Supplementary Material for Chemical Communications This journal is © The Royal Society of Chemistry 2003 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Alan Cowley' 'Jamie N. Jones' 'Charles L. B. Macdonald' 'Jeffrey M. Pietryga' 'Robert J. Wiacek' _publ_contact_author_name 'Prof Alan Cowley' _publ_contact_author_address ; Chemistry & Biochemistry University of Texas at Austin 1 University Station A5300 Austin Texas 78712-0165 UNITED STATES OF AMERICA ; _publ_contact_author_email COWLEY@MAIL.UTEXAS.EDU _publ_requested_journal 'Chemical Communications' _publ_section_title ; The contrasting behaviour of bridged amido-cyclopentadienyl (constrained geometry) group 15 chlorides and cations derived therefrom ; data_pca21 _database_code_CSD 200128 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido phosphium aluminum tetrachloride ; _chemical_name_common '(CGC)phosphium aluminum tetrachloride' _chemical_melting_point ? _chemical_formula_moiety '[C15 H27 N P Si][Al Cl4]' _chemical_formula_sum 'C13.33 H24 Al0.89 Cl3.56 N0.89 P0.89 Si0.89' _chemical_formula_weight 399.30 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.064(4) _cell_length_b 8.3447(17) _cell_length_c 30.103(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4537.6(16) _cell_formula_units_Z 9 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 27.45 _exptl_crystal_description prism _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.682 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8756 _exptl_absorpt_correction_T_max 0.8756 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9381 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9381 _reflns_number_gt 8336 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1150P)^2^+9.5945P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.52(13) _refine_ls_number_reflns 9381 _refine_ls_number_parameters 479 _refine_ls_number_restraints 91 _refine_ls_R_factor_all 0.0862 _refine_ls_R_factor_gt 0.0767 _refine_ls_wR_factor_ref 0.2060 _refine_ls_wR_factor_gt 0.1960 _refine_ls_goodness_of_fit_ref 1.082 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.611 _refine_ls_shift/su_mean 0.108 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 C10 C 0.6933(4) 0.0005(7) 0.3812(3) 0.039(2) Uani 1 1 d . . . H10A H 0.6884 -0.0456 0.4110 0.059 Uiso 1 1 calc R . . H10B H 0.6995 0.1168 0.3835 0.059 Uiso 1 1 calc R . . H10C H 0.7366 -0.0460 0.3664 0.059 Uiso 1 1 calc R . . C11 C 0.6028(4) -0.2547(8) 0.3291(3) 0.0442(17) Uani 1 1 d . . . H11A H 0.6508 -0.2873 0.3169 0.066 Uiso 1 1 calc R . . H11B H 0.5648 -0.2642 0.3061 0.066 Uiso 1 1 calc R . . H11C H 0.5900 -0.3241 0.3542 0.066 Uiso 1 1 calc R . . C26 C 0.1263(4) 1.7707(7) 0.0756(3) 0.0364(14) Uani 1 1 d . . . H26A H 0.1408 1.8511 0.0977 0.055 Uiso 1 1 calc R . . H26B H 0.0723 1.7711 0.0723 0.055 Uiso 1 1 calc R . . H26C H 0.1494 1.7962 0.0470 0.055 Uiso 1 1 calc R . . C30 C 0.1494(4) 1.2439(8) 0.0629(3) 0.0410(15) Uani 1 1 d . . . H30A H 0.1912 1.2335 0.0835 0.062 Uiso 1 1 calc R . . H30B H 0.1574 1.1737 0.0372 0.062 Uiso 1 1 calc R . . H30C H 0.1035 1.2132 0.0780 0.062 Uiso 1 1 calc R . . C31 C 0.0583(5) 1.4908(8) 0.0104(3) 0.0364(19) Uani 1 1 d . . . H31A H 0.0144 1.4765 0.0291 0.055 Uiso 1 1 calc R . . H31B H 0.0568 1.4140 -0.0143 0.055 Uiso 1 1 calc R . . H31C H 0.0590 1.6001 -0.0015 0.055 Uiso 1 1 calc R . . Cl10 Cl 0.3433(3) -0.2566(4) 0.3247(2) 0.0514(11) Uani 0.83 1 d PD . . Cl15 Cl 0.3599(12) -0.2454(11) 0.3260(9) 0.035(4) Uani 0.17 1 d PDU . . Cl16 Cl 0.4600(8) -0.5673(19) 0.3676(5) 0.019(3) Uiso 0.17 1 d PD . . Cl17 Cl 0.2916(7) -0.632(2) 0.3152(8) 0.065(6) Uani 0.17 1 d PDU . . Cl22 Cl 0.40376(15) 1.2464(2) 0.06385(9) 0.0384(5) Uani 0.78 1 d PD . . Cl23 Cl 0.29220(14) 1.0263(3) 0.13508(7) 0.0567(5) Uani 1 1 d . . . Cl25 Cl 0.4337(8) 0.8144(16) 0.0786(5) 0.186(14) Uani 0.22 1 d PDU . . Cl26 Cl 0.4233(9) 1.2280(14) 0.0732(6) 0.211(17) Uani 0.22 1 d PDU . . Cl27 Cl 0.2935(5) 0.996(2) 0.0189(3) 0.085(6) Uani 0.22 1 d PDU . . C21 C 0.1523(3) 1.6015(7) 0.0913(2) 0.0315(12) Uani 1 1 d . . . C22 C 0.1228(4) 1.5546(8) 0.1355(2) 0.0354(13) Uani 1 1 d . . . C23 C 0.1802(5) 1.5201(9) 0.1650(3) 0.0381(16) Uani 1 1 d . . . C24 C 0.2494(4) 1.5439(9) 0.1410(2) 0.0387(14) Uani 1 1 d . . . C25 C 0.2346(3) 1.5885(7) 0.0973(2) 0.0332(12) Uani 1 1 d . . . C27 C 0.0428(5) 1.5544(10) 0.1462(3) 0.0512(18) Uani 1 1 d . . . H27A H 0.0327 1.6348 0.1691 0.077 Uiso 1 1 calc R . . H27B H 0.0284 1.4483 0.1571 0.077 Uiso 1 1 calc R . . H27C H 0.0143 1.5800 0.1194 0.077 Uiso 1 1 calc R . . C28 C 0.1748(7) 1.4678(14) 0.2101(3) 0.064(2) Uani 1 1 d . . . H28A H 0.2246 1.4573 0.2227 0.096 Uiso 1 1 calc R . . H28B H 0.1496 1.3639 0.2112 0.096 Uiso 1 1 calc R . . H28C H 0.1465 1.5465 0.2273 0.096 Uiso 1 1 calc R . . C29 C 0.3254(5) 1.5091(9) 0.1593(3) 0.045(2) Uani 1 1 d . . . H29A H 0.3214 1.4803 0.1908 0.067 Uiso 1 1 calc R . . H29B H 0.3566 1.6044 0.1562 0.067 Uiso 1 1 calc R . . H29C H 0.3476 1.4199 0.1428 0.067 Uiso 1 1 calc R . . C32 C 0.2496(5) 1.4990(5) -0.0328(2) 0.0249(14) Uani 1 1 d . . . C33 C 0.2061(5) 1.6340(9) -0.0563(3) 0.0470(18) Uani 1 1 d . . . H33A H 0.2236 1.7382 -0.0456 0.071 Uiso 1 1 calc R . . H33B H 0.1533 1.6227 -0.0496 0.071 Uiso 1 1 calc R . . H33C H 0.2138 1.6266 -0.0884 0.071 Uiso 1 1 calc R . . C34 C 0.2177(5) 1.3378(9) -0.0479(3) 0.055(2) Uani 1 1 d . . . H34A H 0.2489 1.2507 -0.0366 0.082 Uiso 1 1 calc R . . H34B H 0.2164 1.3338 -0.0804 0.082 Uiso 1 1 calc R . . H34C H 0.1674 1.3258 -0.0362 0.082 Uiso 1 1 calc R . . C35 C 0.3267(5) 1.5159(10) -0.0408(3) 0.044(2) Uani 1 1 d . . . H35A H 0.3360 1.5138 -0.0729 0.067 Uiso 1 1 calc R . . H35B H 0.3534 1.4274 -0.0266 0.067 Uiso 1 1 calc R . . H35C H 0.3439 1.6180 -0.0285 0.067 Uiso 1 1 calc R . . N2 N 0.2273(3) 1.5109(5) 0.0183(2) 0.0234(12) Uani 1 1 d . . . Al2 Al 0.35914(10) 1.0140(2) 0.07785(8) 0.0279(4) Uani 1 1 d D . . Si2 Si 0.14224(9) 1.4565(2) 0.04367(5) 0.0292(3) Uani 1 1 d . . . P2 P 0.29244(8) 1.57128(18) 0.05194(5) 0.0303(3) Uani 1 1 d . . . Cl20 Cl 0.44561(15) 0.8462(3) 0.08654(12) 0.0500(8) Uani 0.78 1 d PD . . Cl21 Cl 0.29392(18) 0.9446(2) 0.02160(10) 0.0283(5) Uani 0.78 1 d PD . . C1 C 0.5976(3) 0.1003(7) 0.3001(2) 0.0314(11) Uani 1 1 d . . . C2 C 0.6273(4) 0.0564(9) 0.2557(2) 0.0387(14) Uani 1 1 d . . . C3 C 0.5696(5) 0.0174(9) 0.2288(3) 0.0378(17) Uani 1 1 d . . . C4 C 0.5004(4) 0.0352(10) 0.2507(2) 0.0389(14) Uani 1 1 d . . . C5 C 0.5149(3) 0.0840(7) 0.29413(19) 0.0312(12) Uani 1 1 d . . . C6 C 0.6210(4) 0.2709(8) 0.3163(2) 0.0371(14) Uani 1 1 d . . . H6A H 0.6019 0.2889 0.3464 0.056 Uiso 1 1 calc R . . H6B H 0.6006 0.3519 0.2962 0.056 Uiso 1 1 calc R . . H6C H 0.6751 0.2789 0.3166 0.056 Uiso 1 1 calc R . . C7 C 0.7085(4) 0.0508(12) 0.2453(3) 0.055(2) Uani 1 1 d . . . H7A H 0.7310 -0.0412 0.2604 0.082 Uiso 1 1 calc R . . H7B H 0.7321 0.1498 0.2556 0.082 Uiso 1 1 calc R . . H7C H 0.7154 0.0400 0.2131 0.082 Uiso 1 1 calc R . . C8 C 0.5761(6) -0.0279(13) 0.1797(3) 0.058(2) Uani 1 1 d . . . H8A H 0.6284 -0.0429 0.1720 0.087 Uiso 1 1 calc R . . H8B H 0.5551 0.0579 0.1614 0.087 Uiso 1 1 calc R . . H8C H 0.5490 -0.1277 0.1743 0.087 Uiso 1 1 calc R . . C9 C 0.4274(5) 0.0043(11) 0.2298(3) 0.052(3) Uani 1 1 d . . . H9A H 0.4254 -0.1070 0.2195 0.079 Uiso 1 1 calc R . . H9B H 0.4207 0.0768 0.2045 0.079 Uiso 1 1 calc R . . H9C H 0.3881 0.0227 0.2516 0.079 Uiso 1 1 calc R . . C12 C 0.5073(5) -0.0083(8) 0.4231(3) 0.0372(18) Uani 1 1 d . . . C13 C 0.5412(4) 0.1313(9) 0.4481(2) 0.0425(16) Uani 1 1 d . . . H13A H 0.5951 0.1300 0.4443 0.064 Uiso 1 1 calc R . . H13B H 0.5292 0.1221 0.4798 0.064 Uiso 1 1 calc R . . H13C H 0.5213 0.2321 0.4365 0.064 Uiso 1 1 calc R . . C14 C 0.5324(5) -0.1708(9) 0.4399(3) 0.051(2) Uani 1 1 d . . . H14A H 0.5861 -0.1807 