# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1688 data_gerhus-2 _audit_creation_date 2000-01-24T12:01:42-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common ; '[Li(thf)2{Si(SiMe3)3(C6H4(NCH2tBu)2)}]' ; _chemical_formula_moiety 'C33 H69 Li N2 O2 Si5' _chemical_formula_structural 'C33 H69 Li N2 O2 Si5' _chemical_formula_sum 'C33 H69 Li N2 O2 Si5' _chemical_formula_weight 673.29 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.8306(11) _cell_length_b 18.4336(13) _cell_length_c 18.7237(15) _cell_angle_alpha 90 _cell_angle_beta 96.161(4) _cell_angle_gamma 90 _cell_volume 4402.8(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 470791 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_diffrn 1.016 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_T_min 0.9455 _exptl_absorpt_correction_T_max 0.9455 #----------------------------------------------------------------------------# # 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 34014 _diffrn_reflns_av_R_equivalents 0.0604 _diffrn_reflns_av_sigmaI/netI 0.0413 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 4.56 _diffrn_reflns_theta_max 25.06 _diffrn_reflns_theta_full 25.06 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 7659 _reflns_number_gt 5962 _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^)+(0.0638P)^2^+2.3709P] 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_number_reflns 7659 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0734 _refine_ls_R_factor_gt 0.0522 _refine_ls_wR_factor_ref 0.1377 _refine_ls_wR_factor_gt 0.1257 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_restrained_S_all 1.007 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.23 _refine_diff_density_min -0.2 _refine_diff_density_rms 0.038 #----------------------------------------------------------------------------# # 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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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 Li Li 0.2092(4) 0.6749(2) 0.3384(3) 0.0606(12) Uani 1 1 d . . . Si1 Si 0.06313(5) 0.72149(3) 0.24151(3) 0.03700(17) Uani 1 1 d . . . Si2 Si -0.10678(5) 0.65803(4) 0.20851(3) 0.04287(18) Uani 1 1 d . . . Si3 Si -0.24614(6) 0.72485(4) 0.14922(4) 0.0575(2) Uani 1 1 d . . . Si4 Si -0.09503(6) 0.55158(4) 0.14007(4) 0.0533(2) Uani 1 1 d . . . Si5 Si -0.16135(7) 0.61360(4) 0.31602(4) 0.0647(2) Uani 1 1 d . . . O1 O 0.33650(14) 0.72808(10) 0.34666(10) 0.0596(5) Uani 1 1 d . . . O2 O 0.22704(17) 0.58214(11) 0.38037(11) 0.0708(6) Uani 1 1 d . . . N1 N 0.10608(15) 0.74506(10) 0.15591(10) 0.0393(4) Uani 1 1 d . . . N2 N 0.02775(15) 0.81530(10) 0.25011(9) 0.0400(4) Uani 1 1 d . . . C1 C 0.06518(18) 0.81130(12) 0.13088(12) 0.0426(5) Uani 1 1 d . . . C2 C 0.01961(19) 0.85133(12) 0.18448(12) 0.0430(5) Uani 1 1 d . . . C3 C -0.0260(2) 0.91828(14) 0.16760(14) 0.0553(7) Uani 1 1 d . . . H3 H -0.0558 0.9455 0.2034 0.066 Uiso 1 1 calc R . . C4 C -0.0282(3) 0.94562(15) 0.09816(16) 0.0672(8) Uani 1 1 d . . . H4 H -0.0605 0.9911 0.0867 0.081 Uiso 1 1 calc R . . C5 C 0.0159(2) 0.90766(15) 0.04618(15) 0.0633(8) Uani 1 1 d . . . H5 H 0.0139 0.9269 -0.001 