Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_global _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Lappert, Michael' 'Farwell, James D.' 'Hitchcock, Peter B.' _publ_contact_author_name 'Prof Michael Lappert' _publ_contact_author_address ; The Chemistry Laboratory Sussex Uni. Falmer Brighton East Sussex BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email 'M.F.LAPPERT@SUSSEX.AC.UK' _publ_section_title ; Sodium and Potassium 3-sila-B-diketiminates show new coordination modes ; data_mar1299 _database_code_CSD 174516 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; '[{Na(RNCR"Si(R)CR"NR)}2] R=SiMe3,R"=C6H3Me2 ' ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H106 N4 Na2 Si8' _chemical_formula_weight 1250.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 14.372(7) _cell_length_b 15.689(4) _cell_length_c 18.281(7) _cell_angle_alpha 90.00 _cell_angle_beta 111.69(4) _cell_angle_gamma 90.00 _cell_volume 3830(3) _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 block _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.190 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6998 _diffrn_reflns_av_R_equivalents 0.0501 _diffrn_reflns_av_sigmaI/netI 0.1242 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 24.97 _reflns_number_total 6721 _reflns_number_gt 3389 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; There are two molecules of toluene solvate, each disordered across an inversion centre and modelled as a rigid body C6 ring without H atoms. 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^)+(0.1094P)^2^+4.7594P] 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 6721 _refine_ls_number_parameters 404 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1790 _refine_ls_R_factor_gt 0.0897 _refine_ls_wR_factor_ref 0.2661 _refine_ls_wR_factor_gt 0.2152 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Na Na 0.03682(19) 0.01156(16) -0.08339(15) 0.0579(7) Uani 1 1 d . . . Si1 Si 0.18878(12) 0.01118(10) 0.09464(8) 0.0349(4) Uani 1 1 d . . . Si2 Si 0.16340(14) 0.19777(12) -0.09996(10) 0.0445(5) Uani 1 1 d . . . Si3 Si 0.19227(19) -0.14378(17) -0.11339(12) 0.0772(8) Uani 1 1 d . . . Si4 Si 0.29526(14) 0.00667(12) 0.22817(9) 0.0448(5) Uani 1 1 d . . . N1 N 0.1603(4) 0.1208(3) -0.0320(3) 0.0407(12) Uani 1 1 d . . . N2 N 0.1795(4) -0.0783(3) -0.0411(3) 0.0492(14) Uani 1 1 d . . . C1 C 0.2018(4) 0.1153(4) 0.0431(3) 0.0378(14) Uani 1 1 d . . . C2 C 0.2213(5) -0.0774(4) 0.0349(3) 0.0444(15) Uani 1 1 d . . . C3 C 0.2516(4) 0.1922(4) 0.0920(3) 0.0387(14) Uani 1 1 d . . . C4 C 0.3534(5) 0.2081(4) 0.1131(4) 0.0479(16) Uani 1 1 d . . . C5 C 0.3946(6) 0.2810(5) 0.1569(4) 0.066(2) Uani 1 1 d . . . H5 H 0.4640 0.2923 0.1708 0.079 Uiso 1 1 calc R . . C6 C 0.3373(6) 0.3372(5) 0.1806(4) 0.074(2) Uani 1 1 d . . . H6 H 0.3667 0.3863 0.2107 0.089 Uiso 1 1 calc R . . C7 C 0.2380(6) 0.3210(4) 0.1599(4) 0.0616(19) Uani 1 1 d . . . H7 H 0.1982 0.3596 0.1760 0.074 Uiso 1 1 calc R . . C8 C 0.1928(5) 0.2496(4) 0.1160(3) 0.0453(16) Uani 1 1 d . . . C9 C 0.4185(5) 0.1486(5) 0.0902(5) 0.073(2) Uani 1 1 d . . . H9A H 0.3782 0.1011 0.0601 0.110 Uiso 1 1 calc R . . H9B H 0.4713 0.1267 0.1376 0.110 Uiso 1 1 calc R . . H9C H 0.4489 0.1790 0.0577 0.110 Uiso 1 1 calc R . . C10 C 0.0823(5) 0.2359(5) 0.0945(4) 0.062(2) Uani 1 1 d . . . H10A H 0.0628 0.2551 0.1378 0.094 Uiso 1 1 calc R . . H10B H 0.0669 0.1751 0.0847 0.094 Uiso 1 1 calc R . . H10C H 0.0452 0.2684 0.0468 0.094 Uiso 1 1 calc R . . C11 C 0.2883(5) -0.1498(4) 0.0797(3) 0.0440(15) Uani 1 1 d . . . C12 C 0.2471(5) -0.2158(4) 0.1077(4) 0.0522(17) Uani 1 1 d . . . C13 C 0.3090(7) -0.2836(5) 0.1471(4) 0.070(2) Uani 1 1 d . . . H13 H 0.2819 -0.3297 0.1665 0.084 