0.4362 0.077 Uiso 1 1 calc R . . H14B H 0.5075 -0.2554 0.4229 0.077 Uiso 1 1 calc R . . H14C H 0.5198 -0.1812 0.4714 0.077 Uiso 1 1 calc R . . C15 C 0.4175(6) -0.0013(8) 0.4308(3) 0.047(2) Uani 1 1 d . . . H15A H 0.4065 -0.0191 0.4623 0.071 Uiso 1 1 calc R . . H15B H 0.3936 -0.0847 0.4130 0.071 Uiso 1 1 calc R . . H15C H 0.3988 0.1040 0.4218 0.071 Uiso 1 1 calc R . . N1 N 0.5202(3) 0.0098(5) 0.3768(2) 0.0259(12) Uani 1 1 d . . . Al1 Al 0.38990(11) -0.4905(2) 0.31444(8) 0.0300(5) Uani 1 1 d D . . Si1 Si 0.60815(9) -0.0452(2) 0.34811(6) 0.0301(3) Uani 1 1 d . . . P1 P 0.45692(8) 0.06645(18) 0.33960(6) 0.0317(3) Uani 1 1 d . . . Cl11 Cl 0.4522(2) -0.5512(6) 0.37247(11) 0.0428(10) Uani 0.83 1 d PD . . Cl12 Cl 0.30445(19) -0.6601(5) 0.30525(17) 0.0621(12) Uani 0.83 1 d PD . . Cl13 Cl 0.45791(13) -0.4875(3) 0.25658(7) 0.0505(5) 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 C10 0.033(4) 0.036(4) 0.048(5) 0.005(2) -0.020(4) 0.000(2) C11 0.045(4) 0.029(3) 0.058(5) -0.007(3) -0.005(3) -0.001(3) C26 0.039(3) 0.026(3) 0.044(4) -0.001(3) -0.003(3) 0.001(2) C30 0.040(3) 0.033(3) 0.050(4) 0.008(3) 0.005(3) 0.003(3) C31 0.029(4) 0.048(4) 0.032(4) -0.003(2) -0.004(3) 0.004(2) Cl10 0.049(2) 0.0452(16) 0.060(2) 0.0043(14) -0.0003(16) 0.0078(12) Cl15 0.043(8) 0.028(5) 0.035(6) 0.004(4) -0.005(5) 0.009(4) Cl17 0.070(10) 0.063(9) 0.061(8) 0.001(6) 0.005(6) -0.028(7) Cl22 0.0422(11) 0.0303(9) 0.0428(12) -0.0015(9) -0.0037(9) -0.0117(9) Cl23 0.0455(12) 0.0960(15) 0.0285(10) 0.0032(9) 0.0053(8) -0.0005(10) Cl25 0.190(18) 0.24(2) 0.131(13) 0.151(14) 0.133(13) 0.209(18) Cl26 0.174(18) 0.31(3) 0.146(17) -0.18(2) 0.110(15) -0.22(2) Cl27 0.008(4) 0.244(18) 0.003(3) 0.015(6) -0.002(3) 0.022(7) C21 0.029(3) 0.035(3) 0.031(3) 0.003(2) 0.005(2) 0.011(2) C22 0.038(3) 0.039(3) 0.029(3) -0.005(3) 0.003(2) 0.004(3) C23 0.036(4) 0.055(4) 0.024(3) -0.007(3) 0.000(3) 0.005(3) C24 0.040(4) 0.042(3) 0.034(3) -0.007(3) -0.007(3) 0.007(3) C25 0.032(3) 0.040(3) 0.027(3) -0.001(2) -0.002(2) -0.002(2) C27 0.054(5) 0.051(4) 0.049(4) 0.010(4) 0.006(4) 0.006(4) C28 0.069(6) 0.088(6) 0.035(4) -0.004(4) 0.003(4) 0.017(5) C29 0.039(5) 0.056(5) 0.039(4) -0.008(3) -0.013(4) 0.001(3) C32 0.041(4) 0.024(3) 0.010(3) 0.0008(15) 0.002(2) 0.003(2) C33 0.061(5) 0.043(4) 0.037(4) 0.009(3) -0.011(3) -0.002(3) C34 0.094(6) 0.038(4) 0.032(4) -0.010(3) 0.001(4) -0.002(4) C35 0.038(4) 0.070(5) 0.025(3) 0.000(3) 0.013(3) 0.007(3) N2 0.026(3) 0.026(2) 0.018(2) -0.0074(16) -0.001(2) 0.0062(16) Al2 0.0222(10) 0.0344(9) 0.0270(10) -0.0032(7) -0.0021(8) -0.0013(6) Si2 0.0240(8) 0.0387(8) 0.0249(8) -0.0011(8) -0.0021(6) 0.0008(7) P2 0.0251(6) 0.0354(8) 0.0304(7) -0.0025(6) -0.0001(5) -0.0004(5) Cl20 0.0348(12) 0.0502(13) 0.0650(17) -0.0141(13) -0.0244(12) 0.0130(11) Cl21 0.0349(12) 0.0205(8) 0.0294(12) -0.0032(7) -0.0062(8) -0.0012(7) C1 0.031(3) 0.035(3) 0.028(3) -0.001(2) -0.001(2) 0.004(2) C2 0.032(3) 0.052(4) 0.033(3) -0.001(3) 0.005(2) -0.006(3) C3 0.045(4) 0.047(4) 0.021(3) -0.002(2) -0.003(3) 0.000(3) C4 0.031(3) 0.067(4) 0.019(3) 0.005(3) -0.008(2) 0.000(3) C5 0.034(3) 0.032(3) 0.028(3) 0.005(2) 0.000(2) -0.003(2) C6 0.036(3) 0.035(3) 0.040(3) -0.001(3) -0.002(3) -0.006(3) C7 0.029(4) 0.092(6) 0.042(4) -0.006(4) 0.017(3) 0.000(4) C8 0.056(5) 0.101(6) 0.016(3) -0.011(3) 0.001(3) -0.001(5) C9 0.037(5) 0.095(8) 0.024(4) 0.011(3) -0.014(3) -0.012(3) C12 0.036(4) 0.044(4) 0.031(4) -0.005(2) 0.009(3) 0.005(3) C13 0.059(4) 0.044(4) 0.025(3) -0.008(3) 0.006(3) -0.004(3) C14 0.070(5) 0.044(4) 0.040(4) 0.022(3) 0.015(4) 0.009(4) C15 0.053(6) 0.044(4) 0.045(5) -0.003(3) 0.019(4) -0.001(3) N1 0.028(3) 0.030(3) 0.020(3) -0.0036(16) 0.006(2) 0.0012(17) Al1 0.0233(11) 0.0410(11) 0.0257(10) 0.0019(6) 0.0008(8) 0.0009(7) Si1 0.0269(8) 0.0327(8) 0.0309(8) -0.0013(8) -0.0011(6) 0.0002(7) P1 0.0280(7) 0.0358(8) 0.0313(7) 0.0033(6) -0.0005(5) 0.0005(6) Cl11 0.0425(17) 0.0534(19) 0.0325(14) 0.0012(12) 0.0005(12) 0.0086(12) Cl12 0.0422(13) 0.0574(16) 0.087(3) 0.0168(19) -0.0232(18) -0.0123(14) Cl13 0.0362(10) 0.0925(15) 0.0229(8) -0.0005(7) 0.0033(7) 0.0090(8) _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 C10 Si1 1.871(8) . ? C11 Si1 1.842(7) . ? C26 C21 1.561(8) . ? C30 Si2 1.870(7) . ? C31 Si2 1.840(8) . ? Cl10 Al1 2.148(3) . ? Cl15 Al1 2.145(7) . ? Cl16 Al1 2.138(7) . ? Cl17 Al1 2.134(7) . ? Cl22 Cl26 0.476(19) . ? Cl22 Al2 2.142(3) . ? Cl23 Al2 2.107(3) . ? Cl25 Al2 2.142(6) . ? Cl26 Al2 2.133(7) . ? Cl27 Al2 2.139(6) . ? C21 C22 1.485(8) . ? C21 C25 1.502(8) . ? C21 Si2 1.885(6) . ? C22 C23 1.396(11) . ? C22 C27 1.481(10) . ? C23 C28 1.429(12) . ? C23 C24 1.457(12) . ? C24 C25 1.395(9) . ? C24 C29 1.508(11) . ? C25 P2 1.724(6) . ? C32 C35 1.420(13) . ? C32 C34 1.532(9) . ? C32 C33 1.544(9) . ? C32 N2 1.593(8) . ? N2 P2 1.633(6) . ? N2 Si2 1.775(6) . ? Al2 Cl20 2.114(3) . ? Al2 Cl21 2.143(3) . ? C1 C2 1.485(8) . ? C1 C5 1.512(8) . ? C1 C6 1.564(8) . ? C1 Si1 1.898(6) . ? C2 C3 1.360(11) . ? C2 C7 1.500(9) . ? C3 C4 1.422(12) . ? C3 C8 1.530(10) . ? C4 C5 1.393(9) . ? C4 C9 1.484(11) . ? C5 P1 1.729(6) . ? C12 N1 1.420(10) . ? C12 C13 1.517(11) . ? C12 C14 1.516(10) . ? C12 C15 1.640(14) . ? N1 P1 1.670(7) . ? N1 Si1 1.865(6) . ? Al1 Cl12 2.112(3) . ? Al1 Cl13 2.131(3) . ? Al1 Cl11 2.139(3) . ? 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 Cl26 Cl22 Al2 82.5(9) . . ? Cl22 Cl26 Al2 84.7(9) . . ? C22 C21 C25 103.3(5) . . ? C22 C21 C26 113.7(5) . . ? C25 C21 C26 113.5(5) . . ? C22 C21 Si2 118.5(5) . . ? C25 C21 Si2 98.0(4) . . ? C26 C21 Si2 108.8(4) . . ? C23 C22 C21 111.0(6) . . ? C23 C22 C27 125.9(7) . . ? C21 C22 C27 123.0(6) . . ? C22 C23 C28 128.2(9) . . ? C22 C23 C24 107.0(7) . . ? C28 C23 C24 124.8(8) . . ? C25 C24 C23 109.9(6) . . ? C25 C24 C29 124.8(7) . . ? C23 C24 C29 125.0(7) . . ? C24 C25 C21 108.7(5) . . ? C24 C25 P2 127.5(5) . . ? C21 C25 P2 120.8(4) . . ? C35 C32 C34 114.0(6) . . ? C35 C32 C33 110.5(6) . . ? C34 C32 C33 108.3(7) . . ? C35 C32 N2 113.9(6) . . ? C34 C32 N2 104.1(5) . . ? C33 C32 N2 105.5(5) . . ? C32 N2 P2 115.8(5) . . ? C32 N2 Si2 128.3(5) . . ? P2 N2 Si2 115.8(4) . . ? Cl23 Al2 Cl20 110.79(16) . . ? Cl23 Al2 Cl26 109.0(5) . . ? Cl20 Al2 Cl26 99.3(5) . . ? Cl23 Al2 Cl25 112.9(3) . . ? Cl20 Al2 Cl25 11.2(5) . . ? Cl26 Al2 Cl25 108.1(4) . . ? Cl23 Al2 Cl27 111.3(3) . . ? Cl20 Al2 Cl27 117.7(4) . . ? Cl26 Al2 Cl27 107.8(4) . . ? Cl25 Al2 Cl27 107.6(4) . . ? Cl23 Al2 Cl21 110.10(15) . . ? Cl20 Al2 Cl21 108.95(13) . . ? Cl26 Al2 Cl21 118.2(5) . . ? Cl25 Al2 Cl21 98.3(5) . . ? Cl27 Al2 Cl21 11.7(5) . . ? Cl23 Al2 Cl22 109.44(14) . . ? Cl20 Al2 Cl22 110.25(14) . . ? Cl26 Al2 Cl22 12.8(5) . . ? Cl25 Al2 Cl22 118.0(5) . . ? Cl27 Al2 Cl22 96.3(4) . . ? Cl21 Al2 Cl22 107.24(14) . . ? N2 Si2 C31 116.0(3) . . ? N2 Si2 C30 108.4(3) . . ? C31 Si2 C30 111.9(3) . . ? N2 Si2 C21 94.6(3) . . ? C31 Si2 C21 113.2(3) . . ? C30 Si2 C21 111.5(3) . . ? N2 P2 C25 94.6(3) . . ? C2 C1 C5 103.2(5) . . ? C2 C1 C6 114.1(6) . . ? C5 C1 C6 112.7(5) . . ? C2 C1 Si1 119.4(5) . . ? C5 C1 Si1 97.6(4) . . ? C6 C1 Si1 108.5(4) . . ? C3 C2 C1 108.5(6) . . ? C3 C2 C7 128.2(7) . . ? C1 C2 C7 123.2(6) . . ? C2 C3 C4 111.9(7) . . ? C2 C3 C8 125.1(9) . . ? C4 C3 C8 122.8(8) . . ? C5 C4 C3 107.6(6) . . ? C5 C4 C9 128.0(7) . . ? C3 C4 C9 124.4(7) . . ? C4 C5 C1 108.8(5) . . ? C4 C5 P1 127.2(5) . . ? C1 C5 P1 120.9(4) . . ? N1 C12 C13 109.8(6) . . ? N1 C12 C14 111.9(6) . . ? C13 C12 C14 113.6(8) . . ? N1 C12 C15 107.4(8) . . ? C13 C12 C15 107.5(6) . . ? C14 C12 C15 106.2(6) . . ? C12 N1 P1 125.2(6) . . ? C12 N1 Si1 124.6(6) . . ? P1 N1 Si1 110.0(3) . . ? Cl12 Al1 Cl13 108.79(19) . . ? Cl12 Al1 Cl17 12.0(7) . . ? Cl13 Al1 Cl17 119.7(7) . . ? Cl12 Al1 Cl16 109.3(5) . . ? Cl13 Al1 Cl16 105.8(5) . . ? Cl17 Al1 Cl16 108.6(5) . . ? Cl12 Al1 Cl15 118.4(6) . . ? Cl13 Al1 Cl15 105.5(7) . . ? Cl17 Al1 Cl15 108.4(5) . . ? Cl16 Al1 Cl15 108.3(5) . . ? Cl12 Al1 Cl11 109.43(16) . . ? Cl13 Al1 Cl11 111.53(16) . . ? Cl17 Al1 Cl11 107.3(6) . . ? Cl16 Al1 Cl11 6.6(6) . . ? Cl15 Al1 Cl11 103.1(6) . . ? Cl12 Al1 Cl10 109.95(19) . . ? Cl13 Al1 Cl10 109.4(2) . . ? Cl17 Al1 Cl10 100.1(6) . . ? Cl16 Al1 Cl10 113.4(6) . . ? Cl15 Al1 Cl10 8.4(6) . . ? Cl11 Al1 Cl10 107.7(2) . . ? C11 Si1 N1 109.4(3) . . ? C11 Si1 C10 113.7(3) . . ? N1 Si1 C10 113.8(4) . . ? C11 Si1 C1 111.4(3) . . ? N1 Si1 C1 96.4(3) . . ? C10 Si1 C1 111.0(3) . . ? N1 P1 C5 98.1(3) . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 2.448 _refine_diff_density_min -0.678 _refine_diff_density_rms 0.121 data_p21overn _database_code_CSD 200129 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido arsenic chloride ; _chemical_name_common '(CGC)arsenic chloride' _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 Cl N AS Si' _chemical_formula_sum 'C15 H27 As Cl N Si' _chemical_formula_weight 359.84 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 6.953(5) _cell_length_b 17.258(5) _cell_length_c 14.991(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 91.669(5) _cell_angle_gamma 90.000(5) _cell_volume 1798.1(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 27.46 _exptl_crystal_description prism _exptl_crystal_colour yello _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 752 _exptl_absorpt_coefficient_mu 2.095 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.6794 _exptl_absorpt_correction_T_max 0.6794 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11122 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_sigmaI/netI 0.0505 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.60 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4068 _reflns_number_gt 3574 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0000P)^2^+1.2728P] 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 SHELXL _refine_ls_extinction_coef 0.0024(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4068 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0350 _refine_ls_R_factor_gt 0.0274 _refine_ls_wR_factor_ref 0.0572 _refine_ls_wR_factor_gt 0.0549 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4594(2) 0.34093(10) 0.42904(11) 0.0214(3) Uani 1 1 d . . . C2 C 0.5938(2) 0.39425(11) 0.45415(11) 0.0251(4) Uani 1 1 d . . . C3 C 0.6659(3) 0.43420(11) 0.37497(13) 0.0278(4) Uani 1 1 d . . . C4 C 0.5807(3) 0.40389(10) 0.30107(12) 0.0250(4) Uani 1 1 d . . . C5 C 0.4342(2) 0.34543(10) 0.32868(11) 0.0208(3) Uani 1 1 d . . . C6 C 0.6702(3) 0.41048(14) 0.54675(14) 0.0352(5) Uani 1 1 d . . . C7 C 0.8132(3) 0.49780(14) 0.38074(19) 0.0424(5) Uani 1 1 d . . . C8 C 0.6181(3) 0.42114(13) 0.20524(14) 0.0346(5) Uani 1 1 d . . . C9 C 0.2290(3) 0.36677(12) 0.29626(13) 0.0274(4) Uani 1 1 d . . . C10 C 0.1202(3) 0.26762(13) 0.52680(14) 0.0313(4) Uani 1 1 d . . . C11 C 0.5279(3) 0.21221(14) 0.56946(14) 0.0354(5) Uani 1 1 d . . . C12 C 0.3160(3) 0.10945(10) 0.37618(11) 0.0259(4) Uani 1 1 d . . . C13 C 0.2261(4) 0.08999(13) 0.28447(14) 0.0355(5) Uani 1 1 d . . . C14 C 0.1714(3) 0.08797(13) 0.44671(14) 0.0338(4) Uani 1 1 d . . . C15 C 0.5002(4) 0.06244(13) 0.39084(17) 0.0401(5) Uani 1 1 d . . . N N 0.3596(2) 0.19471(8) 0.38220(9) 0.0197(3) Uani 1 1 d . . . Si Si 0.36280(7) 0.25194(3) 0.48002(3) 0.02077(11) Uani 1 1 d . . . Cl Cl 0.79221(7) 0.23000(3) 0.32048(4) 0.04112(14) Uani 1 1 d . . . As As 0.47475(3) 0.237674(10) 0.285809(11) 0.02146(8) Uani 1 1 d . . . H6A H 0.606(3) 0.3829(14) 0.5896(16) 0.044(6) Uiso 1 1 d . . . H6B H 0.805(4) 0.3982(15) 0.5529(15) 0.048(7) Uiso 1 1 d . . . H6C H 0.655(3) 0.4664(15) 0.5628(16) 0.050(7) Uiso 1 1 d . . . H7A H 0.933(4) 0.4779(15) 0.4120(17) 0.056(7) Uiso 1 1 d . . . H7B H 0.771(3) 0.5402(16) 0.4154(17) 0.053(7) Uiso 1 1 d . . . H7C H 0.848(4) 0.5169(17) 0.3285(19) 0.063(8) Uiso 1 1 d . . . H8A H 0.704(3) 0.3856(16) 0.1835(16) 0.051(7) Uiso 1 1 d . . . H8B H 0.671(4) 0.4715(18) 0.1965(18) 0.065(8) Uiso 1 1 d . . . H8C H 0.497(4) 0.4174(14) 0.1690(16) 0.048(7) Uiso 1 1 d . . . H9A H 0.140(3) 0.3308(14) 0.3147(14) 0.034(6) Uiso 1 1 d . . . H9B H 0.191(3) 0.4174(13) 0.3205(13) 0.027(5) Uiso 1 1 d . . . H9C H 0.220(3) 0.3701(13) 0.2306(15) 0.039(6) Uiso 1 1 d . . . H10A H 0.067(4) 0.2213(16) 0.5558(17) 0.054(7) Uiso 1 1 d . . . H10B H 0.131(3) 0.3066(16) 0.5671(17) 0.054(7) Uiso 1 1 d . . . H10C H 0.030(3) 0.2828(15) 0.4814(17) 0.047(7) Uiso 1 1 d . . . H11A H 0.493(3) 0.1574(15) 0.5853(16) 0.047(7) Uiso 1 1 d . . . H11B H 0.651(4) 0.2120(15) 0.5512(17) 0.051(7) Uiso 1 1 d . . . H11C H 0.521(4) 0.2433(16) 0.6208(19) 0.059(8) Uiso 1 1 d . . . H13A H 0.319(3) 0.0993(13) 0.2396(15) 0.036(6) Uiso 1 1 d . . . H13B H 0.112(3) 0.1207(15) 0.2706(15) 0.043(6) Uiso 1 1 d . . . H13C H 0.193(3) 0.0347(15) 0.2815(15) 0.047(6) Uiso 1 1 d . . . H14A H 0.050(3) 0.1177(13) 0.4357(13) 0.032(5) Uiso 1 1 d . . . H14B H 0.142(3) 0.0336(14) 0.4424(14) 0.039(6) Uiso 1 1 d . . . H14C H 0.219(3) 0.0973(13) 0.5044(15) 0.032(5) Uiso 1 1 d . . . H15A H 0.472(3) 0.0083(16) 0.3857(16) 0.052(7) Uiso 1 1 d . . . H15B H 0.595(4) 0.0744(15) 0.3463(17) 0.056(7) Uiso 1 1 d . . . H15C H 0.557(3) 0.0736(13) 0.4468(15) 0.035(6) 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 C1 0.0203(9) 0.0244(9) 0.0196(8) -0.0040(7) 0.0024(6) 0.0020(7) C2 0.0219(9) 0.0264(9) 0.0271(9) -0.0070(7) 0.0015(7) 0.0018(7) C3 0.0211(9) 0.0250(10) 0.0375(10) -0.0068(8) 0.0072(7) -0.0032(7) C4 0.0253(9) 0.0204(9) 0.0299(9) -0.0006(7) 0.0076(7) -0.0002(7) C5 0.0232(9) 0.0203(8) 0.0189(8) -0.0005(7) 0.0021(6) -0.0011(6) C6 0.0323(12) 0.0409(13) 0.0322(10) -0.0141(10) -0.0043(9) -0.0008(9) C7 0.0343(13) 0.0361(12) 0.0576(15) -0.0146(12) 0.0122(11) -0.0142(10) C8 0.0422(13) 0.0297(11) 0.0325(10) 0.0041(9) 0.0131(9) -0.0033(10) C9 0.0268(10) 0.0273(10) 0.0279(10) 0.0034(8) -0.0012(7) -0.0008(8) C10 0.0315(11) 0.0352(12) 0.0277(10) -0.0039(9) 0.0105(8) -0.0003(9) C11 0.0367(13) 0.0455(13) 0.0238(9) 0.0056(9) -0.0042(8) 0.0003(10) C12 0.0350(10) 0.0178(9) 0.0253(9) 0.0008(7) 0.0074(7) -0.0009(7) C13 0.0508(14) 0.0256(11) 0.0304(10) -0.0060(8) 0.0060(9) -0.0096(10) C14 0.0456(13) 0.0248(11) 0.0316(11) 0.0019(9) 0.0112(9) -0.0075(9) C15 0.0470(14) 0.0272(12) 0.0467(13) 0.0077(10) 0.0108(11) 0.0110(10) N 0.0223(7) 0.0195(7) 0.0175(6) 0.0006(6) 0.0041(5) -0.0002(5) Si 0.0226(2) 0.0252(3) 0.0147(2) 0.00007(18) 0.00195(17) 0.00031(18) Cl 0.0228(2) 0.0411(3) 0.0599(3) 0.0000(3) 0.0101(2) 0.0025(2) As 0.02698(11) 0.02127(11) 0.01639(10) -0.00102(7) 0.00512(6) -0.00195(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 C1 C2 1.357(2) . ? C1 C5 1.512(2) . ? C1 Si 1.8502(19) . ? C2 C3 1.473(3) . ? C2 C6 1.498(3) . ? C3 C4 1.347(3) . ? C3 C7 1.502(3) . ? C4 C8 1.497(3) . ? C4 C5 1.500(2) . ? C5 C9 1.538(3) . ? C5 As 1.9903(18) . ? C10 Si 1.865(2) . ? C11 Si 1.870(2) . ? C12 N 1.504(2) . ? C12 C14 1.526(3) . ? C12 C15 1.526(3) . ? C12 C13 1.531(3) . ? N Si 1.7676(15) . ? N As 1.8292(14) . ? Cl As 2.2568(16) . ? 