# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1976 data_jun298 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[(Me3Si)2(Me2SiPPh2)CH]' _chemical_formula_analytical ? _chemical_formula_sum 'C21 H35 P Si3' _chemical_formula_weight 402.73 _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)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y+1/2, z+1/2' '-x, -y, -z' '-x, y-1/2, -z-1/2' _cell_length_a 6.852(2) _cell_length_b 19.404(7) _cell_length_c 18.012(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.31(2) _cell_angle_gamma 90.00 _cell_volume 2388.0(14) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.120 _exptl_crystal_density_method ? _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.269 _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 4555 _diffrn_reflns_av_R_equivalents 0.0399 _diffrn_reflns_av_sigmaI/netI 0.0816 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4190 _reflns_number_observed 2940 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0358P)^2^+0.7568P] 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 4190 _refine_ls_number_parameters 226 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_obs 0.0491 _refine_ls_wR_factor_all 0.1149 _refine_ls_wR_factor_obs 0.0982 _refine_ls_goodness_of_fit_all 1.025 _refine_ls_goodness_of_fit_obs 1.057 _refine_ls_restrained_S_all 1.025 _refine_ls_restrained_S_obs 1.057 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group P P 0.44540(12) 0.56216(4) 0.31795(4) 0.0200(2) Uani 1 d . . Si1 Si 0.54637(12) 0.67475(4) 0.31326(5) 0.0188(2) Uani 1 d . . Si2 Si 0.43181(13) 0.68250(5) 0.48156(5) 0.0224(2) Uani 1 d . . Si3 Si 0.62097(14) 0.81124(5) 0.40622(5) 0.0241(2) Uani 1 d . . C1 C 0.5931(4) 0.71429(15) 0.4081(2) 0.0189(7) Uani 1 d . . H1 H 0.7266(4) 0.69735(15) 0.4256(2) 0.023 Uiso 1 calc R . C2 C 0.3373(5) 0.7186(2) 0.2606(2) 0.0273(8) Uani 1 d . . H2A H 0.2212(5) 0.7160(2) 0.2891(2) 0.041 Uiso 1 calc R . H2B H 0.3101(5) 0.6959(2) 0.2124(2) 0.041 Uiso 1 calc R . H2C H 0.3707(5) 0.7670(2) 0.2527(2) 0.041 Uiso 1 calc R . C3 C 0.7689(5) 0.6792(2) 0.2599(2) 0.0285(8) Uani 1 d . . H3A H 0.8780(5) 0.6560(2) 0.2880(2) 0.043 Uiso 1 calc R . H3B H 0.8032(5) 0.7275(2) 0.2519(2) 0.043 Uiso 1 calc R . H3C H 0.7426(5) 0.6564(2) 0.2116(2) 0.043 Uiso 1 calc R . C4 C 0.6732(4) 0.5124(2) 0.3275(2) 0.0201(7) Uani 1 d . . C5 C 0.8257(5) 0.5311(2) 0.3790(2) 0.0223(7) Uani 1 d . . H5 H 0.8181(5) 0.5733(2) 0.4052(2) 0.027 Uiso 1 calc R . C6 C 0.9878(5) 0.4894(2) 0.3925(2) 0.0288(8) Uani 1 d . . H6 H 1.0901(5) 0.5033(2) 0.4279(2) 0.035 Uiso 1 calc R . C7 C 1.0023(5) 0.4279(2) 0.3552(2) 0.0321(8) Uani 1 d . . H7 H 1.1141(5) 0.3994(2) 0.3645(2) 0.039 Uiso 1 calc R . C8 C 0.8525(5) 0.4083(2) 0.3042(2) 0.0331(9) Uani 1 d . . H8 H 0.8613(5) 0.3659(2) 0.2782(2) 0.040 Uiso 1 calc R . C9 C 0.6894(5) 0.4498(2) 0.2905(2) 0.0266(8) Uani 1 d . . H9 H 0.5870(5) 0.4354(2) 0.2554(2) 0.032 Uiso 1 calc R . C10 C 0.3616(4) 0.55089(15) 0.2197(2) 0.0187(7) Uani 1 d . . C11 C 0.4839(5) 0.5502(2) 0.1610(2) 0.0252(8) Uani 1 d . . H11 H 0.6216(5) 0.5525(2) 0.1716(2) 0.030 Uiso 1 calc R . C12 C 0.4086(5) 0.5463(2) 0.0881(2) 0.0276(8) Uani 1 d . . H12 H 0.4940(5) 0.5463(2) 0.0489(2) 0.033 Uiso 1 calc R . C13 C 0.2096(5) 0.5425(2) 0.0721(2) 0.0328(9) Uani 1 d . . H13 H 0.1576(5) 0.5401(2) 0.0218(2) 0.039 Uiso 1 calc R . C14 C 0.0852(5) 0.5423(2) 0.1287(2) 0.0334(9) Uani 1 d . . H14 H -0.0522(5) 0.5398(2) 0.1174(2) 0.040 Uiso 1 calc R . C15 C 0.1606(5) 0.5457(2) 0.2021(2) 0.0252(8) Uani 1 d . . H15 H 0.0743(5) 0.5444(2) 0.2410(2) 0.030 Uiso 1 calc R . C16 C 0.1684(5) 0.6814(2) 0.4462(2) 0.0318(8) Uani 1 d . . H16A H 0.1288(5) 0.7277(2) 0.4293(2) 0.048 Uiso 1 calc R . H16B H 0.0882(5) 0.6669(2) 0.4862(2) 0.048 Uiso 1 calc