Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 186 loop_ _publ_author_name 'John Bradley' 'Stephen J. Archibald' 'Fei Cheng' 'Carl Kruger' 'Frederic Lefebvre' 'Christian W. Lehmann' 'Riccardo Rovai' 'Ralf Supplit' _publ_contact_author_name 'Dr John Bradley' _publ_contact_author_address ; Chemistry University of Hull Cottingham Road Hull HU6 7RX UNITED KINGDOM ; _publ_contact_author_email 'J.S.BRADLEY@HULL.AC.UK' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Precursors for Non-Oxide Sol-Gel Chemistry with Tris(dimethylamino)silylamine and its Derivatives: The Syntheses and Structures of Tris(dimethylamino)silylamidolithium, [((CH3)2N)3SiNHLi]4, Tris(dimethylamino)silylamino)(tetrahydrofuran)alanane, (C4H8O)Al[NHSi(N(CH3)2)3]3, Tris(dimethylamino)alane (((CH3)2N)3SiNH)3Al and Bis(tetrahydrofuran)lithium tetrakis(tris(dimethylamino)silylamino)alanate, Li(THF)2+[(((CH3)2N)3SiNH)4Al]-. ; data_2914 _database_code_CSD 194606 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_compound_source 'see paper' _chemical_formula_moiety ? _chemical_formula_sum 'C24 H76 Li4 N16 Si4' _chemical_formula_weight 729.13 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' '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' '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 'P 1 21/n 1' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.5670(5) _cell_length_b 8.9071(8) _cell_length_c 22.3754(16) _cell_angle_alpha 90.00 _cell_angle_beta 96.861(5) _cell_angle_gamma 90.00 _cell_volume 2288.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 9.3 _cell_measurement_theta_max 22.7 _exptl_crystal_description plate _exptl_crystal_colour white _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.058 _exptl_crystal_density_method none _exptl_crystal_F_000 800 _exptl_absorpt_coefficient_mu 0.165 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details none _publ_section_exptl_prep ; The crystal was mounted in a Lindemann glass capillary under argon. ; _diffrn_ambient_temperature 293 _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4' _diffrn_measurement_method '\w-2\q scan' _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 30 _diffrn_standards_decay_% 20.00 _diffrn_reflns_number 5345 _diffrn_reflns_av_R_equivalents 0.0159 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.46 _diffrn_reflns_theta_max 27.43 _reflns_number_total 5217 _reflns_number_gt 3039 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_cell_refinement 'EXPRESS / CAD4 software (Enraf-Nonius, 1995)' _computing_data_reduction 'DATAP (Coppens,Leiserowitz & Rabinovich, 1965)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP (Johnson, 1976)' _publ_section_exptl_refinement ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef none _refine_ls_number_reflns 5217 _refine_ls_number_parameters 225 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1224 _refine_ls_R_factor_gt 0.0487 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_obs 0.1429 _refine_ls_goodness_of_fit_ref 0.975 _refine_ls_restrained_S_all 0.975 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.2301(3) 1.2532(4) 0.13762(17) 0.0817(10) Uani 1 1 d . . . H1A H 0.2019 1.2971 0.1723 0.123 Uiso 1 1 calc R . . H1B H 0.1750 1.2709 0.1027 0.123 Uiso 1 1 calc R . . H1C H 0.3035 1.2977 0.1318 0.123 Uiso 1 1 calc R . . C2 C 0.3176(3) 1.0564(5) 0.20252(15) 0.1034(14) Uani 1 1 d . . . H2A H 0.3903 1.1090 0.2041 0.155 Uiso 1 1 calc R . . H2B H 0.3318 0.9502 0.2040 0.155 Uiso 1 1 calc R . . H2C H 0.2784 1.0855 0.2362 0.155 Uiso 1 1 calc R . . C3 C 0.3960(2) 0.8505(4) 0.08492(15) 0.0720(9) Uani 1 1 d . . . H3A H 0.4423 0.8768 0.1219 0.108 Uiso 1 1 calc R . . H3B H 0.3916 0.9347 0.0580 0.108 Uiso 1 1 calc R . . H3C H 0.4309 0.7669 0.0668 0.108 Uiso 1 1 calc R . . C4 C 0.2823(3) 0.6793(4) 0.13768(16) 0.0841(11) Uani 1 1 d . . . H4A H 0.3121 0.5938 0.1183 0.126 Uiso 1 1 calc R . . H4B H 0.2051 0.6578 0.1470 0.126 Uiso 1 1 calc R . . H4C H 0.3320 0.7011 0.1741 0.126 Uiso 1 1 calc R . . C5 C 0.0280(3) 0.9219(6) 0.18736(16) 0.1033(14) Uani 1 1 d . . . H5A H -0.0510 0.9563 0.1848 0.155 Uiso 1 1 calc R . . H5B H 0.0792 0.9982 0.2057 0.155 Uiso 1 1 calc R . . H5C H 0.0366 0.8322 0.2113 0.155 Uiso 1 1 calc R . . C6 C -0.0044(3) 0.7603(4) 0.09961(18) 0.0901(12) Uani 1 1 d . . . H6A H 0.0181 0.6720 0.1227 0.135 Uiso 1 1 calc R . . H6B H 0.0146 0.7479 0.0593 0.135 Uiso 1 1 calc R . . H6C H -0.0868 0.7756 0.0986 0.135 Uiso 1 1 calc R . . C7 C 0.3081(3) 0.9572(3) -0.09720(15) 0.0725(9) Uani 1 1 d . . . H7A H 0.3508 1.0219 -0.0682 0.109 Uiso 1 1 calc R . . H7B H 0.2273 0.9849 -0.1018 0.109 Uiso 1 1 calc R . . H7C H 0.3382 0.9669 -0.1352 0.109 Uiso 1 1 calc R . . C8 C 0.4430(2) 0.7567(4) -0.06987(18) 0.0766(10) Uani 1 1 d . . . H8A H 0.4722 0.7632 -0.1082 0.115 Uiso 1 1 calc R . . H8B H 0.4500 0.6553 -0.0554 0.115 Uiso 1 1 calc R . . H8C H 0.4871 0.8222 -0.0417 0.115 Uiso 1 1 calc R . . C9 C 0.2743(3) 0.4422(4) -0.02103(16) 0.0912(11) Uani 1 1 d . . . H9A H 0.2601 0.3361 -0.0207 0.137 Uiso 1 1 calc R . . H9B H 0.2200 0.4927 0.0013 0.137 Uiso 1 1 calc R . . H9C H 0.3523 0.4623 -0.0029 0.137 Uiso 1 1 calc R . . C10 C 0.3207(3) 0.4031(4) -0.12158(19) 0.0956(12) Uani 1 1 d . . . H10A H 0.4029 0.4077 -0.1090 0.143 Uiso 1 1 calc R . . H10B H 0.3049 0.4386 -0.1622 0.143 Uiso 1 1 calc R . . H10C H 0.2945 0.3012 -0.1194 0.143 Uiso 1 1 calc