Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 loop_ _publ_author_name 'Michael F. Lappert' 'James D. Farwell' 'Manuel A. Fernandes' 'Peter B. Hitchcock' 'Marcus Layh' ; B.Omondi ; _publ_contact_author_name 'Prof Michael F. Lappert' _publ_contact_author_address ; Department of Chemistry University of Sussex CPES Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email M.F.LAPPERT@SUSSEX.AC.UK _publ_section_title ; Synthesis, crystal structures and reactions of sila- and germa-b-diketiminate ; data_hgbrke_s _database_code_CSD 199037 _chemical_name_systematic ; Bromo (trimethylsilyl)-bis((trimethylsilyl)imino-(2,6- dimethylphenyl)methyl)silane ; _exptl_crystal_preparation 'grown from hexane at -20 C' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C27 H45 Br N2 Si4' _chemical_formula_sum 'C27 H45 Br N2 Si4' _chemical_formula_weight 589.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5310(15) _cell_length_b 11.3263(16) _cell_length_c 15.066(2) _cell_angle_alpha 73.829(3) _cell_angle_beta 71.999(2) _cell_angle_gamma 86.555(3) _cell_volume 1640.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.194 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 1.416 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5207 _exptl_absorpt_correction_T_max 0.8484 _exptl_absorpt_process_details 'Sheldrick, G. M. (1996). SADABS. University of Gottingen, Germany.' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 deector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10609 _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.48 _diffrn_reflns_theta_max 26.99 _reflns_number_total 7063 _reflns_number_gt 5975 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1419P)^2^+0.7819P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7063 _refine_ls_number_parameters 326 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0750 _refine_ls_wR_factor_ref 0.2008 _refine_ls_wR_factor_gt 0.1933 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.147 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.52612(3) 0.21507(4) 0.13003(3) 0.03826(18) Uani 1 1 d . A . Si1 Si 0.31047(9) 0.18697(8) 0.22531(7) 0.0212(2) Uani 1 1 d D . . Si4 Si 0.35890(11) 0.39094(10) 0.42296(7) 0.0291(3) Uani 1 1 d D A . Si3 Si -0.06932(10) 0.14504(11) 0.17736(8) 0.0322(3) Uani 1 1 d . A . N1 N 0.0817(3) 0.1645(3) 0.1998(2) 0.0242(6) Uani 1 1 d . . . N2 N 0.3405(3) 0.3026(3) 0.3485(2) 0.0255(6) Uani 1 1 d . . . C4 C 0.2024(3) 0.1892(3) 0.1447(2) 0.0210(6) Uani 1 1 d . A . C5 C 0.2475(3) 0.2110(3) 0.0365(3) 0.0226(7) Uani 1 1 d . . . C6 C 0.3001(4) 0.1131(4) -0.0023(3) 0.0299(8) Uani 1 1 d . A . C7 C 0.3364(5) 0.1308(5) -0.1022(3) 0.0434(10) Uani 1 1 d . . . H7 H 0.3711 0.0646 -0.1291 0.052 Uiso 1 1 calc R A . C8 C 0.3222(5) 0.2447(5) -0.1628(3) 0.0475(11) Uani 1 1 d . A . H8 H 0.3476 0.2563 -0.2309 0.057 Uiso 1 1 calc R . . C9 C 0.2714(5) 0.3413(4) -0.1247(3) 0.0396(10) Uani 1 1 d . . . H9 H 0.2621 0.4188 -0.1671 0.048 Uiso 1 1 calc R A . C10 C 0.2333(4) 0.3268(3) -0.0247(3) 0.0286(8) Uani 1 1 d . A . C11 C 0.1805(5) 0.4343(4) 0.0135(3) 0.0421(10) Uani 1 1 d . . . H11A H 0.2181 0.4364 0.0650 0.063 Uiso 1 1 calc R A . H11B H 0.0829 0.4266 0.0397 0.063 Uiso 1 1 calc R . . H11C H 0.2060 0.5105 -0.0392 0.063 Uiso 1 1 calc R . . C12 C 0.3133(5) -0.0119(4) 0.0634(3) 0.0374(9) Uani 1 1 d . . . H12A H 0.2243 -0.0471 0.1030 0.056 Uiso 1 1 calc R A . H12B H 0.3645 -0.0035 0.1058 0.056 Uiso 1 1 calc R . . H12C H 0.3599 -0.0663 0.0239 0.056 Uiso 1 1 calc R . . C13 C 0.2797(3) 0.3205(3) 0.2845(2) 0.0225(7) Uani 1 1 d . A . C14 C 0.1969(4) 0.4302(3) 0.2588(3) 0.0262(7) Uani 1 1 d . . . C15 C 0.2582(5) 0.5369(4) 0.1875(3) 0.0340(9) Uani 1 1 d . A . C16 C 0.1785(6) 0.6366(4) 0.1657(4) 0.0471(12) Uani 1 1 d . . . H16 H 0.2184 0.7097 0.1179 0.056 Uiso 1 1 calc R A . C17 C 0.0427(6) 0.6315(4) 0.2121(4) 0.0535(13) Uani 1 1 d . A . H17 H -0.0102 0.6999 0.1951 0.064 Uiso 1 1 calc R . . C18 C -0.0161(5) 0.5272(4) 0.2830(4) 0.0462(11) Uani 1 1 d . . . H18 H -0.1095 0.5247 0.3152 0.055 Uiso 1 1 calc R A . C19 C 0.0602(4) 0.4243(4) 0.3084(3) 0.0316(8) Uani 1 1 d . A . C20 C -0.0037(4) 0.3126(4) 0.3887(3) 0.0388(9) Uani 1 1 d . . . H20A H 0.0111 0.2401 0.3636 0.058 Uiso 1 1 calc R A . H20B H -0.0999 0.3244 0.4133 0.058 Uiso 1 1 calc R . . H20C H 0.0360 0.3004 0.4413 0.058 Uiso 1 1 calc R . . C21 C 0.4054(5) 0.5438(5) 0.1359(4) 0.0488(12) Uani 1 1 d . . . H21A H 0.4303 0.6258 0.0909 0.073 Uiso 1 1 calc R A . H21B H 0.4276 0.4818 0.0997 0.073 Uiso 1 1 calc R . . H21C H 0.4545 0.5283 0.1835 0.073 Uiso 1 1 calc R . . C22 C 0.2750(9) 0.5406(5) 0.4135(5) 0.077(2) Uani 1 1 d D . . H22A H 0.3109 0.5942 0.3475 0.115 Uiso 1 1 calc R A . H22B H 0.2910 0.5795 0.4597 0.115 Uiso 1 1 calc R . . H22C H 0.1787 0.5271 0.4283 0.115 Uiso 1 1 calc R . . C23 C 0.2915(5) 0.2936(4) 0.5496(3) 0.0443(11) Uani 1 1 d D . . H23A H 0.1959 0.2771 0.5642 0.066 Uiso 1 1 calc R A . H23B H 0.3047 0.3366 0.5943 0.066 Uiso 1 1 calc R . . H23C H 0.3383 0.2157 0.5572 0.066 Uiso 1 1 calc R . . C24 C 0.5421(6) 0.4142(7) 0.3897(5) 0.072(2) Uani 1 1 d D . . H24A H 0.5829 0.3350 0.4094 0.108 Uiso 1 1 calc R A . H24B H 0.5616 0.4708 0.4228 0.108 Uiso 1 1 calc R . . H24C H 0.5787 0.4489 0.3194 0.108 Uiso 1 1 calc R . . C25 C -0.1828(6) 0.2565(7) 0.2313(6) 0.073(2) Uani 1 1 d . . . H25A H -0.2069 0.2277 0.3022 0.109 Uiso 1 1 calc R A . H25B H -0.2639 0.2630 0.2115 0.109 Uiso 1 1 calc R . . H25C H -0.1374 0.3373 0.2086 0.109 Uiso 1 1 calc R . . C26 C -0.1267(7) -0.0146(6) 0.2461(5) 0.0710(19) Uani 1 1 d . . . H26A H -0.0543 -0.0707 0.2296 0.106 Uiso 1 1 calc R A . H26B H -0.2036 -0.0357 0.2293 0.106 Uiso 1 1 calc R . . H26C H -0.1528 -0.0222 0.3158 0.106 Uiso 1 1 calc R . . C27 C -0.0645(5) 0.1684(6) 0.0494(4) 0.0491(12) Uani 1 1 d . . . H27A H -0.0335 0.2527 0.0120 0.074 Uiso 1 1 calc R A . H27B H -0.1542 0.1544 0.0471 0.074 Uiso 1 1 calc R . . H27C H -0.0031 0.1103 0.0216 0.074 Uiso 1 1 calc R . . Si2 Si 0.29163(15) 0.00123(11) 0.34947(9) 0.0443(3) Uani 0.474(16) 1 d PD A 1 C1 C 0.2206(13) 0.0248(8) 0.4722(4) 0.066(3) Uani 0.474(16) 1 d PD A 1 H1A H 0.2111 -0.0545 0.5213 0.099 Uiso 0.474(16) 1 calc PR A 1 H1B H 0.1328 0.0617 0.4781 0.099 Uiso 0.474(16) 1 calc PR A 1 H1C H 0.2804 0.0798 0.4819 0.099 Uiso 0.474(16) 1 calc PR A 1 C2 C 0.4508(8) -0.0779(9) 0.3399(7) 0.066(3) Uani 0.474(16) 1 d PD A 1 H2A H 0.5205 -0.0201 0.3342 0.099 Uiso 0.474(16) 1 calc PR A 1 H2B H 0.4758 -0.1089 0.2824 0.099 Uiso 0.474(16) 1 calc PR A 1 H2C H 0.4411 -0.1468 0.3980 0.099 Uiso 0.474(16) 1 calc PR A 1 C3 C 0.1691(11) -0.1071(7) 0.3397(8) 0.066(3) Uani 0.474(16) 1 d PD A 1 H3A H 0.1945 -0.1142 0.2731 0.099 Uiso 0.474(16) 1 calc PR A 1 H3B H 0.0790 -0.0747 0.3565 0.099 Uiso 0.474(16) 1 calc PR A 1 H3C H 0.1704 -0.1883 0.3845 0.099 Uiso 0.474(16) 1 calc PR A 1 Si2' Si 0.29163(15) 0.00123(11) 0.34947(9) 0.0443(3) Uani 0.526(16) 1 d PD A 2 C1' C 0.1708(10) 0.0194(8) 0.4631(5) 0.064(3) Uani 0.526(16) 1 d PD A 2 H1'A H 0.0819 0.0329 0.4547 0.096 Uiso 0.526(16) 1 calc PR A 2 H1'B H 0.1983 0.0901 0.4790 0.096 Uiso 0.526(16) 1 calc PR A 2 H1'C H 0.1680 -0.0552 0.5158 0.096 Uiso 0.526(16) 1 calc PR A 2 C2' C 0.4615(7) -0.0207(9) 0.3692(7) 0.064(3) Uani 0.526(16) 1 d PD A 2 H2'A H 0.4600 -0.0971 0.4201 0.096 Uiso 0.526(16) 1 calc PR A 2 H2'B H 0.4835 0.0489 0.3890 0.096 Uiso 0.526(16) 1 calc PR A 2 H2'C H 0.5291 -0.0254 0.3087 0.096 Uiso 0.526(16) 1 calc PR A 2 C3' C 0.2507(12) -0.1294(6) 0.3144(7) 0.064(3) Uani 0.526(16) 1 d PD A 2 H3'A H 0.2967 -0.2019 0.3412 0.096 Uiso 0.526(16) 1 calc PR A 2 H3'B H 0.2795 -0.1109 0.2435 0.096 Uiso 0.526(16) 1 calc PR A 2 H3'C H 0.1540 -0.1458 0.3396 0.096 Uiso 0.526(16) 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 Br1 0.0212(2) 0.0606(3) 0.0402(3) -0.0294(2) -0.00627(17) 0.00469(17) Si1 0.0222(5) 0.0243(5) 0.0211(5) -0.0102(4) -0.0097(4) 0.0054(3) Si4 0.0417(6) 0.0290(5) 0.0206(5) -0.0105(4) -0.0118(4) 0.0002(4) Si3 0.0234(5) 0.0442(6) 0.0302(6) -0.0114(5) -0.0075(4) -0.0066(4) N1 0.0253(14) 0.0231(14) 0.0256(15) -0.0072(11) -0.0088(12) -0.0010(11) N2 0.0309(15) 0.0261(15) 0.0204(14) -0.0074(11) -0.0084(12) 0.0012(12) C4 0.0262(16) 0.0155(14) 0.0236(17) -0.0057(12) -0.0104(13) 0.0009(12) C5 0.0216(16) 0.0265(17) 0.0229(17) -0.0075(13) -0.0098(13) -0.0029(12) C6 0.035(2) 0.0308(18) 0.0267(19) -0.0119(15) -0.0101(15) -0.0022(15) C7 0.057(3) 0.048(3) 0.029(2) -0.0210(19) -0.009(2) -0.003(2) C8 0.062(3) 0.058(3) 0.020(2) -0.0070(18) -0.011(2) -0.011(2) C9 0.049(2) 0.045(2) 0.024(2) 0.0003(17) -0.0159(18) -0.0105(19) C10 0.0316(18) 0.0301(18) 0.0238(18) -0.0011(14) -0.0123(15) -0.0062(14) C11 0.058(3) 0.031(2) 0.036(2) -0.0020(17) -0.019(2) 0.0070(19) C12 0.053(3) 0.0264(19) 0.033(2) -0.0144(16) -0.0094(19) 0.0055(17) C13 0.0254(16) 0.0218(16) 0.0187(16) -0.0062(12) -0.0039(13) -0.0007(12) C14 0.0343(19) 0.0242(17) 0.0245(17) -0.0103(13) -0.0125(15) 0.0040(14) C15 0.048(2) 0.0278(18) 0.031(2) -0.0068(15) -0.0183(18) -0.0008(16) C16 0.076(3) 0.026(2) 0.049(3) -0.0076(18) -0.034(3) 0.005(2) C17 0.071(4) 0.037(2) 0.072(4) -0.025(2) -0.043(3) 0.026(2) C18 0.042(2) 0.048(3) 0.061(3) -0.030(2) -0.025(2) 0.024(2) C19 0.0314(19) 0.035(2) 0.034(2) -0.0187(16) -0.0120(16) 0.0090(15) C20 0.031(2) 0.044(2) 0.038(2) -0.0139(18) -0.0031(17) 0.0023(17) C21 0.056(3) 0.041(2) 0.040(2) 0.0049(19) -0.012(2) -0.012(2) C22 0.154(7) 0.043(3) 0.072(4) -0.040(3) -0.075(5) 0.036(4) C23 0.063(3) 0.045(2) 0.026(2) -0.0103(18) -0.015(2) 0.005(2) C24 0.048(3) 0.120(6) 0.064(4) -0.059(4) -0.006(3) -0.019(3) C25 0.037(3) 0.114(5) 0.100(5) -0.072(4) -0.033(3) 0.026(3) C26 0.082(4) 0.068(4) 0.058(4) 0.005(3) -0.025(3) -0.046(3) C27 0.036(2) 0.081(4) 0.038(2) -0.016(2) -0.019(2) -0.008(2) Si2 0.0666(9) 0.0401(6) 0.0249(6) -0.0081(5) -0.0178(6) 0.0286(6) C1 0.096(7) 0.038(4) 0.042(4) 0.004(3) -0.004(4) 0.000(4) C2 0.096(7) 0.038(4) 0.042(4) 0.004(3) -0.004(4) 0.000(4) C3 0.096(7) 0.038(4) 0.042(4) 0.004(3) -0.004(4) 0.000(4) Si2' 0.0666(9) 0.0401(6) 0.0249(6) -0.0081(5) -0.0178(6) 0.0286(6) C1' 0.086(6) 0.046(4) 0.045(4) -0.002(3) -0.009(3) 0.012(3) C2' 0.086(6) 0.046(4) 0.045(4) -0.002(3) -0.009(3) 0.012(3) C3' 0.086(6) 0.046(4) 0.045(4) -0.002(3) -0.009(3) 0.012(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Si1 2.2664(10) . ? Si1 C4 1.899(3) . ? Si1 C13 1.924(4) . ? Si1 Si2 2.3650(15) . ? Si4 N2 1.755(3) . ? Si4 C24 1.853(6) . ? Si4 C22 1.854(5) . ? Si4 C23 1.856(4) . ? Si3 N1 1.763(3) . ? Si3 C26 1.846(6) . ? Si3 C27 1.856(5) . ? Si3 C25 1.863(6) . ? N1 C4 1.282(5) . ? N2 C13 1.280(5) . ? C4 C5 1.502(5) . ? C5 C6 1.403(5) . ? C5 C10 1.407(5) . ? C6 C7 1.392(6) . ? C6 C12 1.512(6) . ? C7 C8 1.388(7) . ? C7 H7 0.9500 . ? C8 C9 1.379(7) . ? C8 H8 0.9500 . ? C9 C10 1.399(6) . ? C9 H9 0.9500 . ? C10 C11 1.495(6) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.505(5) . ? C14 C19 1.398(6) . ? C14 C15 1.405(5) . ? C15 C16 1.392(6) . ? C15 C21 1.500(7) . ? C16 C17 1.381(8) . ? C16 H16 0.9500 . ? C17 C18 1.377(8) . ? C17 H17 0.9500 . ? C18 C19 1.407(6) . ? C18 H18 0.9500 . ? C19 C20 1.505(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? Si2 C2 1.838(5) . ? Si2 C1 1.856(5) . ? Si2 C3 1.897(5) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C1' H1'A 0.9800 . ? C1' H1'B 0.9800 . ? C1' H1'C 0.9800 . ? C2' H2'A 0.9800 . ? C2' H2'B 0.9800 . ? C2' H2'C 0.9800 . ? C3' H3'A 0.9800 . ? C3' H3'B 0.9800 . ? C3' H3'C 0.9800 . ? 