0.076 Uiso 1 1 calc R . . C6 C 0.0639(2) 0.84044(14) 0.06229(13) 0.0513(6) Uani 1 1 d . . . H6 H 0.0956 0.8148 0.0263 0.062 Uiso 1 1 calc R . . C7 C 0.1342(2) 0.69059(13) 0.10506(13) 0.0467(6) Uani 1 1 d . . . H7A H 0.1002 0.7038 0.0569 0.056 Uiso 1 1 calc R . . H7B H 0.1041 0.6436 0.1182 0.056 Uiso 1 1 calc R . . C8 C 0.2519(2) 0.67919(14) 0.09932(14) 0.0569(7) Uani 1 1 d . . . C9 C 0.3047(3) 0.75065(18) 0.08323(19) 0.0800(10) Uani 1 1 d . . . H9A H 0.2706 0.7711 0.0384 0.12 Uiso 1 1 calc R . . H9B H 0.379 0.7419 0.0784 0.12 Uiso 1 1 calc R . . H9C H 0.2986 0.7849 0.1226 0.12 Uiso 1 1 calc R . . C10 C 0.3053(2) 0.64760(16) 0.16897(16) 0.0630(7) Uani 1 1 d . . . H10A H 0.2712 0.6019 0.1796 0.095 Uiso 1 1 calc R . . H10B H 0.2997 0.682 0.2083 0.095 Uiso 1 1 calc R . . H10C H 0.3794 0.6386 0.1639 0.095 Uiso 1 1 calc R . . C11 C 0.2607(3) 0.6246(2) 0.03829(18) 0.0954(12) Uani 1 1 d . . . H11A H 0.2262 0.6444 -0.0067 0.143 Uiso 1 1 calc R . . H11B H 0.2267 0.579 0.0495 0.143 Uiso 1 1 calc R . . H11C H 0.3348 0.6155 0.0332 0.143 Uiso 1 1 calc R . . C12 C -0.01841(19) 0.84673(13) 0.31099(12) 0.0457(6) Uani 1 1 d . . . H12A H -0.0526 0.8074 0.3359 0.055 Uiso 1 1 calc R . . H12B H -0.0739 0.8812 0.2923 0.055 Uiso 1 1 calc R . . C13 C 0.0586(2) 0.88675(14) 0.36662(13) 0.0551(7) Uani 1 1 d . . . C14 C 0.1314(2) 0.83276(16) 0.40735(14) 0.0626(7) Uani 1 1 d . . . H14A H 0.1802 0.8586 0.4424 0.094 Uiso 1 1 calc R . . H14B H 0.1711 0.8066 0.3736 0.094 Uiso 1 1 calc R . . H14C H 0.0902 0.7982 0.4324 0.094 Uiso 1 1 calc R . . C15 C -0.0064(3) 0.9245(2) 0.4198(2) 0.1083(15) Uani 1 1 d . . . H15A H -0.0542 0.9594 0.394 0.163 Uiso 1 1 calc R . . H15B H 0.0405 0.95 0.4562 0.163 Uiso 1 1 calc R . . H15C H -0.0471 0.8882 0.4431 0.163 Uiso 1 1 calc R . . C16 C 0.1246(3) 0.94206(17) 0.32990(18) 0.0811(10) Uani 1 1 d . . . H16A H 0.0782 0.9774 0.3034 0.122 Uiso 1 1 calc R . . H16B H 0.166 0.9168 0.2965 0.122 Uiso 1 1 calc R . . H16C H 0.1718 0.9673 0.3663 0.122 Uiso 1 1 calc R . . C17 C -0.2105(2) 0.76637(17) 0.06380(17) 0.0717(8) Uani 1 1 d . . . H17A H -0.1904 0.728 0.0317 0.108 Uiso 1 1 calc R . . H17B H -0.1516 0.7998 0.0747 0.108 Uiso 1 1 calc R . . H17C H -0.2709 0.7929 0.0403 0.108 Uiso 1 1 calc R . . C18 C -0.2835(3) 0.80134(19) 0.2079(2) 0.0842(10) Uani 1 1 d . . . H18A H -0.3032 0.7817 0.2532 0.126 Uiso 1 1 calc R . . H18B H -0.343 0.8279 0.1832 0.126 Uiso 1 1 calc R . . H18C H -0.2239 0.8343 0.2178 0.126 Uiso 1 1 calc R . . C19 C -0.3675(2) 0.6686(2) 0.1238(2) 0.0847(10) Uani 1 1 d . . . H19A H -0.3902 0.6462 0.167 0.127 Uiso 1 1 calc R . . H19B H -0.3517 0.6306 0.0899 0.127 Uiso 1 1 calc R . . H19C H -0.4236 0.6998 0.1012 0.127 Uiso 1 1 calc R . . C20 C 0.0299(3) 0.50015(15) 0.16499(17) 0.0684(8) Uani 1 1 d . . . H20A H 0.0899 0.532 0.1604 0.103 Uiso 1 1 calc R . . H20B H 0.0329 0.4584 0.1329 0.103 Uiso 1 1 calc R . . H20C H 0.0319 0.4831 0.2147 0.103 Uiso 1 1 calc R . . C21 C -0.1027(3) 0.57166(17) 0.04127(15) 0.0674(8) Uani 1 1 d . . . H21A H -0.1672 0.5986 0.0264 0.101 Uiso 1 1 calc R . . H21B H -0.1029 0.526 0.0144 0.101 Uiso 1 1 calc R . . H21C H -0.0419 0.6008 0.0315 0.101 Uiso 1 1 calc R . . C22 C -0.2035(3) 0.48455(19) 0.1507(2) 0.0864(10) Uani 1 1 d . . . H22A H -0.2715 0.5082 0.1387 0.13 Uiso 1 1 calc R . . H22B H -0.198 0.4674 0.2005 0.13 Uiso 1 1 calc R . . H22C H -0.1972 0.4432 0.1185 0.13 Uiso 1 1 calc R . . C23 C -0.0821(4) 0.5322(2) 0.34832(19) 0.0964(12) Uani 1 1 d . . . H23A H -0.0887 0.4946 0.3111 0.145 Uiso 1 1 calc R . . H23B H -0.1078 0.5134 0.3921 0.145 Uiso 1 1 calc R . . H23C H -0.0083 0.5461 0.3586 0.145 Uiso 1 1 calc R . . C24 C -0.3040(3) 0.5873(3) 0.3089(2) 0.1113(14) Uani 1 1 d . . . H24A H -0.3472 0.6289 0.2918 0.167 Uiso 1 1 calc R . . H24B H -0.3223 0.5723 0.3562 0.167 Uiso 1 1 calc R . . H24C H -0.3167 0.547 0.2749 0.167 Uiso 1 1 calc R . . C25 C -0.1444(4) 0.6811(2) 0.39045(18) 0.1075(15) Uani 1 1 d . . . H25A H -0.1849 0.7248 0.3765 0.161 Uiso 1 1 calc R . . H25B H -0.07 0.6936 0.4004 0.161 Uiso 1 1 calc R . . H25C H -0.1693 0.6602 0.4337 0.161 Uiso 1 1 calc R . . C26 C 0.3583(2) 0.79471(16) 0.3100(2) 0.0734(9) Uani 1 1 d . . . H26A H 0.3425 0.8376 0.3388 0.088 Uiso 1 1 calc R . . H26B H 0.3164 0.7976 0.2625 0.088 Uiso 1 1 calc R . . C27 C 0.4729(3) 0.7905(2) 0.3019(2) 0.0898(11) Uani 1 1 d . . . H27A H 0.5033 0.8393 0.2966 0.108 Uiso 1 1 calc R . . H27B H 0.4864 0.7601 0.2603 0.108 Uiso 1 1 calc R . . C28 C 0.5153(3) 0.7556(3) 0.3719(2) 0.1026(13) Uani 1 1 d . . . H28A H 0.5236 0.7917 0.4113 0.123 Uiso 1 1 calc R . . H28B H 0.5838 0.7321 0.3678 0.123 Uiso 1 1 calc R . . C29 C 0.4322(2) 0.7001(2) 0.38447(19) 0.0873(11) Uani 1 1 d . . . H29A H 0.4498 0.6522 0.3651 0.105 Uiso 1 1 calc R . . H29B H 0.4254 0.695 0.4364 0.105 Uiso 1 1 calc R . . C30 C 0.2608(4) 0.5237(2) 0.3382(2) 0.1166(16) Uani 1 1 d . . . H30A H 0.3383 0.521 0.3431 0.14 Uiso 1 1 calc R . . H30B H 0.2355 0.531 0.2869 0.14 Uiso 1 1 calc R . . C31 C 0.2168(3) 0.45714(18) 0.3647(2) 0.0919(11) Uani 1 1 d . . . H31A H 0.2652 0.4158 0.3612 0.11 Uiso 1 1 calc R . . H31B H 0.1486 0.4455 0.3372 0.11 Uiso 1 1 calc R . . C32 C 0.2033(3) 0.47356(18) 0.44217(19) 0.0866(10) Uani 1 1 d . . . H32A H 0.1329 0.4586 0.4536 0.104 Uiso 1 1 calc R . . H32B H 0.2569 0.4478 0.4748 0.104 Uiso 1 1 calc R . . C33 C 0.2165(4) 0.55353(19) 0.44950(18) 0.0937(12) Uani 1 1 d . . . H33A H 0.1547 0.5751 0.4689 0.112 Uiso 1 1 calc R . . H33B H 0.2796 0.5649 0.4828 0.112 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 Li 0.053(3) 0.057(3) 0.070(3) 0.017(2) -0.004(2) 0.001(2) Si1 0.0384(4) 0.0348(3) 0.0377(3) 0.0025(2) 0.0033(3) 0.0006(3) Si2 0.0410(4) 0.0431(4) 0.0451(4) -0.0024(3) 0.0072(3) -0.0055(3) Si3 0.0385(4) 0.0638(5) 0.0694(5) -0.0021(4) 0.0016(3) 0.0005(3) Si4 0.0563(5) 0.0464(4) 0.0570(4) -0.0087(3) 0.0052(3) -0.0078(3) Si5 0.0793(6) 0.0595(5) 0.0601(5) 0.0002(4) 0.0290(4) -0.0175(4) O1 0.0465(11) 0.0635(12) 0.0669(12) 0.0014(9) -0.0022(9) 0.0009(9) O2 0.0871(15) 0.0541(12) 0.0707(13) 0.0214(10) 0.0051(11) 0.0147(10) N1 0.0422(11) 0.0360(10) 0.0403(10) 0.0019(8) 0.0076(8) -0.0004(8) N2 0.0444(11) 0.0362(10) 0.0390(10) 0.0012(8) 0.0032(8) 0.0009(8) C1 0.0433(13) 0.0392(13) 0.0449(13) 0.0041(10) 0.0029(10) -0.0064(10) C2 0.0481(14) 0.0351(12) 0.0448(13) 0.0017(10) 0.0004(10) -0.0010(10) C3 0.0670(18) 