0.022(3) C12C 0.022(2) 0.040(3) 0.038(3) 0.002(2) -0.011(2) -0.011(2) C13C 0.038(3) 0.036(3) 0.035(3) 0.019(2) -0.017(2) -0.022(2) C14C 0.053(3) 0.060(4) 0.039(3) 0.024(3) -0.014(3) -0.031(3) C15C 0.059(3) 0.042(3) 0.058(4) 0.023(3) -0.032(3) -0.035(3) C16C 0.052(3) 0.035(3) 0.051(3) 0.025(3) -0.026(3) -0.023(3) C17C 0.017(2) 0.034(3) 0.032(3) 0.005(2) -0.008(2) -0.014(2) C18C 0.029(2) 0.050(3) 0.045(3) 0.006(3) -0.015(2) -0.026(2) C19C 0.019(2) 0.046(3) 0.039(3) 0.001(3) -0.004(2) -0.013(2) C20C 0.024(2) 0.045(3) 0.036(3) 0.015(2) -0.015(2) -0.013(2) C21C 0.041(3) 0.024(3) 0.050(3) -0.003(2) -0.013(3) -0.017(2) C22C 0.035(3) 0.030(3) 0.044(3) -0.008(2) -0.008(2) -0.004(2) C23C 0.058(3) 0.021(3) 0.044(3) 0.010(2) -0.016(3) -0.018(2) C24C 0.037(3) 0.046(3) 0.036(3) 0.008(3) -0.021(2) -0.010(3) C25C 0.049(3) 0.042(3) 0.026(3) 0.005(2) -0.016(2) -0.009(3) C26C 0.054(3) 0.034(3) 0.036(3) 0.002(2) -0.029(3) -0.018(3) C27C 0.043(3) 0.021(3) 0.045(3) -0.009(2) -0.016(2) -0.012(2) C28C 0.050(3) 0.032(3) 0.038(3) -0.013(2) -0.005(3) -0.014(3) C29C 0.045(3) 0.018(3) 0.063(4) 0.000(3) -0.025(3) -0.004(2) C30C 0.037(3) 0.053(4) 0.028(3) 0.007(3) -0.007(2) -0.010(3) C31C 0.024(2) 0.038(3) 0.040(3) 0.000(2) -0.001(2) -0.008(2) C32C 0.028(2) 0.033(3) 0.041(3) 0.007(2) -0.008(2) -0.017(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Ge N2 1.875(3) . ? Ge N1 1.885(3) . ? Ge P3 2.3914(11) . ? Ge P6 2.4093(11) . ? P1 C1 1.876(5) . ? P1 C2 1.878(4) . ? P1 C3 1.904(4) . ? P2 C1 1.876(4) . ? P2 C4 1.937(4) . ? P2 P3 2.1846(16) . ? P3 C2 1.864(4) . ? P4 C3 1.873(5) . ? P4 C4 1.888(4) . ? P4 C1 1.902(4) . ? P5 C3 1.872(4) . ? P5 C2 1.934(4) . ? P5 P6 2.1930(16) . ? P6 C4 1.856(4) . ? Si1 N1 1.782(3) . ? Si1 C21 1.868(4) . ? Si1 C22 1.869(5) . ? Si1 C23 1.876(5) . ? Si2 N1 1.776(3) . ? Si2 C26 1.851(4) . ? Si2 C24 1.871(5) . ? Si2 C25 1.889(5) . ? Si3 N2 1.779(3) . ? Si3 C28 1.864(5) . ? Si3 C29 1.867(5) . ? Si3 C27 1.868(4) . ? Si4 N2 1.779(3) . ? Si4 C32 1.860(4) . ? Si4 C31 1.868(5) . ? Si4 C30 1.884(5) . ? C1 C5 1.560(6) . ? C2 C9 1.587(6) . ? C3 C13 1.560(6) . ? C4 C17 1.582(6) . ? C5 C6 1.519(6) . ? C5 C8 1.527(6) . ? C5 C7 1.534(6) . ? C9 C10 1.528(6) . ? C9 C12 1.530(6) . ? C9 C11 1.542(6) . ? C13 C16 1.515(7) . ? C13 C15 1.534(6) . ? C13 C14 1.537(6) . ? C17 C20 1.527(6) . ? C17 C19 1.534(6) . ? C17 C18 1.541(6) . ? Ge1B N2B 1.883(3) . ? Ge1B N1B 1.886(3) . ? Ge1B P6B 2.3869(12) . ? Ge1B P3B 2.3927(12) . ? P1B C1B 1.871(4) . ? P1B C2B 1.883(4) . ? P1B C3B 1.903(4) . ? P2B C1B 1.881(4) . ? P2B C4B 1.934(4) . ? P2B P3B 2.1901(15) . ? P3B C2B 1.859(4) . ? P4B C3B 1.873(4) . ? P4B C4B 1.884(4) . ? P4B C1B 1.898(4) . ? P5B C3B 1.877(4) . ? P5B C2B 1.925(4) . ? P5B P6B 2.1919(14) . ? P6B C4B 1.856(4) . ? Si1B N1B 1.782(4) . ? Si1B C21B 1.867(5) . ? Si1B C22B 1.868(5) . ? Si1B C23B 1.873(5) . ? Si2B N1B 1.771(4) . ? Si2B C26B 1.858(5) . ? Si2B C25B 1.876(5) . ? Si2B C24B 1.885(4) . ? Si3B N2B 1.779(4) . ? Si3B C27B 1.860(5) . ? Si3B C28B 1.870(5) . ? Si3B C29B 1.871(4) . ? Si4B N2B 1.770(4) . ? Si4B C32B 1.863(5) . ? Si4B C31B 1.880(4) . ? Si4B C30B 1.882(5) . ? C1B C5B 1.551(6) . ? C2B C9B 1.578(5) . ? C3B C13B 1.557(6) . ? C4B C17B 1.576(5) . ? C5B C8B 1.530(6) . ? C5B C6B 1.532(6) . ? C5B C7B 1.534(6) . ? C9B C12B 1.522(6) . ? C9B C11B 1.533(6) . ? C9B C10B 1.545(6) . ? C13B C16B 1.526(6) . ? C13B C15B 1.529(6) . ? C13B C14B 1.538(6) . ? C17B C20B 1.530(6) . ? C17B C18B 1.538(6) . ? C17B C19B 1.546(6) . ? Ge1C N2C 1.882(3) . ? Ge1C N1C 1.885(3) . ? Ge1C P6C 2.3928(12) . ? Ge1C P3C 2.4002(12) . ? P1C C1C 1.872(4) . ? P1C C2C 1.880(4) . ? P1C C3C 1.901(5) . ? P2C C1C 1.882(4) . ? P2C C4C 1.921(5) . ? P2C P3C 2.1905(15) . ? P3C C2C 1.860(4) . ? P4C C3C 1.874(4) . ? P4C C4C 1.885(4) . ? P4C C1C 1.907(5) . ? P5C C3C 1.875(4) . ? P5C C2C 1.924(5) . ? P5C P6C 2.1941(15) . ? P6C C4C 1.857(4) . ? Si1C N1C 1.772(4) . ? Si1C C21C 1.862(5) . ? Si1C C22C 1.864(5) . ? Si1C C23C 1.875(5) . ? Si2C N1C 1.767(3) . ? Si2C C26C 1.855(5) . ? Si2C C25C 1.876(5) . ? Si2C C24C 1.878(4) . ? Si3C N2C 1.775(4) . ? Si3C C27C 1.868(5) . ? Si3C C28C 1.877(5) . ? Si3C C29C 1.878(4) . ? Si4C N2C 1.778(4) . ? Si4C C32C 1.863(5) . ? Si4C C31C 1.872(4) . ? Si4C C30C 1.879(5) . ? C1C C5C 1.550(6) . ? C2C C9C 1.592(5) . ? C3C C13C 1.560(6) . ? C4C C17C 1.590(5) . ? C5C C8C 1.530(7) . ? C5C C6C 1.531(7) . ? C5C C7C 1.547(7) . ? C9C C12C 1.522(6) . ? C9C C11C 1.532(7) . ? C9C C10C 1.534(6) . ? C13C C15C 1.530(7) . ? C13C C16C 1.534(6) . ? C13C C14C 1.537(7) . ? C17C C19C 1.533(6) . ? C17C C20C 1.535(6) . ? C17C C18C 1.536(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Ge N1 109.21(15) . . ? N2 Ge P3 117.07(11) . . ? N1 Ge P3 110.33(10) . . ? N2 Ge P6 111.07(10) . . ? N1 Ge P6 117.82(11) . . ? P3 Ge P6 90.65(4) . . ? C1 P1 C2 101.86(19) . . ? C1 P1 C3 87.33(18) . . ? C2 P1 C3 88.03(18) . . ? C1 P2 C4 87.62(18) . . ? C1 P2 P3 97.24(14) . . ? C4 P2 P3 107.77(14) . . ? C2 P3 P2 99.60(14) . . ? C2 P3 Ge 101.50(13) . . ? P2 P3 Ge 91.59(5) . . ? C3 P4 C4 101.57(19) . . ? C3 P4 C1 87.47(18) . . ? C4 P4 C1 88.28(17) . . ? C3 P5 C2 87.28(18) . . ? C3 P5 P6 97.75(14) . . ? C2 P5 P6 107.63(14) . . ? C4 P6 P5 99.23(14) . . ? C4 P6 Ge 100.29(13) . . ? P5 P6 Ge 92.68(5) . . ? N1 Si1 C21 117.81(19) . . ? N1 Si1 C22 114.45(19) . . ? C21 Si1 C22 104.5(2) . . ? N1 Si1 C23 109.5(2) . . ? C21 Si1 C23 103.3(2) . . ? C22 Si1 C23 106.1(2) . . ? N1 Si2 C26 111.61(19) . . ? N1 Si2 C24 113.4(2) . . ? C26 Si2 C24 105.6(2) . . ? N1 Si2 C25 113.8(2) . . ? C26 Si2 C25 107.5(2) . . ? C24 Si2 C25 104.2(2) . . ? N2 Si3 C28 109.33(19) . . ? N2 Si3 C29 114.79(18) . . ? C28 Si3 C29 106.7(2) . . ? N2 Si3 C27 