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 C4 Si1 C13 113.86(15) . . ? C4 Si1 Br1 107.82(11) . . ? C13 Si1 Br1 104.47(11) . . ? C4 Si1 Si2 113.83(11) . . ? C13 Si1 Si2 107.96(11) . . ? Br1 Si1 Si2 108.36(5) . . ? N2 Si4 C24 103.8(2) . . ? N2 Si4 C22 117.5(2) . . ? C24 Si4 C22 110.5(4) . . ? N2 Si4 C23 106.04(19) . . ? C24 Si4 C23 110.7(3) . . ? C22 Si4 C23 108.2(3) . . ? N1 Si3 C26 105.2(2) . . ? N1 Si3 C27 117.73(19) . . ? C26 Si3 C27 108.6(3) . . ? N1 Si3 C25 104.1(2) . . ? C26 Si3 C25 110.7(4) . . ? C27 Si3 C25 110.4(3) . . ? C4 N1 Si3 133.1(3) . . ? C13 N2 Si4 132.8(3) . . ? N1 C4 C5 125.1(3) . . ? N1 C4 Si1 107.5(3) . . ? C5 C4 Si1 127.3(2) . . ? C6 C5 C10 120.6(3) . . ? C6 C5 C4 118.9(3) . . ? C10 C5 C4 120.5(3) . . ? C7 C6 C5 119.4(4) . . ? C7 C6 C12 119.9(4) . . ? C5 C6 C12 120.7(3) . . ? C8 C7 C6 120.2(4) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C9 C8 C7 120.5(4) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C8 C9 C10 120.9(4) . . ? C8 C9 H9 119.6 . . ? C10 C9 H9 119.6 . . ? C9 C10 C5 118.5(4) . . ? C9 C10 C11 119.2(4) . . ? C5 C10 C11 122.3(3) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C6 C12 H12A 109.5 . . ? C6 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C6 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N2 C13 C14 125.0(3) . . ? N2 C13 Si1 110.1(2) . . ? C14 C13 Si1 124.9(3) . . ? C19 C14 C15 121.3(4) . . ? C19 C14 C13 118.9(3) . . ? C15 C14 C13 119.8(3) . . ? C16 C15 C14 118.2(4) . . ? C16 C15 C21 120.6(4) . . ? C14 C15 C21 121.2(4) . . ? C17 C16 C15 121.3(5) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C18 C17 C16 120.1(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C17 C18 C19 120.8(5) . . ? C17 C18 H18 119.6 . . ? C19 C18 H18 119.6 . . ? C14 C19 C18 118.2(4) . . ? C14 C19 C20 121.2(3) . . ? C18 C19 C20 120.5(4) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C15 C21 H21A 109.5 . . ? C15 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C15 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? Si4 C22 H22A 109.5 . . ? Si4 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si4 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si4 C23 H23A 109.5 . . ? Si4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si4 C24 H24A 109.5 . . ? Si4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si3 C25 H25A 109.5 . . ? Si3 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si3 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si3 C26 H26A 109.5 . . ? Si3 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si3 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si3 C27 H27A 109.5 . . ? Si3 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si3 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C2 Si2 C1 110.1(4) . . ? C2 Si2 C3 107.2(4) . . ? C1 Si2 C3 105.6(3) . . ? C2 Si2 Si1 112.7(3) . . ? C1 Si2 Si1 112.0(3) . . ? C3 Si2 Si1 108.9(3) . . ? H1'A C1' H1'B 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? H2'A C2' H2'B 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? H3'A C3' H3'B 109.5 . . ? H3'A C3' H3'C 109.5 . . ? H3'B C3' H3'C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C26 Si3 N1 C4 118.6(4) . . . . ? C27 Si3 N1 C4 -2.5(4) . . . . ? C25 Si3 N1 C4 -125.0(4) . . . . ? C24 Si4 N2 C13 -121.2(4) . . . . ? C22 Si4 N2 C13 1.1(5) . . . . ? C23 Si4 N2 C13 122.2(4) . . . . ? Si3 N1 C4 C5 0.8(5) . . . . ? Si3 N1 C4 Si1 -177.2(2) . . . . ? C13 Si1 C4 N1 -69.1(3) . . . . ? Br1 Si1 C4 N1 175.4(2) . . . . ? Si2 Si1 C4 N1 55.2(3) . . . . ? C13 Si1 C4 C5 112.9(3) . . . . ? Br1 Si1 C4 C5 -2.5(3) . . . . ? Si2 Si1 C4 C5 -122.8(3) . . . . ? N1 C4 C5 C6 -96.4(4) . . . . ? Si1 C4 C5 C6 81.3(4) . . . . ? N1 C4 C5 C10 81.6(4) . . . . ? Si1 C4 C5 C10 -100.8(4) . . . . ? C10 C5 C6 C7 -0.9(6) . . . . ? C4 C5 C6 C7 177.0(4) . . . . ? C10 C5 C6 C12 -179.0(4) . . . . ? C4 C5 C6 C12 -1.0(5) . . . . ? C5 C6 C7 C8 0.7(7) . . . . ? C12 C6 C7 C8 178.8(4) . . . . ? C6 C7 C8 C9 -0.3(8) . . . . ? C7 C8 C9 C10 0.1(7) . . . . ? C8 C9 C10 C5 -0.3(6) . . . . ? C8 C9 C10 C11 179.1(4) . . . . ? C6 C5 C10 C9 0.7(5) . . . . ? C4 C5 C10 C9 -177.2(3) . . . . ? C6 C5 C10 C11 -178.7(4) . . . . ? C4 C5 C10 C11 3.4(5) . . . . ? Si4 N2 C13 C14 -3.1(6) . . . . ? Si4 N2 C13 Si1 176.7(2) . . . . ? C4 Si1 C13 N2 170.2(2) . . . . ? Br1 Si1 C13 N2 -72.4(3) . . . . ? Si2 Si1 C13 N2 42.8(3) . . . . ? C4 Si1 C13 C14 -10.1(3) . . . . ? Br1 Si1 C13 C14 107.3(3) . . . . ? Si2 Si1 C13 C14 -137.5(3) . . . . ? N2 C13 C14 C19 -90.8(5) . . . . ? Si1 C13 C14 C19 89.5(4) . . . . ? N2 C13 C14 C15 87.9(5) . . . . ? Si1 C13 C14 C15 -91.9(4) . . . . ? C19 C14 C15 C16 -1.3(6) . . . . ? C13 C14 C15 C16 -179.9(4) . . . . ? C19 C14 C15 C21 178.7(4) . . . . ? C13 C14 C15 C21 0.1(6) . . . . ? C14 C15 C16 C17 -0.3(7) . . . . ? C21 C15 C16 C17 179.6(5) . . . . ? C15 C16 C17 C18 1.4(8) . . . . ? C16 C17 C18 C19 -0.8(8) . . . . ? C15 C14 C19 C18 1.9(6) . . . . ? C13 C14 C19 C18 -179.5(4) . . . . ? C15 C14 C19 C20 -176.4(4) . . . . ? C13 C14 C19 C20 2.2(6) . . . . ? C17 C18 C19 C14 -0.9(7) . . . . ? C17 C18 C19 C20 177.5(4) . . . . ? C4 Si1 Si2 C2 118.9(5) . . . . ? C13 Si1 Si2 C2 -113.6(5) . . . . ? Br1 Si1 Si2 C2 -1.0(5) . . . . ? C4 Si1 Si2 C1 -116.2(5) . . . . ? C13 Si1 Si2 C1 11.3(5) . . . . ? Br1 Si1 Si2 C1 123.9(4) . . . . ? C4 Si1 Si2 C3 0.2(4) . . . . ? C13 Si1 Si2 C3 127.6(4) . . . . ? Br1 Si1 Si2 C3 -119.8(4) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.436 _refine_diff_density_min -1.415 _refine_diff_density_rms 0.196 data_f:\marcus\pdgeket\work\soln\pdgeket _database_code_CSD 199038 _chemical_name_systematic ; (Trimethylsilyl)-bis[(trimethylsilyl)imino-(phenyl)methyl]digermane ; _exptl_crystal_preparation 'grown from hexane at -60 C' _audit_creation_method SHELXL-97 _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H74 Ge2 N4 Si6' _chemical_formula_sum 'C46 H74 Ge2 N4 Si6' _chemical_formula_weight 996.81 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' 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.2204(13) _cell_length_b 12.0349(15) _cell_length_c 13.3254(17) _cell_angle_alpha 114.225(2) _cell_angle_beta 109.868(2) _cell_angle_gamma 92.296(2) _cell_volume 1374.6(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description 'pearl shape' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.90 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.204 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 526 _exptl_absorpt_coefficient_mu 1.257 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3976 _exptl_absorpt_correction_T_max 0.6892 _exptl_absorpt_process_details ;SADABS: Area-Detector Absorption Correction. (1996) Siemens Industrial Automation, Inc.: Madison, WI.. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8262 _diffrn_reflns_av_R_equivalents 0.0286 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 26.00 _reflns_number_total 5346 _reflns_number_gt 4640 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0771P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5346 _refine_ls_number_parameters 271 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0434 _refine_ls_wR_factor_ref 0.1102 _refine_ls_wR_factor_gt 0.1093 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.46934(3) 0.88880(2) 0.93316(2) 0.01487(10) Uani 1 1 d . . . Si1 Si 0.67948(8) 0.80780(7) 0.92802(6) 0.02143(17) Uani 1 1 d . . . Si2 Si 0.44583(9) 0.77817(8) 1.21394(7) 0.02689(19) Uani 1 1 d . . . Si3 Si 0.03809(8) 0.83714(8) 0.64084(7) 0.02758(19) Uani 1 1 d . . . N1 N 0.4482(2) 0.8456(2) 1.11985(19) 0.0226(5) Uani 1 1 d . . . N2 N 0.1954(2) 0.8650(2) 0.76336(19) 0.0238(5) Uani 1 1 d . . . C1 C 0.8138(3) 0.9304(3) 0.9441(3) 0.0390(8) Uani 1 1 d . . . H1A H 0.8415 1.0007 1.0213 0.059 Uiso 1 1 calc R . . H1B H 0.7732 0.9562 0.8829 0.059 Uiso 1 1 calc R . . H1C H 0.8958 0.8974 0.9365 0.059 Uiso 1 1 calc R . . C2 C 0.7450(3) 0.7698(3) 1.0560(3) 0.0378(8) Uani 1 1 d . . . H2A H 0.8374 0.7504 1.0658 0.057 Uiso 1 1 calc R . . H2B H 0.6803 0.6992 1.0407 0.057 Uiso 1 1 calc R . . H2C H 0.7512 0.8400 1.1276 0.057 Uiso 1 1 calc R . . C3 C 0.6452(3) 0.6624(3) 0.7868(3) 0.0319(7) Uani 1 1 d . . . H3A H 0.7236 0.6212 0.7986 0.048 Uiso 1 1 calc R . . H3B H 0.6351 0.6839 0.7231 0.048 Uiso 1 1 calc R . . H3C H 0.5594 0.6077 0.7666 0.048 Uiso 1 1 calc R . . C4 C 0.3851(3) 0.8063(2) 1.0073(2) 0.0192(5) Uani 1 1 d . . . C5 C 0.2624(3) 0.6970(3) 0.9294(2) 0.0241(6) Uani 1 1 d . . . C6 C 0.1427(3) 0.6924(3) 0.9562(3) 0.0355(7) Uani 1 1 d . . . H6 H 0.1358 0.7604 1.0195 0.043 Uiso 1 1 calc R . . C7 C 0.0341(4) 0.5878(4) 0.8895(4) 0.0491(9) Uani 1 1 d . . . H7 H -0.0444 0.5853 0.9095 0.059 Uiso 1 1 calc R . . C8 C 0.0406(4) 0.4877(4) 0.7940(4) 0.0570(11) Uani 1 1 d . . . H8 H -0.0330 0.4176 0.7496 0.068 Uiso 1 1 calc R . . C9 C 0.1579(4) 0.4918(3) 0.7642(3) 0.0524(10) Uani 1 1 d . . . H9 H 0.1630 0.4241 0.6997 0.063 Uiso 1 1 calc R . . C10 C 0.2679(4) 0.5970(3) 0.8308(3) 0.0377(7) Uani 1 1 d . . . H10 H 0.3449 0.6004 0.8092 0.045 Uiso 1 1 calc R . . C11 C 0.6297(4) 0.8342(4) 1.3307(3) 0.0495(9) Uani 1 1 d . . . H11A H 0.6969 0.8202 1.2932 0.074 Uiso 1 1 calc R . . H11B H 0.6425 0.7896 1.3777 0.074 Uiso 1 1 calc R . . H11C H 0.6448 0.9217 1.3815 0.074 Uiso 1 1 calc R . . C12 C 0.3186(4) 0.8344(4) 1.2852(3) 0.0475(9) Uani 1 1 d . . . H12A H 0.3288 0.9227 1.3125 0.071 Uiso 1 1 calc R . . H12B H 0.3378 0.8162 1.3520 0.071 Uiso 1 1 calc R . . H12C H 0.2233 0.7933 1.2282 0.071 Uiso 1 1 calc R . . C13 C 0.4104(5) 0.6050(3) 1.1374(3) 0.0565(11) Uani 1 1 d . . . H13A H 0.3134 0.5732 1.0809 0.085 Uiso 1 1 calc R . . H13B H 0.4266 0.5739 1.1955 0.085 Uiso 1 1 calc R . . H13C H 0.4728 0.5783 1.0962 0.085 Uiso 1 1 calc R . . C14 C 0.3191(3) 0.8472(2) 0.7715(2) 0.0185(5) Uani 1 1 d . . . C16 C 0.2999(3) 0.6620(3) 0.5835(2) 0.0265(6) Uani 1 1 d . . . H16 H 0.2263 0.6191 0.5883 0.032 Uiso 1 1 calc R . . C17 C 0.3465(3) 0.6033(3) 0.4919(3) 0.0343(7) Uani 1 1 d . . . H17 H 0.3043 0.5209 0.4360 0.041 Uiso 1 1 calc R . . C18 C 0.4543(4) 0.6659(3) 0.4832(3) 0.0361(7) Uani 1 1 d . . . H18 H 0.4854 0.6260 0.4220 0.043 Uiso 1 1 calc R . . C19 C 0.5164(4) 0.7885(3) 0.5660(3) 0.0360(7) Uani 1 1 d . . . H19 H 0.5877 0.8317 0.5590 0.043 Uiso 1 1 calc R . . C20 C 0.4731(3) 0.8476(3) 0.6595(2) 0.0269(6) Uani 1 1 d . . . H20 H 0.5177 0.9292 0.7165 0.032 Uiso 1 1 calc R . . C15 C 0.3631(3) 0.7850(2) 0.6682(2) 0.0205(5) Uani 1 1 d . . . C22 C 0.0601(4) 0.8335(3) 0.5061(3) 0.0407(8) Uani 1 1 d . . . H22A H 0.1256 0.9074 0.5293 0.061 Uiso 1 1 calc R . . H22B H -0.0303 0.8298 0.4494 0.061 Uiso 1 1 calc R . . H22C H 0.0964 0.7615 0.4705 0.061 Uiso 1 1 calc R . . C23 C -0.0507(4) 0.9684(4) 0.6949(3) 0.0498(10) Uani 1 1 d . . . H23A H -0.0662 0.9720 0.7632 0.075 Uiso 1 1 calc R . . H23B H -0.1404 0.9557 0.6324 0.075 Uiso 1 1 calc R . . H23C H 0.0087 1.0453 0.7168 0.075 Uiso 1 1 calc R . . C21 C -0.0732(4) 0.6887(4) 0.6047(4) 0.0519(9) Uani 1 1 d . . . H21A H -0.0301 0.6204 0.5724 0.078 Uiso 1 1 calc R . . H21B H -0.1666 0.6765 0.5470 0.078 Uiso 1 1 calc R . . H21C H -0.0801 0.6927 0.6762 0.078 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 Ge1 0.01856(16) 0.01528(16) 0.01045(15) 0.00506(11) 0.00633(11) 0.00263(10) Si1 0.0221(4) 0.0228(4) 0.0192(4) 0.0074(3) 0.0102(3) 0.0071(3) Si2 