R . H16C H 0.1501(5) 0.6490(2) 0.4045(2) 0.048 Uiso 1 calc R . C17 C 0.4515(6) 0.7353(2) 0.5685(2) 0.0438(10) Uani 1 d . . H17A H 0.4157(6) 0.7831(2) 0.5564(2) 0.066 Uiso 1 calc R . H17B H 0.5863(6) 0.7337(2) 0.5908(2) 0.066 Uiso 1 calc R . H17C H 0.3628(6) 0.7168(2) 0.6037(2) 0.066 Uiso 1 calc R . C18 C 0.5030(6) 0.5945(2) 0.5131(2) 0.0335(9) Uani 1 d . . H18A H 0.4966(6) 0.5633(2) 0.4702(2) 0.050 Uiso 1 calc R . H18B H 0.4131(6) 0.5784(2) 0.5492(2) 0.050 Uiso 1 calc R . H18C H 0.6368(6) 0.5953(2) 0.5365(2) 0.050 Uiso 1 calc R . C19 C 0.7450(6) 0.8443(2) 0.3244(2) 0.0377(9) Uani 1 d . . H19A H 0.8736(6) 0.8224(2) 0.3231(2) 0.057 Uiso 1 calc R . H19B H 0.7615(6) 0.8944(2) 0.3288(2) 0.057 Uiso 1 calc R . H19C H 0.6650(6) 0.8335(2) 0.2785(2) 0.057 Uiso 1 calc R . C20 C 0.3775(5) 0.8550(2) 0.4051(2) 0.0302(8) Uani 1 d . . H20A H 0.3078(5) 0.8389(2) 0.4474(2) 0.045 Uiso 1 calc R . H20B H 0.3005(5) 0.8440(2) 0.3586(2) 0.045 Uiso 1 calc R . H20C H 0.3967(5) 0.9050(2) 0.4088(2) 0.045 Uiso 1 calc R . C21 C 0.7816(5) 0.8414(2) 0.4887(2) 0.0365(9) Uani 1 d . . H21A H 0.9090(5) 0.8184(2) 0.4891(2) 0.055 Uiso 1 calc R . H21B H 0.7199(5) 0.8302(2) 0.5345(2) 0.055 Uiso 1 calc R . H21C H 0.8000(5) 0.8914(2) 0.4855(2) 0.055 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 P 0.0197(4) 0.0213(4) 0.0188(4) -0.0022(4) 0.0013(3) -0.0025(4) Si1 0.0183(4) 0.0194(5) 0.0189(5) 0.0002(4) 0.0024(3) -0.0007(4) Si2 0.0273(5) 0.0211(5) 0.0189(5) -0.0011(4) 0.0032(4) -0.0023(4) Si3 0.0250(5) 0.0175(5) 0.0297(5) -0.0020(4) 0.0016(4) -0.0032(4) C1 0.017(2) 0.017(2) 0.022(2) -0.0005(13) -0.0018(13) 0.0011(13) C2 0.029(2) 0.027(2) 0.026(2) 0.0021(15) -0.0008(15) 0.000(2) C3 0.029(2) 0.030(2) 0.028(2) -0.002(2) 0.0085(15) -0.001(2) C4 0.020(2) 0.021(2) 0.019(2) 0.0024(13) 0.0003(13) -0.0034(13) C5 0.025(2) 0.021(2) 0.021(2) -0.0014(14) 0.0023(14) -0.0015(14) C6 0.024(2) 0.036(2) 0.025(2) 0.004(2) -0.0042(15) -0.002(2) C7 0.032(2) 0.027(2) 0.037(2) 0.002(2) 0.001(2) 0.008(2) C8 0.036(2) 0.024(2) 0.039(2) -0.006(2) 0.000(2) 0.006(2) C9 0.027(2) 0.027(2) 0.025(2) -0.0055(15) -0.0031(15) -0.0013(15) C10 0.021(2) 0.014(2) 0.021(2) -0.0015(13) 0.0000(13) 0.0023(13) C11 0.023(2) 0.025(2) 0.027(2) -0.0038(15) 0.0029(14) -0.0014(14) C12 0.038(2) 0.024(2) 0.021(2) -0.0023(15) 0.002(2) -0.001(2) C13 0.043(2) 0.034(2) 0.020(2) 0.000(2) -0.008(2) 0.001(2) C14 0.026(2) 0.042(2) 0.031(2) -0.002(2) -0.009(2) 0.003(2) C15 0.024(2) 0.027(2) 0.026(2) -0.0015(15) 0.0032(14) 0.0026(15) C16 0.025(2) 0.036(2) 0.035(2) -0.002(2) 0.010(2) -0.001(2) C17 0.069(3) 0.040(2) 0.024(2) -0.007(2) 0.015(2) -0.011(2) C18 0.048(2) 0.027(2) 0.026(2) 0.007(2) 0.002(2) 0.001(2) C19 0.040(2) 0.023(2) 0.051(2) 0.006(2) 0.010(2) -0.008(2) C20 0.031(2) 0.022(2) 0.038(2) 0.000(2) 0.003(2) 0.000(2) C21 0.029(2) 0.030(2) 0.049(2) -0.010(2) -0.006(2) -0.006(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 P C10 1.831(3) . ? P C4 1.832(3) . ? P Si1 2.2952(14) . ? Si1 C3 1.865(3) . ? Si1 C2 1.863(3) . ? Si1 C1 1.879(3) . ? Si2 C18 1.853(3) . ? Si2 C17 1.867(4) . ? Si2 C16 1.868(3) . ? Si2 C1 1.890(3) . ? Si3 C20 1.870(3) . ? Si3 C19 1.869(4) . ? Si3 C21 1.874(4) . ? Si3 C1 1.891(3) . ? C4 C9 1.394(4) . ? C4 C5 1.392(4) . ? C5 C6 1.380(4) . ? C6 C7 1.376(5) . ? C7 C8 1.379(5) . ? C8 C9 1.384(5) . ? C10 C15 1.394(4) . ? C10 C11 1.398(4) . ? C11 C12 1.377(4) . ? C12 C13 1.374(5) . ? C13 C14 1.377(5) . ? C14 C15 1.385(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C10 P C4 103.32(14) . . ? C10 P Si1 98.71(10) . . ? C4 P Si1 104.37(11) . . ? C3 Si1 C2 110.1(2) . . ? C3 Si1 C1 111.11(15) . . ? C2 Si1 C1 110.40(15) . . ? C3 Si1 P 108.86(12) . . ? C2 Si1 P 103.37(11) . . ? C1 Si1 P 112.74(10) . . ? C18 Si2 C17 104.4(2) . . ? C18 Si2 C16 108.6(2) . . ? C17 