# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2009 data_feb795 _audit_creation_date 2000-03-09T09:53:56-00:00 _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 '[(tsi)Al(SMe)3Li(thf)2]' _chemical_formula_moiety 'C21 H52 Al1 Li1 O2 S3 Si3' _chemical_formula_structural 'C21 H52 AL LI O2 S3 SI3' _chemical_formula_sum 'C21 H52 Al Li O2 S3 Si3' _chemical_formula_weight 551 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 16.891(6) _cell_length_b 9.826(4) _cell_length_c 19.456(11) _cell_angle_alpha 90 _cell_angle_beta 98.45(4) _cell_angle_gamma 90 _cell_volume 3194(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _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 0.3 _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method none _exptl_crystal_F_000 1200 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.388 #----------------------------------------------------------------------------# # 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_reflns_number 4589 _diffrn_reflns_av_R_equivalents 0.073 _diffrn_reflns_av_sigmaI/netI 0.061 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.12 _diffrn_reflns_theta_max 22.96 _reflns_number_total 4426 _reflns_number_gt 3385 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1985)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; 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 w=1/[\s^2^(Fo^2^)+(0.1543P)^2^+0.6329P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_extinction_method none _refine_ls_number_reflns 4426 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0921 _refine_ls_R_factor_gt 0.0713 _refine_ls_wR_factor_gt 0.2032 _refine_ls_wR_factor_all 0.2256 _refine_ls_goodness_of_fit_gt 1.115 _refine_ls_goodness_of_fit_all 1.077 _refine_ls_restrained_S_all 1.077 _refine_ls_restrained_S_obs 1.115 _refine_ls_shift/su_max 0 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.71 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.133 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Al Al 0.0645 0.0514 '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_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Al Al 0.78897(8) 0.10208(15) 0.72681(8) 0.0182(4) Uani 1 d . . Li Li 0.7751(6) -0.1199(10) 0.6030(5) 0.037(2) Uani 1 d . . Si1 Si 0.70622(9) 0.11784(15) 0.86327(8) 0.0246(4) Uani 1 d . . Si2 Si 0.74989(9) 0.38505(14) 0.79166(8) 0.0254(4) Uani 1 d . . Si3 Si 0.61067(8) 0.20545(15) 0.72190(8) 0.0230(4) Uani 1 d . . S1 S 0.91843(8) 0.1488(2) 0.76125(8) 0.0335(4) Uani 1 d . . S2 S 0.76376(8) 0.12963(14) 0.60747(7) 0.0281(4) Uani 1 d . . S3 S 0.77325(8) -0.13072(13) 0.73021(8) 0.0277(4) Uani 1 d . . O1 O 0.6785(3) -0.1962(4) 0.5553(2) 0.0435(11) Uani 1 d . . O2 O 0.8648(3) -0.1990(5) 0.5698(2) 0.0503(12) Uani 1 d . . C1 C 0.7122(3) 0.2050(5) 0.7770(3) 0.0188(11) Uani 1 d . . C2 C 0.8059(3) 0.0616(6) 0.9084(3) 0.0331(14) Uani 1 d . . H2A H 0.8425(3) 0.1395(6) 0.9140(3) 0.05 Uiso 1 calc R . H2B H 0.8275(3) -0.0088(6) 0.8806(3) 0.05 Uiso 1 calc R . H2C H 0.8001(3) 0.0246(6) 0.9541(3) 0.05 Uiso 1 calc R . C3 C 0.6645(4) 0.2288(7) 0.9285(3) 0.040(2) Uani 1 d . . H3A H 0.6116(4) 0.2625(7) 0.9083(3) 0.061 Uiso 1 calc R . H3B H 0.7005(4) 0.3061(7) 0.9409(3) 0.061 Uiso 1 calc R . H3C H 0.6598(4) 0.1756(7) 0.9703(3) 0.061 Uiso 1 calc R . C4 C 0.6433(4) -0.0398(6) 0.8562(3) 0.0378(15) Uani 1 d . . H4A H 0.5894(4) -0.0182(6) 0.8328(3) 0.057 Uiso 1 calc R . H4B H 0.6401(4) -0.0752(6) 0.9028(3) 0.057 Uiso 1 calc R . H4C H 0.6675(4) -0.1086(6) 0.8293(3) 0.057 Uiso 1 calc R . C5 C 0.6728(4) 0.5089(6) 0.8144(3) 0.041(2) Uani 1 d . . H5A H 0.6513(4) 0.4765(6) 0.8556(3) 0.061 Uiso 1 calc R . H5B H 0.6292(4) 0.5165(6) 0.7753(3) 0.061 Uiso 1 calc R . H5C H 0.6976(4) 0.5983(6) 0.8241(3) 0.061 Uiso 1 calc R . C6 C 0.8363(3) 0.4018(6) 0.8641(3) 0.0364(15) Uani 1 d . . H6A H 0.8206(3) 0.3667(6) 0.9073(3) 0.055 Uiso 1 calc R . H6B H 0.8513(3) 0.4979(6) 0.8702(3) 0.055 Uiso 1 calc R . H6C H 0.8820(3) 0.3496(6) 0.8526(3) 0.055 Uiso 1 calc R . C7 C 0.7873(3) 0.4551(6) 0.7128(3) 0.0341(14) Uani 1 d . . H7A H 0.7448(3) 0.4493(6) 0.6728(3) 0.051 Uiso 1 calc R . H7B H 0.8337(3) 0.4022(6) 0.7034(3) 0.051 Uiso 1 calc R . H7C H 0.8030(3) 0.5504(6) 0.7210(3) 0.051 Uiso 1 calc R . C8 C 0.5252(3) 0.2343(6) 0.7728(3) 0.039(2) Uani 1 d . . H8A H 0.5338(3) 0.3198(6) 0.7988(3) 0.058 Uiso 1 calc R . H8B H 0.5227(3) 0.1588(6) 0.8053(3) 0.058 Uiso 1 calc R . H8C H 0.4748(3) 0.2394(6) 0.7407(3) 0.058 Uiso 1 calc R . C9 C 0.5968(4) 0.3391(6) 0.6525(3) 0.0352(14) Uani 1 d . . H9A H 0.6076(4) 0.4290(6) 0.6737(3) 0.053 Uiso 1 calc R . H9B H 0.5416(4) 0.3362(6) 0.6285(3) 0.053 Uiso 1 calc R . H9C H 0.6339(4) 0.3222(6) 0.6192(3) 0.053 Uiso 1 calc R . C10 C 0.5883(3) 0.0411(6) 0.6748(3) 0.0288(13) Uani 1 d . . H10A H 0.5944(3) -0.0342(6) 0.7082(3) 0.043 Uiso 1 calc R . H10B H 0.6255(3) 0.0286(6) 0.6411(3) 0.043 Uiso 1 calc R . H10C H 0.5333(3) 0.0427(6) 0.6504(3) 0.043 Uiso 1 calc R . C11 C 0.8474(4) 0.2222(8) 0.5811(3) 0.051(2) Uani 1 d . . H11A H 0.8275(5) 0.304(3) 0.555(2) 0.077 Uiso 1 calc R . H11B H 0.8752(17) 0.1639(18) 0.552(2) 0.077 Uiso 1 calc R . H11C H 0.8845(15) 0.249(4) 0.6224(4) 0.077 Uiso 1 calc R . C12 C 0.9692(4) 0.0363(7) 0.7065(4) 0.051(2) Uani 1 d . . H12A H 1.0111(19) -0.015(4) 0.7357(5) 0.076 Uiso 1 calc R . H12B H 0.993(2) 0.0910(8) 0.6730(16) 0.076 Uiso 1 calc R . H12C H 0.9303(6) -0.027(3) 0.6815(19) 0.076 Uiso 1 calc R . C13 C 0.8612(4) -0.1983(6) 0.7846(3) 0.043(2) Uani 1 d . . H13A H 0.8834(16) -0.273(3) 0.7604(10) 0.064 Uiso 1 calc R . H13B H 0.8462(6) -0.231(4) 0.8284(10) 0.064 Uiso 1 calc R . H13C H 0.9015(11) -0.1263(13) 0.7944(18) 0.064 Uiso 1 calc R . C14 C 0.6416(4) -0.3163(7) 0.5786(4) 0.054(2) Uani 1 d . . H14A H 0.6377(4) -0.3083(7) 0.6287(4) 0.065 Uiso 1 calc R . H14B H 0.6745(4) -0.3973(7) 0.5718(4) 0.065 Uiso 1 calc R . C15 C 0.5602(4) -0.3315(7) 0.5379(4) 0.050(2) Uani 1 d . . H15A H 0.5215(4) -0.3661(7) 0.5673(4) 0.06 Uiso 1 calc R . H15B H 0.5608(4) -0.3932(7) 0.4978(4) 0.06 Uiso 1 calc R . C16 C 0.5407(4) -0.1861(7) 0.5144(4) 0.050(2) Uani 1 d . . H16A H 0.5008(4) -0.1839(7) 0.4717(4) 0.06 Uiso 1 calc R . H16B H 0.5203(4) -0.1326(7) 0.5512(4) 0.06 Uiso 1 calc R . C17 C 0.6198(5) -0.1351(7) 0.5010(3) 0.052(2) Uani 1 d . . H17A H 0.6303(5) -0.1634(7) 0.4544(3) 0.062 Uiso 1 calc R . H17B H 0.6219(5) -0.0346(7) 0.5039(3) 0.062 Uiso 1 calc R . C18 C 0.8914(12) -0.1728(14) 0.5078(8) 0.208(10) Uani 1 d . . H18A H 0.9097(12) -0.0772(14) 0.5069(8) 0.25 Uiso 1 calc R . H18B H 0.8471(12) -0.1859(14) 0.4690(8) 0.25 Uiso 1 calc R . C19 C 0.9556(6) -0.2622(13) 0.4997(6) 0.106(4) Uani 1 d . . H19A H 1.0073(6) -0.2132(13) 0.5083(6) 0.127 Uiso 1 calc R . H19B H 0.9488(6) -0.2999(13) 0.4520(6) 0.127 Uiso 1 calc R . C20 C 0.9536(5) -0.3712(10) 0.5506(5) 0.069(3) Uani 1 d . . H20A H 0.9311(5) -0.4556(10) 0.5277(5) 0.083 Uiso 1 calc R . H20B H 1.0081(5) -0.3906(10) 0.5751(5) 0.083 Uiso 1 calc R . C21 C 0.9030(6) -0.3204(10) 0.5982(5) 0.084(3) Uani 1 d . . H21A H 0.8623(6) -0.3894(10) 0.6052(5) 0.1 Uiso 1 calc R . H21B H 0.9354(6) -0.3006(10) 0.6437(5) 0.1 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 Al 0.0141(8) 0.0140(8) 0.0273(9) 0.0006(6) 0.0057(6) 0.0008(6) Li 0.035(5) 0.032(6) 0.047(6) -0.009(5) 0.015(5) 0.002(4) Si1 0.0233(8) 0.0252(9) 0.0258(8) -0.0010(6) 0.0056(6) -0.0021(6) Si2 0.0242(8) 