Uiso 1 1 calc R . . C14 C 0.4093(7) -0.2835(6) 0.1577(5) 0.083(3) Uani 1 1 d . . . H14 H 0.4508 -0.3297 0.1841 0.100 Uiso 1 1 calc R . . C15 C 0.4488(6) -0.2172(6) 0.1303(5) 0.074(2) Uani 1 1 d . . . H15 H 0.5180 -0.2175 0.1383 0.089 Uiso 1 1 calc R . . C16 C 0.3895(6) -0.1495(4) 0.0910(4) 0.0551(18) Uani 1 1 d . . . C17 C 0.1384(6) -0.2194(5) 0.0964(5) 0.077(2) Uani 1 1 d . . . H17A H 0.1025 -0.2553 0.0509 0.115 Uiso 1 1 calc R . . H17B H 0.1103 -0.1617 0.0875 0.115 Uiso 1 1 calc R . . H17C H 0.1315 -0.2434 0.1436 0.115 Uiso 1 1 calc R . . C18 C 0.4379(6) -0.0775(5) 0.0636(5) 0.070(2) Uani 1 1 d . . . H18A H 0.3861 -0.0386 0.0305 0.105 Uiso 1 1 calc R . . H18B H 0.4757 -0.1005 0.0331 0.105 Uiso 1 1 calc R . . H18C H 0.4834 -0.0465 0.1094 0.105 Uiso 1 1 calc R . . C19 C 0.2846(5) 0.1902(5) -0.1142(4) 0.074(2) Uani 1 1 d . . . H19A H 0.3369 0.2187 -0.0705 0.111 Uiso 1 1 calc R . . H19B H 0.2784 0.2177 -0.1639 0.111 Uiso 1 1 calc R . . H19C H 0.3024 0.1301 -0.1157 0.111 Uiso 1 1 calc R . . C20 C 0.1367(6) 0.3092(4) -0.0791(4) 0.069(2) Uani 1 1 d . . . H20A H 0.0730 0.3111 -0.0711 0.103 Uiso 1 1 calc R . . H20B H 0.1324 0.3457 -0.1238 0.103 Uiso 1 1 calc R . . H20C H 0.1906 0.3296 -0.0316 0.103 Uiso 1 1 calc R . . C21 C 0.0634(5) 0.1623(5) -0.1935(3) 0.0590(19) Uani 1 1 d . . . H21A H 0.0772 0.1038 -0.2055 0.089 Uiso 1 1 calc R . . H21B H 0.0622 0.2002 -0.2365 0.089 Uiso 1 1 calc R . . H21C H -0.0016 0.1643 -0.1876 0.089 Uiso 1 1 calc R . . C22 C 0.2948(8) -0.1049(14) -0.1414(7) 0.257(12) Uani 1 1 d . . . H22A H 0.3042 -0.0437 -0.1304 0.386 Uiso 1 1 calc R . . H22B H 0.2784 -0.1149 -0.1977 0.386 Uiso 1 1 calc R . . H22C H 0.3566 -0.1353 -0.1110 0.386 Uiso 1 1 calc R . . C23 C 0.1930(12) -0.2603(7) -0.0899(6) 0.187(7) Uani 1 1 d . . . H23A H 0.2617 -0.2821 -0.0726 0.280 Uiso 1 1 calc R . . H23B H 0.1508 -0.2914 -0.1369 0.280 Uiso 1 1 calc R . . H23C H 0.1670 -0.2683 -0.0478 0.280 Uiso 1 1 calc R . . C24 C 0.0785(6) -0.1278(5) -0.2006(4) 0.082(3) Uani 1 1 d . . . H24A H 0.0196 -0.1362 -0.1866 0.123 Uiso 1 1 calc R . . H24B H 0.0771 -0.1689 -0.2414 0.123 Uiso 1 1 calc R . . H24C H 0.0780 -0.0698 -0.2206 0.123 Uiso 1 1 calc R . . C25 C 0.2798(7) 0.1074(5) 0.2767(4) 0.084(3) Uani 1 1 d . . . H25A H 0.2084 0.1189 0.2632 0.126 Uiso 1 1 calc R . . H25B H 0.3102 0.1547 0.2585 0.126 Uiso 1 1 calc R . . H25C H 0.3127 0.1016 0.3339 0.126 Uiso 1 1 calc R . . C26 C 0.4323(5) -0.0073(5) 0.2556(4) 0.077(2) Uani 1 1 d . . . H26A H 0.4655 -0.0044 0.3130 0.115 Uiso 1 1 calc R . . H26B H 0.4581 0.0381 0.2315 0.115 Uiso 1 1 calc R . . H26C H 0.4455 -0.0628 0.2369 0.115 Uiso 1 1 calc R . . C27 C 0.2557(8) -0.0841(6) 0.2745(4) 0.111(4) Uani 1 1 d . . . H27A H 0.2748 -0.1377 0.2564 0.166 Uiso 1 1 calc R . . H27B H 0.1828 -0.0825 0.2598 0.166 Uiso 1 1 calc R . . H27C H 0.2884 -0.0801 0.3319 0.166 Uiso 1 1 calc R . . C28 C 0.5658(14) 0.0065(17) 0.4949(15) 0.17(2) Uani 0.50 1 d PG . . C29 C 0.5216(16) 0.0836(15) 0.5012(13) 0.104(11) Uani 0.50 1 d PG . . C30 C 0.4298(17) 0.0843(18) 0.5104(12) 0.41(6) Uani 0.50 1 d PG . . C31 C 0.3822(14) 0.008(2) 0.5132(11) 0.266(14) Uani 1 1 d G . . C32 C 0.4264(18) -0.0691(18) 0.5069(12) 0.44(8) Uani 0.50 1 d PG . . C33 C 0.5182(19) -0.0698(15) 0.4978(15) 0.25(3) Uani 0.50 1 d PG . . C34 C -0.071(3) 0.477(3) -0.0531(19) 0.53(11) Uani 0.50 1 d PG . . C35 C 0.024(3) 0.510(3) -0.0388(13) 0.37(6) Uani 0.50 1 d PG . . C36 C 0.090(2) 0.5241(19) 0.0381(16) 0.20(3) Uani 0.50 1 d PG . . C37 C 0.060(3) 0.5048(18) 0.1007(12) 0.29(5) Uani 0.50 1 d PG . . C38 C -0.035(3) 0.4718(16) 0.086(2) 0.32(2) Uani 1 1 d G . . C39 C -0.100(3) 0.458(2) 0.009(3) 0.34(7) Uani 0.50 1 d PG . . 