0.0366(5) 0.0304(4) 0.0239(4) 0.0181(3) 0.0156(3) 0.0106(3) Si3 0.0218(4) 0.0328(5) 0.0227(4) 0.0108(3) 0.0048(3) 0.0039(3) N1 0.0291(12) 0.0230(12) 0.0184(11) 0.0104(9) 0.0109(9) 0.0060(9) N2 0.0257(12) 0.0239(12) 0.0181(11) 0.0067(10) 0.0082(9) 0.0035(9) C1 0.0279(16) 0.0406(19) 0.0455(19) 0.0143(16) 0.0177(14) 0.0027(13) C2 0.0414(18) 0.0457(19) 0.0268(15) 0.0167(15) 0.0123(14) 0.0200(15) C3 0.0405(17) 0.0286(16) 0.0270(15) 0.0099(13) 0.0158(13) 0.0155(13) C4 0.0225(13) 0.0187(13) 0.0199(13) 0.0094(11) 0.0110(10) 0.0071(10) C5 0.0272(14) 0.0235(14) 0.0216(13) 0.0122(12) 0.0075(11) 0.0012(11) C6 0.0313(16) 0.0365(18) 0.0379(17) 0.0179(15) 0.0118(14) 0.0036(13) C7 0.0301(18) 0.056(2) 0.058(2) 0.029(2) 0.0115(16) -0.0057(16) C8 0.049(2) 0.043(2) 0.056(2) 0.0160(19) 0.0051(19) -0.0213(17) C9 0.067(3) 0.033(2) 0.0364(19) 0.0004(16) 0.0173(18) -0.0102(17) C10 0.0470(19) 0.0291(17) 0.0316(16) 0.0089(14) 0.0166(15) -0.0027(14) C11 0.045(2) 0.080(3) 0.0349(18) 0.0390(19) 0.0129(16) 0.0116(19) C12 0.057(2) 0.069(3) 0.050(2) 0.042(2) 0.0375(19) 0.0302(19) C13 0.094(3) 0.0312(19) 0.049(2) 0.0249(17) 0.025(2) 0.0179(19) C14 0.0258(14) 0.0159(12) 0.0122(11) 0.0051(10) 0.0073(10) 0.0004(10) C16 0.0308(15) 0.0227(14) 0.0205(13) 0.0054(12) 0.0095(11) 0.0023(11) C17 0.0465(19) 0.0265(16) 0.0180(14) 0.0011(12) 0.0105(13) 0.0062(13) C18 0.056(2) 0.0365(18) 0.0201(14) 0.0087(13) 0.0241(14) 0.0144(15) C19 0.050(2) 0.0381(18) 0.0306(16) 0.0163(14) 0.0266(15) 0.0063(14) C20 0.0373(16) 0.0234(15) 0.0193(13) 0.0077(12) 0.0131(12) 0.0032(12) C15 0.0248(13) 0.0241(14) 0.0124(12) 0.0089(11) 0.0061(10) 0.0064(10) C22 0.0379(18) 0.053(2) 0.0253(16) 0.0193(15) 0.0036(13) 0.0075(15) C23 0.0375(19) 0.061(2) 0.0384(19) 0.0154(18) 0.0076(15) 0.0225(17) C21 0.0364(19) 0.053(2) 0.053(2) 0.0245(19) 0.0027(16) -0.0075(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 C4 2.004(3) . ? Ge1 C14 2.014(2) . ? Ge1 Si1 2.4043(8) . ? Ge1 Ge1 2.4340(5) 2_677 ? Si1 C2 1.859(3) . ? Si1 C1 1.867(3) . ? Si1 C3 1.878(3) . ? Si2 N1 1.756(2) . ? Si2 C12 1.853(3) . ? Si2 C11 1.860(4) . ? Si2 C13 1.860(4) . ? Si3 N2 1.757(2) . ? Si3 C23 1.861(3) . ? Si3 C21 1.864(4) . ? Si3 C22 1.867(3) . ? N1 C4 1.275(3) . ? N2 C14 1.266(3) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C5 1.498(4) . ? C5 C10 1.391(4) . ? C5 C6 1.392(4) . ? C6 C7 1.381(5) . ? C6 H6 0.9300 . ? C7 C8 1.371(5) . ? C7 H7 0.9300 . ? C8 C9 1.391(6) . ? C8 H8 0.9300 . ? C9 C10 1.392(5) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.503(3) . ? C16 C17 1.390(4) . ? C16 C15 1.393(4) . ? C16 H16 0.9300 . ? C17 C18 1.375(5) . ? C17 H17 0.9300 . ? C18 C19 1.382(4) . ? C18 H18 0.9300 . ? C19 C20 1.388(4) . ? C19 H19 0.9300 . ? C20 C15 1.392(4) . ? C20 H20 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 Ge1 C14 106.96(11) . . ? C4 Ge1 Si1 105.29(7) . . ? C14 Ge1 Si1 114.64(7) . . ? C4 Ge1 Ge1 106.29(7) . 2_677 ? C14 Ge1 Ge1 112.08(7) . 2_677 ? Si1 Ge1 Ge1 110.91(2) . 2_677 ? C2 Si1 C1 110.96(16) . . ? C2 Si1 C3 108.36(14) . . ? C1 Si1 C3 109.20(15) . . ? C2 Si1 Ge1 106.55(10) . . ? C1 Si1 Ge1 108.50(11) . . ? C3 Si1 Ge1 113.26(10) . . ? N1 Si2 C12 110.93(14) . . ? N1 Si2 C11 104.24(15) . . ? C12 Si2 C11 109.31(17) . . ? N1 Si2 C13 113.17(15) . . ? C12 Si2 C13 111.2(2) . . ? C11 Si2 C13 107.68(19) . . ? N2 Si3 C23 105.82(13) . . ? N2 Si3 C21 106.42(15) . . ? C23 Si3 C21 109.54(19) . . ? N2 Si3 C22 116.26(13) . . ? C23 Si3 C22 106.96(17) . . ? C21 Si3 C22 111.60(17) . . ? C4 N1 Si2 132.0(2) . . ? C14 N2 Si3 132.49(19) . . ? Si1 C1 H1A 109.5 . . ? Si1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Si1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N1 C4 C5 123.4(2) . . ? N1 C4 Ge1 116.5(2) . . ? C5 C4 Ge1 119.81(18) . . ? C10 C5 C6 119.0(3) . . ? C10 C5 C4 120.5(3) . . ? C6 C5 C4 120.5(3) . . ? C7 C6 C5 120.5(3) . . ? C7 C6 H6 119.8 . . ? C5 C6 H6 119.7 . . ? C8 C7 C6 120.7(3) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 119.5(3) . . ? C7 C8 H8 120.2 . . ? C9 C8 H8 120.2 . . ? C8 C9 C10 120.2(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C5 C10 C9 120.0(3) . . ? C5 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? Si2 C11 H11A 109.5 . . ? Si2 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? Si2 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? Si2 C12 H12A 109.5 . . ? Si2 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? Si2 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si2 C13 H13A 109.5 . . ? Si2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N2 C14 C15 125.6(2) . . ? N2 C14 Ge1 119.10(18) . . ? C15 C14 Ge1 114.99(17) . . ? C17 C16 C15 120.1(3) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C18 C17 C16 120.5(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 119.7(3) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C18 C19 C20 120.4(3) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C19 C20 C15 120.1(3) . . ? C19 C20 H20 119.9 . . ? C15 C20 H20 119.9 . . ? C20 C15 C16 119.1(2) . . ? C20 C15 C14 120.3(2) . . ? C16 C15 C14 120.6(2) . . ? Si3 C22 H22A 109.5 . . ? Si3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si3 C23 H23A 109.5 . . ? Si3 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si3 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? Si3 C21 H21A 109.5 . . ? Si3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C4 Ge1 Si1 C2 -29.17(14) . . . . ? C14 Ge1 Si1 C2 -146.44(14) . . . . ? Ge1 Ge1 Si1 C2 85.40(12) 2_677 . . . ? C4 Ge1 Si1 C1 -148.70(14) . . . . ? C14 Ge1 Si1 C1 94.03(14) . . . . ? Ge1 Ge1 Si1 C1 -34.13(12) 2_677 . . . ? C4 Ge1 Si1 C3 89.87(14) . . . . ? C14 Ge1 Si1 C3 -27.39(14) . . . . ? Ge1 Ge1 Si1 C3 -155.56(11) 2_677 . . . ? C12 Si2 N1 C4 -97.1(3) . . . . ? C11 Si2 N1 C4 145.3(3) . . . . ? C13 Si2 N1 C4 28.6(3) . . . . ? C23 Si3 N2 C14 -143.5(3) . . . . ? C21 Si3 N2 C14 100.0(3) . . . . ? C22 Si3 N2 C14 -25.0(3) . . . . ? Si2 N1 C4 C5 14.6(4) . . . . ? Si2 N1 C4 Ge1 -159.87(15) . . . . ? C14 Ge1 C4 N1 -162.98(19) . . . . ? Si1 Ge1 C4 N1 74.7(2) . . . . ? Ge1 Ge1 C4 N1 -43.1(2) 2_677 . . . ? C14 Ge1 C4 C5 22.3(2) . . . . ? Si1 Ge1 C4 C5 -100.05(19) . . . . ? Ge1 Ge1 C4 C5 142.21(18) 2_677 . . . ? N1 C4 C5 C10 -124.5(3) . . . . ? Ge1 C4 C5 C10 49.8(3) . . . . ? N1 C4 C5 C6 53.9(4) . . . . ? Ge1 C4 C5 C6 -131.8(2) . . . . ? C10 C5 C6 C7 3.1(5) . . . . ? C4 C5 C6 C7 -175.3(3) . . . . ? C5 C6 C7 C8 -1.5(6) . . . . ? C6 C7 C8 C9 0.0(6) . . . . ? C7 C8 C9 C10 -0.1(6) . . . . ? C6 C5 C10 C9 -3.3(5) . . . . ? C4 C5 C10 C9 175.2(3) . . . . ? C8 C9 C10 C5 1.8(6) . . . . ? Si3 N2 C14 C15 -4.4(4) . . . . ? Si3 N2 C14 Ge1 -178.07(15) . . . . ? C4 Ge1 C14 N2 50.5(2) . . . . ? Si1 Ge1 C14 N2 166.85(19) . . . . ? Ge1 Ge1 C14 N2 -65.6(2) 2_677 . . . ? C4 Ge1 C14 C15 -123.76(19) . . . . ? Si1 Ge1 C14 C15 -7.4(2) . . . . ? Ge1 Ge1 C14 C15 120.13(17) 2_677 . . . ? C15 C16 C17 C18 -0.5(5) . . . . ? C16 C17 C18 C19 -0.3(5) . . . . ? C17 C18 C19 C20 1.7(5) . . . . ? C18 C19 C20 C15 -2.2(5) . . . . ? C19 C20 C15 C16 1.4(4) . . . . ? C19 C20 C15 C14 178.0(3) . . . . ? C17 C16 C15 C20 0.0(4) . . . . ? C17 C16 C15 C14 -176.6(3) . . . . ? N2 C14 C15 C20 122.6(3) . . . . ? Ge1 C14 C15 C20 -63.6(3) . . . . ? N2 C14 C15 C16 -60.9(4) . . . . ? Ge1 C14 C15 C16 113.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.841 _refine_diff_density_min -1.463 _refine_diff_density_rms 0.106 data_mfl(1b)-jan198 _database_code_CSD 199536 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common "'(Li(NCR)(Si(SiMe3)(CRNSiMe3)2)) pentane solvate (R=C6H3Me2) '" _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38.50 H58 Li N3 Si4' _chemical_formula_weight 682.18 _chemical_melting_point ? _chemical_compound_source ? _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.324(3) _cell_length_b 12.837(4) _cell_length_c 15.253(4) _cell_angle_alpha 80.74(3) _cell_angle_beta 81.55(2) _cell_angle_gamma 67.29(2) _cell_volume 2187.4(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.036 _exptl_crystal_density_method ? _exptl_crystal_F_000 738 _exptl_absorpt_coefficient_mu 0.163 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 7672 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 24.97 _reflns_number_total 7672 _reflns_number_observed 5897 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material SHELXL-93 _refine_special_details ; There is a molecule of pentane solvate disordered across an inversion centre for which the H atoms were omitted. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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^)+(0.0582P)^2^+1.0339P] 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 'riding ; but omitted for solvate' _refine_ls_extinction_method none _refine_ls_number_reflns 7672 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0672 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1317 _refine_ls_wR_factor_gt 0.1193 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.373 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.046 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 '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 Li Li 0.1730(3) 0.3424(3) 0.3221(3) 0.0371(9) Uani 1 1 d . . . Si1 Si 0.14506(6) 0.10793(6) 0.40777(5) 0.03859(18) Uani 1 1 d . . . Si2 Si 0.24995(6) 0.51078(6) 0.41004(5) 0.0446(2) Uani 1 1 d . . . Si3 Si 0.40489(5) 0.23484(5) 0.22481(4) 0.02622(15) Uani 1 1 d . . . Si4 Si 0.59834(6) 0.13980(6) 0.16598(4) 0.03588(18) Uani 1 1 d . . . N1 N 0.23184(16) 0.17661(15) 0.34338(12) 0.0299(4) Uani 1 1 d . . . N2 N 0.29009(16) 0.40090(16) 0.34326(13) 0.0314(4) Uani 1 1 d . . . N3 N 0.04254(19) 0.42952(18) 0.24452(16) 0.0462(5) Uani 1 1 d . . . C1 C 0.32633(19) 0.14149(18) 0.28728(14) 0.0260(5) Uani 1 1 d . . . C2 C 0.38706(19) 0.34924(17) 0.29495(14) 0.0258(5) Uani 1 1 d . . . C3 C 0.1653(3) 0.1084(3) 0.52640(19) 0.0676(9) Uani 1 1 d . . . H3A H 0.2461 0.0584 0.5387 0.101 Uiso 1 1 calc R . . H3B H 0.109 0.0811 0.5657 0.101 Uiso 1 1 calc R . . H3C H 0.1515 0.1859 0.5372 0.101 Uiso 1 1 calc R . . C4 C 0.1708(3) -0.0401(3) 0.3912(2) 0.0660(9) Uani 1 1 d . . . H4A H 0.1616 -0.043 0.329 0.099 Uiso 1 1 calc R . . H4B H 0.1134 -0.0655 0.4307 0.099 Uiso 1 1 calc R . . H4C H 0.251 -0.0899 0.405 0.099 Uiso 1 1 calc R . . C5 C -0.0098(3) 0.1987(3) 0.3867(3) 0.0744(11) Uani 1 1 d . . . H5A H -0.025 0.2773 0.3952 0.112 Uiso 1 1 calc R . . H5B H -0.0639 0.171 0.4284 0.112 Uiso 1 1 calc R . . H5C H -0.0224 0.1956 0.3253 0.112 Uiso 1 1 calc R . . C6 C 0.2275(4) 0.4481(4) 0.5267(2) 0.0981(15) Uani 1 1 d . . . H6A H 0.19 0.5091 0.5652 0.147 Uiso 1 1 calc R . . H6B H 0.3041 0.3975 0.5474 0.147 Uiso 1 1 calc R . . H6C H 0.1767 0.4047 0.529 0.147 Uiso 1 1 calc R . . C7 C 0.1055(4) 0.6134(4) 0.3739(4) 0.133(2) Uani 1 1 d . . . H7A H 0.0768 0.6781 0.4089 0.2 Uiso 1 1 calc R . . H7B H 0.0483 0.5759 0.3832 0.2 Uiso 1 1 calc R . . H7C H 0.1152 0.6404 0.3105 0.2 Uiso 1 1 calc R . . C8 C 0.3497(3) 0.5886(3) 0.4061(2) 0.0660(9) Uani 1 1 d . . . H8A H 0.3134 0.6503 0.444 0.099 Uiso 1 1 calc R . . H8B H 0.3634 0.6203 0.3445 0.099 Uiso 1 1 calc R . . H8C H 0.4252 0.5363 0.4276 0.099 Uiso 1 1 calc R . . C9 C 0.37265(19) 0.02228(18) 0.26252(15) 0.0288(5) Uani 1 1 d . . . C10 C 0.4564(2) -0.06565(19) 0.31266(17) 0.0366(6) Uani 1 1 d . . . C11 C 0.4962(2) -0.1754(2) 0.2887(2) 0.0515(7) Uani 1 1 d . . . H11 H 0.5527 -0.2357 0.3219 0.062 Uiso 1 1 calc R . . C12 C 0.4550(3) -0.1977(2) 0.2180(2) 0.0607(9) Uani 1 1 d . . . H12 H 0.483 -0.2732 0.2029 0.073 Uiso 1 1 calc R . . C13 C 0.3734(3) -0.1115(2) 0.1687(2) 0.0521(7) Uani 1 1 d . . . H13 H 0.3462 -0.128 0.1194 0.062 Uiso 1 1 calc R . . C14 C 0.3302(2) -0.0004(2) 0.19042(16) 0.0384(6) Uani 1 1 d . . . C15 C 0.4981(2) -0.0418(2) 0.39256(18) 0.0467(7) Uani 1 1 d . . . H15A H 0.4361 -0.0316 0.4423 0.07 Uiso 1 1 calc R . . H15B H 0.5158 0.0275 0.3776 0.07 Uiso 1 1 calc R . . H15C H 0.5696 -0.1059 0.4098 0.07 Uiso 1 1 calc R . . C16 C 0.2370(3) 0.0917(2) 0.13870(19) 0.0509(7) Uani 1 1 d . . . H16A H 0.1599 0.1082 0.1734 0.076 Uiso 1 1 calc R . . H16B H 0.2345 0.0664 0.082 0.076 Uiso 1 1 calc R . . H16C H 0.2557 0.1605 0.127 0.076 Uiso 1 1 calc R . . C17 C 0.49318(19) 0.38212(18) 0.28902(14) 0.0275(5) Uani 1 1 d . . . C18 C 0.5738(2) 0.3299(2) 0.35350(15) 0.0329(5) Uani 1 1 d . . . C19 C 0.6730(2) 0.3577(2) 0.34779(18) 0.0443(6) Uani 1 1 d . . . H19 H 0.7281 0.3229 0.3913 0.053 Uiso 1 1 calc R . . C20 C 0.6929(2) 0.4347(3) 0.28039(19) 0.0485(7) Uani 1 1 d . . . H20 H 0.7614 0.4527 0.2773 0.058 Uiso 1 1 calc R . . C21 C 0.6137(2) 0.4859(2) 0.21724(17) 0.0425(6) Uani 1 1 d . . . H21 H 0.6281 0.5391 0.1708 0.051 Uiso 1 1 calc R . . C22 C 0.5126(2) 0.46093(19) 0.22023(15) 0.0339(5) Uani 1 1 d . . . C23 C 0.5543(2) 0.2460(2) 0.42886(17) 0.0423(6) Uani 1 1 d . . . H23A H 0.5181 0.2001 0.4074 0.063 Uiso 1 1 calc R . . H23B H 0.5018 0.2869 0.4772 0.063 Uiso 1 1 calc R . . H23C H 0.6302 0.1962 0.4511 0.063 Uiso 1 1 calc R . . C24 C 0.4253(3) 0.5201(2) 0.15127(18) 0.0474(7) Uani 1 1 d . . . H24A H 0.3553 0.5777 0.1781 0.071 Uiso 1 1 calc R . . H24B H 0.4022 0.4642 0.1301 0.071 Uiso 1 1 calc R . . H24C H 0.462 0.5567 0.1009 0.071 Uiso 1 1 calc R . . C25 C 0.5992(3) 0.0296(2) 0.09902(19) 0.0530(7) Uani 1 1 d . . . H25A H 0.5414 0.0651 0.0548 0.079 Uiso 1 1 calc R . . H25B H 0.5784 -0.0293 0.1387 0.079 Uiso 1 1 calc R . . H25C H 0.6781 -0.0048 0.0684 0.079 Uiso 1 1 calc R . . C26 C 0.7173(3) 0.0677(3) 0.2431(2) 0.0722(10) Uani 1 1 d . . . H26A H 0.7215 0.1234 0.2782 0.108 Uiso 1 1 calc R . . H26B H 0.7933 0.0345 0.2082 0.108 Uiso 1 1 calc R . . H26C H 0.6995 0.0075 0.2833 0.108 Uiso 1 1 calc R . . C27 C 0.6456(3) 0.2437(3) 0.0844(2) 0.0653(9) Uani 1 1 d . . . H27A H 0.5842 0.285 0.0438 0.098 Uiso 1 1 calc R . . H27B H 0.7195 0.2026 0.05 0.098 Uiso 1 1 calc R . . H27C H 0.6579 0.2976 0.1168 0.098 Uiso 1 1 calc R . . C28 C -0.0249(2) 0.4752(2) 0.19372(17) 0.0373(6) Uani 1 1 d . . . C29 C -0.1097(2) 0.5323(2) 0.12961(16) 0.0346(5) Uani 1 1 d . . . C30 C -0.1193(2) 0.4702(2) 0.06585(17) 0.0420(6) Uani 1 1 d . . . C31 C -0.2006(3) 0.5283(3) 0.00377(18) 0.0537(7) Uani 1 1 d . . . H31 H -0.2083 0.4896 -0.0417 0.064 Uiso 1 1 calc R . . C32 C -0.2703(3) 0.6414(3) 0.00747(19) 0.0555(8) Uani 1 1 d . . . H32 H -0.3252 0.6797 -0.0357 0.067 Uiso 1 1 calc R . . C33 C -0.2618(2) 0.6997(2) 0.07221(19) 0.0499(7) Uani 1 1 d . . . H33 H -0.312 0.7772 0.074 0.06 Uiso 1 1 calc R . . C34 C -0.1809(2) 0.6472(2) 0.13539(17) 0.0386(6) Uani 1 1 d . . . C35 C -0.0461(3) 0.3460(3) 0.0651(2) 0.0606(8) Uani 1 1 d . . . H35A H -0.0675 0.3036 0.1198 0.091 Uiso 1 1 calc R . . H35B H 0.0378 0.3342 0.0619 0.091 Uiso 1 1 calc R . . H35C H -0.0607 0.3189 0.0132 0.091 Uiso 1 1 calc R . . C36 C -0.1708(3) 0.7090(2) 0.2073(2) 0.0580(8) Uani 1 1 d . . . H36A H -0.0894 0.705 0.2046 0.087 Uiso 1 1 calc R . . H36B H -0.1922 0.6736 0.2657 0.087 Uiso 1 1 calc R . . H36C H -0.2244 0.7887 0.1988 0.087 Uiso 1 1 calc R . . C37 C 0.0169(9) 0.0011(12) 0.0353(8) 0.244(6) Uani 1 1 d . . . C38 C 0.0388(8) -0.1183(9) 0.0989(6) 0.183(4) Uani 1 1 d . . . C39 C 0.0542(10) -0.1100(12) 0.1752(13) 0.150(5) Uani 0.5 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li 0.028(2) 0.033(2) 0.047(2) -0.0039(18) -0.0106(17) -0.0067(17) Si1 0.0291(3) 0.0392(4) 0.0406(4) 0.0069(3) 0.0003(3) -0.0109(3) Si2 0.0404(4) 0.0443(4) 0.0521(5) -0.0249(4) 0.0029(3) -0.0142(3) Si3 0.0298(3) 0.0244(3) 0.0240(3) -0.0016(2) -0.0015(2) -0.0104(3) Si4 0.0354(4) 0.0333(4) 0.0332(4) -0.0058(3) 0.0068(3) -0.0093(3) N1 0.0263(10) 0.0292(10) 0.0308(10) 0.0006(8) -0.0032(8) -0.0080(8) N2 0.0283(10) 0.0304(10) 0.0350(11) -0.0090(8) -0.0035(8) -0.0079(8) N3 0.0393(12) 0.0394(12) 0.0584(15) 0.0072(11) -0.0172(11) -0.0134(10) C1 0.0277(11) 0.0263(11) 0.0226(11) 0.0033(9) -0.0102(9) -0.0080(9) C2 0.0289(11) 0.0243(11) 0.0224(11) 0.0037(9) -0.0089(9) -0.0082(9) C3 0.067(2) 0.089(2) 0.0418(17) 0.0065(16) 0.0057(15) -0.0329(19) C4 0.067(2) 0.0571(19) 0.078(2) 0.0023(17) 0.0141(17) -0.0389(17) C5 0.0345(15) 0.080(2) 0.090(3) 0.035(2) -0.0068(16) -0.0181(15) C6 0.153(4) 0.103(3) 0.063(2) -0.044(2) 0.046(3) -0.081(3) C7 0.079(3) 0.101(3) 0.201(6) -0.105(4) -0.054(3) 0.037(2) C8 0.085(2) 0.061(2) 0.068(2) -0.0372(17) 0.0210(18) -0.0438(18) C9 0.0311(12) 0.0243(11) 0.0300(12) 0.0005(9) 0.0027(9) -0.0125(9) C10 0.0332(13) 0.0281(12) 0.0419(14) 0.0071(10) 0.0013(10) -0.0101(10) C11 0.0448(16) 0.0270(13) 0.070(2) 0.0051(13) 0.0052(14) -0.0073(12) C12 0.066(2) 0.0309(15) 0.081(2) -0.0187(15) 0.0201(18) -0.0186(14) C13 0.0690(19) 0.0469(17) 0.0513(17) -0.0189(14) 0.0088(14) -0.0334(15) C14 0.0469(14) 0.0375(14) 0.0355(13) -0.0049(11) 0.0029(11) -0.0228(12) C15 0.0403(14) 0.0430(15) 0.0473(16) 0.0164(12) -0.0130(12) -0.0103(12) C16 0.0696(19) 0.0502(16) 0.0438(16) -0.0002(13) -0.0211(14) -0.0306(15) C17 0.0285(11) 0.0250(11) 0.0286(12) -0.0035(9) -0.0017(9) -0.0097(9) C18 0.0333(12) 0.0365(13) 0.0300(12) -0.0014(10) -0.0033(10) -0.0151(10) C19 0.0341(13) 0.0556(16) 0.0460(15) -0.0017(13) -0.0086(11) -0.0195(12) C20 0.0418(15) 0.0644(18) 0.0506(17) -0.0085(14) 0.0023(13) -0.0336(14) C21 0.0527(16) 0.0381(14) 0.0421(15) -0.0062(11) 0.0117(12) -0.0278(12) C22 0.0448(14) 0.0268(12) 0.0303(12) -0.0033(9) -0.0006(10) -0.0146(10) C23 0.0430(14) 0.0496(15) 0.0346(13) 0.0098(11) -0.0138(11) -0.0195(12) C24 0.0664(18) 0.0338(14) 0.0410(15) 0.0090(11) -0.0134(13) -0.0197(13) C25 0.0594(18) 0.0444(16) 0.0522(17) -0.0201(13) 0.0207(14) -0.0197(14) C26 0.0350(16) 0.094(3) 0.062(2) -0.0169(19) -0.0025(14) 0.0065(16) C27 0.066(2) 0.0524(18) 0.072(2) -0.0147(16) 0.0365(17) -0.0280(16) C28 0.0283(12) 0.0354(13) 0.0450(15) 0.0034(11) -0.0036(11) -0.0116(10) C29 0.0257(11) 0.0383(13) 0.0350(13) 0.0089(10) -0.0039(10) -0.0114(10) C30 0.0365(14) 0.0476(15) 0.0377(14) -0.0018(12) 0.0007(11) -0.0138(12) C31 0.0515(17) 0.078(2) 0.0334(15) -0.0018(14) -0.0044(12) -0.0270(16) C32 0.0454(16) 0.072(2) 0.0392(16) 0.0196(15) -0.0134(13) -0.0182(15) C33 0.0408(15) 0.0435(15) 0.0515(17) 0.0169(13) -0.0071(13) -0.0082(12) C34 0.0323(13) 0.0372(13) 0.0398(14) 0.0086(11) -0.0041(11) -0.0105(11) C35 0.0576(19) 0.0526(18) 0.068(2) -0.0156(15) -0.0038(16) -0.0146(15) C36 0.0540(18) 0.0458(17) 0.071(2) -0.0071(15) -0.0102(15) -0.0129(14) C37 0.210(8) 0.341(12) 0.308(15) -0.240(12) 0.135(10) -0.218(9) C38 0.198(8) 0.227(9) 0.180(8) -0.114(7) 0.079(7) -0.138(8) C39 0.078(7) 0.140(11) 0.230(17) -0.046(12) 0.018(9) -0.040(7) #----------------------------------------------------------------------------# # 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 Li N2 1.950(4) . ? Li N1 1.954(4) . ? Li N3 1.995(4) . ? Si1 N1 1.740(2) . ? Si1 C4 1.855(3) . ? Si1 C5 1.857(3) . ? Si1 C3 1.864(3) . ? Si2 N2 1.746(2) . ? Si2 C8 1.849(3) . ? Si2 C7 1.858(4) . ? Si2 C6 1.859(4) . ? Si3 C2 1.881(2) . ? Si3 C1 1.881(2) . ? Si3 Si4 2.3356(11) . ? Si4 C25 1.869(3) . ? Si4 C26 1.871(3) . ? Si4 C27 1.876(3) . ? N1 C1 1.311(3) . ? N2 C2 1.303(3) . ? N3 C28 1.141(3) . ? C1 C9 1.503(3) . ? C2 C17 1.508(3) . ? C9 C14 1.399(3) . ? C9 C10 1.406(3) . ? C10 C11 1.392(4) . ? C10 C15 1.506(4) . ? C11 C12 1.368(4) . ? C12 C13 1.378(5) . ? C13 C14 1.394(4) . ? C14 C16 1.503(4) . ? C17 C22 1.398(3) . ? C17 C18 1.402(3) . ? C18 C19 1.388(3) . ? C18 C23 1.504(3) . ? C19 C20 1.371(4) . ? C20 C21 1.375(4) . ? C21 C22 1.395(3) . ? C22 C24 1.511(3) . ? C28 C29 1.437(3) . ? C29 C30 1.397(4) . ? C29 C34 1.405(3) . ? C30 C31 1.389(4) . ? C30 C35 1.500(4) . ? C31 C32 1.378(4) . ? C32 C33 1.369(4) . ? C33 C34 1.390(4) . ? C34 C36 1.498(4) . ? C37 C37 1.22(2) 2 ? C37 C38 1.626(17) . ? C38 C39 1.233(17) . ? 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 Li N1 111.4(2) . . ? N2 Li N3 123.0(2) . . ? N1 Li N3 121.5(2) . . ? N1 Si1 C4 119.42(12) . . ? N1 Si1 C5 105.66(12) . . ? C4 Si1 C5 108.41(17) . . ? N1 Si1 C3 106.36(13) . . ? C4 Si1 C3 107.69(17) . . ? C5 Si1 C3 108.96(17) . . ? N2 Si2 C8 118.81(12) . . ? N2 Si2 C7 104.68(15) . . ? C8 Si2 C7 108.4(2) . . ? N2 Si2 C6 106.45(14) . . ? C8 Si2 C6 109.04(18) . . ? C7 Si2 C6 109.1(3) . . ? C2 Si3 C1 108.78(10) . . ? C2 Si3 Si4 114.74(8) . . ? C1 Si3 Si4 115.63(8) . . ? C25 Si4 C26 106.89(16) . . ? C25 Si4 C27 105.68(14) . . ? C26 Si4 C27 107.00(17) . . ? C25 Si4 Si3 108.77(10) . . ? C26 Si4 Si3 119.46(10) . . ? C27 Si4 Si3 108.23(10) . . ? C1 N1 Si1 132.70(16) . . ? C1 N1 Li 105.33(19) . . ? Si1 N1 Li 120.47(16) . . ? C2 N2 Si2 132.73(16) . . ? C2 N2 Li 107.00(19) . . ? Si2 N2 Li 120.06(15) . . ? C28 N3 Li 173.7(3) . . ? N1 C1 C9 120.25(19) . . ? N1 C1 Si3 124.39(17) . . ? C9 C1 Si3 115.14(15) . . ? N2 C2 C17 120.98(19) . . ? N2 C2 Si3 123.93(16) . . ? C17 C2 Si3 115.05(15) . . ? C14 C9 C10 120.6(2) . . ? C14 C9 C1 119.4(2) . . ? C10 C9 C1 120.0(2) . . ? C11 C10 C9 118.5(2) . . ? C11 C10 C15 121.0(2) . . ? C9 C10 C15 120.5(2) . . ? C12 C11 C10 121.0(3) . . ? C11 C12 C13 120.6(3) . . ? C12 C13 C14 120.6(3) . . ? C13 C14 C9 118.7(2) . . ? C13 C14 C16 120.0(2) . . ? C9 C14 C16 121.2(2) . . ? C22 C17 C18 120.4(2) . . ? C22 C17 C2 121.2(2) . . ? C18 C17 C2 118.35(19) . . ? C19 C18 C17 118.9(2) . . ? C19 C18 C23 119.6(2) . . ? C17 C18 C23 121.5(2) . . ? C20 C19 C18 121.0(2) . . ? C19 C20 C21 120.0(2) . . ? C20 C21 C22 121.1(2) . . ? C21 C22 C17 118.5(2) . . ? C21 C22 C24 120.3(2) . . ? C17 C22 C24 121.2(2) . . ? N3 C28 C29 179.7(3) . . ? C30 C29 C34 123.1(2) . . ? C30 C29 C28 118.5(2) . . ? C34 C29 C28 118.4(2) . . ? C31 C30 C29 117.1(2) . . ? C31 C30 C35 121.5(3) . . ? C29 C30 C35 121.4(2) . . ? C32 C31 C30 120.7(3) . . ? C33 C32 C31 121.2(3) . . ? C32 C33 C34 121.1(3) . . ? C33 C34 C29 116.8(3) . . ? C33 C34 C36 121.9(2) . . ? C29 C34 C36 121.3(2) . . ? C37 C37 C38 111.0(12) 2 . ? C39 C38 C37 111.0(11) . . ? #===END data_mfl(5)-oct1901 _database_code_CSD 199537 _audit_creation_date 2001-10-24T16:52:49-00:00 _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 ;'((Rb(NCR)(Me3SiNCRSi(SiMe3)CRNSiMe3))2).2(benzene) R=C6H3Me2' ; _chemical_formula_moiety '(C72 H108 N6 Rb2 Si8).2(C6 H6)' _chemical_formula_sum 'C84 H120 N6 Rb2 Si8' _chemical_formula_weight 1609.52 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.4463(10) _cell_length_b 12.8577(6) _cell_length_c 15.1885(12) _cell_angle_alpha 70.970(4) _cell_angle_beta 88.410(3) _cell_angle_gamma 86.368(5) _cell_volume 2293.1(3) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6620 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.166 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 852 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.214 _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 0.825 _exptl_absorpt_correction_T_max 0.883 #----------------------------------------------------------------------------# # 