0.0158(8) 0.0351(9) -0.0048(6) 0.0002(7) -0.0014(6) Si3 0.0152(7) 0.0200(8) 0.0328(9) -0.0036(6) 0.0004(6) 0.0014(6) S1 0.0186(7) 0.0332(9) 0.0481(9) -0.0055(7) 0.0031(6) -0.0009(6) S2 0.0315(8) 0.0257(8) 0.0283(8) 0.0033(6) 0.0083(6) -0.0014(6) S3 0.0292(8) 0.0149(7) 0.0393(9) 0.0016(6) 0.0059(6) 0.0022(5) O1 0.042(2) 0.031(2) 0.057(3) 0.004(2) 0.001(2) -0.008(2) O2 0.053(3) 0.047(3) 0.056(3) 0.007(2) 0.027(2) 0.023(2) C1 0.016(3) 0.013(3) 0.027(3) 0.000(2) 0.003(2) 0.002(2) C2 0.038(3) 0.029(3) 0.031(3) 0.006(3) 0.000(3) 0.004(3) C3 0.036(3) 0.054(4) 0.034(3) -0.009(3) 0.014(3) -0.002(3) C4 0.040(3) 0.034(3) 0.042(4) 0.006(3) 0.013(3) -0.011(3) C5 0.046(4) 0.021(3) 0.054(4) -0.014(3) 0.006(3) 0.007(3) C6 0.033(3) 0.031(3) 0.043(4) -0.009(3) -0.001(3) -0.010(3) C7 0.036(3) 0.013(3) 0.052(4) 0.000(3) 0.002(3) -0.006(2) C8 0.019(3) 0.040(4) 0.057(4) -0.010(3) 0.006(3) 0.003(3) C9 0.033(3) 0.027(3) 0.042(3) 0.001(3) -0.008(3) 0.006(3) C10 0.018(3) 0.029(3) 0.039(3) -0.007(3) 0.003(2) -0.004(2) C11 0.056(4) 0.065(5) 0.038(4) 0.009(3) 0.021(3) -0.023(4) C12 0.025(3) 0.053(4) 0.076(5) -0.010(4) 0.014(3) 0.005(3) C13 0.049(4) 0.025(3) 0.051(4) 0.001(3) -0.005(3) 0.016(3) C14 0.056(4) 0.041(4) 0.060(4) 0.022(4) -0.009(4) -0.014(3) C15 0.050(4) 0.043(4) 0.059(4) -0.005(3) 0.015(3) -0.003(3) C16 0.042(4) 0.045(4) 0.058(4) -0.007(3) -0.014(3) -0.008(3) C17 0.077(5) 0.038(4) 0.037(4) 0.006(3) -0.003(4) -0.007(4) C18 0.36(2) 0.122(10) 0.200(14) 0.095(10) 0.236(17) 0.129(14) C19 0.074(6) 0.160(11) 0.099(7) -0.059(8) 0.067(6) -0.028(7) C20 0.039(4) 0.094(7) 0.073(6) -0.039(5) 0.002(4) 0.018(4) C21 0.089(7) 0.085(6) 0.082(6) 0.027(5) 0.030(5) 0.056(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 Al C1 2.008(5) . ? Al S1 2.239(2) . ? Al S3 2.305(2) . ? Al S2 2.314(2) . ? Al Li 3.233(10) . ? Li O2 1.899(10) . ? Li O1 1.908(11) . ? Li S2 2.462(10) . ? Li S3 2.483(11) . ? Si1 C2 1.864(6) . ? Si1 C4 1.872(6) . ? Si1 C3 1.887(6) . ? Si1 C1 1.900(5) . ? Si2 C7 1.874(6) . ? Si2 C6 1.882(6) . ? Si2 C5 1.882(6) . ? Si2 C1 1.888(5) . ? Si3 C10 1.868(6) . ? Si3 C9 1.873(6) . ? Si3 C1 1.884(5) . ? Si3 C8 1.888(6) . ? S1 C12 1.834(7) . ? S2 C11 1.816(6) . ? S3 C13 1.818(6) . ? O1 C14 1.438(8) . ? O1 C17 1.466(8) . ? O2 C18 1.371(11) . ? O2 C21 1.428(9) . ? C14 C15 1.489(9) . ? C15 C16 1.521(10) . ? C16 C17 1.486(10) . ? C18 C19 1.42(2) . ? C19 C20 1.463(14) . ? C20 C21 1.439(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 C1 Al S1 115.1(2) . . ? C1 Al S3 113.6(2) . . ? S1 Al S3 107.86(8) . . ? C1 Al S2 113.1(2) . . ? S1 Al S2 107.70(9) . . ? S3 Al S2 98.04(8) . . ? C1 Al Li 136.1(2) . . ? S1 Al Li 108.8(2) . . ? S3 Al Li 49.9(2) . . ? S2 Al Li 49.4(2) . . ? O2 Li O1 110.0(5) . . ? O2 Li S2 119.3(5) . . ? O1 Li S2 110.1(5) . . ? O2 Li S3 116.7(5) . . ? O1 Li S3 109.4(5) . . ? S2 Li S3 89.7(3) . . ? O2 Li Al 123.7(5) . . ? O1 Li Al 126.2(4) . . ? S2 Li Al 45.5(2) . . ? S3 Li Al 45.2(2) . . ? C2 Si1 C4 104.7(3) . . ? C2 Si1 C3 104.8(3) . . ? C4 Si1 C3 105.3(3) . . ? C2 Si1 C1 112.8(2) . . ? C4 Si1 C1 114.3(3) . . ? C3 Si1 C1 114.0(3) . . ? C7 Si2 C6 105.3(3) . . ? C7 Si2 C5 106.4(3) . . ? C6 Si2 C5 104.7(3) . . ? C7 Si2 C1 111.6(2) . . ? C6 Si2 C1 113.7(2) . . ? C5 Si2 C1 114.3(3) . . ? C10 Si3 C9 104.9(3) . . ? C10 Si3 C1 112.2(2) . . ? C9 Si3 C1 114.8(2) . . ? C10 Si3 C8 105.8(3) . . ? C9 Si3 C8 104.4(3) . . ? C1 Si3 C8 113.8(3) . . ? C12 S1 Al 102.8(2) . . ? C11 S2 Al 107.8(2) . . ? C11 S2 Li 114.9(3) . . ? Al S2 Li 85.1(3) . . ? C13 S3 Al 106.9(2) . . ? C13 S3 Li 117.9(3) . . ? Al S3 Li 84.9(2) . . ? C14 O1 C17 106.5(5) . . ? C14 O1 Li 123.3(5) . . ? C17 O1 Li 128.9(5) . . ? C18 O2 C21 108.0(7) . . ? C18 O2 Li 127.1(7) . . ? C21 O2 Li 123.2(5) . . ? Si3 C1 Si2 110.0(2) . . ? Si3 C1 Si1 110.0(2) . . ? Si2 C1 Si1 110.5(3) . . ? Si3 C1 Al 108.9(2) . . ? Si2 C1 Al 108.5(2) . . ? Si1 C1 Al 108.9(2) . . ? O1 C14 C15 108.9(5) . . ? C14 C15 C16 102.0(5) . . ? C17 C16 C15 102.0(6) . . ? O1 C17 C16 105.5(5) . . ? O2 C18 C19 109.6(10) . . ? C18 C19 C20 106.4(7) . . ? C21 C20 C19 104.9(7) . . ? O2 C21 C20 108.5(7) . . ? #===END data_jul1198 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(Tsi)AlH(StBu)2Li(thf)]' _chemical_formula_analytical ? _chemical_formula_sum 'C22 H54 Al Li O S2 Si3' _chemical_formula_weight 516.96 _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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 '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 21.737(4) _cell_length_b 14.610(3) _cell_length_c 23.040(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.150(10) _cell_angle_gamma 90.00 _cell_volume 6623.3(22) _cell_formula_units_Z 8 _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 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.037 _exptl_crystal_density_method ? _exptl_crystal_F_000 2272 _exptl_absorpt_coefficient_mu 0.307 _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 11948 _diffrn_reflns_av_R_equivalents 0.0381 _diffrn_reflns_av_sigmaI/netI 0.0785 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 24.99 _reflns_number_total 11632 _reflns_number_observed 7701 _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_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Hydride H atoms were freely refined isotropic; other H atoms were in riding mode. 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^)+(0.0977P)^2^+8.0487P] 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 11630 _refine_ls_number_parameters 549 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1070 _refine_ls_R_factor_obs 0.0628 _refine_ls_wR_factor_all 0.2043 _refine_ls_wR_factor_obs 0.1568 _refine_ls_goodness_of_fit_all 1.020 _refine_ls_goodness_of_fit_obs 0.977 _refine_ls_restrained_S_all 1.030 _refine_ls_restrained_S_obs 0.977 _refine_ls_shift/esd_max 0.002 _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 Al1 Al 0.44324(6) 0.27316(9) 0.36704(6) 0.0290(3) Uani 1 d . . H1 H 0.4670(24) 0.2898(32) 0.4447(23) 0.048(14) Uiso 1 d . . Al2 Al 0.13817(6) 0.74508(9) 0.48091(6) 0.0244(3) Uani 1 d . . H2 H 0.2173(22) 0.7506(29) 0.5262(21) 0.035(12) Uiso 1 d . . Li1 Li 0.5472(6) 0.2546(7) 0.3123(5) 0.063(3) Uani 1 d . . Li2 Li 0.0277(5) 0.7232(7) 0.5284(5) 0.057(2) Uani 1 d . . S1 S 0.49278(6) 0.14236(9) 0.34766(6) 0.0408(3) Uani 1 d . . S2 S 0.49361(6) 0.38692(9) 0.33103(6) 0.0385(3) Uani 1 d . . S3 S 0.09138(6) 0.61126(8) 0.50173(5) 0.0315(3) Uani 1 d . . S4 S 0.07813(6) 0.85589(8) 0.50763(5) 0.0334(3) Uani 1 d . . Si1 Si 0.30285(6) 0.35957(9) 0.34243(7) 0.0354(3) Uani 1 d . . Si2 Si 0.30962(7) 0.15294(9) 0.31960(7) 0.0405(3) Uani 1 d . . Si3 Si 0.32325(7) 0.29239(9) 0.22400(6) 0.0389(3) Uani 1 d . . Si4 Si 0.02862(7) 0.70616(10) 0.33561(6) 0.0375(3) Uani 1 d . . Si5 Si 0.18457(7) 0.68978(10) 0.37661(6) 0.0377(3) Uani 1 d . . Si6 Si 0.11842(7) 0.87974(9) 0.36550(6) 0.0353(3) Uani 1 d . . O1 O 0.5924(2) 0.2500(3) 0.2598(2) 0.0648(12) Uani 1 d . . O2 O -0.0440(2) 0.7162(3) 0.5513(2) 0.0619(12) Uani 1 d . . C1 C 0.3421(2) 0.2689(3) 0.3101(2) 0.0277(9) Uani 1 d . . C2 C 0.3494(3) 0.4714(3) 0.3596(3) 0.0480(13) Uani 1 d . . H2C H 0.3975(3) 0.4610(3) 0.3879(3) 0.072 Uiso 1 calc R . H2B H 0.3297(3) 0.5129(3) 0.3806(3) 0.072 Uiso 1 calc R . H2A H 0.3454(3) 0.4988(3) 0.3193(3) 0.072 Uiso 1 calc R . C3 C 0.2123(2) 0.3889(4) 0.2883(3) 0.0500(14) Uani 1 d . . H3C H 