# Copyright The Royal Society of Chemistry, 1998 data_apr1295 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li(thf)4][(Me3Si)3CAl(NHPh)3]' _chemical_formula_analytical ? _chemical_formula_sum 'C44 H77 Al Li N3 O4 Si3' _chemical_formula_weight 830.28 _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' '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 16.087(5) _cell_length_b 16.907(6) _cell_length_c 18.360(11) _cell_angle_alpha 90.00 _cell_angle_beta 98.59(4) _cell_angle_gamma 90.00 _cell_volume 4937.6(38) _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 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.117 _exptl_crystal_density_method ? _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.154 _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 8985 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.1172 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8666 _reflns_number_observed 4799 _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 ; 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^)+(0.0569P)^2^+4.6808P] 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 8666 _refine_ls_number_parameters 505 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_obs 0.0735 _refine_ls_wR_factor_all 0.1919 _refine_ls_wR_factor_obs 0.1527 _refine_ls_goodness_of_fit_all 1.017 _refine_ls_goodness_of_fit_obs 1.107 _refine_ls_restrained_S_all 1.017 _refine_ls_restrained_S_obs 1.107 _refine_ls_shift/esd_max -0.001 _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 Al Al 0.23846(8) 0.85847(8) 0.05679(7) 0.0341(3) Uani 1 d . . Si1 Si 0.19296(8) 1.00790(7) 0.14779(7) 0.0365(3) Uani 1 d . . Si2 Si 0.11153(8) 0.84891(8) 0.17772(7) 0.0386(3) Uani 1 d . . Si3 Si 0.30120(8) 0.87415(8) 0.22723(7) 0.0384(3) Uani 1 d . . N1 N 0.2830(2) 0.7579(2) 0.0736(2) 0.0402(10) Uani 1 d . . H1 H 0.2526(2) 0.7307(2) 0.1009(2) 0.048 Uiso 1 calc R . N2 N 0.1424(2) 0.8522(2) -0.0124(2) 0.0370(9) Uani 1 d . . H2 H 0.0980(2) 0.8753(2) 0.0008(2) 0.044 Uiso 1 calc R . N3 N 0.3181(2) 0.9215(2) 0.0224(2) 0.0418(10) Uani 1 d . . H3 H 0.3691(2) 0.9099(2) 0.0444(2) 0.050 Uiso 1 calc R . Li Li 0.8167(5) 0.5781(5) 0.1383(5) 0.050(2) Uani 1 d . . O1 O 0.8869(2) 0.6165(2) 0.2234(2) 0.0644(11) Uani 1 d . . O2 O 0.7145(2) 0.5324(2) 0.1598(2) 0.0629(11) Uani 1 d . . O3 O 0.7900(2) 0.6659(2) 0.0755(2) 0.0622(11) Uani 1 d . . O4 O 0.8731(2) 0.5023(2) 0.0852(2) 0.0627(10) Uani 1 d . . C1 C 0.2094(3) 0.8981(2) 0.1551(2) 0.0296(10) Uani 1 d . . C2 C 0.1276(3) 1.0384(3) 0.0590(3) 0.0454(12) Uani 1 d . . H2A H 0.1530(3) 1.0180(3) 0.0175(3) 0.068 Uiso 1 calc R . H2B H 0.1248(3) 1.0963(3) 0.0563(3) 0.068 Uiso 1 calc R . H2C H 0.0707(3) 1.0169(3) 0.0567(3) 0.068 Uiso 1 calc R . C3 C 0.2926(3) 1.0667(3) 0.1529(3) 0.0474(13) Uani 1 d . . H3A H 0.3252(3) 1.0476(3) 0.1154(3) 0.071 Uiso 1 calc R . H3B H 0.3257(3) 1.0605(3) 0.2019(3) 0.071 Uiso 1 calc R . H3C H 0.2788(3) 1.1227(3) 0.1441(3) 0.071 Uiso 1 calc R . C4 C 0.1377(3) 1.0504(3) 0.2216(3) 0.0491(13) Uani 1 d . . H4A H 0.0845(3) 1.0224(3) 0.2223(3) 0.074 Uiso 1 calc R . H4B H 0.1264(3) 1.1067(3) 0.2117(3) 0.074 Uiso 1 calc R . H4C H 0.1733(3) 1.0445(3) 0.2695(3) 0.074 Uiso 1 calc R . C5 C 0.0988(3) 0.8541(3) 0.2780(3) 0.0516(14) Uani 1 d . . H5A H 0.1022(3) 0.9094(3) 0.2942(3) 0.077 Uiso 1 calc R . H5B H 0.1437(3) 0.8235(3) 0.3072(3) 0.077 Uiso 1 calc R . H5C H 0.0441(3) 0.8321(3) 0.2845(3) 0.077 Uiso 1 calc R . C6 C 0.1041(3) 0.7412(3) 0.1530(3) 0.0530(14) Uani 1 d . . H6A H 0.1550(3) 0.7139(3) 0.1763(3) 0.080 Uiso 1 calc R . H6B H 0.0987(3) 0.7353(3) 0.0994(3) 0.080 Uiso 1 calc R . H6C H 0.0548(3) 0.7180(3) 0.1705(3) 0.080 Uiso 1 calc R . C7 C 0.0098(3) 0.8901(3) 0.1287(3) 0.0498(13) Uani 1 d . . H7A H 0.0073(3) 0.9470(3) 0.1382(3) 0.075 Uiso 1 calc R . H7B H -0.0374(3) 0.8637(3) 0.1467(3) 0.075 Uiso 1 calc R . H7C H 0.0064(3) 0.8810(3) 0.0756(3) 0.075 Uiso 1 calc R . C8 C 0.4064(3) 0.8865(3) 0.1957(3) 0.0469(13) Uani 1 d . . H8A H 0.4511(3) 0.8730(3) 0.2361(3) 0.070 Uiso 1 calc R . H8B H 0.4132(3) 0.9415(3) 0.1808(3) 0.070 Uiso 1 calc R . H8C H 0.4098(3) 0.8514(3) 0.1538(3) 0.070 Uiso 1 calc R . C9 C 0.3036(3) 0.7698(3) 0.2627(3) 0.0487(13) Uani 1 d . . H9A H 0.3533(3) 0.7625(3) 0.3000(3) 0.073 Uiso 1 calc R . H9B H 0.3060(3) 0.7330(3) 0.2219(3) 0.073 Uiso 1 calc R . H9C H 0.2528(3) 0.7596(3) 0.2848(3) 0.073 Uiso 1 calc R . C10 C 0.3083(3) 0.9367(3) 0.3133(2) 0.0514(14) Uani 1 d . . H10A H 0.3576(3) 0.9207(3) 0.3482(2) 0.077 Uiso 1 calc R . H10B H 0.2574(3) 0.9293(3) 0.3360(2) 0.077 Uiso 1 calc R . H10C H 0.3135(3) 0.9926(3) 0.3004(2) 0.077 Uiso 1 calc R . C11 C 0.3485(3) 0.7119(3) 0.0570(2) 0.0373(11) Uani 1 d . . C12 C 0.3568(3) 0.6325(3) 0.0802(3) 0.0499(13) Uani 1 d . . H12 H 0.3165(3) 0.6103(3) 0.1072(3) 0.060 Uiso 1 calc R . C13 C 0.4216(4) 0.5870(4) 0.0645(3) 0.065(2) Uani 1 d . . H13 H 0.4263(4) 0.5340(4) 0.0816(3) 0.078 Uiso 1 calc R . C14 C 0.4802(4) 0.6160(4) 0.0247(3) 0.069(2) Uani 1 d . . H14 H 0.5246(4) 0.5835(4) 0.0133(3) 0.083 Uiso 1 calc R . C15 C 0.4733(3) 0.6944(4) 0.0011(3) 0.064(2) Uani 1 d . . H15 H 0.5136(3) 0.7159(4) -0.0263(3) 0.076 Uiso 1 calc R . C16 C 0.4089(3) 0.7403(3) 0.0175(3) 0.0483(13) Uani 1 d . . H16 H 0.4054(3) 0.7937(3) 0.0011(3) 0.058 Uiso 1 calc R . C17 C 0.1284(3) 0.8174(3) -0.0812(2) 0.0340(11) Uani 1 d . . C18 C 0.0538(3) 0.8275(3) -0.1294(3) 0.0429(12) Uani 1 d . . H18 H 0.0110(3) 0.8599(3) -0.1146(3) 0.051 Uiso 1 calc R . C19 C 0.0397(3) 0.7923(3) -0.1977(3) 0.0502(13) Uani 1 d . . H19 H -0.0124(3) 0.7999(3) -0.2287(3) 0.060 Uiso 1 calc R . C20 C 0.1005(3) 0.7463(3) -0.2213(3) 0.0500(13) Uani 1 d . . H20 H 0.0910(3) 0.7220(3) -0.2684(3) 0.060 Uiso 1 calc R . C21 C 0.1759(3) 0.7359(3) -0.1752(3) 0.0488(13) Uani 1 d . . H21 H 0.2184(3) 0.7041(3) -0.1910(3) 0.059 Uiso 1 calc R . C22 C 0.1905(3) 0.7710(3) -0.1066(3) 0.0413(12) Uani 1 d . . H22 H 0.2432(3) 0.7637(3) -0.0763(3) 0.050 Uiso 1 calc R . C23 C 0.3198(3) 0.9814(3) -0.0279(3) 0.0448(12) Uani 1 d . . C24 C 0.2527(3) 0.9947(3) -0.0852(3) 0.058(2) Uani 1 d . . H24 H 0.2056(3) 0.9602(3) -0.0907(3) 0.070 Uiso 1 calc R . C25 C 0.2542(4) 1.0571(4) -0.1334(3) 0.089(2) Uani 1 d . . H25 H 0.2069(4) 1.0663(4) -0.1701(3) 0.106 Uiso 1 calc R . C26 C 0.3234(5) 1.1068(5) -0.1295(4) 0.101(3) Uani 1 d . . H26 H 0.3245(5) 1.1487(5) -0.1639(4) 0.121 Uiso 1 calc R . C27 C 0.3903(4) 1.0941(4) -0.0751(4) 0.076(2) Uani 1 d . . H27 H 0.4384(4) 1.1273(4) -0.0719(4) 0.091 Uiso 1 calc R . C28 C 0.3884(3) 1.0334(3) -0.0249(3) 0.0546(14) Uani 1 d . . H28 H 0.4351(3) 1.0266(3) 0.0128(3) 0.066 Uiso 1 calc R . C29 C 0.8752(5) 0.6938(4) 0.2501(4) 0.090(2) Uani 1 d . . H29A H 0.8150(5) 0.7084(4) 0.2407(4) 0.107 Uiso 1 calc R . H29B H 0.9072(5) 0.7327(4) 0.2251(4) 0.107 Uiso 1 calc R . C30 C 0.9050(6) 0.6933(5) 0.3280(4) 0.116(3) Uani 1 d . . H30A H 0.9316(6) 0.7446(5) 0.3437(4) 0.139 Uiso 1 calc R . H30B H 0.8578(6) 0.6840(5) 0.3560(4) 0.139 Uiso 1 calc R . C31 C 0.9638(5) 0.6319(6) 0.3404(4) 0.129(4) Uani 1 d . . H31A H 0.9615(5) 0.6063(6) 0.3886(4) 0.155 Uiso 1 calc R . H31B H 1.0215(5) 0.6520(6) 0.3396(4) 0.155 Uiso 1 calc R . C32 C 0.9390(6) 0.5753(5) 0.2790(4) 0.124(3) Uani 1 d . . H32A H 0.9895(6) 0.5552(5) 0.2600(4) 0.149 Uiso 1 calc R . H32B H 0.9085(6) 0.5298(5) 0.2963(4) 0.149 Uiso 1 calc R . C33 C 0.6627(4) 0.5737(4) 0.2038(4) 0.088(2) Uani 1 d . . H33A H 0.6399(4) 0.6224(4) 0.1783(4) 0.106 Uiso 1 calc R . H33B H 0.6959(4) 0.5888(4) 0.2516(4) 0.106 Uiso 1 calc R . C34 C 0.5930(4) 0.5200(4) 0.2158(4) 0.081(2) Uani 1 d . . H34A H 0.5379(4) 0.5436(4) 0.1961(4) 0.097 Uiso 1 calc R . H34B H 0.5944(4) 0.5092(4) 0.2690(4) 0.097 Uiso 1 calc R . C35 C 0.6073(4) 0.4457(4) 0.1754(4) 0.087(2) Uani 1 d . . H35A H 0.6220(4) 0.4015(4) 0.2104(4) 0.104 Uiso 1 calc R . H35B H 0.5562(4) 0.4311(4) 0.1410(4) 0.104 Uiso 1 calc R . C36 C 0.6768(5) 0.4630(4) 0.1352(4) 0.099(3) Uani 1 d . . H36A H 0.7183(5) 0.4194(4) 0.1423(4) 0.119 Uiso 1 calc R . H36B H 0.6555(5) 0.4671(4) 0.0819(4) 0.119 Uiso 1 calc R . C37 C 0.7121(4) 0.6882(4) 0.0363(4) 0.103(3) Uani 1 d . . H37A H 0.6772(4) 0.7132(4) 0.0699(4) 0.124 Uiso 1 calc R . H37B H 0.6820(4) 0.6410(4) 0.0139(4) 0.124 Uiso 1 calc R . C38 C 0.7267(7) 0.7444(6) -0.0216(4) 0.127(3) Uani 1 d . . H38A H 0.6957(7) 0.7284(6) -0.0701(4) 0.153 Uiso 1 calc R . H38B H 0.7091(7) 0.7985(6) -0.0099(4) 0.153 Uiso 1 calc R . C39 C 0.8143(8) 0.7407(7) -0.0215(6) 0.165(5) Uani 1 d . . H39A H 0.8267(8) 0.7069(7) -0.0626(6) 0.198 Uiso 1 calc R . H39B H 0.8365(8) 0.7943(7) -0.0284(6) 0.198 Uiso 1 calc R . C40 C 0.8530(5) 0.7095(5) 0.0451(5) 0.108(3) Uani 1 d . . H40A H 0.8756(5) 0.7524(5) 0.0790(5) 0.130 Uiso 1 calc R . H40B H 0.8999(5) 0.6742(5) 0.0371(5) 0.130 Uiso 1 calc R . C41 C 0.8395(4) 0.4844(4) 0.0107(3) 0.079(2) Uani 1 d . . H41A H 0.7773(4) 0.4836(4) 0.0043(3) 0.095 Uiso 1 calc R . H41B H 0.8574(4) 0.5247(4) -0.0229(3) 0.095 Uiso 1 calc R . C42 C 0.8710(6) 0.4085(4) -0.0050(4) 0.116(3) Uani 1 d . . H42A H 0.8848(6) 0.4073(4) -0.0557(4) 0.139 Uiso 1 calc R . H42B H 0.8283(6) 0.3673(4) -0.0006(4) 0.139 Uiso 1 calc R . C43 C 0.9488(4) 0.3937(4) 0.0499(5) 0.092(2) Uani 1 d . . H43A H 0.9528(4) 0.3375(4) 0.0654(5) 0.110 Uiso 1 calc R . H43B H 1.0002(4) 0.4085(4) 0.0295(5) 0.110 Uiso 1 calc R . C44 C 0.9354(4) 0.4461(4) 0.1119(4) 0.078(2) Uani 1 d . . H44A H 0.9170(4) 0.4146(4) 0.1520(4) 0.093 Uiso 1 calc R . H44B H 0.9885(4) 0.4733(4) 0.1316(4) 0.093 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 0.0339(7) 0.0359(8) 0.0322(7) -0.0039(6) 0.0040(6) 0.0044(6) Si1 0.0389(7) 0.0318(7) 0.0381(7) -0.0028(6) 0.0038(6) 0.0038(6) Si2 0.0402(7) 0.0363(7) 0.0401(8) -0.0066(6) 0.0086(6) -0.0008(6) Si3 0.0399(8) 0.0376(8) 0.0354(7) -0.0015(6) -0.0019(6) 0.0067(6) N1 0.044(2) 0.038(2) 0.040(2) -0.006(2) 0.013(2) 0.010(2) N2 0.031(2) 0.045(2) 0.036(2) -0.010(2) 0.006(2) 0.007(2) N3 0.031(2) 0.048(3) 0.045(2) 0.004(2) 0.002(2) 0.006(2) Li 0.040(5) 0.059(6) 0.048(5) 0.000(4) 0.003(4) 0.000(4) O1 0.074(3) 0.063(3) 0.050(2) -0.007(2) -0.010(2) 0.018(2) O2 0.064(3) 0.059(2) 0.073(3) -0.012(2) 0.031(2) -0.009(2) O3 0.049(2) 0.073(3) 0.062(2) 0.024(2) 0.000(2) -0.005(2) O4 0.059(2) 0.077(3) 0.049(2) -0.011(2) -0.003(2) 0.021(2) C1 0.029(2) 0.027(2) 0.032(2) -0.004(2) 0.002(2) 0.002(2) C2 0.047(3) 0.038(3) 0.050(3) 0.003(2) 0.005(2) 0.011(2) C3 0.055(3) 0.032(3) 0.055(3) -0.001(2) 0.007(3) -0.001(2) C4 0.055(3) 0.038(3) 0.055(3) -0.008(2) 0.008(3) 0.009(2) C5 0.054(3) 0.061(3) 0.044(3) 0.000(3) 0.020(3) -0.001(3) C6 0.053(3) 0.043(3) 0.066(4) -0.009(3) 0.018(3) -0.007(3) C7 0.034(3) 0.060(3) 0.057(3) -0.011(3) 0.010(2) 0.001(2) C8 0.039(3) 0.053(3) 