0.0398(14) 0.0587(16) 0.0026(12) 0.0049(13) 0.0067(12) C4 0.091(2) 0.0444(16) 0.0655(18) 0.0153(13) 0.0033(16) 0.0099(15) C5 0.087(2) 0.0513(16) 0.0507(16) 0.0189(13) 0.0021(14) -0.0019(15) C6 0.0624(17) 0.0491(15) 0.0430(13) 0.0035(11) 0.0080(12) -0.0060(12) C7 0.0567(16) 0.0406(13) 0.0436(13) -0.0013(10) 0.0089(11) -0.0021(11) C8 0.0648(18) 0.0537(16) 0.0558(16) -0.0014(12) 0.0234(13) 0.0067(13) C9 0.063(2) 0.080(2) 0.103(3) 0.0259(19) 0.0366(18) 0.0037(16) C10 0.0545(17) 0.0636(18) 0.0727(18) 0.0007(14) 0.0144(14) 0.0120(13) C11 0.119(3) 0.102(3) 0.071(2) -0.0201(19) 0.033(2) 0.034(2) C12 0.0440(14) 0.0461(14) 0.0475(13) -0.0018(11) 0.0071(11) 0.0059(11) C13 0.0592(17) 0.0568(16) 0.0483(14) -0.0147(12) 0.0014(12) 0.0077(13) C14 0.0590(17) 0.0736(19) 0.0523(16) -0.0072(13) -0.0070(13) 0.0025(14) C15 0.089(3) 0.149(4) 0.084(2) -0.063(3) -0.005(2) 0.042(3) C16 0.097(3) 0.0571(19) 0.083(2) -0.0036(16) -0.0196(19) -0.0209(17) C17 0.0627(19) 0.073(2) 0.075(2) 0.0124(16) -0.0138(15) -0.0029(15) C18 0.057(2) 0.084(2) 0.111(3) -0.014(2) 0.0116(18) 0.0176(17) C19 0.0469(18) 0.103(3) 0.102(3) 0.002(2) -0.0039(17) -0.0114(17) C20 0.084(2) 0.0455(16) 0.0753(19) 0.0022(13) 0.0083(16) 0.0061(14) C21 0.072(2) 0.0702(19) 0.0589(17) -0.0155(14) 0.0002(14) 0.0003(15) C22 0.092(3) 0.071(2) 0.097(2) -0.0222(18) 0.015(2) -0.0343(19) C23 0.133(3) 0.086(3) 0.073(2) 0.0228(19) 0.022(2) 0.004(2) C24 0.097(3) 0.128(3) 0.119(3) 0.004(3) 0.057(2) -0.044(3) C25 0.184(4) 0.087(3) 0.061(2) -0.0095(18) 0.057(2) -0.041(3) C26 0.064(2) 0.0546(18) 0.103(2) -0.0053(16) 0.0159(17) -0.0060(14) C27 0.076(2) 0.076(2) 0.124(3) -0.018(2) 0.038(2) -0.0126(18) C28 0.051(2) 0.143(4) 0.112(3) -0.028(3) 0.003(2) -0.007(2) C29 0.0512(19) 0.128(3) 0.079(2) 0.008(2) -0.0084(16) 0.0086(19) C30 0.180(5) 0.078(3) 0.102(3) 0.027(2) 0.060(3) 0.047(3) C31 0.119(3) 0.063(2) 0.091(3) 0.0097(18) -0.003(2) 0.025(2) C32 0.103(3) 0.069(2) 0.089(2) 0.0295(18) 0.019(2) 0.0147(19) C33 0.135(3) 0.081(2) 0.062(2) 0.0155(17) -0.004(2) -0.009(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 Li O2 1.886(5) . ? Li O1 1.897(5) . ? Li Si1 2.609(4) . ? Si1 N2 1.7995(19) . ? Si1 N1 1.8030(19) . ? Si1 Si2 2.4927(9) . ? Si2 Si5 2.3484(10) . ? Si2 Si3 2.3496(10) . ? Si2 Si4 2.3572(10) . ? Si3 C17 1.873(3) . ? Si3 C18 1.881(3) . ? Si3 C19 1.889(3) . ? Si4 C20 1.877(3) . ? Si4 C21 1.879(3) . ? Si4 C22 1.888(3) . ? Si5 C25 1.863(3) . ? Si5 C23 1.876(4) . ? Si5 C24 1.884(4) . ? O1 C29 1.446(4) . ? O1 C26 1.449(4) . ? O2 C33 1.418(4) . ? O2 C30 1.430(4) . ? N1 C1 1.390(3) . ? N1 C7 1.456(3) . ? N2 C2 1.391(3) . ? N2 C12 1.460(3) . ? C1 C6 1.390(3) . ? C1 C2 1.421(3) . ? C2 C3 1.388(3) . ? C3 C4 1.392(4) . ? C4 C5 1.369(4) . ? C5 C6 1.402(4) . ? C7 C8 1.540(4) . ? C8 C10 1.522(4) . ? C8 C9 1.526(4) . ? C8 C11 1.536(4) . ? C12 C13 1.544(3) . ? C13 C14 1.514(4) . ? C13 C15 1.533(4) . ? C13 C16 1.534(4) . ? C26 C27 1.496(4) . ? C27 C28 1.508(5) . ? C28 C29 1.515(5) . ? C30 C31 1.459(5) . ? C31 C32 1.509(5) . ? C32 C33 1.488(5) . ? 