0.1848(2) 0.3329(4) 0.2773(3) 0.075 Uiso 1 calc R . H3B H 0.2102(2) 0.4174(4) 0.2490(3) 0.075 Uiso 1 calc R . H3A H 0.1945(2) 0.4315(4) 0.3103(3) 0.075 Uiso 1 calc R . C4 C 0.3037(3) 0.3271(4) 0.4219(3) 0.0515(14) Uani 1 d . . H4C H 0.2801(3) 0.2686(4) 0.4176(3) 0.077 Uiso 1 calc R . H4B H 0.2806(3) 0.3746(4) 0.4353(3) 0.077 Uiso 1 calc R . H4A H 0.3508(3) 0.3212(4) 0.4541(3) 0.077 Uiso 1 calc R . C5 C 0.3530(3) 0.1066(4) 0.4035(3) 0.0514(14) Uani 1 d . . H5C H 0.3492(3) 0.1512(4) 0.4336(3) 0.077 Uiso 1 calc R . H5B H 0.4010(3) 0.0955(4) 0.4142(3) 0.077 Uiso 1 calc R . H5A H 0.3313(3) 0.0491(4) 0.4064(3) 0.077 Uiso 1 calc R . C6 C 0.2158(3) 0.1511(4) 0.2999(3) 0.062(2) Uani 1 d . . H6C H 0.1899(3) 0.1746(4) 0.2564(3) 0.093 Uiso 1 calc R . H6B H 0.2073(3) 0.1895(4) 0.3305(3) 0.093 Uiso 1 calc R . H6A H 0.2017(3) 0.0881(4) 0.3025(3) 0.093 Uiso 1 calc R . C7 C 0.3205(3) 0.0616(4) 0.2673(3) 0.063(2) Uani 1 d . . H7C H 0.2989(3) 0.0813(4) 0.2224(3) 0.095 Uiso 1 calc R . H7B H 0.2993(3) 0.0047(4) 0.2722(3) 0.095 Uiso 1 calc R . H7A H 0.3691(3) 0.0511(4) 0.2800(3) 0.095 Uiso 1 calc R . C8 C 0.2361(3) 0.2537(4) 0.1651(3) 0.059(2) Uani 1 d . . H8C H 0.2302(3) 0.1888(4) 0.1720(3) 0.089 Uiso 1 calc R . H8B H 0.2314(3) 0.2627(4) 0.1212(3) 0.089 Uiso 1 calc R . H8A H 0.2014(3) 0.2897(4) 0.1714(3) 0.089 Uiso 1 calc R . C9 C 0.3853(3) 0.2369(4) 0.1976(3) 0.058(2) Uani 1 d . . H9C H 0.3871(3) 0.1710(4) 0.2060(3) 0.086 Uiso 1 calc R . H9B H 0.4305(3) 0.2636(4) 0.2214(3) 0.086 Uiso 1 calc R . H9A H 0.3706(3) 0.2473(4) 0.1516(3) 0.086 Uiso 1 calc R . C10 C 0.3262(3) 0.4159(4) 0.2047(3) 0.0517(14) Uani 1 d . . H10C H 0.3159(3) 0.4224(4) 0.1592(3) 0.078 Uiso 1 calc R . H10B H 0.3717(3) 0.4402(4) 0.2308(3) 0.078 Uiso 1 calc R . H10A H 0.2926(3) 0.4499(4) 0.2141(3) 0.078 Uiso 1 calc R . C11 C 0.5585(3) 0.0826(4) 0.4180(3) 0.0492(13) Uani 1 d . . C12 C 0.5378(4) -0.0185(4) 0.4085(4) 0.082(2) Uani 1 d . . H12C H 0.5363(4) -0.0399(4) 0.3676(4) 0.123 Uiso 1 calc R . H12B H 0.4929(4) -0.0255(4) 0.4082(4) 0.123 Uiso 1 calc R . H12A H 0.5711(4) -0.0547(4) 0.4436(4) 0.123 Uiso 1 calc R . C13 C 0.5611(3) 0.1167(4) 0.4811(3) 0.0544(15) Uani 1 d . . H13C H 0.5167(3) 0.1079(4) 0.4816(3) 0.082 Uiso 1 calc R . H13B H 0.5727(3) 0.1819(4) 0.4860(3) 0.082 Uiso 1 calc R . H13A H 0.5957(3) 0.0824(4) 0.5165(3) 0.082 Uiso 1 calc R . C14 C 0.6267(3) 0.0953(5) 0.4157(3) 0.074(2) Uani 1 d . . H14C H 0.6240(3) 0.0730(5) 0.3746(3) 0.111 Uiso 1 calc R . H14B H 0.6616(3) 0.0608(5) 0.4508(3) 0.111 Uiso 1 calc R . H14A H 0.6387(3) 0.1605(5) 0.4204(3) 0.111 Uiso 1 calc R . C15 C 0.5664(3) 0.4407(4) 0.4000(3) 0.0505(14) Uani 1 d . . C16 C 0.6185(3) 0.3675(6) 0.4344(4) 0.105(3) Uani 1 d . . H16C H 0.6340(3) 0.3391(6) 0.4044(4) 0.158 Uiso 1 calc R . H16B H 0.5980(3) 0.3208(6) 0.4512(4) 0.158 Uiso 1 calc R . H16A H 0.6573(3) 0.3953(6) 0.4700(4) 0.158 Uiso 1 calc R . C17 C 0.5975(3) 0.5076(5) 0.3712(4) 0.080(2) Uani 1 d . . H17C H 0.6133(3) 0.4752(5) 0.3429(4) 0.120 Uiso 1 calc R . H17B H 0.6360(3) 0.5381(5) 0.4055(4) 0.120 Uiso 1 calc R . H17A H 0.5634(3) 0.5534(5) 0.3465(4) 0.120 Uiso 1 calc R . C18 C 0.5411(4) 0.4863(6) 0.4437(4) 0.107(3) Uani 1 d . . H18C H 0.5211(4) 0.4404(6) 0.4616(4) 0.160 Uiso 1 calc R . H18B H 0.5066(4) 0.5319(6) 0.4196(4) 0.160 Uiso 1 calc R . H18A H 0.5791(4) 0.5167(6) 0.4787(4) 0.160 Uiso 1 calc R . C19 C 0.6118(6) 0.3295(6) 0.2358(5) 0.137(4) Uani 1 d . . H19B H 0.6533(6) 0.3571(6) 0.2693(5) 0.164 Uiso 1 calc R . H19A H 0.5749(6) 0.3756(6) 0.2217(5) 0.164 Uiso 1 calc R . C20 C 0.6246(8) 0.2983(7) 0.1811(6) 0.173(6) Uani 1 d . . H20B H 0.6015(8) 0.3391(7) 0.1437(6) 0.207 Uiso 1 calc R . H20A H 0.6739(8) 0.2986(7) 0.1925(6) 0.207 Uiso 1 calc R . C21 C 0.6001(9) 0.2146(8) 0.1676(7) 0.205(8) Uani 1 d . . H21B H 0.6291(9) 0.1769(8) 0.1535(7) 0.246 Uiso 1 calc R . H21A H 0.5536(9) 0.2159(8) 0.1326(7) 0.246 Uiso 1 calc R . C22 C 0.5990(6) 0.1749(6) 0.2268(6) 0.143(5) Uani 1 d . . H22B H 0.5600(6) 0.1327(6) 0.2160(6) 0.171 Uiso 1 calc R . H22A H 0.6416(6) 0.1414(6) 0.2522(6) 0.171 Uiso 1 calc R . C23 C 0.1149(2) 0.7552(3) 0.3863(2) 0.0261(9) Uani 1 d . . C24 C -0.0357(2) 0.7380(4) 0.3668(2) 0.0469(13) Uani 1 d . . H24C H -0.0368(2) 0.8047(4) 0.3709(2) 0.070 Uiso 1 calc R . H24B H -0.0232(2) 0.7096(4) 0.4089(2) 0.070 Uiso 1 calc R . H24A H -0.0808(2) 0.7163(4) 0.3369(2) 0.070 Uiso 1 calc R . C25 C 0.0254(3) 0.5782(4) 0.3301(2) 0.0541(15) Uani 1 d . . H25C H -0.0212(3) 0.5587(4) 0.3030(2) 0.081 Uiso 1 calc R . H25B H 0.0399(3) 0.5521(4) 0.3731(2) 0.081 Uiso 1 calc R . H25A H 0.0558(3) 0.5569(4) 0.3115(2) 0.081 Uiso 1 calc R . C26 C -0.0084(3) 0.7446(4) 0.2491(2) 0.058(2) Uani 1 d . . H26C H -0.0087(3) 0.8116(4) 0.2473(2) 0.087 Uiso 1 calc R . H26B H -0.0550(3) 0.7216(4) 0.2267(2) 0.087 Uiso 1 calc R . H26A H 0.0194(3) 0.7205(4) 0.2283(2) 0.087 Uiso 1 calc R . C27 C 0.1666(3) 0.6618(4) 0.2908(3) 0.062(2) Uani 1 d . . H27C H 0.1568(3) 0.7184(4) 0.2656(3) 0.092 Uiso 1 calc R . H27B H 0.1273(3) 0.6207(4) 0.2727(3) 0.092 Uiso 1 calc R . H27A H 0.2064(3) 0.6318(4) 0.2897(3) 0.092 Uiso 1 calc R . C28 C 0.2022(3) 0.5772(4) 0.4191(2) 0.0482(13) Uani 1 d . . H28C H 0.1604(3) 0.5409(4) 0.4037(2) 0.072 Uiso 1 calc R . H28B H 0.2188(3) 0.5875(4) 0.4653(2) 0.072 Uiso 1 calc R . H28A H 0.2368(3) 0.5442(4) 0.4106(2) 0.072 Uiso 1 calc R . C29 C 0.2681(3) 0.7508(4) 0.4106(3) 0.0516(14) Uani 1 d . . H29C H 0.2628(3) 0.8111(4) 0.3904(3) 0.077 Uiso 1 calc R . H29B H 0.3016(3) 0.7150(4) 0.4022(3) 0.077 Uiso 1 calc R . H29A H 0.2836(3) 0.7584(4) 0.4569(3) 0.077 Uiso 1 calc R . C30 C 0.1323(3) 0.8959(4) 0.2904(3) 0.0539(15) Uani 1 d . . H30C H 0.0969(3) 0.8632(4) 0.2547(3) 0.081 Uiso 1 calc R . H30B H 0.1770(3) 0.8716(4) 0.2975(3) 0.081 Uiso 1 calc R . H30A H 0.1303(3) 0.9613(4) 0.2801(3) 0.081 Uiso 1 calc R . C31 C 0.1887(3) 0.9448(4) 0.4297(3) 0.0512(14) Uani 1 d . . H31C H 0.2320(3) 0.9134(4) 0.4404(3) 0.077 Uiso 1 calc R . H31B H 0.1799(3) 0.9484(4) 0.4680(3) 0.077 Uiso 1 calc R . H31A H 0.1910(3) 1.0068(4) 0.4144(3) 0.077 Uiso 1 calc R . C32 C 0.0390(3) 0.9468(4) 0.3497(3) 0.0525(14) Uani 1 d . . H32C H -0.0002(3) 0.9162(4) 0.3163(3) 0.079 Uiso 1 calc R . H32B H 0.0433(3) 1.0087(4) 0.3356(3) 0.079 Uiso 1 calc R . H32A H 0.0323(3) 0.9503(4) 0.3892(3) 0.079 Uiso 1 calc R . C33 C 0.1460(2) 0.5641(3) 0.5826(2) 0.0343(11) Uani 1 d . . C34 C 0.1098(3) 0.4796(4) 0.5901(3) 0.063(2) Uani 1 d . . H34C H 0.0652(3) 0.4969(4) 0.5877(3) 0.094 Uiso 1 calc R . H34B H 0.1369(3) 0.4510(4) 0.6317(3) 0.094 Uiso 1 calc R . H34A H 0.1038(3) 0.4362(4) 0.5557(3) 0.094 Uiso 1 calc R . C35 C 0.1520(4) 0.6328(4) 0.6336(3) 0.078(2) Uani 1 d . . H35C H 0.1066(4) 0.6477(4) 0.6301(3) 0.117 Uiso 1 calc R . H35B H 0.1739(4) 0.6885(4) 0.6278(3) 0.117 Uiso 1 calc R . H35A H 0.1794(4) 0.6067(4) 0.6760(3) 0.117 Uiso 1 calc R . C36 C 0.2145(3) 0.5390(5) 0.5861(3) 0.072(2) Uani 1 d . . H36C H 0.2089(3) 0.4944(5) 0.5525(3) 0.109 Uiso 1 calc R . H36B H 0.2424(3) 0.5123(5) 0.6282(3) 0.109 Uiso 1 calc R . H36A H 0.2368(3) 0.5940(5) 0.5800(3) 0.109 Uiso 1 calc R . C37 C 0.1260(3) 0.9196(3) 0.5834(2) 0.0454(13) Uani 1 d . . C38 C 0.0884(4) 0.9009(5) 0.6262(3) 0.082(2) Uani 1 d . . H38C H 0.0408(4) 0.9200(5) 0.6035(3) 0.123 Uiso 1 calc R . H38B H 0.1102(4) 0.9356(5) 0.6662(3) 0.123 Uiso 1 calc R . H38A H 0.0903(4) 0.8354(5) 0.6359(3) 0.123 Uiso 1 calc R . C39 C 