117.13(19) . . ? C28 Si3 C27 104.3(2) . . ? C29 Si3 C27 103.6(2) . . ? N2 Si4 C32 111.61(19) . . ? N2 Si4 C31 112.80(18) . . ? C32 Si4 C31 106.2(2) . . ? N2 Si4 C30 113.86(19) . . ? C32 Si4 C30 107.3(2) . . ? C31 Si4 C30 104.5(2) . . ? Si2 N1 Si1 114.37(19) . . ? Si2 N1 Ge 119.18(18) . . ? Si1 N1 Ge 126.41(19) . . ? Si4 N2 Si3 113.91(19) . . ? Si4 N2 Ge 119.13(17) . . ? Si3 N2 Ge 126.94(18) . . ? C5 C1 P2 116.4(3) . . ? C5 C1 P1 112.9(3) . . ? P2 C1 P1 116.4(2) . . ? C5 C1 P4 123.5(3) . . ? P2 C1 P4 92.37(18) . . ? P1 C1 P4 92.03(19) . . ? C9 C2 P3 110.6(3) . . ? C9 C2 P1 110.0(3) . . ? P3 C2 P1 112.0(2) . . ? C9 C2 P5 116.9(3) . . ? P3 C2 P5 114.5(2) . . ? P1 C2 P5 91.40(17) . . ? C13 C3 P5 116.7(3) . . ? C13 C3 P4 113.3(3) . . ? P5 C3 P4 116.5(2) . . ? C13 C3 P1 122.3(3) . . ? P5 C3 P1 92.52(18) . . ? P4 C3 P1 92.09(19) . . ? C17 C4 P6 110.9(3) . . ? C17 C4 P4 109.4(3) . . ? P6 C4 P4 112.8(2) . . ? C17 C4 P2 116.9(3) . . ? P6 C4 P2 114.4(2) . . ? P4 C4 P2 90.92(17) . . ? C6 C5 C8 110.1(4) . . ? C6 C5 C7 109.6(4) . . ? C8 C5 C7 108.6(4) . . ? C6 C5 C1 108.3(4) . . ? C8 C5 C1 111.3(4) . . ? C7 C5 C1 109.0(4) . . ? C10 C9 C12 108.8(4) . . ? C10 C9 C11 108.2(4) . . ? C12 C9 C11 108.3(3) . . ? C10 C9 C2 111.7(3) . . ? C12 C9 C2 110.6(3) . . ? C11 C9 C2 109.2(4) . . ? C16 C13 C15 110.6(4) . . ? C16 C13 C14 108.1(4) . . ? C15 C13 C14 108.7(4) . . ? C16 C13 C3 111.3(4) . . ? C15 C13 C3 107.8(4) . . ? C14 C13 C3 110.4(4) . . ? C20 C17 C19 108.5(4) . . ? C20 C17 C18 108.4(4) . . ? C19 C17 C18 108.0(4) . . ? C20 C17 C4 110.7(4) . . ? C19 C17 C4 111.4(3) . . ? C18 C17 C4 109.8(4) . . ? N2B Ge1B N1B 110.66(15) . . ? N2B Ge1B P6B 108.51(11) . . ? N1B Ge1B P6B 118.41(11) . . ? N2B Ge1B P3B 117.89(11) . . ? N1B Ge1B P3B 109.25(11) . . ? P6B Ge1B P3B 91.28(4) . . ? C1B P1B C2B 102.03(17) . . ? C1B P1B C3B 87.16(18) . . ? C2B P1B C3B 87.64(18) . . ? C1B P2B C4B 87.32(18) . . ? C1B P2B P3B 97.82(13) . . ? C4B P2B P3B 107.61(13) . . ? C2B P3B P2B 99.16(13) . . ? C2B P3B Ge1B 100.67(14) . . ? P2B P3B Ge1B 91.76(5) . . ? C3B P4B C4B 101.95(18) . . ? C3B P4B C1B 87.26(18) . . ? C4B P4B C1B 88.26(19) . . ? C3B P5B C2B 87.17(19) . . ? C3B P5B P6B 97.69(13) . . ? C2B P5B P6B 107.81(12) . . ? C4B P6B P5B 99.26(13) . . ? C4B P6B Ge1B 100.53(14) . . ? P5B P6B Ge1B 91.89(5) . . ? N1B Si1B C21B 117.49(19) . . ? N1B Si1B C22B 115.4(2) . . ? C21B Si1B C22B 104.5(2) . . ? N1B Si1B C23B 109.4(2) . . ? C21B Si1B C23B 104.0(2) . . ? C22B Si1B C23B 104.7(2) . . ? N1B Si2B C26B 111.81(19) . . ? N1B Si2B C25B 113.1(2) . . ? C26B Si2B C25B 106.7(2) . . ? N1B Si2B C24B 113.4(2) . . ? C26B Si2B C24B 105.5(2) . . ? C25B Si2B C24B 105.7(2) . . ? N2B Si3B C27B 118.84(19) . . ? N2B Si3B C28B 109.0(2) . . ? C27B Si3B C28B 103.4(2) . . ? N2B Si3B C29B 114.4(2) . . ? C27B Si3B C29B 103.5(2) . . ? C28B Si3B C29B 106.5(2) . . ? N2B Si4B C32B 110.9(2) . . ? N2B Si4B C31B 113.9(2) . . ? C32B Si4B C31B 106.8(2) . . ? N2B Si4B C30B 113.7(2) . . ? C32B Si4B C30B 107.1(2) . . ? C31B Si4B C30B 103.9(2) . . ? Si2B N1B Si1B 114.02(18) . . ? Si2B N1B Ge1B 119.3(2) . . ? Si1B N1B Ge1B 126.6(2) . . ? Si4B N2B Si3B 114.33(19) . . ? Si4B N2B Ge1B 119.2(2) . . ? Si3B N2B Ge1B 126.44(19) . . ? C5B C1B P1B 114.3(3) . . ? C5B C1B P2B 115.2(3) . . ? P1B C1B P2B 115.9(2) . . ? C5B C1B P4B 123.2(3) . . ? P1B C1B P4B 92.42(19) . . ? P2B C1B P4B 92.46(19) . . ? C9B C2B P3B 110.8(3) . . ? C9B C2B P1B 110.1(3) . . ? P3B C2B P1B 112.3(2) . . ? C9B C2B P5B 115.9(3) . . ? P3B C2B P5B 114.7(2) . . ? P1B C2B P5B 91.78(18) . . ? C13B C3B P4B 113.6(3) . . ? C13B C3B P5B 115.5(3) . . ? P4B C3B P5B 116.1(2) . . ? C13B C3B P1B 123.8(3) . . ? P4B C3B P1B 92.19(19) . . ? P5B C3B P1B 92.67(19) . . ? C17B C4B P6B 110.2(3) . . ? C17B C4B P4B 110.2(3) . . ? P6B C4B P4B 112.3(2) . . ? C17B C4B P2B 116.8(3) . . ? P6B C4B P2B 114.7(2) . . ? P4B C4B P2B 91.23(19) . . ? C8B C5B C6B 109.3(4) . . ? C8B C5B C7B 107.1(4) . . ? C6B C5B C7B 110.2(4) . . ? C8B C5B C1B 111.2(4) . . ? C6B C5B C1B 108.4(4) . . ? C7B C5B C1B 110.6(4) . . ? C12B C9B C11B 108.9(4) . . ? C12B C9B C10B 108.3(4) . . ? C11B C9B C10B 108.3(3) . . ? C12B C9B C2B 110.7(3) . . ? C11B C9B C2B 109.7(3) . . ? C10B C9B C2B 111.0(3) . . ? C16B C13B C15B 110.6(4) . . ? C16B C13B C14B 107.9(3) . . ? C15B C13B C14B 109.8(4) . . ? C16B C13B C3B 111.1(3) . . ? C15B C13B C3B 107.6(3) . . ? C14B C13B C3B 109.9(4) . . ? C20B C17B C18B 108.6(4) . . ? C20B C17B C19B 108.2(4) . . ? C18B C17B C19B 108.7(4) . . ? C20B C17B C4B 110.8(3) . . ? C18B C17B C4B 109.4(3) . . ? C19B C17B C4B 111.2(4) . . ? N2C Ge1C N1C 109.42(14) . . ? N2C Ge1C P6C 109.08(11) . . ? N1C Ge1C P6C 118.64(11) . . ? N2C Ge1C P3C 118.56(11) . . ? N1C Ge1C P3C 109.66(11) . . ? P6C Ge1C P3C 90.93(4) . . ? C1C P1C C2C 101.93(18) . . ? C1C P1C C3C 87.5(2) . . ? C2C P1C C3C 88.01(19) . . ? C1C P2C C4C 87.23(19) . . ? C1C P2C P3C 98.09(13) . . ? C4C P2C P3C 107.53(14) . . ? C2C P3C P2C 98.88(13) . . ? C2C P3C Ge1C 100.43(14) . . ? P2C P3C Ge1C 92.47(5) . . ? C3C P4C C4C 101.82(19) . . ? C3C P4C C1C 87.3(2) . . ? C4C P4C C1C 87.58(19) . . ? C3C P5C C2C 87.47(19) . . ? C3C P5C P6C 97.15(13) . . ? C2C P5C P6C 107.89(13) . . ? C4C P6C P5C 99.30(13) . . ? C4C P6C Ge1C 100.88(14) . . ? P5C P6C Ge1C 91.25(5) . . ? N1C Si1C C21C 118.15(19) . . ? N1C Si1C C22C 114.4(2) . . ? C21C Si1C C22C 103.0(2) . . ? N1C Si1C C23C 109.6(2) . . ? C21C Si1C C23C 104.1(2) . . ? C22C Si1C C23C 106.6(2) . . ? N1C Si2C C26C 110.34(18) . . ? N1C Si2C C25C 114.0(2) . . ? C26C Si2C C25C 107.8(2) . . ? N1C Si2C C24C 114.0(2) . . ? C26C Si2C C24C 107.0(2) . . ? C25C Si2C C24C 103.2(2) . . ? N2C Si3C C27C 118.09(19) . . ? N2C Si3C C28C 