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 C2 C1 C5 107.47(15) . . ? C2 C1 Si 134.71(14) . . ? C5 C1 Si 114.89(12) . . ? C1 C2 C3 109.97(15) . . ? C1 C2 C6 127.34(18) . . ? C3 C2 C6 122.64(17) . . ? C4 C3 C2 109.22(16) . . ? C4 C3 C7 127.89(19) . . ? C2 C3 C7 122.89(18) . . ? C3 C4 C8 128.85(18) . . ? C3 C4 C5 108.68(15) . . ? C8 C4 C5 122.46(16) . . ? C4 C5 C1 104.43(14) . . ? C4 C5 C9 112.49(15) . . ? C1 C5 C9 113.97(14) . . ? C4 C5 As 115.82(12) . . ? C1 C5 As 105.07(11) . . ? C9 C5 As 105.10(12) . . ? N C12 C14 109.37(14) . . ? N C12 C15 110.16(16) . . ? C14 C12 C15 109.77(17) . . ? N C12 C13 110.16(15) . . ? C14 C12 C13 107.98(17) . . ? C15 C12 C13 109.36(17) . . ? C12 N Si 126.43(11) . . ? C12 N As 116.17(10) . . ? Si N As 115.70(8) . . ? N Si C1 96.72(7) . . ? N Si C10 113.79(9) . . ? C1 Si C10 112.20(9) . . ? N Si C11 112.49(9) . . ? C1 Si C11 112.21(10) . . ? C10 Si C11 109.07(11) . . ? N As C5 93.11(7) . . ? N As Cl 104.00(5) . . ? C5 As Cl 97.31(5) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.326 _refine_diff_density_min -0.317 _refine_diff_density_rms 0.056 data_shelx _database_code_CSD 200130 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido antimony chloride ; _chemical_name_common '(CGC)antimony chloride' _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 Cl N Sb Si' _chemical_formula_sum 'C15 H27 Cl N Sb Si' _chemical_formula_weight 406.67 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.146(5) _cell_length_b 24.618(5) _cell_length_c 8.984(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 95.488(5) _cell_angle_gamma 90.000(5) _cell_volume 1793.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.01 _cell_measurement_theta_max 30.45 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 824 _exptl_absorpt_coefficient_mu 1.744 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.7218 _exptl_absorpt_correction_T_max 0.7218 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19298 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0477 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -9 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.45 _reflns_number_total 4856 _reflns_number_gt 3895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0415P)^2^+0.3861P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4856 _refine_ls_number_parameters 280 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0329 _refine_ls_wR_factor_ref 0.0826 _refine_ls_wR_factor_gt 0.0742 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _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 0.3346(3) 0.43362(9) 0.6761(3) 0.0214(5) Uani 1 1 d . . . C2 C 0.2814(3) 0.48554(10) 0.6358(3) 0.0250(5) Uani 1 1 d . . . C3 C 0.2416(3) 0.51546(10) 0.7661(3) 0.0273(5) Uani 1 1 d . . . C4 C 0.2643(3) 0.48233(10) 0.8892(3) 0.0278(5) Uani 1 1 d . . . C5 C 0.3173(3) 0.42878(9) 0.8407(3) 0.0230(5) Uani 1 1 d . . . C6 C 0.2594(4) 0.50908(13) 0.4805(3) 0.0352(7) Uani 1 1 d . . . C7 C 0.1788(5) 0.57294(12) 0.7601(4) 0.0412(7) Uani 1 1 d . . . C8 C 0.2400(5) 0.49546(13) 1.0486(3) 0.0377(7) Uani 1 1 d . . . C9 C 0.4314(4) 0.39384(11) 0.9442(3) 0.0288(6) Uani 1 1 d . . . C10 C 0.5731(4) 0.33883(12) 0.6122(4) 0.0310(6) Uani 1 1 d . . . C11 C 0.3420(4) 0.38089(12) 0.3632(3) 0.0339(7) Uani 1 1 d . . . C12 C 0.1509(3) 0.27637(10) 0.6092(3) 0.0238(5) Uani 1 1 d . . . C13 C 0.1951(4) 0.25968(12) 0.4547(3) 0.0331(6) Uani 1 1 d . . . C14 C -0.0355(4) 0.27214(12) 0.6124(3) 0.0324(6) Uani 1 1 d . . . C15 C 0.2377(4) 0.23845(12) 0.7261(4) 0.0342(6) Uani 1 1 d . . . N1 N 0.2054(2) 0.33342(7) 0.6418(2) 0.0208(4) Uani 1 1 d . . . Si1 Si 0.36445(9) 0.36959(3) 0.56981(7) 0.02115(15) Uani 1 1 d . . . Cl1 Cl 0.06838(10) 0.33330(3) 0.99314(7) 0.03772(17) Uani 1 1 d . . . Sb1 Sb 0.08188(2) 0.386289(6) 0.765180(17) 0.02338(7) Uani 1 1 d . . . H6A H 0.145(7) 0.504(2) 0.434(6) 0.117(19) Uiso 1 1 d . . . H6B H 0.291(6) 0.541(2) 0.477(6) 0.108(18) Uiso 1 1 d . . . H6C H 0.314(6) 0.490(2) 0.414(5) 0.096(16) Uiso 1 1 d . . . H7A H 0.148(5) 0.5843(17) 0.848(5) 0.069(12) Uiso 1 1 d . . . H7B H 0.083(5) 0.5791(16) 0.683(5) 0.071(12) Uiso 1 1 d . . . H7C H 0.253(5) 0.5973(17) 0.729(5) 0.063(12) Uiso 1 1 d . . . H8A H 0.342(5) 0.4983(15) 1.103(4) 0.059(11) Uiso 1 1 d . . . H8B H 0.158(4) 0.4695(14) 1.084(4) 0.047(9) Uiso 1 1 d . . . H8C H 0.194(4) 0.5311(15) 1.056(4) 0.056(10) Uiso 1 1 d . . . H9A H 0.543(4) 0.4077(12) 0.952(3) 0.034(8) Uiso 1 1 d . . . H9B H 0.393(4) 0.3934(11) 1.041(4) 0.035(8) Uiso 1 1 d . . . H9C H 0.439(4) 0.3544(13) 0.907(3) 0.043(9) Uiso 1 1 d . . . H10A H 0.577(5) 0.3044(16) 0.573(4) 0.065(11) Uiso 1 1 d . . . H10B H 0.612(5) 0.3372(14) 0.708(5) 0.063(11) Uiso 1 1 d . . . H10C H 0.651(5) 0.3617(17) 0.568(4) 0.063(11) Uiso 1 1 d . . . H11A H 0.416(4) 0.4111(13) 0.333(3) 0.037(8) Uiso 1 1 d . . . H11B H 0.242(5) 0.3924(12) 0.319(4) 0.043(10) Uiso 1 1 d . . . H11C H 0.361(4) 0.3459(14) 0.305(4) 0.055(10) Uiso 1 1 d . . . H91 H -0.074(4) 0.2379(12) 0.587(3) 0.036(8) Uiso 1 1 d . . . H92 H -0.075(4) 0.2818(15) 0.712(4) 0.054(11) Uiso 1 1 d . . . H93 H -0.092(4) 0.2986(14) 0.536(4) 0.051(10) Uiso 1 1 d . . . H101 H 0.205(4) 0.2023(14) 0.704(4) 0.047(9) Uiso 1 1 d . . . H102 H 0.204(4) 0.2444(13) 0.822(4) 0.049(10) Uiso 1 1 d . . . H103 H 0.356(5) 0.2383(12) 0.720(3) 0.042(9) Uiso 1 1 d . . . H111 H 0.311(4) 0.2626(11) 0.449(3) 0.031(8) Uiso 1 1 d . . . H112 H 0.142(4) 0.2793(13) 0.378(4) 0.049(10) Uiso 1 1 d . . . H113 H 0.165(4) 0.2219(15) 0.436(4) 0.051(10) 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 C1 0.0223(12) 0.0225(12) 0.0196(11) 0.0024(9) 0.0029(9) -0.0012(9) C2 0.0257(13) 0.0226(12) 0.0267(12) 0.0048(10) 0.0019(10) -0.0001(10) C3 0.0267(14) 0.0201(12) 0.0355(14) -0.0032(10) 0.0047(11) -0.0012(10) C4 0.0323(15) 0.0243(12) 0.0274(13) -0.0032(10) 0.0066(10) -0.0051(11) C5 0.0283(13) 0.0195(11) 0.0215(11) 0.0012(9) 0.0044(9) -0.0048(10) C6 0.0447(19) 0.0287(15) 0.0325(15) 0.0124(12) 0.0051(13) 0.0045(13) C7 0.049(2) 0.0213(14) 0.054(2) -0.0030(13) 0.0100(17) 0.0044(14) C8 0.051(2) 0.0318(16) 0.0316(15) -0.0096(12) 0.0115(14) -0.0067(14) C9 0.0326(16) 0.0300(14) 0.0229(13) 0.0042(10) -0.0017(11) -0.0042(11) C10 0.0278(15) 0.0302(15) 0.0356(15) 0.0045(12) 0.0054(12) 0.0045(12) C11 0.0432(18) 0.0402(17) 0.0187(12) 0.0043(11) 0.0054(12) 0.0040(14) C12 0.0248(13) 0.0210(12) 0.0246(12) -0.0049(9) -0.0020(10) 0.0003(9) C13 0.0373(18) 0.0314(15) 0.0300(15) -0.0102(11) 0.0007(12) -0.0012(13) C14 0.0291(15) 0.0306(15) 0.0371(16) -0.0078(12) 0.0013(12) -0.0055(12) C15 0.0405(19) 0.0237(14) 0.0374(17) 0.0034(12) -0.0008(13) 0.0032(12) N1 0.0230(11) 0.0188(9) 0.0204(9) -0.0031(7) 0.0010(8) 0.0022(8) Si1 0.0235(4) 0.0227(3) 0.0175(3) 0.0015(2) 0.0032(3) 0.0034(3) Cl1 0.0511(5) 0.0354(4) 0.0288(3) -0.0024(3) 0.0148(3) -0.0142(3) Sb1 0.02279(11) 0.02244(11) 0.02513(10) -0.00435(6) 0.00345(7) 0.00211(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.386(3) . ? C1 C5 1.504(3) . ? C1 Si1 1.871(2) . ? C1 Sb1 2.560(3) . ? C2 C3 1.446(4) . ? C2 C6 1.505(4) . ? C3 C4 1.372(4) . ? C3 C7 1.504(4) . ? C4 C5 1.466(3) . ? C4 C8 1.500(4) . ? C5 C9 1.518(4) . ? C5 Sb1 2.232(3) . ? C10 Si1 1.867(3) . ? C11 Si1 1.869(3) . ? C12 N1 1.493(3) . ? C12 C13 1.523(4) . ? C12 C14 1.525(4) . ? C12 C15 1.527(4) . ? N1 Si1 1.747(2) . ? N1 Sb1 2.037(2) . ? Si1 Sb1 3.0529(15) . ? Cl1 Sb1 2.4396(12) . ? 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 C2 C1 C5 105.9(2) . . ? C2 C1 Si1 134.12(19) . . ? C5 C1 Si1 117.65(16) . . ? C2 C1 Sb1 105.09(17) . . ? C5 C1 Sb1 60.17(12) . . ? Si1 C1 Sb1 85.62(9) . . ? C1 C2 C3 110.3(2) . . ? C1 C2 C6 127.1(2) . . ? C3 C2 C6 122.5(2) . . ? C4 C3 C2 109.0(2) . . ? C4 C3 C7 127.4(3) . . ? C2 C3 C7 123.5(3) . . ? C3 C4 C5 108.4(2) . . ? C3 C4 C8 128.4(2) . . ? C5 C4 C8 123.2(2) . . ? C4 C5 C1 106.2(2) . . ? C4 C5 C9 120.5(2) . . ? C1 C5 C9 122.5(2) . . ? C4 C5 Sb1 104.03(17) . . ? C1 C5 Sb1 84.08(14) . . ? C9 C5 Sb1 112.25(17) . . ? N1 C12 C13 109.9(2) . . ? N1 C12 C14 109.8(2) . . ? C13 C12 C14 108.7(2) . . ? N1 C12 C15 109.3(2) . . ? C13 C12 C15 109.1(2) . . ? C14 C12 C15 110.0(2) . . ? C12 N1 Si1 128.60(16) . . ? C12 N1 Sb1 123.70(16) . . ? Si1 N1 Sb1 107.35(10) . . ? N1 Si1 C10 114.28(12) . . ? N1 Si1 C11 115.97(13) . . ? C10 Si1 C11 105.29(15) . . ? N1 Si1 C1 95.94(10) . . ? C10 Si1 C1 113.45(13) . . ? C11 Si1 C1 112.11(12) . . ? N1 Si1 Sb1 39.55(6) . . ? C10 Si1 Sb1 131.25(10) . . ? C11 Si1 Sb1 122.92(11) . . ? C1 Si1 Sb1 56.72(8) . . ? N1 Sb1 C5 90.59(9) . . ? N1 Sb1 Cl1 100.34(6) . . ? C5 Sb1 Cl1 95.85(6) . . ? N1 Sb1 C1 70.54(8) . . ? C5 Sb1 C1 35.75(8) . . ? Cl1 Sb1 C1 127.46(6) . . ? N1 Sb1 Si1 33.10(6) . . ? C5 Sb1 Si1 64.20(7) . . ? Cl1 Sb1 Si1 120.51(3) . . ? C1 Sb1 Si1 37.66(6) . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 30.45 _diffrn_measured_fraction_theta_full 0.890 _refine_diff_density_max 0.803 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.122 data_shelx2 _database_code_CSD 200131 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido phosporous chloride ; _chemical_name_common '(CGC)phosphorous chloride' _chemical_melting_point ? _chemical_formula_moiety 'C15 H27 Cl N P Si' _chemical_formula_sum 'C15 H27 Cl N P Si' _chemical_formula_weight 315.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pcab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y+1/2, z+1/2' 'x+1/2, -y, -z+1/2' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y-1/2, -z-1/2' '-x-1/2, y, z-1/2' 'x-1/2, -y-1/2, z' _cell_length_a 14.969(5) _cell_length_b 15.300(5) _cell_length_c 15.506(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 90.000(5) _cell_angle_gamma 90.000(5) _cell_volume 3551(2) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1360 _exptl_absorpt_coefficient_mu 0.362 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9311 _exptl_absorpt_correction_T_max 0.9311 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _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 'Nonoius Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7426 _diffrn_reflns_av_R_equivalents 0.0212 _diffrn_reflns_av_sigmaI/netI 0.0332 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4056 _reflns_number_gt 3270 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0384P)^2^+1.3494P] 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 SHELXL _refine_ls_extinction_coef 0.0021(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 4056 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0335 _refine_ls_wR_factor_ref 0.0855 _refine_ls_wR_factor_gt 0.0795 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.62731(10) 0.27777(9) 0.60935(10) 0.0244(3) Uani 1 1 d . . . C2 C 0.64859(10) 0.35084(10) 0.54864(11) 0.0281(3) Uani 1 1 d . . . C3 C 0.69305(10) 0.31955(10) 0.47899(10) 0.0275(3) Uani 1 1 d . . . C4 C 0.70243(10) 0.22498(10) 0.48752(9) 0.0238(3) Uani 1 1 d . . . C5 C 0.66808(9) 0.19972(9) 0.56501(9) 0.0217(3) Uani 1 1 d . . . C6 C 0.65475(12) 0.29459(12) 0.70344(11) 0.0309(4) Uani 1 1 d . . . C7 C 0.62363(15) 0.44382(11) 0.56711(15) 0.0400(4) Uani 1 1 d . . . C8 C 0.72709(14) 0.36952(13) 0.40283(12) 0.0385(4) Uani 1 1 d . . . C9 C 0.73775(12) 0.16756(12) 0.41702(11) 0.0306(4) Uani 1 1 d . . . C10 C 0.46014(15) 0.25155(13) 0.49521(15) 0.0434(5) Uani 1 1 d . . . C11 C 0.43653(14) 0.28924(14) 0.68709(18) 0.0500(6) Uani 1 1 d . . . C12 C 0.46578(10) 0.05686(10) 0.65898(10) 0.0283(3) Uani 1 1 d . . . C13 C 0.37330(12) 0.07412(12) 0.62102(15) 0.0384(4) Uani 1 1 d . . . C14 C 0.46365(15) 0.06410(14) 0.75763(13) 0.0429(5) Uani 1 1 d . . . C15 C 0.49352(13) -0.03602(11) 0.63364(13) 0.0345(4) Uani 1 1 d . . . N1 N 0.53100(8) 0.12281(8) 0.62419(8) 0.0232(3) Uani 1 1 d . . . Si1 Si 0.50800(3) 0.23474(3) 0.60429(3) 0.02659(13) Uani 1 1 d . . . P1 P 0.63435(3) 0.09126(2) 0.59355(2) 0.02206(11) Uani 1 1 d . . . Cl1 Cl 0.70793(3) 0.07325(3) 0.71404(3) 0.03369(13) Uani 1 1 d . . . H14A H 0.4443(14) 0.1211(14) 0.7748(12) 0.043(5) Uiso 1 1 d . . . H14B H 0.4190(13) 0.0240(13) 0.7802(12) 0.044(5) Uiso 1 1 d . . . H14C H 0.5239(16) 0.0550(13) 0.7795(13) 0.050(6) Uiso 1 1 d . . . H15C H 0.4971(11) -0.0421(11) 0.5703(12) 0.029(4) Uiso 1 1 d . . . H15B H 0.5488(13) -0.0493(12) 0.6580(12) 0.036(5) Uiso 1 1 d . . . H13B H 0.3524(13) 0.1303(14) 0.6349(13) 0.044(5) Uiso 1 1 d . . . H13A H 0.3736(14) 0.0664(13) 0.5600(15) 0.049(6) Uiso 1 1 d . . . H7B H 0.5637(17) 0.4509(15) 0.5694(15) 0.063(7) Uiso 1 1 d . . . H7A H 0.6489(16) 0.4641(15) 0.6205(16) 0.063(7) Uiso 1 1 d . . . H7C H 0.6412(15) 0.4821(15) 0.5216(15) 0.059(6) Uiso 1 1 d . . . H6C H 0.6276(14) 0.3480(13) 0.7247(12) 0.045(5) Uiso 1 1 d . . . H6B H 0.6381(12) 0.2471(12) 0.7423(12) 0.036(5) Uiso 1 1 d . . . H6A H 0.7208(15) 0.3025(13) 0.7082(12) 0.048(6) Uiso 1 1 d . . . H9A H 0.7367(13) 0.1047(13) 0.4327(13) 0.041(5) Uiso 1 1 d . . . H8C H 0.7087(15) 0.4297(15) 0.4057(14) 0.057(7) Uiso 1 1 d . . . H8A H 0.7884(17) 0.3666(15) 0.3978(14) 0.059(7) Uiso 1 1 d . . . H10C H 0.4052(17) 0.2237(15) 0.4895(14) 0.064(7) Uiso 1 1 d . . . H10B H 0.4523(17) 0.3124(17) 0.4862(15) 0.074(7) Uiso 1 1 d . . . H10A H 0.5001(16) 0.2319(15) 0.4512(15) 0.059(7) Uiso 1 1 d . . . H8B H 0.7062(15) 0.3474(15) 0.3487(15) 0.058(6) Uiso 1 1 d . . . H9C H 0.7005(14) 0.1720(13) 0.3650(13) 0.047(6) Uiso 1 1 d . . . H9B H 0.7985(16) 0.1831(13) 0.4016(13) 0.053(6) Uiso 1 1 d . . . H11A H 0.4400(16) 0.3475(17) 0.6757(15) 0.067(7) Uiso 1 1 d . . . H11B H 0.377(2) 0.2754(18) 0.6851(18) 0.089(9) Uiso 1 1 d . . . H11C H 0.455(2) 0.278(2) 0.747(2) 0.103(11) Uiso 1 1 d . . . H15A H 0.4513(13) -0.0759(12) 0.6587(12) 0.041(5) Uiso 1 1 d . . . H13C H 0.3304(14) 0.0336(14) 0.6454(13) 0.050(6) 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 C1 0.0238(7) 0.0222(7) 0.0273(8) -0.0048(6) 0.0003(6) -0.0014(6) C2 0.0256(8) 0.0231(7) 0.0354(9) -0.0007(7) -0.0053(7) -0.0058(6) C3 0.0252(8) 0.0293(8) 0.0281(8) 0.0015(6) -0.0052(6) -0.0063(6) C4 0.0184(7) 0.0293(8) 0.0239(7) -0.0021(6) -0.0033(6) -0.0023(6) C5 0.0175(7) 0.0242(7) 0.0235(7) -0.0029(6) -0.0023(6) 0.0013(6) C6 0.0301(9) 0.0348(9) 0.0280(8) -0.0090(7) 0.0007(7) -0.0025(7) C7 0.0420(11) 0.0237(8) 0.0544(12) -0.0035(8) -0.0007(10) -0.0016(8) C8 0.0402(11) 0.0409(10) 0.0345(10) 0.0100(8) -0.0028(8) -0.0083(9) C9 0.0284(9) 0.0385(9) 0.0249(8) -0.0074(7) 0.0031(7) -0.0045(7) C10 0.0380(11) 0.0301(9) 0.0620(13) 0.0066(9) -0.0228(10) -0.0021(8) C11 0.0319(10) 0.0351(10) 0.0830(17) -0.0207(11) 0.0167(11) -0.0006(9) C12 0.0257(8) 0.0278(8) 0.0315(8) 0.0013(6) 0.0040(7) -0.0038(7) C13 0.0248(8) 0.0324(9) 0.0581(13) -0.0007(9) 0.0015(8) -0.0049(8) C14 0.0438(11) 0.0482(12) 0.0368(10) 0.0022(9) 0.0134(9) -0.0054(10) C15 0.0352(10) 0.0272(8) 0.0411(10) 0.0064(7) 0.0017(8) -0.0038(8) N1 0.0202(6) 0.0231(6) 0.0264(6) -0.0017(5) 0.0008(5) -0.0002(5) Si1 0.0208(2) 0.0210(2) 0.0379(3) -0.00478(17) -0.00157(18) 0.00102(16) P1 0.0218(2) 0.02246(19) 0.0220(2) -0.00191(15) -0.00053(15) 0.00186(15) Cl1 0.0344(2) 0.0380(2) 0.0288(2) 0.00114(16) -0.00831(16) 0.00531(17) _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 C2 1.496(2) . ? C1 C5 1.507(2) . ? C1 C6 1.537(2) . ? C1 Si1 1.9051(16) . ? C2 C3 1.356(2) . ? C2 C7 1.499(2) . ? C3 C4 1.460(2) . ? C3 C8 1.496(2) . ? C4 C5 1.363(2) . ? C4 C9 1.499(2) . ? C5 P1 1.7901(16) . ? C10 Si1 1.855(2) . ? C11 Si1 1.868(2) . ? C12 N1 1.504(2) . ? C12 C13 1.527(2) . ? C12 C15 1.532(2) . ? C12 C14 1.534(3) . ? N1 P1 1.6888(14) . ? N1 Si1 1.7738(14) . ? P1 Cl1 2.1863(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C5 102.64(13) . . ? C2 C1 C6 114.54(13) . . ? C5 C1 C6 117.22(13) . . ? C2 C1 Si1 115.59(11) . . ? C5 C1 Si1 94.99(9) . . ? C6 C1 Si1 110.32(11) . . ? C3 C2 C1 110.00(13) . . ? C3 C2 C7 127.57(16) . . ? C1 C2 C7 122.42(15) . . ? C2 C3 C4 108.96(14) . . ? C2 C3 C8 127.98(16) . . ? C4 C3 C8 123.04(15) . . ? C5 C4 C3 108.95(13) . . ? C5 C4 C9 127.59(14) . . ? C3 C4 C9 123.28(14) . . ? C4 C5 C1 109.29(13) . . ? C4 C5 P1 125.96(11) . . ? C1 C5 P1 120.50(11) . . ? N1 C12 C13 109.52(13) . . ? N1 C12 C15 110.75(13) . . ? C13 C12 C15 107.90(14) . . ? N1 C12 C14 108.83(14) . . ? C13 C12 C14 110.67(16) . . ? C15 C12 C14 109.17(15) . . ? C12 N1 P1 120.25(10) . . ? C12 N1 Si1 125.73(10) . . ? P1 N1 Si1 113.88(7) . . ? N1 Si1 C10 111.56(8) . . ? N1 Si1 C11 115.00(9) . . ? C10 Si1 C11 110.10(12) . . ? N1 Si1 C1 98.31(6) . . ? C10 Si1 C1 110.59(9) . . ? C11 Si1 C1 110.76(9) . . ? N1 P1 C5 93.61(6) . . ? N1 P1 Cl1 104.90(5) . . ? C5 P1 Cl1 100.72(5) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.274 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.048 data_pca21new _database_code_CSD 200132 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido arsenium aluminum tetrachloride ; _chemical_name_common '(CGC)phosphium arsenium tetrachloride' _chemical_melting_point ? _chemical_formula_moiety '[C15 H27 N As Si][Al Cl4]' _chemical_formula_sum 'C30 H54 Al2 As2 Cl8 N2 Si2' _chemical_formula_weight 986.