0.1986(3) 0.8906(4) 0.6176(3) 0.071(2) Uani 1 d . . H39C H 0.2006(3) 0.8254(4) 0.6281(3) 0.107 Uiso 1 calc R . H39B H 0.2207(3) 0.9262(4) 0.6572(3) 0.107 Uiso 1 calc R . H39A H 0.2219(3) 0.9014(4) 0.5901(3) 0.107 Uiso 1 calc R . C40 C 0.1191(4) 1.0191(4) 0.5661(3) 0.080(2) Uani 1 d . . H40C H 0.0709(4) 1.0350(4) 0.5438(3) 0.121 Uiso 1 calc R . H40B H 0.1415(4) 1.0313(4) 0.5378(3) 0.121 Uiso 1 calc R . H40A H 0.1405(4) 1.0559(4) 0.6051(3) 0.121 Uiso 1 calc R . C41 C -0.0629(3) 0.6449(4) 0.5828(3) 0.0485(13) Uani 1 d . . H41B H -0.0301(3) 0.6409(4) 0.6284(3) 0.058 Uiso 1 calc R . H41A H -0.0640(3) 0.5853(4) 0.5620(3) 0.058 Uiso 1 calc R . C42 C -0.1316(3) 0.6691(5) 0.5771(4) 0.071(2) Uani 1 d . . H42B H -0.1665(3) 0.6282(5) 0.5462(4) 0.085 Uiso 1 calc R . H42A H -0.1335(3) 0.6643(5) 0.6192(4) 0.085 Uiso 1 calc R . C43 C -0.1423(4) 0.7619(6) 0.5546(6) 0.126(4) Uani 1 d . . H43B H -0.1878(4) 0.7675(6) 0.5184(6) 0.151 Uiso 1 calc R . H43A H -0.1407(4) 0.8028(6) 0.5894(6) 0.151 Uiso 1 calc R . C44 C -0.0937(5) 0.7878(6) 0.5351(6) 0.144(5) Uani 1 d . . H44B H -0.0719(5) 0.8455(6) 0.5566(6) 0.173 Uiso 1 calc R . H44A H -0.1146(5) 0.7983(6) 0.4882(6) 0.173 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 Al1 0.0261(7) 0.0334(7) 0.0294(7) 0.0017(6) 0.0136(6) 0.0025(6) Al2 0.0258(6) 0.0296(7) 0.0207(6) -0.0001(5) 0.0126(5) -0.0014(5) Li1 0.077(7) 0.063(7) 0.075(7) 0.012(5) 0.056(6) 0.004(5) Li2 0.049(5) 0.066(6) 0.072(7) -0.001(5) 0.042(5) -0.003(5) S1 0.0420(7) 0.0409(7) 0.0389(7) 0.0054(6) 0.0167(6) 0.0133(6) S2 0.0382(7) 0.0395(7) 0.0439(7) 0.0023(6) 0.0231(6) -0.0021(5) S3 0.0321(6) 0.0328(6) 0.0285(6) 0.0061(5) 0.0120(5) -0.0031(5) S4 0.0368(6) 0.0382(6) 0.0265(6) -0.0035(5) 0.0148(5) 0.0060(5) Si1 0.0291(7) 0.0329(7) 0.0477(8) -0.0022(6) 0.0199(6) 0.0010(5) Si2 0.0332(7) 0.0287(7) 0.0503(9) 0.0057(6) 0.0088(6) -0.0024(6) Si3 0.0424(8) 0.0371(8) 0.0301(7) 0.0028(6) 0.0086(6) 0.0055(6) Si4 0.0399(8) 0.0426(8) 0.0233(6) 0.0005(6) 0.0070(6) -0.0098(6) Si5 0.0471(8) 0.0445(8) 0.0305(7) -0.0008(6) 0.0253(6) 0.0055(6) Si6 0.0443(8) 0.0339(7) 0.0324(7) 0.0070(6) 0.0208(6) -0.0019(6) O1 0.089(3) 0.048(2) 0.095(3) 0.008(2) 0.076(3) 0.007(2) O2 0.062(2) 0.052(2) 0.098(3) 0.030(2) 0.061(2) 0.017(2) C1 0.027(2) 0.023(2) 0.030(2) 0.002(2) 0.010(2) 0.005(2) C2 0.055(3) 0.036(3) 0.068(4) -0.011(3) 0.040(3) 0.002(2) C3 0.035(3) 0.047(3) 0.064(4) 0.003(3) 0.017(3) 0.005(2) C4 0.044(3) 0.063(4) 0.061(4) 0.001(3) 0.035(3) 0.000(3) C5 0.049(3) 0.042(3) 0.062(4) 0.025(3) 0.023(3) 0.005(2) C6 0.033(3) 0.052(3) 0.085(5) 0.012(3) 0.011(3) -0.008(3) C7 0.060(4) 0.035(3) 0.070(4) -0.010(3) 0.003(3) -0.008(3) C8 0.055(4) 0.059(4) 0.039(3) 0.001(3) -0.004(3) 0.005(3) C9 0.073(4) 0.072(4) 0.029(3) -0.003(3) 0.023(3) 0.014(3) C10 0.058(3) 0.050(3) 0.047(3) 0.014(3) 0.022(3) 0.010(3) C11 0.040(3) 0.051(3) 0.049(3) 0.014(3) 0.012(3) 0.014(2) C12 0.102(6) 0.039(3) 0.089(5) 0.017(3) 0.023(4) 0.019(4) C13 0.052(3) 0.065(4) 0.043(3) 0.022(3) 0.017(3) 0.014(3) C14 0.041(3) 0.104(6) 0.071(4) -0.003(4) 0.019(3) 0.024(3) C15 0.041(3) 0.054(3) 0.061(4) 0.000(3) 0.026(3) -0.014(3) C16 0.050(4) 0.101(6) 0.113(7) 0.044(5) -0.014(4) -0.017(4) C17 0.071(4) 0.074(5) 0.103(6) 0.005(4) 0.044(4) -0.022(4) C18 0.095(6) 0.141(8) 0.099(6) -0.071(6) 0.056(5) -0.067(6) C19 0.245(12) 0.074(6) 0.195(11) 0.008(6) 0.193(11) 0.003(7) C20 0.360(19) 0.079(6) 0.223(13) -0.009(7) 0.262(15) -0.010(9) C21 0.422(25) 0.106(9) 0.221(15) -0.041(9) 0.265(18) -0.049(12) C22 0.255(13) 0.065(5) 0.218(12) -0.007(6) 0.206(12) -0.003(7) C23 0.028(2) 0.034(2) 0.016(2) 0.003(2) 0.010(2) 0.001(2) C24 0.028(3) 0.062(4) 0.041(3) 0.007(3) 0.005(2) -0.004(2) C25 0.070(4) 0.045(3) 0.038(3) -0.006(2) 0.013(3) -0.019(3) C26 0.058(4) 0.076(4) 0.022(3) 0.004(3) 0.000(2) -0.014(3) C27 0.095(5) 0.064(4) 0.044(3) -0.001(3) 0.047(3) 0.012(3) C28 0.059(3) 0.044(3) 0.047(3) -0.001(2) 0.028(3) 0.013(3) C29 0.039(3) 0.075(4) 0.052(3) 0.011(3) 0.030(3) 0.004(3) C30 0.070(4) 0.058(4) 0.043(3) 0.014(3) 0.033(3) -0.004(3) C31 0.063(4) 0.043(3) 0.050(3) 0.002(3) 0.026(3) -0.012(3) C32 0.069(4) 0.046(3) 0.051(3) 0.023(3) 0.033(3) 0.018(3) C33 0.042(3) 0.037(3) 0.026(2) 0.011(2) 0.017(2) 0.003(2) C34 0.061(4) 0.060(4) 0.060(4) 0.028(3) 0.017(3) -0.005(3) C35 0.134(7) 0.058(4) 0.035(3) 0.004(3) 0.030(4) 0.005(4) C36 0.057(4) 0.106(5) 0.061(4) 0.050(4) 0.032(3) 0.025(4) C37 0.071(4) 0.031(3) 0.028(3) -0.007(2) 0.015(3) 0.002(2) C38 0.123(6) 0.093(5) 0.041(4) -0.005(3) 0.046(4) 0.012(5) C39 0.061(4) 0.058(4) 0.056(4) -0.026(3) -0.014(3) 0.003(3) C40 0.115(6) 0.043(4) 0.060(4) -0.010(3) 0.015(4) -0.001(4) C41 0.062(4) 0.045(3) 0.052(3) 0.002(3) 0.037(3) 0.000(3) C42 0.056(4) 0.074(5) 0.100(5) 0.003(4) 0.049(4) -0.015(3) C43 0.098(6) 0.120(7) 0.212(11) 0.088(7) 0.116(8) 0.051(5) C44 0.114(7) 0.101(7) 0.288(15) 0.106(8) 0.152(9) 0.060(6) _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 Al1 C1 2.026(4) . ? Al1 S1 2.328(2) . ? Al1 S2 2.329(2) . ? Al1 Li1 3.032(9) . ? Al1 H1 1.66(5) . ? Al2 C23 2.023(4) . ? Al2 S4 2.321(2) . ? Al2 S3 2.346(2) . ? Al2 Li2 3.049(9) . ? Al2 H2 1.59(4) . ? Li1 O1 1.856(10) . ? Li1 S1 2.361(10) . ? Li1 S2 2.389(10) . ? Li2 O2 1.850(9) . ? Li2 S4 2.374(10) . ? Li2 S3 2.386(10) . ? S1 C11 1.861(5) . ? S2 C15 1.872(6) . ? S3 C33 1.865(4) . ? S4 C37 1.858(5) . ? Si1 C2 1.874(5) . ? Si1 C3 1.879(5) . ? Si1 C4 1.885(5) . ? Si1 C1 1.892(4) . ? Si2 C5 1.880(5) . ? Si2 C7 1.880(6) . ? Si2 C1 1.884(4) . ? Si2 C6 1.891(5) . ? Si3 C10 1.866(5) . ? Si3 C1 1.879(5) . ? Si3 C9 1.883(6) . ? Si3 C8 1.889(6) . ? Si4 C25 1.873(5) . ? Si4 C23 1.880(4) . ? Si4 C24 1.883(5) . ? Si4 C26 1.891(5) . ? Si5 C28 1.869(5) . ? Si5 C29 1.870(5) . ? Si5 C23 1.882(4) . ? Si5 C27 1.889(5) . ? Si6 C31 1.873(5) . ? Si6 C32 1.882(5) . ? Si6 C23 1.891(4) . ? Si6 C30 1.893(5) . ? O1 C22 1.376(8) . ? O1 C19 1.424(8) . ? O2 C41 1.425(6) . ? O2 C44 1.434(8) . ? C2 H2C 0.98 . ? C2 H2B 0.98 . ? C2 H2A 0.98 . ? C3 H3C 0.98 . ? C3 H3B 0.98 . ? C3 H3A 0.98 . ? C4 H4C 0.98 . ? C4 H4B 0.98 . ? C4 H4A 0.98 . ? C5 H5C 0.98 . ? C5 H5B 0.98 . ? C5 H5A 0.98 . ? C6 H6C 0.98 . ? C6 H6B 0.98 . ? C6 H6A 0.98 . ? C7 H7C 0.98 . ? C7 H7B 0.98 . ? C7 H7A 0.98 . ? C8 H8C 0.98 . ? C8 H8B 0.98 . ? C8 H8A 0.98 . ? C9 H9C 0.98 . ? C9 H9B 0.98 . ? C9 H9A 0.98 . ? C10 H10C 0.98 . ? C10 H10B 0.98 . ? C10 H10A 0.98 . ? C11 C13 1.515(8) . ? C11 C14 1.516(8) . ? C11 C12 1.532(8) . ? C12 H12C 0.98 . ? C12 H12B 0.98 . ? C12 H12A 0.98 . ? C13 H13C 0.98 . ? C13 H13B 0.98 . ? C13 H13A 0.98 . ? C14 H14C 0.98 . ? C14 H14B 0.98 . ? C14 H14A 0.98 . ? C15 C18 1.494(9) . ? C15 C17 1.494(8) . ? C15 C16 1.514(9) . ? C16 H16C 0.98 . ? C16 H16B 0.98 . ? C16 H16A 0.98 . ? C17 H17C 0.98 . ? C17 H17B 0.98 . ? C17 H17A 0.98 . ? C18 H18C 0.98 . ? C18 H18B 0.98 . ? C18 H18A 0.98 . ? C19 C20 1.473(10) . ? C19 H19B 0.99 . ? C19 H19A 0.99 . ? C20 C21 1.318(14) . ? C20 H20B 0.99 . ? C20 H20A 0.99 . ? C21 C22 1.492(13) . ? C21 H21B 0.99 . ? C21 H21A 0.99 . ? C22 H22B 0.99 . ? C22 H22A 0.99 . ? C24 H24C 0.98 . ? C24 H24B 0.98 . ? C24 H24A 0.98 . ? C25 H25C 0.98 . ? C25 H25B 0.98 . ? C25 H25A 0.98 . ? C26 H26C 0.98 . ? C26 H26B 0.98 . ? C26 H26A 0.98 . ? C27 H27C 0.98 . ? C27 H27B 0.98 . ? C27 H27A 0.98 . ? C28 H28C 0.98 . ? C28 H28B 0.98 . ? C28 H28A 0.98 . ? C29 H29C 0.98 . ? C29 H29B 0.98 . ? C29 H29A 0.98 . ? C30 H30C 0.98 . ? C30 H30B 0.98 . ? C30 H30A 0.98 . ? C31 H31C 0.98 . ? C31 H31B 0.98 . ? C31 H31A 0.98 . ? C32 H32C 0.98 . ? C32 H32B 0.98 . ? C32 H32A 0.98 . ? C33 C36 1.501(7) . ? C33 C35 1.508(7) . ? C33 C34 1.512(7) . ? C34 H34C 0.98 . ? C34 H34B 0.98 . ? C34 H34A 0.98 . ? C35 H35C 0.98 . ? C35 H35B 0.98 . ? C35 H35A 0.98 . ? C36 H36C 0.98 . ? C36 H36B 0.98 . ? C36 H36A 0.98 . ? C37 C39 1.494(8) . ? C37 C40 1.498(8) . ? C37 C38 1.548(8) . ? C38 H38C 0.98 . ? C38 H38B 0.98 . ? C38 H38A 0.98 . ? C39 H39C 0.98 . ? C39 H39B 0.98 . ? C39 H39A 0.98 . ? C40 H40C 0.98 . ? C40 H40B 0.98 . ? C40 H40A 0.98 . ? C41 C42 1.486(8) . ? C41 H41B 0.99 . ? C41 H41A 0.99 . ? C42 C43 1.433(10) . ? C42 H42B 0.99 . ? C42 H42A 0.99 . ? C43 C44 1.367(9) . ? C43 H43B 0.99 . ? C43 H43A 0.99 . ? C44 H44B 0.99 . ? C44 H44A 0.99 . ? 