110.9(2) . . ? C27C Si3C C28C 102.8(2) . . ? N2C Si3C C29C 113.0(2) . . ? C27C Si3C C29C 105.0(2) . . ? C28C Si3C C29C 105.9(2) . . ? N2C Si4C C32C 111.65(19) . . ? N2C Si4C C31C 113.8(2) . . ? C32C Si4C C31C 105.9(2) . . ? N2C Si4C C30C 112.6(2) . . ? C32C Si4C C30C 108.2(2) . . ? C31C Si4C C30C 104.2(2) . . ? Si2C N1C Si1C 114.68(18) . . ? Si2C N1C Ge1C 118.75(19) . . ? Si1C N1C Ge1C 126.52(19) . . ? Si3C N2C Si4C 113.65(19) . . ? Si3C N2C Ge1C 127.6(2) . . ? Si4C N2C Ge1C 118.76(19) . . ? C5C C1C P1C 113.6(3) . . ? C5C C1C P2C 116.1(3) . . ? P1C C1C P2C 115.8(2) . . ? C5C C1C P4C 123.3(3) . . ? P1C C1C P4C 92.0(2) . . ? P2C C1C P4C 92.51(19) . . ? C9C C2C P3C 109.3(3) . . ? C9C C2C P1C 109.7(3) . . ? P3C C2C P1C 113.0(2) . . ? C9C C2C P5C 117.9(3) . . ? P3C C2C P5C 114.4(2) . . ? P1C C2C P5C 91.44(19) . . ? C13C C3C P4C 114.3(3) . . ? C13C C3C P5C 115.2(3) . . ? P4C C3C P5C 116.3(2) . . ? C13C C3C P1C 123.4(3) . . ? P4C C3C P1C 92.1(2) . . ? P5C C3C P1C 92.3(2) . . ? C17C C4C P6C 110.6(3) . . ? C17C C4C P4C 110.1(3) . . ? P6C C4C P4C 111.7(2) . . ? C17C C4C P2C 115.8(3) . . ? P6C C4C P2C 115.2(2) . . ? P4C C4C P2C 91.98(19) . . ? C8C C5C C6C 110.0(5) . . ? C8C C5C C7C 107.6(4) . . ? C6C C5C C7C 108.8(4) . . ? C8C C5C C1C 112.0(4) . . ? C6C C5C C1C 108.4(4) . . ? C7C C5C C1C 109.9(4) . . ? C12C C9C C11C 108.7(4) . . ? C12C C9C C10C 108.5(4) . . ? C11C C9C C10C 108.8(4) . . ? C12C C9C C2C 110.7(3) . . ? C11C C9C C2C 108.7(4) . . ? C10C C9C C2C 111.4(4) . . ? C15C C13C C16C 109.0(5) . . ? C15C C13C C14C 110.1(4) . . ? C16C C13C C14C 108.0(4) . . ? C15C C13C C3C 108.0(4) . . ? C16C C13C C3C 111.5(4) . . ? C14C C13C C3C 110.2(4) . . ? C19C C17C C20C 108.1(4) . . ? C19C C17C C18C 108.9(4) . . ? C20C C17C C18C 108.4(4) . . ? C19C C17C C4C 111.0(4) . . ? C20C C17C C4C 110.1(3) . . ? C18C C17C C4C 110.2(4) . . ? #===END # Attachment 'mar401.cif' data_mar401 _database_code_depnum_ccdc_archive 'CCDC 674811' _audit_creation_date 2001-03-05T10:44:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[Pb{P6(CtBu)4}{C6H3(NMe2)2}2]' _chemical_formula_moiety 'C40 H66 N4 P6 Pb1' _chemical_formula_structural 'C40 H66 N4 P6 PB' _chemical_formula_sum 'C40 H66 N4 P6 Pb' _chemical_formula_weight 995.98 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.2177(3) _cell_length_b 33.3392(11) _cell_length_c 13.1175(4) _cell_angle_alpha 90 _cell_angle_beta 112.074(2) _cell_angle_gamma 90 _cell_volume 4546.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 33423 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.455 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2024 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.954 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.455 _exptl_absorpt_correction_T_max 0.558 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 23962 _diffrn_reflns_av_R_equivalents 0.0697 _diffrn_reflns_av_unetI/netI 0.0844 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -43 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.82 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.972 _diffrn_measured_fraction_theta_max 0.972 _reflns_number_total 10524 _reflns_number_gt 7750 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldri8ck, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0419P)^2^+0.6017P] 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_number_reflns 10524 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.075 _refine_ls_R_factor_gt 0.0461 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.093 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.344 _refine_diff_density_min -1.844 _refine_diff_density_rms 0.158 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pb Pb 0.257109(18) 0.104479(6) 0.700176(15) 0.01999(7) Uani 1 1 d . . . P1 P 0.08931(14) 0.20057(5) 0.38639(11) 0.0288(3) Uani 1 1 d . . . P2 P 0.35732(13) 0.15809(4) 0.51637(11) 0.0239(3) Uani 1 1 d . . . P3 P 0.26162(13) 0.17711(4) 0.62429(11) 0.0237(3) Uani 1 1 d . . . P4 P 0.19036(15) 0.13749(4) 0.31060(11) 0.0268(3) Uani 1 1 d . . . P5 P 0.01601(13) 0.12986(5) 0.45138(11) 0.0269(3) Uani 1 1 d . . . P6 P 0.16195(13) 0.08377(4) 0.49118(11) 0.0228(3) Uani 1 1 d . . . N1 N 0.3253(4) 0.01411(13) 0.7696(3) 0.0238(10) Uani 1 1 d . . . N2 N 0.5598(4) 0.13838(14) 0.7866(4) 0.0298(11) Uani 1 1 d . . . N3 N 0.3188(5) 0.12514(15) 0.9575(4) 0.0322(11) Uani 1 1 d . . . N4 N -0.0317(4) 0.06559(16) 0.6486(4) 0.0339(12) Uani 1 1 d . . . C1 C 0.2529(5) 0.18586(16) 0.3893(4) 0.0285(12) Uani 1 1 d . . . C2 C 0.0938(5) 0.17983(17) 0.5220(4) 0.0281(12) Uani 1 1 d . . . C3 C 0.0329(5) 0.14897(17) 0.3234(4) 0.0275(12) Uani 1 1 d . . . C4 C 0.2784(5) 0.10932(15) 0.4413(4) 0.0219(11) Uani 1 1 d . . . C5 C 0.3196(6) 0.21898(17) 0.3469(5) 0.0346(14) Uani 1 1 d . . . C6 C 0.3514(6) 0.25413(17) 0.4291(5) 0.0397(15) Uani 1 1 d . . . H6A H 0.2722 0.2636 0.4363 0.06 Uiso 1 1 calc R . . H6B H 0.3901 0.276 0.4024 0.06 Uiso 1 1 calc R . . H6C H 0.412 0.2451 0.501 0.06 Uiso 1 1 calc R . . C7 C 0.2291(6) 0.23373(18) 0.2330(5) 0.0409(15) Uani 1 1 d . . . H7A H 0.1487 0.2434 0.2374 0.061 Uiso 1 1 calc R . . H7B H 0.2105 0.2116 0.1801 0.061 Uiso 1 1 calc R . . H7C H 0.2705 0.2556 0.2087 0.061 Uiso 1 1 calc R . . C8 C 0.4439(6) 0.20404(19) 0.3380(5) 0.0430(16) Uani 1 1 d . . . H8A H 0.4832 0.2258 0.3112 0.064 Uiso 1 1 calc R . . H8B H 0.4247 0.1814 0.2866 0.064 Uiso 1 1 calc R . . H8C H 0.5035 0.1953 0.4106 0.064 Uiso 1 1 calc R . . C9 C 0.0054(6) 0.20430(18) 0.5698(5) 0.0349(14) Uani 1 1 d . . . C10 C -0.1337(6) 0.2075(2) 0.4863(5) 0.0510(19) Uani 1 1 d . . . H10A H -0.1346 0.2215 0.4203 0.077 Uiso 1 1 calc R . . H10B H -0.1854 0.2226 0.5191 0.077 Uiso 1 1 calc