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 O2 Li O1 111.7(2) . . ? O2 Li Si1 129.4(2) . . ? O1 Li Si1 115.8(2) . . ? N2 Si1 N1 87.25(8) . . ? N2 Si1 Si2 104.53(7) . . ? N1 Si1 Si2 103.62(7) . . ? N2 Si1 Li 115.04(13) . . ? N1 Si1 Li 115.59(13) . . ? Si2 Si1 Li 124.16(10) . . ? Si5 Si2 Si3 107.82(4) . . ? Si5 Si2 Si4 102.60(4) . . ? Si3 Si2 Si4 105.63(4) . . ? Si5 Si2 Si1 106.53(4) . . ? Si3 Si2 Si1 118.16(4) . . ? Si4 Si2 Si1 114.84(3) . . ? C17 Si3 C18 107.04(17) . . ? C17 Si3 C19 106.20(15) . . ? C18 Si3 C19 107.69(17) . . ? C17 Si3 Si2 112.00(10) . . ? C18 Si3 Si2 110.24(12) . . ? C19 Si3 Si2 113.34(12) . . ? C20 Si4 C21 107.30(14) . . ? C20 Si4 C22 105.21(16) . . ? C21 Si4 C22 105.77(16) . . ? C20 Si4 Si2 112.83(10) . . ? C21 Si4 Si2 111.82(10) . . ? C22 Si4 Si2 113.36(11) . . ? C25 Si5 C23 106.1(2) . . ? C25 Si5 C24 105.0(2) . . ? C23 Si5 C24 107.8(2) . . ? C25 Si5 Si2 112.75(11) . . ? C23 Si5 Si2 110.73(12) . . ? C24 Si5 Si2 113.92(14) . . ? C29 O1 C26 109.7(2) . . ? C29 O1 Li 122.3(2) . . ? C26 O1 Li 127.4(2) . . ? C33 O2 C30 106.7(2) . . ? C33 O2 Li 134.3(3) . . ? C30 O2 Li 118.9(2) . . ? C1 N1 C7 119.77(18) . . ? C1 N1 Si1 111.78(15) . . ? C7 N1 Si1 122.42(15) . . ? C2 N2 C12 120.14(19) . . ? C2 N2 Si1 112.05(15) . . ? C12 N2 Si1 125.37(15) . . ? N1 C1 C6 128.1(2) . . ? N1 C1 C2 112.76(19) . . ? C6 C1 C2 119.1(2) . . ? C3 C2 N2 128.0(2) . . ? C3 C2 C1 119.8(2) . . ? N2 C2 C1 112.2(2) . . ? C2 C3 C4 120.0(3) . . ? C5 C4 C3 120.7(3) . . ? C4 C5 C6 120.3(2) . . ? C1 C6 C5 120.1(2) . . ? N1 C7 C8 117.0(2) . . ? C10 C8 C9 109.3(3) . . ? C10 C8 C11 108.9(2) . . ? C9 C8 C11 110.4(3) . . ? C10 C8 C7 110.3(2) . . ? C9 C8 C7 110.8(2) . . ? C11 C8 C7 107.0(3) . . ? N2 C12 C13 115.6(2) . . ? C14 C13 C15 108.7(3) . . ? C14 C13 C16 108.8(3) . . ? C15 C13 C16 110.8(3) . . ? C14 C13 C12 110.0(2) . . ? C15 C13 C12 107.5(2) . . ? C16 C13 C12 111.1(2) . . ? O1 C26 C27 104.2(3) . . ? C26 C27 C28 101.6(3) . . ? C27 C28 C29 103.2(3) . . ? O1 C29 C28 104.9(3) . . ? O2 C30 C31 107.1(3) . . ? C30 C31 C32 104.3(3) . . ? C33 C32 C31 105.3(3) . . ? O2 C33 C32 107.8(3) . . ? #===END data_gerhus-3a _audit_creation_date 2000-01-18T09:38:49-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[K{Me3SiNSi(SiMe3)(C6H4(NCH2tBu)2)}]' _chemical_formula_moiety 'C22 H44 K N3 Si3' _chemical_formula_structural 'C22 H44 K N3 Si3' _chemical_formula_sum 'C22 H44 K N3 Si3' _chemical_formula_weight 473.97 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.4645(4) _cell_length_b 12.7533(3) _cell_length_c 16.5858(3) _cell_angle_alpha 90 _cell_angle_beta 91.759(2) _cell_angle_gamma 90 _cell_volume 2846.72(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 10046 _cell_measurement_theta_min 4.529 _cell_measurement_theta_max 27.878 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.106 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1032 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.326 #----------------------------------------------------------------------------# # 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 20621 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 4.55 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _reflns_number_total 6689 _reflns_number_gt 5363 _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^)+(0.0361P)^2^+1.2475P] 