# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1330 data_jds-a _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li(tmeda)2][C(SiMe2PPh2)3]' _chemical_formula_analytical ? _chemical_formula_sum 'C55 H80 Li N4 P3 Si3' _chemical_formula_weight 981.35 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 15.023(4) _cell_length_b 16.592(4) _cell_length_c 23.174(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.78(3) _cell_angle_gamma 90.00 _cell_volume 5775.9(34) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method ? _exptl_crystal_F_000 2112 _exptl_absorpt_coefficient_mu 0.202 _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 8371 _diffrn_reflns_av_R_equivalents 0.0698 _diffrn_reflns_av_sigmaI/netI 0.1873 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.02 _diffrn_reflns_theta_max 22.99 _reflns_number_total 8027 _reflns_number_observed 4106 _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 (Sheldrick, 1993)' _refine_special_details ; 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^)+(0.0000P)^2^+13.9776P] 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 8026 _refine_ls_number_parameters 595 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1887 _refine_ls_R_factor_obs 0.0897 _refine_ls_wR_factor_all 0.1789 _refine_ls_wR_factor_obs 0.1445 _refine_ls_goodness_of_fit_all 1.088 _refine_ls_goodness_of_fit_obs 1.269 _refine_ls_restrained_S_all 1.088 _refine_ls_restrained_S_obs 1.269 _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 P1 P 0.07465(13) 0.19776(13) 0.13444(9) 0.0253(5) Uani 1 d . . P2 P 0.21801(14) 0.23226(13) -0.11360(9) 0.0286(6) Uani 1 d . . P3 P 0.36169(15) 0.37923(13) 0.11547(9) 0.0316(6) Uani 1 d . . Si1 Si 0.14168(15) 0.18056(13) 0.04588(9) 0.0269(6) Uani 1 d . . Si2 Si 0.24343(15) 0.30591(13) -0.03002(9) 0.0262(6) Uani 1 d . . Si3 Si 0.32745(14) 0.24797(13) 0.08660(9) 0.0265(5) Uani 1 d . . C1 C 0.2347(5) 0.2474(4) 0.0358(3) 0.025(2) Uani 1 d . . C2 C 0.0488(5) 0.1872(5) -0.0089(3) 0.039(2) Uani 1 d . . H2C H 0.0021(5) 0.1484(5) 0.0009(3) 0.058 Uiso 1 calc R . H2B H 0.0717(5) 0.1749(5) -0.0472(3) 0.058 Uiso 1 calc R . H2A H 0.0239(5) 0.2418(5) -0.0088(3) 0.058 Uiso 1 calc R . C3 C 0.1708(6) 0.0700(5) 0.0476(4) 0.044(2) Uani 1 d . . H3C H 0.1167(6) 0.0382(5) 0.0532(4) 0.066 Uiso 1 calc R . H3B H 0.2128(6) 0.0597(5) 0.0795(4) 0.066 Uiso 1 calc R . H3A H 0.1982(6) 0.0547(5) 0.0111(4) 0.066 Uiso 1 calc R . C4 C -0.0019(5) 0.2825(5) 0.1255(3) 0.028(2) Uani 1 d . . C5 C -0.0734(5) 0.2912(5) 0.1633(4) 0.041(2) Uani 1 d . . H5 H -0.0868(5) 0.2490(5) 0.1895(4) 0.049 Uiso 1 calc R . C6 C -0.1249(6) 0.3606(5) 0.1631(4) 0.044(2) Uani 1 d . . H6 H -0.1731(6) 0.3654(5) 0.1889(4) 0.052 Uiso 1 calc R . C7 C -0.1069(6) 0.4218(6) 0.1260(4) 0.046(3) Uani 1 d . . H7 H -0.1419(6) 0.4695(6) 0.1265(4) 0.056 Uiso 1 calc R . C8 C -0.0386(6) 0.4150(5) 0.0880(4) 0.038(2) Uani 1 d . . H8 H -0.0268(6) 0.4577(5) 0.0620(4) 0.045 Uiso 1 calc R . C9 C 0.0139(5) 0.3456(5) 0.0872(3) 0.029(2) Uani 1 d . . H9 H 0.0609(5) 0.3414(5) 0.0604(3) 0.035 Uiso 1 calc R . C10 C -0.0016(5) 0.1107(5) 0.1359(3) 0.027(2) Uani 1 d . . C11 C -0.0848(5) 0.1086(5) 0.1088(3) 0.032(2) Uani 1 d . . H11 H -0.1063(5) 0.1546(5) 0.0887(3) 0.039 Uiso 1 calc R . C12 C -0.1361(6) 0.0395(6) 0.1113(4) 0.047(3) Uani 1 d . . H12 H -0.1936(6) 0.0390(6) 0.0937(4) 0.057 Uiso 1 calc R . C13 C -0.1048(6) -0.0286(5) 0.1390(4) 0.045(3) Uani 1 d . . H13 H -0.1401(6) -0.0761(5) 0.1397(4) 0.054 Uiso 1 calc R . C14 C -0.0219(6) -0.0275(5) 0.1656(4) 0.048(3) Uani 1 d . . H14 H 0.0004(6) -0.0745(5) 0.1842(4) 0.057 Uiso 1 calc R . C15 C 0.0283(5) 0.0423(4) 0.1650(3) 0.032(2) Uani 1 d . . H15 H 0.0841(5) 0.0437(4) 0.1848(3) 0.038 Uiso 1 calc R . C16 C 0.1559(5) 0.3859(4) -0.0393(3) 0.033(2) Uani 1 d . . H16C H 0.1653(5) 0.4146(4) -0.0757(3) 0.050 Uiso 1 calc R . H16B H 0.1600(5) 0.4241(4) -0.0071(3) 0.050 Uiso 1 calc R . H16A H 0.0969(5) 0.3608(4) -0.0400(3) 0.050 Uiso 1 calc R . C17 C 0.3523(5) 0.3568(5) -0.0437(3) 0.032(2) Uani 1 d . . H17C H 0.3487(5) 0.3863(5) -0.0803(3) 0.048 Uiso 1 calc R . H17B H 0.3996(5) 0.3163(5) -0.0457(3) 