R . . C11 C 0.2724(4) 0.7109(5) -0.21755(17) 0.1135(15) Uani 1 1 d . . . H11A H 0.2764 0.6267 -0.2440 0.170 Uiso 1 1 calc R . . H11B H 0.3464 0.7244 -0.1938 0.170 Uiso 1 1 calc R . . H11C H 0.2530 0.7997 -0.2409 0.170 Uiso 1 1 calc R . . C12 C 0.0729(4) 0.6388(6) -0.20977(18) 0.1146(16) Uani 1 1 d . . . H12A H 0.0462 0.7144 -0.2388 0.172 Uiso 1 1 calc R . . H12B H 0.0171 0.6270 -0.1816 0.172 Uiso 1 1 calc R . . H12C H 0.0818 0.5453 -0.2300 0.172 Uiso 1 1 calc R . . HN1 H 0.168(3) 1.066(3) 0.0185(14) 0.054(11) Uiso 1 1 d . . . HN5 H -0.054(3) 1.340(4) 0.0615(15) 0.078(11) Uiso 1 1 d . . . Li1 Li -0.0271(4) 1.0786(6) 0.0434(2) 0.0559(11) Uani 1 1 d . . . Li2 Li 0.2154(4) 0.8167(5) 0.0013(2) 0.0516(10) Uani 1 1 d . . . N1 N 0.1381(2) 1.0137(3) 0.02918(10) 0.0444(5) Uani 1 1 d . . . N2 N 0.2451(2) 1.0937(3) 0.14675(10) 0.0626(6) Uani 1 1 d . . . N3 N 0.27869(17) 0.8095(2) 0.09724(10) 0.0506(5) Uani 1 1 d . . . N4 N 0.0575(2) 0.8901(3) 0.12724(11) 0.0706(7) Uani 1 1 d . . . N5 N -0.10252(19) 1.2732(3) 0.06214(11) 0.0533(6) Uani 1 1 d . . . N6 N 0.32023(18) 0.8015(2) -0.07654(11) 0.0515(5) Uani 1 1 d . . . N7 N 0.26024(19) 0.4959(2) -0.08263(10) 0.0562(6) Uani 1 1 d . . . N8 N 0.1833(2) 0.6835(3) -0.17805(11) 0.0685(7) Uani 1 1 d . . . Si1 Si 0.17998(6) 0.95930(8) 0.10007(3) 0.0442(2) Uani 1 1 d . . . Si2 Si 0.20853(6) 0.67257(8) -0.10124(3) 0.0449(2) Uani 1 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 C1 0.083(2) 0.060(2) 0.099(3) -0.0232(19) -0.003(2) -0.0015(18) C2 0.130(3) 0.111(3) 0.059(2) -0.022(2) -0.031(2) 0.009(3) C3 0.0433(14) 0.088(3) 0.082(2) 0.0025(18) -0.0034(14) 0.0106(15) C4 0.105(3) 0.057(2) 0.086(2) 0.0263(18) -0.007(2) 0.0086(18) C5 0.098(3) 0.144(4) 0.075(2) 0.021(2) 0.037(2) 0.011(3) C6 0.069(2) 0.092(3) 0.108(3) 0.021(2) 0.0094(19) -0.028(2) C7 0.076(2) 0.0551(19) 0.088(2) 0.0107(17) 0.0135(17) -0.0058(16) C8 0.0475(15) 0.076(2) 0.108(3) 0.002(2) 0.0177(16) 0.0007(16) C9 0.120(3) 0.065(2) 0.083(2) 0.0150(19) -0.013(2) 0.007(2) C10 0.104(3) 0.059(2) 0.129(3) -0.009(2) 0.032(2) 0.031(2) C11 0.140(4) 0.142(4) 0.062(2) 0.012(2) 0.031(2) -0.014(3) C12 0.106(3) 0.155(4) 0.075(2) -0.027(3) -0.022(2) 0.016(3) Li1 0.046(2) 0.066(3) 0.053(2) -0.009(2) -0.0028(19) 0.015(2) Li2 0.045(2) 0.052(3) 0.054(2) -0.007(2) -0.0055(19) 0.0054(19) N1 0.0426(11) 0.0436(13) 0.0457(12) 0.0009(10) 0.0000(9) 0.0035(10) N2 0.0724(15) 0.0601(15) 0.0516(13) -0.0111(12) -0.0082(11) 0.0034(13) N3 0.0453(11) 0.0472(13) 0.0563(13) 0.0066(10) -0.0060(10) 0.0033(10) N4 0.0646(15) 0.0812(19) 0.0701(17) 0.0047(14) 0.0246(13) -0.0085(14) N5 0.0391(11) 0.0552(14) 0.0653(15) -0.0152(12) 0.0044(10) -0.0003(11) N6 0.0444(11) 0.0429(12) 0.0680(14) 0.0022(10) 0.0099(10) 0.0006(9) N7 0.0624(14) 0.0424(12) 0.0635(15) -0.0001(11) 0.0057(11) 0.0095(11) N8 0.0755(16) 0.0778(18) 0.0506(13) -0.0008(12) 0.0007(12) 0.0092(14) Si1 0.0417(4) 0.0465(4) 0.0433(4) -0.0004(3) 0.0012(3) 0.0018(3) Si2 0.0445(4) 0.0417(4) 0.0482(4) -0.0034(3) 0.0044(3) 0.0056(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 C1 N2 1.443(4) . ? C2 N2 1.456(4) . ? C3 N3 1.462(3) . ? C4 N3 1.468(4) . ? C5 N4 1.454(4) . ? C6 N4 1.458(4) . ? C7 N6 1.463(3) . ? C8 N6 1.465(3) . ? C9 N7 1.450(4) . ? C10 N7 1.441(4) . ? C11 N8 1.455(4) . ? C12 N8 1.442(4) . ? Li1 N5 2.007(5) . ? Li1 N1 2.058(5) . ? Li1 N1 2.113(5) 3_575 ? Li1 Li2 2.468(6) 3_575 ? Li1 Li1 2.535(9) 3_575 ? Li1 N4 2.618(5) . ? Li1 Si1 2.784(4) . ? Li2 N5 1.979(5) 3_575 ? Li2 N1 2.098(5) . ? Li2 N3 2.185(5) . ? Li2 N6 2.242(5) . ? Li2 Li1 2.468(6) 3_575 ? Li2 Si1 2.623(4) . ? Li2 Si2 2.622(4) . ? N1 Si1 1.674(2) . ? N1 Li1 2.113(5) 3_575 ? N2 Si1 1.704(2) . ? N3 Si1 1.762(2) . ? N4 Si1 1.721(2) . ? N5 Si2 1.661(2) 3_575 ? N5 Li2 1.979(5) 3_575 ? N6 Si2 1.767(2) . ? N7 Si2 1.717(2) . ? N8 Si2 1.711(3) . ? Si2 N5 1.661(2) 3_575 ? 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 N5 Li1 N1 135.2(3) . . ? N5 Li1 N1 104.9(2) . 3_575 ? N1 Li1 N1 105.2(2) . 3_575 ? N5 Li1 Li2 51.23(15) . 3_575 ? N1 Li1 Li2 146.5(3) . 3_575 ? N1 Li1 Li2 53.83(15) 3_575 3_575 ? N5 Li1 Li1 142.2(3) . 3_575 ? N1 Li1 Li1 53.57(16) . 3_575 ? N1 Li1 Li1 51.59(17) 3_575 3_575 ? Li2 Li1 Li1 100.7(3) 3_575 3_575 ? N5 Li1 N4 122.6(2) . . ? N1 Li1 N4 69.89(15) . . ? N1 Li1 N4 116.2(2) 3_575 . ? Li2 Li1 N4 140.3(2) 3_575 . ? Li1 Li1 N4 95.1(3) 3_575 . ? N5 Li1 Si1 127.3(2) . . ? N1 Li1 Si1 36.73(10) . . ? N1 Li1 Si1 127.8(2) 3_575 . ? Li2 Li1 Si1 176.8(2) 3_575 . ? Li1 Li1 Si1 81.9(2) 3_575 . ? N4 Li1 Si1 37.01(8) . . ? N5 Li2 N1 106.5(2) 3_575 . ? N5 Li2 N3 143.9(3) 3_575 . ? N1 Li2 N3 80.62(17) . . ? N5 Li2 N6 77.89(17) 3_575 . ? N1 Li2 N6 124.8(2) . . ? N3 Li2 N6 127.8(2) . . ? N5 Li2 Li1 52.24(16) 3_575 3_575 ? N1 Li2 Li1 54.40(16) . 3_575 ? N3 Li2 Li1 125.8(2) . 3_575 ? N6 Li2 Li1 103.9(2) . 3_575 ? N5 Li2 Si1 130.1(2) 3_575 . ? N1 Li2 Si1 39.59(10) . . ? N3 Li2 Si1 41.77(10) . . ? N6 Li2 Si1 146.8(2) . . ? Li1 Li2 Si1 86.55(17) 3_575 . ? N5 Li2 Si2 39.29(10) 3_575 . ? N1 Li2 Si2 134.5(2) . . ? N3 Li2 Si2 144.8(2) . . ? N6 Li2 Si2 41.70(9) . . ? Li1 Li2 Si2 84.09(16) 3_575 . ? Si1 Li2 Si2 169.37(18) . . ? Si1 N1 Li1 95.93(17) . . ? Si1 N1 Li2 87.38(16) . . ? Li1 N1 Li2 135.9(2) . . ? Si1 N1 Li1 134.2(2) . 3_575 ? Li1 N1 Li1 74.8(2) . 3_575 ? Li2 N1 Li1 71.77(18) . 