R . . H10C H -0.1698 0.1806 0.4663 0.077 Uiso 1 1 calc R . . C11 C 0.0605(7) 0.24648(19) 0.6017(5) 0.0486(18) Uani 1 1 d . . . H11A H 0.0623 0.2604 0.5364 0.073 Uiso 1 1 calc R . . H11B H 0.1481 0.2446 0.657 0.073 Uiso 1 1 calc R . . H11C H 0.0065 0.2615 0.6322 0.073 Uiso 1 1 calc R . . C12 C 0.0025(6) 0.18242(19) 0.6724(5) 0.0425(16) Uani 1 1 d . . . H12A H 0.0904 0.1799 0.727 0.064 Uiso 1 1 calc R . . H12B H -0.0347 0.1556 0.6515 0.064 Uiso 1 1 calc R . . H12C H -0.0499 0.1978 0.7039 0.064 Uiso 1 1 calc R . . C13 C -0.0850(6) 0.14324(19) 0.2150(5) 0.0380(15) Uani 1 1 d . . . C14 C -0.0657(7) 0.1654(2) 0.1189(5) 0.0518(18) Uani 1 1 d . . . H14A H 0.0118 0.1552 0.1101 0.078 Uiso 1 1 calc R . . H14B H -0.056 0.1942 0.1347 0.078 Uiso 1 1 calc R . . H14C H -0.1405 0.1608 0.0509 0.078 Uiso 1 1 calc R . . C15 C -0.1023(7) 0.0985(2) 0.1881(5) 0.0530(19) Uani 1 1 d . . . H15A H -0.0243 0.0879 0.1812 0.08 Uiso 1 1 calc R . . H15B H -0.1757 0.0947 0.1187 0.08 Uiso 1 1 calc R . . H15C H -0.1182 0.0844 0.2472 0.08 Uiso 1 1 calc R . . C16 C -0.2070(6) 0.1600(3) 0.2252(6) 0.065(2) Uani 1 1 d . . . H16A H -0.2801 0.1562 0.1555 0.097 Uiso 1 1 calc R . . H16B H -0.1955 0.1886 0.2428 0.097 Uiso 1 1 calc R . . H16C H -0.2236 0.1458 0.284 0.097 Uiso 1 1 calc R . . C17 C 0.3788(5) 0.07849(17) 0.4279(4) 0.0275(12) Uani 1 1 d . . . C18 C 0.3091(6) 0.04507(18) 0.3475(5) 0.0405(15) Uani 1 1 d . . . H18A H 0.2576 0.0568 0.276 0.061 Uiso 1 1 calc R . . H18B H 0.2527 0.0304 0.3762 0.061 Uiso 1 1 calc R . . H18C H 0.3726 0.0266 0.3388 0.061 Uiso 1 1 calc R . . C19 C 0.4729(6) 0.09959(18) 0.3843(5) 0.0412(16) Uani 1 1 d . . . H19A H 0.4244 0.1118 0.3126 0.062 Uiso 1 1 calc R . . H19B H 0.5337 0.0799 0.3763 0.062 Uiso 1 1 calc R . . H19C H 0.5204 0.1205 0.4363 0.062 Uiso 1 1 calc R . . C20 C 0.4586(5) 0.06006(18) 0.5383(4) 0.0355(14) Uani 1 1 d . . . H20A H 0.5034 0.0813 0.59 0.053 Uiso 1 1 calc R . . H20B H 0.5218 0.0416 0.5292 0.053 Uiso 1 1 calc R . . H20C H 0.4022 0.0454 0.5669 0.053 Uiso 1 1 calc R . . C21 C 0.4477(5) 0.07605(15) 0.7881(4) 0.0194(11) Uani 1 1 d . . . C22 C 0.5646(5) 0.09684(16) 0.8153(4) 0.0235(11) Uani 1 1 d . . . C23 C 0.6789(5) 0.07594(19) 0.8624(4) 0.0311(13) Uani 1 1 d . . . H23 H 0.7585 0.0898 0.883 0.037 Uiso 1 1 calc R . . C24 C 0.6781(5) 0.03509(19) 0.8795(4) 0.0336(14) Uani 1 1 d . . . H24 H 0.7574 0.0211 0.9117 0.04 Uiso 1 1 calc R . . C25 C 0.5641(5) 0.01422(18) 0.8507(4) 0.0309(13) Uani 1 1 d . . . H25 H 0.5644 -0.014 0.8616 0.037 Uiso 1 1 calc R . . C26 C 0.4481(5) 0.03505(16) 0.8054(4) 0.0225(11) Uani 1 1 d . . . C27 C 0.3192(6) -0.02019(18) 0.6972(5) 0.0372(14) Uani 1 1 d . . . H27A H 0.2347 -0.033 0.6754 0.056 Uiso 1 1 calc R . . H27B H 0.3863 -0.0396 0.7366 0.056 Uiso 1 1 calc R . . H27C H 0.3326 -0.0108 0.6315 0.056 Uiso 1 1 calc R . . C28 C 0.2959(5) 0.00080(17) 0.8640(4) 0.0315(13) Uani 1 1 d . . . H28A H 0.2128 -0.0131 0.8378 0.047 Uiso 1 1 calc R . . H28B H 0.2919 0.0241 0.9081 0.047 Uiso 1 1 calc R . . H28C H 0.3633 -0.0175 0.9093 0.047 Uiso 1 1 calc R . . C29 C 0.5398(5) 0.16540(18) 0.8659(5) 0.0343(14) Uani 1 1 d . . . H29A H 0.5375 0.1931 0.8405 0.051 Uiso 1 1 calc R . . H29B H 0.6105 0.1623 0.9374 0.051 Uiso 1 1 calc R . . H29C H 0.4581 0.1589 0.8731 0.051 Uiso 1 1 calc R . . C30 C 0.6677(6) 0.15214(19) 0.7580(5) 0.0439(16) Uani 1 1 d . . . H30A H 0.6572 0.1807 0.7395 0.066 Uiso 1 1 calc R . . H30B H 0.6691 0.1369 0.6946 0.066 Uiso 1 1 calc R . . H30C H 0.7487 0.148 0.8207 0.066 Uiso 1 1 calc R . . C31 C 0.1456(5) 0.09198(16) 0.8071(4) 0.0248(12) Uani 1 1 d . . . C32 C 0.2027(5) 0.10088(17) 0.9182(4) 0.0282(12) Uani 1 1 d . . . C33 C 0.1450(6) 0.0873(2) 0.9900(5) 0.0418(16) Uani 1 1 d . . . H33 H 0.1831 0.0932 1.0664 0.05 Uiso 1 1 calc R . . C34 C 0.0324(6) 0.0654(2) 0.9487(5) 0.053(2) Uani 1 1 d . . . H34 H -0.0053 0.0554 0.9975 0.064 Uiso 1 1 calc R . . C35 C -0.0262(6) 0.0579(2) 0.8372(5) 0.0461(18) Uani 1 1 d . . . H35 H -0.1049 0.0434 0.8093 0.055 Uiso 1 1 calc R . . C36 C 0.0303(5) 0.07154(18) 0.7664(4) 0.0294(13) Uani 1 1 d . . . C37 C 0.2935(7) 0.1646(2) 0.9901(6) 0.060(2) Uani 1 1 d . . . H37A H 0.3731 0.1803 1.0154 0.091 Uiso 1 1 calc R . . H37B H 0.2616 0.1622 1.0498 0.091 Uiso 1 1 calc R . . H37C H 0.2287 0.178 0.9271 0.091 Uiso 1 1 calc R . . C38 C 0.4262(6) 0.1051(2) 1.0454(5) 0.0482(18) Uani 1 1 d . . . H38A H 0.5019 0.1226 1.069 0.072 Uiso 1 1 calc R . . H38B H 0.4467 0.0799 1.0175 0.072 Uiso 1 1 calc R . . H38C H 0.4013 0.0996 1.1081 0.072 Uiso 1 1 calc R . . C39 C -0.0114(6) 0.0247(2) 0.6175(5) 0.0477(18) Uani 1 1 d . . . H39A H -0.054 0.0216 0.5377 0.072 Uiso 1 1 calc R . . H39B H -0.0476 0.0055 0.6546 0.072 Uiso 1 1 calc R . . H39C H 0.081 0.0198 0.6395 0.072 Uiso 1 1 calc R . . C40 C -0.1686(5) 0.0756(2) 0.6029(5) 0.0436(16) Uani 1 1 d . . . H40A H -0.2031 0.0709 0.5234 0.065 Uiso 1 1 calc R . . H40B H -0.1799 0.1039 0.6174 0.065 Uiso 1 1 calc R . . H40C H -0.2146 0.0588 0.6374 0.065 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 Pb 0.02349(10) 0.02005(10) 0.01758(10) -0.00073(9) 0.00901(8) 0.00158(9) P1 0.0378(8) 0.0232(8) 0.0245(7) 0.0036(6) 0.0105(7) 0.0091(6) P2 0.0308(7) 0.0221(8) 0.0211(7) -0.0012(6) 0.0124(6) 0.0013(6) P3 0.0311(7) 0.0202(7) 0.0212(7) -0.0028(6) 0.0114(6) 0.0017(6) P4 0.0418(8) 0.0208(8) 0.0183(7) 0.0006(6) 0.0119(6) 0.0034(6) P5 0.0279(7) 0.0279(8) 0.0226(7) 0.0021(6) 0.0069(6) 0.0037(6) P6 0.0314(7) 0.0173(7) 0.0189(7) -0.0010(6) 0.0084(6) 0.0001(6) N1 0.034(2) 0.017(2) 0.024(2) 0.0012(19) 0.016(2) -0.0028(19) N2 0.028(2) 0.029(3) 0.032(3) -0.001(2) 0.012(2) -0.007(2) N3 0.041(3) 0.030(3) 0.026(3) -0.011(2) 0.013(2) -0.009(2) N4 0.024(2) 0.047(3) 