0.048 Uiso 1 calc R . H17A H 0.3657(5) 0.3946(5) -0.0123(3) 0.048 Uiso 1 calc R . C18 C 0.3136(5) 0.1646(5) -0.1211(3) 0.028(2) Uani 1 d . . C19 C 0.3451(5) 0.1229(5) -0.0727(4) 0.040(2) Uani 1 d . . H19 H 0.3222(5) 0.1354(5) -0.0358(4) 0.048 Uiso 1 calc R . C20 C 0.4092(6) 0.0634(5) -0.0778(4) 0.048(3) Uani 1 d . . H20 H 0.4301(6) 0.0362(5) -0.0442(4) 0.058 Uiso 1 calc R . C21 C 0.4427(6) 0.0433(5) -0.1304(4) 0.044(2) Uani 1 d . . H21 H 0.4861(6) 0.0019(5) -0.1335(4) 0.052 Uiso 1 calc R . C22 C 0.4128(6) 0.0839(5) -0.1787(4) 0.042(2) Uani 1 d . . H22 H 0.4363(6) 0.0711(5) -0.2154(4) 0.050 Uiso 1 calc R . C23 C 0.3487(5) 0.1432(5) -0.1740(3) 0.036(2) Uani 1 d . . H23 H 0.3281(5) 0.1700(5) -0.2078(3) 0.043 Uiso 1 calc R . C24 C 0.2314(5) 0.3088(5) -0.1700(3) 0.031(2) Uani 1 d . . C25 C 0.3109(6) 0.3330(5) -0.1949(3) 0.037(2) Uani 1 d . . H25 H 0.3655(6) 0.3100(5) -0.1818(3) 0.044 Uiso 1 calc R . C26 C 0.3117(6) 0.3903(5) -0.2386(4) 0.045(2) Uani 1 d . . H26 H 0.3661(6) 0.4052(5) -0.2561(4) 0.054 Uiso 1 calc R . C27 C 0.2327(7) 0.4255(5) -0.2566(4) 0.047(3) Uani 1 d . . H27 H 0.2332(7) 0.4648(5) -0.2864(4) 0.056 Uiso 1 calc R . C28 C 0.1548(6) 0.4046(5) -0.2322(4) 0.048(3) Uani 1 d . . H28 H 0.1010(6) 0.4298(5) -0.2445(4) 0.058 Uiso 1 calc R . C29 C 0.1534(5) 0.3466(5) -0.1893(3) 0.036(2) Uani 1 d . . H29 H 0.0983(5) 0.3322(5) -0.1727(3) 0.043 Uiso 1 calc R . C30 C 0.4370(5) 0.2108(5) 0.0591(3) 0.043(2) Uani 1 d . . H30C H 0.4820(5) 0.2138(5) 0.0900(3) 0.064 Uiso 1 calc R . H30B H 0.4555(5) 0.2444(5) 0.0266(3) 0.064 Uiso 1 calc R . H30A H 0.4307(5) 0.1548(5) 0.0462(3) 0.064 Uiso 1 calc R . C31 C 0.3101(5) 0.1858(5) 0.1538(3) 0.038(2) Uani 1 d . . H31C H 0.3631(5) 0.1894(5) 0.1787(3) 0.058 Uiso 1 calc R . H31B H 0.2998(5) 0.1295(5) 0.1429(3) 0.058 Uiso 1 calc R . H31A H 0.2583(5) 0.2063(5) 0.1745(3) 0.058 Uiso 1 calc R . C32 C 0.2870(5) 0.3984(5) 0.1762(3) 0.032(2) Uani 1 d . . C33 C 0.1957(5) 0.3913(5) 0.1671(4) 0.035(2) Uani 1 d . . H33 H 0.1741(5) 0.3714(5) 0.1311(4) 0.042 Uiso 1 calc R . C34 C 0.1352(6) 0.4126(5) 0.2092(4) 0.042(2) Uani 1 d . . H34 H 0.0731(6) 0.4078(5) 0.2016(4) 0.051 Uiso 1 calc R . C35 C 0.1649(6) 0.4405(5) 0.2615(4) 0.041(2) Uani 1 d . . H35 H 0.1236(6) 0.4547(5) 0.2905(4) 0.049 Uiso 1 calc R . C36 C 0.2550(6) 0.4480(5) 0.2722(3) 0.039(2) Uani 1 d . . H36 H 0.2753(6) 0.4679(5) 0.3085(3) 0.047 Uiso 1 calc R . C37 C 0.3163(6) 0.4268(5) 0.2308(4) 0.037(2) Uani 1 d . . H37 H 0.3782(6) 0.4313(5) 0.2390(4) 0.045 Uiso 1 calc R . C38 C 0.4719(5) 0.3752(5) 0.1517(3) 0.033(2) Uani 1 d . . C39 C 0.4948(6) 0.3221(6) 0.1947(4) 0.053(3) Uani 1 d . . H39 H 0.4532(6) 0.2821(6) 0.2058(4) 0.064 Uiso 1 calc R . C40 C 0.5769(7) 0.3250(7) 0.2222(4) 0.060(3) Uani 1 d . . H40 H 0.5924(7) 0.2865(7) 0.2509(4) 0.072 Uiso 1 calc R . C41 C 0.6349(6) 0.3841(7) 0.2075(4) 0.059(3) Uani 1 d . . H41 H 0.6903(6) 0.3877(7) 0.2275(4) 0.071 Uiso 1 calc R . C42 C 0.6162(6) 0.4381(6) 0.1650(4) 0.054(3) Uani 1 d . . H42 H 0.6582(6) 0.4782(6) 0.1546(4) 0.065 Uiso 1 calc R . C43 C 0.5339(6) 0.4328(5) 0.1374(4) 0.040(2) Uani 1 d . . H43 H 0.5198(6) 0.4702(5) 0.1076(4) 0.048 Uiso 1 calc R . Li Li 0.2166(7) 0.2053(8) 0.4108(5) 0.026(3) Uani 1 d . . N1 N 0.2149(4) 0.3146(4) 0.4585(3) 0.033(2) Uani 1 d . . N2 N 0.1937(4) 0.1450(4) 0.4875(3) 0.037(2) Uani 1 d . . N3 N 0.3295(4) 0.1711(4) 0.3604(3) 0.038(2) Uani 1 d . . N4 N 0.1327(4) 0.1879(4) 0.3379(3) 0.031(2) Uani 1 d . . C44 C 0.1873(6) 0.2887(5) 0.5153(4) 0.051(3) Uani 1 d . . H44B H 0.1215(6) 0.2896(5) 0.5168(4) 0.061 Uiso 1 calc R . H44A H 0.2103(6) 0.3275(5) 0.5444(4) 0.061 Uiso 1 calc R . C45 C 0.2194(7) 0.2063(5) 0.5305(4) 0.054(3) Uani 1 d . . H45B H 0.2851(7) 0.2074(5) 0.5344(4) 0.065 Uiso 1 calc R . H45A H 0.1950(7) 0.1909(5) 0.5684(4) 0.065 Uiso 1 calc R . C46 C 0.3076(5) 0.3420(5) 0.4611(4) 0.050(3) Uani 1 d . . H46C H 0.3259(5) 0.3593(5) 0.4226(4) 0.075 Uiso 1 calc R . H46B H 0.3459(5) 0.2977(5) 0.4743(4) 0.075 Uiso 1 calc R . H46A H 0.3129(5) 0.3873(5) 0.4880(4) 0.075 Uiso 1 calc R . C47 C 0.1590(6) 0.3825(5) 0.4389(4) 0.060(3) Uani 1 d . . H47C H 0.1778(6) 