3_575 ? C1 N2 C2 113.1(3) . . ? C1 N2 Si1 124.6(2) . . ? C2 N2 Si1 122.2(2) . . ? C3 N3 C4 110.8(2) . . ? C3 N3 Si1 115.9(2) . . ? C4 N3 Si1 123.1(2) . . ? C3 N3 Li2 91.0(2) . . ? C4 N3 Li2 127.6(2) . . ? Si1 N3 Li2 82.56(14) . . ? C5 N4 C6 112.9(3) . . ? C5 N4 Si1 123.4(3) . . ? C6 N4 Si1 121.2(2) . . ? C5 N4 Li1 115.4(3) . . ? C6 N4 Li1 94.7(2) . . ? Si1 N4 Li1 76.73(14) . . ? Si2 N5 Li2 91.73(16) 3_575 3_575 ? Si2 N5 Li1 136.7(2) 3_575 . ? Li2 N5 Li1 76.53(19) 3_575 . ? C7 N6 C8 110.2(2) . . ? C7 N6 Si2 118.55(19) . . ? C8 N6 Si2 121.20(19) . . ? C7 N6 Li2 98.5(2) . . ? C8 N6 Li2 123.0(2) . . ? Si2 N6 Li2 80.73(14) . . ? C10 N7 C9 112.2(3) . . ? C10 N7 Si2 124.0(2) . . ? C9 N7 Si2 122.0(2) . . ? C12 N8 C11 113.4(3) . . ? C12 N8 Si2 120.9(3) . . ? C11 N8 Si2 124.9(2) . . ? N1 Si1 N2 115.74(13) . . ? N1 Si1 N4 106.33(13) . . ? N2 Si1 N4 110.94(13) . . ? N1 Si1 N3 107.49(11) . . ? N2 Si1 N3 108.25(11) . . ? N4 Si1 N3 107.79(12) . . ? N1 Si1 Li2 53.02(12) . . ? N2 Si1 Li2 138.99(14) . . ? N4 Si1 Li2 109.99(14) . . ? N3 Si1 Li2 55.67(12) . . ? N1 Si1 Li1 47.34(12) . . ? N2 Si1 Li1 107.71(13) . . ? N4 Si1 Li1 66.27(14) . . ? N3 Si1 Li1 143.01(12) . . ? Li2 Si1 Li1 90.79(13) . . ? N5 Si2 N8 117.69(12) 3_575 . ? N5 Si2 N7 113.36(13) 3_575 . ? N8 Si2 N7 107.96(13) . . ? N5 Si2 N6 101.79(11) 3_575 . ? N8 Si2 N6 107.91(13) . . ? N7 Si2 N6 107.41(11) . . ? N5 Si2 Li2 48.98(12) 3_575 . ? N8 Si2 Li2 146.59(14) . . ? N7 Si2 Li2 105.25(13) . . ? N6 Si2 Li2 57.57(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.43 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.233 _refine_diff_density_min -0.226 _refine_diff_density_rms 0.048 #===END data_3160 _database_code_CSD 194607 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_compound_source 'see paper' _chemical_formula_sum 'C32 H92 Al1 Li1 N16 O2 Si4' _chemical_formula_weight 879.50 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' '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' 'Al' 'Al' 0.0645 0.0514 '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' 'O' 'O' 0.0106 0.0060 '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' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 12.2318(4) _cell_length_b 21.7844(9) _cell_length_c 20.2211(6) _cell_angle_alpha 90.00 _cell_angle_beta 105.3130(10) _cell_angle_gamma 90.00 _cell_volume 5196.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173 _cell_measurement_reflns_used 7460 _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.124 _exptl_crystal_density_method none _exptl_crystal_F_000 1936 _exptl_absorpt_coefficient_mu 0.175 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'SADABS, Sheldrick, G.W. (1995)' _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 1.00 _publ_section_exptl_prep ; The crystal was mounted at low T on a glass fibre in protective oil ; _diffrn_ambient_temperature 173 _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART-CCD' _diffrn_measurement_method '\w-scan' _diffrn_standards_number 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0.00 _diffrn_reflns_number 27683 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.87 _diffrn_reflns_theta_max 33.79 _reflns_number_total 9089 _reflns_number_gt 7103 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART (Siemens, 1995)' _computing_cell_refinement 'SAINT (Siemens, 1995)' _computing_data_reduction 'XPREP (Siemens, 1995)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP (Siemens, 1995)' _publ_section_exptl_refinement ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0656P)^2^+2.0013P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef 0 _refine_ls_number_reflns 9089 _refine_ls_number_parameters 272 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1175 _refine_ls_wR_factor_gt 0.1083 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 1.0000 0.00881(13) 0.2500 0.0239(6) Uani 1 2 d S . . Al1 Al 1.0000 0.13387(2) 0.2500 0.01381(9) Uani 1 2 d S . . Si1 Si 1.23159(2) 0.079291(14 0.355747(15 0.01666(7) Uani 1 1 d . . . Si2 Si 0.88155(2) 0.208642(14 0.358921(15 0.01611(7) Uani 1 1 d . . . N1 N 1.08904(7) 0.07968(4) 0.31572(5) 0.01612(16) Uani 1 1 d . . . N2 N 0.89949(7) 0.17673(4) 0.28612(5) 0.01796(17) Uani 1 1 d . . . N3 N 1.28584(7) 0.15298(5) 0.36574(5) 0.02018(18) Uani 1 1 d . . . C31 C 1.23199(11) 0.20179(6) 0.39455(8) 0.0325(3) Uani 1 1 d . . . H31A H 1.2689 0.2060 0.4425 0.049 Uiso 1 1 calc R . . H31B H 1.1535 0.1920 0.3887 0.049 Uiso 1 1 calc R . . H31C H 1.2380 0.2397 0.3715 0.049 Uiso 1 1 calc R . . C32 C 1.40547(9) 0.16531(6) 0.37393(7) 0.0257(2) Uani 1 1 d . . . H32A H 1.4140 0.2045 0.3542 0.039 Uiso 1 1 calc R . . H32B H 1.4370 0.1339 0.3511 0.039 Uiso 1 1 calc R . . H32C H 1.4445 0.1656 0.4218 0.039 Uiso 1 1 calc R . . N4 N 1.30801(8) 0.03841(5) 0.30987(5) 0.02325(19) Uani 1 1 d . . . C41 C 1.41195(11) 0.00556(7) 0.34263(8) 0.0356(3) Uani 1 1 d . . . H41A H 1.4151 -0.0319 0.3183 0.053 Uiso 1 1 calc R . . H41B H 1.4131 -0.0037 0.3892 0.053 Uiso 1 1 calc R . . H41C H 1.4762 0.0306 0.3420 0.053 Uiso 1 1 calc R . . C42 C 1.30271(12) 0.05394(7) 0.23916(7) 0.0304(3) Uani 1 1 d . . . H42A H 1.3667 0.0790 0.2379 0.046 Uiso 1 1 calc R . . H42B H 1.2340 0.0761 0.2194 0.046 Uiso 1 1 calc R . . H42C H 1.3039 0.0170 0.2135 0.046 Uiso 1 1 calc R . . N5 N 1.25232(8) 0.04557(5) 0.43533(5) 0.0244(2) Uani 1 1 d . . . C51 C 1.20899(13 -0.01469(7) 0.44446(7) 0.0361(3) Uani 1 1 d . . . H51A H 1.2708 -0.0432 0.4574 0.054 Uiso 1 1 calc R . . H51B H 