0.046(3) 0.000(3) -0.003(2) 0.008(2) C9 0.052(3) 0.044(3) 0.049(3) 0.008(2) 0.004(3) 0.014(3) C10 0.057(3) 0.059(4) 0.035(3) -0.004(3) -0.007(2) 0.005(3) C11 0.044(3) 0.042(3) 0.024(2) -0.007(2) -0.002(2) 0.010(2) C12 0.060(3) 0.044(3) 0.043(3) 0.000(2) -0.002(3) 0.011(3) C13 0.067(4) 0.055(4) 0.068(4) 0.001(3) -0.007(3) 0.025(3) C14 0.059(4) 0.080(5) 0.065(4) -0.013(4) -0.001(3) 0.036(4) C15 0.047(3) 0.083(5) 0.062(4) -0.001(3) 0.010(3) 0.021(3) C16 0.046(3) 0.051(3) 0.046(3) -0.005(3) 0.003(2) 0.017(3) C17 0.034(3) 0.035(3) 0.034(3) -0.005(2) 0.008(2) -0.004(2) C18 0.028(3) 0.053(3) 0.048(3) -0.014(2) 0.005(2) 0.005(2) C19 0.039(3) 0.065(4) 0.044(3) -0.013(3) -0.003(2) 0.000(3) C20 0.048(3) 0.062(4) 0.040(3) -0.018(3) 0.008(2) -0.002(3) C21 0.050(3) 0.051(3) 0.048(3) -0.010(3) 0.016(3) 0.009(3) C22 0.034(3) 0.048(3) 0.043(3) -0.004(2) 0.010(2) 0.006(2) C23 0.045(3) 0.052(3) 0.040(3) -0.001(3) 0.015(2) -0.002(3) C24 0.063(4) 0.069(4) 0.038(3) 0.006(3) -0.005(3) -0.027(3) C25 0.098(5) 0.103(6) 0.055(4) 0.033(4) -0.017(4) -0.041(4) C26 0.126(7) 0.111(6) 0.062(4) 0.033(4) 0.007(4) -0.055(5) C27 0.071(4) 0.087(5) 0.071(4) 0.010(4) 0.018(4) -0.035(4) C28 0.043(3) 0.066(4) 0.057(3) -0.006(3) 0.015(3) -0.008(3) C29 0.110(6) 0.080(5) 0.070(5) -0.001(4) -0.015(4) 0.018(4) C30 0.139(8) 0.130(7) 0.067(5) -0.021(5) -0.024(5) 0.021(6) C31 0.133(7) 0.168(9) 0.069(5) -0.031(6) -0.044(5) 0.058(7) C32 0.165(8) 0.102(6) 0.085(5) -0.013(5) -0.049(6) 0.050(6) C33 0.102(5) 0.085(5) 0.093(5) -0.013(4) 0.065(4) -0.004(4) C34 0.057(4) 0.120(6) 0.065(4) 0.014(4) 0.011(3) 0.006(4) C35 0.084(5) 0.115(6) 0.061(4) 0.008(4) 0.008(4) -0.046(5) C36 0.096(6) 0.078(5) 0.134(7) -0.029(5) 0.053(5) -0.021(4) C37 0.077(5) 0.102(6) 0.124(6) 0.055(5) -0.009(5) 0.005(4) C38 0.179(10) 0.123(8) 0.077(6) 0.042(5) 0.005(6) 0.057(7) C39 0.190(11) 0.178(11) 0.132(9) 0.084(8) 0.040(9) -0.035(10) C40 0.089(6) 0.115(7) 0.120(7) 0.027(6) 0.012(5) -0.031(5) C41 0.081(5) 0.098(5) 0.055(4) -0.022(4) -0.001(3) 0.009(4) C42 0.165(8) 0.073(5) 0.101(6) -0.033(5) -0.009(6) 0.012(5) C43 0.077(5) 0.054(4) 0.151(7) -0.017(5) 0.040(5) 0.008(4) C44 0.071(4) 0.073(4) 0.084(5) 0.007(4) -0.006(4) 0.016(4) _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 N3 1.848(4) . ? Al N2 1.851(4) . ? Al N1 1.853(4) . ? Al C1 2.044(4) . ? Si1 C4 1.872(5) . ? Si1 C3 1.876(5) . ? Si1 C2 1.876(5) . ? Si1 C1 1.877(4) . ? Si2 C6 1.877(5) . ? Si2 C7 1.880(5) . ? Si2 C1 1.881(4) . ? Si2 C5 1.884(5) . ? Si3 C1 1.875(4) . ? Si3 C9 1.879(5) . ? Si3 C8 1.881(5) . ? Si3 C10 1.891(5) . ? N1 C11 1.380(5) . ? N2 C17 1.381(5) . ? N3 C23 1.374(6) . ? Li O3 1.890(9) . ? Li O1 1.900(9) . ? Li O2 1.910(9) . ? Li O4 1.917(9) . ? O1 C32 1.405(7) . ? O1 C29 1.418(7) . ? O2 C36 1.367(7) . ? O2 C33 1.427(6) . ? O3 C37 1.401(7) . ? O3 C40 1.430(7) . ? O4 C44 1.415(6) . ? O4 C41 1.426(6) . ? C11 C16 1.383(6) . ? C11 C12 1.409(6) . ? C12 C13 1.360(7) . ? C13 C14 1.368(8) . ? C14 C15 1.393(8) . ? C15 C16 1.364(7) . ? C17 C18 1.392(6) . ? C17 C22 1.404(6) . ? C18 C19 1.376(6) . ? C19 C20 1.368(6) . ? C20 C21 1.384(6) . ? C21 C22 1.379(6) . ? C23 C28 1.407(7) . ? C23 C24 1.408(7) . ? C24 C25 1.380(7) . ? C25 C26 1.388(8) . ? C26 C27 1.371(9) . ? C27 C28 1.382(8) . ? C29 C30 1.440(8) . ? C30 C31 1.401(9) . ? C31 C32 1.487(9) . ? C33 C34 1.485(8) . ? C34 C35 1.494(9) . ? C35 C36 1.459(8) . ? C37 C38 1.471(10) . ? C38 C39 1.411(12) . ? C39 C40 1.390(11) . ? C41 C42 1.425(9) . ? C42 C43 1.505(9) . ? C43 C44 1.483(8) . ? 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 Al N2 110.4(2) . . ? N3 Al N1 108.4(2) . . ? N2 Al N1 108.9(2) . . ? N3 Al C1 112.0(2) . . ? N2 Al C1 110.4(2) . . ? N1 Al C1 106.7(2) . . ? C4 Si1 C3 104.7(2) . . ? C4 Si1 C2 105.0(2) . . ? C3 Si1 C2 105.2(2) . . ? C4 Si1 C1 113.9(2) . . ? C3 Si1 C1 114.2(2) . . ? C2 Si1 C1 112.9(2) . . ? C6 Si2 C7 103.0(2) . . ? C6 Si2 C1 113.6(2) . . ? C7 Si2 C1 115.4(2) . . ? C6 Si2 C5 105.6(2) . . ? C7 Si2 C5 103.7(2) . . ? C1 Si2 C5 114.3(2) . . ? C1 Si3 C9 114.9(2) . . ? C1 Si3 C8 114.1(2) . . ? C9 Si3 C8 103.8(2) . . ? C1 Si3 C10 114.3(2) . . ? C9 Si3 C10 103.9(2) . . ? C8 Si3 C10 104.5(2) . . ? C11 N1 Al 140.2(3) . . ? C17 N2 Al 131.1(3) . . ? C23 N3 Al 137.6(3) . . ? O3 Li O1 106.6(5) . . ? O3 Li O2 108.6(4) . . ? O1 Li O2 113.1(5) . . ? O3 Li O4 107.2(4) . . ? O1 Li O4 112.2(4) . . ? O2 Li O4 108.8(5) . . ? C32 O1 C29 107.5(5) . . ? C32 O1 Li 130.1(5) . . ? C29 O1 Li 120.4(4) . . ? C36 O2 C33 109.8(5) . . ? C36 O2 Li 129.2(4) . . ? C33 O2 Li 120.8(4) . . ? C37 O3 C40 107.0(5) . . ? C37 O3 Li 129.0(4) . . ? C40 O3 Li 122.2(5) . . ? C44 O4 C41 109.7(5) . . ? C44 O4 Li 129.6(4) . . ? C41 O4 Li 119.3(4) . . ? Si3 C1 Si1 110.6(2) . . ? Si3 C1 Si2 110.2(2) . . ? Si1 C1 Si2 109.8(2) . . ? Si3 C1 Al 107.1(2) . . ? Si1 C1 Al 108.0(2) . . ? Si2 C1 Al 111.1(2) . . ? N1 C11 C16 122.7(4) . . ? N1 C11 C12 120.7(4) . . ? C16 C11 C12 116.5(4) . . ? C13 C12 C11 121.1(5) . . ? C12 C13 C14 121.4(6) . . ? C13 C14 C15 118.6(5) . . ? C16 C15 C14 120.0(6) . . ? C15 C16 C11 122.3(5) . . ? N2 C17 C18 122.4(4) . . ? N2 C17 C22 121.0(4) . . ? C18 C17 C22 116.5(4) . . ? C19 C18 C17 122.3(4) . . ? C20 C19 C18 120.4(5) . . ? C19 C20 C21 118.8(5) . . ? C22 C21 C20 121.2(5) . . ? C21 C22 C17 120.7(4) . . ? N3 C23 C28 121.9(5) . . ? N3 C23 C24 122.1(4) . . ? C28 C23 C24 116.0(5) . . ? C25 C24 C23 121.1(5) . . ? C24 C25 C26 121.3(6) . . ? C27 C26 C25 118.7(6) . . ? C26 C27 C28 120.5(6) . . ? C27 C28 C23 122.3(5) . . ? O1 C29 C30 107.3(6) . . ? C31 C30 C29 106.4(7) . . ? C30 C31 C32 104.8(6) . . ? O1 C32 C31 107.2(6) . . ? O2 C33 C34 107.6(5) . . ? C33 C34 C35 105.4(5) . . ? C36 C35 C34 105.6(5) . . ? O2 C36 C35 109.9(6) . . ? O3 C37 C38 108.5(6) . . ? C39 C38 C37 103.7(7) . . ? C40 C39 C38 109.5(8) . . ? C39 C40 O3 106.8(7) . . ? C42 C41 O4 106.8(6) . . ? C41 C42 C43 107.5(6) . . ? C44 C43 C42 102.3(5) . . ? O4 C44 C43 108.2(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Al N1 C11 -15.4(5) . . . . ? N2 Al N1 C11 104.7(5) . . . . ? C1 Al N1 C11 -136.2(5) . . . . ? N3 Al N2 C17 67.5(4) . . . . ? N1 Al N2 C17 -51.4(4) . . . . ? C1 Al N2 C17 -168.2(4) . . . . ? N2 Al N3 C23 23.6(5) . . . . ? N1 Al N3 C23 142.8(5) . . . . ? C1 Al N3 C23 -99.8(5) . . . . ? O3 Li O1 C32 -164.2(6) . . . . ? O2 Li O1 C32 76.4(8) . . . . ? O4 Li O1 C32 -47.1(9) . . . . ? O3 Li O1 C29 33.7(7) . . . . ? O2 Li O1 C29 -85.6(6) . . . . ? O4 Li O1 C29 150.8(5) . . . . ? O3 Li O2 C36 107.6(7) . . . . ? O1 Li O2 C36 -134.3(6) . . . . ? O4 Li O2 C36 -8.8(8) . . . . ? O3 Li O2 C33 -68.2(6) . . . . ? O1 Li O2 C33 49.9(7) . . . . ? O4 Li O2 C33 175.4(5) . . . . ? O1 Li O3 C37 -135.1(6) . . . . ? O2 Li O3 C37 -12.9(8) . . . . ? O4 Li O3 C37 104.5(7) . . . . ? O1 Li O3 C40 62.4(7) . . . . ? O2 Li O3 C40 -175.4(5) . . . . ? O4 Li O3 C40 -58.0(7) . . . . ? O3 Li O4 C44 149.6(5) . . . . ? O1 Li O4 C44 32.8(8) . . . . ? O2 Li O4 C44 -93.1(6) . . . . ? O3 Li O4 C41 -45.7(6) . . . . ? O1 Li O4 C41 -162.4(5) . . . . ? O2 Li O4 C41 71.7(6) . . . . ? C9 Si3 C1 Si1 160.5(2) . . . . ? C8 Si3 C1 Si1 -79.8(3) . . . . ? C10 Si3 C1 Si1 40.5(3) . . . . ? C9 Si3 C1 Si2 38.9(3) . . . . ? C8 Si3 C1 Si2 158.6(2) . . . . ? C10 Si3 C1 Si2 -81.1(3) . . . . ? C9 Si3 C1 Al -82.0(3) . . . . ? C8 Si3 C1 Al 37.7(3) . . . . ? C10 Si3 C1 Al 158.0(2) . . . . ? C4 Si1 C1 Si3 -79.1(3) . . . . ? C3 Si1 C1 Si3 41.2(3) . . . . ? C2 Si1 C1 Si3 161.3(2) . . . . ? C4 Si1 C1 Si2 42.8(3) . . . . ? C3 Si1 C1 Si2 163.1(2) . . . . ? C2 Si1 C1 Si2 -76.8(3) . . . . ? C4 Si1 C1 Al 164.1(2) . . . . ? C3 Si1 C1 Al -75.6(3) . . . . ? C2 Si1 C1 Al 44.4(3) . . . . ? C6 Si2 C1 Si3 -79.1(3) . . . . ? C7 Si2 C1 Si3 162.3(2) . . . . ? C5 Si2 C1 Si3 42.2(3) . . . . ? C6 Si2 C1 Si1 158.8(2) . . . . ? C7 Si2 C1 Si1 40.2(3) . . . . ? C5 Si2 C1 Si1 -79.9(3) . . . . ? C6 Si2 C1 Al 39.4(3) . . . . ? C7 Si2 C1 Al -79.2(3) . . . . ? C5 Si2 C1 Al 160.7(2) . . . . ? N3 Al C1 Si3 -73.1(2) . . . . ? N2 Al C1 Si3 163.4(2) . . . . ? N1 Al C1 Si3 45.3(2) . . . . ? N3 Al C1 Si1 46.0(2) . . . . ? N2 Al C1 Si1 -77.4(2) . . . . ? N1 Al C1 Si1 164.4(2) . . . . ? N3 Al C1 Si2 166.5(2) . . . . ? N2 Al C1 Si2 43.1(3) . . . . ? N1 Al C1 Si2 -75.1(2) . . . . ? Al N1 C11 C16 3.0(7) . . . . ? Al N1 C11 C12 -177.1(4) . . . . ? N1 C11 C12 C13 -179.5(4) . . . . ? C16 C11 C12 C13 0.5(7) . . . . ? C11 C12 C13 C14 -1.2(8) . . . . ? C12 C13 C14 C15 1.2(9) . . . . ? C13 C14 C15 C16 -0.4(8) . . . . ? C14 C15 C16 C11 -0.3(8) . . . . ? N1 C11 C16 C15 -179.8(5) . . . . ? C12 C11 C16 C15 0.3(7) . . . . ? Al N2 C17 C18 -171.7(4) . . . . ? Al N2 C17 C22 6.9(6) . . . . ? N2 C17 C18 C19 -179.5(4) . . . . ? C22 C17 C18 C19 1.9(7) . . . . ? C17 C18 C19 C20 -1.1(8) . . . . ? C18 C19 C20 C21 0.1(8) . . . . ? C19 C20 C21 C22 -0.1(8) . . . . ? C20 C21 C22 C17 1.0(8) . . . . ? N2 C17 C22 C21 179.5(4) . . . . ? C18 C17 C22 C21 -1.8(7) . . . . ? Al N3 C23 C28 159.8(4) . . . . ? Al N3 C23 C24 -19.7(8) . . . . ? N3 C23 C24 C25 177.5(6) . . . . ? C28 C23 C24 C25 -2.1(8) . . . . ? C23 C24 C25 C26 3.1(11) . . . . ? C24 C25 C26 C27 -1.7(12) . . . . ? C25 C26 C27 C28 -0.4(11) . . . . ? C26 C27 C28 C23 1.3(10) . . . . ? N3 C23 C28 C27 -179.6(5) . . . . ? C24 C23 C28 C27 0.0(8) . . . . ? C32 O1 C29 C30 -12.7(9) . . . . ? Li O1 C29 C30 153.0(6) . . . . ? O1 C29 C30 C31 24.7(10) . . . . ? C29 C30 C31 C32 -25.9(11) . . . . ? C29 O1 C32 C31 -3.3(9) . . . . ? Li O1 C32 C31 -167.1(6) . . . . ? C30 C31 C32 O1 18.4(11) . . . . ? C36 O2 C33 C34 8.5(8) . . . . ? Li O2 C33 C34 -174.9(5) . . . . ? O2 C33 C34 C35 -0.6(7) . . . . ? C33 C34 C35 C36 -6.8(8) . . . . ? C33 O2 C36 C35 -13.2(8) . . . . ? Li O2 C36 C35 170.6(5) . . . . ? C34 C35 C36 O2 12.4(8) . . . . ? C40 O3 C37 C38 2.2(9) . . . . ? Li O3 C37 C38 -162.4(6) . . . . ? O3 C37 C38 C39 10.5(11) . . . . ? C37 C38 C39 C40 -19.8(13) . . . . ? C38 C39 C40 O3 21.8(13) . . . . ? C37 O3 C40 C39 -14.4(10) . . . . ? Li O3 C40 C39 151.5(8) . . . . ? C44 O4 C41 C42 9.9(8) . . . . ? Li O4 C41 C42 -157.6(6) . . . . ? O4 C41 C42 C43 -21.2(9) . . . . ? C41 C42 C43 C44 23.7(9) . . . . ? C41 O4 C44 C43 5.5(7) . . . . ? Li O4 C44 C43 171.4(5) . . . . ? C42 C43 C44 O4 -17.5(7) . . . . ? _refine_diff_density_max 0.328 _refine_diff_density_min -0.281 _refine_diff_density_rms 0.058 #==END data_feb1293 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(tsi)AlI2(thf)]' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H35 Al I2 O Si3' _chemical_formula_weight 584.47 _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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 '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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.506(7) _cell_length_b 13.946(3) _cell_length_c 13.755(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2399.0(15) _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 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.618 _exptl_crystal_density_method ? _exptl_crystal_F_000 1152 _exptl_absorpt_coefficient_mu 2.807 _exptl_absorpt_correction_type 'DIFABS' _exptl_absorpt_correction_T_min 0.74 _exptl_absorpt_correction_T_max 1.38 _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 2208 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0244 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.96 _reflns_number_total 2208 _reflns_number_observed 1792 _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 ; The tsi group is disordered across the mirror plane with alternative silicon atom sites and shared carbon atom sites. 