0.3998(5) 0.4005(4) 0.090 Uiso 1 calc R . H47B H 0.1654(6) 0.4275(5) 0.4661(4) 0.090 Uiso 1 calc R . H47A H 0.0965(6) 0.3655(5) 0.4371(4) 0.090 Uiso 1 calc R . C48 C 0.2370(6) 0.0688(5) 0.5014(4) 0.054(3) Uani 1 d . . H48C H 0.3017(6) 0.0762(5) 0.5016(4) 0.080 Uiso 1 calc R . H48B H 0.2203(6) 0.0284(5) 0.4723(4) 0.080 Uiso 1 calc R . H48A H 0.2181(6) 0.0505(5) 0.5395(4) 0.080 Uiso 1 calc R . C49 C 0.0977(6) 0.1317(6) 0.4876(4) 0.057(3) Uani 1 d . . H49C H 0.0670(6) 0.1823(6) 0.4784(4) 0.085 Uiso 1 calc R . H49B H 0.0797(6) 0.1130(6) 0.5259(4) 0.085 Uiso 1 calc R . H49A H 0.0819(6) 0.0909(6) 0.4587(4) 0.085 Uiso 1 calc R . C50 C 0.2802(5) 0.1341(5) 0.3113(4) 0.044(2) Uani 1 d . . H50B H 0.2601(5) 0.0796(5) 0.3226(4) 0.053 Uiso 1 calc R . H50A H 0.3208(5) 0.1282(5) 0.2783(4) 0.053 Uiso 1 calc R . C51 C 0.2004(6) 0.1836(6) 0.2927(3) 0.050(3) Uani 1 d . . H51B H 0.2202(6) 0.2389(6) 0.2831(3) 0.060 Uiso 1 calc R . H51A H 0.1736(6) 0.1596(6) 0.2575(3) 0.060 Uiso 1 calc R . C52 C 0.3895(6) 0.1104(6) 0.3857(4) 0.058(3) Uani 1 d . . H52C H 0.3545(6) 0.0649(6) 0.3999(4) 0.087 Uiso 1 calc R . H52B H 0.4234(6) 0.1345(6) 0.4178(4) 0.087 Uiso 1 calc R . H52A H 0.4307(6) 0.0914(6) 0.3562(4) 0.087 Uiso 1 calc R . C53 C 0.3854(5) 0.2379(6) 0.3397(4) 0.052(3) Uani 1 d . . H53C H 0.3474(5) 0.2798(6) 0.3225(4) 0.079 Uiso 1 calc R . H53B H 0.4267(5) 0.2177(6) 0.3107(4) 0.079 Uiso 1 calc R . H53A H 0.4193(5) 0.2608(6) 0.3722(4) 0.079 Uiso 1 calc R . C54 C 0.0698(6) 0.2545(5) 0.3249(4) 0.047(2) Uani 1 d . . H54C H 0.1024(6) 0.3056(5) 0.3240(4) 0.070 Uiso 1 calc R . H54B H 0.0244(6) 0.2568(5) 0.3548(4) 0.070 Uiso 1 calc R . H54A H 0.0412(6) 0.2451(5) 0.2873(4) 0.070 Uiso 1 calc R . C55 C 0.0809(6) 0.1146(5) 0.3386(4) 0.045(2) Uani 1 d . . H55C H 0.0360(6) 0.1181(5) 0.3688(4) 0.067 Uiso 1 calc R . H55B H 0.1203(6) 0.0686(5) 0.3464(4) 0.067 Uiso 1 calc R . H55A H 0.0513(6) 0.1073(5) 0.3010(4) 0.067 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 P1 0.0207(12) 0.0273(13) 0.0278(12) 0.0008(10) 0.0003(10) -0.0020(11) P2 0.0302(13) 0.0283(13) 0.0273(12) -0.0011(10) -0.0001(10) -0.0062(11) P3 0.0291(13) 0.0334(13) 0.0322(13) 0.0013(11) -0.0050(11) -0.0038(11) Si1 0.0271(13) 0.0248(13) 0.0289(13) -0.0006(11) 0.0022(10) -0.0026(11) Si2 0.0294(14) 0.0247(13) 0.0247(13) -0.0004(11) 0.0013(10) -0.0053(11) Si3 0.0238(13) 0.0292(13) 0.0265(12) 0.0038(11) 0.0011(10) -0.0030(11) C1 0.019(4) 0.029(5) 0.026(4) 0.002(4) 0.003(4) 0.006(4) C2 0.041(6) 0.044(6) 0.032(5) -0.001(4) 0.005(4) -0.007(5) C3 0.057(6) 0.030(5) 0.046(6) 0.001(4) 0.016(5) 0.001(5) C4 0.023(5) 0.035(5) 0.025(5) -0.001(4) 0.000(4) -0.002(4) C5 0.035(5) 0.052(6) 0.037(5) 0.002(5) 0.001(4) 0.006(5) C6 0.040(6) 0.055(7) 0.035(6) -0.002(5) 0.012(5) 0.026(5) C7 0.049(7) 0.043(6) 0.047(6) 0.001(5) -0.008(5) 0.028(5) C8 0.042(6) 0.037(6) 0.034(5) 0.004(4) -0.002(5) 0.010(5) C9 0.032(5) 0.030(5) 0.026(5) -0.001(4) -0.001(4) 0.001(4) C10 0.025(5) 0.031(5) 0.024(5) -0.002(4) 0.009(4) -0.011(4) C11 0.033(5) 0.032(5) 0.031(5) 0.006(4) -0.004(4) -0.017(4) C12 0.044(6) 0.061(7) 0.037(6) -0.010(5) -0.001(5) -0.015(6) C13 0.054(7) 0.033(6) 0.049(6) -0.004(5) 0.009(5) -0.026(5) C14 0.058(7) 0.028(6) 0.057(7) 0.003(5) 0.004(6) 0.006(5) C15 0.033(5) 0.022(5) 0.040(5) 0.005(4) 0.001(4) -0.003(4) C16 0.039(5) 0.024(5) 0.036(5) 0.000(4) 0.004(4) 0.004(4) C17 0.039(5) 0.034(5) 0.023(5) -0.003(4) 0.001(4) -0.010(4) C18 0.024(5) 0.025(5) 0.036(5) -0.004(4) 0.006(4) -0.007(4) C19 0.038(6) 0.039(6) 0.045(6) -0.009(5) 0.012(5) -0.003(5) C20 0.050(7) 0.037(6) 0.056(7) 0.001(5) 0.006(5) 0.011(5) C21 0.042(6) 0.025(5) 0.063(7) -0.012(5) 0.004(5) 0.005(5) C22 0.039(6) 0.040(6) 0.048(6) -0.014(5) 0.012(5) -0.014(5) C23 0.039(6) 0.040(6) 0.030(5) -0.010(4) -0.003(4) -0.011(5) C24 0.040(6) 0.028(5) 0.023(5) -0.001(4) -0.001(4) -0.004(5) C25 0.041(6) 0.036(6) 0.033(5) 0.007(4) 0.006(4) 0.000(5) C26 0.057(7) 0.042(6) 0.035(6) 0.002(5) 0.018(5) -0.006(5) C27 0.067(8) 0.041(6) 0.033(6) 0.010(5) 0.000(5) 0.011(6) C28 0.041(6) 0.047(6) 0.056(7) 0.004(5) 0.005(5) 0.015(5) C29 0.025(5) 0.045(6) 0.036(5) 0.003(5) 0.011(4) 