1.1575 -0.0278 0.4023 0.054 Uiso 1 1 calc R . . H51C H 1.1699 -0.0131 0.4798 0.054 Uiso 1 1 calc R . . C52 C 1.33387(14) 0.06689(9) 0.49664(7) 0.0442(4) Uani 1 1 d . . . H52A H 1.2995 0.0672 0.5342 0.066 Uiso 1 1 calc R . . H52B H 1.3579 0.1077 0.4892 0.066 Uiso 1 1 calc R . . H52C H 1.3982 0.0399 0.5072 0.066 Uiso 1 1 calc R . . N6 N 0.91145(8) 0.28633(4) 0.36289(5) 0.02054(18) Uani 1 1 d . . . C61 C 1.00721(11) 0.31229(6) 0.34283(7) 0.0283(2) Uani 1 1 d . . . H61A H 0.9844 0.3497 0.3179 0.042 Uiso 1 1 calc R . . H61B H 1.0331 0.2836 0.3143 0.042 Uiso 1 1 calc R . . H61C H 1.0674 0.3208 0.3830 0.042 Uiso 1 1 calc R . . C62 C 0.86572(11) 0.32846(6) 0.40457(7) 0.0292(3) Uani 1 1 d . . . H62A H 0.9224 0.3369 0.4465 0.044 Uiso 1 1 calc R . . H62B H 0.8007 0.3103 0.4149 0.044 Uiso 1 1 calc R . . H62C H 0.8439 0.3661 0.3798 0.044 Uiso 1 1 calc R . . N7 N 0.96637(8) 0.17290(4) 0.43040(5) 0.01986(18) Uani 1 1 d . . . C71 C 0.95411(12) 0.10854(6) 0.44433(7) 0.0292(3) Uani 1 1 d . . . H71A H 1.0275 0.0896 0.4575 0.044 Uiso 1 1 calc R . . H71B H 0.9087 0.0889 0.4039 0.044 Uiso 1 1 calc R . . H71C H 0.9179 0.1044 0.4808 0.044 Uiso 1 1 calc R . . C72 C 1.03056(11) 0.20544(6) 0.49055(6) 0.0292(3) Uani 1 1 d . . . H72A H 0.9915 0.2031 0.5259 0.044 Uiso 1 1 calc R . . H72B H 1.0385 0.2477 0.4791 0.044 Uiso 1 1 calc R . . H72C H 1.1042 0.1871 0.5066 0.044 Uiso 1 1 calc R . . N8 N 0.74344(8) 0.20104(5) 0.36396(5) 0.0246(2) Uani 1 1 d . . . C81 C 0.71009(11) 0.18734(8) 0.42565(7) 0.0371(3) Uani 1 1 d . . . H81A H 0.6671 0.2210 0.4363 0.056 Uiso 1 1 calc R . . H81B H 0.7765 0.1811 0.4629 0.056 Uiso 1 1 calc R . . H81C H 0.6645 0.1508 0.4188 0.056 Uiso 1 1 calc R . . C82 C 0.64856(10) 0.21873(8) 0.30781(7) 0.0348(3) Uani 1 1 d . . . H82A H 0.5932 0.1864 0.2988 0.052 Uiso 1 1 calc R . . H82B H 0.6744 0.2260 0.2676 0.052 Uiso 1 1 calc R . . H82C H 0.6150 0.2555 0.3197 0.052 Uiso 1 1 calc R . . O1' O 0.91707(8) -0.05328(4) 0.29147(5) 0.0298(2) Uani 1 1 d . B . C2' C 0.84647(14 -0.09513(7) 0.24212(7) 0.0368(3) Uani 1 1 d . . . H2'1 H 0.8887 -0.1128 0.2124 0.044 Uiso 1 1 calc R A 1 H2'2 H 0.7803 -0.0742 0.2142 0.044 Uiso 1 1 calc R A 1 C3' C 0.8120(2) -0.14471(10) 0.28639(12) 0.0373(4) Uiso 0.70 1 d P B 1 H3'1 H 0.7410 -0.1640 0.2627 0.045 Uiso 0.70 1 calc PR B 1 H3'2 H 0.8701 -0.1759 0.3000 0.045 Uiso 0.70 1 calc PR B 1 C4' C 0.7999(2) -0.10740(11) 0.34759(12) 0.0379(5) Uiso 0.70 1 d P B 1 H4'1 H 0.7291 -0.0847 0.3371 0.046 Uiso 0.70 1 calc PR B 1 H4'2 H 0.8048 -0.1332 0.3874 0.046 Uiso 0.70 1 calc PR B 1 C3" C 0.7609(4) -0.1232(2) 0.2784(2) 0.0304(9) Uiso 0.30 1 d P B 2 H3"1 H 0.6983 -0.0957 0.2777 0.037 Uiso 0.30 1 calc PR B 2 H3"2 H 0.7319 -0.1626 0.2590 0.037 Uiso 0.30 1 calc PR B 2 C4" C 0.8381(5) -0.1293(2) 0.3473(3) 0.0338(9) Uiso 0.30 1 d P B 2 H4"1 H 0.8914 -0.1627 0.3491 0.041 Uiso 0.30 1 calc PR B 2 H4"2 H 0.7966 -0.1363 0.3814 0.041 Uiso 0.30 1 calc PR B 2 C5' C 0.90043(15 -0.06509(8) 0.35811(7) 0.0402(3) Uani 1 1 d . . . H5'1 H 0.8860 -0.0271 0.3793 0.048 Uiso 1 1 calc R C 1 H5'2 H 0.9673 -0.0842 0.3876 0.048 Uiso 1 1 calc R C 1 H1 H 1.0568(14) 0.0763(7) 0.3481(9) 0.030(4) Uiso 1 1 d . . . H2 H 0.8425(17) 0.1835(9) 0.2535(10) 0.047(5) Uiso 1 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 Li1 0.0250(13) 0.0215(13) 0.0224(14) 0.000 0.0012(11) 0.000 Al1 0.01162(17) 0.0177(2) 0.0122(2) 0.000 0.00337(14) 0.000 Si1 0.01279(12) 0.02199(14) 0.01414(14) 0.00162(10) 0.0017(1) -0.00008(10) Si2 0.01260(12) 0.02241(14) 0.01378(14 -0.00215(10) 0.00428(9) -0.0002(10) N1 0.0128(3) 0.0223(4) 0.0125(4) 0.0018(3) 0.0020(3) -0.0011(3) N2 0.0140(4) 0.0245(4) 0.0152(4) -0.0027(3) 0.0035(3) 0.0017(3) N3 0.0128(3) 0.0257(4) 0.0217(5) -0.0022(3) 0.0038(3) -0.0030(3) C31 0.0205(5) 0.0314(6) 0.0468(8) -0.0155(6) 0.0110(5) -0.0057(5) C32 0.0147(4) 0.0350(6) 0.0271(6) -0.0030(5) 0.0051(4) -0.0056(4) N4 0.0189(4) 0.0271(5) 0.0239(5) 0.0022(4) 0.0059(3) 0.0060(4) C41 0.0261(6) 0.0383(7) 0.0428(8) 0.0069(6) 0.0100(5) 0.0137(6) C42 0.0327(6) 0.0355(7) 0.0262(6) -0.0011(5) 0.0135(5) 0.0074(5) N5 0.0198(4) 0.0334(5) 0.0170(5) 0.0066(4) -0.0006(3) -0.0030(4) C51 0.0437(7) 0.0351(7) 0.0272(7) 0.0119(5) 0.0051(5) -0.0038(6) C52 0.0407(8) 0.0643(11) 0.0187(7) 0.0081(6) -0.0076(5) -0.0137(7) N6 0.0212(4) 0.0220(4) 0.0188(4) -0.0035(3) 0.0061(3) 0.0020(4) C61 0.0303(6) 0.0244(5) 0.0322(7) -0.0017(5) 0.0117(5) -0.0042(5) C62 0.0332(6) 0.0293(6) 0.0250(6) -0.0077(5) 0.0073(5) 0.0056(5) N7 0.0197(4) 0.0238(4) 0.0158(4) 0.0005(3) 0.0042(3) -0.0014(3) C71 0.0391(7) 0.0287(6) 0.0216(6) 0.0046(4) 0.0110(5) -0.0017(5) C72 0.0275(6) 0.0372(7) 0.0186(6) -0.0005(5) -0.0015(4) -0.0015(5) N8 0.0139(4) 0.0416(6) 0.0192(5) -0.0030(4) 0.0059(3) -0.0012(4) C81 0.0217(5) 0.0674(10) 0.0261(7) -0.0032(6) 0.0133(5) -0.0027(6) C82 0.0165(5) 0.0579(9) 0.0297(7) 0.0012(6) 0.0057(4) 0.0042(5) O1' 0.0357(5) 0.0273(4) 0.0231(4) 0.0003(3) 0.0018(4) -0.0105(4) C2' 0.0450(8) 0.0336(7) 0.0273(7) -0.0031(5) 0.0018(6) -0.0168(6) C5' 0.0483(8) 0.0454(8) 0.0222(7) 0.0031(6) 0.0009(6) -0.0163(7) _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 Li1 O1' 2.003(2) 2_755 ? Li1 O1' 2.003(2) . ? Li1 N1 2.138(2) . ? Li1 N1 2.138(2) 2_755 ? Li1 Al1 2.724(3) . ? Al1 N2 1.8414(9) . ? Al1 N2 1.8414(9) 2_755 ? Al1 N1 1.8924(9) 2_755 ? Al1 N1 1.8925(9) . ? Si1 N1 1.7176(9) . ? Si1 N5 1.7257(10) . ? Si1 N4 1.7278(10) . ? Si1 N3 1.7284(10) . ? Si2 