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_number_reflns 6689 _refine_ls_number_parameters 262 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0539 _refine_ls_R_factor_gt 0.0391 _refine_ls_wR_factor_ref 0.0972 _refine_ls_wR_factor_gt 0.0904 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.31 _refine_diff_density_min -0.32 _refine_diff_density_rms 0.048 #----------------------------------------------------------------------------# # 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' 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' 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 0.14060(3) 0.96416(3) 0.25913(3) 0.03950(12) Uani 1 1 d . . . Si1 Si 0.07164(3) 0.71839(3) 0.23769(2) 0.01866(10) Uani 1 1 d . . . Si2 Si 0.00988(4) 0.55003(3) 0.20523(3) 0.02749(12) Uani 1 1 d . . . Si3 Si -0.12226(3) 0.85611(3) 0.23040(3) 0.02323(11) Uani 1 1 d . . . N1 N 0.15214(9) 0.70848(10) 0.32572(7) 0.0217(3) Uani 1 1 d . . . N2 N 0.18089(9) 0.73475(10) 0.17866(7) 0.0205(3) Uani 1 1 d . . . N3 N -0.00309(10) 0.81894(10) 0.23779(8) 0.0227(3) Uani 1 1 d . . . C1 C 0.25134(11) 0.69734(11) 0.30699(9) 0.0216(3) Uani 1 1 d . . . C2 C 0.26822(11) 0.71377(11) 0.22332(9) 0.0206(3) Uani 1 1 d . . . C3 C 0.36466(12) 0.70846(13) 0.19556(10) 0.0270(3) Uani 1 1 d . . . H3 H 0.3764 0.72 0.1401 0.032 Uiso 1 1 calc R . . C4 C 0.44466(13) 0.68619(14) 0.24906(11) 0.0317(4) Uani 1 1 d . . . H4 H 0.5104 0.6841 0.2299 0.038 Uiso 1 1 calc R . . C5 C 0.42807(13) 0.66735(13) 0.32942(11) 0.0313(4) Uani 1 1 d . . . H5 H 0.4824 0.6513 0.3652 0.038 Uiso 1 1 calc R . . C6 C 0.33157(12) 0.67180(13) 0.35858(10) 0.0273(3) Uani 1 1 d . . . H6 H 0.3207 0.6573 0.4138 0.033 Uiso 1 1 calc R . . C7 C 0.11848(13) 0.67750(14) 0.40582(9) 0.0287(4) Uani 1 1 d . . . H7A H 0.1651 0.6238 0.4277 0.034 Uiso 1 1 calc R . . H7B H 0.0528 0.6434 0.3985 0.034 Uiso 1 1 calc R . . C8 C 0.10905(14) 0.76395(16) 0.47004(10) 0.0356(4) Uani 1 1 d . . . C9 C 0.02161(16) 0.83548(18) 0.44776(12) 0.0493(5) Uani 1 1 d . . . H9A H -0.039 0.7934 0.441 0.074 Uiso 1 1 calc R . . H9B H 0.0347 0.872 0.3972 0.074 Uiso 1 1 calc R . . H9C H 0.0129 0.887 0.4908 0.074 Uiso 1 1 calc R . . C10 C 0.08685(17) 0.7083(2) 0.54975(12) 0.0569(7) Uani 1 1 d . . . H10A H 0.0262 0.6664 0.5428 0.085 Uiso 1 1 calc R . . H10B H 0.0776 0.7607 0.5921 0.085 Uiso 1 1 calc R . . H10C H 0.1426 0.6623 0.5652 0.085 Uiso 1 1 calc R . . C11 C 0.20330(17) 0.82847(19) 0.48087(13) 0.0508(5) Uani 1 1 d . . . H11A H 0.2591 0.7821 0.4952 0.076 Uiso 1 1 calc R . . H11B H 0.1948 0.8799 0.524 0.076 Uiso 1 1 calc R . . H11C H 0.2168 0.865 0.4304 0.076 Uiso 1 1 calc R . . C12 C 0.17922(12) 0.71686(12) 0.09107(9) 0.0243(3) Uani 1 1 d . . . H12A H 0.119 0.6755 0.0768 0.029 Uiso 1 1 calc R . . H12B H 0.2374 0.6729 0.0786 0.029 Uiso 1 1 calc R . . C13 C 0.18025(13) 0.81364(13) 0.03564(9) 0.0269(3) Uani 1 1 d . . . C14 C 0.08332(14) 0.87500(15) 0.04316(10) 0.0361(4) Uani 1 1 d . . . H14A H 0.0268 0.8286 0.0309 0.054 Uiso 1 1 calc R . . H14B H 0.0823 0.9338 0.0051 0.054 Uiso 1 1 calc R . . H14C H 0.0787 0.9019 0.0983 0.054 Uiso 1 1 calc R . . C15 