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^)+(0.0367P)^2^+5.6595P] 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 2208 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0444 _refine_ls_R_factor_obs 0.0302 _refine_ls_wR_factor_all 0.0821 _refine_ls_wR_factor_obs 0.0762 _refine_ls_goodness_of_fit_all 1.064 _refine_ls_goodness_of_fit_obs 1.104 _refine_ls_restrained_S_all 1.064 _refine_ls_restrained_S_obs 1.104 _refine_ls_shift/esd_max 0.003 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group I I 0.08472(2) 0.15035(2) 0.10468(2) 0.03687(13) Uani 1 d . . Si1 Si 0.3068(2) -0.0613(2) 0.3789(2) 0.0292(5) Uani 0.50 d P . Si2 Si 0.2634(2) -0.1326(2) 0.1678(2) 0.0299(5) Uani 0.50 d P . Si3 Si 0.3733(2) 0.0654(2) 0.2025(2) 0.0368(6) Uani 0.50 d P . Al Al 0.12954(13) 0.04281(12) 0.2500 0.0206(3) Uani 1 d S . O O 0.0086(3) -0.0380(3) 0.2500 0.0320(9) Uani 1 d S . C1 C 0.2698(4) -0.0231(4) 0.2500 0.0234(12) Uani 1 d S . C2 C 0.4065(4) -0.1675(5) 0.3767(4) 0.065(2) Uani 1 d . . H2A H 0.4705(4) -0.1491(5) 0.3401(4) 0.097 Uiso 1 calc R . H2B H 0.3728(4) -0.2230(5) 0.3455(4) 0.097 Uiso 1 calc R . H2C H 0.4267(4) -0.1842(5) 0.4434(4) 0.097 Uiso 1 calc R . C3 C 0.1932(4) -0.1104(3) 0.4507(3) 0.0406(11) Uani 1 d . . H3A H 0.2183(4) -0.1283(3) 0.5157(3) 0.061 Uiso 1 calc R . H3B H 0.1643(4) -0.1671(3) 0.4178(3) 0.061 Uiso 1 calc R . H3C H 0.1371(4) -0.0616(3) 0.4564(3) 0.061 Uiso 1 calc R . C4 C 0.3668(5) 0.0556(6) 0.4466(5) 0.096(3) Uani 1 d . . H4A H 0.4266(5) 0.0813(6) 0.4087(5) 0.144 Uiso 1 calc R . H4B H 0.3919(5) 0.0377(6) 0.5115(5) 0.144 Uiso 1 calc R . H4C H 0.3108(5) 0.1045(6) 0.4523(5) 0.144 Uiso 1 calc R . C5 C 0.1927(7) -0.2379(6) 0.2500 0.096(4) Uani 1 d S . H5A H 0.2328(7) -0.2463(6) 0.3106 0.145 Uiso 0.50 calc PR . H5B H 0.1926(7) -0.2983(6) 0.2136 0.145 Uiso 0.50 calc PR . H5C H 0.1189(7) -0.2194(6) 0.2650 0.145 Uiso 0.50 calc PR . C6 C 0.5155(6) 0.0342(7) 0.2500 0.078(3) Uani 1 d S . H6A H 0.5349(6) -0.0305(7) 0.2287 0.116 Uiso 0.50 calc PR . H6B H 0.5160(6) 0.0370(7) 0.3212 0.116 Uiso 0.50 calc PR . H6C H 0.5671(6) 0.0804(7) 0.2240 0.116 Uiso 0.50 calc PR . C7 C 0.3509(6) 0.1901(5) 0.2500 0.050(2) Uani 1 d S . H7A H 0.4058(6) 0.2331(5) 0.2238 0.075 Uiso 0.50 calc PR . H7B H 0.3552(6) 0.1897(5) 0.3211 0.075 Uiso 0.50 calc PR . H7C H 0.2801(6) 0.2127(5) 0.2299 0.075 Uiso 0.50 calc PR . C8 C -0.0548(5) -0.0682(5) 0.3336(4) 0.066(2) Uani 1 d . . H8A H -0.0403(5) -0.0263(5) 0.3902(4) 0.079 Uiso 1 calc R . H8B H -0.0373(5) -0.1352(5) 0.3515(4) 0.079 Uiso 1 calc R . C9 C -0.1667(4) -0.0606(5) 0.3045(4) 0.064(2) Uani 1 d . . H9A H -0.1985(4) -0.0006(5) 0.3297(4) 0.077 Uiso 1 calc R . H9B H -0.2082(4) -0.1156(5) 0.3297(4) 0.077 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 I 0.0390(2) 0.0360(2) 0.0357(2) 0.00688(12) -0.00589(13) 0.00843(13) Si1 0.0160(11) 0.0402(13) 0.0315(11) -0.0021(10) -0.0052(9) 0.0086(10) Si2 0.0198(12) 0.0366(12) 0.0334(12) -0.0060(10) -0.0029(10) 0.0079(10) Si3 0.0130(11) 0.0477(14) 0.0497(13) 0.0041(12) 0.0066(11) -0.0052(10) Al 0.0101(8) 0.0243(8) 0.0273(8) 0.000 0.000 0.0000(7) O 0.013(2) 0.035(2) 0.048(2) 0.000 0.000 -0.006(2) C1 0.010(3) 0.032(3) 0.028(3) 0.000 0.000 0.003(2) C2 0.038(3) 0.097(5) 0.059(3) 0.030(3) 0.005(3) 0.041(3) C3 0.040(3) 0.048(3) 0.035(2) 0.009(2) 0.006(2) 0.011(2) C4 0.048(4) 0.165(8) 0.075(4) -0.070(5) -0.038(3) 0.040(5) C5 0.044(5) 0.030(4) 0.216(14) 0.000 0.000 -0.004(4) C6 0.018(4) 0.077(6) 0.138(9) 0.000 0.000 -0.007(4) C7 0.031(4) 0.050(4) 0.069(5) 0.000 0.000 -0.017(3) C8 0.047(3) 0.095(5) 0.056(3) 0.022(3) 0.001(3) -0.039(3) C9 0.026(3) 0.094(5) 0.072(4) 0.006(4) 0.012(3) -0.010(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I Al 2.5611(11) . ? Si1 Si2 1.302(3) 6_556 ? Si1 C3 1.860(5) . ? Si1 C1 1.908(3) . ? Si1 C2 1.937(6) . ? Si1 C4 2.022(7) . ? Si1 Si3 2.251(4) 6_556 ? Si2 Si1 1.302(3) 6_556 ? Si2 C3 1.877(5) 6_556 ? Si2 C1 1.903(5) . ? Si2 C2 1.952(5) 6_556 ? Si2 C5 2.054(7) . ? Si2 Si2 2.262(5) 6_556 ? Si3 Si3 1.307(5) 6_556 ? Si3 C7 1.879(8) . ? Si3 C1 1.905(6) . ? Si3 C6 1.944(8) . ? Si3 C4 2.056(8) 6_556 ? Si3 Si1 2.251(4) 6_556 ? Al O 1.886(4) . ? Al C1 1.980(6) . ? Al I 2.5611(11) 6_556 ? O C8 1.459(6) 6_556 ? O C8 1.459(6) . ? C1 Si2 1.903(5) 6_556 ? C1 Si3 1.905(6) 6_556 ? C1 Si1 1.908(3) 6_556 ? C8 C9 1.458(8) . ? C9 C9 1.498(12) 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 Si2 Si1 C3 70.3(2) 6_556 . ? Si2 Si1 C1 69.8(2) 6_556 . ? C3 Si1 C1 114.2(2) . . ? Si2 Si1 C2 71.1(3) 6_556 . ? C3 Si1 C2 102.6(3) . . ? C1 Si1 C2 110.8(3) . . ? Si2 Si1 C4 176.0(3) 6_556 . ? C3 Si1 C4 109.6(3) . . ? C1 Si1 C4 107.0(3) . . ? C2 Si1 C4 112.6(3) . . ? Si2 Si1 Si3 120.6(2) 6_556 6_556 ? C3 Si1 Si3 146.6(2) . 6_556 ? C1 Si1 Si3 53.7(2) . 6_556 ? C2 Si1 Si3 110.8(2) . 6_556 ? C4 Si1 Si3 57.2(3) . 6_556 ? Si1 Si2 C3 68.9(2) 6_556 6_556 ? Si1 Si2 C1 70.2(2) 6_556 . ? C3 Si2 C1 113.7(2) 6_556 . ? Si1 Si2 C2 69.8(3) 6_556 6_556 ? C3 Si2 C2 101.4(3) 6_556 6_556 ? C1 Si2 C2 110.4(3) . 6_556 ? Si1 Si2 C5 175.5(2) 6_556 . ? C3 Si2 C5 113.3(3) 6_556 . ? C1 Si2 C5 105.3(2) . . ? C2 Si2 C5 112.9(3) 6_556 . ? Si1 Si2 Si2 119.51(14) 6_556 6_556 ? C3 Si2 Si2 150.2(2) 6_556 6_556 ? C1 Si2 Si2 53.52(12) . 6_556 ? C2 Si2 Si2 108.3(2) 6_556 6_556 ? C5 Si2 Si2 56.58(14) . 6_556 ? Si3 Si3 C7 69.64(12) 6_556 . ? Si3 Si3 C1 69.93(10) 6_556 . ? C7 Si3 C1 112.3(3) . . ? Si3 Si3 C6 70.35(11) 6_556 . ? C7 Si3 C6 103.1(4) . . ? C1 Si3 C6 111.2(3) . . ? Si3 Si3 C4 175.6(3) 6_556 6_556 ? C7 Si3 C4 113.7(3) . 6_556 ? C1 Si3 C4 105.8(3) . 6_556 ? C6 Si3 C4 110.9(2) . 6_556 ? Si3 Si3 Si1 119.81(9) 6_556 6_556 ? C7 Si3 Si1 147.6(3) . 6_556 ? C1 Si3 Si1 53.88(12) . 6_556 ? C6 Si3 Si1 109.2(3) . 6_556 ? C4 Si3 Si1 55.8(3) 6_556 6_556 ? O Al C1 115.7(2) . . ? O Al I 100.03(9) . 6_556 ? C1 Al I 117.75(9) . 6_556 ? O Al I 100.03(9) . . ? C1 Al I 117.75(9) . . ? I Al I 102.61(6) 6_556 . ? C8 O C8 104.0(5) 6_556 . ? C8 O Al 127.5(3) 6_556 . ? C8 O Al 127.5(3) . . ? Si2 C1 Si2 73.0(2) . 6_556 ? Si2 C1 Si3 138.8(3) . 6_556 ? Si2 C1 Si3 110.2(2) 6_556 6_556 ? Si2 C1 Si3 110.2(2) . . ? Si2 C1 Si3 138.8(3) 6_556 . ? Si3 C1 Si3 40.1(2) 6_556 . ? Si2 C1 Si1 39.97(13) . 6_556 ? Si2 C1 Si1 109.8(3) 6_556 6_556 ? Si3 C1 Si1 109.6(3) 6_556 6_556 ? Si3 C1 Si1 72.4(2) . 6_556 ? Si2 C1 Si1 109.8(3) . . ? Si2 C1 Si1 39.97(13) 6_556 . ? Si3 C1 Si1 72.4(2) 6_556 . ? Si3 C1 Si1 109.6(3) . . ? Si1 C1 Si1 136.6(3) 6_556 . ? Si2 C1 Al 109.6(2) . . ? Si2 C1 Al 109.6(2) 6_556 . ? Si3 C1 Al 107.5(3) 6_556 . ? Si3 C1 Al 107.5(3) . . ? Si1 C1 Al 110.1(2) 6_556 . ? Si1 C1 Al 110.1(2) . . ? O C8 C9 106.5(5) . . ? C8 C9 C9 105.9(3) . 6_556 ? _refine_diff_density_max 0.902 _refine_diff_density_min -0.977 _refine_diff_density_rms 0.103 #==END data_nov995 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li(tmeda)2][TsiAlH3].0.5toluene' _chemical_formula_analytical ? _chemical_formula_sum 'C102 H264 Al4 Li4 N16 Si12' _chemical_formula_weight 2188.05 _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' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 17.315(7) _cell_length_b 26.471(9) _cell_length_c 32.800(13) _cell_angle_alpha 90.00 _cell_angle_beta 91.16(3) _cell_angle_gamma 90.00 _cell_volume 15030.6(99) _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 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.967 _exptl_crystal_density_method ? _exptl_crystal_F_000 4880 _exptl_absorpt_coefficient_mu 0.168 _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 9558 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_sigmaI/netI 0.1321 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 21.99 _reflns_number_total 9206 _reflns_number_observed 4951 _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 ; The Li(2) cation is has disordered tmeda ligands in the ratio 0.81:0.19 . The Al(2) anion has the Si atoms of the Tsi group disordered over two sets of positions in the ratio 0.75:0.25 .The lower occupancy tmeda sites were left isotropic and their H atoms omitted. Hydride H atoms were freely refined isotropic. 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^)+(0.0851P)^2^+22.5733P] 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 9206 _refine_ls_number_parameters 742 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1571 _refine_ls_R_factor_obs 0.0794 _refine_ls_wR_factor_all 0.2241 _refine_ls_wR_factor_obs 0.1778 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.136 _refine_ls_restrained_S_all 1.023 _refine_ls_restrained_S_obs 1.136 _refine_ls_shift/esd_max -0.006 _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 Li2 Li 0.2312(7) -0.0115(4) 0.3625(3) 0.041(3) Uani 1 d . . Al1 Al 0.75262(12) 0.10285(7) 0.47507(6) 0.0408(6) Uani 1 d . 1 Si1 Si 0.78430(12) 0.09792(7) 0.38080(5) 0.0412(5) Uani 1 d . 1 Si2 Si 0.65398(11) 0.03286(7) 0.41676(6) 0.0415(5) Uani 1 d . 1 Si3 Si 0.82460(11) 0.00611(7) 0.43581(5) 0.0394(5) Uani 1 d . 1 C1 C 0.7539(3) 0.0574(2) 0.4244(2) 0.030(2) Uani 1 d . 1 C2 C 0.8913(4) 0.1100(3) 0.3805(2) 0.057(2) Uani 1 d . 1 H2A H 0.9037(4) 0.1313(3) 0.3571(2) 0.086 Uiso 1 calc R 1 H2B H 0.9189(4) 0.0778(3) 0.3784(2) 0.086 Uiso 1 calc R 1 H2C H 0.9072(4) 0.1272(3) 0.4057(2) 0.086 Uiso 1 calc R 1 C3 C 0.7390(4) 0.1629(2) 0.3801(2) 0.058(2) Uani 1 d . 1 H3A H 0.7574(4) 0.1818(2) 0.3566(2) 0.087 Uiso 1 calc R 1 H3B H 0.7533(4) 0.1808(2) 0.4053(2) 0.087 Uiso 1 calc R 1 H3C H 0.6826(4) 0.1596(2) 0.3781(2) 0.087 Uiso 1 calc R 1 C4 C 0.7618(5) 0.0699(3) 0.3292(2) 0.058(2) Uani 1 d . 1 H4A H 0.7792(5) 0.0930(3) 0.3079(2) 0.088 Uiso 1 calc R 1 H4B H 0.7059(5) 0.0646(3) 0.3262(2) 0.088 Uiso 1 calc R 1 H4C H 0.7885(5) 0.0374(3) 0.3266(2) 0.088 Uiso 1 calc R 1 C5 C 0.6461(4) -0.0246(2) 0.3827(2) 0.055(2) Uani 1 d . 