N2 1.6939(9) . ? Si2 N7 1.7262(10) . ? Si2 N8 1.7270(9) . ? Si2 N6 1.7289(10) . ? N1 H1 0.851(18) . ? N2 H2 0.84(2) . ? N3 C31 1.4514(16) . ? N3 C32 1.4536(14) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? N4 C42 1.4541(17) . ? N4 C41 1.4569(16) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N5 C51 1.4458(17) . ? N5 C52 1.4472(17) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? N6 C61 1.4516(16) . ? N6 C62 1.4540(15) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C61 H61C 0.9600 . ? C62 H62A 0.9600 . ? C62 H62B 0.9600 . ? C62 H62C 0.9600 . ? N7 C71 1.4456(16) . ? N7 C72 1.4471(15) . ? C71 H71A 0.9600 . ? C71 H71B 0.9600 . ? C71 H71C 0.9600 . ? C72 H72A 0.9600 . ? C72 H72B 0.9600 . ? C72 H72C 0.9600 . ? N8 C81 1.4425(16) . ? N8 C82 1.4451(16) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? O1' C5' 1.4382(18) . ? O1' C2' 1.4552(16) . ? C2' C3' 1.531(3) . ? C2' C3" 1.554(5) . ? C2' H2'1 0.9700 . ? C2' H2'2 0.9700 . ? C3' C4' 1.520(3) . ? C3' H3'1 0.9700 . ? C3' H3'2 0.9700 . ? C4' C5' 1.506(3) . ? C4' H4'1 0.9700 . ? C4' H4'2 0.9700 . ? C3" C4" 1.468(7) . ? C3" H3"1 0.9700 . ? C3" H3"2 0.9700 . ? C4" C5' 1.581(5) . ? C4" H4"1 0.9700 . ? C4" H4"2 0.9700 . ? C5' H5'1 0.9700 . ? C5' H5'2 0.9700 . ? 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 O1' Li1 O1' 95.03(13) 2_755 . ? O1' Li1 N1 121.11(4) 2_755 . ? O1' Li1 N1 117.30(4) . . ? O1' Li1 N1 117.30(4) 2_755 2_755 ? O1' Li1 N1 121.12(4) . 2_755 ? N1 Li1 N1 87.54(12) . 2_755 ? O1' Li1 Al1 132.48(7) 2_755 . ? O1' Li1 Al1 132.49(7) . . ? N1 Li1 Al1 43.77(6) . . ? N1 Li1 Al1 43.77(6) 2_755 . ? N2 Al1 N2 119.07(6) . 2_755 ? N2 Al1 N1 105.91(4) . 2_755 ? N2 Al1 N1 111.00(4) 2_755 2_755 ? N2 Al1 N1 111.00(4) . . ? N2 Al1 N1 105.91(4) 2_755 . ? N1 Al1 N1 102.82(6) 2_755 . ? N2 Al1 Li1 120.46(3) . . ? N2 Al1 Li1 120.47(3) 2_755 . ? N1 Al1 Li1 51.41(3) 2_755 . ? N1 Al1 Li1 51.41(3) . . ? N1 Si1 N5 108.81(5) . . ? N1 Si1 N4 112.05(5) . . ? N5 Si1 N4 108.31(5) . . ? N1 Si1 N3 111.16(5) . . ? N5 Si1 N3 109.21(5) . . ? N4 Si1 N3 107.22(5) . . ? N2 Si2 N7 110.82(5) . . ? N2 Si2 N8 111.42(5) . . ? N7 Si2 N8 106.76(5) . . ? N2 Si2 N6 111.58(5) . . ? N7 Si2 N6 109.25(5) . . ? N8 Si2 N6 106.82(5) . . ? Si1 N1 Al1 131.18(5) . . ? Si1 N1 Li1 125.20(6) . . ? Al1 N1 Li1 84.82(6) . . ? Si1 N1 H1 104.8(12) . . ? Al1 N1 H1 107.2(11) . . ? Li1 N1 H1 98.8(11) . . ? Si2 N2 Al1 143.72(6) . . ? Si2 N2 H2 110.0(13) . . ? Al1 N2 H2 106.3(13) . . ? C31 N3 C32 111.64(9) . . ? C31 N3 Si1 121.76(8) . . ? C32 N3 Si1 121.93(8) . . ? N3 C31 H31A 109.5 . . ? N3 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N3 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N3 C32 H32A 109.5 . . ? N3 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? N3 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C42 N4 C41 111.61(10) . . ? C42 N4 Si1 121.20(8) . . ? C41 N4 Si1 122.68(9) . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C51 N5 C52 112.02(11) . . ? C51 N5 Si1 122.48(9) . . ? C52 N5 Si1 124.10(9) . . ? N5 C51 H51A 109.5 . . ? N5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N5 C52 H52A 109.5 . . ? N5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C61 N6 C62 112.24(10) . . ? C61 N6 Si2 123.01(8) . . ? C62 N6 Si2 122.39(8) . . ? N6 C61 H61A 109.5 . . ? N6 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? N6 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? N6 C62 H62A 109.5 . . ? N6 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? N6 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C71 N7 C72 111.87(10) . . ? C71 N7 Si2 122.03(8) . . ? C72 N7 Si2 123.74(8) . . ? N7 C71 H71A 109.5 . . ? N7 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? N7 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? N7 C72 H72A 109.5 . . ? N7 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? N7 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C81 N8 C82 112.51(10) . . ? C81 N8 Si2 125.12(9) . . ? C82 N8 Si2 121.55(9) . . ? N8 C81 H81A 109.5 . . ? N8 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? N8 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? N8 C82 H82A 109.5 . . ? N8 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? N8 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C5' O1' C2' 108.99(10) . . ? C5' O1' Li1 136.53(9) . . ? C2' O1' Li1 114.23(9) . . ? O1' C2' C3' 104.24(13) . . ? O1' C2' C3" 105.9(2) . . ? C3' C2' C3" 28.65(17) . . ? O1' C2' H2'1 110.9 . . ? C3' C2' H2'1 110.9 . . ? C3" C2' H2'1 132.3 . . ? O1' C2' H2'2 110.9 . . ? C3' C2' H2'2 110.9 . . ? C3" C2' H2'2 84.2 . . ? H2'1 C2' H2'2 108.9 . . ? C4' C3' C2' 101.53(17) . . ? C4' C3' H3'1 111.5 . . ? C2' C3' H3'1 111.5 . . ? C4' C3' H3'2 111.5 . . ? C2' C3' H3'2 111.5 . . ? H3'1 C3' H3'2 109.3 . . ? C5' C4' C3' 101.01(17) . . ? C5' C4' H4'1 111.6 . . ? C3' C4' H4'1 111.6 . . ? C5' C4' H4'2 111.6 . . ? C3' C4' H4'2 111.6 . . ? H4'1 C4' H4'2 109.4 . . ? C4" C3" C2' 98.0(3) . . ? C4" C3" H3"1 112.2 . . ? C2' C3" H3"1 112.2 . . ? C4" C3" H3"2 112.2 . . ? C2' C3" H3"2 112.2 . . ? H3"1 C3" H3"2 109.8 . . ? C3" C4" C5' 102.5(4) . . ? C3" C4" H4"1 111.3 . . ? C5' C4" H4"1 111.3 . . ? C3" C4" H4"2 111.3 . . ? C5' C4" H4"2 111.3 . . ? H4"1 C4" H4"2 109.2 . . ? O1' C5' C4' 106.81(13) . . ? O1' C5' C4" 102.2(2) . . ? C4' C5' C4" 24.89(18) . . ? O1' C5' H5'1 110.4 . . ? C4' C5' H5'1 110.4 . . ? C4" C5' H5'1 132.8 . . ? O1' C5' H5'2 110.4 . . ? C4' C5' H5'2 110.4 . . ? C4" C5' H5'2 90.1 . . ? H5'1 C5' H5'2 108.6 . . ? _diffrn_measured_fraction_theta_max 0.871 _diffrn_reflns_theta_full 33.79 _diffrn_measured_fraction_theta_full 0.871 _refine_diff_density_max 0.648 _refine_diff_density_min -0.427 _refine_diff_density_rms 0.056 #===END data_jsb23_01 _database_code_CSD 172029 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C22 H65 Al N12 O Si3' _chemical_formula_weight 625.11 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' '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 P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 9.7875(16) _cell_length_b 17.413(2) _cell_length_c 21.810(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.536(14) _cell_angle_gamma 90.00 _cell_volume 3433.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour white _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.209 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_absorpt_coefficient_mu 0.200 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Stoe IPDSII image plate' _diffrn_measurement_method '170 frames at 1^o intervals, exposure time 1 minute' _diffrn_reflns_number 29973 _diffrn_reflns_av_R_equivalents 0.2043 _diffrn_reflns_av_sigmaI/netI 0.2475 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 30.28 _reflns_number_total 10569 _reflns_number_gt 3202 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-AREA' _computing_cell_refinement 'X-AREA' _computing_data_reduction 'X-RED' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP II (Johnson, 1976)' _computing_publication_material 'SHELXL 97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0821P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10569 _refine_ls_number_parameters 352 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2143 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.2146 _refine_ls_wR_factor_gt 0.1620 _refine_ls_goodness_of_fit_ref 0.775 _refine_ls_restrained_S_all 0.775 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 1.0518(6) 0.2095(4) -0.0681(3) 0.0580(14) Uani 1 1 d . . . H1A H 1.0517 0.2657 -0.0660 0.087 Uiso 1 1 calc R . . H1B H 0.9884 0.1927 -0.1129 0.087 Uiso 1 1 calc R . . H1C H 1.1530 0.1911 -0.0576 0.087 Uiso 1 1 calc R . . C2 C 0.9953(5) 0.0965(3) -0.0228(3) 0.0527(12) Uani 1 1 d . . . H2A H 0.9574 0.0781 0.0101 0.079 Uiso 1 1 calc R . . H2B H 1.0957 0.0768 -0.0119 0.079 Uiso 1 1 calc R . . H2C H 0.9309 0.0783 -0.0670 0.079 Uiso 1 1 calc R . . C3 C 0.6589(6) 0.2354(5) -0.1111(2) 0.074(2) Uani 1 1 d . . . H3A H 0.7382 0.2634 -0.1184 0.111 Uiso 1 1 calc R . . H3B H 0.5686 0.2666 -0.1267 0.111 Uiso 1 1 calc R . . H3C H 0.6401 0.1869 -0.1357 0.111 Uiso 1 1 calc R . . C4 C 0.5848(5) 0.1798(3) -0.0340(3) 0.0483(12) Uani 1 1 d . . . H4A H 0.6165 0.1696 0.0136 0.072 Uiso 1 1 calc R . . H4B H 0.5656 0.1310 -0.0583 0.072 Uiso 1 1 calc R . . H4C H 0.4942 0.2107 -0.0491 0.072 Uiso 1 1 calc R . . C5 C 0.8297(5) 0.3881(3) -0.0248(3) 0.0524(13) Uani 1 1 d . . . H5A H 0.7277 0.3693 -0.0450 0.079 Uiso 1 1 calc R . . H5B H 0.8572 0.4125 -0.0589 0.079 Uiso 1 1 calc R . . H5C H 0.8373 0.4257 0.0098 0.079 Uiso 1 1 calc R . . C6 C 1.0809(5) 0.3496(3) 0.0349(3) 0.0544(13) Uani 1 1 d . . . H6A H 1.1448 0.3054 0.0543 0.082 Uiso 1 1 calc R . . H6B H 1.0903 0.3870 0.0699 0.082 Uiso 1 1 calc R . . H6C H 1.1107 0.3737 0.0013 0.082 Uiso 1 1 calc R . . C7 C 0.4891(5) 0.3535(3) 0.0196(3) 0.0489(12) Uani 1 1 d . . . H7A H 0.5670 0.3152 0.0267 0.073 Uiso 1 1 calc R . . H7B H 0.4601 0.3754 -0.0250 0.073 Uiso 1 1 calc R . . H7C H 0.4031 0.3291 0.0240 0.073 Uiso 1 1 calc R . . C8 C 0.4305(5) 0.4714(3) 0.0591(3) 0.0577(14) Uani 1 1 d . . . H8A H 0.4720 0.5112 0.0930 0.087 Uiso 1 1 calc R . . H8B H 0.3441 0.4482 0.0641 0.087 Uiso 1 1 calc R . . H8C H 0.4005 0.4945 0.0149 0.087 Uiso 1 1 calc R . . C9 C 0.4859(6) 0.3363(3) 0.1771(3) 0.0623(16) Uani 1 1 d . . . H9A H 0.4273 0.3360 0.1292 0.093 Uiso 1 1 calc R . . H9B H 0.4367 0.3684 0.1994 0.093 Uiso 1 1 calc R . . H9C H 0.4953 0.2838 0.1943 0.093 Uiso 1 1 calc R . . C10 C 0.7234(7) 0.3701(3) 0.2557(3) 0.0663(16) Uani 1 1 d . . . H10A H 0.8193 0.3919 0.2607 0.099 Uiso 1 1 calc R . . H10B H 0.7377 0.3180 0.2741 0.099 Uiso 1 1 calc R . . H10C H 0.6775 0.4022 0.2794 0.099 Uiso 1 1 calc R . . C11 C 0.7063(6) 0.5433(3) 0.1931(3) 0.0561(13) Uani 1 1 d . . . H11A H 0.6416 0.5157 0.2106 0.084 Uiso 1 1 calc R . . H11B H 0.6486 0.5820 0.1610 0.084 Uiso 1 1 calc R . . H11C H 0.7859 0.5685 0.2297 0.084 Uiso 1 1 calc R . . C12 C 0.8635(6) 0.5300(3) 0.1360(3) 0.0547(13) Uani 1 1 d . . . H12A H 0.9051 0.4930 0.1140 0.082 Uiso 1 1 calc R . . H12B H 0.9439 0.5547 0.1727 0.082 Uiso 1 1 calc R . . H12C H 0.8071 0.5691 0.1040 0.082 Uiso 1 1 calc R . . C13 C 0.6823(6) 0.0053(3) 0.0722(3) 0.0527(12) Uani 1 1 d . . . H13A H 0.5785 0.0215 0.0549 0.079 Uiso 1 1 calc R . . H13B H 0.6878 -0.0508 0.0749 0.079 Uiso 1 1 calc R . . H13C H 0.7293 0.0235 0.0424 0.079 Uiso 1 1 calc R . . C14 C 0.9091(5) 0.0137(3) 0.1617(3) 0.0560(13) Uani 1 1 d . . . H14A H 0.9568 0.0363 0.2060 0.084 Uiso 1 1 calc R . . H14B H 0.9582 0.0323 0.1329 0.084 Uiso 1 1 calc R . . H14C H 0.9170 -0.0424 0.1650 0.084 Uiso 1 1 calc R . . C15 C 0.3982(5) 0.1450(3) 0.0800(3) 0.0566(14) Uani 1 1 d . . . H15A H 0.4592 0.1875 0.0754 0.085 Uiso 1 1 calc R . . H15B H 0.3160 0.1655 0.0902 