Si2 C16 107.4(2) . . ? C18 Si2 C1 111.2(2) . . ? C17 Si2 C1 113.5(2) . . ? C16 Si2 C1 111.46(15) . . ? C20 Si3 C19 107.1(2) . . ? C20 Si3 C21 109.7(2) . . ? C19 Si3 C21 104.0(2) . . ? C20 Si3 C1 111.14(15) . . ? C19 Si3 C1 114.1(2) . . ? C21 Si3 C1 110.5(2) . . ? Si1 C1 Si2 115.8(2) . . ? Si1 C1 Si3 113.6(2) . . ? Si2 C1 Si3 113.7(2) . . ? C9 C4 C5 117.6(3) . . ? C9 C4 P 120.8(2) . . ? C5 C4 P 121.1(2) . . ? C6 C5 C4 121.3(3) . . ? C7 C6 C5 120.5(3) . . ? C8 C7 C6 119.1(3) . . ? C7 C8 C9 120.6(3) . . ? C8 C9 C4 120.9(3) . . ? C15 C10 C11 117.7(3) . . ? C15 C10 P 117.4(2) . . ? C11 C10 P 124.8(2) . . ? C12 C11 C10 121.3(3) . . ? C13 C12 C11 119.8(3) . . ? C14 C13 C12 120.4(3) . . ? C13 C14 C15 120.0(3) . . ? C14 C15 C10 120.8(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C10 P Si1 C3 -69.2(2) . . . . ? C4 P Si1 C3 37.1(2) . . . . ? C10 P Si1 C2 47.85(15) . . . . ? C4 P Si1 C2 154.11(15) . . . . ? C10 P Si1 C1 167.06(14) . . . . ? C4 P Si1 C1 -86.68(15) . . . . ? C3 Si1 C1 Si2 -155.3(2) . . . . ? C2 Si1 C1 Si2 82.3(2) . . . . ? P Si1 C1 Si2 -32.8(2) . . . . ? C3 Si1 C1 Si3 70.4(2) . . . . ? C2 Si1 C1 Si3 -52.0(2) . . . . ? P Si1 C1 Si3 -167.09(11) . . . . ? C18 Si2 C1 Si1 74.0(2) . . . . ? C17 Si2 C1 Si1 -168.7(2) . . . . ? C16 Si2 C1 Si1 -47.3(2) . . . . ? C18 Si2 C1 Si3 -151.8(2) . . . . ? C17 Si2 C1 Si3 -34.5(2) . . . . ? C16 Si2 C1 Si3 86.9(2) . . . . ? C20 Si3 C1 Si1 86.0(2) . . . . ? C19 Si3 C1 Si1 -35.2(2) . . . . ? C21 Si3 C1 Si1 -152.0(2) . . . . ? C20 Si3 C1 Si2 -49.2(2) . . . . ? C19 Si3 C1 Si2 -170.4(2) . . . . ? C21 Si3 C1 Si2 72.8(2) . . . . ? C10 P C4 C9 -38.6(3) . . . . ? Si1 P C4 C9 -141.4(2) . . . . ? C10 P C4 C5 149.8(3) . . . . ? Si1 P C4 C5 47.1(3) . . . . ? C9 C4 C5 C6 0.5(5) . . . . ? P C4 C5 C6 172.3(2) . . . . ? C4 C5 C6 C7 -0.1(5) . . . . ? C5 C6 C7 C8 -0.2(5) . . . . ? C6 C7 C8 C9 0.0(5) . . . . ? C7 C8 C9 C4 0.4(5) . . . . ? C5 C4 C9 C8 -0.6(5) . . . . ? P C4 C9 C8 -172.5(3) . . . . ? C4 P C10 C15 143.8(2) . . . . ? Si1 P C10 C15 -109.1(2) . . . . ? C4 P C10 C11 -39.2(3) . . . . ? Si1 P C10 C11 68.0(3) . . . . ? C15 C10 C11 C12 1.7(5) . . . . ? P C10 C11 C12 -175.4(2) . . . . ? C10 C11 C12 C13 -0.5(5) . . . . ? C11 C12 C13 C14 -0.3(5) . . . . ? C12 C13 C14 C15 -0.2(5) . . . . ? C13 C14 C15 C10 1.4(5) . . . . ? C11 C10 C15 C14 -2.1(5) . . . . ? P C10 C15 C14 175.1(3) . . . . ? _refine_diff_density_max 0.313 _refine_diff_density_min -0.259 _refine_diff_density_rms 0.061 data_nov1199 _audit_creation_date 1999-11-10T16:02:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.1beta5 _audit_conform_dict_location ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic _publ_requested_category FM #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_name_common '[KPPh2].1/14(toluene)' _chemical_formula_moiety '(C12 H10 K1 P1) 1/14(C7 H8)' _chemical_formula_sum 'C12.50 H10.57 K P' _chemical_formula_weight 230.85 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1313(2) _cell_length_b 13.7513(2) _cell_length_c 39.8676(6) _cell_angle_alpha 90 _cell_angle_beta 94.8510(10) _cell_angle_gamma 90 _cell_volume 8265.7(2) _cell_formula_units_Z 28 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 50571 _cell_measurement_theta_min 4.246 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3348 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION NOT APPLIED # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.546 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device KappaCCD _diffrn_measurement_method CCD _diffrn_reflns_number 41955 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0646 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 47 _diffrn_reflns_theta_min 4.27 _diffrn_reflns_theta_max 25.03 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.989 _diffrn_measured_fraction_theta_max 0.989 _reflns_number_total 14434 _reflns_number_gt 9528 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _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)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The asymmetric unit contains seven KPPh2 units and a molecule of toluene disordered about an inversion centre for which the methyl position could not be reliably located. H atoms for the toluene were omitted. 