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 12835 _diffrn_reflns_av_R_equivalents 0.0624 _diffrn_reflns_av_unetI/netI 0.1259 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.74 _diffrn_reflns_theta_max 24.99 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.975 _diffrn_measured_fraction_theta_max 0.975 _reflns_number_total 7865 _reflns_number_gt 4958 _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^)+(0.0175P)^2^+2.4395P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 7865 _refine_ls_number_parameters 466 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1259 _refine_ls_R_factor_gt 0.0656 _refine_ls_wR_factor_ref 0.1278 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.367 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # 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' Rb Rb -0.9393 2.9676 '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 Rb Rb -0.13800(4) 0.09257(4) 0.05047(4) 0.03783(17) Uani 1 1 d . . . Si1 Si -0.30857(12) -0.10348(11) 0.25512(11) 0.0393(4) Uani 1 1 d . . . Si2 Si -0.02070(12) 0.23918(10) 0.21717(11) 0.0369(4) Uani 1 1 d . . . Si3 Si 0.05048(10) -0.10082(9) 0.19031(9) 0.0259(3) Uani 1 1 d . . . Si4 Si 0.18553(11) -0.23711(10) 0.26077(10) 0.0316(3) Uani 1 1 d . . . N1 N -0.1745(3) -0.0845(3) 0.2219(3) 0.0338(10) Uani 1 1 d . . . N2 N -0.0080(3) 0.1121(3) 0.2004(3) 0.0333(10) Uani 1 1 d . . . N3 N -0.3280(4) 0.2522(4) 0.0167(3) 0.0587(14) Uani 1 1 d . . . C1 C -0.0883(4) -0.1496(3) 0.2355(3) 0.0271(11) Uani 1 1 d . . . C2 C 0.0663(4) 0.0328(3) 0.2170(3) 0.0257(11) Uani 1 1 d . . . C3 C -0.0974(4) -0.2726(3) 0.2837(3) 0.0271(11) Uani 1 1 d . . . C4 C -0.0990(4) -0.3164(4) 0.3808(3) 0.0323(12) Uani 1 1 d . . . C5 C -0.1095(4) -0.4289(4) 0.4229(4) 0.0444(14) Uani 1 1 d . . . H5 H -0.1093 -0.4591 0.4889 0.053 Uiso 1 1 calc R . . C6 C -0.1203(4) -0.4969(4) 0.3707(4) 0.0505(16) Uani 1 1 d . . . H6 H -0.128 -0.5735 0.4005 0.061 Uiso 1 1 calc R . . C7 C -0.1199(4) -0.4535(4) 0.2749(4) 0.0427(14) Uani 1 1 d . . . H7 H -0.1273 -0.501 0.2391 0.051 Uiso 1 1 calc R . . C8 C -0.1090(4) -0.3418(4) 0.2295(4) 0.0358(13) Uani 1 1 d . . . C9 C -0.0927(4) -0.2451(4) 0.4418(4) 0.0452(14) Uani 1 1 d . . . H9A H -0.0449 -0.1854 0.4126 0.068 Uiso 1 1 calc R . . H9B H -0.0643 -0.2898 0.5029 0.068 Uiso 1 1 calc R . . H9C H -0.1648 -0.2137 0.4495 0.068 Uiso 1 1 calc R . . C10 C -0.1132(5) -0.2966(4) 0.1251(4) 0.0485(15) Uani 1 1 d . . . H10A H -0.1029 -0.3573 0.0994 0.073 Uiso 1 1 calc R . . H10B H -0.0561 -0.2452 0.1018 0.073 Uiso 1 1 calc R . . H10C H -0.1834 -0.2578 0.1058 0.073 Uiso 1 1 calc R . . C11 C 0.1743(4) 0.0473(3) 0.2537(3) 0.0283(11) Uani 1 1 d . . . C12 C 0.2579(4) 0.0902(4) 0.1913(4) 0.0360(13) Uani 1 1 d . . . C13 C 0.3562(4) 0.1030(4) 0.2265(5) 0.0514(16) Uani 1 1 d . . . H13 H 0.4134 0.1321 0.1847 0.062 Uiso 1 1 calc R . . C14 C 0.3718(5) 0.0744(5) 0.3206(6) 0.0608(18) Uani 1 1 d . . . H14 H 0.4399 0.0828 0.3434 0.073 Uiso 1 1 calc R . . C15 C 0.2894(5) 0.0335(4) 0.3824(4) 0.0528(16) Uani 1 1 d . . . H15 H 0.3008 0.015 0.4474 0.063 Uiso 1 1 calc R . . C16 C 0.1895(4) 0.0191(4) 0.3500(4) 0.0360(13) Uani 1 1 d . . . C17 C 0.2443(5) 0.1237(4) 0.0881(4) 0.0572(16) Uani 1 1 d . . . H17A H 0.3125 0.1488 0.057 0.086 Uiso 1 1 calc R . . H17B H 0.1885 0.1838 0.0683 0.086 Uiso 1 1 calc R . . H17C H 0.2229 0.0607 0.0712 0.086 Uiso 1 1 calc R . . C18 C 0.0997(5) -0.0190(4) 0.4180(4) 0.0509(15) Uani 1 1 d . . . H18A H 0.1295 -0.0625 0.4788 0.076 Uiso 1 1 calc R . . H18B H 0.0538 -0.0644 0.3959 0.076 Uiso 1 1 calc R . . H18C H 0.0568 0.0451 0.4238 0.076 Uiso 1 1 calc R . . C19 C -0.3547(4) -0.2449(4) 0.3130(4) 0.0435(14) Uani 1 1 d . . . H19A H -0.3376 -0.2903 0.2731 0.065 Uiso 1 1 calc R . . H19B H -0.4327 -0.241 0.3236 0.065 Uiso 1 1 calc R . . H19C H -0.3181 -0.278 0.3728 0.065 Uiso 1 1 calc R . . C20 C -0.3874(4) -0.0422(4) 0.1449(4) 0.0611(17) Uani 1 1 d . . . H20A H -0.3766 0.037 0.1194 0.092 Uiso 1 1 calc R . . H20B H -0.464 -0.0534 0.1583 0.092 Uiso 1 1 calc R . . H20C H -0.3626 -0.078 0.0995 0.092 Uiso 1 1 calc R . . C21 C -0.3369(5) -0.0224(4) 0.3363(4) 0.0600(17) Uani 1 1 d . . . H21A H -0.2771 -0.0354 0.3799 0.09 Uiso 1 1 calc R . . H21B H -0.4035 -0.0456 0.371 0.09 Uiso 1 1 calc R . . H21C H -0.3448 0.0562 0.3004 0.09 Uiso 1 1 calc R . . C22 C -0.1405(5) 0.2325(4) 0.2948(5) 0.0647(19) Uani 1 1 d . . . H22A H -0.2002 0.2036 0.2708 0.097 Uiso 1 1 calc R . . H22B H -0.1617 0.3065 0.2965 0.097 Uiso 1 1 calc R . . H22C H -0.1227 0.1839 0.3578 0.097 Uiso 1 1 calc R . . C23 C -0.0515(6) 0.3417(4) 0.0995(4) 0.0672(19) Uani 1 1 d . . . H23A H 0.0056 0.3356 0.0554 0.101 Uiso 1 1 calc R . . H23B H -0.0554 0.4163 0.1037 0.101 Uiso 1 1 calc R . . H23C H -0.1206 0.3269 0.078 0.101 Uiso 1 1 calc R . . C24 C 0.0946(4) 0.2891(4) 0.2657(4) 0.0547(16) Uani 1 1 d . . . H24A H 0.111 0.2384 0.3283 0.082 Uiso 1 1 calc R . . H24B H 0.0752 0.3628 0.2689 0.082 Uiso 1 1 calc R . . H24C H 0.1578 0.2921 0.2252 0.082 Uiso 1 1 calc R . . C25 C 0.3221(4) -0.1856(4) 0.2210(4) 0.0470(15) Uani 1 1 d . . . H25A H 0.3384 -0.13 0.2492 0.071 Uiso 1 1 calc R . . H25B H 0.3229 -0.1527 0.153 0.071 Uiso 1 1 calc R . . H25C H 0.3764 -0.2472 0.2399 0.071 Uiso 1 1 calc R . . C26 C 0.1914(5) -0.2956(4) 0.3912(4) 0.0534(16) Uani 1 1 d . . . H26A H 0.2486 -0.3542 0.4094 0.08 Uiso 1 1 calc R . . H26B H 0.1222 -0.3258 0.4156 0.08 Uiso 1 1 calc R . . H26C H 0.2063 -0.2372 0.4167 0.08 Uiso 1 1 calc R . . C27 C 0.1732(4) -0.3578(4) 0.2180(4) 0.0473(15) Uani 1 1 d . . . H27A H 0.2401 -0.4043 0.2304 0.071 Uiso 1 1 calc R . . H27B H 0.1596 -0.3309 0.1508 0.071 Uiso 1 1 calc R . . H27C H 0.1133 -0.401 0.2504 0.071 Uiso 1 1 calc R . . C28 C -0.4086(5) 0.2966(4) 0.0244(4) 0.0441(14) Uani 1 1 d . . . C29 C -0.5098(4) 0.3505(3) 0.0361(4) 0.0334(12) Uani 1 1 d . . . C30 C -0.5826(4) 0.3856(4) -0.0375(4) 0.0399(13) Uani 1 1 d . . . C31 C -0.6799(4) 0.4370(4) -0.0225(5) 0.0506(16) Uani 1 1 d . . . H31 H -0.7314 0.4619 -0.0711 0.061 Uiso 1 1 calc R . . C32 C -0.7024(5) 0.4523(4) 0.0614(5) 0.0552(17) Uani 1 1 d . . . H32 H -0.769 0.4882 0.07 0.066 Uiso 1 1 calc R . . C33 C -0.6303(5) 0.4167(4) 0.1327(4) 0.0515(16) Uani 1 1 d . . . H33 H -0.6483 0.4273 0.1905 0.062 Uiso 1 1 calc R . . C34 C -0.5318(4) 0.3656(4) 0.1227(4) 0.0367(13) Uani 1 1 d . . . C35 C -0.5574(5) 0.3660(4) -0.1280(4) 0.0617(18) Uani 1 1 d . . . H35A H -0.49 0.3996 -0.1537 0.093 Uiso 1 1 calc R . . H35B H -0.616 0.399 -0.172 0.093 Uiso 1 1 calc R . . H35C H -0.5497 0.2866 -0.1175 0.093 Uiso 1 1 calc R . . C36 C -0.4515(5) 0.3281(4) 0.2002(4) 0.0574(16) Uani 1 1 d . . . H36A H -0.4428 0.2475 0.2219 0.086 Uiso 1 1 calc R . . H36B H -0.4771 0.3534 0.2518 0.086 Uiso 1 1 calc R . . H36C H -0.3821 0.3591 0.1775 0.086 Uiso 1 1 calc R . . C37 C -0.5000(9) 0.2474(6) 0.4520(5) 0.084(2) Uani 1 1 d . . . H37 H -0.4858 0.1697 0.4733 0.101 Uiso 1 1 calc R . . C38 C -0.6023(7) 0.2902(6) 0.4313(5) 0.076(2) Uani 1 1 d . . . H38 H -0.6595 0.2426 0.4377 0.092 Uiso 1 1 calc R . . C39 C -0.6227(6) 0.4003(7) 0.4017(4) 0.073(2) Uani 1 1 d . . . H39 H -0.6944 0.4299 0.3878 0.087 Uiso 1 1 calc R . . C40 C -0.5415(9) 0.4695(6) 0.3917(5) 0.087(3) Uani 1 1 d . . . H40 H -0.5567 0.547 0.3711 0.105 Uiso 1 1 calc R . . C41 C -0.4382(9) 0.4272(9) 0.4111(6) 0.104(3) Uani 1 1 d . . . H41 H -0.381 0.4751 0.4031 0.125 Uiso 1 1 calc R . . C42 C -0.4175(7) 0.3151(9) 0.4423(5) 0.092(3) Uani 1 1 d . . . H42 H -0.346 0.2849 0.457 0.111 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Rb 0.0391(3) 0.0388(3) 0.0327(3) -0.0097(2) -0.0052(2) 0.0106(2) Si1 0.0282(9) 0.0356(8) 0.0518(11) -0.0115(7) 0.0009(7) -0.0001(6) Si2 0.0396(9) 0.0262(7) 0.0472(10) -0.0158(7) 0.0000(7) 0.0020(6) Si3 0.0240(8) 0.0235(7) 0.0297(8) -0.0084(6) -0.0024(6) 0.0019(5) Si4 0.0275(8) 0.0290(7) 0.0368(9) -0.0096(6) -0.0042(7) 0.0058(6) N1 0.027(3) 0.031(2) 0.042(3) -0.0099(19) -0.002(2) -0.0005(18) N2 0.035(3) 0.028(2) 0.039(3) -0.0138(19) -0.005(2) 0.0067(18) N3 0.056(4) 0.047(3) 0.068(4) -0.015(3) 0.002(3) 0.015(2) C1 0.028(3) 0.026(2) 0.027(3) -0.008(2) -0.001(2) -0.001(2) C2 0.028(3) 0.025(2) 0.023(3) -0.007(2) 0.005(2) -0.006(2) C3 0.024(3) 0.026(2) 0.030(3) -0.007(2) -0.003(2) -0.0010(19) C4 0.027(3) 0.036(3) 0.031(3) -0.006(2) -0.006(2) 0.000(2) C5 0.047(4) 0.039(3) 0.038(4) -0.001(3) 0.000(3) -0.003(2) C6 0.058(4) 0.025(3) 0.056(4) 0.005(3) -0.009(3) -0.005(2) C7 0.046(4) 0.026(3) 0.058(4) -0.016(3) -0.005(3) -0.003(2) C8 0.032(3) 0.035(3) 0.043(4) -0.017(3) -0.006(3) 0.000(2) C9 0.054(4) 0.049(3) 0.031(3) -0.010(3) -0.001(3) -0.007(3) C10 0.067(4) 0.049(3) 0.039(4) -0.026(3) -0.004(3) -0.012(3) C11 0.025(3) 0.024(2) 0.036(3) -0.010(2) -0.001(2) 0.000(2) C12 0.031(3) 0.029(3) 0.053(4) -0.019(3) 0.003(3) -0.001(2) C13 0.030(4) 0.039(3) 0.091(5) -0.028(3) 0.010(3) -0.008(2) C14 0.042(4) 0.054(4) 0.095(6) -0.037(4) -0.022(4) 0.006(3) C15 0.056(4) 0.053(4) 0.053(4) -0.023(3) -0.021(4) 0.005(3) C16 0.039(3) 0.034(3) 0.035(3) -0.010(2) -0.013(3) 0.001(2) C17 0.064(5) 0.056(4) 0.051(4) -0.015(3) 0.019(3) -0.022(3) C18 0.070(4) 0.057(3) 0.025(3) -0.012(3) 0.009(3) -0.012(3) C19 0.032(3) 0.048(3) 0.050(4) -0.016(3) 0.004(3) -0.005(2) C20 0.040(4) 0.061(4) 0.065(5) 0.003(3) -0.009(3) -0.003(3) C21 0.042(4) 0.062(4) 0.085(5) -0.037(3) 0.017(3) -0.002(3) C22 0.056(4) 0.044(3) 0.099(6) -0.033(3) 0.018(4) 0.001(3) C23 0.103(6) 0.038(3) 0.059(4) -0.014(3) -0.016(4) 0.012(3) C24 0.057(4) 0.040(3) 0.078(5) -0.033(3) -0.002(3) -0.002(3) C25 0.034(3) 0.041(3) 0.064(4) -0.017(3) 0.001(3) 0.007(2) C26 0.052(4) 0.057(3) 0.043(4) -0.007(3) -0.011(3) 0.018(3) C27 0.047(4) 0.031(3) 0.065(4) -0.020(3) -0.007(3) 0.007(2) C28 0.049(4) 0.032(3) 0.052(4) -0.016(3) -0.002(3) 0.002(3) C29 0.035(3) 0.023(2) 0.040(3) -0.008(2) 0.002(3) -0.003(2) C30 0.052(4) 0.029(3) 0.041(4) -0.013(2) -0.001(3) -0.008(2) C31 0.038(4) 0.035(3) 0.075(5) -0.012(3) -0.015(3) 0.000(2) C32 0.041(4) 0.043(3) 0.084(5) -0.024(3) 0.010(4) -0.004(3) C33 0.060(4) 0.043(3) 0.053(4) -0.018(3) 0.020(4) -0.009(3) C34 0.038(3) 0.031(3) 0.036(3) -0.004(2) 0.007(3) -0.007(2) C35 0.084(5) 0.053(4) 0.055(4) -0.026(3) -0.019(4) -0.003(3) C36 0.071(5) 0.054(3) 0.046(4) -0.014(3) -0.008(3) 0.000(3) C37 0.120(8) 0.074(5) 0.049(5) -0.011(4) -0.004(5) 0.018(5) C38 0.092(7) 0.080(5) 0.065(5) -0.033(4) 0.025(5) -0.020(4) C39 0.073(6) 0.094(6) 0.051(5) -0.026(4) 0.004(4) 0.014(4) C40 0.130(8) 0.063(5) 0.072(6) -0.030(4) 0.007(6) 0.007(5) C41 0.122(9) 0.123(8) 0.100(7) -0.077(6) 0.004(6) -0.044(6) C42 0.076(6) 0.153(8) 0.066(6) -0.064(6) -0.035(5) 0.030(6) #----------------------------------------------------------------------------# # 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 Rb N1 2.892(4) . ? Rb N2 2.915(4) . ? Rb N3 2.972(5) . ? Rb Si3 3.5058(13) . ? Rb Si3 3.7567(15) 2 ? Si1 N1 1.739(4) . ? Si1 C19 1.863(5) . ? Si1 C21 1.870(5) . ? Si1 C20 1.876(6) . ? Si2 N2 1.731(4) . ? Si2 C22 1.864(6) . ? Si2 C24 1.869(5) . ? Si2 C23 1.875(6) . ? Si3 C1 1.908(5) . ? Si3 C2 1.912(4) . ? Si3 Si4 2.3548(17) . ? Si3 Rb 3.7567(15) 2 ? Si4 C25 1.876(5) . ? Si4 C26 1.877(5) . ? Si4 C27 1.883(5) . ? N1 C1 1.296(5) . ? N2 C2 1.298(5) . ? N3 C28 1.144(6) . ? C1 C3 1.521(6) . ? C2 C11 1.515(6) . ? C3 C4 1.396(6) . ? C3 C8 1.412(6) . ? C4 C5 1.390(6) . ? C4 C9 1.507(6) . ? C5 C6 1.372(7) . ? C6 C7 1.378(7) . ? C7 C8 1.389(6) . ? C8 C10 1.502(7) . ? C11 C12 1.401(7) . ? C11 C16 1.402(6) . ? C12 C13 1.388(7) . ? C12 C17 1.495(7) . ? C13 C14 1.372(8) . ? C14 C15 1.379(8) . ? C15 C16 1.395(7) . ? C16 C18 1.494(7) . ? C28 C29 1.435(7) . ? C29 C30 1.396(7) . ? C29 C34 1.409(7) . ? C30 C31 1.392(7) . ? C30 C35 1.497(7) . ? C31 C32 1.370(8) . ? C32 C33 1.367(8) . ? C33 C34 1.383(7) . ? C34 C36 1.500(7) . ? C37 C38 1.358(10) . ? C37 C42 1.362(10) . ? C38 C39 1.348(9) . ? C39 C40 1.361(9) . ? C40 C41 1.365(11) . ? C41 C42 1.372(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Rb N2 69.22(10) . . ? N1 Rb N3 108.26(12) . . ? N2 Rb N3 110.23(12) . . ? N1 Rb Si3 51.50(8) . . ? N2 Rb Si3 51.50(7) . . ? N3 Rb Si3 154.42(10) . . ? N1 Rb Si3 133.56(8) . 