0.032(3) -0.012(2) 0.012(2) -0.006(2) C1 0.041(3) 0.020(3) 0.026(3) 0.000(2) 0.015(3) -0.001(3) C2 0.033(3) 0.028(3) 0.027(3) 0.002(2) 0.016(3) 0.011(2) C3 0.032(3) 0.027(3) 0.019(3) 0.003(2) 0.005(2) 0.004(2) C4 0.038(3) 0.016(3) 0.017(2) -0.001(2) 0.016(2) 0.004(2) C5 0.057(4) 0.022(3) 0.032(3) 0.004(3) 0.024(3) 0.001(3) C6 0.060(4) 0.021(3) 0.041(4) -0.001(3) 0.022(3) -0.011(3) C7 0.066(4) 0.026(3) 0.033(3) 0.005(3) 0.022(3) -0.001(3) C8 0.060(4) 0.031(4) 0.054(4) 0.008(3) 0.039(4) -0.002(3) C9 0.045(3) 0.029(3) 0.035(3) 0.004(3) 0.021(3) 0.016(3) C10 0.041(4) 0.063(5) 0.054(4) 0.009(4) 0.023(3) 0.029(4) C11 0.076(5) 0.032(4) 0.047(4) 0.001(3) 0.034(4) 0.023(4) C12 0.057(4) 0.036(4) 0.051(4) 0.008(3) 0.039(4) 0.022(3) C13 0.044(3) 0.035(4) 0.027(3) 0.006(3) 0.004(3) 0.004(3) C14 0.057(4) 0.054(5) 0.029(3) 0.015(3) -0.002(3) -0.006(4) C15 0.068(5) 0.048(5) 0.031(4) -0.001(3) 0.005(3) -0.011(4) C16 0.049(4) 0.088(7) 0.043(4) 0.001(4) 0.000(3) 0.007(4) C17 0.036(3) 0.027(3) 0.025(3) 0.002(2) 0.018(3) 0.006(3) C18 0.059(4) 0.027(3) 0.037(3) -0.013(3) 0.021(3) 0.004(3) C19 0.059(4) 0.035(4) 0.044(4) 0.007(3) 0.035(3) 0.012(3) C20 0.042(3) 0.036(4) 0.033(3) 0.003(3) 0.020(3) 0.017(3) C21 0.025(3) 0.021(3) 0.016(2) -0.001(2) 0.012(2) 0.000(2) C22 0.029(3) 0.022(3) 0.016(2) 0.000(2) 0.005(2) -0.001(2) C23 0.023(3) 0.041(4) 0.027(3) 0.002(3) 0.007(2) -0.001(3) C24 0.026(3) 0.042(4) 0.033(3) 0.014(3) 0.013(3) 0.013(3) C25 0.038(3) 0.027(3) 0.029(3) 0.013(3) 0.013(3) 0.009(3) C26 0.029(3) 0.025(3) 0.018(3) 0.003(2) 0.014(2) 0.005(2) C27 0.045(3) 0.040(4) 0.031(3) -0.011(3) 0.019(3) -0.004(3) C28 0.043(3) 0.024(3) 0.035(3) 0.004(3) 0.024(3) 0.000(3) C29 0.034(3) 0.028(3) 0.035(3) -0.009(3) 0.007(3) -0.002(3) C30 0.057(4) 0.031(4) 0.056(4) 0.001(3) 0.035(4) -0.011(3) C31 0.028(3) 0.025(3) 0.025(3) -0.003(2) 0.015(2) 0.002(2) C32 0.030(3) 0.034(3) 0.018(3) -0.003(2) 0.006(2) 0.003(3) C33 0.045(4) 0.065(5) 0.021(3) -0.007(3) 0.019(3) -0.008(3) C34 0.052(4) 0.074(6) 0.049(4) -0.011(4) 0.038(4) -0.019(4) C35 0.036(3) 0.067(5) 0.043(4) -0.011(4) 0.022(3) -0.015(3) C36 0.028(3) 0.036(4) 0.030(3) -0.012(3) 0.018(3) -0.005(3) C37 0.071(5) 0.045(5) 0.070(5) -0.032(4) 0.032(4) -0.017(4) C38 0.039(3) 0.066(5) 0.033(3) 0.005(3) 0.006(3) -0.011(4) C39 0.043(4) 0.060(5) 0.041(4) -0.031(3) 0.017(3) -0.005(3) C40 0.032(3) 0.051(4) 0.046(4) -0.013(3) 0.012(3) -0.005(3) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pb C21 2.224(5) . ? Pb C31 2.241(5) . ? Pb P3 2.6257(14) . ? Pb P6 2.6330(13) . ? P1 C1 1.886(5) . ? P1 C2 1.891(5) . ? P1 C3 1.910(6) . ? P2 C1 1.881(6) . ? P2 C4 1.935(5) . ? P2 P3 2.1682(18) . ? P3 C2 1.859(6) . ? P4 C4 1.877(5) . ? P4 C3 1.876(5) . ? P4 C1 1.901(6) . ? P5 C3 1.870(5) . ? P5 C2 1.946(6) . ? P5 P6 2.161(2) . ? P6 C4 1.872(5) . ? N1 C26 1.456(6) . ? N1 C28 1.466(6) . ? N1 C27 1.471(6) . ? N2 C22 1.431(7) . ? N2 C29 1.455(7) . ? N2 C30 1.469(7) . ? N3 C32 1.452(7) . ? N3 C37 1.443(8) . ? N3 C38 1.478(8) . ? N4 C36 1.450(7) . ? N4 C40 1.462(7) . ? N4 C39 1.465(8) . ? C1 C5 1.550(7) . ? C2 C9 1.584(7) . ? C3 C13 1.548(8) . ? C4 C17 1.582(7) . ? C5 C8 1.525(8) . ? C5 C7 1.538(8) . ? C5 C6 1.541(8) . ? C9 C12 1.541(7) . ? C9 C10 1.537(8) . ? C9 C11 1.530(8) . ? C13 C15 1.527(9) . ? C13 C16 1.531(8) . ? C13 C14 1.545(8) . ? C17 C20 1.517(7) . ? C17 C18 1.531(8) . ? C17 C19 1.547(7) . ? C21 C26 1.385(7) . ? C21 C22 1.405(7) . ? C22 C23 1.385(7) . ? C23 C24 1.381(8) . ? C24 C25 1.379(8) . ? C25 C26 1.395(7) . ? C31 C36 1.380(7) . ? C31 C32 1.387(7) . ? C32 C33 1.403(8) . ? C33 C34 1.382(9) . ? C34 C35 1.384(8) . ? C35 C36 1.383(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C21 Pb C31 104.48(18) . . ? C21 Pb P3 115.97(13) . . ? C31 Pb P3 120.23(14) . . ? C21 Pb P6 111.28(12) . . ? C31 Pb P6 119.96(14) . . ? P3 Pb P6 84.55(4) . . ? C1 P1 C2 101.8(2) . . ? C1 P1 C3 86.4(2) . . ? C2 P1 C3 88.0(2) . . ? C1 P2 C4 87.1(2) . . ? C1 P2 P3 97.95(17) . . ? C4 P2 P3 109.53(15) . . ? C2 P3 P2 99.13(16) . . ? C2 P3 Pb 99.21(19) . . ? P2 P3 Pb 93.59(6) . . ? C4 P4 C3 102.1(2) . . ? C4 P4 C1 88.2(2) . . ? C3 P4 C1 86.9(2) . . ? C3 P5 C2 87.5(2) . . ? C3 P5 P6 97.82(18) . . ? C2 P5 P6 109.29(17) . . ? C4 P6 P5 99.04(17) . . ? C4 P6 Pb 100.47(16) . . ? P5 P6 Pb 92.23(6) . . ? C26 N1 C28 111.0(4) . . ? C26 N1 C27 113.0(4) . . ? C28 N1 C27 109.8(4) . . ? C22 N2 C29 114.3(4) . . ? C22 N2 C30 114.6(5) . . ? C29 N2 C30 110.6(5) . . ? C32 N3 C37 111.3(5) . . ? C32 N3 C38 112.6(5) . . ? C37 N3 C38 111.9(5) . . ? C36 N4 C40 114.5(4) . . ? C36 N4 C39 111.2(5) . . ? C40 N4 C39 110.4(5) . . ? C5 C1 P2 116.4(4) . . ? C5 C1 P1 113.9(4) . . ? P2 C1 P1 115.0(3) . . ? C5 C1 P4 122.6(4) . . ? P2 C1 P4 92.5(2) . . ? P1 C1 P4 93.0(2) . . ? C9 C2 P3 110.7(4) . . ? C9 C2 P1 112.6(4) . . ? P3 C2 P1 111.0(3) . . ? C9 C2 P5 113.2(4) . . ? P3 C2 P5 116.9(3) . . ? P1 C2 P5 91.0(2) . . ? C13 C3 P5 116.3(4) . . ? C13 C3 P4 113.6(4) . . ? P5 C3 P4 115.3(3) . . ? C13 C3 P1 122.6(4) . . ? P5 C3 P1 92.7(2) . . ? P4 C3 P1 93.0(2) . . ? C17 C4 P6 111.2(3) . . ? C17 C4 P4 112.1(3) . . ? P6 C4 P4 110.5(3) . . ? C17 C4 P2 113.2(4) . . ? P6 C4 P2 116.8(2) . . ? P4 C4 P2 91.6(2) . . ? C8 C5 C7 108.6(4) . . ? C8 C5 C6 108.9(5) . . ? C7 C5 C6 109.4(5) . . ? C8 C5 C1 111.9(5) . . ? C7 C5 C1 110.2(5) . . ? C6 C5 C1 107.8(4) . . ? C12 C9 C10 107.9(5) . . ? C12 C9 C11 109.6(5) . . ? C10 C9 C11 109.2(5) . . ? C12 C9 C2 108.9(4) . . ? C10 C9 C2 111.9(5) . . ? C11 C9 C2 109.5(5) . . ? C15 C13 C16 109.6(6) . . ? C15 C13 C3 108.9(5) . . ? C16 C13 C3 110.9(5) . . ? C15 C13 C14 108.9(5) . . ? C16 C13 C14 107.6(5) . . ? C3 C13 C14 111.0(5) . . ? C20 C17 C18 109.2(5) . . ? C20 C17 C19 107.3(5) . . ? C18 