0.000(4) C30 0.036(5) 0.051(6) 0.042(6) -0.004(5) 0.002(4) -0.003(5) C31 0.037(5) 0.042(5) 0.036(5) 0.004(5) -0.004(4) -0.002(5) C32 0.030(5) 0.032(5) 0.035(5) 0.006(4) 0.004(4) -0.002(4) C33 0.023(5) 0.039(6) 0.043(6) -0.009(5) -0.006(4) -0.001(4) C34 0.028(5) 0.043(6) 0.057(7) -0.015(5) 0.003(5) -0.003(5) C35 0.032(6) 0.045(6) 0.046(6) 0.001(5) 0.008(5) -0.002(5) C36 0.053(6) 0.039(6) 0.026(5) -0.004(4) 0.006(5) -0.011(5) C37 0.031(5) 0.041(6) 0.039(6) 0.005(5) -0.002(5) -0.007(5) C38 0.028(5) 0.039(5) 0.031(5) -0.006(4) 0.000(4) 0.002(5) C39 0.043(6) 0.055(7) 0.062(7) 0.013(6) -0.019(5) 0.001(5) C40 0.054(7) 0.076(8) 0.050(7) 0.001(6) -0.020(6) 0.015(6) C41 0.025(6) 0.106(10) 0.046(7) -0.016(7) -0.004(5) 0.007(7) C42 0.029(6) 0.079(8) 0.053(7) -0.028(6) 0.000(5) -0.018(6) C43 0.037(6) 0.045(6) 0.039(6) -0.017(5) 0.009(5) 0.005(5) Li 0.009(7) 0.035(8) 0.034(8) -0.001(7) -0.011(6) -0.002(6) N1 0.033(4) 0.033(4) 0.032(4) -0.001(4) 0.001(3) 0.001(4) N2 0.035(5) 0.040(5) 0.036(4) 0.006(4) -0.002(4) -0.001(4) N3 0.031(4) 0.046(5) 0.035(4) 0.000(4) 0.002(4) 0.005(4) N4 0.027(4) 0.033(4) 0.033(4) 0.004(3) -0.003(3) 0.004(4) C44 0.051(6) 0.049(7) 0.053(6) -0.014(5) 0.006(5) 0.002(5) C45 0.088(8) 0.043(6) 0.030(5) 0.002(5) -0.004(5) -0.002(6) C46 0.037(6) 0.046(6) 0.066(7) -0.005(5) 0.003(5) -0.017(5) C47 0.072(8) 0.045(6) 0.061(7) 0.001(5) -0.019(6) 0.010(6) C48 0.071(7) 0.038(6) 0.051(7) 0.012(5) -0.011(6) 0.010(6) C49 0.052(7) 0.069(7) 0.049(6) 0.015(6) 0.012(5) -0.013(6) C50 0.039(6) 0.056(6) 0.037(5) -0.004(5) 0.009(5) 0.011(5) C51 0.052(6) 0.070(7) 0.028(5) 0.003(5) -0.003(5) -0.009(6) C52 0.044(6) 0.064(7) 0.067(7) 0.001(6) -0.005(5) 0.010(6) C53 0.036(6) 0.064(7) 0.058(7) 0.004(6) 0.005(5) -0.001(5) C54 0.049(6) 0.039(6) 0.052(6) 0.008(5) -0.008(5) 0.008(5) C55 0.052(6) 0.034(5) 0.049(6) -0.001(5) 0.002(5) -0.007(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 P1 C4 1.826(8) . ? P1 C10 1.844(8) . ? P1 Si1 2.316(3) . ? P2 C18 1.832(8) . ? P2 C24 1.835(8) . ? P2 Si2 2.318(3) . ? P3 C32 1.839(8) . ? P3 C38 1.847(8) . ? P3 Si3 2.334(3) . ? Si1 C1 1.802(7) . ? Si1 C2 1.876(7) . ? Si1 C3 1.886(8) . ? Si2 C1 1.815(7) . ? Si2 C17 1.872(7) . ? Si2 C16 1.878(7) . ? Si3 C1 1.811(7) . ? Si3 C30 1.877(8) . ? Si3 C31 1.888(8) . ? C4 C9 1.396(10) . ? C4 C5 1.404(10) . ? C5 C6 1.387(11) . ? C6 C7 1.359(11) . ? C7 C8 1.364(11) . ? C8 C9 1.396(10) . ? C10 C11 1.390(10) . ? C10 C15 1.392(10) . ? C11 C12 1.382(10) . ? C12 C13 1.379(11) . ? C13 C14 1.382(11) . ? C14 C15 1.383(11) . ? C18 C23 1.387(10) . ? C18 C19 1.394(10) . ? C19 C20 1.384(11) . ? C20 C21 1.367(11) . ? C21 C22 1.377(11) . ? C22 C23 1.382(11) . ? C24 C25 1.393(10) . ? C24 C29 1.398(10) . ? C25 C26 1.390(10) . ? C26 C27 1.381(11) . ? C27 C28 1.352(12) . ? C28 C29 1.384(11) . ? C32 C33 1.390(10) . ? C32 C37 1.414(10) . ? C33 C34 1.387(11) . ? C34 C35 1.368(11) . ? C35 C36 1.378(11) . ? C36 C37 1.385(11) . ? C38 C39 1.371(11) . ? C38 C43 1.377(11) . ? C39 C40 1.381(11) . ? C40 C41 1.358(13) . ? C41 C42 1.356(13) . ? C42 C43 1.388(11) . ? Li N2 2.073(14) . ? Li N4 2.115(13) . ? Li N1 2.123(14) . ? Li N3 2.149(14) . ? N1 C44 1.451(10) . ? N1 C46 1.466(9) . ? N1 C47 1.474(10) . ? N2 C48 1.455(9) . ? N2 C49 1.459(10) . ? N2 C45 1.472(10) . ? N3 C52 1.468(10) . ? N3 C53 1.476(10) . ? N3 C50 1.481(9) . ? N4 C55 1.444(9) . ? N4 C51 1.471(9) . ? N4 C54 1.481(9) . ? C44 C45 1.491(11) . ? C50 C51 1.512(11) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C4 P1 C10 102.4(3) . . ? C4 P1 Si1 106.0(3) . . ? C10 P1 Si1 101.4(3) . . ? C18 P2 C24 105.2(4) . . ? C18 P2 Si2 106.3(3) . . ? C24 P2 Si2 102.2(3) . . ? C32 P3 C38 102.2(4) . . ? C32 P3 Si3 104.2(3) . . ? C38 P3 Si3 106.8(3) . . ? C1 Si1 C2 116.6(3) . . ? C1 Si1 C3 114.9(4) . . ? C2 Si1 C3 104.0(4) . . ? C1 Si1 P1 112.7(2) . . ? C2 Si1 P1 105.3(3) . . ? C3 Si1 P1 101.8(3) . . ? C1 Si2 C17 117.2(3) . . ? C1 Si2 C16 114.6(3) . . ? C17 Si2 C16 105.9(4) . . ? C1 Si2 P2 114.1(3) . . ? C17 Si2 P2 103.3(2) . . ? C16 Si2 P2 99.8(3) . . ? C1 Si3 C30 116.6(3) . . ? C1 Si3 C31 114.7(3) . . ? C30 Si3 C31 103.4(4) . . ? C1 Si3 P3 