1 H5A H 0.5919(4) -0.0351(2) 0.3802(2) 0.082 Uiso 1 calc R 1 H5B H 0.6769(4) -0.0522(2) 0.3945(2) 0.082 Uiso 1 calc R 1 H5C H 0.6654(4) -0.0163(2) 0.3556(2) 0.082 Uiso 1 calc R 1 C6 C 0.6065(4) 0.0145(3) 0.4658(2) 0.052(2) Uani 1 d . 1 H6A H 0.5543(4) 0.0019(3) 0.4598(2) 0.078 Uiso 1 calc R 1 H6B H 0.6036(4) 0.0441(3) 0.4837(2) 0.078 Uiso 1 calc R 1 H6C H 0.6370(4) -0.0120(3) 0.4794(2) 0.078 Uiso 1 calc R 1 C7 C 0.5868(4) 0.0809(3) 0.3931(2) 0.057(2) Uani 1 d . 1 H7A H 0.5352(4) 0.0662(3) 0.3897(2) 0.085 Uiso 1 calc R 1 H7B H 0.6061(4) 0.0910(3) 0.3664(2) 0.085 Uiso 1 calc R 1 H7C H 0.5842(4) 0.1107(3) 0.4108(2) 0.085 Uiso 1 calc R 1 C8 C 0.8604(4) -0.0277(2) 0.3896(2) 0.050(2) Uani 1 d . 1 H8A H 0.8972(4) -0.0540(2) 0.3980(2) 0.075 Uiso 1 calc R 1 H8B H 0.8860(4) -0.0035(2) 0.3717(2) 0.075 Uiso 1 calc R 1 H8C H 0.8167(4) -0.0432(2) 0.3749(2) 0.075 Uiso 1 calc R 1 C9 C 0.7843(4) -0.0454(2) 0.4682(2) 0.051(2) Uani 1 d . 1 H9A H 0.8240(4) -0.0712(2) 0.4731(2) 0.077 Uiso 1 calc R 1 H9B H 0.7397(4) -0.0607(2) 0.4541(2) 0.077 Uiso 1 calc R 1 H9C H 0.7681(4) -0.0313(2) 0.4942(2) 0.077 Uiso 1 calc R 1 C10 C 0.9127(4) 0.0290(3) 0.4650(2) 0.052(2) Uani 1 d . 1 H10A H 0.9478(4) 0.0005(3) 0.4701(2) 0.079 Uiso 1 calc R 1 H10B H 0.8971(4) 0.0435(3) 0.4910(2) 0.079 Uiso 1 calc R 1 H10C H 0.9391(4) 0.0548(3) 0.4490(2) 0.079 Uiso 1 calc R 1 Al2 Al 0.7564(2) 0.28996(8) 0.86580(7) 0.0605(7) Uani 1 d . 1 Si4 Si 0.6658(2) 0.24143(15) 0.79221(12) 0.0643(11) Uani 0.809(5) d P 1 Si5 Si 0.7953(2) 0.18042(8) 0.83551(7) 0.0426(10) Uani 0.809(5) d P 1 Si6 Si 0.8372(2) 0.27069(11) 0.78040(9) 0.0563(10) Uani 0.809(5) d P 1 C11 C 0.7611(4) 0.2426(2) 0.8158(2) 0.051(2) Uani 1 d . 1 C12 C 0.5991(5) 0.1967(4) 0.8230(3) 0.122(4) Uani 1 d . 1 H12A H 0.5475(5) 0.1961(4) 0.8103(3) 0.183 Uiso 1 calc R 1 H12B H 0.5955(5) 0.2091(4) 0.8511(3) 0.183 Uiso 1 calc R 1 H12C H 0.6208(5) 0.1625(4) 0.8233(3) 0.183 Uiso 1 calc R 1 C13 C 0.6122(6) 0.3028(3) 0.7925(3) 0.120(4) Uani 1 d . 1 H13A H 0.5615(6) 0.2984(3) 0.7791(3) 0.179 Uiso 1 calc R 1 H13B H 0.6417(6) 0.3284(3) 0.7778(3) 0.179 Uiso 1 calc R 1 H13C H 0.6052(6) 0.3139(3) 0.8207(3) 0.179 Uiso 1 calc R 1 C14 C 0.6608(5) 0.2179(3) 0.7378(2) 0.091(3) Uani 1 d . 1 H14A H 0.6071(5) 0.2187(3) 0.7279(2) 0.137 Uiso 1 calc R 1 H14B H 0.6802(5) 0.1832(3) 0.7368(2) 0.137 Uiso 1 calc R 1 H14C H 0.6924(5) 0.2396(3) 0.7207(2) 0.137 Uiso 1 calc R 1 C15 C 0.7687(5) 0.1257(2) 0.8002(2) 0.064(2) Uani 1 d . 1 H15A H 0.7880(5) 0.0940(2) 0.8121(2) 0.095 Uiso 1 calc R 1 H15B H 0.7919(5) 0.1310(2) 0.7736(2) 0.095 Uiso 1 calc R 1 H15C H 0.7124(5) 0.1238(2) 0.7969(2) 0.095 Uiso 1 calc R 1 C16 C 0.7518(4) 0.1634(3) 0.8861(2) 0.061(2) Uani 1 d . 1 H16A H 0.7716(4) 0.1305(3) 0.8951(2) 0.092 Uiso 1 calc R 1 H16B H 0.6955(4) 0.1618(3) 0.8830(2) 0.092 Uiso 1 calc R 1 H16C H 0.7659(4) 0.1891(3) 0.9064(2) 0.092 Uiso 1 calc R 1 C17 C 0.9039(5) 0.1776(3) 0.8451(2) 0.076(3) Uani 1 d . 1 H17A H 0.9181(5) 0.1440(3) 0.8553(2) 0.114 Uiso 1 calc R 1 H17B H 0.9190(5) 0.2032(3) 0.8653(2) 0.114 Uiso 1 calc R 1 H17C H 0.9305(5) 0.1841(3) 0.8195(2) 0.114 Uiso 1 calc R 1 C18 C 0.7943(7) 0.3249(3) 0.7496(3) 0.135(5) Uani 1 d . 1 H18A H 0.7489(7) 0.3129(3) 0.7341(3) 0.202 Uiso 1 calc R 1 H18B H 0.8329(7) 0.3376(3) 0.7307(3) 0.202 Uiso 1 calc R 1 H18C H 0.7791(7) 0.3520(3) 0.7680(3) 0.202 Uiso 1 calc R 1 C19 C 0.9209(5) 0.2981(3) 0.8076(3) 0.090(3) Uani 1 d . 1 H19A H 0.9031(5) 0.3229(3) 0.8275(3) 0.135 Uiso 1 calc R 1 H19B H 0.9545(5) 0.3149(3) 0.7881(3) 0.135 Uiso 1 calc R 1 H19C H 0.9497(5) 0.2713(3) 0.8218(3) 0.135 Uiso 1 calc R 1 C20 C 0.8732(5) 0.2234(3) 0.7425(2) 0.083(3) Uani 1 d . 1 H20A H 0.8292(5) 0.2084(3) 0.7277(2) 0.125 Uiso 1 calc R 1 H20B H 0.9022(5) 0.1968(3) 0.7569(2) 0.125 Uiso 1 calc R 1 H20C H 0.9070(5) 0.2404(3) 0.7231(2) 0.125 Uiso 1 calc R 1 Li1 Li 0.4989(6) 0.2390(4) 0.5063(3) 0.036(3) Uani 1 d . 1 N1 N 0.5589(3) 0.2599(2) 0.4539(2) 0.0440(15) Uani 1 d . 1 N2 N 0.4311(3) 0.3048(2) 0.4998(2) 0.0417(14) Uani 1 d . 1 N3 N 0.5616(3) 0.2204(2) 0.5601(2) 0.048(2) Uani 1 d . 1 N4 N 0.4411(3) 0.1685(2) 0.5118(2) 0.047(2) Uani 1 d . 1 C21 C 0.5307(4) 0.3121(2) 0.4475(2) 0.053(2) Uani 1 d . 1 H21A H 0.5391(4) 0.3220(2) 0.4188(2) 0.063 Uiso 1 calc R 1 H21B H 0.5612(4) 0.3354(2) 0.4651(2) 0.063 Uiso 1 calc R 1 C22 C 0.4464(4) 0.3177(2) 0.4568(2) 0.047(2) Uani 1 d . 1 H22A H 0.4301(4) 0.3530(2) 0.4514(2) 0.057 Uiso 1 calc R 1 H22B H 0.4156(4) 0.2953(2) 0.4386(2) 0.057 Uiso 1 calc R 1 C23 C 0.5330(5) 0.2283(3) 0.4196(2) 0.065(2) Uani 1 d . 1 H23A H 0.4764(5) 0.2279(3) 0.4182(2) 0.097 Uiso 1 calc R 1 H23B H 0.5523(5) 0.1938(3) 0.4236(2) 0.097 Uiso 1 calc R 1 H23C H 0.5530(5) 0.2421(3) 0.3942(2) 0.097 Uiso 1 calc R 1 C24 C 0.6436(4) 0.2607(3) 0.4561(2) 0.062(2) Uani 1 d . 1 H24A H 0.6607(4) 0.2819(3) 0.4791(2) 0.093 Uiso 1 calc R 1 H24B H 0.6637(4) 0.2744(3) 0.4307(2) 0.093 Uiso 1 calc R 1 H24C H 0.6630(4) 0.2262(3) 0.4601(2) 0.093 Uiso 1 calc R 1 C25 C 0.4616(4) 0.3441(2) 0.5270(2) 0.058(2) Uani 1 d . 1 H25A H 0.5177(4) 0.3462(2) 0.5243(2) 0.087 Uiso 1 calc R 1 H25B H 0.4493(4) 0.3357(2) 0.5552(2) 0.087 Uiso 1 calc R 1 H25C H 0.4382(4) 0.3766(2) 0.5197(2) 0.087 Uiso 1 calc R 1 C26 C 0.3466(4) 0.3024(3) 0.5044(2) 0.059(2) Uani 1 d . 1 H26A H 0.3251(4) 0.2763(3) 0.4863(2) 0.089 Uiso 1 calc R 1 H26B H 0.3238(4) 0.3352(3) 0.4972(2) 0.089 Uiso 1 calc R 1 H26C H 0.3348(4) 0.2942(3) 0.5327(2) 0.089 Uiso 1 calc R 1 C27 C 0.5399(5) 0.1671(3) 0.5668(3) 0.073(3) Uani 1 d . 1 H27A H 0.5472(5) 0.1588(3) 0.5961(3) 0.087 Uiso 1 calc R 1 H27B H 0.5747(5) 0.1450(3) 0.5511(3) 0.087 Uiso 1 calc R 1 C28 C 0.4585(5) 0.1564(3) 0.5543(3) 0.076(3) Uani 1 d . 1 H28A H 0.4477(5) 0.1202(3) 0.5589(3) 0.091 Uiso 1 calc R 1 H28B H 0.4238(5) 0.1762(3) 0.5718(3) 0.091 Uiso 1 calc R 1 C29 C 0.6457(4) 0.2241(3) 0.5597(2) 0.069(2) Uani 1 d . 1 H29A H 0.6654(4) 0.2037(3) 0.5372(2) 0.104 Uiso 1 calc R 1 H29B H 0.6674(4) 0.2117(3) 0.5856(2) 0.104 Uiso 1 calc R 1 H29C H 0.6607(4) 0.2594(3) 0.5558(2) 0.104 Uiso 1 calc R 1 C30 C 0.5342(5) 0.2513(3) 0.5940(2) 0.071(2) Uani 1 d . 1 H30A H 0.4777(5) 0.2494(3) 0.5949(2) 0.106 Uiso 1 calc R 1 H30B H 0.5499(5) 0.2865(3) 0.5900(2) 0.106 Uiso 1 calc R 1 H30C H 0.5566(5) 0.2387(3) 0.6197(2) 0.106 Uiso 1 calc R 1 C31 C 0.3564(4) 0.1682(3) 0.5056(3) 0.070(2) Uani 1 d . 1 H31A H 0.3331(4) 0.1932(3) 0.5237(3) 0.105 Uiso 1 calc R 1 H31B H 0.3363(4) 0.1345(3) 0.5119(3) 0.105 Uiso 1 calc R 1 H31C H 0.3437(4) 0.1766(3) 0.4772(3) 0.105 Uiso 1 calc R 1 C32 C 0.4721(4) 0.1309(3) 0.4845(3) 0.069(2) Uani 1 d . 1 H32A H 0.4593(4) 0.1403(3) 0.4562(3) 0.104 Uiso 1 calc R 1 H32B H 0.4496(4) 0.0979(3) 0.4905(3) 0.104 Uiso 1 calc R 1 H32C H 0.5283(4) 0.1293(3) 0.4882(3) 0.104 Uiso 1 calc R 1 N5 N 0.1351(6) 0.0227(3) 0.3870(3) 0.045(2) Uani 0.748(6) d P 1 N6 N 0.1751(6) -0.0837(3) 0.3691(3) 0.044(2) Uani 0.748(6) d P 1 N7 N 0.3428(6) 0.0029(4) 0.3866(3) 0.045(3) Uani 0.748(6) d P 1 N8 N 0.2664(9) 0.0096(4) 0.3052(3) 0.055(3) Uani 0.748(6) d P 1 C33 C 0.0775(6) -0.0184(4) 0.3847(3) 0.063(3) Uani 0.748(6) d P 1 H33A H 0.0545(6) -0.0197(4) 0.3568(3) 0.075 Uiso 0.748(6) calc PR 1 H33B H 0.0355(6) -0.0112(4) 0.4039(3) 0.075 Uiso 0.748(6) calc PR 1 C34 C 0.1125(6) -0.0681(4) 0.3948(3) 0.059(3) Uani 0.748(6) d P 1 H34A H 0.1318(6) -0.0671(4) 0.4234(3) 0.071 Uiso 0.748(6) calc PR 1 H34B H 0.0714(6) -0.0941(4) 0.3931(3) 0.071 Uiso 0.748(6) calc PR 1 C35 C 0.1023(14) 0.0680(9) 0.3681(6) 0.078(7) Uani 0.748(6) d P 1 H35A H 0.0901(14) 0.0612(9) 0.3393(6) 0.117 Uiso 0.748(6) calc PR 1 H35B H 0.1398(14) 0.0957(9) 0.3702(6) 0.117 Uiso 0.748(6) calc PR 1 H35C H 0.0550(14) 0.0775(9) 0.3821(6) 0.117 Uiso 0.748(6) calc PR 1 C36 C 0.1532(7) 0.0334(5) 0.4304(3) 0.063(3) Uani 0.748(6) d P 1 H36A H 0.1753(7) 0.0031(5) 0.4433(3) 0.095 Uiso 0.748(6) calc PR 1 H36B H 0.1059(7) 0.0430(5) 0.4442(3) 0.095 Uiso 0.748(6) calc PR 1 H36C H 0.1906(7) 0.0611(5) 0.4323(3) 0.095 Uiso 0.748(6) calc PR 1 C37 C 0.2190(7) -0.1241(4) 0.3878(4) 0.066(3) Uani 0.748(6) d P 1 H37A H 0.2610(7) -0.1340(4) 0.3698(4) 0.099 Uiso 0.748(6) calc PR 1 H37B H 0.1852(7) -0.1532(4) 0.3922(4) 0.099 Uiso 0.748(6) calc PR 1 H37C H 0.2408(7) -0.1127(4) 0.4140(4) 0.099 Uiso 0.748(6) calc PR 1 C38 C 0.1462(7) -0.1001(4) 0.3286(4) 0.080(4) Uani 0.748(6) d P 1 H38A H 0.1163(7) -0.0727(4) 0.3159(4) 0.120 Uiso 0.748(6) calc PR 1 H38B H 0.1131(7) -0.1299(4) 0.3317(4) 0.120 Uiso 0.748(6) calc PR 1 H38C H 0.1900(7) -0.1087(4) 0.3115(4) 0.120 Uiso 0.748(6) calc PR 1 C39 C 0.3858(6) 0.0122(5) 0.3493(3) 0.088(4) Uani 0.748(6) d P 1 H39A H 0.4060(6) -0.0204(5) 0.3392(3) 0.105 Uiso 0.748(6) calc PR 1 H39B H 0.4306(6) 0.0341(5) 0.3560(3) 0.105 Uiso 0.748(6) calc PR 1 C40 C 0.3384(6) 0.0367(4) 0.3160(4) 0.073(4) Uani 0.748(6) d P 1 H40A H 0.3251(6) 0.0714(4) 0.3245(4) 0.087 Uiso 0.748(6) calc PR 1 H40B H 0.3702(6) 0.0393(4) 0.2913(4) 0.087 Uiso 0.748(6) calc PR 1 C41 C 0.3800(9) -0.0404(6) 0.4089(5) 0.081(5) Uani 0.748(6) d P 1 H41A H 0.3783(9) -0.0705(6) 0.3916(5) 0.122 Uiso 0.748(6) calc PR 1 H41B H 0.3521(9) -0.0469(6) 0.4340(5) 0.122 Uiso 0.748(6) calc PR 1 H41C H 0.4338(9) -0.0319(6) 0.4156(5) 0.122 Uiso 0.748(6) calc PR 1 C42 C 0.3458(7) 0.0463(5) 0.4121(4) 0.077(4) Uani 0.748(6) d P 1 H42A H 0.3168(7) 0.0397(5) 0.4370(4) 0.115 Uiso 0.748(6) calc PR 1 H42B H 0.3228(7) 0.0752(5) 0.3976(4) 0.115 Uiso 0.748(6) calc PR 1 H42C H 0.3997(7) 0.0539(5) 0.4195(4) 0.115 Uiso 0.748(6) calc PR 1 C43 C 0.2145(12) 0.0453(8) 0.2859(5) 0.088(7) Uani 0.748(6) d P 1 H43A H 0.2040(12) 0.0730(8) 0.3048(5) 0.132 Uiso 0.748(6) calc PR 1 H43B H 0.1659(12) 0.0284(8) 0.2784(5) 0.132 Uiso 0.748(6) calc PR 1 H43C H 0.2382(12) 0.0588(8) 0.2613(5) 0.132 Uiso 0.748(6) calc PR 1 C44 C 0.2843(10) -0.0335(5) 0.2782(4) 0.118(6) Uani 0.748(6) d P 1 H44A H 0.3195(10) -0.0568(5) 0.2925(4) 0.177 Uiso 0.748(6) calc PR 1 H44B H 0.3088(10) -0.0210(5) 0.2535(4) 0.177 Uiso 0.748(6) calc PR 1 H44C H 0.2364(10) -0.0513(5) 0.2706(4) 0.177 Uiso 0.748(6) calc PR 1 C45 C 1.0000 0.0846(4) 0.2500 0.115(6) Uani 1 d S 1 C46 C 1.0000 0.0267(4) 0.2500 0.061(3) Uani 1 d S 1 C47 C 0.9629(4) 0.0003(4) 0.2793(2) 0.068(2) Uani 1 d . 1 H47 H 0.9372(4) 0.0180(4) 0.3002(2) 0.082 Uiso 1 calc R 1 C48 C 0.9618(6) -0.0512(4) 0.2792(3) 0.093(3) Uani 1 d . 1 H48 H 0.9342(6) -0.0687(4) 0.2995(3) 0.111 Uiso 1 calc R 1 C49 C 1.0000 -0.0779(5) 0.2500 0.093(5) Uani 1 d S 1 H49 H 1.0000 -0.1138(5) 0.2500 0.112 Uiso 1 calc SR 1 C50 C 0.5000 0.0794(4) 0.2500 0.131(7) Uani 1 d S 1 C51 C 0.5000 0.0241(8) 0.2500 0.137(7) Uani 1 d S 1 C52 C 0.5339(5) -0.0024(5) 0.2807(3) 0.086(3) Uani 1 d . 1 H52 H 0.5593(5) 0.0154(5) 0.3022(3) 0.104 Uiso 1 calc R 1 C53 C 0.5330(6) -0.0552(5) 0.2818(3) 0.117(4) Uani 1 d . 