C17 C19 108.6(4) . . ? C20 C17 C4 110.3(4) . . ? C18 C17 C4 110.4(4) . . ? C19 C17 C4 111.0(4) . . ? C26 C21 C22 120.0(5) . . ? C26 C21 Pb 116.7(4) . . ? C22 C21 Pb 123.0(4) . . ? C23 C22 C21 119.0(5) . . ? C23 C22 N2 122.8(5) . . ? C21 C22 N2 118.1(5) . . ? C24 C23 C22 120.5(5) . . ? C25 C24 C23 121.0(5) . . ? C24 C25 C26 119.1(5) . . ? C21 C26 C25 120.4(5) . . ? C21 C26 N1 118.4(4) . . ? C25 C26 N1 121.1(5) . . ? C36 C31 C32 120.5(5) . . ? C36 C31 Pb 120.8(4) . . ? C32 C31 Pb 118.2(4) . . ? C31 C32 C33 119.3(5) . . ? C31 C32 N3 119.4(5) . . ? C33 C32 N3 121.3(5) . . ? C34 C33 C32 119.4(5) . . ? C33 C34 C35 120.8(6) . . ? C36 C35 C34 119.6(6) . . ? C35 C36 C31 120.2(5) . . ? C35 C36 N4 120.8(5) . . ? C31 C36 N4 118.9(5) . . ? #===END # Attachment 'sep1700.cif' data_sep1700 _database_code_depnum_ccdc_archive 'CCDC 674812' _audit_creation_date 2000-09-13T16:25:32-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H72 N2 P6 Si4 Sn' _chemical_formula_sum 'C32 H72 N2 P6 Si4 Sn' _chemical_formula_weight 901.79 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9453(17) _cell_length_b 13.7446(14) _cell_length_c 15.126(2) _cell_angle_alpha 114.191(7) _cell_angle_beta 93.524(5) _cell_angle_gamma 94.335(9) _cell_volume 2247.2(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18767 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description 'very fine needle' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.333 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 948 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.913 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.982 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 13494 _diffrn_reflns_av_R_equivalents 0.0956 _diffrn_reflns_av_unetI/netI 0.1342 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.76 _diffrn_reflns_theta_max 23.02 _diffrn_reflns_theta_full 23.02 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 6186 _reflns_number_gt 4261 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0369P)^2^+0.9339P] 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_number_reflns 6186 _refine_ls_number_parameters 419 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0607 _refine_ls_wR_factor_ref 0.1356 _refine_ls_wR_factor_gt 0.1202 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.657 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.114 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' P P 0.1023 0.0942 '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' 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 Sn Sn 0.71186(5) 0.78224(4) 0.71910(4) 0.02472(18) Uani 1 1 d . . . P1 P 0.66272(18) 0.53905(15) 0.88417(14) 0.0254(5) Uani 1 1 d . . . P2 P 0.82338(18) 0.57008(16) 0.73552(14) 0.0261(5) Uani 1 1 d . . . P3 P 0.64921(18) 0.59523(15) 0.70765(14) 0.0255(5) Uani 1 1 d . . . P4 P 0.88482(19) 0.62001(16) 0.92623(14) 0.0276(5) Uani 1 1 d . . . P5 P 0.67868(19) 0.75525(15) 0.93855(14) 0.0263(5) Uani 1 1 d . . . P6 P 0.82202(19) 0.81698(15) 0.88664(14) 0.0273(5) Uani 1 1 d . . . Si1 Si 0.8516(2) 0.68176(18) 0.51540(15) 0.0313(6) Uani 1 1 d . . . Si2 Si 0.8772(2) 0.92062(18) 0.64027(17) 0.0375(6) Uani 1 1 d . . . Si3 Si 0.5499(2) 0.98578(17) 0.80190(16) 0.0326(6) Uani 1 1 d . . . Si4 Si 0.4857(2) 0.81481(19) 0.59874(17) 0.0378(6) Uani 1 1 d . . . N1 N 0.8198(6) 0.7904(4) 0.6193(4) 0.0260(16) Uani 1 1 d . . . N2 N 0.5787(6) 0.8667(5) 0.7063(4) 0.0302(16) Uani 1 1 d . A . C1 C 0.7949(7) 0.5069(6) 0.8215(5) 0.0266(19) Uani 1 1 d . . . C2 C 0.6028(6) 0.6302(6) 0.8322(5) 0.0245(18) Uani 1 1 d . . . C3 C 0.7510(7) 0.6638(6) 0.9811(5) 0.0278(19) Uani 1 1 d . . . C4 C 0.8990(7) 0.6941(6) 0.8458(5) 0.0266(19) Uani 1 1 d . . . C5 C 0.8127(7) 0.3864(6) 0.7861(5) 0.029(2) Uani 1 1 d . . . C6 C 0.7175(7) 0.3186(6) 0.7073(5) 0.036(2) Uani 1 1 d . . . H6A H 0.7173 0.3403 0.6532 0.054 Uiso 1 1 calc R . . H6B H 0.6449 0.3293 0.7348 0.054 Uiso 1 1 calc R . . H6C H 0.7293 0.2426 0.6835 0.054 Uiso 1 1 calc R . . C7 C 0.8152(8) 0.3542(6) 0.8713(6) 0.038(2) Uani 1 1 d . . . H7A H 0.8265 0.2781 0.848 0.058 Uiso 1 1 calc R . . H7B H 0.7435 0.366 0.9002 0.058 Uiso 1 1 calc R . . H7C H 0.8772 0.3977 0.9205 0.058 Uiso 1 1 calc R . . C8 C 0.9252(7) 0.3633(6) 0.7420(6) 0.042(2) Uani 1 1 d . . . H8A H 0.9263 0.3824 0.6863 0.062 Uiso 1 1 calc R . . H8B H 0.9337 0.2868 0.7202 0.062 Uiso 1 1 calc R . . H8C H 0.9875 0.4059 0.7912 0.062 Uiso 1 1 calc R . . C9 C 0.4698(7) 0.6259(6) 0.8323(5) 0.030(2) Uani 1 1 d . . . C10 C 0.4311(7) 0.6412(6) 0.9311(5) 0.032(2) Uani 1 1 d . . . H10A H 0.4665 0.7101 0.9812 0.048 Uiso 1 1 calc R . . H10B H 0.4532 0.5828 0.9474 0.048 Uiso 1 1 calc R . . H10C H 0.3488 0.6405 0.9282 0.048 Uiso 1 1 calc R . . C11 C 0.4135(7) 0.5183(6) 0.7570(6) 0.038(2) Uani 1 1 d . . . H11A H 0.4383 0.4607 0.7732 0.056 Uiso 1 1 calc R . . H11B H 0.4345 0.5078 0.6924 0.056 Uiso 1 1 calc R . . H11C H 0.3313 0.5172 0.7571 0.056 Uiso 1 1 calc R . . C12 C 0.4322(7) 0.7168(7) 0.8090(6) 0.044(2) Uani 1 1 d . . . H12A H 0.4691 0.7855 0.8582 0.066 Uiso 1 1 calc R . . H12B H 0.3501 0.7162 0.8093 0.066 Uiso 1 1 calc R . . H12C H 0.4532 0.7072 0.7446 0.066 Uiso 1 1 calc R . . C13 C 0.7557(7) 0.6892(6) 1.0914(5) 0.029(2) Uani 1 1 d . . . C14 C 0.7953(8) 0.5939(6) 1.1079(6) 0.040(2) Uani 1 1 d . . . H14A H 0.7985 0.6098 1.1774 0.06 Uiso 1 1 calc R . . H14B H 0.8705 0.5812 1.0859 0.06 Uiso 1 1 calc R . . H14C H 0.7422 0.5297 1.0709 0.06 Uiso 1 1 calc R . . C15 C 0.8418(8) 0.7902(6) 1.1464(6) 0.043(2) Uani 1 1 d . . . H15A H 0.8467 0.8084 1.2165 0.065 Uiso 1 1 calc R . . H15B H 0.8169 0.8505 1.1345 0.065 Uiso 1 1 calc R . . H15C H 0.9161 0.7755 1.1232 0.065 Uiso 1 