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 C1 Al1 S1 108.28(13) . . ? C1 Al1 S2 109.65(14) . . ? S1 Al1 S2 101.05(7) . . ? C1 Al1 Li1 121.5(3) . . ? S1 Al1 Li1 50.2(2) . . ? S2 Al1 Li1 50.9(2) . . ? C1 Al1 H1 117.3(16) . . ? S1 Al1 H1 111.8(16) . . ? S2 Al1 H1 107.6(16) . . ? Li1 Al1 H1 121.2(17) . . ? C23 Al2 S4 108.88(13) . . ? C23 Al2 S3 110.49(14) . . ? S4 Al2 S3 100.70(6) . . ? C23 Al2 Li2 121.4(2) . . ? S4 Al2 Li2 50.3(2) . . ? S3 Al2 Li2 50.4(2) . . ? C23 Al2 H2 114.1(16) . . ? S4 Al2 H2 111.4(16) . . ? S3 Al2 H2 110.5(15) . . ? Li2 Al2 H2 124.6(16) . . ? O1 Li1 S1 133.0(6) . . ? O1 Li1 S2 125.6(5) . . ? S1 Li1 S2 98.4(3) . . ? O1 Li1 Al1 165.8(6) . . ? S1 Li1 Al1 49.2(2) . . ? S2 Li1 Al1 49.1(2) . . ? O2 Li2 S4 128.3(5) . . ? O2 Li2 S3 133.4(5) . . ? S4 Li2 S3 98.0(3) . . ? O2 Li2 Al2 175.0(5) . . ? S4 Li2 Al2 48.7(2) . . ? S3 Li2 Al2 49.3(2) . . ? C11 S1 Al1 117.7(2) . . ? C11 S1 Li1 108.3(3) . . ? Al1 S1 Li1 80.6(3) . . ? C15 S2 Al1 110.6(2) . . ? C15 S2 Li1 101.1(3) . . ? Al1 S2 Li1 80.0(2) . . ? C33 S3 Al2 111.4(2) . . ? C33 S3 Li2 100.9(3) . . ? Al2 S3 Li2 80.3(2) . . ? C37 S4 Al2 116.4(2) . . ? C37 S4 Li2 110.0(3) . . ? Al2 S4 Li2 81.0(2) . . ? C2 Si1 C3 105.2(2) . . ? C2 Si1 C4 103.5(3) . . ? C3 Si1 C4 106.1(2) . . ? C2 Si1 C1 113.6(2) . . ? C3 Si1 C1 114.8(2) . . ? C4 Si1 C1 112.7(2) . . ? C5 Si2 C7 105.0(3) . . ? C5 Si2 C1 113.2(2) . . ? C7 Si2 C1 114.1(2) . . ? C5 Si2 C6 105.1(3) . . ? C7 Si2 C6 104.6(3) . . ? C1 Si2 C6 113.9(2) . . ? C10 Si3 C1 114.4(2) . . ? C10 Si3 C9 103.7(3) . . ? C1 Si3 C9 113.4(2) . . ? C10 Si3 C8 104.1(3) . . ? C1 Si3 C8 114.0(2) . . ? C9 Si3 C8 106.1(3) . . ? C25 Si4 C23 114.9(2) . . ? C25 Si4 C24 105.0(3) . . ? C23 Si4 C24 112.1(2) . . ? C25 Si4 C26 103.8(3) . . ? C23 Si4 C26 114.0(2) . . ? C24 Si4 C26 106.1(3) . . ? C28 Si5 C29 104.7(3) . . ? C28 Si5 C23 112.4(2) . . ? C29 Si5 C23 113.2(2) . . ? C28 Si5 C27 105.2(3) . . ? C29 Si5 C27 105.9(3) . . ? C23 Si5 C27 114.5(2) . . ? C31 Si6 C32 105.2(3) . . ? C31 Si6 C23 113.3(2) . . ? C32 Si6 C23 114.6(2) . . ? C31 Si6 C30 105.4(3) . . ? C32 Si6 C30 104.4(2) . . ? C23 Si6 C30 113.0(2) . . ? C22 O1 C19 108.6(5) . . ? C22 O1 Li1 126.6(5) . . ? C19 O1 Li1 123.3(5) . . ? C41 O2 C44 108.6(4) . . ? C41 O2 Li2 130.2(5) . . ? C44 O2 Li2 121.1(5) . . ? Si3 C1 Si2 111.2(2) . . ? Si3 C1 Si1 110.8(2) . . ? Si2 C1 Si1 109.3(2) . . ? Si3 C1 Al1 111.6(2) . . ? Si2 C1 Al1 108.0(2) . . ? Si1 C1 Al1 105.7(2) . . ? Si1 C2 H2C 109.5(2) . . ? Si1 C2 H2B 109.5(2) . . ? H2C C2 H2B 109.5 . . ? Si1 C2 H2A 109.5(2) . . ? H2C C2 H2A 109.5 . . ? H2B C2 H2A 109.5 . . ? Si1 C3 H3C 109.5(2) . . ? Si1 C3 H3B 109.5(2) . . ? H3C C3 H3B 109.5 . . ? Si1 C3 H3A 109.5(2) . . ? H3C C3 H3A 109.5 . . ? H3B C3 H3A 109.5 . . ? Si1 C4 H4C 109.5(2) . . ? Si1 C4 H4B 109.5(2) . . ? H4C C4 H4B 109.5 . . ? Si1 C4 H4A 109.5(2) . . ? H4C C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? Si2 C5 H5C 109.5(2) . . ? Si2 C5 H5B 109.5(2) . . ? H5C C5 H5B 109.5 . . ? Si2 C5 H5A 109.5(2) . . ? H5C C5 H5A 109.5 . . ? H5B C5 H5A 109.5 . . ? Si2 C6 H6C 109.5(2) . . ? Si2 C6 H6B 109.5(2) . . ? H6C C6 H6B 109.5 . . ? Si2 C6 H6A 109.5(2) . . ? H6C C6 H6A 109.5 . . ? H6B C6 H6A 109.5 . . ? Si2 C7 H7C 109.5(2) . . ? Si2 C7 H7B 109.5(2) . . ? H7C C7 H7B 109.5 . . ? Si2 C7 H7A 109.5(2) . . ? H7C C7 H7A 109.5 . . ? H7B C7 H7A 109.5 . . ? Si3 C8 H8C 109.5(2) . . ? Si3 C8 H8B 109.5(2) . . ? H8C C8 H8B 109.5 . . ? Si3 C8 H8A 109.5(2) . . ? H8C C8 H8A 109.5 . . ? H8B C8 H8A 109.5 . . ? Si3 C9 H9C 109.5(2) . . ? Si3 C9 H9B 109.5(2) . . ? H9C C9 H9B 109.5 . . ? Si3 C9 H9A 109.5(2) . . ? H9C C9 H9A 109.5 . . ? H9B C9 H9A 109.5 . . ? Si3 C10 H10C 109.5(2) . . ? Si3 C10 H10B 109.5(2) . . ? H10C C10 H10B 109.5 . . ? Si3 C10 H10A 109.5(2) . . ? H10C C10 H10A 109.5 . . ? H10B C10 H10A 109.5 . . ? C13 C11 C14 110.7(5) . . ? C13 C11 C12 110.1(5) . . ? C14 C11 C12 110.2(5) . . ? C13 C11 S1 112.5(4) . . ? C14 C11 S1 108.2(4) . . ? C12 C11 S1 104.9(4) . . ? C11 C12 H12C 109.5(4) . . ? C11 C12 H12B 109.5(4) . . ? H12C C12 H12B 109.5 . . ? C11 C12 H12A 109.5(3) . . ? H12C C12 H12A 109.5 . . ? H12B C12 H12A 109.5 . . ? C11 C13 H13C 109.5(3) . . ? C11 C13 H13B 109.5(3) . . ? H13C C13 H13B 109.5 . . ? C11 C13 H13A 109.5(3) . . ? H13C C13 H13A 109.5 . . ? H13B C13 H13A 109.5 . . ? C11 C14 H14C 109.5(3) . . ? C11 C14 H14B 109.5(3) . . ? H14C C14 H14B 109.5 . . ? C11 C14 H14A 109.5(4) . . ? H14C C14 H14A 109.5 . . ? H14B C14 H14A 109.5 . . ? C18 C15 C17 111.8(6) . . ? C18 C15 C16 111.7(7) . . ? C17 C15 C16 108.4(5) . . ? C18 C15 S2 109.9(4) . . ? C17 C15 S2 106.0(4) . . ? C16 C15 S2 108.8(4) . . ? C15 C16 H16C 109.5(4) . . ? C15 C16 H16B 109.5(3) . . ? H16C C16 H16B 109.5 . . ? C15 C16 H16A 109.5(4) . . ? H16C C16 H16A 109.5 . . ? H16B C16 H16A 109.5 . . ? C15 C17 H17C 109.5(4) . . ? C15 C17 H17B 109.5(4) . . ? H17C C17 H17B 109.5 . . ? C15 C17 H17A 109.5(4) . . ? H17C C17 H17A 109.5 . . ? H17B C17 H17A 109.5 . . ? C15 C18 H18C 109.5(4) . . ? C15 C18 H18B 109.5(5) . . ? H18C C18 H18B 109.5 . . ? C15 C18 H18A 109.5(3) . . ? H18C C18 H18A 109.5 . . ? H18B C18 H18A 109.5 . . ? O1 C19 C20 106.0(7) . . ? O1 C19 H19B 110.5(6) . . ? C20 C19 H19B 110.5(8) . . ? O1 C19 H19A 110.5(5) . . ? C20 C19 H19A 110.5(7) . . ? H19B C19 H19A 108.7 . . ? C21 C20 C19 106.5(8) . . ? C21 C20 H20B 110.4(10) . . ? C19 C20 H20B 110.4(7) . . ? C21 C20 H20A 110.4(10) . . ? C19 C20 H20A 110.4(8) . . ? H20B C20 H20A 108.6 . . ? C20 C21 C22 107.8(10) . . ? C20 C21 H21B 110.1(8) . . ? C22 C21 H21B 110.1(6) . . ? C20 C21 H21A 110.1(11) . . ? C22 C21 H21A 110.1(8) . . ? H21B C21 H21A 108.5 . . ? O1 C22 C21 104.0(7) . . ? O1 C22 H22B 111.0(5) . . ? C21 C22 H22B 111.0(8) . . ? O1 C22 H22A 111.0(6) . . ? C21 C22 H22A 111.0(8) . . ? H22B C22 H22A 109.0 . . ? Si5 C23 Si4 111.9(2) . . ? Si5 C23 Si6 109.7(2) . . ? Si4 C23 Si6 110.3(2) . . ? Si5 C23 Al2 104.2(2) . . ? Si4 C23 Al2 111.6(2) . . ? Si6 C23 Al2 109.0(2) . . ? Si4 C24 H24C 109.5(2) . . ? Si4 C24 H24B 109.5(2) . . ? H24C C24 H24B 109.5 . . ? Si4 C24 H24A 109.5(2) . . ? H24C C24 H24A 109.5 . . ? H24B C24 H24A 109.5 . . ? Si4 C25 H25C 109.5(2) . . ? Si4 C25 H25B 109.5(2) . . ? H25C C25 H25B 109.5 . . ? Si4 C25 H25A 109.5(2) . . ? H25C C25 H25A 109.5 . . ? H25B C25 H25A 109.5 . . ? Si4 C26 H26C 109.5(2) . . ? Si4 C26 H26B 109.5(2) . . ? H26C C26 H26B 109.5 . . ? Si4 C26 H26A 109.5(2) . . ? H26C C26 H26A 109.5 . . ? H26B C26 H26A 109.5 . . ? Si5 C27 H27C 109.5(2) . . ? Si5 C27 H27B 109.5(2) . . ? H27C C27 H27B 109.5 . . ? Si5 C27 H27A 109.5(2) . . ? H27C C27 H27A 