C 0.18690(16) 0.77285(16) -0.05111(10) 0.0411(5) Uani 1 1 d . . . H15A H 0.1302 0.7268 -0.0636 0.062 Uiso 1 1 calc R . . H15B H 0.2488 0.7335 -0.0565 0.062 Uiso 1 1 calc R . . H15C H 0.1859 0.8322 -0.0886 0.062 Uiso 1 1 calc R . . C16 C 0.26859(15) 0.88480(15) 0.05455(12) 0.0407(5) Uani 1 1 d . . . H16A H 0.3303 0.845 0.0495 0.061 Uiso 1 1 calc R . . H16B H 0.2644 0.9115 0.1097 0.061 Uiso 1 1 calc R . . H16C H 0.2679 0.9437 0.0166 0.061 Uiso 1 1 calc R . . C17 C 0.12238(15) 0.46476(15) 0.19205(15) 0.0484(5) Uani 1 1 d . . . H17A H 0.164 0.4661 0.2416 0.073 Uiso 1 1 calc R . . H17B H 0.1606 0.4912 0.147 0.073 Uiso 1 1 calc R . . H17C H 0.1011 0.3926 0.1807 0.073 Uiso 1 1 calc R . . C18 C -0.06219(16) 0.48891(16) 0.28780(13) 0.0455(5) Uani 1 1 d . . . H18A H -0.0225 0.4909 0.3383 0.068 Uiso 1 1 calc R . . H18B H -0.0777 0.4159 0.2738 0.068 Uiso 1 1 calc R . . H18C H -0.1241 0.5279 0.2945 0.068 Uiso 1 1 calc R . . C19 C -0.06770(16) 0.54555(17) 0.10913(12) 0.0451(5) Uani 1 1 d . . . H19A H -0.0307 0.5773 0.0654 0.068 Uiso 1 1 calc R . . H19B H -0.1295 0.5845 0.1163 0.068 Uiso 1 1 calc R . . H19C H -0.0833 0.4725 0.0955 0.068 Uiso 1 1 calc R . . C20 C -0.15237(15) 0.95692(15) 0.30934(13) 0.0418(5) Uani 1 1 d . . . H20A H -0.1055 1.0155 0.3065 0.063 Uiso 1 1 calc R . . H20B H -0.1471 0.9248 0.363 0.063 Uiso 1 1 calc R . . H20C H -0.2202 0.9828 0.2995 0.063 Uiso 1 1 calc R . . C21 C -0.21584(13) 0.74839(15) 0.24077(12) 0.0354(4) Uani 1 1 d . . . H21A H -0.2031 0.7112 0.2917 0.053 Uiso 1 1 calc R . . H21B H -0.2105 0.6993 0.1957 0.053 Uiso 1 1 calc R . . H21C H -0.2828 0.7785 0.2403 0.053 Uiso 1 1 calc R . . C22 C -0.15254(14) 0.92271(17) 0.13149(12) 0.0428(5) Uani 1 1 d . . . H22A H -0.1053 0.9799 0.1232 0.064 Uiso 1 1 calc R . . H22B H -0.2201 0.9512 0.1322 0.064 Uiso 1 1 calc R . . H22C H -0.148 0.8718 0.0875 0.064 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 0.0343(2) 0.0288(2) 0.0551(3) -0.00227(17) -0.00398(19) -0.00847(16) Si1 0.0181(2) 0.01777(19) 0.0201(2) 0.00267(15) -0.00053(15) -0.00044(15) Si2 0.0242(2) 0.0190(2) 0.0391(3) 0.00114(18) -0.00208(19) -0.00259(17) Si3 0.0184(2) 0.0236(2) 0.0277(2) 0.00451(17) 0.00016(17) 0.00199(17) N1 0.0188(7) 0.0279(7) 0.0185(6) 0.0036(5) 0.0008(5) 0.0019(5) N2 0.0206(7) 0.0226(6) 0.0183(6) 0.0028(5) 0.0004(5) 0.0008(5) N3 0.0209(7) 0.0225(6) 0.0245(7) 0.0022(5) -0.0014(5) 0.0013(5) C1 0.0206(8) 0.0187(7) 0.0253(8) 0.0008(6) -0.0008(6) 0.0003(6) C2 0.0199(8) 0.0164(7) 0.0256(8) 0.0012(6) 0.0006(6) 0.0009(6) C3 0.0232(8) 0.0270(8) 0.0309(9) 0.0036(7) 0.0045(7) 0.0036(7) C4 0.0198(8) 0.0312(9) 0.0443(10) 0.0017(7) 0.0016(7) 0.0042(7) C5 0.0221(9) 0.0328(9) 0.0386(10) -0.0004(7) -0.0073(7) 0.0058(7) C6 0.0259(9) 0.0303(8) 0.0253(8) 0.0010(7) -0.0037(6) 0.0055(7) C7 0.0266(9) 0.0359(9) 0.0237(8) 0.0094(7) 0.0011(6) 0.0000(7) C8 0.0316(10) 0.0546(12) 0.0208(8) 0.0010(8) 0.0022(7) 0.0088(9) C9 0.0486(13) 0.0664(14) 0.0328(10) -0.0024(10) 0.0028(9) 0.0228(11) C10 0.0474(13) 0.0994(19) 0.0245(10) 0.0139(11) 0.0090(9) 0.0163(13) C11 0.0489(13) 0.0625(14) 0.0411(11) -0.0203(10) 0.0010(9) -0.0013(11) C12 0.0277(9) 0.0238(8) 0.0213(8) 0.0008(6) 