0.085 Uiso 1 1 calc R . . H15C H 0.3589 0.1160 0.0383 0.085 Uiso 1 1 calc R . . C16 C 0.3985(6) 0.0330(4) 0.1394(4) 0.077(2) Uani 1 1 d . . . H16A H 0.4614 0.0000 0.1756 0.116 Uiso 1 1 calc R . . H16B H 0.3596 0.0032 0.0982 0.116 Uiso 1 1 calc R . . H16C H 0.3161 0.0525 0.1499 0.116 Uiso 1 1 calc R . . C17 C 0.7334(7) -0.0112(3) 0.2590(3) 0.0684(16) Uani 1 1 d . . . H17A H 0.7423 -0.0420 0.2231 0.103 Uiso 1 1 calc R . . H17B H 0.6426 -0.0255 0.2652 0.103 Uiso 1 1 calc R . . H17C H 0.8190 -0.0207 0.3002 0.103 Uiso 1 1 calc R . . C18 C 0.7146(6) 0.1194(4) 0.2895(3) 0.0619(15) Uani 1 1 d . . . H18A H 0.7107 0.1724 0.2739 0.093 Uiso 1 1 calc R . . H18B H 0.8001 0.1133 0.3314 0.093 Uiso 1 1 calc R . . H18C H 0.6237 0.1077 0.2965 0.093 Uiso 1 1 calc R . . C19 C 1.1710(4) 0.2661(3) 0.2011(2) 0.0509(13) Uani 1 1 d . . . H19A H 1.1981 0.2397 0.1672 0.061 Uiso 1 1 calc R . . H19B H 1.1546 0.3212 0.1894 0.061 Uiso 1 1 calc R . . C20 C 1.2853(5) 0.2571(4) 0.2652(2) 0.0537(14) Uani 1 1 d . . . H20A H 1.3612 0.2979 0.2751 0.064 Uiso 1 1 calc R . . H20B H 1.3332 0.2061 0.2708 0.064 Uiso 1 1 calc R . . C21 C 1.1954(5) 0.2651(4) 0.3053(3) 0.0597(14) Uani 1 1 d . . . H21A H 1.1899 0.3198 0.3166 0.072 Uiso 1 1 calc R . . H21B H 1.2408 0.2358 0.3472 0.072 Uiso 1 1 calc R . . C22 C 1.0458(5) 0.2355(4) 0.2670(2) 0.0544(14) Uani 1 1 d . . . H22A H 1.0321 0.1841 0.2831 0.065 Uiso 1 1 calc R . . H22B H 0.9695 0.2706 0.2705 0.065 Uiso 1 1 calc R . . Al1 Al 0.85191(12) 0.24022(7) 0.13459(6) 0.0316(3) Uani 1 1 d . . . N1 N 0.9002(4) 0.1978(2) 0.07440(17) 0.0369(8) Uani 1 1 d . . . H1 H 0.9412 0.1521 0.0844 0.044 Uiso 1 1 calc R . . N2 N 0.8180(4) 0.3428(2) 0.12340(18) 0.0355(8) Uani 1 1 d . . . H2 H 0.8797 0.3667 0.1093 0.043 Uiso 1 1 calc R . . N3 N 0.7284(4) 0.1914(2) 0.16311(18) 0.0341(8) Uani 1 1 d . . . H3 H 0.6830 0.2237 0.1800 0.041 Uiso 1 1 calc R . . N4 N 0.9981(4) 0.1794(2) -0.02238(19) 0.0402(9) Uani 1 1 d . . . N5 N 0.6994(4) 0.2210(3) -0.04622(18) 0.0454(10) Uani 1 1 d . . . N6 N 0.9284(4) 0.3243(2) 0.00428(19) 0.0401(9) Uani 1 1 d . . . N7 N 0.5421(4) 0.4122(2) 0.0670(2) 0.0446(9) Uani 1 1 d . . . N8 N 0.6331(4) 0.3674(2) 0.1896(2) 0.0456(9) Uani 1 1 d . . . N9 N 0.7677(4) 0.4908(2) 0.1614(2) 0.0424(9) Uani 1 1 d . . . N10 N 0.7538(4) 0.0357(2) 0.13366(19) 0.0415(9) Uani 1 1 d . . . N11 N 0.7279(4) 0.0692(2) 0.2421(2) 0.0472(10) Uani 1 1 d . . . N12 N 0.4844(4) 0.0965(2) 0.13130(19) 0.0428(9) Uani 1 1 d . . . O1 O 1.0376(3) 0.23184(19) 0.20440(14) 0.0372(7) Uani 1 1 d . . . Si1 Si 0.88117(12) 0.22957(7) 0.00355(6) 0.0335(3) Uani 1 1 d . . . Si2 Si 0.69256(13) 0.40192(7) 0.13448(6) 0.0363(3) Uani 1 1 d . . . Si3 Si 0.67361(12) 0.10015(7) 0.16694(6) 0.0352(3) Uani 1 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 C1 0.071(3) 0.073(4) 0.041(3) 0.004(3) 0.034(3) 0.010(3) C2 0.051(3) 0.047(3) 0.065(4) -0.009(3) 0.028(3) 0.000(2) C3 0.052(3) 0.132(6) 0.029(3) 0.007(3) 0.005(2) -0.012(3) C4 0.043(2) 0.055(3) 0.048(3) -0.010(2) 0.019(2) -0.014(2) C5 0.061(3) 0.046(3) 0.046(3) 0.010(2) 0.016(2) 0.010(2) C6 0.046(3) 0.055(3) 0.055(3) 0.001(3) 0.012(2) -0.009(2) C7 0.051(3) 0.042(3) 0.048(3) -0.006(2) 0.013(2) -0.001(2) C8 0.047(3) 0.037(3) 0.087(4) 0.002(3) 0.023(3) 0.007(2) C9 0.068(3) 0.051(3) 0.092(5) 0.014(3) 0.057(4) 0.008(3) C10 0.112(5) 0.051(3) 0.048(3) 0.000(3) 0.043(3) 0.014(3) C11 0.074(3) 0.037(3) 0.056(3) -0.007(2) 0.024(3) 0.005(2) C12 0.066(3) 0.043(3) 0.056(3) -0.004(3) 0.025(3) -0.014(2) C13 0.066(3) 0.050(3) 0.037(3) -0.010(2) 0.014(2) -0.001(2) C14 0.055(3) 0.051(3) 0.058(3) -0.009(3) 0.018(3) 0.009(2) C15 0.045(3) 0.067(4) 0.054(3) 0.001(3) 0.015(2) 0.002(2) C16 0.054(3) 0.067(4) 0.105(5) 0.022(4) 0.025(3) -0.019(3) C17 0.097(4) 0.050(3) 0.053(4) 0.012(3) 0.022(3) -0.012(3) C18 0.082(4) 0.065(4) 0.040(3) -0.002(3) 0.025(3) -0.004(3) C19 0.035(2) 0.075(4) 0.040(3) 0.010(3) 0.0104(18) -0.012(2) C20 0.044(2) 0.078(4) 0.034(2) 0.008(3) 0.009(2) -0.011(2) C21 0.058(3) 0.077(4) 0.038(3) -0.006(3) 0.012(2) -0.020(3) C22 0.046(2) 0.090(4) 0.026(2) 0.000(3) 0.0133(19) -0.004(3) Al1 0.0330(6) 0.0323(6) 0.0272(6) -0.0004(5) 0.0090(5) 0.0001(5) N1 0.046(2) 0.035(2) 0.0280(18) 0.0039(15) 0.0130(16) 0.0109(15) N2 0.0396(18) 0.0323(18) 0.037(2) 0.0018(16) 0.0170(15) -0.0035(14) N3 0.0375(17) 0.0334(19) 0.0338(19) 0.0023(15) 0.0163(15) 0.0018(14) N4 0.0448(19) 0.046(2) 0.035(2) -0.0017(18) 0.0212(17) 0.0024(16) N5 0.0379(19) 0.063(3) 0.0304(19) 0.001(2) 0.0079(15) -0.0116(18) N6 0.0413(19) 0.035(2) 0.041(2) 0.0069(17) 0.0126(16) 0.0037(15) N7 0.0389(18) 0.044(2) 0.045(2) 0.0000(19) 0.0091(16) 0.0068(16) N8 0.062(2) 0.044(2) 0.042(2) 0.0033(19) 0.033(2) 0.0044(18) N9 0.052(2) 0.031(2) 0.044(2) -0.0036(17) 0.0182(18) -0.0009(16) N10 0.0415(18) 0.042(2) 0.038(2) -0.0099(18) 0.0112(16) 0.0003(16) N11 0.063(2) 0.040(2) 0.038(2) 0.0023(19) 0.0188(19) -0.0027(19) N12 0.0378(18) 0.050(2) 0.041(2) 0.0009(19) 0.0158(16) -0.0100(17) O1 0.0333(13) 0.0485(18) 0.0257(15) 0.0044(14) 0.0067(11) -0.0005(13) Si1 0.0364(5) 0.0364(6) 0.0260(6) 0.0000(5) 0.0102(4) 0.0025(5) Si2 0.0408(6) 0.0316(6) 0.0374(7) 0.0017(5) 0.0160(5) 0.0027(5) Si3 0.0404(6) 0.0336(6) 0.0315(6) -0.0012(5) 0.0135(5) -0.0029(5) _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 C1 N4 1.396(6) . ? C2 N4 1.444(6) . ? C3 N5 1.339(6) . ? C4 N5 1.439(5) . ? C5 N6 1.450(6) . ? C6 N6 1.450(6) . ? C7 N7 1.404(6) . ? C8 N7 1.464(6) . ? C9 N8 1.464(6) . ? C10 N8 1.373(7) . ? C11 N9 1.411(6) . ? C12 N9 1.431(6) . ? C13 N10 1.359(6) . ? C14 N10 1.456(6) . ? C15 N12 1.398(6) . ? C16 N12 1.441(6) . ? C17 N11 1.444(7) . ? C18 N11 1.397(7) . ? C19 C20 1.426(6) . ? C19 O1 1.462(5) . ? C20 C21 1.465(7) . ? C21 C22 1.473(6) . ? C22 O1 1.338(5) . ? Al1 N1 1.722(4) . ? Al1 N3 1.774(4) . ? Al1 N2 1.817(4) . ? Al1 O1 1.877(3) . ? N1 Si1 1.583(4) . ? N2 Si2 1.689(4) . ? N3 Si3 1.689(4) . ? N4 Si1 1.700(4) . ? N5 Si1 1.699(4) . ? N6 Si1 1.712(4) . ? N7 Si2 1.645(4) . ? N8 Si2 1.636(4) . ? N9 Si2 1.718(4) . ? N10 Si3 1.685(4) . ? N11 Si3 1.610(4) . ? N12 Si3 1.713(4) . ? 