110.8(3) . . ? C30 Si3 P3 102.3(3) . . ? C31 Si3 P3 107.8(3) . . ? Si1 C1 Si3 120.7(4) . . ? Si1 C1 Si2 120.2(4) . . ? Si3 C1 Si2 118.6(4) . . ? C9 C4 C5 117.3(7) . . ? C9 C4 P1 122.5(6) . . ? C5 C4 P1 119.7(6) . . ? C6 C5 C4 120.9(8) . . ? C7 C6 C5 120.5(8) . . ? C6 C7 C8 120.2(8) . . ? C7 C8 C9 120.5(8) . . ? C4 C9 C8 120.6(8) . . ? C11 C10 C15 118.7(7) . . ? C11 C10 P1 124.5(6) . . ? C15 C10 P1 116.7(6) . . ? C12 C11 C10 120.1(8) . . ? C13 C12 C11 120.7(8) . . ? C12 C13 C14 119.7(8) . . ? C13 C14 C15 119.7(8) . . ? C14 C15 C10 120.9(8) . . ? C23 C18 C19 117.0(8) . . ? C23 C18 P2 123.2(7) . . ? C19 C18 P2 119.1(6) . . ? C20 C19 C18 121.0(8) . . ? C21 C20 C19 121.0(9) . . ? C20 C21 C22 119.0(9) . . ? C21 C22 C23 120.3(8) . . ? C22 C23 C18 121.7(8) . . ? C25 C24 C29 117.2(7) . . ? C25 C24 P2 126.7(6) . . ? C29 C24 P2 116.0(6) . . ? C26 C25 C24 121.0(8) . . ? C27 C26 C25 119.6(9) . . ? C28 C27 C26 120.7(8) . . ? C27 C28 C29 120.0(8) . . ? C28 C29 C24 121.4(8) . . ? C33 C32 C37 117.2(8) . . ? C33 C32 P3 118.7(6) . . ? C37 C32 P3 123.8(6) . . ? C34 C33 C32 121.8(8) . . ? C35 C34 C33 120.1(8) . . ? C34 C35 C36 119.8(8) . . ? C35 C36 C37 120.9(8) . . ? C36 C37 C32 120.2(8) . . ? C39 C38 C43 117.2(8) . . ? C39 C38 P3 124.6(7) . . ? C43 C38 P3 118.1(7) . . ? C38 C39 C40 121.8(9) . . ? C41 C40 C39 118.8(10) . . ? C42 C41 C40 122.1(9) . . ? C41 C42 C43 117.8(10) . . ? C38 C43 C42 122.3(9) . . ? N2 Li N4 121.0(6) . . ? N2 Li N1 87.9(5) . . ? N4 Li N1 121.4(6) . . ? N2 Li N3 118.7(6) . . ? N4 Li N3 89.7(5) . . ? N1 Li N3 121.6(6) . . ? C44 N1 C46 109.8(7) . . ? C44 N1 C47 109.7(7) . . ? C46 N1 C47 108.2(7) . . ? C44 N1 Li 103.1(6) . . ? C46 N1 Li 105.5(6) . . ? C47 N1 Li 120.2(6) . . ? C48 N2 C49 107.9(7) . . ? C48 N2 C45 109.8(6) . . ? C49 N2 C45 110.7(7) . . ? C48 N2 Li 122.0(6) . . ? C49 N2 Li 104.5(6) . . ? C45 N2 Li 101.6(6) . . ? C52 N3 C53 107.2(6) . . ? C52 N3 C50 108.7(7) . . ? C53 N3 C50 110.1(6) . . ? C52 N3 Li 116.7(6) . . ? C53 N3 Li 115.8(6) . . ? C50 N3 Li 97.9(5) . . ? C55 N4 C51 110.2(7) . . ? C55 N4 C54 106.8(6) . . ? C51 N4 C54 109.6(6) . . ? C55 N4 Li 115.0(6) . . ? C51 N4 Li 99.5(6) . . ? C54 N4 Li 115.6(6) . . ? N1 C44 C45 112.9(7) . . ? N2 C45 C44 113.2(7) . . ? N3 C50 C51 112.3(7) . . ? N4 C51 C50 112.1(7) . . ? _refine_diff_density_max 0.333 _refine_diff_density_min -0.301 _refine_diff_density_rms 0.073 #=END data_jds-b _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[HC(SiMe2PPh2)3]' _chemical_formula_analytical ? _chemical_formula_sum 'C43 H49 P3 Si3' _chemical_formula_weight 743.00 _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' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, -z-1/2' _cell_length_a 18.314(4) _cell_length_b 10.398(3) _cell_length_c 21.859(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.61(2) _cell_angle_gamma 90.00 _cell_volume 4091.4(20) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description block _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.206 _exptl_crystal_density_method ? _exptl_crystal_F_000 1576 _exptl_absorpt_coefficient_mu 0.263 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.93 _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 ' 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 5170 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0956 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 21.97 _reflns_number_total 4993 _reflns_number_observed 3229 _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 ? _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material 'SHELXL-93 (Sheldrick, 1993)' _refine_special_details ; The hydrogen atom on C(1) was refined; all other H atoms were in riding mode. 