# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 182/1181 data_mfl1 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[AlMe2(Me3SiNCPhCHCPhNSiMe3)]' _chemical_formula_analytical ? _chemical_formula_sum 'C23 H35 Al N2 Si2' _chemical_formula_weight 422.69 _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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.335(2) _cell_length_b 12.139(3) _cell_length_c 17.103(4) _cell_angle_alpha 78.55(2) _cell_angle_beta 79.90(3) _cell_angle_gamma 74.84(3) _cell_volume 1233.6(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method ? _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.190 _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 4338 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4338 _reflns_number_observed 3026 _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^)+(0.1365P)^2^+1.2933P] 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 4338 _refine_ls_number_parameters 253 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1143 _refine_ls_R_factor_obs 0.0787 _refine_ls_wR_factor_all 0.2354 _refine_ls_wR_factor_obs 0.1955 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.043 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.043 _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 Si1 Si 0.9477(2) 0.70828(11) 0.08192(8) 0.0247(4) Uani 1 d . . Si2 Si 0.7056(2) 0.95096(10) 0.34298(8) 0.0227(4) Uani 1 d . . Al Al 1.0957(2) 0.80723(11) 0.22317(8) 0.0208(4) Uani 1 d . . N1 N 0.9998(6) 0.6953(3) 0.1822(2) 0.0199(8) Uani 1 d . . N2 N 0.8747(6) 0.8203(3) 0.3161(2) 0.0206(8) Uani 1 d . . C1 C 0.9815(7) 0.6060(4) 0.2403(3) 0.0203(10) Uani 1 d . . C2 C 0.9416(7) 0.6131(4) 0.3221(3) 0.0222(10) Uani 1 d . . H2 H 0.9636(7) 0.5419(4) 0.3582(3) 0.027 Uiso 1 calc R . C3 C 0.8722(7) 0.7145(4) 0.3568(3) 0.0213(10) Uani 1 d . . C4 C 1.0121(8) 0.4885(4) 0.2203(3) 0.0231(10) Uani 1 d . . C5 C 0.8547(9) 0.4276(4) 0.2451(3) 0.0310(12) Uani 1 d . . H5 H 0.7206(9) 0.4594(4) 0.2760(3) 0.037 Uiso 1 calc R . C6 C 0.8918(11) 0.3159(4) 0.2244(3) 0.0420(15) Uani 1 d . . H6 H 0.7803(11) 0.2736(4) 0.2397(3) 0.050 Uiso 1 calc R . C7 C 1.0882(11) 0.2697(4) 0.1825(3) 0.044(2) Uani 1 d . . H7 H 1.1142(11) 0.1945(4) 0.1693(3) 0.052 Uiso 1 calc R . C8 C 1.2465(10) 0.3304(4) 0.1596(3) 0.0405(15) Uani 1 d . . H8 H 1.3830(10) 0.2967(4) 0.1309(3) 0.049 Uiso 1 calc R . C9 C 1.2133(8) 0.4399(4) 0.1773(3) 0.0284(11) Uani 1 d . . H9 H 1.3250(8) 0.4819(4) 0.1605(3) 0.034 Uiso 1 calc R . C10 C 0.7974(8) 0.6982(4) 0.4451(3) 0.0250(11) Uani 1 d . . C11 C 0.9008(9) 0.7378(4) 0.4951(3) 0.0333(12) Uani 1 d . . H11 H 1.0169(9) 0.7755(4) 0.4731(3) 0.040 Uiso 1 calc R . C12 C 0.8342(10) 0.7220(5) 0.5772(3) 0.0424(15) Uani 1 d . . H12 H 0.9078(10) 0.7473(5) 0.6117(3) 0.051 Uiso 1 calc R . C13 C 0.6637(11) 0.6704(5) 0.6093(3) 0.045(2) Uani 1 d . . H13 H 0.6163(11) 0.6622(5) 0.6656(3) 0.054 Uiso 1 calc R . C14 C 0.5602(11) 0.6300(5) 0.5599(3) 0.0422(14) Uani 1 d . . H14 H 0.4425(11) 0.5935(5) 0.5820(3) 0.051 Uiso 1 calc R . C15 C 0.6296(9) 0.6434(4) 0.4782(3) 0.0321(12) Uani 1 d . . H15 H 0.5607(9) 0.6143(4) 0.4443(3) 0.039 Uiso 1 calc R . C16 C 1.1156(9) 0.9511(4) 0.1487(3) 0.0356(12) Uani 1 d . . H16C H 1.1659(9) 1.0020(4) 0.1755(3) 0.053 Uiso 1 calc R . H16B H 0.9700(9) 0.9900(4) 0.1324(3) 0.053 Uiso 1 calc R . H16A H 1.2206(9) 0.9330(4) 0.1010(3) 0.053 Uiso 1 calc R . C17 C 1.3778(8) 0.7301(4) 0.2623(3) 0.0321(12) Uani 1 d . . H17C H 1.4320(8) 0.7851(4) 0.2838(3) 0.048 Uiso 1 calc R . H17B H 1.4849(8) 0.7014(4) 0.2178(3) 0.048 Uiso 1 calc R . H17A H 1.3581(8) 0.6651(4) 0.3049(3) 0.048 Uiso 1 calc R . C18 C 1.2082(10) 0.7003(6) 0.0127(3) 0.0453(15) Uani 1 d . . H18C H 1.2825(10) 0.7575(6) 0.0212(3) 0.068 Uiso 1 calc R . H18B H 1.1761(10) 0.7165(6) -0.0431(3) 0.068 Uiso 1 calc R . H18A H 1.3041(10) 0.6227(6) 0.0231(3) 0.068 Uiso 1 calc R . C19 C 0.7609(10) 0.8521(5) 0.0574(3) 0.0401(14) Uani 1 d . . H19C H 0.6224(10) 0.8568(5) 0.0940(3) 0.060 Uiso 1 calc R . H19B H 0.7303(10) 0.8632(5) 0.0018(3) 0.060 Uiso 1 calc R . H19A H 0.8312(10) 0.9124(5) 0.0635(3) 0.060 Uiso 1 calc R . C20 C 0.8036(9) 0.6013(5) 0.0673(3) 0.0351(12) Uani 1 d . . H20C H 0.6660(9) 0.6066(5) 0.1044(3) 0.053 Uiso 1 calc R . H20B H 0.8982(9) 0.5234(5) 0.0779(3) 0.053 Uiso 1 calc R . H20A H 0.7702(9) 0.6172(5) 0.0117(3) 0.053 Uiso 1 calc R . C21 C 0.4653(8) 0.9330(4) 0.4181(3) 0.0312(12) Uani 1 d . . H21C H 0.3797(8) 0.8898(4) 0.3987(3) 0.047 Uiso 1 calc R . H21B H 0.3726(8) 1.0092(4) 0.4265(3) 0.047 Uiso 1 calc R . H21A H 0.5159(8) 0.8904(4) 0.4690(3) 0.047 Uiso 1 calc R . C22 C 0.8731(9) 1.0323(4) 0.3769(3) 0.0343(12) Uani 1 d . . H22C H 0.9997(9) 1.0406(4) 0.3360(3) 0.051 Uiso 1 calc R . H22B H 0.9257(9) 0.9903(4) 0.4277(3) 0.051 Uiso 1 calc R . H22A H 0.7826(9) 1.1091(4) 0.3851(3) 0.051 Uiso 1 calc R . C23 C 0.5883(9) 1.0377(5) 0.2513(3) 0.0379(13) Uani 1 d . . H23C H 0.7086(9) 1.0505(5) 0.2086(3) 0.057 Uiso 1 calc R . H23B H 0.4972(9) 1.1123(5) 0.2638(3) 0.057 Uiso 1 calc R . H23A H 0.4975(9) 0.9958(5) 0.2333(3) 0.057 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 Si1 0.0218(7) 0.0266(7) 0.0203(7) -0.0028(5) -0.0040(5) 0.0037(5) Si2 0.0206(7) 0.0134(6) 0.0308(7) -0.0078(5) -0.0067(5) 0.0072(5) Al 0.0194(7) 0.0131(7) 0.0267(7) -0.0051(5) -0.0040(6) 0.0039(5) N1 0.019(2) 0.013(2) 0.024(2) -0.0008(15) -0.006(2) 0.0027(15) N2 0.016(2) 0.015(2) 0.028(2) -0.008(2) -0.004(2) 0.0050(15) C1 0.018(2) 0.017(2) 0.024(2) -0.006(2) -0.004(2) 0.002(2) C2 0.024(2) 0.014(2) 0.022(2) -0.003(2) -0.005(2) 0.008(2) C3 0.021(2) 0.013(2) 0.028(2) -0.007(2) -0.009(2) 0.006(2) C4 0.031(3) 0.013(2) 0.022(2) -0.004(2) -0.011(2) 0.007(2) C5 0.041(3) 0.020(2) 0.027(3) -0.005(2) -0.006(2) 0.004(2) C6 0.080(5) 0.015(2) 0.039(3) -0.003(2) -0.019(3) -0.017(3) C7 0.076(5) 0.008(2) 0.044(3) -0.011(2) -0.024(3) 