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^)+(0.0845P)^2^+4.5202P] 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_number_reflns 14434 _refine_ls_number_parameters 895 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0941 _refine_ls_R_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.1626 _refine_ls_wR_factor_gt 0.1401 _refine_ls_goodness_of_fit_ref 0.981 _refine_ls_restrained_S_all 0.981 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.636 _refine_diff_density_min -0.417 _refine_diff_density_rms 0.066 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 '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' 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 K1 K 0.34147(5) 0.44286(6) 0.23433(2) 0.0506(2) Uani 1 1 d . . . K2 K 0.28284(5) 0.12962(6) 0.22341(2) 0.0518(2) Uani 1 1 d . . . K3 K 0.26478(6) 0.14620(7) 0.11230(2) 0.0595(3) Uani 1 1 d . . . K4 K -0.07588(5) -0.08887(6) 0.16595(2) 0.0470(2) Uani 1 1 d . . . K5 K -0.04590(6) 0.16436(7) 0.11913(2) 0.0642(3) Uani 1 1 d . . . K6 K -0.35449(6) -0.04371(7) 0.15179(3) 0.0628(3) Uani 1 1 d . . . K7 K -0.02620(8) -0.10003(8) 0.04054(2) 0.0752(3) Uani 1 1 d . . . P1 P 0.23127(6) 0.30885(8) 0.17197(2) 0.0485(3) Uani 1 1 d . . . P2 P -0.19060(7) 0.09653(8) 0.18454(3) 0.0552(3) Uani 1 1 d . . . P3 P -0.17956(8) -0.07388(9) 0.09193(3) 0.0635(3) Uani 1 1 d . . . P4 P 0.02021(9) 0.14890(9) 0.03984(3) 0.0682(3) Uani 1 1 d . . . P5 P 0.48674(7) 0.09445(8) 0.19913(3) 0.0563(3) Uani 1 1 d . . . P6 P 0.10934(7) 0.00815(8) 0.14261(3) 0.0507(3) Uani 1 1 d . . . P7 P 0.30288(7) 0.27406(7) 0.29093(3) 0.0492(3) Uani 1 1 d . . . C1 C 0.1201(2) 0.3421(3) 0.15594(9) 0.0439(9) Uani 1 1 d . . . C2 C 0.0519(3) 0.3299(3) 0.17750(10) 0.0578(11) Uani 1 1 d . . . H2 H 0.0663 0.3062 0.1997 0.069 Uiso 1 1 calc R . . C3 C -0.0358(3) 0.3518(4) 0.16720(12) 0.0698(13) Uani 1 1 d . . . H3 H -0.08 0.3426 0.1825 0.084 Uiso 1 1 calc R . . C4 C -0.0601(3) 0.3862(3) 0.13561(13) 0.0666(12) Uani 1 1 d . . . H4 H -0.1199 0.4039 0.1292 0.08 Uiso 1 1 calc R . . C5 C 0.0046(3) 0.3948(3) 0.11315(11) 0.0612(11) Uani 1 1 d . . . H5 H -0.0114 0.4158 0.0908 0.073 Uiso 1 1 calc R . . C6 C 0.0927(2) 0.3729(3) 0.12305(10) 0.0504(9) Uani 1 1 d . . . H6 H 0.1357 0.3791 0.1071 0.061 Uiso 1 1 calc R . . C7 C 0.3038(2) 0.3681(3) 0.14410(10) 0.0489(9) Uani 1 1 d . . . C8 C 0.2884(3) 0.4568(3) 0.12710(11) 0.0561(10) Uani 1 1 d . . . H8 H 0.2345 0.4905 0.1294 0.067 Uiso 1 1 calc R . . C9 C 0.3494(3) 0.4964(3) 0.10717(13) 0.0728(13) Uani 1 1 d . . . H9 H 0.3365 0.556 0.0957 0.087 Uiso 1 1 calc R . . C10 C 0.4289(3) 0.4500(4) 0.10385(15) 0.0865(16) Uani 1 1 d . . . H10 H 0.4708 0.4772 0.0901 0.104 Uiso 1 1 calc R . . C11 C 0.4469(3) 0.3647(4) 0.12045(14) 0.0783(15) Uani 1 1 d . . . H11 H 0.502 0.3331 0.1184 0.094 Uiso 1 1 calc R . . C12 C 0.3866(2) 0.3236(3) 0.14019(11) 0.0591(11) Uani 1 1 d . . . H12 H 0.4009 0.264 0.1514 0.071 Uiso 1 1 calc R . . C13 C -0.2112(2) 0.1130(2) 0.22836(9) 0.0433(9) Uani 1 1 d . . . C14 C -0.1548(2) 0.0634(3) 0.25251(11) 0.0495(9) Uani 1 1 d . . . H14 H -0.1059 0.0282 0.2453 0.059 Uiso 1 1 calc R . . C15 C -0.1680(3) 0.0640(3) 0.28628(11) 0.0557(11) Uani 1 1 d . . . H15 H -0.1293 0.0281 0.3017 0.067 Uiso 1 1 calc R . . C16 C -0.2373(3) 