1 H53 H 0.5552(6) -0.0723(5) 0.3047(3) 0.141 Uiso 1 calc R 1 C54 C 0.5000 -0.0835(5) 0.2500 0.111(5) Uani 1 d S 1 H54 H 0.5000 -0.1194(5) 0.2500 0.133 Uiso 1 calc SR 1 H111 H 0.6818(30) 0.1342(19) 0.4748(15) 0.042(16) Uiso 1 d . 1 H112 H 0.8284(31) 0.2775(19) 0.8967(16) 0.048(17) Uiso 1 d . 1 H113 H 0.7634(31) 0.0697(20) 0.5159(16) 0.049(17) Uiso 1 d . 1 H211 H 0.6829(36) 0.2817(22) 0.8903(18) 0.069(20) Uiso 1 d . 1 H212 H 0.8215(34) 0.1404(21) 0.4753(17) 0.061(19) Uiso 1 d . 1 H213 H 0.7480(42) 0.3469(27) 0.8543(22) 0.105(26) Uiso 1 d . 1 Si41 Si 0.6824(12) 0.2675(6) 0.7771(5) 0.085(6) Uani 0.191(5) d P 2 Si51 Si 0.7178(7) 0.1780(4) 0.8361(3) 0.047(4) Uani 0.191(5) d P 2 Si61 Si 0.8543(9) 0.2398(6) 0.8023(4) 0.076(5) Uani 0.191(5) d P 2 C55 C 0.1851(18) -0.0417(11) 0.2858(9) 0.060(9) Uiso 0.252(6) d P 2 C56 C 0.2191(20) -0.0885(12) 0.3078(10) 0.070(10) Uiso 0.252(6) d P 2 C57 C 0.1224(27) -0.0952(16) 0.3612(15) 0.081(13) Uiso 0.252(6) d P 2 C58 C 0.2596(23) -0.1244(16) 0.3740(12) 0.072(13) Uiso 0.252(6) d P 2 C59 C 0.3026(27) 0.0009(20) 0.2825(17) 0.090(15) Uiso 0.252(6) d P 2 C60 C 0.1845(35) 0.0460(27) 0.2827(22) 0.071(18) Uiso 0.252(6) d P 2 C61 C 0.2221(14) 0.0705(8) 0.4207(7) 0.029(6) Uiso 0.252(6) d P 2 C62 C 0.2953(17) 0.0361(10) 0.4337(8) 0.040(7) Uiso 0.252(6) d P 2 C63 C 0.1189(22) 0.0049(14) 0.4272(12) 0.070(12) Uiso 0.252(6) d P 2 C64 C 0.1013(37) 0.0754(24) 0.3789(18) 0.034(12) Uiso 0.252(6) d P 2 C65 C 0.3924(35) -0.0191(19) 0.4120(19) 0.072(18) Uiso 0.252(6) d P 2 C66 C 0.3708(18) 0.0585(12) 0.3745(10) 0.061(9) Uiso 0.252(6) d P 2 N9 N 0.2080(16) -0.0835(10) 0.3529(8) 0.042(9) Uiso 0.252(6) d P 2 N10 N 0.2360(21) 0.0011(15) 0.2967(12) 0.059(14) Uiso 0.252(6) d P 2 N11 N 0.1638(15) 0.0376(10) 0.3990(10) 0.034(8) Uiso 0.252(6) d P 2 N12 C 0.3276(26) 0.0151(17) 0.3992(14) 0.035(12) Uiso 0.252(6) d P 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 Li2 0.055(8) 0.041(6) 0.027(6) -0.003(5) 0.000(5) 0.003(6) Al1 0.0486(14) 0.0360(12) 0.0377(12) -0.0149(10) -0.0031(10) 0.0018(11) Si1 0.0526(14) 0.0360(11) 0.0350(11) -0.0042(9) -0.0016(9) 0.0017(10) Si2 0.0429(13) 0.0364(11) 0.0448(12) -0.0108(9) -0.0082(10) -0.0006(9) Si3 0.0428(12) 0.0368(11) 0.0383(11) -0.0086(9) -0.0052(9) 0.0067(9) C1 0.034(4) 0.025(3) 0.032(4) -0.007(3) -0.007(3) -0.005(3) C2 0.068(6) 0.052(5) 0.053(5) 0.001(4) 0.014(4) -0.010(4) C3 0.082(6) 0.036(4) 0.055(5) 0.002(4) 0.003(4) -0.003(4) C4 0.085(6) 0.050(5) 0.040(4) -0.006(4) -0.008(4) 0.006(4) C5 0.059(5) 0.045(4) 0.059(5) -0.015(4) -0.015(4) -0.007(4) C6 0.051(5) 0.049(5) 0.057(5) -0.001(4) 0.002(4) -0.012(4) C7 0.041(5) 0.062(5) 0.066(5) -0.006(4) -0.011(4) 0.002(4) C8 0.052(5) 0.042(4) 0.056(5) -0.014(4) 0.007(4) 0.011(4) C9 0.056(5) 0.051(5) 0.048(4) 0.000(4) -0.003(4) 0.006(4) C10 0.051(5) 0.057(5) 0.049(5) 0.000(4) -0.004(4) 0.008(4) Al2 0.084(2) 0.0405(14) 0.057(2) -0.0150(11) 0.0027(14) 0.0063(13) Si4 0.070(2) 0.052(2) 0.070(3) -0.011(2) -0.019(2) 0.017(2) Si5 0.059(2) 0.0298(14) 0.0388(15) -0.0011(11) 0.0042(13) 0.0014(12) Si6 0.086(2) 0.036(2) 0.047(2) 0.0060(15) 0.003(2) 0.0008(15) C11 0.076(6) 0.031(4) 0.044(4) -0.001(3) -0.007(4) 0.007(4) C12 0.056(6) 0.156(10) 0.155(10) -0.084(8) 0.010(6) -0.013(7) C13 0.126(9) 0.084(7) 0.146(10) -0.025(7) -0.058(8) 0.061(7) C14 0.118(8) 0.080(6) 0.074(6) -0.011(5) -0.037(6) 0.016(6) C15 0.102(7) 0.039(4) 0.050(5) -0.003(4) -0.003(5) -0.003(4) C16 0.083(6) 0.054(5) 0.048(5) 0.004(4) 0.006(4) -0.011(4) C17 0.085(7) 0.075(6) 0.066(6) -0.013(5) -0.018(5) 0.029(5) C18 0.270(15) 0.045(5) 0.088(7) 0.022(5) -0.013(9) 0.003(7) C19 0.137(9) 0.052(5) 0.082(6) 0.002(5) 0.031(6) -0.034(6) C20 0.102(7) 0.081(6) 0.068(6) -0.009(5) 0.030(5) -0.006(5) Li1 0.032(6) 0.027(6) 0.049(7) -0.004(5) 0.000(5) -0.005(5) N1 0.047(4) 0.035(3) 0.050(4) -0.004(3) -0.003(3) 0.008(3) N2 0.043(4) 0.037(3) 0.045(4) -0.008(3) -0.001(3) 0.007(3) N3 0.044(4) 0.039(3) 0.060(4) 0.005(3) -0.014(3) -0.003(3) N4 0.044(4) 0.038(3) 0.059(4) -0.003(3) 0.001(3) -0.005(3) C21 0.059(5) 0.043(4) 0.057(5) 0.002(4) 0.002(4) 0.008(4) C22 0.051(5) 0.039(4) 0.052(5) 0.002(4) 0.000(4) 0.016(4) C23 0.076(6) 0.048(5) 0.071(6) -0.010(4) 0.003(5) 0.003(4) C24 0.058(6) 0.064(5) 0.064(5) 0.000(4) 0.005(4) 0.009(4) C25 0.064(5) 0.045(4) 0.064(5) -0.016(4) -0.011(4) 0.011(4) C26 0.046(5) 0.057(5) 0.075(6) 0.007(4) -0.001(4) 0.011(4) C27 0.081(7) 0.048(5) 0.088(6) 0.022(4) -0.027(5) -0.013(5) C28 0.091(7) 0.053(5) 0.084(7) 0.013(5) 0.001(5) -0.023(5) C29 0.054(6) 0.067(5) 0.085(6) 0.010(5) -0.027(5) 0.000(4) C30 0.083(7) 0.065(5) 0.065(6) 0.008(5) -0.002(5) 0.001(5) C31 0.044(5) 0.050(5) 0.115(7) -0.007(5) 0.003(5) -0.010(4) C32 0.066(6) 0.040(5) 0.103(7) -0.014(5) 0.024(5) -0.009(4) N5 0.042(6) 0.049(6) 0.043(6) -0.004(4) -0.003(4) 0.002(5) N6 0.040(6) 0.045(5) 0.047(6) 0.003(4) 0.002(6) 0.000(5) N7 0.039(6) 0.072(8) 0.025(6) -0.002(5) 0.004(5) -0.008(5) N8 0.074(9) 0.062(7) 0.028(6) -0.010(5) -0.006(6) -0.018(7) C33 0.035(6) 0.069(8) 0.084(8) 0.001(6) 0.000(6) 0.000(6) C34 0.054(7) 0.059(7) 0.065(7) -0.001(6) 0.007(6) -0.027(6) C35 0.077(10) 0.072(12) 0.086(17) 0.000(12) 0.007(12) 0.038(9) C36 0.075(9) 0.085(9) 0.031(7) -0.018(6) 0.005(6) 0.023(8) C37 0.075(9) 0.047(7) 0.077(9) 0.021(6) 0.009(8) 0.009(7) C38 0.087(10) 0.068(8) 0.085(9) -0.020(7) -0.014(8) -0.025(7) C39 0.055(8) 0.143(12) 0.066(8) -0.010(8) 0.007(7) -0.040(8) C40 0.059(8) 0.077(8) 0.084(9) 0.004(7) 0.016(7) -0.032(7) C41 0.049(9) 0.097(15) 0.097(12) 0.007(11) -0.029(7) 0.008(10) C42 0.059(9) 0.101(10) 0.069(9) -0.028(8) -0.012(7) -0.009(8) C43 0.110(19) 0.109(13) 0.044(8) 0.034(7) -0.025(11) -0.014(14) C44 0.192(17) 0.079(10) 0.086(10) -0.047(8) 0.084(10) -0.042(11) C45 0.163(15) 0.042(8) 0.138(13) 0.000 -0.051(11) 0.000 C46 0.054(8) 0.080(9) 0.049(7) 0.000 -0.014(6) 0.000 C47 0.048(6) 0.108(8) 0.048(5) -0.009(5) -0.003(4) 0.006(5) C48 0.075(8) 0.113(10) 0.088(8) 0.038(7) -0.026(6) -0.038(7) C49 0.100(13) 0.048(8) 0.127(15) 0.000 -0.074(11) 0.000 C50 0.126(14) 0.021(7) 0.249(20) 0.000 0.101(13) 0.000 C51 0.051(11) 0.182(21) 0.179(20) 0.000 0.031(12) 0.000 C52 0.051(6) 0.114(9) 0.093(8) 0.011(7) -0.014(5) 0.011(6) C53 0.121(10) 0.132(11) 0.098(9) -0.008(8) -0.020(7) -0.004(9) C54 0.110(13) 0.062(9) 0.159(16) 0.000 -0.019(12) 0.000 Si41 0.146(16) 0.049(10) 0.060(10) 0.034(8) -0.004(9) 0.034(10) Si51 0.050(10) 0.038(6) 0.052(7) -0.007(5) 0.001(6) 0.003(5) Si61 0.114(13) 0.060(10) 0.054(9) -0.004(8) 0.022(8) -0.026(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li2 N9 1.97(3) . ? Li2 N8 2.064(15) . ? Li2 N5 2.071(14) . ? Li2 N7 2.107(15) . ? Li2 N11 2.13(3) . ? Li2 N12 2.16(5) . ? Li2 N6 2.157(14) . ? Li2 N10 2.19(4) . ? Li2 C56 2.72(3) . ? Li2 C40 2.741(15) . ? Li2 C55 2.74(3) . ? Li2 C34 2.772(15) . ? Al1 C1 2.052(6) . ? Al1 H111 1.48(5) . ? Al1 H113 1.61(5) . ? Al1 H212 1.55(6) . ? Si1 C1 1.871(6) . ? Si1 C2 1.881(7) . ? Si1 C4 1.882(6) . ? Si1 C3 1.890(7) . ? Si2 C1 1.860(6) . ? Si2 C7 1.881(7) . ? Si2 C6 1.884(7) . ? Si2 C5 1.891(6) . ? Si3 C1 1.862(6) . ? Si3 C9 1.872(7) . ? Si3 C8 1.877(6) . ? Si3 C10 1.884(7) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? Al2 C11 2.066(7) . ? Al2 H112 1.63(5) . ? Al2 H211 1.53(6) . ? Al2 H213 1.56(7) . ? Si4 C11 1.810(8) . ? Si4 C13 1.872(8) . ? Si4 C14 1.889(8) . ? Si4 C12 1.950(11) . ? Si5 C11 1.860(7) . ? Si5 C16 1.890(7) . ? Si5 C17 1.901(8) . ? Si5 C15 1.906(7) . ? Si6 C19 1.837(9) . ? Si6 C20 1.881(8) . ? Si6 C18 1.897(9) . ? Si6 C11 1.923(8) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? Li1 N1 2.102(12) . ? Li1 N2 2.109(11) . ? Li1 N3 2.112(12) . ? Li1 N4 2.129(11) . ? Li1 C22 2.783(12) . ? N1 C23 1.463(8) . ? N1 C24 1.468(8) . ? N1 C21 1.478(8) . ? N2 C25 1.462(8) . ? N2 C26 1.475(8) . ? N2 C22 1.479(8) . ? N3 C29 1.460(8) . ? N3 C30 1.467(9) . ? N3 C27 1.477(8) . ? N4 C32 1.449(8) . ? N4 C28 1.454(9) . ? N4 C31 1.476(8) . ? C21 C22 1.505(9) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.487(10) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? N5 C35 1.46(2) . ? N5 C36 1.478(13) . ? N5 C33 1.477(13) . ? N6 C37 1.441(12) . ? N6 C34 1.446(14) . ? N6 C38 1.475(14) . ? N7 C42 1.42(2) . ? N7 C39 1.464(14) . ? N7 C41 1.50(2) . ? N8 C43 1.44(2) . ? N8 C44 1.48(2) . ? N8 C40 1.48(2) . ? C33 C34 1.484(13) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 C40 1.501(14) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? C40 H40A 0.99 . ? C40 H40B 0.99 . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C45 C46 1.53(2) . ? C46 C47 1.361(10) 6_756 ? C46 C47 1.361(10) . ? C47 C48 1.362(12) . ? C47 H47 0.95 . ? C48 C49 1.371(12) . ? C48 H48 0.95 . ? C49 C48 1.371(12) 6_756 ? C49 H49 0.95 . ? C50 C51 1.46(2) . ? C51 C52 1.352(12) 6_656 ? C51 C52 1.352(12) . ? C52 C53 1.399(13) . ? C52 H52 0.95 . ? C53 C54 1.397(11) . ? C53 H53 0.95 . ? C54 C53 1.397(11) 6_656 ? C54 H54 0.95 . ? C55 N10 1.47(4) . ? C55 C56 1.54(4) . ? C56 N9 1.50(4) . ? C57 N9 1.54(5) . ? C58 N9 1.56(5) . ? C59 N10 1.25(6) . ? C60 N10 1.55(9) . ? C61 N11 1.50(4) . ? C61 C62 1.61(3) . ? C62 N12 1.39(5) . ? C63 N11 1.50(5) . ? C64 N11 1.61(8) . ? C65 N12 1.49(8) . ? C66 N12 1.60(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N8 Li2 N5 119.3(7) . . ? N8 Li2 N7 90.4(6) . . ? N5 Li2 N7 120.9(6) . . ? N9 Li2 N11 124.5(13) . . ? N9 Li2 N12 123.9(15) . . ? N11 Li2 N12 85.0(14) . . ? N8 Li2 N6 118.2(6) . . ? N5 Li2 N6 88.9(6) . . ? N7 Li2 N6 122.3(6) . . ? N9 Li2 N10 90.1(14) . . ? N11 Li2 N10 119.6(14) . . ? N12 Li2 N10 117.2(16) . . ? N9 Li2 C56 32.6(10) . . ? N11 Li2 C56 142.3(12) . . ? N12 Li2 C56 131.4(14) . . ? N10 Li2 C56 57.9(13) . . ? N8 Li2 C40 32.0(5) . . ? N5 Li2 C40 124.8(6) . . ? N7 Li2 C40 59.9(4) . . ? N6 Li2 C40 141.2(6) . . ? N9 Li2 C55 61.1(10) . . ? N11 Li2 C55 122.7(11) . . ? N12 Li2 C55 144.6(14) . . ? N10 Li2 C55 32.4(11) . . ? C56 Li2 C55 32.9(9) . . ? N8 Li2 C34 136.8(6) . . ? N5 Li2 C34 58.7(4) . . ? N7 Li2 C34 129.5(5) . . ? N6 Li2 C34 31.1(4) . . ? C40 Li2 C34 168.5(5) . . ? C1 Al1 H111 110.2(19) . . ? C1 Al1 H113 110.6(19) . . ? H111 Al1 H113 113.2(27) . . ? C1 Al1 H212 111.0(21) . . ? H111 Al1 H212 106.1(28) . . ? H113 Al1 H212 105.6(28) . . ? C1 Si1 C2 113.2(3) . . ? C1 Si1 C4 113.9(3) . . ? C2 Si1 C4 104.4(3) . . ? C1 Si1 C3 114.0(3) . . ? C2 Si1 C3 104.8(3) . . ? C4 Si1 C3 105.6(3) . . ? C1 Si2 C7 112.6(3) . . ? C1 Si2 C6 113.3(3) . . ? C7 Si2 C6 104.5(3) . . ? C1 Si2 C5 114.6(3) . . ? C7 Si2 C5 105.3(3) . . ? C6 Si2 C5 105.6(3) . . ? C1 Si3 C9 113.2(3) . . ? C1 Si3 C8 114.3(3) . . ? C9 Si3 C8 104.1(3) . . ? C1 Si3 C10 113.0(3) . . ? C9 Si3 C10 104.7(3) . . ? C8 Si3 C10 106.6(3) . . ? Si2 C1 Si3 112.2(3) . . ? Si2 C1 Si1 111.9(3) . . ? Si3 C1 Si1 112.2(3) . . ? Si2 C1 Al1 106.8(3) . . ? Si3 C1 Al1 106.4(3) . . ? Si1 C1 Al1 106.9(3) . . ? Si1 C2 H2A 109.5(2) . . ? Si1 C2 H2B 109.5(2) . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5(2) . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5(2) . . ? Si1 C3 H3B 109.5(2) . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5(2) . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5(2) . . ? Si1 C4 H4B 109.5(2) . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5(2) . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5(2) . . ? Si2 C5 H5B 109.5(2) . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5(2) . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5(2) . . ? Si2 C6 H6B 109.5(2) . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5(2) . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5(2) . . ? Si2 C7 H7B 109.5(2) . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5(2) . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? Si3 C8 H8A 109.5(2) . . ? Si3 C8 H8B 109.5(2) . . ? H8A C8 H8B 109.5 . . ? Si3 C8 H8C 109.5(2) . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? Si3 C9 H9A 109.5(2) . . ? Si3 C9 H9B 109.5(2) . . ? H9A C9 H9B 109.5 . . ? Si3 C9 H9C 109.5(2) . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? Si3 C10 H10A 109.5(2) . . ? Si3 C10 H10B 109.5(2) . . ? H10A C10 H10B 109.5 . . ? Si3 C10 H10C 109.5(2) . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C11 Al2 H112 109.3(18) . . ? C11 Al2 H211 112.0(22) . . ? H112 Al2 H211 106.1(29) . . ? C11 Al2 H213 113.6(26) . . ? H112 Al2 H213 114.4(33) . . ? H211 Al2 H213 100.9(34) . . ? C11 Si4 C13 115.5(4) . . ? C11 Si4 C14 115.7(4) . . ? C13 Si4 C14 106.1(4) . . ? C11 Si4 C12 109.4(4) . . ? C13 Si4 C12 103.0(5) . . ? C14 Si4 C12 105.8(4) . . ? C11 Si5 C16 112.7(3) . . ? C11 Si5 C17 113.5(4) . . ? C16 Si5 C17 104.8(4) . . ? C11 Si5 C15 113.0(3) . . ? C16 Si5 C15 104.8(3) . . ? C17 Si5 C15 107.2(4) . . ? C19 Si6 C20 108.4(4) . . ? C19 Si6 C18 104.8(4) . . ? C20 Si6 C18 106.4(4) . . ? C19 Si6 C11 113.7(4) . . ? C20 Si6 C11 112.5(3) . . ? C18 Si6 C11 110.4(4) . . ? Si4 C11 Si5 114.5(4) . . ? Si4 C11 Si6 112.2(4) . . ? Si5 C11 Si6 109.5(4) . . ? Si4 C11 Al2 107.5(4) . . ? Si5 C11 Al2 106.2(3) . . ? Si6 C11 Al2 106.5(3) . . ? Si4 C12 H12A 109.5(3) . . ? Si4 C12 H12B 109.5(3) . . ? H12A C12 H12B 109.5 . . ? Si4 C12 H12C 109.5(3) . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? Si4 C13 H13A 109.5(3) . . ? Si4 C13 H13B 109.5(4) . . ? H13A C13 H13B 109.5 . . ? Si4 C13 H13C 109.5(3) . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si4 C14 H14A 109.5(3) . . ? Si4 C14 H14B 109.5(3) . . ? H14A C14 H14B 109.5 . . ? Si4 C14 H14C 109.5(3) . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si5 C15 H15A 109.5(2) . . ? Si5 C15 H15B 109.5(2) . . ? H15A C15 H15B 109.5 . . ? Si5 C15 H15C 109.5(3) . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? Si5 C16 H16A 109.5(2) . . ? Si5 C16 H16B 109.5(3) . . ? H16A C16 H16B 109.5 . . ? Si5 C16 H16C 109.5(2) . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? Si5 C17 H17A 109.5(3) . . ? Si5 C17 H17B 109.5(2) . . ? H17A C17 H17B 109.5 . . ? Si5 C17 H17C 109.5(3) . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? Si6 C18 H18A 109.5(3) . . ? Si6 C18 H18B 109.5(4) . . ? H18A C18 H18B 109.5 . . ? Si6 C18 H18C 109.5(3) . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? Si6 C19 H19A 109.5(3) . . ? Si6 C19 H19B 109.5(3) . . ? H19A C19 H19B 109.5 . . ? Si6 C19 H19C 109.5(3) . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si6 C20 H20A 109.5(3) . . ? Si6 C20 H20B 109.5(3) . . ? H20A C20 H20B 109.5 . . ? Si6 C20 H20C 109.5(3) . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N1 Li1 N2 89.0(4) . . ? N1 Li1 N3 119.4(5) . . ? N2 Li1 N3 123.7(5) . . ? N1 Li1 N4 122.7(5) . . ? N2 Li1 N4 118.2(5) . . ? N3 Li1 N4 87.6(4) . . ? N1 Li1 C22 59.1(3) . . ? N2 Li1 C22 31.5(2) . . ? N3 Li1 C22 145.0(5) . . ? N4 Li1 C22 123.9(5) . . ? C23 N1 C24 109.7(6) . . ? C23 N1 C21 109.3(5) . . ? C24 N1 C21 108.7(5) . . ? C23 N1 Li1 109.2(5) . . ? C24 N1 Li1 118.2(5) . . ? C21 N1 Li1 101.3(5) . . ? C25 N2 C26 108.3(5) . . ? C25 N2 C22 110.4(5) . . ? C26 N2 C22 107.8(5) . . ? C25 N2 Li1 109.3(5) . . ? C26 N2 Li1 120.3(5) . . ? C22 N2 Li1 100.2(5) . . ? C29 N3 C30 108.0(6) . . ? C29 N3 C27 108.9(6) . . ? C30 N3 C27 109.5(6) . . ? C29 N3 Li1 118.1(5) . . ? C30 N3 Li1 109.4(5) . . ? C27 N3 Li1 102.6(5) . . ? C32 N4 C28 111.7(6) . . ? C32 N4 C31 106.9(6) . . ? C28 N4 C31 108.5(6) . . ? C32 N4 Li1 111.6(5) . . ? C28 N4 Li1 100.6(5) . . ? C31 N4 Li1 117.4(5) . . ? N1 C21 C22 112.4(6) . . ? N1 C21 H21A 109.1(4) . . ? C22 C21 H21A 109.1(4) . . ? N1 C21 H21B 109.1(4) . . ? C22 C21 H21B 109.1(4) . . ? H21A C21 H21B 107.9 . . ? N2 C22 C21 111.4(6) . . ? N2 C22 Li1 48.2(3) . . ? C21 C22 Li1 74.8(4) . . ? N2 C22 H22A 109.4(3) . . ? C21 C22 H22A 109.4(4) . . ? Li1 C22 H22A 154.0(2) . . ? N2 C22 H22B 109.4(3) . . ? C21 C22 H22B 109.4(4) . . ? Li1 C22 H22B 94.0(2) . . ? H22A C22 H22B 108.0 . . ? N1 C23 H23A 109.5(4) . . ? N1 C23 H23B 109.5(4) . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5(4) . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C24 H24A 109.5(4) . . ? N1 C24 H24B 109.5(4) . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5(4) . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 109.5(4) . . ? N2 C25 H25B 109.5(4) . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5(3) . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5(4) . . ? N2 C26 H26B 109.5(3) . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5(4) . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N3 C27 C28 112.5(6) . . ? N3 C27 H27A 109.1(4) . . ? C28 C27 H27A 109.1(5) . . ? N3 C27 H27B 109.1(4) . . ? C28 C27 H27B 109.1(5) . . ? H27A C27 H27B 107.8 . . ? N4 C28 C27 113.6(7) . . ? N4 C28 H28A 108.8(4) . . ? C27 C28 H28A 108.8(4) . . ? N4 C28 H28B 108.8(4) . . ? C27 C28 H28B 108.8(5) . . ? H28A C28 H28B 107.7 . . ? N3 C29 H29A 109.5(4) . . ? N3 C29 H29B 109.5(4) . . ? H29A C29 H29B 109.5 . . ? N3 C29 H29C 109.5(4) . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 H30A 109.5(4) . . ? N3 C30 H30B 109.5(4) . . ? H30A C30 H30B 109.5 . . ? N3 C30 H30C 109.5(4) . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N4 C31 H31A 109.5(4) . . ? N4 C31 H31B 109.5(4) . . ? H31A C31 H31B 109.5 . . ? N4 C31 H31C 109.5(4) . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N4 C32 H32A 109.5(4) . . ? N4 C32 H32B 109.5(4) . . ? H32A C32 H32B 109.5 . . ? N4 C32 H32C 109.5(4) . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C35 N5 C36 108.9(11) . . ? C35 N5 C33 109.1(12) . . ? C36 N5 C33 108.6(9) . . ? C35 N5 Li2 120.3(10) . . ? C36 N5 Li2 107.5(7) . . ? C33 N5 Li2 101.8(7) . . ? C37 N6 C34 111.1(9) . . ? C37 N6 C38 109.3(8) . . ? C34 N6 C38 111.3(10) . . ? C37 N6 Li2 117.7(8) . . ? C34 N6 Li2 98.6(6) . . ? C38 N6 Li2 108.4(7) . . ? C42 N7 C39 110.1(10) . . ? C42 N7 C41 108.6(10) . . ? C39 N7 C41 108.4(11) . . ? C42 N7 Li2 112.9(9) . . ? C39 N7 Li2 101.3(7) . . ? C41 N7 Li2 115.2(9) . . ? C43 N8 C44 112.2(12) . . ? C43 N8 C40 107.6(13) . . ? C44 N8 C40 109.4(13) . . ? C43 N8 Li2 112.7(11) . . ? C44 N8 Li2 114.0(9) . . ? C40 N8 Li2 100.2(7) . . ? N5 C33 C34 111.7(8) . . ? N5 C33 Li2 46.8(5) . . ? C34 C33 Li2 74.2(6) . . ? N5 C33 H33A 109.3(5) . . ? C34 C33 H33A 109.3(6) . . ? Li2 C33 H33A 97.4(3) . . ? N5 C33 H33B 109.3(5) . . ? C34 C33 H33B 109.3(6) . . ? Li2 C33 H33B 150.8(3) . . ? H33A C33 H33B 107.9 . . ? N6 C34 C33 115.5(8) . . ? N6 C34 Li2 50.3(5) . . ? C33 C34 Li2 74.8(6) . . ? N6 C34 H34A 108.4(5) . . ? C33 C34 H34A 108.4(6) . . ? Li2 C34 H34A 96.2(3) . . ? N6 C34 H34B 108.4(5) . . ? C33 C34 H34B 108.4(5) . . ? Li2 C34 H34B 153.2(3) . . ? H34A C34 H34B 107.5 . . ? N5 C35 H35A 109.5(9) . . ? N5 C35 H35B 109.5(10) . . ? H35A C35 H35B 109.5 . . ? N5 C35 H35C 109.5(9) . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N5 C36 H36A 109.5(6) . . ? N5 C36 H36B 109.5(6) . . ? H36A C36 H36B 109.5 . . ? N5 C36 H36C 109.5(8) . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N6 C37 H37A 109.5(7) . . ? N6 C37 H37B 109.5(6) . . ? H37A C37 H37B 109.5 . . ? N6 C37 H37C 109.5(6) . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N6 C38 H38A 109.5(6) . . ? N6 C38 H38B 109.5(6) . . ? H38A C38 H38B 109.5 . . ? N6 C38 H38C 109.5(7) . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N7 C39 C40 113.6(10) . . ? N7 C39 H39A 108.8(7) . . ? C40 C39 H39A 108.8(7) . . ? N7 C39 H39B 108.8(6) . . ? C40 C39 H39B 108.8(6) . . ? H39A C39 H39B 107.7 . . ? N8 C40 C39 114.3(9) . . ? N8 C40 Li2 47.8(5) . . ? C39 C40 Li2 76.1(6) . . ? N8 C40 H40A 108.7(7) . . ? C39 C40 H40A 108.7(7) . . ? Li2 C40 H40A 96.4(3) . . ? N8 C40 H40B 108.7(6) . . ? C39 C40 H40B 108.7(6) . . ? Li2 C40 H40B 151.8(3) . . ? H40A C40 H40B 107.6 . . ? N7 C41 H41A 109.5(8) . . ? N7 C41 H41B 109.5(8) . . ? H41A C41 H41B 109.5 . . ? N7 C41 H41C 109.5(8) . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 H42A 109.5(7) . . ? N7 C42 H42B 109.5(6) . . ? H42A C42 H42B 109.5 . . ? N7 C42 H42C 109.5(7) . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N8 C43 H43A 109.5(9) . . ? N8 C43 H43B 109.5(10) . . ? H43A C43 H43B 109.5 . . ? N8 C43 H43C 109.5(10) . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N8 C44 H44A 109.5(8) . . ? N8 C44 H44B 109.5(8) . . ? H44A C44 H44B 109.5 . . ? N8 C44 H44C 109.5(10) . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C47 C46 C47 118.1(12) 6_756 . ? C47 C46 C45 121.0(6) 6_756 . ? C47 C46 C45 121.0(6) . . ? C46 C47 C48 121.3(9) . . ? C46 C47 H47 119.4(6) . . ? C48 C47 H47 119.4(6) . . ? C47 C48 C49 120.7(11) . . ? C47 C48 H48 119.6(6) . . ? C49 C48 H48 119.6(7) . . ? C48 C49 C48 117.9(14) . 6_756 ? C48 C49 H49 121.1(7) . . ? C48 C49 H49 121.1(7) 6_756 . ? C52 C51 C52 117.4(19) 6_656 . ? C52 C51 C50 121.3(9) 6_656 . ? C52 C51 C50 121.3(9) . . ? C51 C52 C53 122.3(13) . . ? C51 C52 H52 118.9(9) . . ? C53 C52 H52 118.9(6) . . ? C54 C53 C52 121.3(11) . . ? C54 C53 H53 119.4(7) . . ? C52 C53 H53 119.4(6) . . ? C53 C54 C53 115.3(14) . 