109.5 . . ? H27B C27 H27A 109.5 . . ? Si5 C28 H28C 109.5(2) . . ? Si5 C28 H28B 109.5(2) . . ? H28C C28 H28B 109.5 . . ? Si5 C28 H28A 109.5(2) . . ? H28C C28 H28A 109.5 . . ? H28B C28 H28A 109.5 . . ? Si5 C29 H29C 109.5(2) . . ? Si5 C29 H29B 109.5(2) . . ? H29C C29 H29B 109.5 . . ? Si5 C29 H29A 109.5(2) . . ? H29C C29 H29A 109.5 . . ? H29B C29 H29A 109.5 . . ? Si6 C30 H30C 109.5(2) . . ? Si6 C30 H30B 109.5(2) . . ? H30C C30 H30B 109.5 . . ? Si6 C30 H30A 109.5(2) . . ? H30C C30 H30A 109.5 . . ? H30B C30 H30A 109.5 . . ? Si6 C31 H31C 109.5(2) . . ? Si6 C31 H31B 109.5(2) . . ? H31C C31 H31B 109.5 . . ? Si6 C31 H31A 109.5(2) . . ? H31C C31 H31A 109.5 . . ? H31B C31 H31A 109.5 . . ? Si6 C32 H32C 109.5(2) . . ? Si6 C32 H32B 109.5(2) . . ? H32C C32 H32B 109.5 . . ? Si6 C32 H32A 109.5(2) . . ? H32C C32 H32A 109.5 . . ? H32B C32 H32A 109.5 . . ? C36 C33 C35 111.4(5) . . ? C36 C33 C34 110.3(5) . . ? C35 C33 C34 109.3(5) . . ? C36 C33 S3 109.9(3) . . ? C35 C33 S3 109.9(4) . . ? C34 C33 S3 105.9(3) . . ? C33 C34 H34C 109.5(3) . . ? C33 C34 H34B 109.5(3) . . ? H34C C34 H34B 109.5 . . ? C33 C34 H34A 109.5(3) . . ? H34C C34 H34A 109.5 . . ? H34B C34 H34A 109.5 . . ? C33 C35 H35C 109.5(4) . . ? C33 C35 H35B 109.5(3) . . ? H35C C35 H35B 109.5 . . ? C33 C35 H35A 109.5(3) . . ? H35C C35 H35A 109.5 . . ? H35B C35 H35A 109.5 . . ? C33 C36 H36C 109.5(3) . . ? #===END  data_feb599 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Li(tmeda)2][(tsi)Al(StBu)3].2.5(benzene)' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H101 Al Li N4 S3 Si3' _chemical_formula_weight 960.71 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' 'S' 'S' 0.1246 0.1234 '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' 'Al' 'Al' 0.0645 0.0514 '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c 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 34.256(7) _cell_length_b 11.863(3) _cell_length_c 30.519(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.88(2) _cell_angle_gamma 90.00 _cell_volume 12218(4) _cell_formula_units_Z 8 _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 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.045 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4232 _exptl_absorpt_coefficient_mu 0.227 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 8619 _diffrn_reflns_av_R_equivalents 0.0824 _diffrn_reflns_av_sigmaI/netI 0.1813 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 2.21 _diffrn_reflns_theta_max 22.99 _reflns_number_total 8468 _reflns_number_gt 4068 _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 ; The C19 t-butyl methyl groups are disordered 0.51:0.49 over two orientations. 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^)+(0.0568P)^2^+19.2268P] 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 8468 _refine_ls_number_parameters 579 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1906 _refine_ls_R_factor_gt 0.0860 _refine_ls_wR_factor_ref 0.2114 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _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 Al Al 0.12904(6) 0.48620(17) 0.42352(7) 0.0270(5) Uani 1 1 d . . . Li Li 0.3751(4) 0.4687(11) 0.3587(4) 0.040(3) Uani 1 1 d . . . S1 S 0.15871(6) 0.5256(2) 0.49499(6) 0.0484(6) Uani 1 1 d . . . S2 S 0.17059(6) 0.39444(17) 0.38398(7) 0.0407(5) Uani 1 1 d . . . S3 S 0.07212(6) 0.38421(18) 0.42213(6) 0.0414(5) Uani 1 1 d . A . Si1 Si 0.07114(6) 0.70419(18) 0.41782(8) 0.0371(6) Uani 1 1 d . . . Si2 Si 0.09416(6) 0.61631(18) 0.33085(7) 0.0341(5) Uani 1 1 d . . . Si3 Si 0.15601(6) 0.73813(18) 0.39974(7) 0.0344(6) Uani 1 1 d . . . N1 N 0.4269(2) 0.5280(7) 0.3984(3) 0.069(2) Uani 1 1 d . . . N2 N 0.3408(3) 0.5364(8) 0.4037(3) 0.091(3) Uani 1 1 d . . . N3 N 0.3701(3) 0.2957(7) 0.3424(3) 0.086(3) Uani 1 1 d . . . N4 N 0.3664(3) 0.5131(9) 0.2920(3) 0.089(3) Uani 1 1 d . . . C1 C 0.11188(19) 0.6391(6) 0.3920(2) 0.0253(17) Uani 1 1 d . . . C2 C 0.0202(2) 0.6490(7) 0.3969(3) 0.048(2) Uani 1 1 d . . . H2A H 0.0145 0.6552 0.3644 0.073 Uiso 1 1 calc R . . H2B H 0.0008 0.6930 0.4098 0.073 Uiso 1 1 calc R . . H2C H 0.0187 0.5697 0.4055 0.073 Uiso 1 1 calc R . . C3 C 0.0769(2) 0.6872(7) 0.4795(2) 0.054(2) Uani 1 1 d . . . H3A H 0.0546 0.7235 0.4901 0.080 Uiso 1 1 calc R . . H3B H 0.1017 0.7224 0.4937 0.080 Uiso 1 1 calc R . . H3C H 0.0773 0.6068 0.4869 0.080 Uiso 1 1 calc R . . C4 C 0.0658(2) 0.8619(7) 0.4092(3) 0.059(3) Uani 1 1 d . . . H4A H 0.0624 0.8789 0.3774 0.089 Uiso 1 1 calc R . . H4B H 0.0896 0.8998 0.4248 0.089 Uiso 1 1 calc R . . H4C H 0.0426 0.8886 0.4211 0.089 Uiso 1 1 calc R . . C5 C 0.0614(2) 0.4901(6) 0.3166(2) 0.042(2) Uani 1 1 d . . . H5A H 0.0536 0.4848 0.2843 0.064 Uiso 1 1 calc R . . H5B H 0.0377 0.4978 0.3304 0.064 Uiso 1 1 calc R . . H5C H 0.0759 0.4218 0.3278 0.064 Uiso 1 1 calc R . . C6 C 0.0638(2) 0.7366(7) 0.3019(3) 0.054(2) Uani 1 1 d . . . H6A H 0.0558 0.7185 0.2703 0.081 Uiso 1 1 calc R . . H6B H 0.0797 0.8056 0.3049 0.081 Uiso 1 1 calc R . . H6C H 0.0401 0.7478 0.3155 0.081 Uiso 1 1 calc R . . C7 C 0.1346(2) 0.5966(7) 0.2967(2) 0.047(2) Uani 1 1 d . . . H7A H 0.1227 0.5857 0.2654 0.071 Uiso 1 1 calc R . . H7B H 0.1505 0.5303 0.3074 0.071 Uiso 1 1 calc R . . H7C H 0.1516 0.6636 0.2995 0.071 Uiso 1 1 calc R . . C8 C 0.2035(2) 0.6705(6) 0.3908(3) 0.042(2) Uani 1 1 d . . . H8A H 0.2092 0.6053 0.4106 0.064 Uiso 1 1 calc R . . H8B H 0.2252 0.7252 0.3973 0.064 Uiso 1 1 calc R . . H8C H 0.2010 0.6457 0.3598 0.064 Uiso 1 1 calc R . . C9 C 0.1676(2) 0.8093(7) 0.4556(3) 0.054(2) Uani 1 1 d . . . H9A H 0.1438 0.8466 0.4622 0.081 Uiso 1 1 calc R . . H9B H 0.1885 0.8655 0.4552 0.081 Uiso 1 1 calc R . . H9C H 0.1766 0.7529 0.4786 0.081 Uiso 1 1 calc R . . C10 C 0.1501(2) 0.8600(6) 0.3597(3) 0.053(2) Uani 1 1 d . . . H10A H 0.1256 0.9008 0.3618 0.080 Uiso 1 1 calc R . . H10B H 0.1488 0.8316 0.3293 0.080 Uiso 1 1 calc R . . H10C H 0.1728 0.9110 0.3670 0.080 Uiso 1 1 calc R . . C11 C 0.2073(2) 0.4644(7) 0.5187(2) 0.0354(19) Uani 1 1 d . . . C12 C 0.2381(2) 0.4848(8) 0.4894(3) 0.064(3) Uani 1 1 d . . . H12A H 0.2299 0.4472 0.4607 0.097 Uiso 1 1 calc R . . H12B H 0.2637 0.4545 0.5040 0.097 Uiso 1 1 calc R . . H12C H 0.2406 0.5660 0.4847 0.097 Uiso 1 1 calc R . . C13 C 0.2039(3) 0.3382(8) 0.5258(3) 0.067(3) Uani 1 1 d . . . H13A H 0.1954 0.3011 0.4970 0.101 Uiso 1 1 calc R . . H13B H 0.1844 0.3239 0.5451 0.101 Uiso 1 1 calc R . . H13C H 0.2298 0.3083 0.5397 0.101 Uiso 1 1 calc R . . C14 C 0.2198(2) 0.5233(8) 0.5630(3) 0.066(3) Uani 1 1 d . . . H14A H 0.2216 0.6046 0.5581 0.100 Uiso 1 1 calc R . . H14B H 0.2457 0.4946 0.5773 0.100 Uiso 1 1 calc R . . H14C H 0.2002 0.5086 0.5822 0.100 Uiso 1 1 calc R . . C15 C 0.1626(2) 0.2405(6) 0.3755(2) 0.0353(19) Uani 1 1 d . . . C16 C 0.1234(3) 0.2160(7) 0.3469(3) 0.074(3) Uani 1 1 d . . . H16A H 0.1020 0.2406 0.3622 0.110 Uiso 1 1 calc R . . H16B H 0.1210 0.1348 0.3411 0.110 Uiso 1 1 calc R . . H16C H 0.1215 0.2566 0.3186 0.110 Uiso 1 1 calc R . . C17 C 0.1654(3) 0.1789(7) 0.4195(3) 0.068(3) Uani 1 1 d . . . H17A H 0.1435 0.2024 0.4343 0.102 Uiso 1 1 calc R . . H17B H 0.1906 0.1971 0.4386 0.102 Uiso 1 1 calc R . . H17C H 0.1639 0.0975 0.4141 0.102 Uiso 1 1 calc R . . C18 C 0.1966(3) 0.2020(7) 0.3525(3) 0.070(3) Uani 1 1 d . . . H18A H 0.1950 0.2414 0.3240 0.105 Uiso 1 1 calc R . . H18B H 0.1946 0.1205 0.3472 0.105 Uiso 1 1 calc R . . H18C H 0.2220 