0.009(3) C8 0.054(4) 0.025(3) 0.031(3) -0.013(2) -0.011(3) 0.020(3) C9 0.027(3) 0.024(2) 0.029(3) -0.009(2) -0.010(2) 0.010(2) C10 0.031(3) 0.013(2) 0.026(2) -0.008(2) -0.006(2) 0.009(2) C11 0.034(3) 0.026(3) 0.034(3) -0.011(2) -0.014(2) 0.015(2) C12 0.054(4) 0.036(3) 0.031(3) -0.015(2) -0.019(3) 0.017(3) C13 0.066(4) 0.034(3) 0.019(3) 0.001(2) -0.002(3) 0.010(3) C14 0.057(4) 0.029(3) 0.030(3) -0.001(2) 0.006(3) -0.002(3) C15 0.042(3) 0.020(2) 0.032(3) -0.008(2) 0.001(2) -0.003(2) C16 0.035(3) 0.021(3) 0.046(3) -0.001(2) -0.002(2) -0.005(2) C17 0.024(3) 0.030(3) 0.038(3) -0.008(2) -0.004(2) 0.004(2) C18 0.034(3) 0.070(4) 0.030(3) -0.008(3) -0.005(2) -0.010(3) C19 0.045(3) 0.029(3) 0.041(3) 0.000(2) -0.021(3) 0.006(2) C20 0.036(3) 0.034(3) 0.029(3) -0.008(2) -0.009(2) 0.007(2) C21 0.020(3) 0.024(3) 0.044(3) -0.011(2) -0.004(2) 0.010(2) C22 0.032(3) 0.023(3) 0.048(3) -0.014(2) -0.006(2) -0.001(2) C23 0.031(3) 0.029(3) 0.042(3) -0.005(2) -0.010(2) 0.016(2) _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 Si1 N1 1.773(4) . ? Si1 C18 1.847(6) . ? Si1 C20 1.847(6) . ? Si1 C19 1.851(5) . ? Si2 N2 1.761(4) . ? Si2 C21 1.842(5) . ? Si2 C22 1.852(5) . ? Si2 C23 1.860(5) . ? Al N1 1.914(4) . ? Al N2 1.928(4) . ? Al C17 1.953(5) . ? Al C16 1.966(5) . ? N1 C1 1.331(6) . ? N2 C3 1.336(6) . ? C1 C2 1.394(6) . ? C1 C4 1.489(6) . ? C2 C3 1.406(6) . ? C3 C10 1.490(6) . ? C4 C5 1.354(7) . ? C4 C9 1.401(7) . ? C5 C6 1.419(7) . ? C6 C7 1.363(9) . ? C7 C8 1.355(8) . ? C8 C9 1.376(7) . ? C10 C15 1.380(7) . ? C10 C11 1.384(7) . ? C11 C12 1.385(7) . ? C12 C13 1.368(9) . ? C13 C14 1.382(8) . ? C14 C15 1.380(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C18 110.0(2) . . ? N1 Si1 C20 113.9(2) . . ? C18 Si1 C20 110.5(3) . . ? N1 Si1 C19 107.0(2) . . ? C18 Si1 C19 109.1(3) . . ? C20 Si1 C19 106.2(3) . . ? N2 Si2 C21 114.1(2) . . ? N2 Si2 C22 109.9(2) . . ? C21 Si2 C22 111.1(2) . . ? N2 Si2 C23 107.4(2) . . ? C21 Si2 C23 105.2(2) . . ? C22 Si2 C23 108.8(3) . . ? N1 Al N2 97.1(2) . . ? N1 Al C17 107.3(2) . . ? N2 Al C17 107.2(2) . . ? N1 Al C16 116.1(2) . . ? N2 Al C16 116.6(2) . . ? C17 Al C16 111.3(2) . . ? C1 N1 Si1 125.5(3) . . ? C1 N1 Al 109.5(3) . . ? Si1 N1 Al 125.0(2) . . ? C3 N2 Si2 125.8(3) . . ? C3 N2 Al 108.9(3) . . ? Si2 N2 Al 125.3(2) . . ? N1 C1 C2 124.0(4) . . ? N1 C1 C4 120.5(4) . . ? C2 C1 C4 115.5(4) . . ? C1 C2 C3 126.8(4) . . ? N2 C3 C2 124.2(4) . . ? N2 C3 C10 120.1(4) . . ? C2 C3 C10 115.7(4) . . ? C5 C4 C9 120.3(4) . . ? C5 C4 C1 121.6(4) . . ? C9 C4 C1 118.1(4) . . ? C4 C5 C6 119.4(5) . . ? C7 C6 C5 119.6(5) . . ? C8 C7 C6 120.4(5) . . ? C7 C8 C9 121.3(5) . . ? C8 C9 C4 119.0(5) . . ? C15 C10 C11 119.2(5) . . ? C15 C10 C3 121.7(4) . . ? C11 C10 C3 119.1(5) . . ? C10 C11 C12 119.6(6) . . ? C13 C12 C11 120.7(5) . . ? C12 C13 C14 120.0(5) . . ? C15 C14 C13 119.3(6) . . ? C10 C15 C14 121.1(5) . . ? _refine_diff_density_max 0.615 _refine_diff_density_min -0.784 _refine_diff_density_rms 0.122 #=END data_mfl2 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; '[AlMe(OEt2)(Me3SiNCPhCHCPHNSiMe3)][BMe(C6F5)3].0.5(Et2O)' ; _chemical_formula_analytical ? _chemical_formula_sum 'C47 H48 Al B F15 N2 O1.50 Si2' _chemical_formula_weight 1043.84 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.016(3) _cell_length_b 13.439(5) _cell_length_c 16.409(7) _cell_angle_alpha 99.44(3) _cell_angle_beta 91.80(3) _cell_angle_gamma 108.31(2) _cell_volume 2471.8(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.402 _exptl_crystal_density_method ? _exptl_crystal_F_000 1074 _exptl_absorpt_coefficient_mu 0.185 _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 8664 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8664 _reflns_number_observed 5806 _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 diethylether solvate molecule is disordered across an inversion centre. 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^)+(0.1320P)^2^+4.8461P] 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 8663 _refine_ls_number_parameters 637 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0942 _refine_ls_R_factor_obs 0.0526 _refine_ls_wR_factor_all 0.2013 _refine_ls_wR_factor_obs 0.1458 _refine_ls_goodness_of_fit_all 0.833 _refine_ls_goodness_of_fit_obs 0.748 _refine_ls_restrained_S_all 0.837 _refine_ls_restrained_S_obs 0.748 _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 Si1 Si 0.60646(12) 0.64580(10) 0.17274(8) 0.0385(3) Uani 1 d . . Si2 Si 0.18658(10) 0.73346(9) 0.24853(7) 0.0305(3) Uani 1 d . . Al Al 0.44928(11) 0.80066(10) 0.18971(7) 0.0280(3) Uani 1 d . . F1 F -0.1329(2) 1.2367(2) 0.2788(2) 0.0449(7) Uani 1 d . . F2 F -0.2412(2) 1.3386(2) 0.1968(2) 0.0538(8) Uani 1 d . . F3 F -0.1516(3) 1.4192(2) 0.0635(2) 0.0543(8) Uani 1 d . . F4 F 0.0583(3) 1.4018(2) 0.0166(2) 0.0487(7) Uani 1 d . . F5 F 0.1782(2) 1.3147(2) 0.10473(15) 0.0384(6) Uani 1 d . . F6 F -0.0758(2) 1.0073(2) 0.15706(15) 0.0353(6) Uani 1 d . . F7 F -0.0507(2) 0.8590(2) 0.03933(15) 0.0393(6) Uani 1 d . . F8 F 0.1600(2) 0.8819(2) -0.02561(15) 0.0431(6) Uani 1 d . . F9 F 0.3455(2) 1.0603(2) 0.0315(2) 0.0438(6) Uani 1 d . . F10 F 0.3259(2) 1.2094(2) 0.15005(14) 0.0352(6) Uani 1 d . . F11 F 0.1902(2) 1.4485(2) 0.2892(2) 0.0449(7) Uani 1 d . . F12 F 0.3917(3) 1.5682(2) 0.3735(2) 0.0590(8) Uani 1 d . . F13 F 0.5498(2) 1.4785(2) 0.4250(2) 0.0569(8) Uani 1 d . . F14 F 0.4969(2) 1.2626(2) 0.3897(2) 0.0519(7) Uani 1 d . . F15 F 0.2966(2) 1.1406(2) 0.30491(15) 0.0383(6) Uani 1 d . . O1 O 0.5335(2) 0.9469(2) 0.2149(2) 0.0324(7) Uani 1 d . . N1 N 0.5595(3) 0.7459(3) 0.2332(2) 0.0280(7) Uani 1 d . . N2 N 0.3426(3) 0.7917(3) 0.2705(2) 0.0260(7) Uani 1 d . . C1 C 0.5853(3) 0.7844(3) 0.3152(2) 0.0257(8) Uani 1 d . . C2 C 0.5151(3) 0.8302(3) 0.3657(2) 0.0269(8) Uani 1 d . . H2 H 0.5514(3) 0.8700(3) 0.4184(2) 0.032 Uiso 1 calc R . C3 