0.1168(3) 0.29798(11) 0.0565(10) Uani 1 1 d . . . H16 H -0.2456 0.1189 0.3213 0.068 Uiso 1 1 calc R . . C17 C -0.2938(3) 0.1662(3) 0.27491(10) 0.0490(9) Uani 1 1 d . . . H17 H -0.3413 0.203 0.2826 0.059 Uiso 1 1 calc R . . C18 C -0.2828(2) 0.1631(2) 0.24096(9) 0.0449(9) Uani 1 1 d . . . H18 H -0.3244 0.1955 0.2257 0.054 Uiso 1 1 calc R . . C19 C -0.2441(2) 0.1955(3) 0.16050(9) 0.0461(9) Uani 1 1 d . . . C20 C -0.2625(3) 0.1807(4) 0.12559(10) 0.0600(11) Uani 1 1 d . . . H20 H -0.2523 0.1185 0.1163 0.072 Uiso 1 1 calc R . . C21 C -0.2949(3) 0.2546(4) 0.10457(11) 0.0677(13) Uani 1 1 d . . . H21 H -0.3062 0.2421 0.0812 0.081 Uiso 1 1 calc R . . C22 C -0.3111(3) 0.3457(4) 0.11680(12) 0.0671(12) Uani 1 1 d . . . H22 H -0.3328 0.3963 0.1021 0.081 Uiso 1 1 calc R . . C23 C -0.2949(3) 0.3619(3) 0.15102(11) 0.0604(11) Uani 1 1 d . . . H23 H -0.3069 0.4241 0.1599 0.073 Uiso 1 1 calc R . . C24 C -0.2616(2) 0.2895(3) 0.17237(10) 0.0499(9) Uani 1 1 d . . . H24 H -0.2502 0.3032 0.1957 0.06 Uiso 1 1 calc R . . C25 C -0.1701(3) -0.1996(3) 0.07852(10) 0.0609(11) Uani 1 1 d . . . C26 C -0.1049(4) -0.2567(4) 0.09635(12) 0.0812(15) Uani 1 1 d . . . H26 H -0.0675 -0.227 0.1138 0.097 Uiso 1 1 calc R . . C27 C -0.0929(4) -0.3540(4) 0.08963(13) 0.0934(18) Uani 1 1 d . . . H27 H -0.0488 -0.3902 0.1026 0.112 Uiso 1 1 calc R . . C28 C -0.1449(4) -0.3986(4) 0.06420(13) 0.0881(16) Uani 1 1 d . . . H28 H -0.1383 -0.466 0.0599 0.106 Uiso 1 1 calc R . . C29 C -0.2063(4) -0.3441(4) 0.04510(12) 0.0762(14) Uani 1 1 d . . . H29 H -0.2408 -0.3736 0.0269 0.091 Uiso 1 1 calc R . . C30 C -0.2187(3) -0.2463(3) 0.05215(10) 0.0628(11) Uani 1 1 d . . . H30 H -0.2616 -0.2103 0.0385 0.075 Uiso 1 1 calc R . . C31 C -0.2609(3) -0.0214(3) 0.06094(9) 0.0534(10) Uani 1 1 d . . . C32 C -0.2385(3) 0.0579(3) 0.04161(10) 0.0616(11) Uani 1 1 d . . . H32 H -0.1783 0.0782 0.0429 0.074 Uiso 1 1 calc R . . C33 C -0.2996(4) 0.1081(4) 0.02066(12) 0.0804(14) Uani 1 1 d . . . H33 H -0.2817 0.1636 0.0088 0.096 Uiso 1 1 calc R . . C34 C -0.3835(4) 0.0791(5) 0.01707(14) 0.0895(16) Uani 1 1 d . . . H34 H -0.4246 0.1128 0.0019 0.107 Uiso 1 1 calc R . . C35 C -0.4119(3) 0.0020(5) 0.03466(14) 0.0887(18) Uani 1 1 d . . . H35 H -0.4724 -0.0171 0.032 0.106 Uiso 1 1 calc R . . C36 C -0.3509(3) -0.0495(4) 0.05682(11) 0.0737(13) Uani 1 1 d . . . H36 H -0.3706 -0.1036 0.069 0.088 Uiso 1 1 calc R . . C37 C -0.0373(3) 0.2577(3) 0.02365(11) 0.0668(12) Uani 1 1 d . . . C38 C -0.1206(3) 0.2833(4) 0.03423(13) 0.0748(13) Uani 1 1 d . . . H38 H -0.1436 0.2451 0.0514 0.09 Uiso 1 1 calc R . . C39 C -0.1699(4) 0.3588(5) 0.02149(17) 0.0932(17) Uani 1 1 d . . . H39 H -0.2263 0.3716 0.0294 0.112 Uiso 1 1 calc R . . C40 C -0.1382(4) 0.4173(4) -0.00289(16) 0.0946(17) Uani 1 1 d . . . H40 H -0.1722 0.4707 -0.0119 0.113 Uiso 1 1 calc R . . C41 C -0.0561(4) 0.3969(3) -0.01407(14) 0.0817(15) Uani 1 1 d . . . H41 H -0.0333 0.4373 -0.0306 0.098 Uiso 1 1 calc R . . C42 C -0.0071(3) 0.3189(3) -0.00142(11) 0.0694(12) Uani 1 1 d . . . H42 H 0.0487 0.3058 -0.0098 0.083 Uiso 1 1 calc R . . C43 C 0.1361(3) 0.1818(3) 0.03760(9) 0.0624(11) Uani 1 1 d . . . C44 C 0.1717(3) 0.2743(3) 0.04576(11) 0.0700(13) Uani 1 1 d . . . H44 H 0.1324 0.325 0.0509 0.084 Uiso 1 1 calc R . . C45 C 0.2614(4) 0.2943(4) 0.04652(12) 0.0854(15) Uani 1 1 d . . . H45 H 0.283 0.3575 0.0523 0.102 Uiso 1 1 calc R . . C46 C 0.3202(4) 0.2206(5) 0.03868(13) 0.0876(16) Uani 1 1 d . . . H46 H 0.3821 0.233 0.0391 0.105 Uiso 1 1 calc R . . C47 C 0.2863(4) 0.1292(4) 0.03027(11) 0.0781(14) Uani 1 1 d . . . H47 H 0.3256 0.0786 0.0251 0.094 Uiso 1 1 calc R . . C48 C 0.1975(4) 0.1109(3) 0.02931(10) 0.0669(12) Uani 1 1 d . . . H48 H 0.1765 0.048 0.0228 0.08 Uiso 1 1 calc R . . C49 C 0.4521(2) 0.0417(3) 0.15905(10) 