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' As As 0.0499 2.0058 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pca2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x+1/2, -y, z' '-x+1/2, y, z+1/2' _cell_length_a 18.184(4) _cell_length_b 8.2774(17) _cell_length_c 30.284(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4558.2(16) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.02 _cell_measurement_theta_max 30.49 _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.437 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 2.050 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.6846 _exptl_absorpt_correction_T_max 0.6846 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9823 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0563 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 30.49 _reflns_number_total 9823 _reflns_number_gt 7802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1054P)^2^+4.2551P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.488(13) _refine_ls_number_reflns 9823 _refine_ls_number_parameters 434 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0918 _refine_ls_R_factor_gt 0.0678 _refine_ls_wR_factor_ref 0.1720 _refine_ls_wR_factor_gt 0.1544 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.034 _refine_ls_shift/su_mean 0.003 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 C26 C 0.1269(4) 0.7249(9) 0.4019(3) 0.0320(16) Uani 1 1 d . . . H26A H 0.1477 0.6417 0.3826 0.048 Uiso 1 1 calc R . . H26B H 0.0731 0.7187 0.4011 0.048 Uiso 1 1 calc R . . H26C H 0.1440 0.7073 0.4322 0.048 Uiso 1 1 calc R . . C1 C 0.0959(4) 0.6067(8) 0.1772(2) 0.0277(14) Uani 1 1 d . . . C2 C 0.1268(4) 0.5618(9) 0.2213(2) 0.0335(15) Uani 1 1 d . . . C3 C 0.0734(6) 0.5207(10) 0.2504(4) 0.039(2) Uani 1 1 d . . . C4 C 0.0017(4) 0.5391(11) 0.2280(3) 0.0337(16) Uani 1 1 d . . . C5 C 0.0146(4) 0.5929(8) 0.1854(3) 0.0315(15) Uani 1 1 d . . . C6 C 0.1223(4) 0.7772(9) 0.1622(3) 0.0325(17) Uani 1 1 d . . . H6A H 0.1097 0.8569 0.1849 0.049 Uiso 1 1 calc R . . H6B H 0.0981 0.8062 0.1344 0.049 Uiso 1 1 calc R . . H6C H 0.1757 0.7758 0.1579 0.049 Uiso 1 1 calc R . . C7 C 0.2083(5) 0.5540(13) 0.2307(3) 0.051(2) Uani 1 1 d . . . H7A H 0.2162 0.5375 0.2624 0.076 Uiso 1 1 calc R . . H7B H 0.2315 0.6555 0.2215 0.076 Uiso 1 1 calc R . . H7C H 0.2301 0.4640 0.2142 0.076 Uiso 1 1 calc R . . C8 C 0.0782(6) 0.4662(13) 0.2962(3) 0.048(2) Uani 1 1 d . . . H8A H 0.0479 0.3693 0.3001 0.072 Uiso 1 1 calc R . . H8B H 0.0605 0.5518 0.3158 0.072 Uiso 1 1 calc R . . H8C H 0.1295 0.4409 0.3033 0.072 Uiso 1 1 calc R . . C9 C -0.0691(5) 0.5092(12) 0.2502(4) 0.048(3) Uani 1 1 d . . . H9A H -0.1092 0.5522 0.2320 0.072 Uiso 1 1 calc R . . H9B H -0.0693 0.5628 0.2790 0.072 Uiso 1 1 calc R . . H9C H -0.0760 0.3927 0.2542 0.072 Uiso 1 1 calc R . . C10 C 0.1018(4) 0.2458(9) 0.1489(3) 0.0388(19) Uani 1 1 d . . . H10A H 0.0626 0.2347 0.1710 0.058 Uiso 1 1 calc R . . H10B H 0.1489 0.2143 0.1620 0.058 Uiso 1 1 calc R . . H10C H 0.0910 0.1757 0.1236 0.058 Uiso 1 1 calc R . . C11 C 0.1933(5) 0.5018(9) 0.0961(4) 0.038(3) Uani 1 1 d . . . H11A H 0.2349 0.4420 0.1086 0.057 Uiso 1 1 calc R . . H11B H 0.2041 0.6178 0.0968 0.057 Uiso 1 1 calc R . . H11C H 0.1853 0.4674 0.0655 0.057 Uiso 1 1 calc R . . C12 C 0.0109(5) 0.4919(8) 0.0535(3) 0.026(2) Uani 1 1 d . . . C13 C 0.0396(5) 0.3281(9) 0.0373(3) 0.0371(19) Uani 1 1 d . . . H13A H 0.0168 0.2414 0.0546 0.056 Uiso 1 1 calc R . . H13B H 0.0931 0.3239 0.0411 0.056 Uiso 1 1 calc R . . H13C H 0.0274 0.3143 0.0060 0.056 Uiso 1 1 calc R . . C14 C -0.0736(7) 0.4946(13) 0.0413(4) 0.055(3) Uani 1 1 d . . . H14A H -0.0998 0.4145 0.0592 0.082 Uiso 1 1 calc R . . H14B H -0.0797 0.4685 0.0099 0.082 Uiso 1 1 calc R . . H14C H -0.0937 0.6023 0.0471 0.082 Uiso 1 1 calc R . . C15 C 0.0460(5) 0.6322(12) 0.0287(3) 0.042(2) Uani 1 1 d . . . H15A H 0.0271 0.7344 0.0404 0.063 Uiso 1 1 calc R . . H15B H 0.0341 0.6241 -0.0027 0.063 Uiso 1 1 calc R . . H15C H 0.0995 0.6284 0.0326 0.063 Uiso 1 1 calc R . . C21 C 0.1523(4) 0.8957(8) 0.3858(2) 0.0288(14) Uani 1 1 d . . . C22 C 0.1223(4) 0.9484(10) 0.3424(2) 0.0328(15) Uani 1 1 d . . . C23 C 0.1800(5) 0.9804(10) 0.3140(3) 0.0310(19) Uani 1 1 d . . . C24 C 0.2474(4) 0.9520(9) 0.3361(3) 0.0314(15) Uani 1 1 d . . . C25 C 0.2337(4) 0.9067(8) 0.3784(2) 0.0287(14) Uani 1 1 d . . . C27 C 0.0411(4) 0.9463(11) 0.3326(3) 0.0435(19) Uani 1 1 d . . . H27A H 0.0260 1.0524 0.3215 0.065 Uiso 1 1 calc R . . H27B H 0.0139 0.9215 0.3597 0.065 Uiso 1 1 calc R . . H27C H 0.0308 0.8637 0.3103 0.065 Uiso 1 1 calc R . . C28 C 0.1721(7) 1.0360(15) 0.2668(3) 0.058(3) Uani 1 1 d . . . H28A H 0.1207 1.0251 0.2576 0.087 Uiso 1 1 calc R . . H28B H 0.2034 0.9696 0.2477 0.087 Uiso 1 1 calc R . . H28C H 0.1872 1.1494 0.2645 0.087 Uiso 1 1 calc R . . C29 C 0.3247(6) 0.9873(11) 0.3166(3) 0.044(3) Uani 1 1 d . . . H29A H 0.3249 1.0949 0.3031 0.067 Uiso 1 1 calc R . . H29B H 0.3365 0.9061 0.2941 0.067 Uiso 1 1 calc R . . H29C H 0.3615 0.9832 0.3402 0.067 Uiso 1 1 calc R . . C30 C 0.1489(4) 1.2555(8) 0.4128(3) 0.0361(18) Uani 1 1 d . . . H30A H 0.1508 1.3304 0.4378 0.054 Uiso 1 1 calc R . . H30B H 0.1057 1.2798 0.3946 0.054 Uiso 1 1 calc R . . H30C H 0.1935 1.2675 0.3949 0.054 Uiso 1 1 calc R . . C31 C 0.0577(5) 1.0083(9) 0.4633(3) 0.031(2) Uani 1 1 d . . . H31A H 0.0516 1.0909 0.4862 0.046 Uiso 1 1 calc R . . H31B H 0.0592 0.9012 0.4770 0.046 Uiso 1 1 calc R . . H31C H 0.0162 1.0136 0.4426 0.046 Uiso 1 1 calc R . . C32 C 0.2420(6) 1.0027(8) 0.5113(3) 0.032(2) Uani 1 1 d . . . C33 C 0.1993(5) 0.8674(11) 0.5352(3) 0.041(2) Uani 1 1 d . . . H33A H 0.2205 0.7624 0.5274 0.062 Uiso 1 1 calc R . . H33B H 0.1476 0.8706 0.5262 0.062 Uiso 1 1 calc R . . H33C H 0.2028 0.8834 0.5672 0.062 Uiso 1 1 calc R . . C34 C 0.2109(5) 1.1656(11) 0.5257(3) 0.051(2) Uani 1 1 d . . . H34A H 0.2137 1.1747 0.5579 0.077 Uiso 1 1 calc R . . H34B H 0.1595 1.1741 0.5163 0.077 Uiso 1 1 calc R . . H34C H 0.2396 1.2527 0.5121 0.077 Uiso 1 1 calc R . . C35 C 0.3221(6) 0.9911(9) 0.5194(3) 0.036(2) Uani 1 1 d . . . H35A H 0.3316 0.9982 0.5512 0.055 Uiso 1 1 calc R . . H35B H 0.3473 1.0797 0.5042 0.055 Uiso 1 1 calc R . . H35C H 0.3404 0.8875 0.5082 0.055 Uiso 1 1 calc R . . N1 N 0.0240(3) 0.5083(5) 0.0996(2) 0.0151(13) Uani 1 1 d . . . N2 N 0.2270(4) 0.9881(7) 0.4603(3) 0.0294(18) Uani 1 1 d . . . Al1 Al -0.10935(14) 0.0161(3) 0.16490(10) 0.0261(5) Uani 1 1 d . . . Al2 Al -0.14250(14) 0.5222(3) 0.39803(10) 0.0277(5) Uani 1 1 d . . . Si1 Si 0.10684(10) 0.4593(3) 0.13012(7) 0.0253(4) Uani 1 1 d . . . Si2 Si 0.14258(10) 1.0437(3) 0.43368(7) 0.0261(4) Uani 1 1 d . . . Cl1 Cl -0.04205(13) 0.0202(3) 0.22208(8) 0.0451(6) Uani 1 1 d . . . Cl2 Cl -0.15107(11) 0.2545(2) 0.15291(7) 0.0426(4) Uani 1 1 d . . . Cl3 Cl -0.04668(9) -0.0576(2) 0.10830(6) 0.0327(4) Uani 1 1 d . . . Cl4 Cl -0.19699(12) -0.1489(3) 0.17287(10) 0.0619(7) Uani 1 1 d . . . Cl21 Cl -0.20718(9) 0.4468(3) 0.45407(6) 0.0327(4) Uani 1 1 d . . . Cl22 Cl -0.20825(14) 0.5383(4) 0.34084(9) 0.0518(6) Uani 1 1 d . . . Cl23 Cl -0.05585(11) 0.3535(3) 