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 Na 0.0494(15) 0.0510(15) 0.0598(16) 0.0020(13) 0.0044(12) 0.0008(13) Si1 0.0383(9) 0.0413(9) 0.0238(8) 0.0010(7) 0.0101(7) 0.0008(8) Si2 0.0528(11) 0.0481(11) 0.0366(9) 0.0118(8) 0.0211(8) 0.0018(9) Si3 0.0892(17) 0.0981(18) 0.0364(11) -0.0239(11) 0.0141(11) 0.0271(14) Si4 0.0527(11) 0.0497(11) 0.0260(8) -0.0007(8) 0.0075(7) 0.0020(9) N1 0.042(3) 0.050(3) 0.030(3) 0.007(2) 0.013(2) -0.002(2) N2 0.053(3) 0.063(4) 0.030(3) -0.006(2) 0.014(2) 0.009(3) C1 0.031(3) 0.047(4) 0.037(3) 0.009(3) 0.016(3) 0.006(3) C2 0.052(4) 0.049(4) 0.032(3) -0.003(3) 0.015(3) -0.002(3) C3 0.043(4) 0.045(4) 0.027(3) 0.003(3) 0.011(3) 0.000(3) C4 0.041(4) 0.056(4) 0.048(4) 0.006(3) 0.017(3) -0.002(3) C5 0.048(4) 0.075(5) 0.063(5) 0.009(4) 0.008(4) -0.014(4) C6 0.075(6) 0.073(6) 0.064(5) -0.013(4) 0.015(4) -0.020(5) C7 0.081(6) 0.055(4) 0.051(4) -0.009(4) 0.027(4) -0.002(4) C8 0.047(4) 0.053(4) 0.037(3) -0.009(3) 0.016(3) -0.003(3) C9 0.046(4) 0.091(6) 0.083(6) 0.015(5) 0.024(4) 0.006(4) C10 0.062(5) 0.070(5) 0.070(5) -0.016(4) 0.040(4) -0.003(4) C11 0.050(4) 0.049(4) 0.030(3) -0.010(3) 0.011(3) 0.002(3) C12 0.061(5) 0.048(4) 0.037(4) 0.001(3) 0.006(3) 0.006(4) C13 0.087(6) 0.059(5) 0.057(5) 0.005(4) 0.018(4) 0.011(5) C14 0.085(7) 0.067(6) 0.075(6) -0.003(5) 0.003(5) 0.027(5) C15 0.062(5) 0.073(6) 0.078(6) -0.007(5) 0.015(4) 0.020(5) C16 0.064(5) 0.054(4) 0.045(4) -0.014(3) 0.017(3) 0.013(4) C17 0.073(6) 0.075(6) 0.077(6) 0.014(4) 0.022(4) -0.005(5) C18 0.055(5) 0.072(5) 0.090(6) -0.017(4) 0.036(4) 0.001(4) C19 0.069(5) 0.093(6) 0.078(5) 0.029(5) 0.047(4) 0.009(5) C20 0.089(6) 0.054(4) 0.068(5) 0.010(4) 0.034(4) -0.007(4) C21 0.069(5) 0.068(5) 0.038(4) 0.012(3) 0.017(3) 0.010(4) C22 0.072(7) 0.60(3) 0.122(10) -0.205(16) 0.059(7) -0.079(13) C23 0.303(19) 0.125(10) 0.087(8) -0.030(7) 0.017(10) 0.121(11) C24 0.100(6) 0.102(6) 0.041(4) -0.020(4) 0.023(4) -0.044(6) C25 0.116(7) 0.091(6) 0.035(4) -0.011(4) 0.017(4) 0.034(5) C26 0.063(5) 0.104(7) 0.043(4) -0.003(4) -0.005(3) 0.010(5) C27 0.136(9) 0.130(8) 0.041(5) 0.023(5) 0.003(5) -0.063(7) C28 0.069(16) 0.37(6) 0.033(12) -0.04(2) -0.015(9) 0.10(3) C29 0.103(19) 0.13(3) 0.053(16) -0.019(16) -0.003(13) 0.056(19) C30 0.46(8) 0.60(10) 0.049(18) -0.06(3) -0.06(3) 0.50(9) C31 0.41(4) 0.26(3) 0.075(12) 0.028(18) 0.021(18) 0.00(4) C32 0.72(15) 0.25(5) 0.12(3) 0.11(4) -0.13(6) -0.39(8) C33 0.42(7) 0.12(3) 0.056(18) 0.034(17) -0.07(3) -0.21(4) C34 0.16(4) 0.07(3) 1.4(3) -0.07(10) 0.32(12) -0.01(3) C35 0.64(12) 0.25(6) 0.47(10) 0.32(7) 0.48(10) 0.38(8) C36 0.37(7) 0.08(2) 0.044(12) 0.000(13) -0.04(2) 0.11(3) C37 0.48(10) 0.11(4) 0.11(3) -0.01(2) -0.08(4) 0.15(5) C38 0.39(6) 0.079(19) 0.44(7) -0.03(2) 0.08(5) 0.10(3) C39 0.15(4) 0.10(3) 0.65(18) 0.02(8) 0.01(8) 0.04(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 Na N2 2.370(6) . ? Na N1 2.395(6) . ? Na C2 3.068(7) . ? Na Si1 3.179(3) . ? Na Si1 3.192(4) 3 ? Si1 C2 1.928(6) . ? Si1 C1 1.929(6) . ? Si1 Si4 2.355(2) . ? Si2 N1 1.744(5) . ? Si2 C19 1.858(7) . ? Si2 C20 1.860(7) . ? Si2 C21 1.866(7) . ? Si3 N2 1.736(5) . ? Si3 C24 1.831(8) . ? Si3 C22 1.834(12) . ? Si3 C23 1.878(12) . ? Si4 C27 1.851(8) . ? Si4 C26 1.856(8) . ? Si4 C25 1.866(7) . ? N1 C1 1.282(7) . ? N2 C2 1.295(7) . ? C1 C3 1.513(8) . ? C2 C11 1.519(9) . ? C3 C4 1.391(8) . ? C3 C8 1.412(8) . ? C4 C5 1.396(10) . ? C4 C9 1.488(9) . ? C5 C6 1.381(10) . ? C6 C7 1.358(10) . ? C7 C8 1.391(9) . ? C8 C10 1.503(9) . ? C11 C12 1.383(9) . ? C11 C16 1.392(9) . ? C12 C13 1.402(10) . ? C12 C17 1.499(10) . ? C13 C14 1.381(11) . ? C14 C15 1.367(11) . ? C15 C16 1.385(10) . ? C16 C18 1.506(10) . ? C28 C31 0.85(3) 3_656 ? C28 C32 0.99(6) 3_656 ? C28 C29 1.3900 . ? C28 C33 1.3900 . ? C28 C30 1.43(5) 3_656 ? C28 C33 1.61(3) 3_656 ? C28 C29 1.91(6) 3_656 ? C28 C28 1.98(4) 3_656 ? C29 C33 0.62(5) 3_656 ? C29 C32 0.85(4) 3_656 ? C29 C30 1.3900 . ? C29 C28 1.91(5) 3_656 ? C30 C33 0.85(3) 3_656 ? C30 C31 1.3900 . ? C30 C28 1.43(4) 3_656 ? C31 C28 0.85(3) 3_656 ? C31 C32 1.3900 . ? C31 C33 1.80(5) 3_656 ? C32 C29 0.85(6) 3_656 ? C32 C28 0.99(5) 3_656 ? C32 C33 1.3900 . ? C33 C29 0.62(6) 3_656 ? C33 C30 0.85(5) 3_656 ? C33 C28 1.61(3) 3_656 ? C33 C31 1.80(6) 3_656 ? C34 C36 0.45(9) 3_565 ? C34 C37 0.98(8) 3_565 ? C34 C35 1.3900 . ? C34 C39 1.3900 . ? C34 C35 1.57(6) 3_565 ? C34 C38 2.00(9) 3_565 ? C35 C38 0.98(5) 3_565 ? C35 C39 1.14(7) 3_565 ? C35 C37 1.34(6) 3_565 ? C35 C36 1.3900 . ? C35 C34 1.57(5) 3_565 ? C35 C36 1.72(7) 3_565 ? C35 C35 1.82(6) 3_565 ? C36 C34 0.45(6) 3_565 ? C36 C39 0.98(6) 3_565 ? C36 C37 1.3900 . ? C36 C35 1.72(7) 3_565 ? C37 C34 0.98(5) 3_565 ? C37 C35 1.34(7) 3_565 ? C37 C38 1.3900 . ? C38 C35 0.98(5) 3_565 ? C38 C39 1.3900 . ? C38 C34 2.00(6) 3_565 ? C39 C36 0.98(9) 3_565 ? C39 C35 1.14(7) 3_565 ? 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 Na N1 82.6(2) . . ? N2 Na C2 23.33(15) . . ? N1 Na C2 74.18(18) . . ? N2 Na Si1 58.74(13) . . ? N1 Na Si1 58.06(12) . . ? C2 Na Si1 35.90(12) . . ? N2 Na Si1 133.65(17) . 3 ? N1 Na Si1 133.86(16) . 3 ? C2 Na Si1 125.94(15) . 3 ? Si1 Na Si1 111.28(10) . 3 ? C2 Si1 C1 104.3(3) . . ? C2 Si1 Si4 111.4(2) . . ? C1 Si1 Si4 112.87(19) . . ? C2 Si1 Na 68.90(19) . . ? C1 Si1 Na 69.66(18) . . ? Si4 Si1 Na 177.03(10) . . ? N1 Si2 C19 109.1(3) . . ? N1 Si2 C20 116.3(3) . . ? C19 Si2 C20 111.4(4) . . ? N1 Si2 C21 103.4(3) . . ? C19 Si2 C21 107.3(3) . . ? C20 Si2 C21 108.7(3) . . ? N2 Si3 C24 105.7(3) . . ? N2 Si3 C22 109.7(5) . . ? C24 Si3 C22 105.2(5) . . ? N2 Si3 C23 113.3(4) . . ? C24 Si3 C23 105.1(5) . . ? C22 Si3 C23 116.8(8) . . ? C27 Si4 C26 105.1(4) . . ? C27 Si4 C25 108.9(4) . . ? C26 Si4 C25 105.8(4) . . ? C27 Si4 Si1 107.8(3) . . ? C26 Si4 Si1 120.1(2) . . ? C25 Si4 Si1 108.8(2) . . ? C1 N1 Si2 133.2(4) . . ? C1 N1 Na 110.8(4) . . ? Si2 N1 Na 115.2(2) . . ? C2 N2 Si3 133.3(5) . . ? C2 N2 Na 110.2(4) . . ? Si3 N2 Na 115.2(3) . . ? N1 C1 C3 120.7(5) . . ? N1 C1 Si1 119.3(5) . . ? C3 C1 Si1 119.7(4) . . ? N2 C2 C11 121.4(5) . . ? N2 C2 Si1 120.2(5) . . ? C11 C2 Si1 118.1(4) . . ? N2 C2 Na 46.5(3) . . ? C11 C2 Na 158.6(4) . . ? Si1 C2 Na 75.2(2) . . ? C4 C3 C8 119.2(6) . . ? C4 C3 C1 121.8(5) . . ? C8 C3 C1 119.0(5) . . ? C3 C4 C5 119.2(6) . . ? C3 C4 C9 121.0(6) . . ? C5 C4 C9 119.8(6) . . ? C6 C5 C4 121.7(7) . . ? C7 C6 C5 118.7(7) . . ? C6 C7 C8 122.0(7) . . ? C7 C8 C3 119.2(6) . . ? C7 C8 C10 119.3(6) . . ? C3 C8 C10 121.5(6) . . ? C12 C11 C16 121.0(6) . . ? C12 C11 C2 119.2(6) . . ? C16 C11 C2 119.9(6) . . ? C11 C12 C13 118.8(7) . . ? C11 C12 C17 123.0(6) . . ? C13 C12 C17 118.3(7) . . ? C14 C13 C12 120.1(8) . . ? C15 C14 C13 120.2(8) . . ? C14 C15 C16 120.9(8) . . ? C15 C16 C11 118.9(7) . . ? C15 C16 C18 118.4(7) . . ? C11 C16 C18 122.6(6) . . ? C31 C28 C32 98(5) 3_656 3_656 ? C31 C28 C29 135(5) 3_656 . ? C32 C28 C29 37(2) 3_656 . ? C31 C28 C33 105(5) 3_656 . ? C32 C28 C33 157(2) 3_656 . ? C29 C28 C33 120.0 . . ? C31 C28 C30 70(3) 3_656 3_656 ? C32 C28 C30 168(4) 3_656 3_656 ? C29 C28 C30 155(2) . 3_656 ? C33 C28 C30 35(2) . 3_656 ? C31 C28 C33 157(6) 3_656 3_656 ? C32 C28 C33 59.2(16) 3_656 3_656 ? C29 C28 C33 22.3(19) . 3_656 ? C33 C28 C33 97.7(19) . 3_656 ? C30 C28 C33 132(3) 3_656 3_656 ? C31 C28 C29 116(4) 3_656 3_656 ? C32 C28 C29 145(3) 3_656 3_656 ? C29 C28 C29 108.3(15) . 3_656 ? C33 C28 C29 11.8(15) . 3_656 ? C30 C28 C29 46.5(17) 3_656 3_656 ? C33 C28 C29 86.0(19) 3_656 3_656 ? C31 C28 C28 158(6) 3_656 3_656 ? C32 C28 C28 103(2) 3_656 3_656 ? C29 C28 C28 66.4(13) . 