C 0.3992(3) 0.8243(3) 0.3480(2) 0.0245(8) Uani 1 d . . C4 C 0.6962(3) 0.7848(3) 0.3590(2) 0.0269(8) Uani 1 d . . C5 C 0.6930(4) 0.7408(3) 0.4306(3) 0.0335(9) Uani 1 d . . H5 H 0.6194(4) 0.7067(3) 0.4499(3) 0.040 Uiso 1 calc R . C6 C 0.7957(4) 0.7466(4) 0.4731(3) 0.0387(10) Uani 1 d . . H6 H 0.7931(4) 0.7142(4) 0.5206(3) 0.046 Uiso 1 calc R . C7 C 0.9024(4) 0.7993(4) 0.4470(3) 0.0478(12) Uani 1 d . . H7 H 0.9732(4) 0.8043(4) 0.4773(3) 0.057 Uiso 1 calc R . C8 C 0.9074(4) 0.8448(4) 0.3772(3) 0.0434(11) Uani 1 d . . H8 H 0.9814(4) 0.8826(4) 0.3603(3) 0.052 Uiso 1 calc R . C9 C 0.8043(4) 0.8355(4) 0.3318(3) 0.0354(10) Uani 1 d . . H9 H 0.8075(4) 0.8637(4) 0.2821(3) 0.042 Uiso 1 calc R . C10 C 0.3382(3) 0.8583(3) 0.4191(2) 0.0261(8) Uani 1 d . . C11 C 0.2840(3) 0.9358(3) 0.4157(3) 0.0306(9) Uani 1 d . . H11 H 0.2864(3) 0.9669(3) 0.3676(3) 0.037 Uiso 1 calc R . C12 C 0.2270(4) 0.9673(3) 0.4819(3) 0.0395(11) Uani 1 d . . H12 H 0.1905(4) 1.0201(3) 0.4792(3) 0.047 Uiso 1 calc R . C13 C 0.2230(4) 0.9220(4) 0.5522(3) 0.0463(12) Uani 1 d . . H13 H 0.1825(4) 0.9427(4) 0.5973(3) 0.056 Uiso 1 calc R . C14 C 0.2780(4) 0.8468(4) 0.5563(3) 0.0457(12) Uani 1 d . . H14 H 0.2758(4) 0.8159(4) 0.6046(3) 0.055 Uiso 1 calc R . C15 C 0.3365(4) 0.8160(4) 0.4902(3) 0.0352(10) Uani 1 d . . H15 H 0.3756(4) 0.7654(4) 0.4940(3) 0.042 Uiso 1 calc R . C16 C 0.4024(5) 0.7763(4) 0.0713(3) 0.0483(12) Uani 1 d . . H16A H 0.4722(5) 0.7850(4) 0.0403(3) 0.072 Uiso 1 calc R . H16B H 0.3641(5) 0.8278(4) 0.0603(3) 0.072 Uiso 1 calc R . H16C H 0.3474(5) 0.7038(4) 0.0538(3) 0.072 Uiso 1 calc R . C17 C 0.6881(6) 0.5819(5) 0.2334(4) 0.073(2) Uani 1 d . . H17A H 0.6397(6) 0.5515(5) 0.2759(4) 0.109 Uiso 1 calc R . H17B H 0.7615(6) 0.6353(5) 0.2601(4) 0.109 Uiso 1 calc R . H17C H 0.7061(6) 0.5251(5) 0.1962(4) 0.109 Uiso 1 calc R . C18 C 0.6916(6) 0.7054(5) 0.0910(3) 0.066(2) Uani 1 d . . H18A H 0.6453(6) 0.7381(5) 0.0606(3) 0.099 Uiso 1 calc R . H18B H 0.7097(6) 0.6497(5) 0.0525(3) 0.099 Uiso 1 calc R . H18C H 0.7651(6) 0.7599(5) 0.1164(3) 0.099 Uiso 1 calc R . C19 C 0.4686(5) 0.5399(4) 0.1253(4) 0.063(2) Uani 1 d . . H19A H 0.4239(5) 0.5087(4) 0.1690(4) 0.094 Uiso 1 calc R . H19B H 0.4880(5) 0.4843(4) 0.0877(4) 0.094 Uiso 1 calc R . H19C H 0.4211(5) 0.5708(4) 0.0941(4) 0.094 Uiso 1 calc R . C20 C 0.1635(4) 0.6210(4) 0.1606(3) 0.0513(13) Uani 1 d . . H20A H 0.2024(4) 0.6479(4) 0.1133(3) 0.077 Uiso 1 calc R . H20B H 0.0790(4) 0.5869(4) 0.1448(3) 0.077 Uiso 1 calc R . H20C H 0.1969(4) 0.5689(4) 0.1773(3) 0.077 Uiso 1 calc R . C21 C 0.1110(4) 0.6773(4) 0.3359(3) 0.0375(10) Uani 1 d . . H21A H 0.1215(4) 0.7348(4) 0.3836(3) 0.056 Uiso 1 calc R . H21B H 0.1448(4) 0.6248(4) 0.3512(3) 0.056 Uiso 1 calc R . H21C H 0.0269(4) 0.6428(4) 0.3188(3) 0.056 Uiso 1 calc R . C22 C 0.1271(4) 0.8335(4) 0.2145(3) 0.0523(13) Uani 1 d . . H22A H 0.1388(4) 0.8933(4) 0.2605(3) 0.078 Uiso 1 calc R . H22B H 0.0428(4) 0.8003(4) 0.1974(3) 0.078 Uiso 1 calc R . H22C H 0.1682(4) 0.8595(4) 0.1677(3) 0.078 Uiso 1 calc R . C23 C 0.4776(4) 1.0300(3) 0.2393(3) 0.0391(11) Uani 1 d . . H23A H 0.4734(4) 1.0438(3) 0.3000(3) 0.047 Uiso 1 calc R . H23B H 0.3971(4) 1.0082(3) 0.2114(3) 0.047 Uiso 1 calc R . C24 C 0.5574(4) 1.1282(4) 0.2108(3) 0.0394(10) Uani 1 d . . H24A H 0.5111(4) 1.1696(4) 0.1900(3) 0.047 Uiso 1 calc R . H24B H 0.6153(4) 1.1749(4) 0.2566(3) 0.047 Uiso 1 calc R . C25 C 0.6182(4) 1.0828(4) 0.1419(3) 0.0439(11) Uani 1 d . . H25A H 0.5667(4) 1.0565(4) 0.0894(3) 0.053 Uiso 1 calc R . H25B H 0.6926(4) 1.1363(4) 0.1326(3) 0.053 Uiso 1 calc R . C26 C 0.6408(4) 0.9929(4) 0.1755(3) 0.0400(11) Uani 1 d . . H26A H 0.6531(4) 0.9397(4) 0.1304(3) 0.048 Uiso 1 calc R . H26B H 0.7106(4) 1.0195(4) 0.2165(3) 0.048 Uiso 1 calc R . B B 0.1039(4) 1.2048(3) 0.2418(3) 0.0256(9) Uani 1 d . . C27 C 0.0370(4) 1.1448(3) 0.3141(3) 0.0332(9) Uani 1 d . . H27A H 0.0866(4) 1.1095(3) 0.3381(3) 0.050 Uiso 1 calc R . H27B H -0.0380(4) 1.0916(3) 0.2900(3) 0.050 Uiso 1 calc R . H27C H 0.0222(4) 1.1974(3) 0.3576(3) 0.050 Uiso 1 calc R . C28 C 0.0303(3) 1.2676(3) 0.1960(2) 0.0264(8) Uani 1 d . . C29 C -0.0777(4) 1.2779(3) 0.2150(3) 0.0303(9) Uani 1 d . . C30 C -0.1368(4) 1.3301(3) 0.1738(3) 0.0356(10) Uani 1 d . . C31 C -0.0925(4) 1.3710(3) 0.1059(3) 0.0369(10) Uani 1 d . . C32 C 0.0122(4) 1.3619(3) 0.0826(3) 0.0342(10) Uani 1 d . . C33 C 0.0707(4) 1.3142(3) 0.1283(2) 0.0286(9) Uani 1 d . . C34 C 0.1247(3) 1.1164(3) 0.1653(2) 0.0246(8) Uani 1 d . . C35 C 0.0328(3) 1.0245(3) 0.1303(2) 0.0277(9) Uani 1 d . . C36 C 0.0418(4) 0.9461(3) 0.0675(2) 0.0292(9) Uani 1 d . . C37 C 0.1478(4) 0.9577(3) 0.0344(2) 0.0306(9) Uani 1 d . . C38 C 0.2412(4) 1.0473(3) 0.0639(2) 0.0292(9) Uani 1 d . . C39 C 0.2287(3) 1.1237(3) 0.1274(2) 0.0269(8) Uani 1 d . . C40 C 0.2316(4) 1.2870(3) 0.2898(2) 0.0266(9) Uani 1 d . . C41 C 0.2632(4) 1.3968(3) 0.3116(2) 0.0318(9) Uani 1 d . . C42 C 0.3666(4) 1.4611(3) 0.3559(3) 0.0385(10) Uani 1 d . . C43 C 0.4471(4) 1.4171(4) 0.3823(3) 0.0377(10) Uani 1 d . . C44 C 0.4196(4) 1.3080(4) 0.3648(3) 0.0346(10) Uani 1 d . . C45 C 0.3159(4) 1.2478(3) 0.3201(2) 0.0303(9) Uani 1 d . . O2 O 0.0000 0.5000 0.5000 0.086(2) Uani 1 d S . C46 C -0.1040(16) 0.5148(13) 0.4809(10) 0.088(4) Uani 0.50 d P 1 H46A H -0.0859(16) 0.5902(13) 0.4749(10) 0.105 Uiso 0.50 calc PR 1 H46B H -0.1503(16) 0.5055(13) 0.5296(10) 0.105 Uiso 0.50 calc PR 1 C47 C -0.1759(9) 0.4538(8) 0.4129(7) 0.122(3) Uani 0.50 d P 1 H47A H -0.2464(9) 0.4751(8) 0.4087(7) 0.182 Uiso 0.50 calc PR 1 H47B H -0.1988(9) 0.3786(8) 0.4181(7) 0.182 Uiso 0.50 calc PR 1 H47C H -0.1340(9) 0.4639(8) 0.3630(7) 0.182 Uiso 0.50 calc PR 1 C46A C -0.0713(13) 0.4372(11) 0.4338(9) 0.078(4) Uani 0.50 d P 2 H46C H -0.0912(13) 0.3627(11) 0.4425(9) 0.093 Uiso 0.50 calc PR 2 H46D H -0.0249(13) 0.4429(11) 0.3849(9) 0.093 Uiso 0.50 calc PR 2 C47A C -0.1759(9) 0.4538(8) 