0.38964(9) 0.0523(6) Uani 1 1 d . . . Cl24 Cl -0.09890(11) 0.7560(2) 0.41367(7) 0.0439(4) Uani 1 1 d . . . As1 As -0.04872(3) 0.57617(7) 0.13703(2) 0.02673(16) Uani 1 1 d . . . As2 As 0.29747(4) 0.91995(8) 0.42643(2) 0.02663(16) 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 C26 0.035(4) 0.032(4) 0.029(4) 0.003(3) 0.003(3) -0.003(3) C1 0.023(3) 0.032(3) 0.027(3) 0.000(3) 0.000(3) 0.000(3) C2 0.038(4) 0.035(4) 0.027(4) -0.003(3) -0.004(3) -0.008(3) C3 0.039(5) 0.042(4) 0.036(5) -0.003(4) 0.003(4) -0.015(3) C4 0.033(4) 0.048(4) 0.020(3) -0.006(4) 0.009(3) -0.002(4) C5 0.026(3) 0.035(3) 0.033(4) -0.002(3) 0.004(3) 0.001(3) C6 0.023(4) 0.031(4) 0.043(4) 0.002(3) 0.003(3) -0.005(3) C7 0.038(5) 0.071(6) 0.043(5) 0.010(5) -0.014(4) -0.009(4) C8 0.045(5) 0.071(5) 0.028(4) -0.012(4) 0.014(4) -0.004(5) C9 0.017(4) 0.075(7) 0.052(6) -0.010(4) -0.010(4) -0.011(3) C10 0.034(4) 0.037(4) 0.045(5) 0.003(4) -0.002(3) -0.001(3) C11 0.019(4) 0.048(6) 0.047(6) -0.006(3) 0.019(4) 0.002(3) C12 0.027(5) 0.025(4) 0.027(5) -0.002(2) -0.003(4) 0.001(2) C13 0.053(5) 0.030(4) 0.028(4) -0.021(3) -0.003(3) 0.004(3) C14 0.046(7) 0.090(9) 0.028(6) 0.006(4) 0.005(5) -0.006(4) C15 0.051(5) 0.052(5) 0.023(4) 0.020(4) 0.001(3) -0.007(4) C21 0.020(3) 0.031(3) 0.035(4) -0.001(3) 0.001(3) -0.005(3) C22 0.030(4) 0.048(4) 0.021(3) -0.003(3) -0.003(3) 0.002(3) C23 0.034(5) 0.049(4) 0.010(3) -0.001(3) -0.002(3) 0.005(3) C24 0.035(4) 0.030(3) 0.030(4) -0.004(3) 0.007(3) -0.005(3) C25 0.025(4) 0.034(3) 0.027(3) -0.004(3) 0.004(3) 0.000(3) C27 0.029(4) 0.058(5) 0.043(5) -0.001(4) -0.008(4) 0.005(4) C28 0.066(7) 0.083(6) 0.023(4) 0.027(5) -0.012(4) -0.012(6) C29 0.048(6) 0.065(6) 0.020(4) -0.003(3) 0.030(4) 0.003(4) C30 0.035(4) 0.022(3) 0.051(5) 0.006(3) 0.000(3) -0.004(3) C31 0.032(5) 0.035(5) 0.024(4) 0.002(3) 0.002(4) -0.001(3) C32 0.049(6) 0.033(5) 0.013(4) -0.001(2) -0.004(4) -0.004(3) C33 0.048(5) 0.034(4) 0.041(5) 0.001(4) 0.001(4) 0.001(3) C34 0.073(6) 0.044(5) 0.036(5) -0.011(4) -0.006(4) 0.012(4) C35 0.039(6) 0.042(5) 0.028(5) -0.002(3) -0.027(4) -0.003(3) N1 0.013(3) 0.020(3) 0.013(3) 0.0033(17) 0.006(2) -0.0020(16) N2 0.032(4) 0.025(3) 0.031(4) -0.009(2) -0.004(3) -0.001(2) Al1 0.0213(12) 0.0335(11) 0.0235(12) -0.0016(9) 0.0020(10) 0.0013(8) Al2 0.0196(12) 0.0352(10) 0.0284(13) 0.0055(10) -0.0002(10) 0.0013(8) Si1 0.0189(9) 0.0328(8) 0.0241(10) -0.0016(9) 0.0023(7) -0.0012(8) Si2 0.0221(10) 0.0282(8) 0.0280(10) 0.0009(9) 0.0025(7) 0.0016(8) Cl1 0.0370(12) 0.0789(14) 0.0194(10) 0.0001(9) -0.0039(8) 0.0104(10) Cl2 0.0470(11) 0.0373(9) 0.0436(10) -0.0056(8) -0.0024(8) 0.0116(8) Cl3 0.0322(10) 0.0343(10) 0.0315(10) -0.0046(8) 0.0034(6) 0.0036(7) Cl4 0.0409(12) 0.0563(13) 0.089(2) -0.0185(13) 0.0276(12) -0.0195(9) Cl21 0.0286(9) 0.0425(11) 0.0269(9) 0.0044(8) 0.0045(6) 0.0011(7) Cl22 0.0389(13) 0.0839(15) 0.0326(13) 0.0005(12) -0.0039(9) -0.0005(11) Cl23 0.0374(10) 0.0513(12) 0.0682(15) 0.0092(11) 0.0195(10) 0.0158(8) Cl24 0.0452(11) 0.0362(9) 0.0504(11) 0.0017(8) 0.0004(8) -0.0114(7) As1 0.0204(3) 0.0300(3) 0.0297(3) -0.0031(3) 0.0001(2) 0.0004(2) As2 0.0214(3) 0.0293(3) 0.0292(3) -0.0021(3) 0.0003(3) -0.0013(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 C26 C21 1.565(9) . ? C1 C2 1.497(10) . ? C1 C5 1.503(9) . ? C1 C6 1.559(10) . ? C1 Si1 1.888(7) . ? C2 C3 1.354(13) . ? C2 C7 1.510(11) . ? C3 C8 1.461(14) . ? C3 C4 1.477(13) . ? C4 C5 1.385(11) . ? C4 C9 1.474(13) . ? C5 As1 1.867(8) . ? C10 Si1 1.859(8) . ? C11 Si1 1.912(9) . ? C12 N1 1.424(12) . ? C12 C15 1.522(12) . ? C12 C13 1.533(10) . ? C12 C14 1.579(16) . ? C21 C22 1.486(10) . ? C21 C25 1.500(9) . ? C21 Si2 1.908(8) . ? C22 C23 1.383(12) . ? C22 C27 1.505(11) . ? C23 C24 1.416(12) . ? C23 C28 1.509(11) . ? C24 C25 1.358(11) . ? C24 C29 1.552(12) . ? C25 As2 1.864(7) . ? C30 Si2 1.867(7) . ? C31 Si2 1.809(10) . ? C32 C35 1.481(15) . ? C32 C34 1.526(12) . ? C32 C33 1.543(12) . ? C32 N2 1.574(12) . ? N1 Si1 1.814(7) . ? N1 As1 1.830(6) . ? N2 As2 1.735(8) . ? N2 Si2 1.793(8) . ? Al1 Cl4 2.112(3) . ? Al1 Cl1 2.121(4) . ? Al1 Cl2 2.145(3) . ? Al1 Cl3 2.147(3) . ? Al2 Cl22 2.109(4) . ? Al2 Cl23 2.121(3) . ? Al2 Cl24 2.144(3) . ? Al2 Cl21 2.157(3) . ? 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 C2 C1 C5 101.8(6) . . ? C2 C1 C6 111.6(6) . . ? C5 C1 C6 114.8(6) . . ? C2 C1 Si1 118.3(5) . . ? C5 C1 Si1 100.3(5) . . ? C6 C1 Si1 109.4(5) . . ? C3 C2 C1 111.8(7) . . ? C3 C2 C7 124.9(8) . . ? C1 C2 C7 123.1(7) . . ? C2 C3 C8 130.6(10) . . ? C2 C3 C4 108.0(9) . . ? C8 C3 C4 121.4(9) . . ? C5 C4 C9 128.8(8) . . ? C5 C4 C3 108.2(7) . . ? C9 C4 C3 123.0(9) . . ? C4 C5 C1 110.1(7) . . ? C4 C5 As1 127.0(6) . . ? C1 C5 As1 118.9(5) . . ? N1 C12 C15 109.8(7) . . ? N1 C12 C13 109.9(7) . . ? C15 C12 C13 112.0(8) . . ? N1 C12 C14 113.0(8) . . ? C15 C12 C14 106.4(7) . . ? C13 C12 C14 105.7(7) . . ? C22 C21 C25 102.3(6) . . ? C22 C21 C26 115.7(6) . . ? C25 C21 C26 113.1(6) . . ? C22 C21 Si2 116.7(5) . . ? C25 C21 Si2 99.5(4) . . ? C26 C21 Si2 108.4(5) . . ? C23 C22 C21 109.1(7) . . ? C23 C22 C27 128.6(7) . . ? C21 C22 C27 122.1(7) . . ? C22 C23 C24 109.4(7) . . ? C22 C23 C28 125.2(9) . . ? C24 C23 C28 125.5(9) . . ? C25 C24 C23 109.4(7) . . ? C25 C24 C29 125.3(8) . . ? C23 C24 C29 124.9(8) . . ? C24 C25 C21 109.8(6) . . ? C24 C25 As2 127.3(6) . . ? C21 C25 As2 120.1(5) . . ? C35 C32 C34 112.0(7) . . ? C35 C32 C33 111.7(7) . . ? C34 C32 C33 108.7(9) . . ? C35 C32 N2 109.2(8) . . ? C34 C32 N2 106.5(7) . . ? C33 C32 N2 108.5(7) . . ? C12 N1 Si1 128.2(6) . . ? C12 N1 As1 121.1(6) . . ? Si1 N1 As1 110.7(4) . . ? C32 N2 As2 118.4(7) . . ? C32 N2 Si2 124.7(7) . . ? As2 N2 Si2 116.8(5) . . ? Cl4 Al1 Cl1 110.63(17) . . ? Cl4 Al1 Cl2 110.32(15) . . ? Cl1 Al1 Cl2 109.13(14) . . ? Cl4 Al1 Cl3 107.94(14) . . ? Cl1 Al1 Cl3 110.50(14) . . ? Cl2 Al1 Cl3 108.30(15) . . ? Cl22 Al2 Cl23 111.38(17) . . ? Cl22 Al2 Cl24 109.51(15) . . ? Cl23 Al2 Cl24 110.25(14) . . ? Cl22 Al2 Cl21 110.82(14) . . ? Cl23 Al2 Cl21 107.98(14) . . ? Cl24 Al2 Cl21 106.79(15) . . ? N1 Si1 C10 109.1(3) . . ? N1 Si1 C1 98.8(3) . . ? C10 Si1 C1 112.2(3) . . ? N1 Si1 C11 111.5(4) . . ? C10 Si1 C11 112.4(4) . . ? C1 Si1 C11 112.0(4) . . ? N2 Si2 C31 117.8(4) . . ? N2 Si2 C30 109.9(3) . . ? C31 Si2 C30 111.9(4) . . ? N2 Si2 C21 95.6(3) . . ? C31 Si2 C21 110.6(4) . . ? C30 Si2 C21 109.8(4) . . ? N1 As1 C5 93.6(3) . . ? N2 As2 C25 91.2(3) . . ? _diffrn_measured_fraction_theta_max 0.846 _diffrn_reflns_theta_full 30.49 _diffrn_measured_fraction_theta_full 0.846 _refine_diff_density_max 5.011 _refine_diff_density_min -0.991 _refine_diff_density_rms 0.150 data_p1bar _database_code_CSD 200133 _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl(dimetyl(tetra-methylcyclopentadienyl)silyl)amido stibocenium aluminum tetrachloride ; _chemical_name_common '(CGC)phosphium stibocenium tetrachloride' _chemical_melting_point ? _chemical_formula_moiety '[C15 H27 N Sb Si][Al Cl4]' _chemical_formula_sum 'C15 H27 Al Cl4 N Sb Si' _chemical_formula_weight 540.