0.0507(10) Uani 1 1 d . . . C50 C 0.4829(3) 0.0882(3) 0.13029(12) 0.0641(12) Uani 1 1 d . . . H50 H 0.5214 0.1426 0.1336 0.077 Uiso 1 1 calc R . . C51 C 0.4590(4) 0.0571(5) 0.09796(14) 0.0850(16) Uani 1 1 d . . . H51 H 0.4797 0.0913 0.0794 0.102 Uiso 1 1 calc R . . C52 C 0.4057(4) -0.0229(5) 0.09230(14) 0.0930(17) Uani 1 1 d . . . H52 H 0.3911 -0.0454 0.07 0.112 Uiso 1 1 calc R . . C53 C 0.3734(3) -0.0704(4) 0.11911(13) 0.0778(14) Uani 1 1 d . . . H53 H 0.336 -0.1254 0.1153 0.093 Uiso 1 1 calc R . . C54 C 0.3955(3) -0.0379(3) 0.15169(11) 0.0582(10) Uani 1 1 d . . . H54 H 0.3713 -0.0707 0.1698 0.07 Uiso 1 1 calc R . . C55 C 0.4686(2) 0.0024(3) 0.23043(10) 0.0456(9) Uani 1 1 d . . . C56 C 0.4732(2) -0.0991(3) 0.22689(10) 0.0457(9) Uani 1 1 d . . . H56 H 0.4795 -0.1258 0.2052 0.055 Uiso 1 1 calc R . . C57 C 0.4691(2) -0.1608(3) 0.25383(10) 0.0489(9) Uani 1 1 d . . . H57 H 0.4725 -0.229 0.2503 0.059 Uiso 1 1 calc R . . C58 C 0.4601(2) -0.1261(3) 0.28607(10) 0.0502(9) Uani 1 1 d . . . H58 H 0.4573 -0.1695 0.3045 0.06 Uiso 1 1 calc R . . C59 C 0.4555(3) -0.0271(3) 0.29058(11) 0.0553(10) Uani 1 1 d . . . H59 H 0.4501 -0.0014 0.3124 0.066 Uiso 1 1 calc R . . C60 C 0.4585(2) 0.0355(3) 0.26343(10) 0.0521(10) Uani 1 1 d . . . H60 H 0.4536 0.1035 0.2672 0.063 Uiso 1 1 calc R . . C61 C 0.1355(3) -0.1025(3) 0.12104(9) 0.0539(10) Uani 1 1 d . . . C62 C 0.1356(3) -0.1975(3) 0.13385(11) 0.0718(13) Uani 1 1 d . . . H62 H 0.1232 -0.2073 0.1566 0.086 Uiso 1 1 calc R . . C63 C 0.1532(5) -0.2769(4) 0.11455(15) 0.112(2) Uani 1 1 d . . . H63 H 0.1538 -0.3401 0.1242 0.135 Uiso 1 1 calc R . . C64 C 0.1700(5) -0.2658(6) 0.08113(17) 0.126(3) Uani 1 1 d . . . H64 H 0.1817 -0.3206 0.0677 0.152 Uiso 1 1 calc R . . C65 C 0.1694(4) -0.1750(7) 0.06822(14) 0.113(2) Uani 1 1 d . . . H65 H 0.18 -0.1667 0.0452 0.135 Uiso 1 1 calc R . . C66 C 0.1538(3) -0.0937(4) 0.08723(11) 0.0768(14) Uani 1 1 d . . . H66 H 0.1556 -0.031 0.0773 0.092 Uiso 1 1 calc R . . C67 C 0.1313(2) -0.0154(3) 0.18739(9) 0.0413(8) Uani 1 1 d . . . C68 C 0.1949(2) -0.0790(3) 0.20293(9) 0.0459(9) Uani 1 1 d . . . H68 H 0.2276 -0.1198 0.1892 0.055 Uiso 1 1 calc R . . C69 C 0.2114(3) -0.0841(3) 0.23746(10) 0.0488(9) Uani 1 1 d . . . H69 H 0.2552 -0.1277 0.247 0.059 Uiso 1 1 calc R . . C70 C 0.1649(2) -0.0264(3) 0.25837(10) 0.0493(9) Uani 1 1 d . . . H70 H 0.1763 -0.0302 0.2821 0.059 Uiso 1 1 calc R . . C71 C 0.1016(2) 0.0369(3) 0.24385(10) 0.0484(9) Uani 1 1 d . . . H71 H 0.0693 0.0772 0.2578 0.058 Uiso 1 1 calc R . . C72 C 0.0847(2) 0.0422(3) 0.20943(10) 0.0456(9) Uani 1 1 d . . . H72 H 0.0404 0.0858 0.2002 0.055 Uiso 1 1 calc R . . C73 C 0.1849(2) 0.2541(2) 0.29380(9) 0.0432(8) Uani 1 1 d . . . C74 C 0.1428(3) 0.1911(3) 0.31599(10) 0.0547(10) Uani 1 1 d . . . H74 H 0.1779 0.1543 0.3323 0.066 Uiso 1 1 calc R . . C75 C 0.0506(3) 0.1831(3) 0.31395(10) 0.0587(11) Uani 1 1 d . . . H75 H 0.024 0.1405 0.3289 0.07 Uiso 1 1 calc R . . C76 C -0.0029(3) 0.2354(3) 0.29074(10) 0.0568(10) Uani 1 1 d . . . H76 H -0.0656 0.2308 0.2902 0.068 Uiso 1 1 calc R . . C77 C 0.0369(3) 0.2945(3) 0.26834(9) 0.0485(9) Uani 1 1 d . . . H77 H 0.0011 0.3294 0.2517 0.058 Uiso 1 1 calc R . . C78 C 0.1276(2) 0.3034(3) 0.26987(9) 0.0447(9) Uani 1 1 d . . . H78 H 0.1528 0.3445 0.2541 0.054 Uiso 1 1 calc R . . C79 C 0.3626(3) 0.2329(3) 0.32986(9) 0.0490(9) Uani 1 1 d . . . C80 C 0.3311(3) 0.2275(3) 0.36188(11) 0.0626(11) Uani 1 1 d . . . H80 H 0.2701 0.2399 0.3641 0.075 Uiso 1 1 calc R . . C81 C 0.3864(3) 0.2045(4) 0.39049(11) 0.0768(14) Uani 1 1 d . . . H81 H 0.3623 0.1996 0.4117 0.092 Uiso 1 1 calc R . . C82 C 0.4749(4) 0.1888(4) 0.38836(12) 0.0848(16) Uani 1 1 d . . . H82 H 0.5124 0.1741 0.408 0.102 Uiso 1 1 calc R . . C83 C 0.5092(3) 0.1945(3) 0.35756(12) 0.0720(13) Uani 1 1 