0.4129(7) 0.122(3) Uani 0.50 d P 2 H47D H -0.2169(4704) 0.4017(4704) 0.3636(75) 0.182 Uiso 0.50 calc PR 2 H47E H -0.1590(4704) 0.5261(4704) 0.4012(75) 0.182 Uiso 0.50 calc PR 2 H47F H -0.2256(4704) 0.4453(4704) 0.4591(75) 0.182 Uiso 0.50 calc PR 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 Si1 0.0458(8) 0.0376(7) 0.0342(7) -0.0009(5) 0.0116(6) 0.0194(6) Si2 0.0258(6) 0.0326(6) 0.0320(6) 0.0105(5) 0.0005(5) 0.0059(5) Al 0.0298(7) 0.0321(7) 0.0232(6) 0.0060(5) 0.0058(5) 0.0107(5) F1 0.0410(15) 0.055(2) 0.052(2) 0.0263(13) 0.0241(13) 0.0239(13) F2 0.037(2) 0.049(2) 0.086(2) 0.023(2) 0.0112(15) 0.0227(13) F3 0.056(2) 0.047(2) 0.067(2) 0.0243(14) -0.0080(15) 0.0224(14) F4 0.065(2) 0.046(2) 0.0381(14) 0.0233(12) 0.0070(13) 0.0144(14) F5 0.0404(15) 0.0421(14) 0.0374(14) 0.0182(11) 0.0173(11) 0.0132(11) F6 0.0250(12) 0.0372(13) 0.0381(13) 0.0033(10) 0.0049(10) 0.0038(10) F7 0.0408(15) 0.0296(13) 0.0365(14) -0.0012(10) 0.0002(11) 0.0000(11) F8 0.049(2) 0.0401(14) 0.0358(14) -0.0089(11) 0.0043(12) 0.0162(12) F9 0.0362(14) 0.054(2) 0.0382(14) -0.0013(12) 0.0130(11) 0.0140(12) F10 0.0282(13) 0.0356(13) 0.0328(13) 0.0000(10) 0.0072(10) 0.0003(10) F11 0.052(2) 0.0301(13) 0.052(2) 0.0005(11) -0.0123(13) 0.0181(12) F12 0.060(2) 0.0287(14) 0.073(2) -0.0033(13) -0.012(2) 0.0017(13) F13 0.038(2) 0.062(2) 0.055(2) -0.0053(14) -0.0111(13) 0.0044(14) F14 0.045(2) 0.065(2) 0.050(2) 0.0057(14) -0.0101(13) 0.0278(14) F15 0.047(2) 0.0318(13) 0.0411(14) 0.0069(11) -0.0008(12) 0.0204(11) O1 0.031(2) 0.036(2) 0.036(2) 0.0123(13) 0.0144(13) 0.0148(13) N1 0.032(2) 0.028(2) 0.026(2) 0.0038(14) 0.0102(14) 0.0119(15) N2 0.026(2) 0.029(2) 0.025(2) 0.0074(13) 0.0063(14) 0.0093(14) C1 0.024(2) 0.026(2) 0.026(2) 0.006(2) 0.007(2) 0.007(2) C2 0.022(2) 0.030(2) 0.025(2) 0.001(2) 0.002(2) 0.006(2) C3 0.028(2) 0.019(2) 0.025(2) 0.0039(15) 0.002(2) 0.005(2) C4 0.026(2) 0.031(2) 0.025(2) 0.001(2) 0.005(2) 0.013(2) C5 0.032(2) 0.039(2) 0.030(2) 0.003(2) 0.006(2) 0.013(2) C6 0.039(3) 0.048(3) 0.033(2) 0.005(2) 0.004(2) 0.021(2) C7 0.034(3) 0.067(3) 0.045(3) 0.000(2) -0.002(2) 0.025(2) C8 0.024(2) 0.061(3) 0.047(3) 0.007(2) 0.009(2) 0.017(2) C9 0.035(2) 0.043(3) 0.032(2) 0.008(2) 0.012(2) 0.017(2) C10 0.020(2) 0.027(2) 0.029(2) 0.002(2) 0.004(2) 0.005(2) C11 0.025(2) 0.027(2) 0.037(2) 0.005(2) 0.010(2) 0.005(2) C12 0.031(2) 0.029(2) 0.054(3) -0.004(2) 0.016(2) 0.008(2) C13 0.034(3) 0.051(3) 0.044(3) -0.006(2) 0.018(2) 0.007(2) C14 0.047(3) 0.061(3) 0.029(2) 0.009(2) 0.014(2) 0.015(2) C15 0.030(2) 0.046(3) 0.029(2) 0.005(2) 0.007(2) 0.013(2) C16 0.050(3) 0.064(3) 0.030(2) 0.010(2) 0.004(2) 0.018(3) C17 0.104(5) 0.060(4) 0.071(4) -0.007(3) -0.001(4) 0.060(4) C18 0.075(4) 0.071(4) 0.053(3) 0.003(3) 0.040(3) 0.025(3) C19 0.073(4) 0.046(3) 0.061(4) -0.012(3) 0.005(3) 0.019(3) C20 0.042(3) 0.054(3) 0.041(3) -0.002(2) -0.001(2) -0.003(2) C21 0.029(2) 0.039(2) 0.044(3) 0.015(2) 0.007(2) 0.006(2) C22 0.040(3) 0.066(3) 0.061(3) 0.034(3) 0.003(2) 0.020(3) C23 0.040(3) 0.036(2) 0.047(3) 0.012(2) 0.019(2) 0.017(2) C24 0.039(3) 0.036(2) 0.046(3) 0.012(2) 0.009(2) 0.013(2) C25 0.047(3) 0.039(3) 0.044(3) 0.014(2) 0.014(2) 0.007(2) C26 0.029(2) 0.041(3) 0.051(3) 0.011(2) 0.016(2) 0.010(2) B 0.027(2) 0.024(2) 0.026(2) 0.005(2) 0.001(2) 0.008(2) C27 0.034(2) 0.033(2) 0.033(2) 0.011(2) 0.006(2) 0.009(2) C28 0.027(2) 0.021(2) 0.028(2) 0.003(2) 0.002(2) 0.004(2) C29 0.030(2) 0.026(2) 0.034(2) 0.008(2) 0.003(2) 0.007(2) C30 0.029(2) 0.027(2) 0.050(3) 0.005(2) 0.000(2) 0.009(2) C31 0.037(3) 0.028(2) 0.044(3) 0.009(2) -0.013(2) 0.008(2) C32 0.047(3) 0.023(2) 0.028(2) 0.008(2) -0.004(2) 0.005(2) C33 0.028(2) 0.025(2) 0.029(2) 0.003(2) 0.004(2) 0.004(2) C34 0.028(2) 0.024(2) 0.025(2) 0.008(2) 0.002(2) 0.010(2) C35 0.027(2) 0.031(2) 0.030(2) 0.011(2) 0.005(2) 0.012(2) C36 0.034(2) 0.025(2) 0.026(2) 0.005(2) -0.003(2) 0.005(2) C37 0.039(2) 0.032(2) 0.023(2) 0.004(2) 0.001(2) 0.015(2) C38 0.030(2) 0.038(2) 0.023(2) 0.008(2) 0.010(2) 0.014(2) C39 0.025(2) 0.029(2) 0.024(2) 0.005(2) 0.002(2) 0.006(2) C40 0.034(2) 0.027(2) 0.021(2) 0.006(2) 0.006(2) 0.011(2) C41 0.036(2) 0.030(2) 0.028(2) 0.003(2) -0.003(2) 0.011(2) C42 0.044(3) 0.025(2) 0.038(2) 0.002(2) 0.003(2) 0.003(2) C43 0.031(2) 0.046(3) 0.029(2) 0.001(2) -0.003(2) 0.005(2) C44 0.036(2) 0.045(3) 0.028(2) 0.005(2) 0.001(2) 0.020(2) C45 0.035(2) 0.028(2) 0.028(2) 0.004(2) 0.006(2) 0.011(2) O2 0.087(5) 0.082(5) 0.091(5) 0.021(4) 0.009(4) 0.027(4) C46 0.111(13) 0.092(11) 0.087(10) 0.023(9) 0.011(10) 0.066(10) C47 0.097(7) 0.102(7) 0.165(10) 0.036(7) -0.009(7) 0.026(5) C46A 0.078(10) 0.069(9) 0.076(9) 0.003(7) 0.006(8) 0.012(7) C47A 0.097(7) 0.102(7) 0.165(10) 0.036(7) -0.009(7) 0.026(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 Si1 N1 1.786(3) . ? Si1 C18 1.847(5) . ? Si1 C17 1.854(6) . ? Si1 C19 1.857(6) . ? Si2 N2 1.789(3) . ? Si2 C20 1.854(5) . ? Si2 C21 1.858(4) . ? Si2 C22 1.859(5) . ? Al N2 1.865(3) . ? Al O1 1.875(3) . ? Al N1 1.878(4) . ? Al C16 1.951(5) . ? F1 C29 1.359(5) . ? F2 C30 1.355(5) . ? F3 C31 1.347(5) . ? F4 C32 1.344(5) . ? F5 C33 1.358(5) . ? F6 C35 1.353(5) . ? F7 C36 1.339(5) . ? F8 C37 1.343(5) . ? F9 C38 1.348(5) . ? F10 C39 1.347(5) . ? F11 C41 1.354(5) . ? F12 C42 1.353(5) . ? F13 C43 1.346(5) . ? F14 C44 1.347(5) . ? F15 C45 1.365(5) . ? O1 C26 1.464(5) . ? O1 C23 1.483(5) . ? N1 C1 1.349(5) . ? N2 C3 1.359(5) . ? C1 C2 1.407(5) . ? C1 C4 1.492(6) . ? C2 C3 1.388(6) . ? C3 C10 1.482(5) . ? C4 C9 1.390(6) . ? C4 C5 1.395(6) . ? C5 C6 1.373(6) . ? C6 C7 1.375(7) . ? C7 C8 1.379(7) . ? C8 C9 1.385(6) . ? C10 C15 1.377(6) . ? C10 C11 1.398(6) . ? C11 C12 1.381(6) . ? C12 C13 1.385(7) . ? C13 C14 1.380(7) . ? C14 C15 1.387(6) . ? C23 C24 1.522(6) . ? C24 C25 1.514(6) . ? C25 C26 1.502(6) . ? B C27 1.635(6) . ? B C28 1.641(6) . ? B C34 1.663(6) . ? B C40 1.664(6) . ? C28 