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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 10.064(5) _cell_length_b 11.154(5) _cell_length_c 12.120(5) _cell_angle_alpha 92.411(5) _cell_angle_beta 114.403(5) _cell_angle_gamma 110.722(5) _cell_volume 1130.2(9) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 3.04 _cell_measurement_theta_max 27.48 _exptl_crystal_description prism _exptl_crystal_colour red-orange _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.587 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 540 _exptl_absorpt_coefficient_mu 1.784 _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 293(2) _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 'Nonius Kappa CCD' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8924 _diffrn_reflns_av_R_equivalents 0.0146 _diffrn_reflns_av_sigmaI/netI 0.0324 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _reflns_number_total 5163 _reflns_number_gt 4752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement Denzo-SMN _computing_data_reduction Scalepack _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.0000P)^2^+0.5814P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5163 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0240 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0443 _refine_ls_wR_factor_gt 0.0431 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.004 _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 Sb1 Sb 0.496932(13) 0.121191(11) 0.834837(10) 0.01820(4) Uani 1 1 d . . . Cl1 Cl 0.82678(6) 0.11117(5) 1.16284(5) 0.03715(12) Uani 1 1 d . . . Cl4 Cl 0.78249(6) 0.38476(5) 1.05565(5) 0.03713(12) Uani 1 1 d . . . Cl2 Cl 1.14184(6) 0.35112(5) 1.14188(5) 0.03664(12) Uani 1 1 d . . . Cl3 Cl 1.03308(7) 0.42010(6) 1.36889(5) 0.04487(14) Uani 1 1 d . . . Si1 Si 0.39787(6) 0.20460(5) 0.59933(4) 0.02063(11) Uani 1 1 d . . . Al1 Al 0.95017(6) 0.31971(5) 1.18554(5) 0.02307(12) Uani 1 1 d . . . C6 C 0.2696(3) -0.1367(2) 0.5728(2) 0.0348(5) Uani 1 1 d . . . C5 C 0.6805(2) 0.14216(19) 0.74453(16) 0.0221(4) Uani 1 1 d . . . C2 C 0.4404(2) -0.04340(18) 0.65468(16) 0.0220(4) Uani 1 1 d . . . C9 C 0.8066(3) 0.2782(2) 0.7741(2) 0.0322(5) Uani 1 1 d . . . C12 C 0.3137(2) 0.30655(18) 0.77880(17) 0.0231(4) Uani 1 1 d . . . C1 C 0.5098(2) 0.09588(17) 0.65650(15) 0.0190(4) Uani 1 1 d . . . N1 N 0.38297(16) 0.22723(14) 0.73738(13) 0.0186(3) Uani 1 1 d . . . C3 C 0.5646(2) -0.08019(19) 0.73154(17) 0.0254(4) Uani 1 1 d . . . C4 C 0.7092(2) 0.0313(2) 0.78393(16) 0.0253(4) Uani 1 1 d . . . C15 C 0.3176(3) 0.2799(3) 0.9015(2) 0.0353(5) Uani 1 1 d . . . C13 C 0.4136(4) 0.4518(2) 0.7960(3) 0.0491(7) Uani 1 1 d . . . C14 C 0.1415(3) 0.2678(3) 0.6820(2) 0.0480(7) Uani 1 1 d . . . C10 C 0.2038(3) 0.1182(3) 0.4582(2) 0.0382(5) Uani 1 1 d . . . C11 C 0.5141(4) 0.3562(2) 0.5659(3) 0.0415(6) Uani 1 1 d . . . C8 C 0.8686(3) 0.0347(3) 0.8721(2) 0.0415(6) Uani 1 1 d . . . C7 C 0.5408(4) -0.2140(3) 0.7575(3) 0.0459(6) Uani 1 1 d . . . H14A H 0.085(3) 0.178(3) 0.674(3) 0.058(9) Uiso 1 1 d . . . H9C H 0.773(3) 0.347(3) 0.787(2) 0.047(7) Uiso 1 1 d . . . H15B H 0.425(3) 0.306(3) 0.966(2) 0.055(8) Uiso 1 1 d . . . H9A H 0.828(3) 0.291(2) 0.709(2) 0.043(7) Uiso 1 1 d . . . H9B H 0.908(3) 0.295(2) 0.849(2) 0.046(7) Uiso 1 1 d . . . H15C H 0.274(3) 0.333(2) 0.929(2) 0.036(6) Uiso 1 1 d . . . H15A H 0.258(3) 0.189(3) 0.897(2) 0.057(8) Uiso 1 1 d . . . H14B H 0.134(3) 0.284(3) 0.603(3) 0.070(9) Uiso 1 1 d . . . H14C H 0.096(3) 0.318(3) 0.707(2) 0.051(7) Uiso 1 1 d . . . H10C H 0.122(3) 0.051(3) 0.472(2) 0.042(7) Uiso 1 1 d . . . H6A H 0.195(3) -0.104(3) 0.577(2) 0.050(7) Uiso 1 1 d . . . H11A H 0.595(4) 0.419(3) 0.636(3) 0.070(9) Uiso 1 1 d . . . H6B H 0.250(3) -0.213(3) 0.596(2) 0.048(7) Uiso 1 1 d . . . H6C H 0.253(3) -0.147(2) 0.491(3) 0.050(7) Uiso 1 1 d . . . H10B H 0.222(3) 0.079(3) 0.403(2) 0.052(8) Uiso 1 1 d . . . H11B H 0.557(4) 0.335(3) 0.514(3) 0.077(10) Uiso 1 1 d . . . H10A H 0.162(3) 0.178(3) 0.427(3) 0.062(8) Uiso 1 1 d . . . H11C H 0.446(4) 0.393(3) 0.525(3) 0.081(10) Uiso 1 1 d . . . H7B H 0.435(4) -0.272(4) 0.717(3) 0.091(12) Uiso 1 1 d . . . H8B H 0.913(4) 0.011(4) 0.835(3) 0.100(13) Uiso 1 1 d . . . H8C H 0.930(4) 0.105(4) 0.930(3) 0.084(11) Uiso 1 1 d . . . H31C H 0.598(5) -0.211(4) 0.830(4) 0.106(14) Uiso 1 1 d . . . H8A H 0.858(4) -0.020(4) 0.923(4) 0.106(14) Uiso 1 1 d . . . H7C H 0.595(5) -0.248(4) 0.731(4) 0.113(14) Uiso 1 1 d . . . H13C H 0.371(3) 0.506(3) 0.826(2) 0.058(8) Uiso 1 1 d . . . H13B H 0.532(4) 0.478(3) 0.858(3) 0.094(11) Uiso 1 1 d . . . H13A H 0.406(3) 0.466(3) 0.719(3) 0.059(8) 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 Sb1 0.01957(7) 0.02052(7) 0.01592(6) 0.00426(4) 0.00822(5) 0.00953(5) Cl1 0.0381(3) 0.0228(2) 0.0472(3) 0.0047(2) 0.0247(2) 0.0031(2) Cl4 0.0334(3) 0.0385(3) 0.0369(3) 0.0031(2) 0.0082(2) 0.0219(2) Cl2 0.0266(2) 0.0328(3) 0.0529(3) 0.0064(2) 0.0230(2) 0.0093(2) Cl3 0.0546(3) 0.0373(3) 0.0281(3) -0.0020(2) 0.0179(2) 0.0053(3) Si1 0.0237(3) 0.0225(2) 0.0177(2) 0.00612(19) 0.0085(2) 0.0126(2) Al1 0.0202(3) 0.0210(3) 0.0248(3) 0.0028(2) 0.0097(2) 0.0059(2) C6 0.0314(12) 0.0279(11) 0.0299(12) -0.0005(9) 0.0097(9) 0.0020(10) C5 0.0193(9) 0.0284(10) 0.0205(9) 0.0021(7) 0.0105(7) 0.0104(8) C2 0.0259(9) 0.0204(9) 0.0200(9) 0.0025(7) 0.0112(7) 0.0091(8) C9 0.0261(11) 0.0341(12) 0.0297(11) -0.0001(9) 0.0151(9) 0.0031(9) C12 0.0214(9) 0.0223(9) 0.0283(10) 0.0017(7) 0.0115(8) 0.0120(8) C1 0.0208(9) 0.0217(9) 0.0173(8) 0.0029(7) 0.0104(7) 0.0097(7) N1 0.0177(7) 0.0178(7) 0.0195(7) 0.0020(6) 0.0073(6) 0.0083(6) C3 0.0369(11) 0.0262(10) 0.0206(9) 0.0058(7) 0.0145(8) 0.0191(9) C4 0.0276(10) 0.0376(11) 0.0185(9) 0.0044(8) 0.0107(8) 0.0216(9) C15 0.0410(13) 0.0434(14) 0.0336(12) 0.0054(10) 0.0213(10) 0.0255(11) C13 0.0674(19) 0.0232(11) 0.080(2) 0.0065(12) 0.0543(17) 0.0195(12) C14 0.0329(13) 0.072(2) 0.0373(14) -0.0068(13) 0.0056(10) 0.0342(14) C10 0.0384(13) 0.0500(15) 0.0211(11) -0.0014(10) 0.0023(9) 0.0273(12) C11 0.0566(16) 0.0359(13) 0.0490(15) 0.0249(12) 0.0348(14) 0.0225(13) C8 0.0380(13) 0.0631(17) 0.0293(12) 0.0046(12) 0.0086(10) 0.0358(13) C7 0.0694(19) 0.0321(13) 0.0396(14) 0.0133(11) 0.0193(14) 0.0306(14) _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 Sb1 N1 2.0169(15) . ? Sb1 C1 2.2304(19) . ? Sb1 C5 2.460(2) . ? Sb1 C2 2.5215(19) . ? Sb1 Si1 2.9215(11) . ? Cl1 Al1 2.1560(12) . ? Cl4 Al1 2.1494(10) . ? Cl2 Al1 2.1223(12) . ? Cl3 Al1 2.1179(11) . ? Si1 N1 1.7562(17) . ? Si1 C10 1.854(2) . ? Si1 C11 1.855(2) . ? Si1 C1 1.9007(19) . ? C6 C2 1.503(3) . ? C5 C4 1.424(3) . ? C5 C1 1.472(2) . ? C5 C9 1.502(3) . ? C2 C3 1.425(3) . ? C2 C1 1.455(3) . ? C12 N1 1.486(2) . ? C12 C15 1.516(3) . ? C12 C14 1.521(3) . ? C12 C13 1.525(3) . ? C3 C4 1.399(3) . ? C3 C7 1.494(3) . ? C4 C8 1.501(3) . ? 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 Sb1 C1 76.71(6) . . ? N1 Sb1 C5 99.03(7) . . ? C1 Sb1 C5 36.17(6) . . ? N1 Sb1 C2 98.38(7) . . ? C1 Sb1 C2 34.99(6) . . ? C5 Sb1 C2 55.63(6) . . ? N1 Sb1 Si1 36.13(4) . . ? C1 Sb1 Si1 40.59(5) . . ? C5 Sb1 Si1 67.31(5) . . ? C2 Sb1 Si1 66.60(5) . . ? N1 Si1 C10 114.67(11) . . ? N1 Si1 C11 115.25(11) . . ? C10 Si1 C11 107.75(13) . . ? N1 Si1 C1 92.38(7) . . ? C10 Si1 C1 112.96(10) . . ? C11 Si1 C1 113.41(11) . . ? N1 Si1 Sb1 42.62(5) . . ? C10 Si1 Sb1 125.95(10) . . ? C11 Si1 Sb1 126.26(9) . . ? C1 Si1 Sb1 49.77(5) . . ? Cl3 Al1 Cl2 111.37(4) . . ? Cl3 Al1 Cl4 109.79(4) . . ? Cl2 Al1 Cl4 109.58(5) . . ? Cl3 Al1 Cl1 110.62(4) . . ? Cl2 Al1 Cl1 108.12(3) . . ? Cl4 Al1 Cl1 107.25(4) . . ? C4 C5 C1 107.91(16) . . ? C4 C5 C9 125.52(18) . . ? C1 C5 C9 126.07(17) . . ? C4 C5 Sb1 93.44(12) . . ? C1 C5 Sb1 63.38(10) . . ? C9 C5 Sb1 115.25(13) . . ? C3 C2 C1 108.84(16) . . ? C3 C2 C6 125.26(18) . . ? C1 C2 C6 125.48(17) . . ? C3 C2 Sb1 91.88(11) . . ? C1 C2 Sb1 61.50(9) . . ? C6 C2 Sb1 117.93(14) . . ? N1 C12 C15 109.24(15) . . ? N1 C12 C14 109.29(16) . . ? C15 C12 C14 109.3(2) . . ? N1 C12 C13 108.83(16) . . ? C15 C12 C13 109.43(19) . . ? C14 C12 C13 110.7(2) . . ? C2 C1 C5 105.16(15) . . ? C2 C1 Si1 126.75(13) . . ? C5 C1 Si1 125.65(13) . . ? C2 C1 Sb1 83.50(10) . . ? C5 C1 Sb1 80.46(10) . . ? Si1 C1 Sb1 89.65(7) . . ? C12 N1 Si1 131.29(12) . . ? C12 N1 Sb1 127.39(12) . . ? Si1 N1 Sb1 101.26(7) . . ? C4 C3 C2 108.61(17) . . ? C4 C3 C7 126.2(2) . . ? C2 C3 C7 125.1(2) . . ? C3 C4 C5 109.31(16) . . ? C3 C4 C8 125.4(2) . . ? C5 C4 C8 125.3(2) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.375 _refine_diff_density_min -0.410 _refine_diff_density_rms 0.063