2 ? N2 Rb Si3 128.56(8) . 2 ? N3 Rb Si3 103.45(10) . 2 ? Si3 Rb Si3 102.13(3) . 2 ? N1 Si1 C19 120.2(2) . . ? N1 Si1 C21 105.4(2) . . ? C19 Si1 C21 107.8(3) . . ? N1 Si1 C20 105.2(2) . . ? C19 Si1 C20 107.3(2) . . ? C21 Si1 C20 110.8(3) . . ? N2 Si2 C22 105.2(2) . . ? N2 Si2 C24 119.7(2) . . ? C22 Si2 C24 109.3(3) . . ? N2 Si2 C23 105.5(2) . . ? C22 Si2 C23 109.3(3) . . ? C24 Si2 C23 107.5(3) . . ? C1 Si3 C2 106.71(19) . . ? C1 Si3 Si4 110.55(14) . . ? C2 Si3 Si4 112.06(15) . . ? C1 Si3 Rb 73.44(13) . . ? C2 Si3 Rb 74.21(14) . . ? Si4 Si3 Rb 170.23(6) . . ? C1 Si3 Rb 119.65(14) . 2 ? C2 Si3 Rb 114.76(14) . 2 ? Si4 Si3 Rb 92.53(5) . 2 ? Rb Si3 Rb 77.87(3) . 2 ? C25 Si4 C26 106.2(3) . . ? C25 Si4 C27 105.3(2) . . ? C26 Si4 C27 106.2(2) . . ? C25 Si4 Si3 110.26(16) . . ? C26 Si4 Si3 119.41(17) . . ? C27 Si4 Si3 108.56(17) . . ? C1 N1 Si1 133.7(3) . . ? C1 N1 Rb 106.1(3) . . ? Si1 N1 Rb 115.53(17) . . ? C2 N2 Si2 135.0(3) . . ? C2 N2 Rb 106.2(3) . . ? Si2 N2 Rb 115.05(17) . . ? C28 N3 Rb 163.2(4) . . ? N1 C1 C3 119.4(4) . . ? N1 C1 Si3 123.3(3) . . ? C3 C1 Si3 117.2(3) . . ? N2 C2 C11 119.6(4) . . ? N2 C2 Si3 123.3(3) . . ? C11 C2 Si3 117.0(3) . . ? C4 C3 C8 120.0(4) . . ? C4 C3 C1 120.6(4) . . ? C8 C3 C1 119.4(4) . . ? C5 C4 C3 119.3(4) . . ? C5 C4 C9 118.7(5) . . ? C3 C4 C9 122.0(4) . . ? C6 C5 C4 121.2(5) . . ? C5 C6 C7 119.6(4) . . ? C6 C7 C8 121.4(5) . . ? C7 C8 C3 118.5(5) . . ? C7 C8 C10 120.0(4) . . ? C3 C8 C10 121.5(4) . . ? C12 C11 C16 120.5(4) . . ? C12 C11 C2 119.8(4) . . ? C16 C11 C2 119.7(4) . . ? C13 C12 C11 118.8(5) . . ? C13 C12 C17 119.0(5) . . ? C11 C12 C17 122.1(5) . . ? C14 C13 C12 121.0(6) . . ? C13 C14 C15 120.5(6) . . ? C14 C15 C16 120.4(6) . . ? C15 C16 C11 118.9(5) . . ? C15 C16 C18 119.3(5) . . ? C11 C16 C18 121.7(4) . . ? N3 C28 C29 178.7(6) . . ? C30 C29 C34 122.5(5) . . ? C30 C29 C28 119.5(5) . . ? C34 C29 C28 117.9(5) . . ? C31 C30 C29 117.3(5) . . ? C31 C30 C35 121.7(5) . . ? C29 C30 C35 121.0(5) . . ? C32 C31 C30 120.8(5) . . ? C33 C32 C31 120.9(6) . . ? C32 C33 C34 121.5(6) . . ? C33 C34 C29 116.9(5) . . ? C33 C34 C36 121.8(5) . . ? C29 C34 C36 121.3(5) . . ? C38 C37 C42 120.4(7) . . ? C39 C38 C37 119.9(7) . . ? C38 C39 C40 120.7(7) . . ? C39 C40 C41 119.7(7) . . ? C40 C41 C42 119.6(8) . . ? C37 C42 C41 119.6(8) . . ? #===END data_mfl(6)-jul798 _database_code_CSD 199538 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common (Hg(Si(SiMe3)(C(NSiMe3)(C6H3Me2))2)2) _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C54 H90 Hg N4 Si8' _chemical_formula_weight 1220.61 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hg Hg -2.3894 9.2266 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 11.651(3) _cell_length_b 13.661(5) _cell_length_c 20.070(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.72(3) _cell_angle_gamma 90.00 _cell_volume 3183.6(18) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.273 _exptl_crystal_density_method ? _exptl_crystal_F_000 1268 _exptl_absorpt_coefficient_mu 2.603 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ' Enraf-Nonius CAD4' _diffrn_measurement_method \w--2\q _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 5880 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0719 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5598 _reflns_number_observed 4048 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+4.8406P] 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 riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5596 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_obs 0.0426 _refine_ls_wR_factor_all 0.1372 _refine_ls_wR_factor_obs 0.1023 _refine_ls_goodness_of_fit_all 1.082 _refine_ls_goodness_of_fit_obs 0.962 _refine_ls_restrained_S_all 1.087 _refine_ls_restrained_S_obs 0.962 _refine_ls_shift/esd_max -0.003 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Hg Hg 0.0000 0.0000 0.0000 0.01972(8) Uani 1 d S . Si1 Si -0.35586(15) -0.07684(15) 0.18482(9) 0.0328(5) Uani 1 d . . Si2 Si 0.25981(15) -0.26448(15) -0.00251(9) 0.0325(4) Uani 1 d . . Si3 Si -0.06591(13) -0.14500(11) 0.06117(8) 0.0184(3) Uani 1 d . . Si4 Si -0.20383(14) -0.22686(13) -0.01077(9) 0.0279(4) Uani 1 d . . N1 N -0.2501(4) -0.1052(4) 0.1306(3) 0.0263(12) Uani 1 d . . N2 N 0.1303(4) -0.2151(4) 0.0190(2) 0.0223(11) Uani 1 d . . C1 C -0.1409(5) -0.1124(4) 0.1399(3) 0.0243(14) Uani 1 d . . C2 C 0.0752(5) -0.2183(4) 0.0721(3) 0.0230(14) Uani 1 d . . C3 C -0.0733(5) -0.0936(5) 0.2063(3) 0.0263(15) Uani 1 d . . C4 C -0.0322(6) -0.0007(6) 0.2220(3) 0.038(2) Uani 1 d . . C5 C 0.0264(6) 0.0172(6) 0.2841(3) 0.046(2) Uani 1 d . . H5 H 0.0540(6) 0.0811(6) 0.2950(3) 0.056 Uiso 1 calc R . C6 C 0.0439(6) -0.0569(7) 0.3289(4) 0.056(2) Uani 1 d . . H6 H 0.0849(6) -0.0449(7) 0.3710(4) 0.067 Uiso 1 calc R . C7 C 0.0029(5) -0.1488(6) 0.3138(3) 0.044(2) Uani 1 d . . H7 H 0.0160(5) -0.2000(6) 0.3455(3) 0.053 Uiso 1 calc R . C8 C -0.0588(5) -0.1687(5) 0.2515(3) 0.030(2) Uani 1 d . . C9 C -0.0493(8) 0.0839(6) 0.1738(4) 0.058(2) Uani 1 d . . H9C H -0.1302(13) 0.0866(25) 0.1561(22) 0.087 Uiso 1 calc R . H9B H -0.0003(37) 0.0749(22) 0.1369(15) 0.087 Uiso 1 calc R . H9A H -0.0286(47) 0.1452(7) 0.1972(8) 0.087 Uiso 1 calc R . C10 C -0.1069(6) -0.2681(5) 0.2395(3) 0.037(2) Uani 1 d . . H10C H -0.1129(36) -0.2820(13) 0.1914(4) 0.055 Uiso 1 calc R . H10B H -0.1835(17) -0.2717(11) 0.2561(20) 0.055 Uiso 1 calc R . H10A H -0.0561(20) -0.3164(6) 0.2629(18) 0.055 Uiso 1 calc R . C11 C 0.1187(5) -0.2738(4) 0.1330(3) 0.0231(14) Uani 1 d . . C12 C 0.1897(5) -0.2274(5) 0.1819(3) 0.029(2) Uani 1 d . . C13 C 0.2303(6) -0.2815(6) 0.2370(3) 0.042(2) Uani 1 d . . H13 H 0.2789(6) -0.2504(6) 0.2710(3) 0.050 Uiso 1 calc R . C14 C 0.2032(6) -0.3780(5) 0.2445(4) 0.040(2) Uani 1 d . . H14 H 0.2315(6) -0.4127(5) 0.2834(4) 0.048 Uiso 1 calc R . C15 C 0.1346(6) -0.4242(5) 0.1951(4) 0.038(2) Uani 1 d . . H15 H 0.1171(6) -0.4917(5) 0.1993(4) 0.046 Uiso 1 calc R . C16 C 0.0912(5) -0.3730(5) 0.1392(3) 0.029(2) Uani 1 d . . C17 C 0.2224(6) -0.1207(5) 0.1760(4) 0.040(2) Uani 1 d . . H17C H 0.1600(18) -0.0855(8) 0.1504(20) 0.060 Uiso 1 calc R . H17B H 0.2931(23) -0.1155(5) 0.1529(21) 0.060 Uiso 1 calc R . H17A H 0.2351(39) -0.0920(10) 0.2207(4) 0.060 Uiso 1 calc R . C18 C 0.0153(6) -0.4244(5) 0.0862(3) 0.036(2) Uani 1 d . . H18C H -0.0010(32) -0.4909(12) 0.1012(10) 0.054 Uiso 1 calc R . H18B H 0.0545(17) -0.4277(30) 0.0449(8) 0.054 Uiso 1 calc R . H18A H -0.0571(17) -0.3883(19) 0.0779(16) 0.054 Uiso 1 calc R . C19 C -0.4530(6) 0.0111(6) 0.1376(3) 0.045(2) Uani 1 d . . H19C H -0.4836(35) -0.0188(15) 0.0955(12) 0.067 Uiso 1 calc R . H19B H -0.4099(12) 0.0704(16) 0.1282(22) 0.067 Uiso 1 calc R . H19A H -0.5168(24) 0.0282(29) 0.1644(11) 0.067 Uiso 1 calc R . C20 C -0.4337(7) -0.1939(6) 0.1964(4) 0.059(2) Uani 1 d . . H20C H -0.4556(44) -0.2233(22) 0.1527(5) 0.089 Uiso 1 calc R . H20B H -0.5030(27) -0.1810(9) 0.2196(26) 0.089 Uiso 1 calc R . H20A H -0.3833(19) -0.2391(17) 0.2232(25) 0.089 Uiso 1 calc R . C21 C -0.3080(6) -0.0222(6) 0.2658(4) 0.052(2) Uani 1 d . . H21C H -0.2663(39) 0.0387(20) 0.2586(4) 0.077 Uiso 1 calc R . H21B H -0.2569(36) -0.0681(16) 0.2914(11) 0.077 Uiso 1 calc R . H21A H -0.3750(7) -0.0081(35) 0.2906(11) 0.077 Uiso 1 calc R . C22 C 0.2306(8) -0.3078(9) -0.0889(4) 0.080(3) Uani 1 d . . H22C H 0.1720(44) -0.3593(36) -0.0903(7) 0.121 Uiso 1 calc R . H22B H 0.3016(16) -0.3340(48) -0.1050(13) 0.121 Uiso 1 calc R . H22A H 0.2028(57) -0.2531(13) -0.1174(8) 0.121 Uiso 1 calc R . C23 C 0.3603(7) -0.1601(7) 0.0022(5) 0.071(3) Uani 1 d . . H23C H 0.3305(28) -0.1086(20) -0.0285(24) 0.107 Uiso 1 calc R . H23B H 0.4358(16) -0.1818(13) -0.0104(31) 0.107 Uiso 1 calc R . H23A H 0.3680(42) -0.1345(30) 0.0479(9) 0.107 Uiso 1 calc R . C24 C 0.3255(7) -0.3643(7) 0.0494(5) 0.080(3) Uani 1 d . . H24C H 0.2714(26) -0.4192(21) 0.0497(29) 0.121 Uiso 1 calc R . H24B H 0.3434(57) -0.3407(16) 0.0952(10) 0.121 Uiso 1 calc R . H24A H 0.3964(34) -0.3860(37) 0.0309(22) 0.121 Uiso 1 calc R . C25 C -0.2967(6) -0.3163(6) 0.0328(4) 0.048(2) Uani 1 d . . H25C H -0.3337(35) -0.2823(10) 0.0684(17) 0.072 Uiso 1 calc R . H25B H -0.2487(10) -0.3696(21) 0.0522(23) 0.072 Uiso 1 calc R . H25A H -0.3560(28) -0.3431(29) 0.0004(7) 0.072 Uiso 1 calc R . C26 C -0.2992(6) -0.1319(6) -0.0537(4) 0.047(2) Uani 1 d . . H26C H -0.2522(7) -0.0856(22) -0.0770(21) 0.070 Uiso 1 calc R . H26B H -0.3405(33) -0.0967(25) -0.0204(5) 0.070 Uiso 1 calc R . H26A H -0.3548(28) -0.1636(7) -0.0860(18) 0.070 Uiso 1 calc R . C27 C -0.1287(6) -0.2948(5) -0.0762(3) 0.041(2) Uani 1 d . . H27C H -0.1862(6) -0.3219(30) -0.1096(13) 0.062 Uiso 1 calc R . H27B H -0.0828(33) -0.3481(22) -0.0550(5) 0.062 Uiso 1 calc R . H27A H -0.0781(31) -0.2497(9) -0.0980(16) 0.062 Uiso 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 Hg 0.01990(14) 0.01888(14) 0.02023(14) 0.0030(2) 0.00071(10) 0.0022(2) Si1 0.0216(8) 0.0423(11) 0.0352(10) 0.0073(9) 0.0061(7) 0.0093(8) Si2 0.0269(8) 0.0431(11) 0.0285(9) 0.0038(8) 0.0083(7) 0.0095(8) Si3 0.0184(7) 0.0185(8) 0.0181(7) 0.0012(6) -0.0002(6) 0.0019(6) Si4 0.0223(8) 0.0285(9) 0.0313(9) -0.0005(8) -0.0074(7) -0.0006(8) N1 0.023(2) 0.024(3) 0.032(3) 0.004(2) -0.001(2) 0.002(2) N2 0.027(2) 0.026(3) 0.013(2) 0.005(2) -0.006(2) -0.002(2) C1 0.020(3) 0.012(3) 0.042(4) 0.002(3) 0.010(3) 0.000(2) C2 0.024(3) 0.017(3) 0.028(3) 0.002(3) 0.001(2) -0.008(2) C3 0.018(3) 0.032(3) 0.029(3) -0.006(3) 0.006(2) -0.004(3) C4 0.035(3) 0.045(4) 0.037(3) -0.016(4) 0.011(3) -0.006(4) C5 0.046(4) 0.072(6) 0.021(3) -0.016(3) -0.001(3) -0.025(4) C6 0.037(4) 0.085(6) 0.045(5) -0.015(5) -0.005(4) -0.008(4) C7 0.026(3) 0.080(6) 0.026(3) 0.005(4) -0.002(3) 0.020(4) C8 0.023(3) 0.043(4) 0.025(3) 0.006(3) 0.007(2) 0.006(3) C9 0.112(7) 0.034(4) 0.029(4) -0.005(3) 0.012(4) -0.017(5) C10 0.043(4) 0.039(4) 0.030(3) 0.016(3) 0.007(3) 0.009(3) C11 0.017(3) 0.022(3) 0.031(3) 0.000(3) 0.004(2) 0.006(2) C12 0.020(3) 0.031(3) 0.038(4) 0.000(3) 0.004(3) 0.003(3) C13 0.038(4) 0.063(5) 0.023(3) -0.010(3) -0.008(3) 0.014(4) C14 0.037(4) 0.043(4) 0.042(4) 0.013(3) 0.008(3) 0.017(3) C15 0.034(3) 0.025(3) 0.055(4) 0.014(3) 0.007(3) 0.006(3) C16 0.021(3) 0.028(3) 0.038(4) 0.002(3) 0.003(3) -0.001(3) C17 0.028(3) 0.035(4) 0.056(5) -0.016(3) -0.007(3) -0.001(3) C18 0.044(4) 0.018(3) 0.045(4) 0.000(3) 0.004(3) -0.001(3) C19 0.037(3) 0.066(5) 0.029(3) 0.000(4) -0.003(3) 0.025(4) C20 0.041(4) 0.067(6) 0.073(6) 0.026(5) 0.022(4) 0.001(4) C21 0.042(4) 0.072(6) 0.042(4) -0.007(4) 0.010(3) 0.026(4) C22 0.058(5) 0.127(9) 0.057(5) -0.023(6) 0.012(4) 0.039(6) C23 0.044(4) 0.077(7) 0.097(7) -0.006(6) 0.033(5) -0.007(5) C24 0.051(4) 0.090(6) 0.107(7) 0.044(6) 0.050(5) 0.051(5) C25 0.034(4) 0.051(5) 0.056(5) -0.010(4) -0.010(3) -0.007(4) C26 0.034(4) 0.044(4) 0.059(5) 0.000(4) -0.018(3) 0.003(3) C27 0.048(4) 0.036(4) 0.038(4) -0.014(3) -0.006(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hg Si3 2.485(2) . ? Hg Si3 2.485(2) 3 ? Si1 N1 1.753(5) . ? Si1 C21 1.832(8) . ? Si1 C19 1.856(7) . ? Si1 C20 1.862(8) . ? Si2 N2 1.740(5) . ? Si2 C22 1.836(9) . ? Si2 C23 1.842(9) . ? Si2 C24 1.843(9) . ? Si3 C1 1.920(6) . ? Si3 C2 1.923(6) . ? Si3 Si4 2.353(2) . ? Si4 C26 1.871(7) . ? Si4 C27 1.881(7) . ? Si4 C25 1.893(8) . ? N1 C1 1.275(7) . ? N2 C2 1.288(7) . ? C1 C3 1.513(8) . ? C2 C11 1.491(8) . ? C3 C8 1.370(9) . ? C3 C4 1.384(9) . ? C4 C5 1.391(9) . ? C4 C9 1.510(10) . ? C5 C6 1.360(12) . ? C6 C7 1.368(12) . ? C7 C8 1.417(9) . ? C8 C10 1.481(10) . ? C11 C12 1.384(8) . ? C11 C16 1.400(9) . ? C12 C13 1.381(9) . ? C12 C17 1.514(9) . ? C13 C14 1.366(10) . ? C14 C15 1.375(10) . ? C15 C16 1.382(9) . ? C16 C18 1.501(9) . ? 