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^)+(0.0473P)^2^+8.2290P] 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 4992 _refine_ls_number_parameters 446 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1045 _refine_ls_R_factor_obs 0.0527 _refine_ls_wR_factor_all 0.1365 _refine_ls_wR_factor_obs 0.1069 _refine_ls_goodness_of_fit_all 0.945 _refine_ls_goodness_of_fit_obs 0.943 _refine_ls_restrained_S_all 0.946 _refine_ls_restrained_S_obs 0.943 _refine_ls_shift/esd_max 0.008 _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 P1 P 0.08656(8) -0.00516(14) 0.07466(6) 0.0255(4) Uani 1 d . . P2 P 0.34418(8) 0.07653(15) -0.03745(6) 0.0279(4) Uani 1 d . . P3 P 0.38194(8) -0.1082(2) 0.20301(7) 0.0312(4) Uani 1 d . . Si1 Si 0.18835(8) 0.08265(15) 0.13515(6) 0.0237(4) Uani 1 d . . Si2 Si 0.26188(8) 0.15952(15) 0.01852(7) 0.0256(4) Uani 1 d . . Si3 Si 0.36254(8) 0.0783(2) 0.14788(7) 0.0276(4) Uani 1 d . . C1 C 0.2697(3) 0.0631(6) 0.0931(2) 0.0248(13) Uani 1 d . . H1 H 0.2655(26) -0.0129(50) 0.0802(21) 0.018(15) Uiso 1 d . . C2 C 0.1622(3) 0.2560(5) 0.1406(3) 0.0358(15) Uani 1 d . . H2C H 0.1550(3) 0.2951(5) 0.0991(3) 0.054 Uiso 1 calc R . H2B H 0.2020(3) 0.3014(5) 0.1684(3) 0.054 Uiso 1 calc R . H2A H 0.1160(3) 0.2621(5) 0.1570(3) 0.054 Uiso 1 calc R . C3 C 0.2012(3) 0.0145(6) 0.2157(2) 0.0346(15) Uani 1 d . . H3C H 0.2150(3) -0.0764(6) 0.2147(2) 0.052 Uiso 1 calc R . H3B H 0.1547(3) 0.0225(6) 0.2315(2) 0.052 Uiso 1 calc R . H3A H 0.2406(3) 0.0619(6) 0.2430(2) 0.052 Uiso 1 calc R . C4 C 0.0230(3) -0.0156(5) 0.1302(2) 0.0273(14) Uani 1 d . . C5 C 0.0105(3) -0.1274(6) 0.1617(2) 0.0304(14) Uani 1 d . . H5 H 0.0383(3) -0.2025(6) 0.1564(2) 0.036 Uiso 1 calc R . C6 C -0.0408(3) -0.1323(6) 0.2004(2) 0.0342(15) Uani 1 d . . H6 H -0.0487(3) -0.2104(6) 0.2208(2) 0.041 Uiso 1 calc R . C7 C -0.0808(3) -0.0245(6) 0.2095(3) 0.037(2) Uani 1 d . . H7 H -0.1161(3) -0.0275(6) 0.2363(3) 0.045 Uiso 1 calc R . C8 C -0.0692(3) 0.0883(6) 0.1795(3) 0.039(2) Uani 1 d . . H8 H -0.0961(3) 0.1635(6) 0.1861(3) 0.047 Uiso 1 calc R . C9 C -0.0187(3) 0.0925(6) 0.1400(3) 0.0350(15) Uani 1 d . . H9 H -0.0121(3) 0.1704(6) 0.1190(3) 0.042 Uiso 1 calc R . C10 C 0.1085(3) -0.1748(5) 0.0642(2) 0.0247(13) Uani 1 d . . C11 C 0.1694(3) -0.2418(6) 0.0950(3) 0.038(2) Uani 1 d . . H11 H 0.2044(3) -0.1993(6) 0.1259(3) 0.045 Uiso 1 calc R . C12 C 0.1806(4) -0.3702(6) 0.0816(3) 0.049(2) Uani 1 d . . H12 H 0.2227(4) -0.4152(6) 0.1032(3) 0.059 Uiso 1 calc R . C13 C 0.1301(4) -0.4312(6) 0.0366(3) 0.050(2) Uani 1 d . . H13 H 0.1377(4) -0.5185(6) 0.0268(3) 0.060 Uiso 1 calc R . C14 C 0.0692(4) -0.3675(6) 0.0062(3) 0.048(2) Uani 1 d . . H14 H 0.0338(4) -0.4108(6) -0.0241(3) 0.058 Uiso 1 calc R . C15 C 0.0590(3) -0.2394(6) 0.0195(2) 0.0323(14) Uani 1 d . . H15 H 0.0171(3) -0.1950(6) -0.0027(2) 0.039 Uiso 1 calc R . C16 C 0.1670(3) 0.1731(6) -0.0295(2) 0.0350(15) Uani 1 d . . H16C H 0.1468(3) 0.0869(6) -0.0396(2) 0.053 Uiso 1 calc R . H16B H 0.1697(3) 0.2195(6) -0.0680(2) 0.053 Uiso 1 calc R . H16A H 0.1348(3) 0.2201(6) -0.0061(2) 0.053 Uiso 1 calc R . C17 C 0.2958(3) 0.3284(5) 0.0354(3) 0.041(2) Uani 1 d . . H17C H 0.3459(3) 0.3265(5) 0.0608(3) 0.062 Uiso 1 calc R . H17B H 0.2622(3) 0.3737(5) 0.0581(3) 0.062 Uiso 1 calc R . H17A H 0.2971(3) 0.3732(5) -0.0038(3) 0.062 Uiso 1 calc R . C18 C 0.3093(3) -0.0822(6) -0.0672(2) 0.0272(13) Uani 1 d . . C19 C 0.2477(3) -0.1449(6) -0.0550(3) 0.038(2) Uani 1 d . . H19 H 0.2164(3) -0.1033(6) -0.0309(3) 0.045 Uiso 1 calc R . C20 C 0.2305(3) -0.2685(6) -0.0773(3) 0.047(2) Uani 1 d . . H20 H 0.1878(3) -0.3112(6) -0.0683(3) 0.056 Uiso 1 calc R . C21 C 0.2754(3) -0.3287(7) -0.1125(3) 0.046(2) Uani 1 d . . H21 H 0.2638(3) -0.4132(7) -0.1277(3) 0.055 Uiso 1 calc R . C22 C 0.3368(3) -0.2667(6) -0.1254(3) 0.042(2) Uani 1 d . . H22 H 0.3676(3) -0.3081(6) -0.1499(3) 0.050 Uiso 1 calc R . C23 C 0.3537(3) -0.1454(6) -0.1031(2) 0.0342(15) Uani 1 d . . H23 H 0.3965(3) -0.1034(6) -0.1123(2) 0.041 Uiso 1 calc R . C24 C 0.3206(3) 0.1776(5) -0.1072(2) 0.0266(13) Uani 1 d . . C25 C 0.3660(3) 0.2803(6) -0.1134(3) 0.036(2) Uani 1 d . . H25 H 0.4085(3) 0.2964(6) -0.0822(3) 0.043 Uiso 1 calc R . C26 C 0.3503(3) 0.3604(6) -0.1647(3) 0.046(2) Uani 1 d . . H26 H 0.3820(3) 0.4315(6) -0.1679(3) 0.055 Uiso 1 calc R . C27 C 0.2899(3) 0.3390(6) -0.2109(3) 0.043(2) Uani 1 d . . H27 H 0.2793(3) 0.3946(6) -0.2459(3) 0.052 Uiso 1 calc R . C28 C 0.2451(3) 0.2354(7) -0.2054(3) 0.045(2) Uani 1 d . . H28 H 0.2033(3) 0.2186(7) -0.2371(3) 0.054 Uiso 1 calc R . C29 