d . . . H83 H 0.5709 0.1846 0.3559 0.086 Uiso 1 1 calc R . . C84 C 0.4538(3) 0.2147(3) 0.32885(11) 0.0552(10) Uani 1 1 d . . . H84 H 0.4785 0.2163 0.3077 0.066 Uiso 1 1 calc R . . C85 C 0.5470(14) 0.3723(16) 0.0076(5) 0.311(8) Uiso 1 1 d . . . C86 C 0.4620(11) 0.4274(12) -0.0135(4) 0.247(6) Uiso 1 1 d . . . C87 C 0.4185(12) 0.5198(17) -0.0212(5) 0.292(7) 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 K1 0.0400(5) 0.0477(5) 0.0634(6) 0.0071(4) -0.0008(4) 0.0014(4) K2 0.0501(5) 0.0480(5) 0.0568(5) 0.0002(4) 0.0026(4) -0.0058(4) K3 0.0674(6) 0.0648(6) 0.0488(5) -0.0101(4) 0.0193(4) -0.0093(5) K4 0.0540(5) 0.0428(4) 0.0450(5) 0.0076(4) 0.0081(4) 0.0032(4) K5 0.0736(6) 0.0669(6) 0.0540(6) 0.0157(5) 0.0156(5) 0.0145(5) K6 0.0514(5) 0.0644(6) 0.0728(6) 0.0149(5) 0.0061(4) 0.0057(4) K7 0.1024(8) 0.0716(7) 0.0531(6) -0.0060(5) 0.0158(5) -0.0154(6) P1 0.0449(6) 0.0566(6) 0.0441(6) -0.0040(5) 0.0046(4) 0.0060(5) P2 0.0591(7) 0.0508(6) 0.0577(7) -0.0060(5) 0.0166(5) 0.0068(5) P3 0.0822(8) 0.0612(7) 0.0458(6) -0.0068(5) -0.0025(5) 0.0037(6) P4 0.0949(9) 0.0615(7) 0.0509(7) -0.0067(6) 0.0216(6) -0.0218(6) P5 0.0547(6) 0.0471(6) 0.0670(7) 0.0057(5) 0.0050(5) -0.0079(5) P6 0.0541(6) 0.0519(6) 0.0469(6) 0.0055(5) 0.0090(5) 0.0019(5) P7 0.0538(6) 0.0507(6) 0.0441(6) 0.0010(5) 0.0098(4) 0.0023(5) C1 0.044(2) 0.046(2) 0.042(2) -0.0083(17) 0.0049(16) -0.0006(16) C2 0.049(2) 0.084(3) 0.042(2) -0.007(2) 0.0093(18) -0.007(2) C3 0.044(3) 0.095(4) 0.072(3) -0.021(3) 0.017(2) -0.007(2) C4 0.040(2) 0.077(3) 0.082(3) -0.008(3) -0.002(2) 0.007(2) C5 0.055(3) 0.067(3) 0.060(3) 0.010(2) -0.007(2) -0.003(2) C6 0.045(2) 0.058(2) 0.049(2) 0.0024(19) 0.0033(17) -0.0013(18) C7 0.041(2) 0.046(2) 0.059(2) -0.0124(19) -0.0012(17) -0.0042(17) C8 0.045(2) 0.049(2) 0.075(3) -0.008(2) 0.007(2) -0.0050(19) C9 0.069(3) 0.058(3) 0.092(4) 0.004(3) 0.016(3) -0.014(2) C10 0.070(3) 0.068(3) 0.126(5) 0.002(3) 0.032(3) -0.023(3) C11 0.041(3) 0.069(3) 0.128(4) -0.016(3) 0.027(3) -0.010(2) C12 0.038(2) 0.055(2) 0.084(3) -0.010(2) 0.003(2) -0.0020(19) C13 0.041(2) 0.0349(18) 0.054(2) -0.0054(16) 0.0034(17) -0.0052(16) C14 0.039(2) 0.041(2) 0.068(3) 0.0015(19) 0.0034(18) -0.0043(16) C15 0.053(2) 0.044(2) 0.067(3) 0.010(2) -0.013(2) -0.0105(19) C16 0.075(3) 0.047(2) 0.048(2) 0.0020(19) 0.005(2) -0.018(2) C17 0.058(2) 0.0386(19) 0.051(2) 0.0013(18) 0.0111(18) -0.0002(17) C18 0.048(2) 0.0386(19) 0.048(2) 0.0022(17) 0.0061(17) 0.0015(17) C19 0.035(2) 0.058(2) 0.047(2) -0.0042(18) 0.0137(16) -0.0053(17) C20 0.052(2) 0.079(3) 0.051(3) -0.013(2) 0.0148(19) -0.010(2) C21 0.046(2) 0.109(4) 0.049(3) 0.007(3) 0.0083(19) -0.010(3) C22 0.041(2) 0.095(4) 0.066(3) 0.020(3) 0.009(2) 0.009(2) C23 0.053(3) 0.066(3) 0.065(3) 0.010(2) 0.021(2) 0.013(2) C24 0.044(2) 0.060(2) 0.047(2) -0.0021(19) 0.0124(17) -0.0018(19) C25 0.087(3) 0.060(3) 0.037(2) 0.000(2) 0.016(2) 0.001(2) C26 0.117(4) 0.076(3) 0.050(3) -0.012(2) 0.006(3) 0.024(3) C27 0.157(5) 0.070(3) 0.054(3) -0.004(3) 0.016(3) 0.036(3) C28 0.152(5) 0.059(3) 0.058(3) -0.003(3) 0.036(3) 0.001(3) C29 0.108(4) 0.067(3) 0.057(3) -0.011(3) 0.025(3) -0.015(3) C30 0.087(3) 0.059(3) 0.044(2) 0.001(2) 0.016(2) -0.009(2) C31 0.058(3) 0.062(3) 0.040(2) -0.0133(19) 0.0042(17) -0.004(2) C32 0.074(3) 0.054(2) 0.056(3) 0.000(2) 0.000(2) -0.005(2) C33 0.099(4) 0.075(3) 0.065(3) -0.001(3) -0.011(3) 0.007(3) C34 0.094(4) 0.103(4) 0.069(4) -0.014(3) -0.011(3) 0.016(4) C35 0.055(3) 0.142(6) 0.068(3) -0.038(4) -0.001(3) 0.001(3) C36 0.077(3) 0.094(4) 0.052(3) -0.014(3) 0.021(2) -0.012(3) C37 0.089(3) 0.062(3) 0.051(3) -0.019(2) 0.013(2) -0.023(2) C38 0.082(3) 0.075(3) 0.070(3) -0.018(3) 0.023(3) -0.022(3) C39 0.091(4) 0.082(4) 0.109(5) -0.026(4) 0.022(3) -0.009(3) C40 0.110(5) 0.070(3) 0.104(5) -0.027(3) 