1 calc R . . C16 C 0.6416(8) 0.7098(7) 1.1302(6) 0.040(2) Uani 1 1 d . . . H16A H 0.6486 0.7256 1.1997 0.06 Uiso 1 1 calc R . . H16B H 0.5874 0.646 1.0949 0.06 Uiso 1 1 calc R . . H16C H 0.615 0.771 1.1209 0.06 Uiso 1 1 calc R . . C17 C 1.0281(7) 0.7239(6) 0.8403(6) 0.032(2) Uani 1 1 d . . . C18 C 1.0880(7) 0.7922(6) 0.9429(6) 0.039(2) Uani 1 1 d . . . H18A H 1.0799 0.7524 0.9836 0.059 Uiso 1 1 calc R . . H18B H 1.054 0.8595 0.9722 0.059 Uiso 1 1 calc R . . H18C H 1.1683 0.808 0.9384 0.059 Uiso 1 1 calc R . . C19 C 1.0877(7) 0.6224(7) 0.7954(6) 0.044(2) Uani 1 1 d . . . H19A H 1.0783 0.5799 0.8335 0.065 Uiso 1 1 calc R . . H19B H 1.1682 0.6425 0.7957 0.065 Uiso 1 1 calc R . . H19C H 1.0546 0.5797 0.7282 0.065 Uiso 1 1 calc R . . C20 C 1.0430(7) 0.7895(6) 0.7807(6) 0.037(2) Uani 1 1 d . . . H20A H 1.0053 0.8547 0.8093 0.055 Uiso 1 1 calc R . . H20B H 1.0098 0.7467 0.7136 0.055 Uiso 1 1 calc R . . H20C H 1.1236 0.8092 0.7809 0.055 Uiso 1 1 calc R . . C21 C 0.7604(8) 0.5519(6) 0.4886(6) 0.048(3) Uani 1 1 d . . . H21A H 0.6807 0.563 0.4835 0.071 Uiso 1 1 calc R . . H21B H 0.7758 0.5293 0.5413 0.071 Uiso 1 1 calc R . . H21C H 0.7778 0.4961 0.427 0.071 Uiso 1 1 calc R . . C22 C 0.9979(8) 0.6455(7) 0.5224(6) 0.048(3) Uani 1 1 d . . . H22A H 1.0112 0.6292 0.5792 0.073 Uiso 1 1 calc R . . H22B H 1.0519 0.7059 0.5286 0.073 Uiso 1 1 calc R . . H22C H 1.0076 0.5825 0.4631 0.073 Uiso 1 1 calc R . . C23 C 0.8355(8) 0.7107(7) 0.4051(6) 0.047(3) Uani 1 1 d . . . H23A H 0.7594 0.7301 0.3975 0.071 Uiso 1 1 calc R . . H23B H 0.8475 0.6469 0.3473 0.071 Uiso 1 1 calc R . . H23C H 0.8913 0.7704 0.4127 0.071 Uiso 1 1 calc R . . C24 C 1.0252(8) 0.9253(7) 0.6094(7) 0.052(3) Uani 1 1 d . . . H24A H 1.0282 0.8768 0.541 0.079 Uiso 1 1 calc R . . H24B H 1.073 0.903 0.6511 0.079 Uiso 1 1 calc R . . H24C H 1.0522 0.9987 0.6199 0.079 Uiso 1 1 calc R . . C25 C 0.7942(9) 0.9800(7) 0.5684(7) 0.059(3) Uani 1 1 d . . . H25A H 0.7897 0.9326 0.4989 0.088 Uiso 1 1 calc R . . H25B H 0.8318 1.0506 0.5801 0.088 Uiso 1 1 calc R . . H25C H 0.7179 0.9875 0.589 0.088 Uiso 1 1 calc R . . C26 C 0.8815(8) 1.0152(6) 0.7705(6) 0.043(2) Uani 1 1 d . . . H26A H 0.8052 1.0165 0.7911 0.065 Uiso 1 1 calc R . . H26B H 0.9107 1.0874 0.7788 0.065 Uiso 1 1 calc R . . H26C H 0.931 0.9917 0.8103 0.065 Uiso 1 1 calc R . . C27 C 0.6279(8) 1.0109(6) 0.9199(5) 0.042(2) Uani 1 1 d . . . H27A H 0.709 1.0119 0.9133 0.063 Uiso 1 1 calc R . . H27B H 0.6034 0.9539 0.9398 0.063 Uiso 1 1 calc R . . H27C H 0.6125 1.0803 0.9693 0.063 Uiso 1 1 calc R . . C28 C 0.5877(8) 1.1056(6) 0.7764(6) 0.051(3) Uani 1 1 d . . . H28A H 0.5473 1.0957 0.7144 0.076 Uiso 1 1 calc R . . H28B H 0.6692 1.1141 0.7725 0.076 Uiso 1 1 calc R . . H28C H 0.5664 1.1699 0.8289 0.076 Uiso 1 1 calc R . . C29 C 0.3975(7) 0.9866(6) 0.8236(6) 0.039(2) Uani 1 1 d . . . H29A H 0.3515 0.9736 0.763 0.058 Uiso 1 1 calc R . . H29B H 0.3855 1.0565 0.874 0.058 Uiso 1 1 calc R . . H29C H 0.3756 0.9301 0.8449 0.058 Uiso 1 1 calc R . . C30 C 0.4486(14) 0.9254(11) 0.5647(10) 0.078(5) Uani 0.777(13) 1 d P A 1 H30A H 0.4173 0.9803 0.6194 0.118 Uiso 0.777(13) 1 calc PR A 1 H30B H 0.3924 0.8965 0.5077 0.118 Uiso 0.777(13) 1 calc PR A 1 H30C H 0.5165 0.9575 0.5494 0.118 Uiso 0.777(13) 1 calc PR A 1 C31 C 0.3425(10) 0.7520(11) 0.6079(9) 0.063(5) Uani 0.777(13) 1 d P A 1 H31A H 0.3068 0.8042 0.6611 0.095 Uiso 0.777(13) 1 calc PR A 1 H31B H 0.352 0.6886 0.6208 0.095 Uiso 0.777(13) 1 calc PR A 1 H31C H 0.2948 0.7306 0.5464 0.095 Uiso 0.777(13) 1 calc PR A 1 C32 C 0.5410(14) 0.7096(14) 0.5004(9) 0.106(8) Uani 0.777(13) 1 d P A 1 H32A H 0.5602 0.6535 0.521 0.158 Uiso 0.777(13) 1 calc PR A 1 H32B H 0.6089 0.7392 0.4827 0.158 Uiso 0.777(13) 1 calc PR A 1 H32C H 0.4841 0.6789 0.4439 0.158 Uiso 0.777(13) 1 calc PR A 1 C30A C 0.370(5) 0.884(4) 0.587(4) 0.072(16) Uiso 0.223(13) 1 d P A 2 H30D H 0.3938 0.961 0.6161 0.108 Uiso 0.223(13) 1 calc PR A 2 H30E H 0.3082 0.8676 0.6197 0.108 Uiso 0.223(13) 1 calc PR A 2 H30F H 0.3453 0.8602 0.5175 0.108 Uiso 0.223(13) 1 calc PR A 2 C31A C 0.446(4) 0.668(3) 0.550(3) 0.050(13) Uiso 0.223(13) 1 d P A 2 H31D H 0.5123 0.6325 0.5551 0.076 Uiso 0.223(13) 1 calc PR A 2 H31E H 0.4151 0.6409 0.4817 0.076 Uiso 0.223(13) 1 calc PR A 2 H31F H 0.3883 0.6531 0.5879 0.076 Uiso 0.223(13) 1 calc PR A 2 C32A C 0.567(3) 0.809(3) 0.486(3) 0.038(11) Uiso 0.223(13) 1 d P A 2 H32D H 0.636 0.7743 0.4852 0.057 Uiso 0.223(13) 1 calc PR A 2 H32E H 0.5878 0.8826 0.4926 0.057 Uiso 0.223(13) 1 calc PR A 2 H32F H 0.5186 0.7688 0.4254 0.057 Uiso 0.223(13) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn 0.0264(4) 0.0273(3) 0.0215(3) 0.0115(2) 0.0011(2) 0.0021(2) P1 0.0258(13) 0.0271(11) 0.0256(12) 0.0139(9) 0.0001(10) 0.0004(10) P2 0.0244(13) 0.0316(12) 0.0234(11) 0.0125(9) 0.0010(10) 0.0035(10) P3 0.0258(13) 0.0281(11) 0.0233(11) 0.0119(9) -0.0003(10) 0.0017(10) P4 0.0258(13) 0.0345(12) 0.0250(12) 0.0154(9) 0.0000(10) 0.0013(10) P5 0.0290(14) 0.0284(11) 0.0219(11) 0.0112(9) 0.0008(10) 0.0018(10) P6 0.0309(14) 0.0259(11) 0.0239(12) 0.0103(9) 0.0002(10) -0.0017(10) Si1 0.0332(15) 0.0373(13) 0.0217(12) 0.0100(10) 0.0050(11) 0.0049(11) Si2 0.0457(18) 0.0356(14) 0.0382(15) 0.0208(11) 0.0137(13) 0.0063(12) Si3 0.0364(16) 0.0266(12) 0.0351(14) 0.0120(10) 0.0066(12) 0.0064(11) Si4 0.0354(16) 0.0437(15) 0.0354(14) 0.0194(11) -0.0071(12) 0.0030(12) N1 0.036(4) 0.021(3) 0.025(4) 0.013(3) 0.007(3) 0.003(3) N2 0.032(4) 0.032(4) 0.026(4) 0.012(3) -0.002(3) 0.007(3) C1 0.021(5) 0.034(5) 0.026(4) 0.014(4) -0.001(4) 0.001(4) C2 0.021(5) 0.030(4) 0.026(4) 0.015(4) 0.002(4) -0.001(4) C3 0.028(5) 0.037(5) 0.023(4) 0.018(4) -0.001(4) -0.001(4) C4 0.021(5) 0.037(5) 0.022(4) 