C 0.2604(3) 0.1552(6) -0.1542(2) 0.037(2) Uani 1 d . . H29 H 0.2291(3) 0.0836(6) -0.1513(2) 0.045 Uiso 1 calc R . C30 C 0.3592(3) 0.2092(6) 0.2062(2) 0.039(2) Uani 1 d . . H30C H 0.3162(3) 0.1958(6) 0.2264(2) 0.059 Uiso 1 calc R . H30B H 0.3546(3) 0.2927(6) 0.1850(2) 0.059 Uiso 1 calc R . H30A H 0.4048(3) 0.2076(6) 0.2376(2) 0.059 Uiso 1 calc R . C31 C 0.4461(3) 0.1162(6) 0.1137(3) 0.040(2) Uani 1 d . . H31C H 0.4517(3) 0.0512(6) 0.0824(3) 0.060 Uiso 1 calc R . H31B H 0.4904(3) 0.1160(6) 0.1466(3) 0.060 Uiso 1 calc R . H31A H 0.4402(3) 0.2012(6) 0.0940(3) 0.060 Uiso 1 calc R . C32 C 0.4088(3) -0.2298(6) 0.1504(2) 0.0302(14) Uani 1 d . . C33 C 0.4000(3) -0.2168(6) 0.0862(3) 0.043(2) Uani 1 d . . H33 H 0.3825(3) -0.1377(6) 0.0672(3) 0.051 Uiso 1 calc R . C34 C 0.4164(3) -0.3183(7) 0.0493(3) 0.048(2) Uani 1 d . . H34 H 0.4096(3) -0.3081(7) 0.0054(3) 0.058 Uiso 1 calc R . C35 C 0.4422(3) -0.4322(6) 0.0759(3) 0.046(2) Uani 1 d . . H35 H 0.4540(3) -0.5008(6) 0.0507(3) 0.055 Uiso 1 calc R . C36 C 0.4512(3) -0.4473(6) 0.1398(3) 0.045(2) Uani 1 d . . H36 H 0.4689(3) -0.5266(6) 0.1585(3) 0.055 Uiso 1 calc R . C37 C 0.4344(3) -0.3469(6) 0.1764(3) 0.038(2) Uani 1 d . . H37 H 0.4405(3) -0.3584(6) 0.2202(3) 0.045 Uiso 1 calc R . C38 C 0.4711(3) -0.0646(5) 0.2522(2) 0.0301(14) Uani 1 d . . C39 C 0.5396(3) -0.0820(6) 0.2360(2) 0.0338(14) Uani 1 d . . H39 H 0.5429(3) -0.1220(6) 0.1975(2) 0.041 Uiso 1 calc R . C40 C 0.6038(3) -0.0419(6) 0.2750(3) 0.043(2) Uani 1 d . . H40 H 0.6506(3) -0.0552(6) 0.2632(3) 0.052 Uiso 1 calc R . C41 C 0.6004(4) 0.0172(6) 0.3310(3) 0.044(2) Uani 1 d . . H41 H 0.6446(4) 0.0452(6) 0.3575(3) 0.053 Uiso 1 calc R . C42 C 0.5324(4) 0.0352(6) 0.3480(3) 0.042(2) Uani 1 d . . H42 H 0.5294(4) 0.0761(6) 0.3863(3) 0.051 Uiso 1 calc R . C43 C 0.4686(3) -0.0063(5) 0.3094(3) 0.0361(15) Uani 1 d . . H43 H 0.4220(3) 0.0050(5) 0.3219(3) 0.043 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 P1 0.0249(8) 0.0210(9) 0.0302(8) 0.0017(7) 0.0041(6) 0.0027(7) P2 0.0269(8) 0.0300(9) 0.0273(8) 0.0014(7) 0.0064(6) -0.0036(7) P3 0.0287(8) 0.0349(10) 0.0291(8) 0.0037(7) 0.0033(7) 0.0009(7) Si1 0.0255(8) 0.0212(9) 0.0246(8) -0.0001(7) 0.0051(6) 0.0007(7) Si2 0.0280(8) 0.0235(9) 0.0260(8) 0.0035(7) 0.0066(7) 0.0003(7) Si3 0.0241(8) 0.0290(10) 0.0285(8) 0.0028(8) 0.0019(7) -0.0014(8) C1 0.032(3) 0.018(4) 0.024(3) -0.003(3) 0.004(2) -0.001(3) C2 0.043(4) 0.021(3) 0.044(4) -0.008(3) 0.009(3) 0.005(3) C3 0.030(3) 0.042(4) 0.032(3) -0.003(3) 0.005(3) 0.001(3) C4 0.018(3) 0.030(4) 0.032(3) -0.004(3) -0.002(2) -0.003(3) C5 0.029(3) 0.024(4) 0.039(3) -0.003(3) 0.010(3) 0.003(3) C6 0.028(3) 0.038(4) 0.035(3) -0.002(3) 0.002(3) -0.003(3) C7 0.030(3) 0.050(5) 0.034(4) -0.007(3) 0.010(3) -0.003(3) C8 0.029(3) 0.043(4) 0.046(4) -0.019(3) 0.005(3) 0.007(3) C9 0.035(3) 0.025(4) 0.045(4) -0.007(3) 0.007(3) 0.007(3) C10 0.026(3) 0.019(3) 0.032(3) 0.002(3) 0.011(3) 0.003(3) C11 0.039(4) 0.027(4) 0.047(4) 0.005(3) 0.010(3) 0.003(3) C12 0.059(4) 0.025(4) 0.062(4) 0.007(3) 0.010(4) 0.018(3) C13 0.077(5) 0.020(4) 0.059(4) -0.004(4) 0.028(4) -0.002(4) C14 0.068(5) 0.031(4) 0.047(4) -0.006(3) 0.014(4) -0.010(4) C15 0.031(3) 0.030(4) 0.036(3) -0.001(3) 0.007(3) -0.001(3) C16 0.035(3) 0.043(4) 0.029(3) 0.008(3) 0.013(3) 0.005(3) C17 0.054(4) 0.021(4) 0.051(4) 0.007(3) 0.014(3) 0.001(3) C18 0.026(3) 0.032(4) 0.023(3) 0.003(3) 0.002(2) 0.000(3) C19 0.037(4) 0.039(4) 0.040(4) -0.007(3) 0.011(3) -0.002(3) C20 0.044(4) 0.044(5) 0.056(4) -0.009(4) 0.016(3) -0.024(3) C21 0.048(4) 0.044(4) 0.044(4) -0.012(3) 0.002(3) -0.002(4) C22 0.035(4) 0.048(5) 0.041(4) -0.015(3) 0.007(3) 0.002(3) C23 0.036(3) 0.035(4) 0.034(3) -0.003(3) 0.013(3) -0.005(3) C24 0.027(3) 0.031(4) 0.025(3) -0.001(3) 0.012(3) 0.001(3) C25 0.038(4) 0.033(4) 0.036(4) 0.002(3) 0.009(3) -0.011(3) C26 0.052(4) 0.036(4) 0.054(4) 0.011(3) 0.018(4) -0.010(3) C27 0.042(4) 0.044(4) 0.046(4) 0.018(3) 0.016(3) 0.008(4) C28 0.039(4) 0.060(5) 0.033(4) 0.008(3) 0.001(3) -0.002(4) C29 0.043(4) 0.036(4) 0.032(3) 0.005(3) 0.006(3) -0.009(3) C30 0.043(4) 0.031(4) 0.039(4) -0.004(3) -0.005(3) -0.008(3) C31 