6_656 ? C53 C54 H54 122.3(7) . . ? C53 C54 H54 122.3(7) 6_656 . ? N10 C55 C56 106.5(27) . . ? N10 C55 Li2 52.6(19) . . ? C56 C55 Li2 72.8(16) . . ? N9 C56 C55 109.5(25) . . ? N9 C56 Li2 45.1(14) . . ? C55 C56 Li2 74.4(17) . . ? N11 C61 C62 108.3(19) . . ? N12 C62 C61 109.8(25) . . ? C56 N9 C57 107.4(27) . . ? C56 N9 C58 107.0(25) . . ? C57 N9 C58 109.0(27) . . ? C56 N9 Li2 102.3(19) . . ? C57 N9 Li2 111.1(23) . . ? C58 N9 Li2 119.2(22) . . ? C59 N10 C55 117.2(43) . . ? C59 N10 C60 114.9(45) . . ? C55 N10 C60 100.4(33) . . ? C59 N10 Li2 114.9(36) . . ? C55 N10 Li2 95.0(23) . . ? C60 N10 Li2 112.1(34) . . ? C63 N11 C61 113.3(31) . . ? C63 N11 C64 105.1(30) . . ? C61 N11 C64 105.8(27) . . ? C63 N11 Li2 107.0(20) . . ? C61 N11 Li2 104.5(17) . . ? C64 N11 Li2 121.5(26) . . ? C62 N12 C65 109.1(40) . . ? C62 N12 C66 108.9(37) . . ? C65 N12 C66 102.8(34) . . ? C62 N12 Li2 105.4(27) . . ? C65 N12 Li2 121.8(33) . . ? C66 N12 Li2 108.4(27) . . ? _refine_diff_density_max 0.439 _refine_diff_density_min -0.285 _refine_diff_density_rms 0.057 #==END data_oct1794 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[{(Me3Si)3C}AlBr2(C4H8O)]' _chemical_formula_analytical ? _chemical_formula_sum 'C14 H35 Al Br2 O Si3' _chemical_formula_weight 490.49 _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' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 12.558(4) _cell_length_b 13.394(4) _cell_length_c 13.434(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2259.6(14) _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 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.442 _exptl_crystal_density_method ? _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 3.784 _exptl_absorpt_correction_type ? _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 2827 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1181 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.95 _reflns_number_total 2827 _reflns_number_observed 1408 _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 ; The (Me3Si)3C group is disordered across the mirror plane with alternative Si atom sites and common C atom sites. Refinement on F^2^ for ALL reflections except for 1 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^)+(0.0415P)^2^+3.0778P] 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 2826 _refine_ls_number_parameters 118 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1620 _refine_ls_R_factor_obs 0.0650 _refine_ls_wR_factor_all 0.1344 _refine_ls_wR_factor_obs 0.1024 _refine_ls_goodness_of_fit_all 1.041 _refine_ls_goodness_of_fit_obs 1.146 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.146 _refine_ls_shift/esd_max 0.000 _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 Br Br 0.08742(6) 0.15192(5) 0.11304(5) 0.0380(2) Uani 1 d . . Si1 Si 0.3027(3) -0.0541(2) 0.3819(3) 0.0261(7) Uani 0.50 d P . Si2 Si 0.2558(3) -0.1322(2) 0.1686(2) 0.0247(8) Uani 0.50 d P . Si3 Si 0.3668(3) 0.0734(3) 0.1985(3) 0.0320(9) Uani 0.50 d P . Al Al 0.1256(2) 0.0534(2) 0.2500 0.0222(6) Uani 1 d S . O O 0.0058(5) -0.0309(4) 0.2500 0.0312(15) Uani 1 d S . C1 C 0.2639(6) -0.0165(6) 0.2500 0.020(2) Uani 1 d S . C2 C 0.3991(5) -0.1675(6) 0.3794(5) 0.067(3) Uani 1 d . . H2A H 0.4637(5) -0.1496(6) 0.3426(5) 0.101 Uiso 1 calc R . H2B H 0.3642(5) -0.2241(6) 0.3467(5) 0.101 Uiso 1 calc R . H2C H 0.4181(5) -0.1860(6) 0.4477(5) 0.101 Uiso 1 calc R . C3 C 0.1878(5) -0.1072(5) 0.4552(5) 0.036(2) Uani 1 d . . H3A H 0.2122(5) -0.1252(5) 0.5221(5) 0.055 Uiso 1 calc R . H3B H 0.1604(5) -0.1667(5) 0.4214(5) 0.055 Uiso 1 calc R . H3C H 0.1311(5) -0.0571(5) 0.4602(5) 0.055 Uiso 1 calc R . C4 C 0.3596(6) 0.0653(7) 0.4514(6) 0.073(3) Uani 1 d . . H4A H 0.4193(6) 0.0928(7) 0.4134(6) 0.110 Uiso 1 calc R . H4B H 0.3842(6) 0.0462(7) 0.5180(6) 0.110 Uiso 1 calc R . H4C H 0.3034(6) 0.1157(7) 0.4573(6) 0.110 Uiso 1 calc R . C5 C 0.1826(8) -0.2389(7) 0.2500 0.063(4) Uani 1 d S . H5A H 0.1768(8) -0.3002(7) 0.2105 0.094 Uiso 0.50 calc PR . H5B H 0.1113(8) -0.2160(7) 0.2687 0.094 Uiso 0.50 calc PR . H5C H 0.2243(8) -0.2523(7) 0.3102 0.094 Uiso 0.50 calc PR . C6 C 0.5083(8) 0.0395(8) 0.2500 0.077(4) Uani 1 d S . H6A H 0.5610(8) 0.0863(8) 0.2231 0.116 Uiso 0.50 calc PR . H6B H 0.5269(8) -0.0287(8) 0.2298 0.116 Uiso 0.50 calc PR . H6C H 0.5079(8) 0.0439(8) 0.3228 0.116 Uiso 0.50 calc PR . C7 C 0.3462(8) 0.2042(6) 0.2500 0.048(3) Uani 1 d S . H7A H 0.4003(8) 0.2491(6) 0.2224 0.071 Uiso 0.50 calc PR . H7B H 0.3526(8) 0.2028(6) 0.3227 0.071 Uiso 0.50 calc PR . H7C H 0.2752(8) 0.2282(6) 0.2315 0.071 Uiso 0.50 calc PR . C8 C -0.0578(5) -0.0603(6) 0.3366(6) 0.061(2) Uani 1 d . . H8A H -0.0373(5) -0.1279(6) 0.3592(6) 0.073 Uiso 1 calc R . H8B H -0.0464(5) -0.0129(6) 0.3921(6) 0.073 Uiso 1 calc R . C9 C -0.1693(5) -0.0590(6) 0.3053(5) 0.054(2) Uani 1 d . . H9A H -0.2054(5) 0.0014(6) 0.3310(5) 0.065 Uiso 1 calc R . H9B H -0.2069(5) -0.1187(6) 0.3310(5) 0.065 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 Br 0.0421(4) 0.0316(3) 0.0403(4) 0.0093(4) -0.0060(4) 0.0080(4) Si1 0.024(2) 0.032(2) 0.023(2) -0.003(2) -0.005(2) 0.0042(15) Si2 0.025(2) 0.023(2) 0.026(2) -0.0038(15) -0.006(2) 0.0038(15) Si3 0.019(2) 0.035(2) 0.042(2) 0.001(2) 0.006(2) -0.002(2) Al 0.0187(14) 0.0205(13) 0.0275(14) 0.000 0.000 -0.0011(11) O 0.017(3) 0.034(4) 0.042(4) 0.000 0.000 -0.002(3) C1 0.015(5) 0.023(4) 0.021(4) 0.000 0.000 -0.006(4) C2 0.041(4) 0.105(7) 0.057(5) 0.045(5) 0.013(4) 0.043(5) C3 0.044(4) 0.042(4) 0.023(3) 0.004(3) 0.003(3) 0.010(3) C4 0.045(5) 0.126(8) 0.048(5) -0.044(6) -0.027(4) 0.018(6) C5 0.040(7) 0.016(5) 0.132(11) 0.000 0.000 -0.006(5) C6 0.021(6) 0.048(7) 0.163(14) 0.000 0.000 -0.008(6) C7 0.032(6) 0.030(5) 0.081(8) 0.000 0.000 -0.011(5) C8 0.049(5) 0.085(6) 0.049(5) 0.014(5) 0.003(4) -0.031(5) C9 0.031(4) 0.072(5) 0.058(5) 0.000(4) 0.002(4) -0.009(4) _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 Br Al 2.315(2) . ? Si1 Si2 1.378(5) 6_556 ? Si1 C3 1.886(7) . ? Si1 C1 1.905(5) . ? Si1 C2 1.942(7) . ? Si1 C4 1.985(8) . ? Si1 Si3 2.175(5) 6_556 ? Si2 Si1 1.378(5) 6_556 ? Si2 C1 1.898(7) . ? Si2 C3 1.900(7) 6_556 ? Si2 C2 1.969(7) 6_556 ? Si2 C5 2.021(8) . ? Si2 Si2 2.186(7) 6_556 ? Si3 Si3 1.384(7) 6_556 ? Si3 C1 1.897(8) . ? Si3 C7 1.901(9) . ? Si3 C6 1.961(10) . ? Si3 C4 2.019(9) 6_556 ? Si3 Si1 2.175(5) 6_556 ? Al O 1.881(6) . ? Al C1 1.973(8) . ? Al Br 2.315(2) 6_556 ? O C8 1.465(7) 6_556 ? O C8 1.465(7) . ? C1 Si3 1.897(8) 6_556 ? C1 Si2 1.898(7) 6_556 ? C1 Si1 1.905(5) 6_556 ? C8 C9 1.462(9) . ? C9 C9 1.486(13) 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 Si2 Si1 C3 69.2(3) 6_556 . ? Si2 Si1 C1 68.5(3) 6_556 . ? C3 Si1 C1 112.9(3) . . ? Si2 Si1 C2 70.4(3) 6_556 . ? C3 Si1 C2 101.0(3) . . ? C1 Si1 C2 110.5(3) . . ? Si2 Si1 C4 175.1(3) 6_556 . ? C3 Si1 C4 109.4(4) . . ? C1 Si1 C4 108.5(4) . . ? C2 Si1 C4 114.4(4) . . ? Si2 Si1 Si3 120.6(3) 6_556 6_556 ? C3 Si1 Si3 146.9(3) . 6_556 ? C1 Si1 Si3 54.9(3) . 6_556 ? C2 Si1 Si3 112.0(3) . 6_556 ? C4 Si1 Si3 57.9(3) . 6_556 ? Si1 Si2 C1 69.0(2) 6_556 . ? Si1 Si2 C3 68.1(3) 6_556 6_556 ? C1 Si2 C3 112.6(3) . 6_556 ? Si1 Si2 C2 68.3(3) 6_556 6_556 ? C1 Si2 C2 109.6(4) . 6_556 ? C3 Si2 C2 99.6(3) 6_556 6_556 ? Si1 Si2 C5 175.7(3) 6_556 . ? C1 Si2 C5 106.9(3) . . ? C3 Si2 C5 113.2(3) 6_556 . ? C2 Si2 C5 115.0(4) 6_556 . ? Si1 Si2 Si2 119.5(2) 6_556 6_556 ? C1 Si2 Si2 54.8(2) . 6_556 ? C3 Si2 Si2 151.1(2) 6_556 6_556 ? C2 Si2 Si2 109.1(2) 6_556 6_556 ? C5 Si2 Si2 57.3(2) . 6_556 ? Si3 Si3 C1 68.62(14) 6_556 . ? Si3 Si3 C7 68.66(15) 6_556 . ? C1 Si3 C7 111.1(4) . . ? Si3 Si3 C6 69.34(15) 6_556 . ? C1 Si3 C6 110.0(4) . . ? C7 Si3 C6 102.0(4) . . ? Si3 Si3 C4 176.0(3) 6_556 6_556 ? C1 Si3 C4 107.4(3) . 6_556 ? C7 Si3 C4 114.0(3) . 6_556 ? C6 Si3 C4 112.3(3) . 6_556 ? Si3 Si3 Si1 119.75(13) 6_556 6_556 ? C1 Si3 Si1 55.3(2) . 6_556 ? C7 Si3 Si1 148.7(4) . 6_556 ? C6 Si3 Si1 109.2(3) . 6_556 ? C4 Si3 Si1 56.3(3) 6_556 6_556 ? O Al C1 114.8(3) . . ? O Al Br 100.16(13) . 6_556 ? C1 Al Br 116.94(12) . 6_556 ? O Al Br 100.16(13) . . ? C1 Al Br 116.94(12) . . ? Br Al Br 105.30(11) 6_556 . ? C8 O C8 105.1(7) 6_556 . ? C8 O Al 126.7(4) 6_556 . ? C8 O Al 126.7(4) . . ? Si3 C1 Si3 42.8(3) 6_556 . ? Si3 C1 Si2 139.9(5) 6_556 . ? Si3 C1 Si2 110.2(3) . . ? Si3 C1 Si2 110.2(3) 6_556 6_556 ? Si3 C1 Si2 139.9(5) . 6_556 ? Si2 C1 Si2 70.3(3) . 6_556 ? Si3 C1 Si1 109.4(4) 6_556 6_556 ? Si3 C1 Si1 69.8(2) . 6_556 ? Si2 C1 Si1 42.5(2) . 6_556 ? Si2 C1 Si1 109.5(4) 6_556 6_556 ? Si3 C1 Si1 69.8(2) 6_556 . ? Si3 C1 Si1 109.4(4) . . ? Si2 C1 Si1 109.5(4) . . ? Si2 C1 Si1 42.5(2) 6_556 . ? Si1 C1 Si1 136.8(5) 6_556 . ? Si3 C1 Al 107.3(4) 6_556 . ? Si3 C1 Al 107.3(4) . . ? Si2 C1 Al 109.9(4) . . ? Si2 C1 Al 109.9(4) 6_556 . ? Si1 C1 Al 110.5(2) 6_556 . ? Si1 C1 Al 110.5(2) . . ? C9 C8 O 106.9(6) . . ? C8 C9 C9 106.7(4) . 6_556 ? _refine_diff_density_max 0.572 _refine_diff_density_min -0.514 _refine_diff_density_rms 0.120 #==END data_oct596 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(thf)2Li(C6H5NH)2AlH(Tsi)]' _chemical_formula_analytical ? _chemical_formula_sum 'C30 H56 Al Li N2 O2 Si3' _chemical_formula_weight 594.96 _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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.549(3) _cell_length_b 16.885(5) _cell_length_c 21.913(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3533.1(17) _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 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.118 _exptl_crystal_density_method ? _exptl_crystal_F_000 1296 _exptl_absorpt_coefficient_mu 0.186 _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 3494 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1423 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3494 _reflns_number_observed 2221 _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 ; 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^)+(0.1126P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.08(44) _refine_ls_number_reflns 3494 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1343 _refine_ls_R_factor_obs 0.0798 _refine_ls_wR_factor_all 0.2268 _refine_ls_wR_factor_obs 0.1915 _refine_ls_goodness_of_fit_all 1.035 _refine_ls_goodness_of_fit_obs 1.120 _refine_ls_restrained_S_all 1.035 _refine_ls_restrained_S_obs 1.120 _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 Al Al 0.6030(3) 0.0780(2) 0.81362(12) 0.0199(7) Uani 1 d . . H3 H 0.6823(104) 0.0265(52) 0.7827(39) 0.030 Uiso 1 d . . Si1 Si 0.5850(3) 0.1677(2) 0.94258(11) 0.0252(7) Uani 1 d . . Si2 Si 0.8128(3) 0.0427(2) 0.91629(12) 0.0259(7) Uani 1 d . . Si3 Si 0.5043(3) -0.0094(2) 0.93325(13) 0.0303(7) Uani 1 d . . O1 O 0.3123(8) 0.2539(4) 0.7623(3) 0.034(2) Uani 1 d . . O2 O 0.4365(7) 0.1836(4) 0.6467(3) 0.032(2) Uani 1 d . . N1 N 0.6461(8) 0.1782(5) 0.7803(3) 0.020(2) Uani 1 d . . H1 H 0.6337(106) 0.2189(57) 0.8024(43) 0.030 Uiso 1 d . . N2 N 0.4160(10) 0.0723(5) 0.7885(3) 0.028(2) Uani 1 d . . H2 H 0.3393(122) 0.0948(64) 0.8043(50) 0.042 Uiso 1 d . . C1 C 0.6252(11) 0.0728(5) 0.9053(4) 0.024(2) Uani 1 d . . C2 C 0.5623(13) 0.1597(7) 