C29 1.388(6) . ? C28 C33 1.391(5) . ? C29 C30 1.374(6) . ? C30 C31 1.372(6) . ? C31 C32 1.362(7) . ? C32 C33 1.369(6) . ? C34 C35 1.394(6) . ? C34 C39 1.396(5) . ? C35 C36 1.380(6) . ? C36 C37 1.374(6) . ? C37 C38 1.367(6) . ? C38 C39 1.386(6) . ? C40 C41 1.384(6) . ? C40 C45 1.393(6) . ? C41 C42 1.372(6) . ? C42 C43 1.376(7) . ? C43 C44 1.375(6) . ? C44 C45 1.364(6) . ? O2 C46A 1.346(14) . ? O2 C46A 1.346(14) 2_566 ? O2 C46 1.36(2) . ? O2 C46 1.36(2) 2_566 ? C46 C47 1.36(2) . ? C46A C47A 1.39(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 N1 Si1 C18 107.9(2) . . ? N1 Si1 C17 114.7(2) . . ? C18 Si1 C17 112.3(3) . . ? N1 Si1 C19 105.1(2) . . ? C18 Si1 C19 109.9(3) . . ? C17 Si1 C19 106.7(3) . . ? N2 Si2 C20 105.8(2) . . ? N2 Si2 C21 113.4(2) . . ? C20 Si2 C21 107.3(2) . . ? N2 Si2 C22 108.8(2) . . ? C20 Si2 C22 108.7(3) . . ? C21 Si2 C22 112.5(2) . . ? N2 Al O1 99.88(14) . . ? N2 Al N1 102.57(15) . . ? O1 Al N1 100.02(15) . . ? N2 Al C16 123.2(2) . . ? O1 Al C16 103.4(2) . . ? N1 Al C16 122.9(2) . . ? C26 O1 C23 109.0(3) . . ? C26 O1 Al 121.4(3) . . ? C23 O1 Al 123.4(2) . . ? C1 N1 Si1 127.0(3) . . ? C1 N1 Al 110.5(3) . . ? Si1 N1 Al 122.2(2) . . ? C3 N2 Si2 124.6(3) . . ? C3 N2 Al 111.2(3) . . ? Si2 N2 Al 123.9(2) . . ? N1 C1 C2 124.3(4) . . ? N1 C1 C4 121.1(3) . . ? C2 C1 C4 114.5(3) . . ? C3 C2 C1 128.0(4) . . ? N2 C3 C2 123.6(4) . . ? N2 C3 C10 120.2(3) . . ? C2 C3 C10 116.2(3) . . ? C9 C4 C5 119.4(4) . . ? C9 C4 C1 120.0(4) . . ? C5 C4 C1 120.5(4) . . ? C6 C5 C4 120.2(4) . . ? C5 C6 C7 120.1(4) . . ? C6 C7 C8 120.5(4) . . ? C7 C8 C9 119.9(4) . . ? C8 C9 C4 119.8(4) . . ? C15 C10 C11 119.0(4) . . ? C15 C10 C3 120.6(4) . . ? C11 C10 C3 120.5(3) . . ? C12 C11 C10 120.4(4) . . ? C11 C12 C13 120.1(4) . . ? C14 C13 C12 119.7(4) . . ? C13 C14 C15 120.2(4) . . ? C10 C15 C14 120.6(4) . . ? O1 C23 C24 104.4(3) . . ? C25 C24 C23 103.7(4) . . ? C26 C25 C24 101.9(4) . . ? O1 C26 C25 103.6(3) . . ? C27 B C28 114.7(3) . . ? C27 B C34 110.3(3) . . ? C28 B C34 104.4(3) . . ? C27 B C40 104.3(3) . . ? C28 B C40 112.2(3) . . ? C34 B C40 111.2(3) . . ? C29 C28 C33 111.6(4) . . ? C29 C28 B 126.9(3) . . ? C33 C28 B 121.4(3) . . ? F1 C29 C30 114.5(4) . . ? F1 C29 C28 120.8(3) . . ? C30 C29 C28 124.7(4) . . ? F2 C30 C31 118.6(4) . . ? F2 C30 C29 121.4(4) . . ? C31 C30 C29 120.0(4) . . ? F3 C31 C32 121.0(4) . . ? F3 C31 C30 120.4(4) . . ? C32 C31 C30 118.5(4) . . ? F4 C32 C31 120.0(4) . . ? F4 C32 C33 120.8(4) . . ? C31 C32 C33 119.2(4) . . ? F5 C33 C32 115.8(4) . . ? F5 C33 C28 118.4(3) . . ? C32 C33 C28 125.8(4) . . ? C35 C34 C39 112.3(3) . . ? C35 C34 B 121.0(3) . . ? C39 C34 B 126.6(3) . . ? F6 C35 C36 114.7(3) . . ? F6 C35 C34 120.1(3) . . ? C36 C35 C34 125.2(4) . . ? F7 C36 C37 119.9(4) . . ? F7 C36 C35 121.0(4) . . ? C37 C36 C35 119.2(4) . . ? F8 C37 C38 120.3(4) . . ? F8 C37 C36 120.6(4) . . ? C38 C37 C36 119.1(4) . . ? F9 C38 C37 119.8(4) . . ? F9 C38 C39 120.3(4) . . ? C37 C38 C39 119.9(4) . . ? F10 C39 C38 114.5(3) . . ? F10 C39 C34 121.2(3) . . ? C38 C39 C34 124.3(4) . . ? C41 C40 C45 112.2(4) . . ? C41 C40 B 126.5(4) . . ? C45 C40 B 121.0(3) . . ? F11 C41 C42 115.0(4) . . ? F11 C41 C40 120.3(4) . . ? C42 C41 C40 124.7(4) . . ? F12 C42 C41 121.0(4) . . ? F12 C42 C43 119.0(4) . . ? C41 C42 C43 120.0(4) . . ? F13 C43 C44 120.6(4) . . ? F13 C43 C42 121.2(4) . . ? C44 C43 C42 118.3(4) . . ? F14 C44 C45 121.1(4) . . ? F14 C44 C43 119.6(4) . . ? C45 C44 C43 119.3(4) . . ? C44 C45 F15 115.2(4) . . ? C44 C45 C40 125.5(4) . . ? F15 C45 C40 119.2(4) . . ? C46A O2 C46A 180.000(4) . 2_566 ? C46 O2 C46 180.000(6) . 2_566 ? O2 C46 C47 120.4(12) . . ? O2 C46A C47A 119.8(12) . . ? _refine_diff_density_max 0.356 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.066 #=END data_mfl3 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ; '[AlMe(Et2O)(Me3SiNCPhCHCPhNSiMe3)][B(C6F5)4].0.5(Et2O)' ; _chemical_formula_analytical ? _chemical_formula_sum 'C52 H47 Al B F20 N2 O1.50 Si2' _chemical_formula_weight 1197.89 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.503(5) _cell_length_b 14.557(11) _cell_length_c 15.403(7) _cell_angle_alpha 69.39(5) _cell_angle_beta 88.02(3) _cell_angle_gamma 74.04(5) _cell_volume 2718.1(26) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.464 _exptl_crystal_density_method ? _exptl_crystal_F_000 1222 _exptl_absorpt_coefficient_mu 0.191 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9546 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0798 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.97 _reflns_number_total 9546 _reflns_number_observed 6098 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; There is a molecule of Et2O disordered across an inversion centre for which the C and O atoms were isotropic and H atoms were omitted. Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1022P)^2^+3.7127P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9544 _refine_ls_number_parameters 707 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1159 _refine_ls_R_factor_obs 0.0673 _refine_ls_wR_factor_all 0.2142 _refine_ls_wR_factor_obs 0.1693 _refine_ls_goodness_of_fit_all 1.027 _refine_ls_goodness_of_fit_obs 1.032 _refine_ls_restrained_S_all 1.028 _refine_ls_restrained_S_obs 1.032 _refine_ls_shift/esd_max 0.004 _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 0.07359(11) 0.19772(10) 0.30140(10) 0.0299(3) Uani 1 d . . Si1 Si 0.28345(10) 0.01727(10) 0.38519(9) 0.0296(3) Uani 1 d . . Si2 Si -0.10935(10) 0.14680(11) 0.21676(10) 0.0367(3) Uani 1 d . . O1 O 0.0792(3) 0.3345(2) 0.2538(2) 0.0428(9) Uani 1 d . . N1 N 0.2082(3) 0.1264(3) 0.2912(2) 0.0262(8) Uani 1 d . . N2 N 0.0045(3) 0.1909(3) 0.2013(3) 0.0293(9) Uani 1 d . . C1 C 0.2352(3) 0.1552(3) 0.2025(3) 0.0283(10) Uani 1 d . . C2 C 0.1635(3) 0.2031(3) 0.1248(3) 0.0299(10) Uani 1 d . . H2 H 0.1891(3) 