0.025(3) 0.055(4) 0.036(3) 0.008(3) -0.002(3) -0.003(3) C32 0.024(3) 0.035(4) 0.028(3) -0.004(3) -0.003(2) 0.001(3) C33 0.045(4) 0.036(4) 0.041(4) 0.001(3) -0.008(3) 0.009(3) C34 0.049(4) 0.052(5) 0.041(4) -0.004(4) -0.001(3) 0.004(4) C35 0.041(4) 0.035(4) 0.061(5) -0.013(4) 0.005(3) -0.007(3) C36 0.054(4) 0.025(4) 0.055(5) 0.003(3) 0.004(3) -0.002(3) C37 0.044(4) 0.031(4) 0.036(3) 0.005(3) 0.003(3) -0.008(3) C38 0.036(3) 0.026(3) 0.027(3) 0.004(3) 0.001(3) 0.007(3) C39 0.034(3) 0.032(4) 0.033(3) -0.005(3) -0.002(3) 0.009(3) C40 0.032(4) 0.035(4) 0.058(4) -0.006(3) -0.002(3) 0.012(3) C41 0.043(4) 0.035(4) 0.047(4) -0.003(3) -0.015(3) 0.003(3) C42 0.058(4) 0.027(4) 0.036(4) 0.000(3) -0.009(3) 0.010(3) C43 0.045(4) 0.028(4) 0.036(4) 0.007(3) 0.011(3) 0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P1 C10 1.833(5) . ? P1 C4 1.834(5) . ? P1 Si1 2.269(2) . ? P2 C24 1.836(5) . ? P2 C18 1.845(6) . ? P2 Si2 2.279(2) . ? P3 C32 1.836(6) . ? P3 C38 1.838(5) . ? P3 Si3 2.277(2) . ? Si1 C3 1.872(5) . ? Si1 C2 1.874(5) . ? Si1 C1 1.900(6) . ? Si2 C16 1.862(5) . ? Si2 C17 1.877(6) . ? Si2 C1 1.897(6) . ? Si3 C31 1.866(5) . ? Si3 C30 1.873(6) . ? Si3 C1 1.898(5) . ? C4 C5 1.392(8) . ? C4 C9 1.396(7) . ? C5 C6 1.377(7) . ? C6 C7 1.374(8) . ? C7 C8 1.379(8) . ? C8 C9 1.377(8) . ? C10 C11 1.381(7) . ? C10 C15 1.379(7) . ? C11 C12 1.390(8) . ? C12 C13 1.374(9) . ? C13 C14 1.362(9) . ? C14 C15 1.383(8) . ? C18 C19 1.370(7) . ? C18 C23 1.396(7) . ? C19 C20 1.390(8) . ? C20 C21 1.375(8) . ? C21 C22 1.370(8) . ? C22 C23 1.367(8) . ? C24 C25 1.375(7) . ? C24 C29 1.382(7) . ? C25 C26 1.384(8) . ? C26 C27 1.373(8) . ? C27 C28 1.372(8) . ? C28 C29 1.382(8) . ? C32 C37 1.390(8) . ? C32 C33 1.388(7) . ? C33 C34 1.395(8) . ? C34 C35 1.365(8) . ? C35 C36 1.385(8) . ? C36 C37 1.384(8) . ? C38 C39 1.378(7) . ? C38 C43 1.398(7) . ? C39 C40 1.383(7) . ? C40 C41 1.381(8) . ? C41 C42 1.377(8) . ? C42 C43 1.378(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 C10 P1 C4 101.9(2) . . ? C10 P1 Si1 106.5(2) . . ? C4 P1 Si1 101.1(2) . . ? C24 P2 C18 101.9(2) . . ? C24 P2 Si2 98.7(2) . . ? C18 P2 Si2 107.9(2) . . ? C32 P3 C38 103.0(2) . . ? C32 P3 Si3 106.8(2) . . ? C38 P3 Si3 97.7(2) . . ? C3 Si1 C2 107.1(3) . . ? C3 Si1 C1 116.1(2) . . ? C2 Si1 C1 111.5(3) . . ? C3 Si1 P1 110.1(2) . . ? C2 Si1 P1 103.4(2) . . ? C1 Si1 P1 107.9(2) . . ? C16 Si2 C17 106.3(3) . . ? C16 Si2 C1 116.1(2) . . ? C17 Si2 C1 110.8(3) . . ? C16 Si2 P2 111.5(2) . . ? C17 Si2 P2 103.4(2) . . ? C1 Si2 P2 108.0(2) . . ? C31 Si3 C30 104.6(3) . . ? C31 Si3 C1 118.1(2) . . ? C30 Si3 C1 110.6(3) . . ? C31 Si3 P3 109.4(2) . . ? C30 Si3 P3 106.3(2) . . ? C1 Si3 P3 107.3(2) . . ? Si2 C1 Si3 114.5(3) . . ? Si2 C1 Si1 114.7(3) . . ? Si3 C1 Si1 112.1(3) . . ? C5 C4 C9 116.9(5) . . ? C5 C4 P1 124.0(4) . . ? C9 C4 P1 119.1(4) . . ? C6 C5 C4 121.9(5) . . ? C7 C6 C5 120.1(6) . . ? C8 C7 C6 119.5(5) . . ? C7 C8 C9 120.3(6) . . ? C8 C9 C4 121.3(6) . . ? C11 C10 C15 117.8(5) . . ? C11 C10 P1 126.9(4) . . ? C15 C10 P1 115.3(4) . . ? C10 C11 C12 121.2(6) . . ? C13 C12 C11 119.2(6) . . ? C14 C13 C12 120.6(6) . . ? C13 C14 C15 119.7(6) . . ? C10 C15 C14 121.5(6) . . ? C19 C18 C23 118.2(5) . . ? C19 C18 P2 126.9(4) . . ? C23 C18 P2 114.8(4) . . ? C18 C19 C20 120.8(6) . . ? C21 C20 C19 119.8(6) . . ? C22 C21 C20 119.9(6) . . ? C23 C22 C21 120.1(6) . . ? C22 C23 C18 121.1(6) . . ? C25 C24 C29 118.1(5) . . ? C25 C24 P2 118.2(4) . . ? C29 C24 P2 123.7(4) . . ? C24 C25 C26 120.6(5) . . ? C27 C26 C25 121.2(6) . . ? C26 C27 C28 118.5(6) . . ? C27 C28 C29 120.6(6) . . ? C24 C29 C28 121.1(6) . . ? C37 C32 C33 117.9(5) . . ? C37 C32 P3 117.1(4) . . ? C33 C32 P3 124.8(5) . . ? C32 C33 C34 120.9(6) . . ? C35 C34 C33 120.3(6) . . ? C34 C35 C36 119.7(6) . . ? C35 C36 C37 120.0(6) . . ? C36 C37 C32 121.2(5) . . ? C39 C38 C43 117.9(5) . . ? C39 C38 P3 124.8(4) . . ? C43 C38 P3 117.3(4) . . ? C38 C39 C40 120.9(5) . . ? C41 C40 C39 120.6(6) . . ? C42 C41 C40 119.4(6) . . ? C41 C42 C43 120.0(6) . . ? C42 C43 C38 121.3(6) . . ? _refine_diff_density_max 0.346 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.063