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 Si3 Hg Si3 180.0 . 3 ? N1 Si1 C21 117.5(3) . . ? N1 Si1 C19 104.9(3) . . ? C21 Si1 C19 108.5(3) . . ? N1 Si1 C20 105.2(3) . . ? C21 Si1 C20 110.8(4) . . ? C19 Si1 C20 109.7(4) . . ? N2 Si2 C22 105.2(3) . . ? N2 Si2 C23 104.4(3) . . ? C22 Si2 C23 111.4(5) . . ? N2 Si2 C24 118.3(3) . . ? C22 Si2 C24 109.3(5) . . ? C23 Si2 C24 108.1(4) . . ? C1 Si3 C2 118.0(3) . . ? C1 Si3 Si4 106.3(2) . . ? C2 Si3 Si4 110.9(2) . . ? C1 Si3 Hg 113.7(2) . . ? C2 Si3 Hg 100.1(2) . . ? Si4 Si3 Hg 107.39(8) . . ? C26 Si4 C27 108.3(3) . . ? C26 Si4 C25 108.6(3) . . ? C27 Si4 C25 108.7(3) . . ? C26 Si4 Si3 107.6(2) . . ? C27 Si4 Si3 109.2(2) . . ? C25 Si4 Si3 114.3(2) . . ? C1 N1 Si1 132.1(5) . . ? C2 N2 Si2 133.9(4) . . ? N1 C1 C3 123.8(5) . . ? N1 C1 Si3 114.4(5) . . ? C3 C1 Si3 121.7(4) . . ? N2 C2 C11 122.4(5) . . ? N2 C2 Si3 111.5(4) . . ? C11 C2 Si3 126.0(4) . . ? C8 C3 C4 121.0(6) . . ? C8 C3 C1 118.8(6) . . ? C4 C3 C1 120.1(6) . . ? C3 C4 C5 120.0(7) . . ? C3 C4 C9 122.1(6) . . ? C5 C4 C9 117.9(7) . . ? C6 C5 C4 119.8(7) . . ? C5 C6 C7 120.3(7) . . ? C6 C7 C8 121.0(7) . . ? C3 C8 C7 117.8(7) . . ? C3 C8 C10 123.7(6) . . ? C7 C8 C10 118.5(6) . . ? C12 C11 C16 120.5(6) . . ? C12 C11 C2 119.4(5) . . ? C16 C11 C2 120.0(5) . . ? C13 C12 C11 118.0(6) . . ? C13 C12 C17 120.4(6) . . ? C11 C12 C17 121.7(6) . . ? C14 C13 C12 122.4(7) . . ? C13 C14 C15 119.4(7) . . ? C14 C15 C16 120.3(6) . . ? C15 C16 C11 119.4(6) . . ? C15 C16 C18 119.5(6) . . ? C11 C16 C18 121.0(6) . . ? _refine_diff_density_max 1.319 _refine_diff_density_min -1.038 _refine_diff_density_rms 0.153 #===END data_mfl(8)-feb3800 _database_code_CSD 199539 _audit_creation_date 2000-02-29T11:25:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta3 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core2.1beta.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common (SiCl(SiMe3)(C(NSiMe3)(C6H3Me2))2) _chemical_formula_moiety 'C27 H45 Cl N2 Si4' _chemical_formula_structural 'C27 H45 Cl N2 Si4' _chemical_formula_sum 'C27 H45 Cl N2 Si4' _chemical_formula_weight 545.46 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4495(5) _cell_length_b 11.3914(6) _cell_length_c 14.9617(7) _cell_angle_alpha 73.957(3) _cell_angle_beta 71.919(2) _cell_angle_gamma 86.173(3) _cell_volume 1626.72(14) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9282 _cell_measurement_theta_min 4.529 _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 0.1 _exptl_crystal_density_diffrn 1.114 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 588 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION not applied # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_T_min 0.9457 _exptl_absorpt_correction_T_max 0.9723 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 15573 _diffrn_reflns_av_R_equivalents 0.0809 _diffrn_reflns_av_sigmaI/netI 0.0918 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 4.54 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_full 25.07 _diffrn_measured_fraction_theta_full 0.979 _diffrn_measured_fraction_theta_max 0.979 _reflns_number_total 5667 _reflns_number_gt 3953 _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 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1998)' #----------------------------------------------------------------------------# # 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 _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_number_reflns 5667 _refine_ls_number_parameters 307 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0996 _refine_ls_R_factor_gt 0.0647 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1594 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.478 _refine_diff_density_min -0.46 _refine_diff_density_rms 0.074 #----------------------------------------------------------------------------# # 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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 Si1 Si 0.31533(9) 0.18646(9) 0.22280(7) 0.0313(3) Uani 1 1 d . . . Si2 Si 0.30073(14) 0.00543(11) 0.34890(8) 0.0534(4) Uani 1 1 d . . . Si3 Si -0.06795(10) 0.13843(11) 0.17733(8) 0.0422(3) Uani 1 1 d . . . Si4 Si 0.36023(11) 0.39135(10) 0.42120(7) 0.0399(3) Uani 1 1 d . . . Cl Cl 0.51565(9) 0.21296(10) 0.13212(7) 0.0490(3) Uani 1 1 d . . . N1 N 0.0840(3) 0.1619(3) 0.1990(2) 0.0329(7) Uani 1 1 d . . . N2 N 0.3433(3) 0.3027(3) 0.3461(2) 0.0334(7) Uani 1 1 d . . . C1 C 0.1924(6) 0.0247(5) 0.4657(4) 0.0799(17) Uani 1 1 d . . . H1A H 0.2266 0.0932 0.4801 0.12 Uiso 1 1 calc R . . H1B H 0.1919 -0.0502 0.5175 0.12 Uiso 1 1 calc R . . H1C H 0.1006 0.0414 0.4623 0.12 Uiso 1 1 calc R . . C2 C 0.4735(7) -0.0236(9) 0.3615(5) 0.164(5) Uani 1 1 d . . . H2A H 0.5045 0.0465 0.3759 0.246 Uiso 1 1 calc R . . H2B H 0.5354 -0.0353 0.3004 0.246 Uiso 1 1 calc R . . H2C H 0.4712 -0.0971 0.4149 0.246 Uiso 1 1 calc R . . C3 C 0.2365(13) -0.1227(5) 0.3226(5) 0.197(6) Uani 1 1 d . . . H3A H 0.2947 -0.1336 0.2602 0.295 Uiso 1 1 calc R . . H3B H 0.1447 -0.1058 0.319 0.295 Uiso 1 1 calc R . . H3C H 0.2355 -0.1974 0.3747 0.295 Uiso 1 1 calc R . . C4 C 0.2040(3) 0.1859(3) 0.1436(2) 0.0298(8) Uani 1 1 d . . . C5 C 0.2494(3) 0.2075(3) 0.0342(2) 0.0315(8) Uani 1 1 d . . . C6 C 0.3037(4) 0.1087(3) -0.0044(3) 0.0380(9) Uani 1 1 d . . . C7 C 0.3414(4) 0.1264(4) -0.1044(3) 0.0505(11) Uani 1 1 d . . . H7 H 0.3786 0.0608 -0.1313 0.061 Uiso 1 1 calc R . . C8 C 0.3260(5) 0.2374(5) -0.1655(3) 0.0573(12) Uani 1 1 d . . . H8 H 0.3511 0.2475 -0.2339 0.069 Uiso 1 1 calc R . . C9 C 0.2745(4) 0.3340(4) -0.1280(3) 0.0477(10) Uani 1 1 d . . . H9 H 0.2653 0.4107 -0.171 0.057 Uiso 1 1 calc R . . C10 C 0.2353(4) 0.3209(4) -0.0275(3) 0.0394(9) Uani 1 1 d . . . C11 C 0.1788(5) 0.4278(4) 0.0111(3) 0.0539(11) Uani 1 1 d . . . H11A H 0.1767 0.4986 -0.0434 0.081 Uiso 0.5 1 calc PR . . H11B H 0.2354 0.4473 0.0466 0.081 Uiso 0.5 1 calc PR . . H11C H 0.0871 0.4074 0.0554 0.081 Uiso 0.5 1 calc PR . . H11D H 0.1561 0.4036 0.0825 0.081 Uiso 0.5 1 calc PR . . H11E H 0.0974 0.4549 -0.0075 0.081 Uiso 0.5 1 calc PR . . H11F H 0.2458 0.4947 -0.0163 0.081 Uiso 0.5 1 calc PR . . C12 C 0.3165(4) -0.0143(4) 0.0615(3) 0.0466(10) Uani 1 1 d . . . H12A H 0.2852 -0.0104 0.1296 0.07 Uiso 0.5 1 calc PR . . H12B H 0.411 -0.0382 0.045 0.07 Uiso 0.5 1 calc PR . . H12C H 0.2617 -0.0746 0.0531 0.07 Uiso 0.5 1 calc PR . . H12D H 0.3534 -0.0717 0.0223 0.07 Uiso 0.5 1 calc PR . . H12E H 0.2276 -0.0439 0.1068 0.07 Uiso 0.5 1 calc PR . . H12F H 0.3769 -0.0076 0.0987 0.07 Uiso 0.5 1 calc PR . . C13 C 0.2825(3) 0.3201(3) 0.2819(2) 0.0316(8) Uani 1 1 d . . . C14 C 0.1980(4) 0.4286(3) 0.2557(3) 0.0353(8) Uani 1 1 d . . . C15 C 0.2593(4) 0.5333(4) 0.1840(3) 0.0434(9) Uani 1 1 d . . . C16 C 0.1785(5) 0.6333(4) 0.1624(3) 0.0588(12) Uani 1 1 d . . . H16 H 0.2183 0.7055 0.1141 0.071 Uiso 1 1 calc R . . C17 C 0.0419(6) 0.6291(5) 0.2100(4) 0.0657(14) Uani 1 1 d . . . H17 H -0.0119 0.6974 0.1941 0.079 Uiso 1 1 calc R . . C18 C -0.0154(5) 0.5252(4) 0.2807(3) 0.0558(12) Uani 1 1 d . . . H18 H -0.1095 0.5228 0.3129 0.067 Uiso 1 1 calc R . . C19 C 0.0598(4) 0.4241(4) 0.3062(3) 0.0415(9) Uani 1 1 d . . . C20 C -0.0039(4) 0.3139(4) 0.3863(3) 0.0503(11) Uani 1 1 d . . . H20A H 0.0647 0.2523 0.3945 0.075 Uiso 0.5 1 calc PR . . H20B H -0.0743 0.28 0.3695 0.075 Uiso 0.5 1 calc PR . . H20C H -0.0436 0.3371 0.4474 0.075 Uiso 0.5 1 calc PR . . H20D H -0.1002 0.3274 0.4131 0.075 Uiso 0.5 1 calc PR . . H20E H 0.0388 0.2996 0.4381 0.075 Uiso 0.5 1 calc PR . . H20F H 0.0081 0.2425 0.3603 0.075 Uiso 0.5 1 calc PR . . C21 C 0.4079(5) 0.5404(4) 0.1315(3) 0.0588(12) Uani 1 1 d . . . H21A H 0.4489 0.4629 0.1554 0.088 Uiso 0.5 1 calc PR . . H21B H 0.4492 0.6068 0.1436 0.088 Uiso 0.5 1 calc PR . . H21C H 0.4225 0.556 0.0612 0.088 Uiso 0.5 1 calc PR . . H21D H 0.4316 0.6209 0.0847 0.088 Uiso 0.5 1 calc PR . . H21E H 0.4312 0.477 0.0965 0.088 Uiso 0.5 1 calc PR . . H21F H 0.4579 0.5278 0.1789 0.088 Uiso 0.5 1 calc PR . . C22 C 0.2775(7) 0.5416(5) 0.4094(4) 0.089(2) Uani 1 1 d . . . H22A H 0.1801 0.5296 0.4257 0.133 Uiso 1 1 calc R . . H22B H 0.3128 0.5926 0.3422 0.133 Uiso 1 1 calc R . . H22C H 0.2959 0.5822 0.4541 0.133 Uiso 1 1 calc R . . C23 C 0.2900(5) 0.2967(4) 0.5483(3) 0.0582(12) Uani 1 1 d . . . H23A H 0.1925 0.2867 0.5637 0.087 Uiso 1 1 calc R . . H23B H 0.3087 0.337 0.5931 0.087 Uiso 1 1 calc R . . H23C H 0.3317 0.2164 0.5555 0.087 Uiso 1 1 calc R . . C24 C 0.5448(5) 0.4113(6) 0.3904(4) 0.0856(18) Uani 1 1 d . . . H24A H 0.5808 0.4614 0.323 0.128 Uiso 1 1 calc R . . H24B H 0.5869 0.3311 0.3973 0.128 Uiso 1 1 calc R . . H24C H 0.5643 0.4518 0.4348 0.128 Uiso 1 1 calc R . . C25 C -0.1876(5) 0.2431(6) 0.2340(4) 0.0758(16) Uani 1 1 d . . . H25A H -0.1599 0.3278 0.1975 0.114 Uiso 1 1 calc R . . H25B H -0.1883 0.2298 0.3017 0.114 Uiso 1 1 calc R . . H25C H -0.278 0.2274 0.2328 0.114 Uiso 1 1 calc R . . C26 C -0.1147(6) -0.0233(5) 0.2437(4) 0.0767(16) Uani 1 1 d . . . H26A H -0.0494 -0.0764 0.212 0.115 Uiso 1 1 calc R . . H26B H -0.2048 -0.041 0.2429 0.115 Uiso 1 1 calc R . . H26C H -0.1148 -0.0379 0.3114 0.115 Uiso 1 1 calc R . . C27 C -0.0637(4) 0.1642(5) 0.0480(3) 0.0608(13) Uani 1 1 d . . . H27A H 0 0.1083 0.0185 0.091 Uiso 1 1 calc R . . H27B H -0.0351 0.2488 0.0118 0.091 Uiso 1 1 calc R . . H27C H -0.1537 0.1492 0.0458 0.091 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 Si1 0.0282(5) 0.0367(6) 0.0355(5) -0.0143(4) -0.0155(4) 0.0053(4) Si2 0.0731(9) 0.0477(7) 0.0428(6) -0.0123(5) -0.0276(6) 0.0255(6) Si3 0.0304(6) 0.0554(7) 0.0446(6) -0.0140(5) -0.0146(5) -0.0072(5) Si4 0.0489(7) 0.0412(7) 0.0360(6) -0.0146(5) -0.0182(5) -0.0001(5) Cl 0.0287(5) 0.0728(7) 0.0550(6) -0.0325(5) -0.0135(4) 0.0054(5) N1 0.0294(16) 0.0353(17) 0.0377(16) -0.0124(13) -0.0129(14) -0.0008(13) N2 0.0335(16) 0.0366(17) 0.0325(15) -0.0103(13) -0.0125(13) 0.0008(13) C1 0.090(4) 0.052(3) 0.064(3) -0.002(2) 0.015(3) -0.013(3) C2 0.089(5) 0.252(10) 0.073(4) 0.044(5) -0.011(3) 0.097(6) C3 0.489(19) 0.032(3) 0.109(5) 0.016(3) -0.167(9) -0.050(6) C4 0.033(2) 0.0237(18) 0.0367(19) -0.0099(15) -0.0153(16) 0.0023(14) C5 0.0245(17) 0.037(2) 0.0373(19) -0.0094(16) -0.0154(15) -0.0031(15) C6 0.036(2) 0.042(2) 0.041(2) -0.0145(17) -0.0156(17) -0.0026(17) C7 0.053(3) 0.064(3) 0.044(2) -0.027(2) -0.015(2) -0.002(2) C8 0.061(3) 