0.2340(3) 0.0668(3) 0.036 Uiso 1 calc R . C3 C 0.0572(3) 0.2100(3) 0.1244(3) 0.0265(10) Uani 1 d . . C4 C 0.3461(4) 0.1387(4) 0.1846(3) 0.0319(11) Uani 1 d . . C5 C 0.4102(4) 0.1641(4) 0.2350(4) 0.0360(11) Uani 1 d . . H5 H 0.3822(4) 0.1937(4) 0.2796(4) 0.043 Uiso 1 calc R . C6 C 0.5132(4) 0.1470(4) 0.2214(4) 0.0498(15) Uani 1 d . . H6 H 0.5561(4) 0.1662(4) 0.2556(4) 0.060 Uiso 1 calc R . C7 C 0.5553(4) 0.1018(5) 0.1577(4) 0.055(2) Uani 1 d . . H7 H 0.6274(4) 0.0874(5) 0.1500(4) 0.066 Uiso 1 calc R . C8 C 0.4919(4) 0.0778(5) 0.1058(4) 0.0515(15) Uani 1 d . . H8 H 0.5203(4) 0.0483(5) 0.0611(4) 0.062 Uiso 1 calc R . C9 C 0.3881(4) 0.0963(4) 0.1181(3) 0.0384(12) Uani 1 d . . H9 H 0.3447(4) 0.0803(4) 0.0816(3) 0.046 Uiso 1 calc R . C10 C 0.0031(3) 0.2442(3) 0.0307(3) 0.0300(10) Uani 1 d . . C11 C -0.0921(4) 0.3185(4) 0.0097(4) 0.0366(11) Uani 1 d . . H11 H -0.1211(4) 0.3475(4) 0.0545(4) 0.044 Uiso 1 calc R . C12 C -0.1447(4) 0.3504(4) -0.0764(4) 0.0418(13) Uani 1 d . . H12 H -0.2099(4) 0.4005(4) -0.0903(4) 0.050 Uiso 1 calc R . C13 C -0.1021(5) 0.3093(4) -0.1411(4) 0.0514(15) Uani 1 d . . H13 H -0.1378(5) 0.3311(4) -0.2001(4) 0.062 Uiso 1 calc R . C14 C -0.0076(5) 0.2364(5) -0.1211(4) 0.054(2) Uani 1 d . . H14 H 0.0216(5) 0.2089(5) -0.1667(4) 0.065 Uiso 1 calc R . C15 C 0.0450(4) 0.2032(4) -0.0357(3) 0.0384(12) Uani 1 d . . H15 H 0.1097(4) 0.1524(4) -0.0223(3) 0.046 Uiso 1 calc R . C16 C 0.3871(4) -0.0690(4) 0.3450(3) 0.0366(11) Uani 1 d . . H16A H 0.3572(4) -0.0895(4) 0.3001(3) 0.055 Uiso 1 calc R . H16B H 0.4210(4) -0.1299(4) 0.3984(3) 0.055 Uiso 1 calc R . H16C H 0.4380(4) -0.0332(4) 0.3153(3) 0.055 Uiso 1 calc R . C17 C 0.3351(5) 0.0588(5) 0.4703(4) 0.053(2) Uani 1 d . . H17A H 0.2785(5) 0.1041(5) 0.4900(4) 0.080 Uiso 1 calc R . H17B H 0.3857(5) 0.0955(5) 0.4415(4) 0.080 Uiso 1 calc R . H17C H 0.3686(5) -0.0013(5) 0.5245(4) 0.080 Uiso 1 calc R . C18 C 0.1894(4) -0.0537(4) 0.4412(4) 0.0448(13) Uani 1 d . . H18A H 0.1617(4) -0.0760(4) 0.3965(4) 0.067 Uiso 1 calc R . H18B H 0.1328(4) -0.0090(4) 0.4617(4) 0.067 Uiso 1 calc R . H18C H 0.2240(4) -0.1137(4) 0.4950(4) 0.067 Uiso 1 calc R . C19 C -0.1428(4) 0.1083(5) 0.1223(4) 0.0494(14) Uani 1 d . . H19A H -0.1577(4) 0.1673(5) 0.0639(4) 0.074 Uiso 1 calc R . H19B H -0.2038(4) 0.0831(5) 0.1370(4) 0.074 Uiso 1 calc R . H19C H -0.0847(4) 0.0540(5) 0.1156(4) 0.074 Uiso 1 calc R . C20 C -0.2160(4) 0.2474(5) 0.2375(5) 0.057(2) Uani 1 d . . H20A H -0.1940(4) 0.2648(5) 0.2882(5) 0.086 Uiso 1 calc R . H20B H -0.2767(4) 0.2220(5) 0.2543(5) 0.086 Uiso 1 calc R . H20C H -0.2335(4) 0.3085(5) 0.1808(5) 0.086 Uiso 1 calc R . C21 C -0.0824(4) 0.0317(5) 0.3243(4) 0.0506(15) Uani 1 d . . H21A H -0.0642(4) 0.0491(5) 0.3764(4) 0.076 Uiso 1 calc R . H21B H -0.0249(4) -0.0219(5) 0.3159(4) 0.076 Uiso 1 calc R . H21C H -0.1440(4) 0.0071(5) 0.3373(4) 0.076 Uiso 1 calc R . C22 C 0.0153(4) 0.1879(4) 0.4202(4) 0.0474(14) Uani 1 d . . H22A H -0.0561(4) 0.2314(4) 0.4097(4) 0.071 Uiso 1 calc R . H22B H 0.0561(4) 0.2105(4) 0.4558(4) 0.071 Uiso 1 calc R . H22C H 0.0165(4) 0.1168(4) 0.4551(4) 0.071 Uiso 1 calc R . C23 C 0.1673(5) 0.3658(5) 0.2727(5) 0.062(2) Uani 1 d . . H23A H 0.2285(5) 0.3052(5) 0.2912(5) 0.074 Uiso 1 calc R . H23B H 0.1814(5) 0.4158(5) 0.2143(5) 0.074 Uiso 1 calc R . C24 C 0.1559(6) 0.4107(8) 0.3440(6) 0.100(3) Uani 1 d . . H24A H 0.2189(6) 0.4290(8) 0.3515(6) 0.149 Uiso 1 calc R . H24B H 0.1442(6) 0.3612(8) 0.4030(6) 0.149 Uiso 1 calc R . H24C H 0.0970(6) 0.4722(8) 0.3259(6) 0.149 Uiso 1 calc R . C25 C -0.0253(6) 0.4171(6) 0.2232(6) 0.086(2) Uani 1 d . . H25A H -0.0805(6) 0.3837(6) 0.2252(6) 0.103 Uiso 1 calc R . H25B H -0.0402(6) 0.4536(6) 0.2677(6) 0.103 Uiso 1 calc R . C26 C -0.0269(8) 0.4860(7) 0.1362(9) 0.145(5) Uani 1 d . . H26A H -0.0947(8) 0.5368(7) 0.1200(9) 0.217 Uiso 1 calc R . H26B H -0.0137(8) 0.4505(7) 0.0916(9) 0.217 Uiso 1 calc R . H26C H 0.0266(8) 0.5205(7) 0.1342(9) 0.217 Uiso 1 calc R . B B 0.5076(4) 0.6592(4) 0.2220(4) 0.0298(12) Uani 1 d . . C27 C 0.5807(3) 0.7201(4) 0.2496(3) 0.0318(11) Uani 1 d . . C28 C 0.5863(4) 0.7188(4) 0.3394(4) 0.0365(11) Uani 1 d . . C29 C 0.6404(4) 0.7702(4) 0.3697(4) 0.0451(13) Uani 1 d . . C30 C 0.6932(4) 0.8292(4) 0.3071(5) 0.0497(15) Uani 1 d . . C31 C 0.6903(4) 0.8348(4) 0.2167(4) 0.0446(13) Uani 1 d . . C32 C 0.6346(4) 0.7818(4) 0.1900(4) 0.0373(12) Uani 1 d . . C33 C 0.5319(3) 0.6433(3) 0.1211(3) 0.0296(10) Uani 1 d . . C34 C 0.6329(4) 0.6023(4) 0.1027(3) 0.0367(12) Uani 1 d . . C35 C 0.6607(4) 0.5816(4) 0.0235(4) 0.0432(13) Uani 1 d . . C36 C 0.5859(4) 0.5970(4) -0.0418(4) 0.0438(13) Uani 1 d . . C37 C 0.4853(4) 0.6340(4) -0.0270(3) 0.0389(12) Uani 1 d . . C38 C 0.4604(4) 0.6564(4) 0.0525(3) 0.0344(11) Uani 1 d . . C39 C 0.5288(4) 0.5389(4) 0.2923(3) 0.0310(10) Uani 1 d . . C40 C 0.6181(4) 0.4786(4) 0.3476(3) 0.0348(11) Uani 1 d . . C41 C 0.6379(4) 0.3731(4) 0.3954(3) 0.0404(12) Uani 1 d . . C42 C 0.5666(4) 0.3257(4) 0.3874(3) 0.0415(13) Uani 1 d . . C43 C 0.4764(4) 0.3823(4) 0.3346(3) 0.0364(12) Uani 1 d . . C44 C 0.4602(4) 0.4847(4) 0.2894(3) 0.0318(11) Uani 1 d . . C45 C 0.3900(4) 0.7323(3) 0.2226(3) 0.0322(11) Uani 1 d . . C46 C 0.3216(4) 0.7134(4) 0.2910(4) 0.0364(12) Uani 1 d . . C47 C 0.2240(4) 0.7798(5) 0.2867(4) 0.0483(15) Uani 1 d . . C48 C 0.1917(4) 0.8680(5) 0.2115(5) 0.051(2) Uani 1 d . . C49 C 0.2558(4) 0.8915(4) 0.1424(4) 0.0472(14) Uani 1 d . . C50 C 0.3532(4) 0.8254(4) 0.1510(4) 0.0372(12) Uani 1 d . . F1 F 0.5340(2) 0.6643(2) 0.4046(2) 0.0448(7) Uani 1 d . . F2 F 0.6427(3) 0.7624(3) 0.4590(2) 0.0662(10) Uani 1 d . . F3 F 0.7465(3) 0.8817(3) 0.3342(3) 0.0744(11) Uani 1 d . . F4 F 0.7412(3) 0.8934(3) 0.1542(3) 0.0587(9) Uani 1 d . . F5 F 0.6364(2) 0.7944(2) 0.0989(2) 0.0450(7) Uani 1 d . . F6 F 0.7109(2) 0.5816(2) 0.1655(2) 0.0495(8) Uani 1 d . . F7 F 0.7611(2) 0.5430(3) 0.0112(2) 