3_656 ? C33 C28 C28 53.6(13) . 3_656 ? C30 C28 C28 88(3) 3_656 3_656 ? C33 C28 C28 44.1(11) 3_656 3_656 ? C29 C28 C28 41.8(15) 3_656 3_656 ? C33 C29 C32 143(7) 3_656 3_656 ? C33 C29 C30 21(4) 3_656 . ? C32 C29 C30 165(4) 3_656 . ? C33 C29 C28 99(4) 3_656 . ? C32 C29 C28 45(4) 3_656 . ? C30 C29 C28 120.0 . . ? C33 C29 C28 27(3) 3_656 3_656 ? C32 C29 C28 116(4) 3_656 3_656 ? C30 C29 C28 48.3(9) . 3_656 ? C28 C29 C28 71.7(9) . 3_656 ? C33 C30 C29 15(4) 3_656 . ? C33 C30 C31 105(4) 3_656 . ? C29 C30 C31 120.0 . . ? C33 C30 C28 70(3) 3_656 3_656 ? C29 C30 C28 85.2(16) . 3_656 ? C31 C30 C28 34.8(16) . 3_656 ? C28 C31 C30 75(3) 3_656 . ? C28 C31 C32 45(3) 3_656 . ? C30 C31 C32 120.0 . . ? C28 C31 C33 48(3) 3_656 3_656 ? C30 C31 C33 27.0(11) . 3_656 ? C32 C31 C33 93.1(11) . 3_656 ? C29 C32 C28 98(5) 3_656 3_656 ? C29 C32 C33 15(3) 3_656 . ? C28 C32 C33 83(2) 3_656 . ? C29 C32 C31 135(3) 3_656 . ? C28 C32 C31 37(2) 3_656 . ? C33 C32 C31 120.0 . . ? C29 C33 C30 143(7) 3_656 3_656 ? C29 C33 C32 21(4) 3_656 . ? C30 C33 C32 165(4) 3_656 . ? C29 C33 C28 141(4) 3_656 . ? C30 C33 C28 75(4) 3_656 . ? C32 C33 C28 120.0 . . ? C29 C33 C28 59(3) 3_656 3_656 ? C30 C33 C28 157(6) 3_656 3_656 ? C32 C33 C28 37.7(19) . 3_656 ? C28 C33 C28 82.3(18) . 3_656 ? C29 C33 C31 167(5) 3_656 3_656 ? C30 C33 C31 48(3) 3_656 3_656 ? C32 C33 C31 146.9(15) . 3_656 ? C28 C33 C31 27.0(15) . 3_656 ? C28 C33 C31 109(3) 3_656 3_656 ? C36 C34 C37 152(10) 3_565 3_565 ? C36 C34 C35 132(8) 3_565 . ? C37 C34 C35 66(5) 3_565 . ? C36 C34 C39 19(9) 3_565 . ? C37 C34 C39 171(6) 3_565 . ? C35 C34 C39 120.0 . . ? C36 C34 C35 58(6) 3_565 3_565 ? C37 C34 C35 140(6) 3_565 3_565 ? C35 C34 C35 75(2) . 3_565 ? C39 C34 C35 45(2) . 3_565 ? C36 C34 C38 154(10) 3_565 3_565 ? C37 C34 C38 40(3) 3_565 3_565 ? C35 C34 C38 27(2) . 3_565 ? C39 C34 C38 146(2) . 3_565 ? C35 C34 C38 102(3) 3_565 3_565 ? C38 C35 C39 82(5) 3_565 3_565 ? C38 C35 C37 72(3) 3_565 3_565 ? C39 C35 C37 153(5) 3_565 3_565 ? C38 C35 C34 114(6) 3_565 . ? C39 C35 C34 163(4) 3_565 . ? C37 C35 C34 42(4) 3_565 . ? C38 C35 C36 126(6) 3_565 . ? C39 C35 C36 44(3) 3_565 . ? C37 C35 C36 161(4) 3_565 . ? C34 C35 C36 120.0 . . ? C38 C35 C34 140(8) 3_565 3_565 ? C39 C35 C34 59(3) 3_565 3_565 ? C37 C35 C34 145(6) 3_565 3_565 ? C34 C35 C34 105(2) . 3_565 ? C36 C35 C34 16(2) . 3_565 ? C38 C35 C36 124(5) 3_565 3_565 ? C39 C35 C36 152(4) 3_565 3_565 ? C37 C35 C36 52(3) 3_565 3_565 ? C34 C35 C36 11(3) . 3_565 ? C36 C35 C36 109(3) . 3_565 ? C34 C35 C36 94(4) 3_565 3_565 ? C38 C35 C35 166(7) 3_565 3_565 ? C39 C35 C35 107(3) 3_565 3_565 ? C37 C35 C35 98(4) 3_565 3_565 ? C34 C35 C35 57(2) . 3_565 ? C36 C35 C35 63(2) . 3_565 ? C34 C35 C35 48(2) 3_565 3_565 ? C36 C35 C35 46.1(17) 3_565 3_565 ? C34 C36 C39 152(10) 3_565 3_565 ? C34 C36 C35 106(6) 3_565 . ? C39 C36 C35 54(4) 3_565 . ? C34 C36 C37 19(6) 3_565 . ? C39 C36 C37 171(5) 3_565 . ? C35 C36 C37 120.0 . . ? C34 C36 C35 37(6) 3_565 3_565 ? C39 C36 C35 124(4) 3_565 3_565 ? C35 C36 C35 71(2) . 3_565 ? C37 C36 C35 49(2) . 3_565 ? C34 C37 C35 72(3) 3_565 3_565 ? C34 C37 C38 114(3) 3_565 . ? C35 C37 C38 42(2) 3_565 . ? C34 C37 C36 9(4) 3_565 . ? C35 C37 C36 78(2) 3_565 . ? C38 C37 C36 120.0 . . ? C35 C38 C37 66(4) 3_565 . ? C35 C38 C39 54(4) 3_565 . ? C37 C38 C39 120.0 . . ? C35 C38 C34 40(3) 3_565 3_565 ? C37 C38 C34 26.6(13) . 3_565 ? C39 C38 C34 93.6(13) . 