0.2193 0.3715 0.105 Uiso 1 1 calc R . . C19 C 0.0621(2) 0.3087(7) 0.4718(3) 0.044(2) Uani 1 1 d . . . C23 C 0.4135(5) 0.5631(18) 0.4361(7) 0.238(15) Uani 1 1 d . . . H23A H 0.4309 0.6260 0.4488 0.285 Uiso 1 1 calc R . . H23B H 0.4181 0.5004 0.4577 0.285 Uiso 1 1 calc R . . C24 C 0.3737(6) 0.5994(14) 0.4344(5) 0.180(8) Uani 1 1 d . . . H24A H 0.3723 0.6797 0.4255 0.216 Uiso 1 1 calc R . . H24B H 0.3678 0.5956 0.4650 0.216 Uiso 1 1 calc R . . C25 C 0.4588(3) 0.4527(9) 0.4150(4) 0.107(4) Uani 1 1 d . . . H25A H 0.4702 0.4225 0.3901 0.160 Uiso 1 1 calc R . . H25B H 0.4488 0.3904 0.4311 0.160 Uiso 1 1 calc R . . H25C H 0.4793 0.4937 0.4353 0.160 Uiso 1 1 calc R . . C26 C 0.4411(5) 0.6205(14) 0.3746(6) 0.225(11) Uani 1 1 d . . . H26A H 0.4499 0.5917 0.3478 0.338 Uiso 1 1 calc R . . H26B H 0.4634 0.6573 0.3937 0.338 Uiso 1 1 calc R . . H26C H 0.4197 0.6753 0.3661 0.338 Uiso 1 1 calc R . . C27 C 0.3074(4) 0.6054(14) 0.3863(6) 0.189(8) Uani 1 1 d . . . H27A H 0.3160 0.6675 0.3690 0.284 Uiso 1 1 calc R . . H27B H 0.2958 0.6361 0.4110 0.284 Uiso 1 1 calc R . . H27C H 0.2876 0.5598 0.3671 0.284 Uiso 1 1 calc R . . C28 C 0.3253(4) 0.4493(14) 0.4279(5) 0.186(8) Uani 1 1 d . . . H28A H 0.3467 0.3978 0.4404 0.279 Uiso 1 1 calc R . . H28B H 0.3048 0.4076 0.4080 0.279 Uiso 1 1 calc R . . H28C H 0.3137 0.4827 0.4521 0.279 Uiso 1 1 calc R . . C29 C 0.3475(7) 0.303(3) 0.2981(8) 0.34(3) Uani 1 1 d . . . H29A H 0.3201 0.3278 0.2992 0.414 Uiso 1 1 calc R . . H29B H 0.3463 0.2283 0.2835 0.414 Uiso 1 1 calc R . . C30 C 0.3674(9) 0.386(3) 0.2729(7) 0.32(2) Uani 1 1 d . . . H30A H 0.3543 0.3847 0.2413 0.379 Uiso 1 1 calc R . . H30B H 0.3953 0.3625 0.2740 0.379 Uiso 1 1 calc R . . C31 C 0.4090(4) 0.2384(10) 0.3493(4) 0.122(5) Uani 1 1 d . . . H31A H 0.4203 0.2386 0.3810 0.184 Uiso 1 1 calc R . . H31B H 0.4268 0.2782 0.3327 0.184 Uiso 1 1 calc R . . H31C H 0.4055 0.1605 0.3387 0.184 Uiso 1 1 calc R . . C32 C 0.3446(5) 0.2325(12) 0.3661(6) 0.183(8) Uani 1 1 d . . . H32A H 0.3568 0.2271 0.3975 0.274 Uiso 1 1 calc R . . H32B H 0.3407 0.1566 0.3534 0.274 Uiso 1 1 calc R . . H32C H 0.3189 0.2706 0.3635 0.274 Uiso 1 1 calc R . . C33 C 0.3971(4) 0.5666(17) 0.2747(5) 0.202(10) Uani 1 1 d . . . H33A H 0.4007 0.6433 0.2867 0.303 Uiso 1 1 calc R . . H33B H 0.3903 0.5699 0.2422 0.303 Uiso 1 1 calc R . . H33C H 0.4218 0.5239 0.2832 0.303 Uiso 1 1 calc R . . C34 C 0.3317(4) 0.5816(13) 0.2808(4) 0.149(6) Uani 1 1 d . . . H34A H 0.3360 0.6542 0.2962 0.224 Uiso 1 1 calc R . . H34B H 0.3091 0.5432 0.2899 0.224 Uiso 1 1 calc R . . H34C H 0.3263 0.5943 0.2486 0.224 Uiso 1 1 calc R . . C35 C 0.2228(2) 0.4179(7) 0.2652(3) 0.046(2) Uani 1 1 d . . . H35 H 0.2134 0.4203 0.2927 0.055 Uiso 1 1 calc R . . C36 C 0.2379(2) 0.3195(7) 0.2513(3) 0.055(2) Uani 1 1 d . . . H36 H 0.2392 0.2540 0.2694 0.066 Uiso 1 1 calc R . . C37 C 0.2511(3) 0.3158(8) 0.2111(3) 0.057(3) Uani 1 1 d . . . H37 H 0.2613 0.2476 0.2011 0.069 Uiso 1 1 calc R . . C38 C 0.2495(2) 0.4115(8) 0.1858(3) 0.051(2) Uani 1 1 d . . . H38 H 0.2590 0.4094 0.1583 0.061 Uiso 1 1 calc R . . C39 C 0.2347(2) 0.5092(7) 0.1991(3) 0.049(2) Uani 1 1 d . . . H39 H 0.2335 0.5748 0.1811 0.059 Uiso 1 1 calc R . . C40 C 0.2211(2) 0.5120(7) 0.2393(3) 0.048(2) Uani 1 1 d . . . H40 H 0.2107 0.5800 0.2490 0.058 Uiso 1 1 calc R . . C41 C 0.0779(5) 0.4040(9) 0.1844(4) 0.088(4) Uani 1 1 d . . . H41 H 0.0669 0.3987 0.2109 0.106 Uiso 1 1 calc R . . C42 C 0.0535(3) 0.4171(8) 0.1437(5) 0.077(3) Uani 1 1 d . . . H42 H 0.0255 0.4188 0.1416 0.092 Uiso 1 1 calc R . . C43 C 0.0704(3) 0.4276(8) 0.1067(4) 0.068(3) Uani 1 1 d . . . H43 H 0.0539 0.4389 0.0786 0.082 Uiso 1 1 calc R . . C44 C 0.1100(3) 0.4221(7) 0.1091(3) 0.061(3) Uani 1 1 d . . . H44 H 0.1213 0.4288 0.0829 0.073 Uiso 1 1 calc R . . C45 C 0.1336(3) 0.4070(8) 0.1488(5) 0.073(3) Uani 1 1 d . . . H45 H 0.1615 0.4022 0.1504 0.087 Uiso 1 1 calc R . . C46 C 0.1179(4) 0.3988(9) 0.1860(4) 0.082(4) Uani 1 1 d . . . H46 H 0.1349 0.3892 0.2138 0.098 Uiso 1 1 calc R . . C47 C 0.0000 0.2327(13) 0.2500 0.077(5) Uani 1 2 d S . . H47 H 0.0000 0.3128 0.2500 0.093 Uiso 1 2 calc SR . . C48 C 0.0177(3) 0.1791(12) 0.2865(4) 0.094(4) Uani 1 1 d . . . H48 H 0.0300 0.2203 0.3118 0.113 Uiso 1 1 calc R . . C49 C 0.0178(3) 0.0629(13) 0.2867(5) 0.106(5) Uani 1 1 d . . . H49 H 0.0301 0.0223 0.3122 0.128 Uiso 1 1 calc R . . C50 C 0.0000 0.0080(18) 0.2500 0.114(8) Uani 1 2 d S . . H50 H 0.0000 -0.0721 0.2500 0.137 Uiso 1 2 calc SR . . C20 C 0.0962(7) 0.300(2) 0.5089(7) 0.050(7) Uani 0.51(3) 1 d P A 1 H20A H 0.1179 0.2598 0.4988 0.075 Uiso 0.51(3) 1 calc PR A 1 H20B H 0.0880 0.2588 0.5337 0.075 Uiso 0.51(3) 1 calc PR A 1 H20C H 0.1050 0.3758 0.5189 0.075 Uiso 0.51(3) 1 calc PR A 1 C21 C 0.0267(8) 0.365(4) 0.4860(10) 0.132(19) Uani 0.51(3) 1 d P A 1 H21A H 0.0053 0.3726 0.4603 0.198 Uiso 0.51(3) 1 calc PR A 1 H21B H 0.0343 0.4403 0.4980 0.198 Uiso 0.51(3) 1 calc PR A 1 H21C H 0.0174 0.3196 0.5090 0.198 Uiso 0.51(3) 1 calc PR A 1 C22 C 0.0514(12) 0.185(2) 0.4531(8) 0.091(12) Uani 0.51(3) 1 d P A 1 H22A H 0.0285 0.1886 0.4290 0.136 Uiso 0.51(3) 1 calc PR A 1 H22B H 0.0450 0.1372 0.4771 0.136 Uiso 0.51(3) 1 calc PR A 1 H22C H 0.0741 0.1532 0.4418 0.136 Uiso 0.51(3) 1 calc PR A 1 C20A C 0.0964(7) 0.233(3) 0.4917(11) 0.077(11) Uani 0.49(3) 1 d P A 2 H20D H 0.1209 0.2769 0.4967 0.115 Uiso 0.49(3) 1 calc PR A 2 H20E H 0.0988 0.1711 0.4711 0.115 Uiso 0.49(3) 1 calc PR A 2 H20F H 0.0914 0.2022 0.5200 0.115 Uiso 0.49(3) 1 calc PR A 2 C21A C 0.0548(10) 0.396(2) 0.5078(9) 0.080(10) Uani 0.49(3) 1 d P A 2 H21D H 0.0784 0.4434 0.5159 0.120 Uiso 0.49(3) 1 calc PR A 2 H21E H 0.0495 0.3561 0.5342 0.120 Uiso 0.49(3) 1 calc PR A 2 H21F H 0.0321 0.4437 0.4959 0.120 Uiso 0.49(3) 1 calc PR A 2 C22A C 0.0254(7) 0.240(2) 0.4598(7) 0.057(8) Uani 0.49(3) 1 d P A 2 H22D H 0.0030 0.2903 0.4495 0.086 Uiso 0.49(3) 1 calc PR A 2 H22E H 0.0205 0.1984 0.4860 0.086 Uiso 0.49(3) 1 calc PR A 2 H22F H 0.0287 0.1873 0.4361 0.086 Uiso 0.49(3) 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 Al 0.0288(12) 0.0241(13) 0.0296(12) -0.0011(10) 0.0089(10) -0.0022(10) Li 0.046(8) 0.034(8) 0.043(8) 0.004(7) 0.013(6) 0.010(7) S1 0.0417(13) 0.0717(17) 0.0301(12) -0.0089(11) 0.0018(10) 0.0124(12) S2 0.0486(13) 0.0268(11) 0.0526(13) -0.0027(11) 0.0257(11) 0.0008(10) S3 0.0417(12) 0.0454(13) 0.0361(12) 0.0052(11) 0.0033(10) -0.0145(11) Si1 0.0324(13) 0.0329(13) 0.0490(14) -0.0039(11) 0.0156(11) 0.0016(11) Si2 0.0400(13) 0.0321(13) 0.0309(12) 0.0043(11) 0.0082(10) 0.0019(11) Si3 0.0326(12) 0.0296(13) 0.0435(14) -0.0005(11) 0.0135(10) -0.0070(10) N1 0.045(5) 0.045(5) 0.112(7) -0.006(5) -0.004(5) -0.005(4) N2 0.098(7) 0.090(7) 0.103(7) 0.019(6) 0.070(6) 0.039(6) N3 0.120(8) 0.046(6) 0.080(7) -0.015(5) -0.014(6) 0.022(6) N4 0.113(8) 0.114(8) 0.044(5) 0.021(5) 0.025(5) 0.031(7) C1 0.027(4) 0.023(4) 0.027(4) 0.002(3) 0.010(3) -0.001(3) C2 0.034(5) 0.051(6) 0.064(6) 0.005(5) 0.018(4) 0.004(4) C3 0.050(5) 0.066(6) 0.051(6) -0.027(5) 0.026(5) 0.001(5) C4 0.056(6) 0.045(6) 0.081(7) -0.006(5) 0.022(5) 0.008(5) C5 0.058(5) 0.045(5) 0.021(4) 0.005(4) 0.000(4) -0.002(4) C6 0.053(6) 0.055(6) 0.052(6) 0.016(5) 0.004(5) 0.010(5) C7 0.062(6) 0.046(5) 0.037(5) 0.001(4) 0.019(4) 0.009(5) C8 0.037(5) 0.038(5) 0.055(5) 0.003(4) 0.014(4) -0.013(4) C9 0.047(5) 0.051(6) 0.064(6) -0.018(5) 0.011(5) -0.021(5) C10 0.050(5) 0.034(5) 0.081(7) 