0.0636(10) Uani 1 d . . F8 F 0.6125(3) 0.5758(3) -0.1190(2) 0.0606(10) Uani 1 d . . F9 F 0.4103(3) 0.6495(2) -0.0904(2) 0.0554(9) Uani 1 d . . F10 F 0.3580(2) 0.6930(2) 0.0592(2) 0.0419(7) Uani 1 d . . F11 F 0.6946(2) 0.5185(2) 0.3577(2) 0.0468(8) Uani 1 d . . F12 F 0.7282(3) 0.3200(2) 0.4456(2) 0.0595(9) Uani 1 d . . F13 F 0.5860(3) 0.2232(2) 0.4307(2) 0.0613(9) Uani 1 d . . F14 F 0.4059(2) 0.3338(2) 0.3287(2) 0.0496(8) Uani 1 d . . F15 F 0.3693(2) 0.5343(2) 0.2364(2) 0.0372(7) Uani 1 d . . F16 F 0.3461(2) 0.6284(2) 0.3679(2) 0.0485(8) Uani 1 d . . F17 F 0.1612(3) 0.7551(3) 0.3557(3) 0.0698(11) Uani 1 d . . F18 F 0.0966(2) 0.9312(3) 0.2057(3) 0.0770(12) Uani 1 d . . F19 F 0.2251(3) 0.9779(2) 0.0669(3) 0.0647(10) Uani 1 d . . F20 F 0.4143(2) 0.8548(2) 0.0807(2) 0.0466(8) Uani 1 d . . O2 O 0.0000 0.5000 0.5000 0.188(5) Uiso 1 d S . C51 C 0.0957(12) 0.4409(12) 0.5738(11) 0.077(4) Uiso 0.50 d P . C52 C 0.0420(10) 0.3446(10) 0.6097(9) 0.145(4) Uiso 1 d . . C51A C 0.0542(14) 0.5804(14) 0.4737(13) 0.095(5) Uiso 0.50 d P . 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 0.0280(7) 0.0287(7) 0.0324(8) -0.0119(6) 0.0037(6) -0.0056(6) Si1 0.0311(7) 0.0289(7) 0.0289(7) -0.0128(5) -0.0004(5) -0.0050(5) Si2 0.0236(7) 0.0441(8) 0.0435(8) -0.0157(7) 0.0048(6) -0.0115(6) O1 0.051(2) 0.027(2) 0.049(2) -0.016(2) -0.003(2) -0.006(2) N1 0.026(2) 0.023(2) 0.030(2) -0.009(2) 0.002(2) -0.009(2) N2 0.025(2) 0.027(2) 0.034(2) -0.011(2) 0.002(2) -0.005(2) C1 0.030(2) 0.030(2) 0.033(3) -0.015(2) 0.005(2) -0.015(2) C2 0.032(3) 0.028(2) 0.028(2) -0.003(2) 0.002(2) -0.015(2) C3 0.028(2) 0.018(2) 0.033(2) -0.009(2) 0.002(2) -0.006(2) C4 0.030(3) 0.032(3) 0.033(3) -0.006(2) 0.006(2) -0.015(2) C5 0.030(3) 0.030(3) 0.051(3) -0.017(2) 0.003(2) -0.009(2) C6 0.030(3) 0.045(3) 0.073(4) -0.014(3) -0.003(3) -0.018(2) C7 0.028(3) 0.060(4) 0.074(4) -0.020(3) 0.017(3) -0.017(3) C8 0.041(3) 0.067(4) 0.050(3) -0.024(3) 0.019(3) -0.017(3) C9 0.030(3) 0.050(3) 0.038(3) -0.015(2) 0.009(2) -0.017(2) C10 0.028(2) 0.029(2) 0.031(2) -0.004(2) -0.003(2) -0.013(2) C11 0.034(3) 0.030(3) 0.045(3) -0.013(2) -0.003(2) -0.008(2) C12 0.034(3) 0.031(3) 0.055(3) -0.008(2) -0.013(2) -0.011(2) C13 0.058(4) 0.045(3) 0.051(3) -0.014(3) -0.022(3) -0.016(3) C14 0.066(4) 0.054(4) 0.045(3) -0.023(3) -0.006(3) -0.013(3) C15 0.040(3) 0.037(3) 0.035(3) -0.014(2) -0.001(2) -0.003(2) C16 0.037(3) 0.032(3) 0.038(3) -0.013(2) 0.006(2) -0.005(2) C17 0.068(4) 0.054(4) 0.038(3) -0.021(3) -0.013(3) -0.009(3) C18 0.044(3) 0.034(3) 0.046(3) -0.006(2) 0.010(3) -0.007(2) C19 0.043(3) 0.056(4) 0.056(4) -0.016(3) -0.003(3) -0.028(3) C20 0.024(3) 0.078(4) 0.074(4) -0.036(4) 0.010(3) -0.008(3) C21 0.043(3) 0.062(4) 0.047(3) -0.011(3) 0.010(3) -0.029(3) C22 0.046(3) 0.047(3) 0.044(3) -0.020(3) 0.009(3) 0.000(3) C23 0.056(4) 0.056(4) 0.100(5) -0.050(4) 0.031(4) -0.032(3) C24 0.070(5) 0.165(9) 0.113(7) -0.101(7) 0.015(5) -0.044(6) C25 0.085(6) 0.071(5) 0.116(7) -0.038(5) -0.005(5) -0.035(4) C26 0.132(9) 0.081(7) 0.201(12) 0.006(7) -0.065(9) -0.063(7) B 0.025(3) 0.033(3) 0.034(3) -0.017(2) -0.001(2) -0.006(2) C27 0.025(2) 0.032(3) 0.040(3) -0.019(2) -0.003(2) -0.001(2) C28 0.034(3) 0.038(3) 0.043(3) -0.022(2) 0.005(2) -0.009(2) C29 0.047(3) 0.055(3) 0.053(3) -0.040(3) 0.004(3) -0.019(3) C30 0.041(3) 0.051(3) 0.078(4) -0.043(3) 0.002(3) -0.019(3) C31 0.039(3) 0.043(3) 0.063(4) -0.027(3) 0.011(3) -0.019(3) C32 0.032(3) 0.042(3) 0.043(3) -0.022(2) 0.000(2) -0.008(2) C33 0.029(2) 0.025(2) 0.035(3) -0.011(2) -0.003(2) -0.006(2) C34 0.031(3) 0.040(3) 0.041(3) -0.021(2) -0.006(2) -0.003(2) C35 0.040(3) 0.039(3) 0.049(3) -0.023(3) 0.002(2) 0.000(2) C36 0.058(4) 0.036(3) 0.040(3) -0.026(2) 0.000(3) 0.001(3) C37 0.050(3) 0.029(3) 0.038(3) -0.013(2) -0.015(2) -0.008(2) C38 0.037(3) 0.030(3) 0.037(3) -0.012(2) -0.004(2) -0.010(2) C39 0.032(3) 0.031(3) 0.031(3) -0.018(2) -0.002(2) -0.003(2) C40 0.038(3) 0.034(3) 0.035(3) -0.017(2) -0.005(2) -0.008(2) C41 0.043(3) 0.036(3) 0.034(3) -0.012(2) -0.012(2) 0.003(2) C42 0.061(4) 0.023(3) 0.034(3) -0.004(2) 0.000(3) -0.010(2) C43 0.047(3) 0.034(3) 0.038(3) -0.022(2) 0.003(2) -0.016(2) C44 0.037(3) 0.031(3) 0.028(2) -0.017(2) -0.003(2) -0.001(2) C45 0.026(2) 0.029(3) 0.049(3) -0.023(2) 0.001(2) -0.007(2) C46 0.038(3) 0.034(3) 0.047(3) -0.027(2) 0.003(2) -0.010(2) C47 0.034(3) 0.062(4) 0.074(4) -0.050(4) 0.019(3) -0.020(3) C48 0.029(3) 0.048(3) 0.083(5) -0.040(3) -0.007(3) 0.001(3) C49 0.035(3) 0.031(3) 0.078(4) -0.026(3) -0.009(3) -0.003(2) C50 0.033(3) 0.031(3) 0.051(3) -0.020(2) 0.000(2) -0.006(2) F1 0.053(2) 0.050(2) 0.043(2) -0.0257(15) 0.0070(14) -0.022(2) F2 0.081(3) 0.090(3) 0.059(2) -0.053(2) 0.007(2) -0.039(2) F3 0.077(3) 0.094(3) 0.099(3) -0.067(2) 0.014(2) -0.055(2) F4 0.053(2) 0.063(2) 0.083(2) -0.040(2) 0.024(2) -0.036(2) F5 0.048(2) 0.053(2) 0.040(2) -0.0198(14) 0.0069(14) -0.0214(15) F6 0.029(2) 0.066(2) 0.054(2) -0.035(2) -0.0107(14) 0.0059(14) F7 0.044(2) 0.078(2) 0.070(2) -0.046(2) 0.007(2) 0.006(2) F8 0.088(3) 0.057(2) 0.043(2) -0.035(2) 0.004(2) -0.008(2) F9 0.068(2) 0.054(2) 0.045(2) -0.018(2) -0.024(2) -0.014(2) F10 0.029(2) 0.048(2) 0.047(2) -0.0184(14) -0.0081(13) -0.0070(13) F11 0.038(2) 0.041(2) 0.061(2) -0.0194(15) -0.0168(14) -0.0062(14) F12 0.058(2) 0.044(2) 0.060(2) -0.012(2) -0.024(2) 0.006(2) F13 0.085(3) 0.029(2) 0.055(2) -0.0037(15) -0.006(2) -0.006(2) F14 0.062(2) 0.038(2) 0.057(2) -0.0172(15) 0.001(2) -0.026(2) F15 0.036(2) 0.0345(15) 0.043(2) -0.0165(13) -0.0055(13) -0.0089(12) F16 0.054(2) 0.048(2) 0.050(2) -0.025(2) 0.0168(15) -0.0172(15) F17 0.048(2) 0.082(3) 0.103(3) -0.058(2) 0.035(2) -0.025(2) F18 0.032(2) 0.073(3) 0.134(4) -0.062(3) 0.000(2) 0.009(2) F19 0.050(2) 0.036(2) 0.095(3) -0.022(2) -0.021(2) 0.010(2) F20 0.045(2) 0.033(2) 0.056(2) -0.0107(14) 0.0025(15) -0.0069(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Al