3_565 ? C36 C39 C35 82(5) 3_565 3_565 ? C36 C39 C38 126(3) 3_565 . ? C35 C39 C38 44(3) 3_565 . ? C36 C39 C34 9(4) 3_565 . ? C35 C39 C34 76(3) 3_565 . ? C38 C39 C34 120.0 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.229 _refine_diff_density_min -0.525 _refine_diff_density_rms 0.073 data_jan1199 _database_code_CSD 174517 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[{K(Si(SiMe3)(C(C6H3Me2)NSiMe3)2)}2]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C54 H90 K2 N4 Si8' _chemical_formula_weight 1098.22 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' 'K' 'K' 0.2009 0.2494 '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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 10.539(5) _cell_length_b 22.920(9) _cell_length_c 13.200(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.26(4) _cell_angle_gamma 90.00 _cell_volume 3183(2) _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 block _exptl_crystal_colour orange _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1184 _exptl_absorpt_coefficient_mu 0.335 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.85 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4685 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.1062 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 22.99 _reflns_number_total 4418 _reflns_number_gt 2808 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Methyl H atoms included as AFIX 137 (torsion angle refined). 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^)+(0.0596P)^2^+0.5782P] 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 4418 _refine_ls_number_parameters 320 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1103 _refine_ls_R_factor_gt 0.0602 _refine_ls_wR_factor_ref 0.1528 _refine_ls_wR_factor_gt 0.1302 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _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 K K 0.13058(13) 0.07757(5) 0.05080(9) 0.0357(4) Uani 1 1 d . . . Si1 Si 0.08772(14) -0.05429(6) 0.14426(10) 0.0195(4) Uani 1 1 d . . . Si2 Si 0.37676(14) 0.06672(6) 0.28987(11) 0.0248(4) Uani 1 1 d . . . Si3 Si -0.11459(15) -0.22404(6) 0.09611(11) 0.0281(4) Uani 1 1 d . . . Si4 Si -0.08188(15) -0.02441(7) 0.23915(11) 0.0278(4) Uani 1 1 d . . . N1 N 0.2581(4) 0.02618(18) 0.2261(3) 0.0220(10) Uani 1 1 d . . . N2 N -0.0495(4) -0.15467(18) 0.1102(3) 0.0245(11) Uani 1 1 d . . . C1 C 0.2400(5) -0.0300(2) 0.2166(3) 0.0195(12) Uani 1 1 d . . . C2 C 0.0658(5) -0.1363(2) 0.1283(3) 0.0181(12) Uani 1 1 d . . . C3 C 0.3386(4) -0.0717(2) 0.2579(3) 0.0177(11) Uani 1 1 d . . . C4 C 0.4360(5) -0.0901(2) 0.1973(4) 0.0250(13) Uani 1 1 d . . . C5 C 0.5286(5) -0.1276(2) 0.2376(4) 0.0315(14) Uani 1 1 d . . . H5 H 0.5942 -0.1403 0.1964 0.038 Uiso 1 1 calc R . . C6 C 0.5273(6) -0.1466(2) 0.3364(4) 0.0356(15) Uani 1 1 d . . . H6 H 0.5927 -0.1716 0.3636 0.043 Uiso 1 1 calc R . . C7 C 0.4306(5) -0.1293(2) 0.3956(4) 0.0319(14) Uani 1 1 d . . . H7 H 0.4285 -0.1436 0.4630 0.038 Uiso 1 1 calc R . . C8 C 0.3362(5) -0.0914(2) 0.3584(4) 0.0240(13) Uani 1 1 d . . . C9 C 0.4428(5) -0.0668(2) 0.0903(4) 0.0293(13) Uani 1 1 d . . . H9A H 0.4980 -0.0920 0.0521 0.044 Uiso 1 1 calc R . . H9B H 0.4775 -0.0272 0.0928 0.044 Uiso 1 1 calc R . . H9C H 0.3574 -0.0662 0.0569 0.044 Uiso 1 1 calc R . . C10 C 0.2351(5) -0.0706(2) 0.4269(4) 0.0337(14) Uani 1 1 d . . . H10A H 0.1560 -0.0632 0.3863 0.051 Uiso 1 1 calc R . . H10B H 0.2635 -0.0345 0.4609 0.051 Uiso 1 1 calc R . . H10C H 0.2204 -0.1006 0.4778 0.051 Uiso 1 1 calc R . . C11 C 0.1780(5) -0.1766(2) 0.1242(4) 0.0227(12) Uani 1 1 d . . . C12 C 0.2412(5) -0.1826(2) 0.0332(4) 0.0263(13) Uani 1 1 d . . . C13 C 0.3440(5) -0.2196(2) 0.0315(4) 0.0328(14) Uani 1 1 d . . . H13 H 0.3863 -0.2242 -0.0297 0.039 Uiso 1 1 calc R . . C14 C 0.3870(6) -0.2501(3) 0.1163(4) 0.0381(15) Uani 1 1 d . . . H14 H 0.4595 -0.2746 0.1141 0.046 Uiso 1 1 calc R . . C15 C 0.3238(6) -0.2449(2) 0.2046(4) 0.0361(15) Uani 1 1 d . . . H15 H 0.3526 -0.2665 0.2629 0.043 Uiso 1 1 calc R . . C16 C 0.2192(5) -0.2085(2) 0.2097(4) 0.0254(13) Uani 1 1 d . . . C17 C 