0.013(4) 0.002(4) 0.001(4) C5 0.027(5) 0.031(5) 0.031(5) 0.013(4) -0.001(4) 0.007(4) C6 0.050(6) 0.022(4) 0.035(5) 0.013(4) -0.004(5) 0.006(4) C7 0.047(6) 0.038(5) 0.037(5) 0.020(4) 0.013(5) 0.018(5) C8 0.039(6) 0.040(5) 0.047(6) 0.018(4) 0.009(5) 0.005(4) C9 0.028(5) 0.039(5) 0.028(5) 0.021(4) 0.000(4) 0.004(4) C10 0.028(5) 0.041(5) 0.028(5) 0.016(4) 0.005(4) -0.007(4) C11 0.032(6) 0.043(5) 0.036(5) 0.016(4) -0.001(4) 0.001(4) C12 0.023(5) 0.056(6) 0.065(6) 0.039(5) 0.004(5) 0.003(4) C13 0.035(6) 0.036(5) 0.019(4) 0.013(3) 0.002(4) 0.002(4) C14 0.040(6) 0.058(6) 0.031(5) 0.030(4) -0.002(4) 0.004(5) C15 0.051(7) 0.043(5) 0.023(5) 0.004(4) -0.007(4) -0.011(5) C16 0.043(6) 0.052(6) 0.026(5) 0.017(4) 0.015(4) 0.002(5) C17 0.019(5) 0.051(5) 0.035(5) 0.027(4) -0.001(4) 0.003(4) C18 0.024(5) 0.050(5) 0.037(5) 0.015(4) -0.008(4) -0.009(4) C19 0.021(5) 0.061(6) 0.056(6) 0.031(5) 0.004(5) 0.005(5) C20 0.026(5) 0.051(5) 0.039(5) 0.024(4) 0.009(4) 0.006(4) C21 0.057(7) 0.045(5) 0.027(5) 0.005(4) -0.006(5) -0.008(5) C22 0.041(6) 0.063(6) 0.046(6) 0.023(5) 0.010(5) 0.022(5) C23 0.054(7) 0.061(6) 0.030(5) 0.020(4) 0.011(5) 0.015(5) C24 0.047(7) 0.048(6) 0.063(7) 0.025(5) 0.013(5) -0.009(5) C25 0.074(8) 0.051(6) 0.062(7) 0.034(5) 0.013(6) 0.005(6) C26 0.037(6) 0.034(5) 0.059(6) 0.019(4) 0.011(5) 0.000(4) C27 0.043(6) 0.036(5) 0.035(5) 0.002(4) 0.006(5) 0.011(4) C28 0.056(7) 0.035(5) 0.056(6) 0.015(4) 0.006(5) 0.004(5) C29 0.040(6) 0.033(5) 0.039(5) 0.011(4) 0.007(5) 0.008(4) C30 0.091(14) 0.098(12) 0.067(10) 0.062(9) -0.020(9) -0.004(10) C31 0.039(9) 0.108(12) 0.054(9) 0.053(8) -0.018(7) -0.023(8) C32 0.072(13) 0.153(17) 0.041(9) -0.014(10) -0.019(9) 0.057(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Sn N1 2.077(6) . ? Sn N2 2.083(6) . ? Sn P3 2.554(2) . ? Sn P6 2.624(2) . ? P1 C1 1.879(8) . ? P1 C2 1.891(7) . ? P1 C3 1.918(8) . ? P2 C1 1.869(7) . ? P2 C4 1.938(8) . ? P2 P3 2.179(3) . ? P3 C2 1.874(7) . ? P4 C3 1.872(8) . ? P4 C4 1.886(7) . ? P4 C1 1.898(8) . ? P5 C3 1.872(7) . ? P5 C2 1.919(7) . ? P5 P6 2.182(3) . ? P6 C4 1.879(7) . ? Si1 N1 1.755(6) . ? Si1 C22 1.861(9) . ? Si1 C23 1.870(8) . ? Si1 C21 1.896(9) . ? Si2 N1 1.760(6) . ? Si2 C26 1.858(8) . ? Si2 C24 1.859(9) . ? Si2 C25 1.883(9) . ? Si3 N2 1.759(6) . ? Si3 C27 1.848(8) . ? Si3 C28 1.870(8) . ? Si3 C29 1.870(9) . ? Si4 N2 1.760(6) . ? Si4 C30A 1.77(5) . ? Si4 C32 1.801(13) . ? Si4 C31A 1.85(4) . ? Si4 C30 1.867(12) . ? Si4 C31 1.895(12) . ? Si4 C32A 1.99(4) . ? C1 C5 1.554(10) . ? C2 C9 1.586(11) . ? C3 C13 1.554(10) . ? C4 C17 1.583(11) . ? C5 C7 1.525(10) . ? C5 C6 1.532(11) . ? C5 C8 1.535(11) . ? C9 C12 1.520(10) . ? C9 C11 1.520(10) . ? C9 C10 1.528(10) . ? C13 C16 1.518(11) . ? C13 C14 1.533(10) . ? C13 C15 1.552(11) . ? C17 C20 1.521(10) . ? C17 C19 1.533(10) . ? C17 C18 1.540(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Sn N2 105.2(2) . . ? N1 Sn P3 116.57(16) . . ? N2 Sn P3 113.83(19) . . ? N1 Sn P6 111.92(18) . . ? N2 Sn P6 123.18(17) . . ? P3 Sn P6 86.02(6) . . ? C1 P1 C2 101.9(3) . . ? C1 P1 C3 86.8(3) . . ? C2 P1 C3 87.7(3) . . ? C1 P2 C4 87.9(3) . . ? C1 P2 P3 96.3(3) . . ? C4 P2 P3 110.1(2) . . ? C2 P3 P2 99.3(2) . . ? C2 P3 Sn 100.5(2) . . ? P2 P3 Sn 91.07(9) . . ? C3 P4 C4 101.9(3) . . ? C3 P4 C1 87.6(3) . . ? C4 P4 C1 88.6(3) . . ? C3 P5 C2 88.2(3) . . ? C3 P5 P6 99.0(3) . . ? C2 P5 P6 108.6(2) . . ? C4 P6 P5 97.9(3) . . ? C4 P6 Sn 98.8(2) . . ? P5 P6 Sn 94.09(10) . . ? N1 Si1 C22 114.7(4) . . ? N1 Si1 C23 111.0(3) . . ? C22 Si1 C23 105.8(4) . . ? N1 Si1 C21 113.5(4) . . ? C22 Si1 C21 103.4(4) . . ? C23 Si1 C21 107.9(4) . . ? N1 Si2 C26 111.8(3) . . ? N1 Si2 C24 112.6(4) . . ? C26 Si2 C24 105.7(4) . . ? N1 Si2 C25 112.8(4) . . ? C26 Si2 C25 106.5(4) . . ? C24 Si2 C25 107.0(4) . . ? N2 Si3 C27 113.1(3) . . ? N2 Si3 C28 111.5(4) . . ? C27 Si3 C28 106.9(4) . . ? N2 Si3 C29 113.0(4) . . ? C27 Si3 C29 105.7(4) . . ? C28 Si3 C29 106.2(4) . . ? N2 Si4 C30A 120.6(16) . . ? N2 Si4 C32 112.2(5) . . ? C30A Si4 C32 125.6(17) . . ? N2 Si4 C31A 113.7(13) . . ? C30A Si4 C31A 112(2) . . ? N2 Si4 C30 110.2(5) . . ? C32 Si4 C30 111.8(8) . . ? C31A Si4 C30 136.1(13) . . ? N2 Si4 C31 115.4(4) . . ? C32 Si4 C31 104.2(8) . . ? C30 Si4 C31 102.7(7) . . ? N2 Si4 C32A 110.3(12) . . ? C30A Si4 C32A 101(2) . . ? C31A Si4 C32A 95.5(18) . . ? Si1 N1 Si2 118.6(3) . . ? Si1 N1 Sn 126.1(3) . . ? Si2 N1 Sn 115.2(3) . . ? Si3 N2 Si4 117.7(4) . . ? Si3 N2 Sn 122.6(3) . . ? Si4 N2 Sn 119.6(3) . . ? C5 C1 P2 116.7(5) . . ? C5 C1 P1 112.2(5) . . ? P2 C1 P1 116.1(4) . . ? C5 C1 P4 124.1(5) . . ? P2 C1 P4 92.2(3) . . ? P1 C1 P4 92.5(3) . . ? C9 C2 P3 112.5(5) . . ? C9 C2 P1 111.8(5) . . ? P3 C2 P1 109.1(4) . . ? C9 C2 P5 111.9(5) . . ? P3 C2 P5 118.2(4) . . ? P1 C2 P5 91.4(3) . . ? C13 C3 P5 117.5(5) . . ? C13 C3 P4 113.9(5) . . ? P5 C3 P4 115.4(4) . . ? C13 C3 P1 121.9(5) . . ? P5 C3 P1 92.0(3) . . ? P4 C3 P1 92.1(3) . . ? C17 C4 P6 110.8(5) . . ? C17 C4 P4 109.9(5) . . ? P6 C4 P4 112.8(4) . . ? C17 C4 P2 116.1(5) . . ? P6 C4 P2 115.3(4) . . ? P4 C4 P2 90.5(3) . . ? C7 C5 C6 110.6(7) . . ? C7 C5 C8 107.2(6) . . ? C6 C5 C8 108.0(6) . . ? C7 C5 C1 110.3(6) . . ? C6 C5 C1 109.1(6) . . ? C8 C5 C1 111.5(7) . . ? C12 C9 C11 110.5(6) . . ? C12 C9 C10 107.8(6) . . ? C11 C9 C10 107.8(7) . . ? C12 C9 C2 108.0(6) . . ? C11 C9 C2 110.3(6) . . ? C10 C9 C2 112.5(6) . . ? C16 C13 C14 108.1(7) . . ? C16 C13 C15 109.8(7) . . ? C14 C13 C15 109.8(7) . . ? C16 C13 C3 112.3(7) . . ? C14 C13 C3 109.3(6) . . ? C15 C13 C3 107.5(6) . . ? C20 C17 C19 109.2(7) . . ? C20 C17 C18 107.2(7) . . ? C19 C17 C18 107.7(6) . . ? C20 C17 C4 111.4(6) . . ? C19 C17 C4 110.7(7) . . ? C18 C17 C4 110.5(6) . . ? #===END