N1 1.861(4) . ? Al N2 1.875(4) . ? Al O1 1.887(4) . ? Al C22 1.941(5) . ? Si1 N1 1.802(4) . ? Si1 C17 1.851(5) . ? Si1 C16 1.855(5) . ? Si1 C18 1.855(5) . ? Si2 N2 1.800(4) . ? Si2 C19 1.843(6) . ? Si2 C21 1.853(6) . ? Si2 C20 1.860(6) . ? O1 C23 1.456(7) . ? O1 C25 1.541(9) . ? N1 C1 1.351(6) . ? N2 C3 1.344(6) . ? C1 C2 1.406(6) . ? C1 C4 1.482(6) . ? C2 C3 1.410(6) . ? C3 C10 1.494(6) . ? C4 C5 1.382(7) . ? C4 C9 1.401(7) . ? C5 C6 1.367(7) . ? C6 C7 1.389(9) . ? C7 C8 1.379(8) . ? C8 C9 1.374(7) . ? C10 C15 1.388(7) . ? C10 C11 1.395(7) . ? C11 C12 1.389(7) . ? C12 C13 1.369(8) . ? C13 C14 1.379(8) . ? C14 C15 1.376(7) . ? C23 C24 1.448(9) . ? C25 C26 1.359(13) . ? B C27 1.647(7) . ? B C45 1.652(7) . ? B C39 1.654(7) . ? B C33 1.659(7) . ? C27 C28 1.382(7) . ? C27 C32 1.383(7) . ? C28 F1 1.355(6) . ? C28 C29 1.371(7) . ? C29 F2 1.341(6) . ? C29 C30 1.372(8) . ? C30 F3 1.351(6) . ? C30 C31 1.368(8) . ? C31 F4 1.352(6) . ? C31 C32 1.375(7) . ? C32 F5 1.349(6) . ? C33 C38 1.384(6) . ? C33 C34 1.394(7) . ? C34 F6 1.352(5) . ? C34 C35 1.372(7) . ? C35 F7 1.352(6) . ? C35 C36 1.368(7) . ? C36 F8 1.344(6) . ? C36 C37 1.360(8) . ? C37 F9 1.348(6) . ? C37 C38 1.382(7) . ? C38 F10 1.353(6) . ? C39 C44 1.383(7) . ? C39 C40 1.383(7) . ? C40 F11 1.353(6) . ? C40 C41 1.402(7) . ? C41 F12 1.344(6) . ? C41 C42 1.360(8) . ? C42 F13 1.354(6) . ? C42 C43 1.367(7) . ? C43 F14 1.353(6) . ? C43 C44 1.363(7) . ? C44 F15 1.364(5) . ? C45 C46 1.380(7) . ? C45 C50 1.383(7) . ? C46 F16 1.347(6) . ? C46 C47 1.392(7) . ? C47 F17 1.347(6) . ? C47 C48 1.364(9) . ? C48 F18 1.344(6) . ? C48 C49 1.356(9) . ? C49 F19 1.350(7) . ? C49 C50 1.378(7) . ? C50 F20 1.359(6) . ? O2 C51A 1.48(2) . ? O2 C51A 1.48(2) 2_566 ? O2 C51 1.58(2) . ? O2 C51 1.58(2) 2_566 ? C51 C52 1.67(2) . ? C51 C51A 2.01(2) . ? C52 C51A 1.70(2) 2_566 ? C51A C52 1.70(2) 2_566 ? 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 N1 Al N2 100.8(2) . . ? N1 Al O1 102.0(2) . . ? N2 Al O1 101.2(2) . . ? N1 Al C22 122.8(2) . . ? N2 Al C22 123.7(2) . . ? O1 Al C22 102.3(2) . . ? N1 Si1 C17 110.5(2) . . ? N1 Si1 C16 113.1(2) . . ? C17 Si1 C16 111.6(3) . . ? N1 Si1 C18 104.3(2) . . ? C17 Si1 C18 109.0(3) . . ? C16 Si1 C18 107.9(2) . . ? N2 Si2 C19 114.6(2) . . ? N2 Si2 C21 106.6(2) . . ? C19 Si2 C21 107.0(3) . . ? N2 Si2 C20 107.5(2) . . ? C19 Si2 C20 113.0(3) . . ? C21 Si2 C20 107.8(3) . . ? C23 O1 C25 117.6(4) . . ? C23 O1 Al 123.1(4) . . ? C25 O1 Al 116.1(4) . . ? C1 N1 Si1 124.2(3) . . ? C1 N1 Al 111.9(3) . . ? Si1 N1 Al 123.1(2) . . ? C3 N2 Si2 126.5(3) . . ? C3 N2 Al 111.7(3) . . ? Si2 N2 Al 121.3(2) . . ? N1 C1 C2 123.6(4) . . ? N1 C1 C4 119.1(4) . . ? C2 C1 C4 117.3(4) . . ? C1 C2 C3 126.6(4) . . ? N2 C3 C2 124.0(4) . . ? N2 C3 C10 120.4(4) . . ? C2 C3 C10 115.6(4) . . ? C5 C4 C9 119.0(4) . . ? C5 C4 C1 119.8(4) . . ? C9 C4 C1 121.2(4) . . ? C6 C5 C4 120.8(5) . . ? C5 C6 C7 120.1(5) . . ? C8 C7 C6 119.6(5) . . ? C9 C8 C7 120.4(5) . . ? C8 C9 C4 119.9(5) . . ? C15 C10 C11 119.2(4) . . ? C15 C10 C3 121.6(4) . . ? C11 C10 C3 119.2(4) . . ? C12 C11 C10 120.3(5) . . ? C13 C12 C11 119.7(5) . . ? C12 C13 C14 120.3(5) . . ? C15 C14 C13 120.7(6) . . ? C14 C15 C10 119.8(5) . . ? C24 C23 O1 115.7(5) . . ? C26 C25 O1 112.5(8) . . ? C27 B C45 102.4(4) . . ? C27 B C39 113.8(4) . . ? C45 B C39 114.2(4) . . ? C27 B C33 113.5(4) . . ? C45 B C33 113.2(4) . . ? C39 B C33 100.3(4) . . ? C28 C27 C32 112.8(4) . . ? C28 C27 B 119.9(4) . . ? C32 C27 B 127.1(4) . . ? F1 C28 C29 115.4(4) . . ? F1 C28 C27 119.2(4) . . ? C29 C28 C27 125.4(5) . . ? F2 C29 C28 120.8(5) . . ? F2 C29 C30 120.3(5) . . ? C28 C29 C30 118.9(5) . . ? F3 C30 C31 120.5(5) . . ? F3 C30 C29 120.6(5) . . ? C31 C30 C29 118.9(5) . . ? F4 C31 C30 119.5(5) . . ? F4 C31 C32 120.7(5) . . ? C30 C31 C32 119.8(5) . . ? F5 C32 C31 114.4(5) . . ? F5 C32 C27 121.4(4) . . ? C31 C32 C27 124.2(5) . . ? C38 C33 C34 112.5(4) . . ? C38 C33 B 127.0(4) . . ? C34 C33 B 120.2(4) . . ? F6 C34 C35 116.2(4) . . ? F6 C34 C33 119.1(4) . . ? C35 C34 C33 124.7(5) . . ? F7 C35 C36 119.9(5) . . ? F7 C35 C34 120.5(5) . . ? C36 C35 C34 119.6(5) . . ? F8 C36 C37 121.2(5) . . ? F8 C36 C35 119.9(5) . . ? C37 C36 C35 118.8(5) . . ? F9 C37 C36 119.8(5) . . ? F9 C37 C38 120.3(5) . . ? C36 C37 C38 119.9(5) . . ? F10 C38 C37 114.4(4) . . ? F10 C38 C33 121.2(4) . . ? C37 C38 C33 124.4(5) . . ? C44 C39 C40 113.2(4) . . ? C44 C39 B 120.0(4) . . ? C40 C39 B 126.1(4) . . ? F11 C40 C39 121.4(4) . . ? F11 C40 C41 115.0(4) . . ? C39 C40 C41 123.6(5) . . ? F12 C41 C42 121.2(5) . . ? F12 C41 C40 119.5(5) . . ? C42 C41 C40 119.2(5) . . ? F13 C42 C41 120.0(5) . . ? F13 C42 C43 120.7(5) . . ? C41 C42 C43 119.3(4) . . ? F14 C43 C44 122.1(5) . . ? F14 C43 C42 118.4(4) . . ? C44 C43 C42 119.5(5) . . ? C43 C44 F15 115.4(4) . . ? C43 C44 C39 125.1(5) . . ? F15 C44 C39 119.5(4) . . ? C46 C45 C50 113.3(4) . . ? C46 C45 B 126.8(4) . . ? C50 C45 B 119.8(4) . . ? F16 C46 C45 121.6(4) . . ? F16 C46 C47 115.1(5) . . ? C45 C46 C47 123.3(5) . . ? F17 C47 C48 120.6(5) . . ? F17 C47 C46 119.7(6) . . ? C48 C47 C46 119.7(5) . . ? F18 C48 C49 120.1(6) . . ? F18 C48 C47 120.0(6) . . ? C49 C48 C47 119.8(5) . . ? F19 C49 C48 120.8(5) . . ? F19 C49 C50 120.6(5) . . ? C48 C49 C50 118.6(5) . . ? F20 C50 C49 115.6(5) . . ? F20 C50 C45 119.2(4) . . ? C49 C50 C45 125.2(5) . . ? C51A O2 C51A 180.000(3) . 2_566 ? C51A O2 C51 82.1(9) . . ? C51A O2 C51 97.9(9) 2_566 . ? C51A O2 C51 97.9(9) . 2_566 ? C51A O2 C51 82.1(9) 2_566 2_566 ? C51 O2 C51 180.000(3) . 2_566 ? O2 C51 C52 86.5(9) . . ? O2 C51 C51A 46.8(7) . . ? C52 C51 C51A 133.2(11) . . ? C51 C52 C51A 86.7(10) . 2_566 ? O2 C51A C52 88.8(10) . 2_566 ? O2 C51A C51 51.2(7) . . ? C52 C51A C51 140.0(13) 2_566 . ? _refine_diff_density_max 1.208 _refine_diff_density_min -0.440 _refine_diff_density_rms 0.087 #=END