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 C20 C19 O1 106.7(4) . . ? C19 C20 C21 98.6(4) . . ? C20 C21 C22 108.8(4) . . ? O1 C22 C21 104.7(4) . . ? N1 Al1 N3 119.00(19) . . ? N1 Al1 N2 114.11(18) . . ? N3 Al1 N2 113.84(17) . . ? N1 Al1 O1 97.00(15) . . ? N3 Al1 O1 104.86(16) . . ? N2 Al1 O1 104.82(16) . . ? Si1 N1 Al1 129.1(2) . . ? Si2 N2 Al1 133.3(2) . . ? Si3 N3 Al1 137.7(2) . . ? C1 N4 C2 112.4(4) . . ? C1 N4 Si1 122.1(4) . . ? C2 N4 Si1 120.2(3) . . ? C3 N5 C4 110.6(4) . . ? C3 N5 Si1 118.2(3) . . ? C4 N5 Si1 128.7(3) . . ? C5 N6 C6 111.4(4) . . ? C5 N6 Si1 127.0(3) . . ? C6 N6 Si1 121.6(3) . . ? C7 N7 C8 112.2(4) . . ? C7 N7 Si2 122.1(3) . . ? C8 N7 Si2 123.6(4) . . ? C10 N8 C9 113.5(5) . . ? C10 N8 Si2 119.5(4) . . ? C9 N8 Si2 126.9(4) . . ? C11 N9 C12 110.3(4) . . ? C11 N9 Si2 122.9(3) . . ? C12 N9 Si2 123.7(3) . . ? C13 N10 C14 111.8(4) . . ? C13 N10 Si3 122.4(3) . . ? C14 N10 Si3 125.4(3) . . ? C18 N11 C17 115.0(5) . . ? C18 N11 Si3 117.2(4) . . ? C17 N11 Si3 123.3(4) . . ? C15 N12 C16 111.1(4) . . ? C15 N12 Si3 123.9(3) . . ? C16 N12 Si3 123.5(4) . . ? C22 O1 C19 109.0(3) . . ? C22 O1 Al1 119.0(3) . . ? C19 O1 Al1 122.3(3) . . ? N1 Si1 N5 107.19(19) . . ? N1 Si1 N4 107.7(2) . . ? N5 Si1 N4 114.6(2) . . ? N1 Si1 N6 113.4(2) . . ? N5 Si1 N6 107.7(2) . . ? N4 Si1 N6 106.50(19) . . ? N8 Si2 N7 104.4(2) . . ? N8 Si2 N2 111.3(2) . . ? N7 Si2 N2 112.87(19) . . ? N8 Si2 N9 107.8(2) . . ? N7 Si2 N9 109.1(2) . . ? N2 Si2 N9 111.01(18) . . ? N11 Si3 N10 100.9(2) . . ? N11 Si3 N3 112.2(2) . . ? N10 Si3 N3 113.31(19) . . ? N11 Si3 N12 109.1(2) . . ? N10 Si3 N12 112.4(2) . . ? N3 Si3 N12 108.69(19) . . ? 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 O1 C19 C20 C21 -34.0(6) . . . . ? C19 C20 C21 C22 31.0(6) . . . . ? C20 C21 C22 O1 -16.1(7) . . . . ? N3 Al1 N1 Si1 122.3(3) . . . . ? N2 Al1 N1 Si1 -16.7(3) . . . . ? O1 Al1 N1 Si1 -126.4(3) . . . . ? N1 Al1 N2 Si2 141.1(3) . . . . ? N3 Al1 N2 Si2 -0.1(4) . . . . ? O1 Al1 N2 Si2 -114.1(3) . . . . ? N1 Al1 N3 Si3 23.6(4) . . . . ? N2 Al1 N3 Si3 162.7(3) . . . . ? O1 Al1 N3 Si3 -83.3(3) . . . . ? C21 C22 O1 C19 -6.2(6) . . . . ? C21 C22 O1 Al1 -152.9(4) . . . . ? C20 C19 O1 C22 27.1(6) . . . . ? C20 C19 O1 Al1 172.5(4) . . . . ? N1 Al1 O1 C22 -159.4(4) . . . . ? N3 Al1 O1 C22 -36.8(4) . . . . ? N2 Al1 O1 C22 83.4(4) . . . . ? N1 Al1 O1 C19 58.5(4) . . . . ? N3 Al1 O1 C19 -179.0(4) . . . . ? N2 Al1 O1 C19 -58.8(4) . . . . ? Al1 N1 Si1 N5 -75.3(3) . . . . ? Al1 N1 Si1 N4 160.9(3) . . . . ? Al1 N1 Si1 N6 43.4(3) . . . . ? C3 N5 Si1 N1 -171.9(5) . . . . ? C4 N5 Si1 N1 -11.6(5) . . . . ? C3 N5 Si1 N4 -52.5(6) . . . . ? C4 N5 Si1 N4 107.8(4) . . . . ? C3 N5 Si1 N6 65.8(5) . . . . ? C4 N5 Si1 N6 -133.9(4) . . . . ? C1 N4 Si1 N1 -155.0(4) . . . . ? C2 N4 Si1 N1 52.7(4) . . . . ? C1 N4 Si1 N5 85.8(4) . . . . ? C2 N4 Si1 N5 -66.5(4) . . . . ? C1 N4 Si1 N6 -33.1(4) . . . . ? C2 N4 Si1 N6 174.6(4) . . . . ? C5 N6 Si1 N1 -111.2(4) . . . . ? C6 N6 Si1 N1 70.0(4) . . . . ? C5 N6 Si1 N5 7.2(5) . . . . ? C6 N6 Si1 N5 -171.6(4) . . . . ? C5 N6 Si1 N4 130.6(4) . . . . ? C6 N6 Si1 N4 -48.2(4) . . . . ? C10 N8 Si2 N7 -163.5(4) . . . . ? C9 N8 Si2 N7 12.7(5) . . . . ? C10 N8 Si2 N2 74.4(4) . . . . ? C9 N8 Si2 N2 -109.4(4) . . . . ? C10 N8 Si2 N9 -47.6(4) . . . . ? C9 N8 Si2 N9 128.6(4) . . . . ? C7 N7 Si2 N8 -90.4(4) . . . . ? C8 N7 Si2 N8 71.8(4) . . . . ? C7 N7 Si2 N2 30.7(5) . . . . ? C8 N7 Si2 N2 -167.2(4) . . . . ? C7 N7 Si2 N9 154.6(4) . . . . ? C8 N7 Si2 N9 -43.3(4) . . . . ? Al1 N2 Si2 N8 25.7(4) . . . . ? Al1 N2 Si2 N7 -91.3(3) . . . . ? Al1 N2 Si2 N9 145.8(3) . . . . ? C11 N9 Si2 N8 -38.4(5) . . . . ? C12 N9 Si2 N8 163.4(4) . . . . ? C11 N9 Si2 N7 74.4(4) . . . . ? C12 N9 Si2 N7 -83.7(4) . . . . ? C11 N9 Si2 N2 -160.6(4) . . . . ? C12 N9 Si2 N2 41.2(5) . . . . ? C18 N11 Si3 N10 163.9(4) . . . . ? C17 N11 Si3 N10 -41.1(5) . . . . ? C18 N11 Si3 N3 43.0(4) . . . . ? C17 N11 Si3 N3 -162.0(4) . . . . ? C18 N11 Si3 N12 -77.5(4) . . . . ? C17 N11 Si3 N12 77.5(5) . . . . ? C13 N10 Si3 N11 138.0(4) . . . . ? C14 N10 Si3 N11 -50.5(5) . . . . ? C13 N10 Si3 N3 -101.8(4) . . . . ? C14 N10 Si3 N3 69.7(5) . . . . ? C13 N10 Si3 N12 21.9(5) . . . . ? C14 N10 Si3 N12 -166.6(4) . . . . ? Al1 N3 Si3 N11 112.1(3) . . . . ? Al1 N3 Si3 N10 -1.4(4) . . . . ? Al1 N3 Si3 N12 -127.1(3) . . . . ? C15 N12 Si3 N11 152.7(4) . . . . ? C16 N12 Si3 N11 -42.3(5) . . . . ? C15 N12 Si3 N10 -96.1(5) . . . . ? C16 N12 Si3 N10 68.8(5) . . . . ? C15 N12 Si3 N3 30.1(5) . . . . ? C16 N12 Si3 N3 -165.0(5) . . . . ? _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 30.28 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.394 _refine_diff_density_min -0.477 _refine_diff_density_rms 0.082 #===END