0.1926(6) -0.1514(2) -0.0622(4) 0.0326(14) Uani 1 1 d . . . H17A H 0.1140 -0.1700 -0.0890 0.049 Uiso 1 1 calc R . . H17B H 0.2567 -0.1536 -0.1131 0.049 Uiso 1 1 calc R . . H17C H 0.1758 -0.1105 -0.0465 0.049 Uiso 1 1 calc R . . C18 C 0.1495(5) -0.2047(2) 0.3060(4) 0.0322(14) Uani 1 1 d . . . H18A H 0.0813 -0.2338 0.3043 0.048 Uiso 1 1 calc R . . H18B H 0.1131 -0.1656 0.3119 0.048 Uiso 1 1 calc R . . H18C H 0.2089 -0.2122 0.3644 0.048 Uiso 1 1 calc R . . C19 C 0.2962(6) 0.1092(3) 0.3880(4) 0.0447(17) Uani 1 1 d . . . H19A H 0.2731 0.0830 0.4426 0.067 Uiso 1 1 calc R . . H19B H 0.2194 0.1275 0.3571 0.067 Uiso 1 1 calc R . . H19C H 0.3540 0.1395 0.4158 0.067 Uiso 1 1 calc R . . C20 C 0.4384(6) 0.1169(3) 0.1939(5) 0.0493(18) Uani 1 1 d . . . H20A H 0.3702 0.1430 0.1685 0.074 Uiso 1 1 calc R . . H20B H 0.4691 0.0941 0.1374 0.074 Uiso 1 1 calc R . . H20C H 0.5085 0.1400 0.2250 0.074 Uiso 1 1 calc R . . C21 C 0.5168(5) 0.0295(3) 0.3527(4) 0.0372(15) Uani 1 1 d . . . H21A H 0.5551 0.0035 0.3040 0.056 Uiso 1 1 calc R . . H21B H 0.4897 0.0066 0.4104 0.056 Uiso 1 1 calc R . . H21C H 0.5793 0.0587 0.3768 0.056 Uiso 1 1 calc R . . C22 C -0.2472(6) -0.2163(3) -0.0030(5) 0.0490(18) Uani 1 1 d . . . H22A H -0.2121 -0.2087 -0.0689 0.074 Uiso 1 1 calc R . . H22B H -0.3020 -0.1837 0.0146 0.074 Uiso 1 1 calc R . . H22C H -0.2971 -0.2524 -0.0068 0.074 Uiso 1 1 calc R . . C23 C -0.1876(6) -0.2426(2) 0.2177(4) 0.0394(16) Uani 1 1 d . . . H23A H -0.2160 -0.2068 0.2500 0.059 Uiso 1 1 calc R . . H23B H -0.1246 -0.2624 0.2632 0.059 Uiso 1 1 calc R . . H23C H -0.2606 -0.2685 0.2038 0.059 Uiso 1 1 calc R . . C24 C -0.0090(6) -0.2844(2) 0.0586(5) 0.0454(17) Uani 1 1 d . . . H24A H 0.0483 -0.2953 0.1166 0.068 Uiso 1 1 calc R . . H24B H 0.0412 -0.2714 0.0025 0.068 Uiso 1 1 calc R . . H24C H -0.0607 -0.3181 0.0370 0.068 Uiso 1 1 calc R . . C25 C -0.1276(6) -0.0745(3) 0.3437(4) 0.0435(16) Uani 1 1 d . . . H25A H -0.2079 -0.0612 0.3700 0.065 Uiso 1 1 calc R . . H25B H -0.0609 -0.0741 0.3986 0.065 Uiso 1 1 calc R . . H25C H -0.1380 -0.1142 0.3172 0.065 Uiso 1 1 calc R . . C26 C -0.2271(5) -0.0162(3) 0.1516(4) 0.0394(15) Uani 1 1 d . . . H26A H -0.2063 0.0071 0.0926 0.059 Uiso 1 1 calc R . . H26B H -0.2940 0.0034 0.1874 0.059 Uiso 1 1 calc R . . H26C H -0.2569 -0.0548 0.1291 0.059 Uiso 1 1 calc R . . C27 C -0.0505(6) 0.0498(3) 0.2966(5) 0.0466(17) Uani 1 1 d . . . H27A H -0.1232 0.0615 0.3351 0.070 Uiso 1 1 calc R . . H27B H -0.0383 0.0782 0.2426 0.070 Uiso 1 1 calc R . . H27C H 0.0261 0.0482 0.3422 0.070 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 K 0.0506(9) 0.0265(7) 0.0283(7) 0.0078(6) -0.0134(6) -0.0062(6) Si1 0.0257(8) 0.0154(8) 0.0169(7) 0.0004(6) -0.0019(6) -0.0012(7) Si2 0.0301(9) 0.0239(9) 0.0199(8) -0.0036(6) -0.0034(7) -0.0039(7) Si3 0.0383(10) 0.0206(8) 0.0255(9) 0.0004(7) 0.0029(7) -0.0084(7) Si4 0.0274(9) 0.0304(9) 0.0257(8) 0.0007(7) 0.0031(7) -0.0003(7) N1 0.030(3) 0.021(3) 0.015(2) -0.0004(19) -0.0026(19) -0.002(2) N2 0.037(3) 0.019(2) 0.017(2) 0.0019(19) 0.000(2) -0.004(2) C1 0.031(3) 0.023(3) 0.006(2) -0.001(2) 0.007(2) 0.000(3) C2 0.026(3) 0.023(3) 0.005(2) 0.004(2) -0.003(2) -0.003(3) C3 0.019(3) 0.016(3) 0.017(3) -0.003(2) -0.006(2) -0.003(2) C4 0.029(3) 0.021(3) 0.024(3) -0.003(2) -0.005(3) -0.001(3) C5 0.032(3) 0.029(3) 0.033(3) 0.003(3) 0.002(3) 0.006(3) C6 0.038(4) 0.029(3) 0.039(4) 0.010(3) -0.006(3) 0.009(3) C7 0.042(4) 0.029(3) 0.023(3) 0.008(3) -0.012(3) -0.001(3) C8 0.030(3) 0.023(3) 0.019(3) 0.000(2) -0.004(2) -0.006(3) C9 0.032(3) 0.033(3) 0.023(3) 0.001(2) 0.004(3) 0.003(3) C10 0.041(4) 0.040(4) 0.020(3) 0.004(3) 0.002(3) -0.008(3) C11 0.030(3) 0.015(3) 0.024(3) 0.002(2) 0.001(2) -0.004(2) C12 0.036(4) 0.021(3) 0.021(3) -0.006(2) 