0.076(3) 0.037(2) -0.014(2) -0.016(2) -0.013(2) C9 0.049(2) 0.052(3) 0.043(2) -0.0013(19) -0.0244(19) -0.008(2) C10 0.032(2) 0.046(2) 0.043(2) -0.0064(18) -0.0190(17) -0.0048(17) C11 0.069(3) 0.039(2) 0.057(3) -0.003(2) -0.033(2) 0.006(2) C12 0.055(3) 0.042(2) 0.052(2) -0.0243(19) -0.019(2) 0.0071(19) C13 0.0279(18) 0.035(2) 0.0323(18) -0.0106(15) -0.0083(15) 0.0002(15) C14 0.040(2) 0.037(2) 0.0365(19) -0.0161(16) -0.0182(17) 0.0051(16) C15 0.053(2) 0.038(2) 0.045(2) -0.0102(18) -0.0237(19) -0.0001(19) C16 0.088(4) 0.040(3) 0.060(3) -0.010(2) -0.042(3) 0.006(2) C17 0.078(4) 0.051(3) 0.087(4) -0.028(3) -0.050(3) 0.027(3) C18 0.051(3) 0.051(3) 0.074(3) -0.026(2) -0.027(2) 0.021(2) C19 0.038(2) 0.045(2) 0.050(2) -0.0224(19) -0.0201(18) 0.0109(18) C20 0.035(2) 0.063(3) 0.053(2) -0.024(2) -0.0074(19) 0.006(2) C21 0.060(3) 0.057(3) 0.051(3) -0.001(2) -0.015(2) -0.011(2) C22 0.165(6) 0.054(3) 0.088(4) -0.043(3) -0.083(4) 0.039(4) C23 0.072(3) 0.065(3) 0.040(2) -0.018(2) -0.018(2) 0.003(2) C24 0.062(3) 0.137(5) 0.074(3) -0.060(4) -0.010(3) -0.031(3) C25 0.039(3) 0.111(4) 0.102(4) -0.054(4) -0.037(3) 0.014(3) C26 0.078(4) 0.082(4) 0.070(3) -0.005(3) -0.029(3) -0.036(3) C27 0.045(2) 0.089(4) 0.053(3) -0.012(2) -0.025(2) -0.016(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 Si1 C4 1.902(3) . ? Si1 C13 1.924(4) . ? Si1 Cl 2.0997(13) . ? Si1 Si2 2.3555(15) . ? Si2 C3 1.830(7) . ? Si2 C1 1.827(5) . ? Si2 C2 1.871(7) . ? Si3 N1 1.767(3) . ? Si3 C25 1.845(5) . ? Si3 C26 1.851(5) . ? Si3 C27 1.861(4) . ? Si4 N2 1.757(3) . ? Si4 C23 1.850(4) . ? Si4 C22 1.854(5) . ? Si4 C24 1.853(5) . ? N1 C4 1.269(4) . ? N2 C13 1.274(4) . ? C4 C5 1.508(5) . ? C5 C10 1.394(5) . ? C5 C6 1.412(5) . ? C6 C7 1.383(5) . ? C6 C12 1.498(5) . ? C7 C8 1.373(6) . ? C8 C9 1.374(6) . ? C9 C10 1.398(5) . ? C10 C11 1.499(6) . ? C13 C14 1.504(5) . ? C14 C19 1.403(5) . ? C14 C15 1.398(5) . ? C15 C16 1.396(6) . ? C15 C21 1.503(6) . ? C16 C17 1.381(7) . ? C17 C18 1.373(7) . ? C18 C19 1.383(6) . ? C19 C20 1.497(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 C4 Si1 C13 113.69(15) . . ? C4 Si1 Cl 107.93(11) . . ? C13 Si1 Cl 104.77(11) . . ? C4 Si1 Si2 114.21(12) . . ? C13 Si1 Si2 107.20(11) . . ? Cl Si1 Si2 108.53(6) . . ? C3 Si2 C1 109.3(4) . . ? C3 Si2 C2 111.7(5) . . ? C1 Si2 C2 106.5(3) . . ? C3 Si2 Si1 111.3(2) . . ? C1 Si2 Si1 111.03(17) . . ? C2 Si2 Si1 107.0(3) . . ? N1 Si3 C25 104.69(18) . . ? N1 Si3 C26 104.2(2) . . ? C25 Si3 C26 111.4(3) . . ? N1 Si3 C27 117.35(17) . . ? C25 Si3 C27 109.9(2) . . ? C26 Si3 C27 109.1(2) . . ? N2 Si4 C23 106.07(18) . . ? N2 Si4 C22 117.64(18) . . ? C23 Si4 C22 108.4(2) . . ? N2 Si4 C24 103.77(19) . . ? C23 Si4 C24 110.2(3) . . ? C22 Si4 C24 110.5(3) . . ? C4 N1 Si3 133.0(2) . . ? C13 N2 Si4 132.5(3) . . ? N1 C4 C5 125.4(3) . . ? N1 C4 Si1 108.1(2) . . ? C5 C4 Si1 126.5(2) . . ? C10 C5 C6 120.5(3) . . ? C10 C5 C4 121.2(3) . . ? C6 C5 C4 118.2(3) . . ? C7 C6 C5 118.7(4) . . ? C7 C6 C12 120.4(3) . . ? C5 C6 C12 120.9(3) . . ? C8 C7 C6 121.1(4) . . ? C7 C8 C9 120.2(4) . . ? C8 C9 C10 120.9(4) . . ? C9 C10 C5 118.6(4) . . ? C9 C10 C11 119.6(4) . . ? C5 C10 C11 121.8(3) . . ? N2 C13 C14 125.4(3) . . ? N2 C13 Si1 109.7(2) . . ? C14 C13 Si1 124.9(2) . . ? C19 C14 C15 121.3(3) . . ? C19 C14 C13 119.3(3) . . ? C15 C14 C13 119.4(3) . . ? C16 C15 C14 118.1(4) . . ? C16 C15 C21 120.2(4) . . ? C14 C15 C21 121.7(4) . . ? C17 C16 C15 121.2(4) . . ? C18 C17 C16 119.4(4) . . ? C17 C18 C19 122.0(4) . . ? C18 C19 C14 118.0(4) . . ? C18 C19 C20 121.0(4) . . ? C14 C19 C20 121.0(3) . . ? #===END data_mfl(11)-jun2300 _database_code_CSD 199540 _audit_creation_date 2000-06-20T10:18:36-00:00 _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 (Si(SnMe3)(SiMe3)(C(PhMe2)NSiMe3)2) _chemical_formula_moiety 'C30 H54 N2 Si4 Sn1' _chemical_formula_structural 'C30 H54 N2 SI4 SN' _chemical_formula_sum 'C30 H54 N2 Si4 Sn' _chemical_formula_weight 673.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 17.2307(4) _cell_length_b 11.5761(3) _cell_length_c 19.7605(5) _cell_angle_alpha 90 _cell_angle_beta 109.685(2) _cell_angle_gamma 90 _cell_volume 3711.17(16) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9823 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 30.034 _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 0.15 _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.837 _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 0.845 _exptl_absorpt_correction_T_max 0.877 #----------------------------------------------------------------------------# # 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 16328 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_unetI/netI 0.0378 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.96 _diffrn_reflns_theta_max 30.03 _diffrn_reflns_theta_full 30.03 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _reflns_number_total 5415 _reflns_number_gt 4581 _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 ; The molecule lies on a 2-fold rotation axis, with unresolved disorder of the SnMe3 and SiMe3 groups about that axis. 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^)+(0.0230P)^2^+2.5319P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 5415 _refine_ls_number_parameters 176 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0378 _refine_ls_R_factor_gt 0.0293 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.458 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.05 #----------------------------------------------------------------------------# # 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' 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 0.075470(10) 0.798715(13) 0.193458(9) 0.02980(6) Uani 0.5 1 d P A 1 Si1 Si 0 0.92892(5) 0.25 0.02610(11) Uani 1 2 d S . 1 Si2 Si 0.23628(3) 0.97537(4) 0.42929(2) 0.03871(11) Uani 1 1 d . B 1 N N 0.14454(8) 0.94831(11) 0.35783(7) 0.0318(3) Uani 1 1 d . B 1 C1 C 0.16897(13) 0.88224(18) 0.17452(12) 0.0565(5) Uani 1 1 d . A 1 H1A H 0.2071 0.9125 0.2198 0.085 Uiso 1 1 calc R A 1 H1B H 0.1469 0.9463 0.1411 0.085 Uiso 1 1 calc R A 1 H1C H 0.1983 0.8284 0.1534 0.085 Uiso 1 1 calc R A 1 C2 C 0.12200(15) 0.6656(2) 0.25911(13) 0.0609(5) Uani 1 1 d . A 1 H2A H 0.0771 0.623 0.2678 0.091 Uiso 1 1 calc R A 1 H2B H 0.1601 0.6944 0.3049 0.091 Uiso 1 1 calc R A 1 H2C H 0.1516 0.6141 0.2369 0.091 Uiso 1 1 calc R A 1 C3 C -0.00286(15) 0.7352(2) 0.10094(12) 0.0634(6) Uani 1 1 d . A 1 H3A H 0.0266 0.6817 0.0798 0.095 Uiso 1 1 calc R A 1 H3B H -0.0256 0.7989 0.0674 0.095 Uiso 1 1 calc R A 1 H3C H -0.0478 0.6942 0.1105 0.095 Uiso 1 1 calc R A 1 C4 C 0.08468(8) 1.01308(12) 0.32247(7) 0.0262(3) Uani 1 1 d . B 1 C5 C 0.07881(8) 1.14049(12) 0.33526(7) 0.0262(3) Uani 1 1 d . B 1 C6 C 0.10854(9) 1.21957(13) 0.29593(8) 0.0307(3) Uani 1 1 d . B 1 C7 C 0.10263(10) 1.33703(14) 0.30766(9) 0.0396(4) Uani 1 1 d . B 1 H7 H 0.1233 1.3912 0.2818 0.047 Uiso 1 1 calc R B 1 C8 C 0.06711(11) 1.37592(14) 0.35647(10) 0.0444(4) Uani 1 1 d . B 1 H8 H 0.0628 1.4565 0.3636 0.053 Uiso 1 1 calc R B 1 C9 C 0.03783(11) 1.29815(14) 0.39501(9) 0.0400(4) Uani 1 1 d . B 1 H9 H 0.0134 1.3258 0.4284 0.048 Uiso 1 1 calc R B 1 C10 C 0.04368(9) 1.17939(13) 0.38565(8) 0.0321(3) Uani 1 1 d . B 1 C11 C 0.14872(10) 1.17745(15) 0.24347(9) 0.0386(4) Uani 1 1 d . B 1 H11A H 0.158 1.243 0.2158 0.058 Uiso 1 1 calc R B 1 H11B H 0.1126 1.1211 0.2107 0.058 Uiso 1 1 calc R B 1 H11C H 0.2016 1.1409 0.2699 0.058 Uiso 1 1 calc R B 1 C12 C 0.01337(12) 1.09665(16) 0.43018(9) 0.0436(4) Uani 1 1 d . B 1 H12A H 0.0559 1.087 0.4774 0.065 Uiso 1 1 calc R B 1 H12B H 0.0014 1.0217 0.4058 0.065 Uiso 1 1 calc R B 1 H12C H -0.0369 1.1275 0.4362 0.065 Uiso 1 1 calc R B 1 C13 C 0.27003(18) 1.1278(2) 0.44330(16) 0.0977(11) Uani 1 1 d . B 1 H13A H 0.277 1.158 0.3993 0.147 Uiso 1 1 calc R B 1 H13B H 0.3226 1.1326 0.483 0.147 Uiso 1 1 calc R B 1 H13C H 0.2284 1.1736 0.455 0.147 Uiso 1 1 calc R B 1 C14 C 0.22144(16) 0.9168(3) 0.51152(11) 0.0741(7) Uani 1 1 d . B 1 H14A H 0.1873 0.9701 0.5279 0.111 Uiso 1 1 calc R B 1 H14B H 0.2752 0.9078 0.5493 0.111 Uiso 1 1 calc R B 1 H14C H 0.194 0.8415 0.5007 0.111 Uiso 1 1 calc R B 1 C15 C 0.31686(14) 0.8922(3) 0.40711(13) 0.0754(7) Uani 1 1 d . B 1 H15A H 0.2999 0.8112 0.3985 0.113 Uiso 1 1 calc R B 1 H15B H 0.369 0.8971 0.4473 0.113 Uiso 1 1 calc R B 1 H15C H 0.3241 0.9246 0.3638 0.113 Uiso 1 1 calc R B 1 Si Si 0.075470(10) 0.798715(13) 0.193458(9) 0.02980(6) Uani 0.5 1 d P C 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 0.03575(10) 0.02449(9) 0.03444(9) 0.00103(6) 0.01875(7) 0.00442(6) Si1 0.0293(3) 0.0215(2) 0.0259(2) 0 0.0072(2) 0 Si2 0.0335(2) 0.0434(3) 0.0330(2) 0.00421(18) 0.00300(18) 0.00451(18) N 0.0332(7) 0.0299(6) 0.0309(6) 0.0021(5) 0.0088(5) 0.0021(5) C1 0.0575(12) 0.0462(11) 0.0750(14) 0.0023(10) 0.0346(11) 0.0135(9) C2 0.0659(14) 0.0590(13) 0.0667(13) 0.0032(11) 0.0343(12) -0.0030(10) C3 0.0728(15) 0.0638(13) 0.0588(13) 0.0063(11) 0.0289(11) 0.0056(11) C4 0.0279(7) 0.0268(6) 0.0252(6) 0.0011(5) 0.0105(5) -0.0021(5) C5 0.0222(6) 0.0260(6) 0.0274(6) -0.0007(5) 0.0044(5) -0.0018(5) C6 0.0242(7) 0.0306(7) 0.0334(7) 0.0027(6) 0.0047(6) -0.0031(5) C7 0.0348(8) 0.0281(7) 0.0497(9) 0.0051(7) 0.0063(7) -0.0046(6) C8 0.0432(10) 0.0273(8) 0.0533(10) -0.0070(7) 0.0041(8) -0.0002(7) C9 0.0382(9) 0.0369(8) 0.0418(9) -0.0117(7) 0.0092(7) 0.0024(7) C10 0.0292(7) 0.0351(8) 0.0297(7) -0.0035(6) 0.0070(6) -0.0022(6) C11 0.0356(8) 0.0415(9) 0.0418(8) 0.0070(7) 0.0171(7) -0.0036(7) C12 0.0514(10) 0.0474(10) 0.0388(8) -0.0050(7) 0.0242(8) -0.0046(8) C13 0.0776(18) 0.0630(15) 0.097(2) 0.0066(14) -0.0438(15) -0.0196(13) C14 0.0614(14) 0.116(2) 0.0398(10) 0.0153(12) 0.0108(10) 0.0124(14) C15 0.0462(12) 0.112(2) 0.0649(14) 0.0016(14) 0.0149(10) 0.0223(13) Si 0.03575(10) 0.02449(9) 0.03444(9) 0.00103(6) 0.01875(7) 0.00442(6) #----------------------------------------------------------------------------# # 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 C2 2.000(2) . ? Sn C3 2.010(2) . ? Sn C1 2.019(2) . ? Sn Si1 2.4880(4) . ? Si1 C4 1.9291(14) . ? Si1 C4 1.9291(14) 2 ? Si1 Sn 2.4880(4) 2 ? Si2 N 1.7571(13) . ? Si2 C13 1.849(3) . ? Si2 C14 1.856(2) . ? Si2 C15 1.859(2) . ? N C4 1.2761(18) . ? C4 C5 1.5055(19) . ? C5 C10 1.402(2) . ? C5 C6 1.405(2) . ? C6 C7 1.389(2) . ? C6 C11 1.508(2) . ? C7 C8 1.380(3) . ? C8 C9 1.380(3) . ? C9 C10 1.395(2) . ? C10 C12 1.508(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 Sn C3 107.93(10) . . ? C2 Sn C1 108.58(9) . . ? C3 Sn C1 109.86(9) . . ? C2 Sn Si1 109.36(7) . . ? C3 Sn Si1 109.72(7) . . ? C1 Sn Si1 111.32(6) . . ? C4 Si1 C4 119.33(9) . 2 ? C4 Si1 Sn 105.09(4) . . ? C4 Si1 Sn 110.59(4) 2 . ? C4 Si1 Sn 110.59(4) . 2 ? C4 Si1 Sn 105.09(4) 2 2 ? Sn Si1 Sn 105.42(2) . 2 ? N Si2 C13 116.29(9) . . ? N Si2 C14 106.64(10) . . ? C13 Si2 C14 110.29(15) . . ? N Si2 C15 105.04(9) . . ? C13 Si2 C15 107.89(16) . . ? C14 Si2 C15 110.56(12) . . ? C4 N Si2 132.66(11) . . ? N C4 C5 124.85(13) . . ? N C4 Si1 112.29(11) . . ? C5 C4 Si1 122.85(10) . . ? C10 C5 C6 120.58(13) . . ? C10 C5 C4 120.21(13) . . ? C6 C5 C4 119.21(13) . . ? C7 C6 C5 119.00(15) . . ? C7 C6 C11 120.51(14) . . ? C5 C6 C11 120.46(13) . . ? C8 C7 C6 120.70(16) . . ? C9 C8 C7 120.23(15) . . ? C8 C9 C10 120.90(16) . . ? C9 C10 C5 118.57(15) . . ? C9 C10 C12 119.60(15) . . ? C5 C10 C12 121.83(14) . . ? #===END