1.0281(4) 0.043(3) Uani 1 d . . H2C H 0.5411(13) 0.2121(7) 1.0450(4) 0.064 Uiso 1 calc R . H2B H 0.6488(13) 0.1395(7) 1.0464(4) 0.064 Uiso 1 calc R . H2A H 0.4850(13) 0.1233(7) 1.0372(4) 0.064 Uiso 1 calc R . C3 C 0.7234(13) 0.2452(6) 0.9321(5) 0.043(3) Uani 1 d . . H3C H 0.6951(13) 0.2939(6) 0.9530(5) 0.065 Uiso 1 calc R . H3B H 0.7356(13) 0.2560(6) 0.8885(5) 0.065 Uiso 1 calc R . H3A H 0.8121(13) 0.2261(6) 0.9492(5) 0.065 Uiso 1 calc R . C4 C 0.4232(13) 0.2154(6) 0.9124(4) 0.037(3) Uani 1 d . . H4C H 0.4071(13) 0.2655(6) 0.9339(4) 0.055 Uiso 1 calc R . H4B H 0.3431(13) 0.1801(6) 0.9189(4) 0.055 Uiso 1 calc R . H4A H 0.4344(13) 0.2257(6) 0.8687(4) 0.055 Uiso 1 calc R . C5 C 0.9309(11) 0.0993(7) 0.8661(5) 0.040(3) Uani 1 d . . H5C H 0.9177(11) 0.1561(7) 0.8732(5) 0.060 Uiso 1 calc R . H5B H 0.9097(11) 0.0870(7) 0.8234(5) 0.060 Uiso 1 calc R . H5A H 1.0282(11) 0.0849(7) 0.8750(5) 0.060 Uiso 1 calc R . C6 C 0.8849(12) 0.0584(7) 0.9953(4) 0.038(3) Uani 1 d . . H6C H 0.8269(12) 0.0298(7) 1.0249(4) 0.056 Uiso 1 calc R . H6B H 0.8840(12) 0.1151(7) 1.0050(4) 0.056 Uiso 1 calc R . H6A H 0.9812(12) 0.0385(7) 0.9972(4) 0.056 Uiso 1 calc R . C7 C 0.8486(13) -0.0637(6) 0.8981(5) 0.044(3) Uani 1 d . . H7C H 0.7888(13) -0.0976(6) 0.9234(5) 0.066 Uiso 1 calc R . H7B H 0.9472(13) -0.0757(6) 0.9065(5) 0.066 Uiso 1 calc R . H7A H 0.8287(13) -0.0736(6) 0.8549(5) 0.066 Uiso 1 calc R . C8 C 0.5592(14) -0.0522(7) 1.0087(5) 0.050(3) Uani 1 d . . H8C H 0.6558(14) -0.0715(7) 1.0057(5) 0.075 Uiso 1 calc R . H8B H 0.4970(14) -0.0962(7) 1.0194(5) 0.075 Uiso 1 calc R . H8A H 0.5536(14) -0.0111(7) 1.0402(5) 0.075 Uiso 1 calc R . C9 C 0.4896(16) -0.0952(6) 0.8794(5) 0.051(4) Uani 1 d . . H9C H 0.5832(16) -0.1165(6) 0.8711(5) 0.077 Uiso 1 calc R . H9B H 0.4468(16) -0.0774(6) 0.8411(5) 0.077 Uiso 1 calc R . H9A H 0.4313(16) -0.1365(6) 0.8978(5) 0.077 Uiso 1 calc R . C10 C 0.3204(11) 0.0249(8) 0.9450(5) 0.048(3) Uani 1 d . . H10C H 0.3198(11) 0.0702(8) 0.9730(5) 0.073 Uiso 1 calc R . H10B H 0.2646(11) -0.0183(8) 0.9624(5) 0.073 Uiso 1 calc R . H10A H 0.2801(11) 0.0408(8) 0.9057(5) 0.073 Uiso 1 calc R . C11 C 0.7462(10) 0.2026(6) 0.7360(4) 0.022(2) Uani 1 d . . C12 C 0.8162(12) 0.1480(6) 0.7008(4) 0.030(2) Uani 1 d . . H12 H 0.8020(12) 0.0931(6) 0.7081(4) 0.036 Uiso 1 calc R . C13 C 0.9072(13) 0.1714(7) 0.6548(4) 0.040(3) Uani 1 d . . H13 H 0.9593(13) 0.1329(7) 0.6328(4) 0.048 Uiso 1 calc R . C14 C 0.9218(12) 0.2509(7) 0.6411(5) 0.038(3) Uani 1 d . . H14 H 0.9802(12) 0.2675(7) 0.6084(5) 0.045 Uiso 1 calc R . C15 C 0.8504(12) 0.3051(7) 0.6755(5) 0.040(3) Uani 1 d . . H15 H 0.8596(12) 0.3599(7) 0.6665(5) 0.048 Uiso 1 calc R . C16 C 0.7665(11) 0.2821(6) 0.7224(5) 0.032(3) Uani 1 d . . H16 H 0.7208(11) 0.3212(6) 0.7464(5) 0.038 Uiso 1 calc R . C17 C 0.3494(10) 0.0287(5) 0.7426(4) 0.025(2) Uani 1 d . . C18 C 0.2062(12) 0.0172(6) 0.7398(5) 0.034(3) Uani 1 d . . H18 H 0.1500(12) 0.0376(6) 0.7719(5) 0.041 Uiso 1 calc R . C19 C 0.1416(12) -0.0220(7) 0.6931(6) 0.042(3) Uani 1 d . . H19 H 0.0427(12) -0.0282(7) 0.6932(6) 0.051 Uiso 1 calc R . C20 C 0.2195(14) -0.0520(7) 0.6465(6) 0.050(3) Uani 1 d . . H20 H 0.1748(14) -0.0790(7) 0.6138(6) 0.060 Uiso 1 calc R . C21 C 0.3618(14) -0.0435(7) 0.6466(5) 0.045(3) Uani 1 d . . H21 H 0.4163(14) -0.0649(7) 0.6143(5) 0.054 Uiso 1 calc R . C22 C 0.4259(12) -0.0035(6) 0.6941(4) 0.030(2) Uani 1 d . . H22 H 0.5249(12) 0.0023(6) 0.6938(4) 0.036 Uiso 1 calc R . C23 C 0.1719(11) 0.2377(7) 0.7817(6) 0.044(3) Uani 1 d . . H23B H 0.1718(11) 0.2006(7) 0.8167(6) 0.053 Uiso 1 calc R . H23A H 0.1170(11) 0.2139(7) 0.7480(6) 0.053 Uiso 1 calc R . C24 C 0.1118(15) 0.3153(8) 0.7997(6) 0.061(4) Uani 1 d . . H24B H 0.0529(15) 0.3370(8) 0.7665(6) 0.073 Uiso 1 calc R . H24A H 0.0535(15) 0.3097(8) 0.8368(6) 0.073 Uiso 1 calc R . C25 C 0.2326(13) 0.3679(6) 0.8116(6) 0.047(3) Uani 1 d . . H25B H 0.2609(13) 0.3656(6) 0.8550(6) 0.056 Uiso 1 calc R . H25A H 0.2103(13) 0.4234(6) 0.8008(6) 0.056 Uiso 1 calc R . C26 C 0.3442(13) 0.3357(6) 0.7714(6) 0.045(3) Uani 1 d . . H26B H 0.3454(13) 0.3641(6) 0.7319(6) 0.054 Uiso 1 calc R . H26A H 0.4371(13) 0.3416(6) 0.7910(6) 0.054 Uiso 1 calc R . C27 C 0.2995(13) 0.1843(9) 0.6214(5) 0.052(3) Uani 1 d . . H27B H 0.2502(13) 0.2341(9) 0.6316(5) 0.062 Uiso 1 calc R . H27A H 0.2439(13) 0.1390(9) 0.6367(5) 0.062 Uiso 1 calc R . C28 C 0.3225(18) 0.1778(13) 0.5547(6) 0.101(7) Uani 1 d . . H28B H 0.2900(18) 0.1254(13) 0.5402(6) 0.121 Uiso 1 calc R . H28A H 0.2676(18) 0.2191(13) 0.5334(6) 0.121 Uiso 1 calc R . C29 C 0.4658(18) 0.1871(12) 0.5412(6) 0.083(5) Uani 1 d . . H29B H 0.4857(18) 0.2417(12) 0.5271(6) 0.099 Uiso 1 calc R . H29A H 0.4955(18) 0.1494(12) 0.5091(6) 0.099 Uiso 1 calc R . C30 C 0.5396(12) 0.1703(8) 0.6000(5) 0.043(3) Uani 1 d . . H30B H 0.5734(12) 0.1149(8) 0.6011(5) 0.051 Uiso 1 calc R . H30A H 0.6205(12) 0.2063(8) 0.6053(5) 0.051 Uiso 1 calc R . Li Li 0.4476(19) 0.1788(10) 0.7351(8) 0.034(4) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Al 0.021(2) 0.0221(14) 0.0161(12) -0.0023(12) -0.0005(14) 0.0015(13) Si1 0.029(2) 0.0292(14) 0.0178(12) -0.0028(11) -0.0038(13) 0.0054(14) Si2 0.0192(15) 0.035(2) 0.0234(13) -0.0017(12) -0.0018(12) 0.0071(14) Si3 0.031(2) 0.0303(15) 0.0296(15) 0.0096(13) -0.0011(14) -0.0076(15) O1 0.033(4) 0.038(4) 0.031(4) -0.004(3) 0.005(4) 0.003(4) O2 0.026(4) 0.044(4) 0.027(4) 0.001(3) 0.001(3) -0.005(4) N1 0.022(5) 0.018(4) 0.020(4) -0.006(3) 0.003(3) 0.006(4) N2 0.035(5) 0.032(5) 0.018(4) -0.008(4) 0.003(4) 0.001(4) C1 0.038(6) 0.020(5) 0.015(4) 0.003(4) -0.005(4) 0.000(5) C2 0.054(8) 0.055(7) 0.019(5) -0.011(5) -0.007(5) 0.019(7) C3 0.060(8) 0.025(5) 0.045(7) -0.008(5) -0.016(7) 0.005(6) C4 0.053(8) 0.034(6) 0.023(5) -0.006(5) 0.004(6) 0.013(6) C5 0.015(6) 0.076(8) 0.029(5) -0.005(6) 0.008(5) 0.003(6) C6 0.030(6) 0.052(7) 0.031(5) -0.008(5) -0.006(5) 0.000(6) C7 0.051(8) 0.039(7) 0.042(6) -0.013(5) -0.012(6) 0.024(6) C8 0.063(9) 0.048(7) 0.040(6) 0.019(6) -0.001(6) -0.007(7) C9 0.071(10) 0.037(6) 0.047(7) 0.003(5) -0.009(7) -0.033(7) C10 0.021(6) 0.076(9) 0.049(7) 0.012(7) 0.009(6) -0.010(6) C11 0.021(5) 0.028(5) 0.018(5) -0.002(4) -0.001(4) -0.005(5) C12 0.035(6) 0.028(5) 0.028(5) -0.004(4) 0.003(5) -0.006(5) C13 0.041(7) 0.054(7) 0.024(5) -0.002(5) 0.002(6) -0.003(7) C14 0.025(6) 0.057(7) 0.031(5) 0.006(6) 0.008(5) -0.017(6) C15 0.031(7) 0.042(7) 0.047(7) 0.015(6) 0.006(6) 0.003(5) C16 0.031(6) 0.034(6) 0.030(5) -0.001(5) -0.003(5) -0.008(5) C17 0.027(6) 0.023(5) 0.026(5) 0.002(4) -0.007(4) -0.010(5) C18 0.029(6) 0.030(6) 0.043(6) -0.001(5) -0.003(6) -0.001(5) C19 0.024(6) 0.036(6) 0.067(8) 0.003(6) -0.010(6) -0.009(5) C20 0.046(8) 0.053(8) 0.050(7) -0.009(6) -0.012(7) -0.021(7) C21 0.066(9) 0.035(6) 0.033(6) -0.017(5) -0.009(6) 0.007(7) C22 0.032(6) 0.031(6) 0.028(5) -0.003(5) -0.002(5) 0.014(5) C23 0.020(6) 0.050(7) 0.062(8) -0.005(6) -0.004(6) -0.003(6) C24 0.050(8) 0.073(10) 0.059(8) -0.029(7) 0.006(7) 0.004(8) C25 0.053(8) 0.028(6) 0.060(8) 0.002(6) 0.027(7) 0.009(6) C26 0.047(8) 0.031(6) 0.057(7) -0.004(6) 0.017(6) 0.004(6) C27 0.042(8) 0.079(9) 0.035(6) 0.006(6) -0.009(6) -0.006(8) C28 0.064(11) 0.202(21) 0.036(7) 0.000(11) -0.027(8) -0.029(14) C29 0.086(13) 0.129(15) 0.033(7) 0.005(8) 0.000(8) 0.022(12) C30 0.034(7) 0.057(7) 0.037(6) -0.004(6) 0.009(5) 0.012(6) Li 0.037(11) 0.032(9) 0.032(9) 0.009(8) 0.007(8) -0.004(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al N2 1.871(10) . ? Al N1 1.888(8) . ? Al C1 2.022(9) . ? Al Li 2.84(2) . ? Si1 C1 1.840(10) . ? Si1 C4 1.863(11) . ? Si1 C3 1.874(12) . ? Si1 C2 1.891(10) . ? Si2 C5 1.842(11) . ? Si2 C7 1.873(10) . ? Si2 C1 1.877(11) . ? Si2 C6 1.882(10) . ? Si3 C10 1.867(12) . ? Si3 C9 1.873(11) . ? Si3 C8 1.878(11) . ? Si3 C1 1.907(10) . ? O1 C26 1.428(13) . ? O1 C23 1.433(13) . ? O1 Li 1.91(2) . ? O2 C27 1.421(13) . ? O2 C30 1.438(12) . ? O2 Li 1.94(2) . ? N1 C11 1.423(12) . ? N1 Li 2.14(2) . ? N2 C17 1.400(12) . ? N2 Li 2.17(2) . ? C11 C12 1.375(13) . ? C11 C16 1.389(13) . ? C12 C13 1.388(15) . ? C13 C14 1.38(2) . ? C14 C15 1.37(2) . ? C15 C16 1.360(14) . ? C17 C18 1.382(15) . ? C17 C22 1.400(14) . ? C17 Li 2.71(2) . ? C18 C19 1.37(2) . ? C19 C20 1.36(2) . ? C20 C21 1.37(2) . ? C21 C22 1.383(14) . ? C23 C24 1.48(2) . ? C24 C25 1.48(2) . ? C25 C26 1.486(15) . ? C27 C28 1.48(2) . ? C28 C29 1.41(2) . ? C29 C30 1.49(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 N2 Al N1 98.1(4) . . ? N2 Al C1 113.0(4) . . ? N1 Al C1 113.6(4) . . ? N2 Al Li 49.8(4) . . ? N1 Al Li 48.9(4) . . ? C1 Al Li 133.1(5) . . ? C1 Si1 C4 113.1(5) . . ? C1 Si1 C3 114.0(5) . . ? C4 Si1 C3 103.9(5) . . ? C1 Si1 C2 113.7(5) . . ? C4 Si1 C2 106.7(5) . . ? C3 Si1 C2 104.6(5) . . ? C5 Si2 C7 105.0(5) . . ? C5 Si2 C1 111.5(5) . . ? C7 Si2 C1 114.0(5) . . ? C5 Si2 C6 104.7(5) . . ? C7 Si2 C6 105.3(5) . . ? C1 Si2 C6 115.4(5) . . ? C10 Si3 C9 104.9(6) . . ? C10 Si3 C8 105.1(6) . . ? C9 Si3 C8 106.1(5) . . ? C10 Si3 C1 112.8(5) . . ? C9 Si3 C1 113.9(5) . . ? C8 Si3 C1 113.2(5) . . ? C26 O1 C23 110.1(8) . . ? C26 O1 Li 122.8(9) . . ? C23 O1 Li 126.9(9) . . ? C27 O2 C30 110.6(8) . . ? C27 O2 Li 116.1(8) . . ? C30 O2 Li 131.8(9) . . ? C11 N1 Al 132.0(6) . . ? C11 N1 Li 106.2(7) . . ? Al N1 Li 89.4(6) . . ? C17 N2 Al 132.3(7) . . ? C17 N2 Li 96.4(7) . . ? Al N2 Li 89.0(6) . . ? Si1 C1 Si2 112.2(5) . . ? Si1 C1 Si3 111.4(5) . . ? Si2 C1 Si3 109.9(5) . . ? Si1 C1 Al 112.4(5) . . ? Si2 C1 Al 103.9(5) . . ? Si3 C1 Al 106.7(5) . . ? C12 C11 C16 117.4(9) . . ? C12 C11 N1 121.0(9) . . ? C16 C11 N1 121.3(9) . . ? C11 C12 C13 121.4(10) . . ? C14 C13 C12 119.8(11) . . ? C15 C14 C13 118.7(10) . . ? C16 C15 C14 121.3(11) . . ? C15 C16 C11 121.3(10) . . ? C18 C17 C22 115.4(10) . . ? C18 C17 N2 123.7(10) . . ? C22 C17 N2 120.9(9) . . ? C18 C17 Li 118.1(8) . . ? C22 C17 Li 97.8(7) . . ? N2 C17 Li 52.7(6) . . ? C19 C18 C17 123.2(11) . . ? C20 C19 C18 119.7(11) . . ? C19 C20 C21 120.2(11) . . ? C20 C21 C22 119.5(12) . . ? C21 C22 C17 122.0(11) . . ? O1 C23 C24 105.8(10) . . ? C25 C24 C23 106.0(11) . . ? C24 C25 C26 103.6(9) . . ? O1 C26 C25 106.5(9) . . ? O2 C27 C28 104.4(11) . . ? C29 C28 C27 110.0(12) . . ? C28 C29 C30 104.8(12) . . ? O2 C30 C29 105.2(10) . . ? O1 Li O2 104.3(9) . . ? O1 Li N1 117.3(9) . . ? O2 Li N1 120.7(9) . . ? O1 Li N2 106.8(8) . . ? O2 Li N2 124.5(9) . . ? N1 Li N2 82.5(7) . . ? O1 Li C17 111.6(8) . . ? O2 Li C17 94.7(8) . . ? N1 Li C17 105.9(7) . . ? N2 Li C17 30.9(4) . . ? O1 Li Al 124.3(8) . . ? O2 Li Al 131.2(9) . . ? N1 Li Al 41.7(4) . . ? N2 Li Al 41.2(4) . . ? C17 Li Al 65.4(4) . . ? _refine_diff_density_max 0.388 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.096