0.000(3) -0.002(3) C13 0.040(4) 0.028(3) 0.030(3) -0.012(3) 0.005(3) 0.000(3) C14 0.042(4) 0.036(4) 0.036(4) -0.005(3) -0.006(3) 0.012(3) C15 0.051(4) 0.026(3) 0.030(3) 0.003(3) -0.007(3) 0.016(3) C16 0.030(3) 0.020(3) 0.026(3) -0.002(2) 0.001(3) -0.001(3) C17 0.052(4) 0.030(3) 0.017(3) -0.003(2) 0.004(3) -0.001(3) C18 0.044(4) 0.028(3) 0.024(3) 0.010(2) 0.002(3) -0.003(3) C19 0.052(4) 0.043(4) 0.039(4) -0.015(3) -0.001(3) 0.002(3) C20 0.057(4) 0.052(4) 0.038(4) 0.004(3) 0.000(3) -0.028(4) C21 0.042(4) 0.037(4) 0.032(3) -0.009(3) -0.006(3) 0.002(3) C22 0.061(5) 0.042(4) 0.042(4) -0.005(3) -0.006(3) -0.021(4) C23 0.051(4) 0.025(3) 0.042(4) 0.005(3) 0.006(3) -0.008(3) C24 0.052(4) 0.028(4) 0.056(4) -0.012(3) 0.013(3) -0.013(3) C25 0.037(4) 0.058(4) 0.036(4) 0.010(3) 0.011(3) -0.003(3) C26 0.026(3) 0.050(4) 0.042(4) 0.000(3) 0.001(3) 0.002(3) C27 0.050(4) 0.041(4) 0.050(4) -0.016(3) 0.015(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 K N2 2.857(4) 3 ? K N1 2.863(4) . ? K Si1 3.305(2) . ? K Si1 3.396(2) 3 ? Si1 C1 1.903(5) . ? Si1 C2 1.904(5) . ? Si1 Si4 2.343(2) . ? Si1 K 3.396(2) 3 ? Si2 N1 1.736(4) . ? Si2 C20 1.855(6) . ? Si2 C21 1.859(6) . ? Si2 C19 1.863(6) . ? Si3 N2 1.737(4) . ? Si3 C24 1.859(6) . ? Si3 C22 1.868(6) . ? Si3 C23 1.869(6) . ? Si4 C26 1.874(6) . ? Si4 C25 1.879(6) . ? Si4 C27 1.883(6) . ? N1 C1 1.307(6) . ? N2 C2 1.295(6) . ? N2 K 2.857(4) 3 ? C1 C3 1.492(7) . ? C2 C11 1.505(7) . ? C3 C4 1.402(7) . ? C3 C8 1.403(7) . ? C4 C5 1.383(7) . ? C4 C9 1.515(7) . ? C5 C6 1.376(7) . ? C6 C7 1.377(8) . ? C7 C8 1.390(7) . ? C8 C10 1.513(7) . ? C11 C16 1.394(7) . ? C11 C12 1.413(7) . ? C12 C13 1.378(7) . ? C12 C17 1.512(7) . ? C13 C14 1.374(8) . ? C14 C15 1.381(8) . ? C15 C16 1.387(7) . ? C16 C18 1.506(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 K N1 164.27(13) 3 . ? N2 K Si1 143.30(10) 3 . ? N1 K Si1 52.40(9) . . ? N2 K Si1 51.11(9) 3 3 ? N1 K Si1 144.58(10) . 3 ? Si1 K Si1 92.19(5) . 3 ? C1 Si1 C2 116.0(2) . . ? C1 Si1 Si4 107.06(16) . . ? C2 Si1 Si4 104.83(16) . . ? C1 Si1 K 77.91(16) . . ? C2 Si1 K 151.63(14) . . ? Si4 Si1 K 93.26(7) . . ? C1 Si1 K 160.36(15) . 3 ? C2 Si1 K 71.84(14) . 3 ? Si4 Si1 K 86.94(7) . 3 ? K Si1 K 87.81(5) . 3 ? N1 Si2 C20 105.7(2) . . ? N1 Si2 C21 120.1(2) . . ? C20 Si2 C21 106.8(3) . . ? N1 Si2 C19 105.8(2) . . ? C20 Si2 C19 110.0(3) . . ? C21 Si2 C19 108.1(3) . . ? N2 Si3 C24 118.1(2) . . ? N2 Si3 C22 105.2(2) . . ? C24 Si3 C22 108.6(3) . . ? N2 Si3 C23 107.2(2) . . ? C24 Si3 C23 109.9(3) . . ? C22 Si3 C23 107.2(3) . . ? C26 Si4 C25 106.2(3) . . ? C26 Si4 C27 106.0(3) . . ? C25 Si4 C27 107.6(3) . . ? C26 Si4 Si1 108.72(19) . . ? C25 Si4 Si1 116.7(2) . . ? C27 Si4 Si1 111.0(2) . . ? C1 N1 Si2 132.2(4) . . ? C1 N1 K 105.5(3) . . ? Si2 N1 K 117.6(2) . . ? C2 N2 Si3 132.7(4) . . ? C2 N2 K 100.0(3) . 3 ? Si3 N2 K 112.8(2) . 3 ? N1 C1 C3 120.1(4) . . ? N1 C1 Si1 116.8(4) . . ? C3 C1 Si1 123.1(4) . . ? N2 C2 C11 121.7(4) . . ? N2 C2 Si1 116.6(4) . . ? C11 C2 Si1 121.3(4) . . ? C4 C3 C8 119.7(5) . . ? C4 C3 C1 120.2(4) . . ? C8 C3 C1 120.1(4) . . ? C5 C4 C3 119.4(5) . . ? C5 C4 C9 120.5(5) . . ? C3 C4 C9 120.0(5) . . ? C6 C5 C4 121.1(5) . . ? C5 C6 C7 119.6(5) . . ? C6 C7 C8 121.2(5) . . ? C7 C8 C3 119.0(5) . . ? C7 C8 C10 120.0(5) . . ? C3 C8 C10 121.0(5) . . ? C16 C11 C12 119.9(5) . . ? C16 C11 C2 120.1(4) . . ? C12 C11 C2 120.0(4) . . ? C13 C12 C11 118.9(5) . . ? C13 C12 C17 120.5(5) . . ? C11 C12 C17 120.6(5) . . ? C14 C13 C12 121.5(5) . . ? C13 C14 C15 119.4(5) . . ? C14 C15 C16 121.1(5) . . ? C15 C16 C11 119.2(5) . . ? C15 C16 C18 120.2(5) . . ? C11 C16 C18 120.6(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.356 _refine_diff_density_min -0.302 _refine_diff_density_rms 0.073