0.0015(6) 0.0022(6) C13 0.0318(9) 0.0292(8) 0.0199(8) 0.0040(6) 0.0042(6) 0.0040(7) C14 0.0421(11) 0.0407(10) 0.0256(9) 0.0079(7) 0.0048(7) 0.0146(8) C15 0.0543(13) 0.0464(11) 0.0228(9) 0.0031(8) 0.0066(8) 0.0141(10) C16 0.0430(12) 0.0384(10) 0.0408(10) 0.0131(8) 0.0032(9) -0.0059(9) C17 0.0372(11) 0.0267(9) 0.0814(16) 0.0050(10) 0.0043(10) 0.0052(8) C18 0.0416(12) 0.0362(10) 0.0589(13) 0.0137(9) 0.0016(10) -0.0129(9) C19 0.0416(12) 0.0467(12) 0.0467(12) -0.0128(9) -0.0063(9) -0.0077(9) C20 0.0321(10) 0.0380(10) 0.0553(12) -0.0102(9) 0.0002(9) 0.0106(8) C21 0.0252(9) 0.0350(9) 0.0462(11) 0.0039(8) 0.0055(8) -0.0021(8) C22 0.0258(10) 0.0570(12) 0.0454(11) 0.0238(10) -0.0014(8) 0.0056(9) #----------------------------------------------------------------------------# # 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 K N3 2.6938(14) . ? Si1 N3 1.6302(13) . ? Si1 N1 1.7959(13) . ? Si1 N2 1.8040(13) . ? Si1 Si2 2.3588(6) . ? Si2 C18 1.873(2) . ? Si2 C19 1.880(2) . ? Si2 C17 1.883(2) . ? Si3 N3 1.6739(14) . ? Si3 C21 1.8757(18) . ? Si3 C22 1.8809(18) . ? Si3 C20 1.8878(19) . ? N1 C1 1.388(2) . ? N1 C7 1.4709(19) . ? N2 C2 1.3962(19) . ? N2 C12 1.4700(19) . ? C1 C6 1.396(2) . ? C1 C2 1.429(2) . ? C2 C3 1.393(2) . ? C3 C4 1.403(2) . ? C4 C5 1.379(3) . ? C4 K 3.0569(18) 2_545 ? C5 C6 1.401(2) . ? C5 K 3.1054(18) 2_545 ? C7 C8 1.541(2) . ? C8 C11 1.518(3) . ? C8 C9 1.526(3) . ? C8 C10 1.538(3) . ? C12 C13 1.539(2) . ? C13 C16 1.521(3) . ? C13 C14 1.530(2) . ? C13 C15 1.535(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 N3 Si1 N1 114.31(6) . . ? N3 Si1 N2 115.04(6) . . ? N1 Si1 N2 88.15(6) . . ? N3 Si1 Si2 120.20(5) . . ? N1 Si1 Si2 108.74(5) . . ? N2 Si1 Si2 105.61(5) . . ? N3 Si1 K 54.67(5) . . ? N1 Si1 K 79.49(4) . . ? N2 Si1 K 73.50(4) . . ? Si2 Si1 K 171.75(2) . . ? C18 Si2 C19 108.70(10) . . ? C18 Si2 C17 106.34(10) . . ? C19 Si2 C17 108.19(11) . . ? C18 Si2 Si1 113.51(7) . . ? C19 Si2 Si1 113.83(7) . . ? C17 Si2 Si1 105.84(7) . . ? N3 Si3 C21 115.53(7) . . ? N3 Si3 C22 111.92(8) . . ? C21 Si3 C22 106.41(9) . . ? N3 Si3 C20 111.58(8) . . ? C21 Si3 C20 106.02(9) . . ? C22 Si3 C20 104.59(10) . . ? C1 N1 C7 120.00(12) . . ? C1 N1 Si1 112.72(10) . . ? C7 N1 Si1 123.93(10) . . ? C2 N2 C12 118.80(13) . . ? C2 N2 Si1 112.17(10) . . ? C12 N2 Si1 122.03(10) . . ? Si1 N3 Si3 144.40(9) . . ? Si1 N3 K 95.74(6) . . ? Si3 N3 K 119.86(6) . . ? N1 C1 C6 128.23(14) . . ? N1 C1 C2 112.66(13) . . ? C6 C1 C2 119.11(14) . . ? C3 C2 N2 127.77(14) . . ? C3 C2 C1 119.46(14) . . ? N2 C2 C1 112.77(13) . . ? C2 C3 C4 120.41(15) . . ? C5 C4 C3 120.15(16) . . ? C5 C4 K 79.04(10) . 2_545 ? C3 C4 K 83.08(10) . 2_545 ? C4 C5 C6 120.38(15) . . ? C4 C5 K 75.11(10) . 2_545 ? C6 C5 K 86.06(10) . 2_545 ? C1 C6 C5 120.42(15) . . ? N1 C7 C8 117.80(14) . . ? C11 C8 C9 109.91(18) . . ? C11 C8 C10 109.41(17) . . ? C9 C8 C10 108.38(16) . . ? C11 C8 C7 112.54(15) . . ? C9 C8 C7 109.86(15) . . ? C10 C8 C7 106.62(17) . . ? N2 C12 C13 117.76(13) . . ? C16 C13 C14 109.97(16) . . ? C16 C13 C15 109.12(15) . . ? C14 C13 C15 108.92(14) . . ? C16 C13 C12 112.12(14) . . ? C14 C13 C12 109.76(13) . . ? C15 C13 C12 106.86(14) . . ? #===END