0.011(5) 0.025(5) 0.006(4) C11 0.032(4) 0.045(5) 0.026(4) -0.002(4) -0.004(4) -0.008(4) C12 0.036(5) 0.101(8) 0.054(6) 0.027(6) 0.000(4) -0.003(5) C13 0.051(6) 0.065(7) 0.083(7) -0.001(6) 0.000(5) -0.005(5) C14 0.056(6) 0.095(8) 0.042(5) -0.018(5) -0.010(5) -0.002(6) C15 0.050(5) 0.018(4) 0.039(5) 0.001(4) 0.009(4) 0.011(4) C16 0.083(7) 0.046(6) 0.083(7) -0.028(5) -0.010(6) 0.003(5) C17 0.100(8) 0.050(6) 0.057(6) 0.014(5) 0.019(6) 0.016(6) C18 0.096(8) 0.042(6) 0.084(7) -0.009(5) 0.050(6) 0.013(5) C19 0.037(5) 0.047(6) 0.049(5) 0.012(5) 0.008(4) -0.016(4) C23 0.123(14) 0.31(3) 0.24(2) -0.20(2) -0.103(15) 0.138(17) C24 0.26(2) 0.181(17) 0.113(12) -0.120(13) 0.066(14) -0.062(17) C25 0.059(7) 0.083(9) 0.165(12) 0.016(8) -0.020(8) 0.009(7) C26 0.168(16) 0.176(17) 0.30(2) 0.137(17) -0.059(16) -0.119(14) C27 0.121(12) 0.216(19) 0.25(2) 0.043(16) 0.094(13) 0.101(13) C28 0.129(12) 0.24(2) 0.226(17) 0.119(16) 0.143(13) 0.061(13) C29 0.17(2) 0.65(7) 0.21(3) -0.36(4) 0.025(19) -0.12(3) C30 0.31(4) 0.52(6) 0.136(19) -0.21(3) 0.08(2) -0.02(4) C31 0.116(11) 0.067(9) 0.182(14) -0.048(9) 0.018(10) 0.003(8) C32 0.23(2) 0.107(13) 0.23(2) -0.048(13) 0.081(17) -0.075(14) C33 0.137(13) 0.32(3) 0.178(16) 0.156(17) 0.102(13) 0.062(15) C34 0.122(11) 0.225(18) 0.092(10) 0.021(11) -0.007(9) 0.073(13) C35 0.047(5) 0.045(6) 0.051(6) -0.008(5) 0.027(4) -0.001(4) C36 0.063(6) 0.046(6) 0.062(6) 0.010(5) 0.027(5) 0.012(5) C37 0.067(7) 0.042(6) 0.067(7) -0.007(5) 0.021(5) 0.019(5) C38 0.042(5) 0.068(7) 0.044(5) 0.003(5) 0.013(4) 0.003(5) C39 0.036(5) 0.045(6) 0.068(6) 0.021(5) 0.009(5) 0.000(4) C40 0.049(5) 0.034(5) 0.067(6) -0.005(5) 0.024(5) 0.000(4) C41 0.133(12) 0.060(8) 0.088(10) -0.021(7) 0.066(9) -0.002(8) C42 0.056(7) 0.052(7) 0.126(11) -0.007(7) 0.024(8) 0.012(5) C43 0.067(8) 0.051(7) 0.083(8) 0.010(6) 0.000(6) 0.005(5) C44 0.069(7) 0.048(6) 0.074(8) -0.017(5) 0.034(6) -0.013(5) C45 0.052(6) 0.042(6) 0.114(10) -0.022(7) -0.017(7) -0.006(5) C46 0.128(12) 0.064(8) 0.044(7) -0.007(6) -0.012(7) 0.000(8) C47 0.049(10) 0.050(10) 0.135(16) 0.000 0.020(10) 0.000 C48 0.049(7) 0.096(10) 0.131(12) 0.000(9) -0.006(7) -0.011(7) C49 0.044(8) 0.122(13) 0.155(15) 0.070(11) 0.019(8) 0.030(8) C50 0.060(14) 0.094(16) 0.19(3) 0.000 0.031(15) 0.000 C20 0.071(14) 0.044(15) 0.034(12) 0.018(10) 0.007(11) -0.032(13) C21 0.047(18) 0.26(5) 0.10(2) 0.09(3) 0.054(18) 0.03(3) C22 0.13(3) 0.059(18) 0.076(16) 0.016(13) -0.018(17) -0.053(18) C20A 0.031(12) 0.10(3) 0.09(2) 0.07(2) -0.009(14) -0.006(16) C21A 0.07(2) 0.10(2) 0.080(18) -0.003(15) 0.044(16) -0.029(18) C22A 0.047(15) 0.062(18) 0.068(14) 0.008(13) 0.026(12) -0.021(13) _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 Al C1 2.090(7) . ? Al S3 2.289(3) . ? Al S1 2.291(3) . ? Al S2 2.293(3) . ? Li N4 2.076(14) . ? Li N1 2.090(15) . ? Li N3 2.111(15) . ? Li N2 2.112(14) . ? S1 C11 1.846(7) . ? S2 C15 1.858(7) . ? S3 C19 1.842(8) . ? Si1 C2 1.869(7) . ? Si1 C3 1.869(8) . ? Si1 C1 1.883(7) . ? Si1 C4 1.893(8) . ? Si2 C5 1.876(7) . ? Si2 C1 1.879(7) . ? Si2 C7 1.886(7) . ? Si2 C6 1.893(8) . ? Si3 C8 1.877(7) . ? Si3 C10 1.882(8) . ? Si3 C9 1.884(8) . ? Si3 C1 1.897(7) . ? N1 C23 1.372(19) . ? N1 C25 1.437(11) . ? N1 C26 1.448(14) . ? N2 C28 1.426(14) . ? N2 C27 1.431(14) . ? N2 C24 1.532(16) . ? N3 C32 1.437(15) . ? N3 C29 1.44(3) . ? N3 C31 1.478(13) . ? N4 C33 1.407(15) . ? N4 C34 1.432(13) . ? N4 C30 1.62(3) . ? C11 C12 1.512(10) . ? C11 C14 1.517(10) . ? C11 C13 1.520(11) . ? C15 C16 1.500(10) . ? C15 C17 1.517(10) . ? C15 C18 1.529(10) . ? C19 C20 1.49(2) . ? C19 C22A 1.49(2) . ? C19 C21 1.51(2) . ? C19 C20A 1.52(2) . ? C19 C21A 1.56(2) . ? C19 C22 1.59(2) . ? C23 C24 1.421(19) . ? C29 C30 1.48(4) . ? C35 C40 1.362(10) . ? C35 C36 1.372(10) . ? C36 C37 1.381(11) . ? C37 C38 1.369(11) . ? C38 C39 1.357(11) . ? C39 C40 1.384(10) . ? C41 C46 1.365(14) . ? C41 C42 1.382(14) . ? C42 C43 1.359(13) . ? C43 C44 1.348(12) . ? C44 C45 1.348(12) . ? C45 C46 1.340(14) . ? C47 C48 1.334(13) . ? C47 C48 1.334(13) 6_556 ? C48 C49 1.379(16) . ? C49 C50 1.348(16) . ? C50 C49 1.348(16) 6_556 ? 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 C1 Al S3 106.2(2) . . ? C1 Al S1 107.8(2) . . ? S3 Al S1 111.27(11) . . ? C1 Al S2 108.7(2) . . ? S3 Al S2 110.07(11) . . ? S1 Al S2 112.58(12) . . ? N4 Li N1 116.6(7) . . ? N4 Li N3 91.3(6) . . ? N1 Li N3 119.4(7) . . ? N4 Li N2 122.6(7) . . ? N1 Li N2 90.4(6) . . ? N3 Li N2 119.4(7) . . ? C11 S1 Al 121.0(2) . . ? C15 S2 Al 116.8(3) . . ? C19 S3 Al 121.4(3) . . ? C2 Si1 C3 103.7(4) . . ? C2 Si1 C1 115.3(3) . . ? C3 Si1 C1 114.9(3) . . ? C2 Si1 C4 103.7(4) . . ? C3 Si1 C4 103.7(4) . . ? C1 Si1 C4 114.1(3) . . ? C5 Si2 C1 115.0(3) . . ? C5 Si2 C7 103.9(4) . . ? C1 Si2 C7 115.1(3) . . ? C5 Si2 C6 103.6(3) . . ? C1 Si2 C6 114.4(3) . . ? C7 Si2 C6 103.4(4) . . ? C8 Si3 C10 103.5(3) . . ? C8 Si3 C9 105.6(4) . . ? C10 Si3 C9 103.1(4) . . ? C8 Si3 C1 114.2(3) . . ? C10 Si3 C1 113.6(3) . . ? C9 Si3 C1 115.6(3) . . ? C23 N1 C25 103.7(10) . . ? C23 N1 C26 112.3(13) . . ? C25 N1 C26 110.3(10) . . ? C23 N1 Li 102.5(9) . . ? C25 N1 Li 121.0(7) . . ? C26 N1 Li 106.9(8) . . ? C28 N2 C27 105.2(10) . . ? C28 N2 C24 109.6(12) . . ? C27 N2 C24 113.9(13) . . ? C28 N2 Li 111.1(9) . . ? C27 N2 Li 118.4(9) . . ? C24 N2 Li 98.6(8) . . ? C32 N3 C29 103.2(15) . . ? C32 N3 C31 107.4(10) . . ? C29 N3 C31 119.1(14) . . ? C32 N3 Li 114.9(9) . . ? C29 N3 Li 100.0(16) . . ? C31 N3 Li 112.2(8) . . ? C33 N4 C34 107.3(11) . . ? C33 N4 C30 102.9(13) . . ? C34 N4 C30 120.7(15) . . ? C33 N4 Li 119.5(10) . . ? C34 N4 Li 110.6(8) . . ? C30 N4 Li 96.2(12) . . ? Si2 C1 Si1 109.8(3) . . ? Si2 C1 Si3 109.1(3) . . ? Si1 C1 Si3 109.0(3) . . ? Si2 C1 Al 110.5(3) . . ? Si1 C1 Al 109.4(3) . . ? Si3 C1 Al 109.0(3) . . ? C12 C11 C14 109.4(7) . . ? C12 C11 C13 108.6(7) . . ? C14 C11 C13 110.1(7) . . ? C12 C11 S1 112.3(5) . . ? C14 C11 S1 105.4(5) . . ? C13 C11 S1 110.9(5) . . ? C16 C15 C17 109.6(7) . . ? C16 C15 C18 110.6(7) . . ? C17 C15 C18 109.0(7) . . ? C16 C15 S2 111.5(5) . . ? C17 C15 S2 111.4(6) . . ? C18 C15 S2 104.6(5) . . ? C20 C19 C22A 132.0(13) . . ? C20 C19 C21 112.0(16) . . ? C22A C19 C21 68.2(14) . . ? C20 C19 C20A 37.0(12) . . ? C22A C19 C20A 109.7(14) . . ? C21 C19 C20A 138.5(15) . . ? C20 C19 C21A 73.0(13) . . ? C22A C19 C21A 107.8(12) . . ? C21 C19 C21A 43.2(13) . . ? C20A C19 C21A 108.4(16) . . ? C20 C19 C22 108.1(12) . . ? C22A C19 C22 43.7(11) . . ? C21 C19 C22 111.4(17) . . ? C20A C19 C22 73.3(14) . . ? C21A C19 C22 143.9(15) . . ? C20 C19 S3 115.4(9) . . ? C22A C19 S3 109.4(10) . . ? C21 C19 S3 107.0(10) . . ? C20A C19 S3 112.0(11) . . ? C21A C19 S3 109.3(10) . . ? C22 C19 S3 102.6(10) . . ? N1 C23 C24 121.1(13) . . ? C23 C24 N2 118.4(12) . . ? N3 C29 C30 107.8(19) . . ? C29 C30 N4 113.0(18) . . ? C40 C35 C36 119.9(8) . . ? C35 C36 C37 120.0(8) . . ? C38 C37 C36 119.2(8) . . ? C39 C38 C37 121.3(8) . . ? C38 C39 C40 119.1(8) . . ? C35 C40 C39 120.4(8) . . ? C46 C41 C42 118.9(11) . . ? C43 C42 C41 118.8(10) . . ? C44 C43 C42 121.0(10) . . ? C43 C44 C45 120.0(10) . . ? C46 C45 C44 120.3(10) . . ? C45 C46 C41 120.9(11) . . ? C48 C47 C48 123.1(17) . 6_556 ? C47 C48 C49 118.8(14) . . ? C50 C49 C48 118.6(16) . . ? C49 C50 C49 122(2) 6_556 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.380 _refine_diff_density_min -0.374 _refine_diff_density_rms 0.068 #===END