0.008(4) 0.003(3) C41 0.113(4) 0.052(3) 0.083(4) -0.013(3) 0.023(3) -0.011(3) C42 0.097(3) 0.053(3) 0.060(3) -0.012(2) 0.022(2) -0.011(3) C43 0.098(3) 0.059(3) 0.032(2) -0.0033(19) 0.014(2) -0.007(2) C44 0.094(4) 0.068(3) 0.050(3) -0.008(2) 0.015(2) -0.017(3) C45 0.106(4) 0.087(4) 0.065(3) -0.003(3) 0.011(3) -0.025(3) C46 0.082(4) 0.121(5) 0.061(3) 0.012(3) 0.016(3) -0.013(4) C47 0.109(4) 0.084(4) 0.044(3) 0.003(2) 0.021(3) 0.013(3) C48 0.092(4) 0.070(3) 0.042(2) 0.003(2) 0.021(2) -0.009(3) C49 0.037(2) 0.055(2) 0.062(3) 0.008(2) 0.0152(18) 0.0119(18) C50 0.054(3) 0.069(3) 0.073(3) 0.012(2) 0.022(2) 0.020(2) C51 0.102(4) 0.088(4) 0.070(4) 0.012(3) 0.036(3) 0.039(3) C52 0.133(5) 0.086(4) 0.061(3) -0.003(3) 0.013(3) 0.037(4) C53 0.092(4) 0.063(3) 0.077(4) -0.011(3) -0.003(3) 0.015(3) C54 0.058(3) 0.058(3) 0.060(3) 0.002(2) 0.009(2) 0.010(2) C55 0.0311(19) 0.045(2) 0.061(3) -0.0009(18) 0.0027(16) 0.0003(16) C56 0.041(2) 0.047(2) 0.050(2) -0.0010(18) 0.0066(16) -0.0020(17) C57 0.042(2) 0.0374(19) 0.067(3) -0.0034(19) 0.0048(18) -0.0038(16) C58 0.047(2) 0.047(2) 0.057(3) 0.0056(19) 0.0085(18) -0.0039(18) C59 0.055(2) 0.056(2) 0.056(3) -0.007(2) 0.0105(19) -0.001(2) C60 0.053(2) 0.041(2) 0.061(3) -0.0002(19) -0.0004(19) 0.0031(18) C61 0.058(2) 0.065(3) 0.039(2) -0.0003(19) 0.0086(17) 0.004(2) C62 0.104(4) 0.061(3) 0.049(3) -0.008(2) 0.002(2) 0.006(3) C63 0.186(6) 0.073(3) 0.071(4) -0.026(3) -0.031(4) 0.041(4) C64 0.168(7) 0.136(6) 0.070(4) -0.055(4) -0.025(4) 0.059(5) C65 0.125(5) 0.171(7) 0.042(3) -0.022(4) 0.005(3) 0.036(5) C66 0.094(4) 0.096(4) 0.042(3) -0.005(3) 0.014(2) 0.000(3) C67 0.040(2) 0.0420(19) 0.043(2) -0.0011(16) 0.0072(15) -0.0052(16) C68 0.051(2) 0.041(2) 0.047(2) -0.0025(17) 0.0134(17) 0.0021(17) C69 0.056(2) 0.042(2) 0.049(2) 0.0062(17) 0.0072(18) 0.0081(18) C70 0.057(2) 0.049(2) 0.044(2) -0.0044(18) 0.0113(18) -0.0019(19) C71 0.044(2) 0.053(2) 0.049(2) -0.0143(18) 0.0112(17) -0.0010(18) C72 0.037(2) 0.044(2) 0.056(2) -0.0077(18) 0.0042(17) 0.0041(16) C73 0.057(2) 0.0355(18) 0.039(2) -0.0079(16) 0.0138(17) -0.0003(17) C74 0.077(3) 0.046(2) 0.043(2) -0.0017(18) 0.0183(19) -0.004(2) C75 0.077(3) 0.050(2) 0.053(3) -0.013(2) 0.030(2) -0.024(2) C76 0.062(3) 0.055(2) 0.054(3) -0.018(2) 0.016(2) -0.013(2) C77 0.054(2) 0.050(2) 0.044(2) -0.0094(18) 0.0134(17) -0.0019(18) C78 0.052(2) 0.044(2) 0.039(2) -0.0059(16) 0.0133(16) 0.0023(17) C79 0.064(3) 0.039(2) 0.045(2) -0.0010(17) 0.0087(18) 0.0083(18) C80 0.070(3) 0.064(3) 0.056(3) -0.001(2) 0.015(2) 0.019(2) C81 0.094(4) 0.090(4) 0.047(3) 0.006(2) 0.011(2) 0.034(3) C82 0.103(4) 0.097(4) 0.053(3) 0.008(3) 0.001(3) 0.043(3) C83 0.072(3) 0.071(3) 0.074(3) 0.003(2) 0.006(2) 0.022(2) C84 0.069(3) 0.042(2) 0.055(3) -0.0005(19) 0.010(2) 0.010(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 K1 C16 3.086(4) 2 ? K1 C56 3.138(4) 2_655 ? K1 C15 3.159(4) 2 ? K1 C17 3.169(4) 2 ? K1 C55 3.197(3) 2_655 ? K1 C57 3.200(4) 2_655 ? K1 C60 3.278(4) 2_655 ? K1 C58 3.315(4) 2_655 ? K1 P7 3.3232(13) . ? K1 C18 3.328(4) 2 ? K1 C59 3.334(4) 2_655 ? K1 C14 3.354(4) 2 ? K2 C70 3.186(4) . ? K2 C71 3.193(4) . ? K2 C69 3.197(4) . ? K2 C72 3.235(4) . ? K2 C68 3.238(4) . ? K2 C60 3.251(4) . ? K2 P1 3.2585(13) . ? K2 C67 3.278(3) . ? K2 C55 3.302(3) . ? K2 P7 3.3386(13) . ? K2 P5 3.3459(14) . ? K3 C12 3.199(4) . ? K3 C51 3.279(5) . ? K3 C46 3.284(5) . ? K3 C52 3.298(5) . ? K3 C45 3.318(5) . ? K3 C47 3.322(4) . ? K3 P6 3.3281(14) . ? K3 P1 3.3350(13) . ? K3 C7 3.337(4) . ? K3 C44 3.390(5) . ? K3 C53 3.401(5) . ? K3 C50 3.413(4) . ? K4 C77 3.086(4) 2_545 ? K4 C78 3.114(3) 2_545 ? K4 C76 3.146(4) 2_545 ? K4 P2 3.2062(13) . ? K4 C73 3.226(3) 2_545 ? K4 P3 3.2291(14) . ? K4 C75 3.251(4) 2_545 ? K4 C74 3.290(4) 2_545 ? K4 P6 3.3077(13) . ? K4 C67 3.335(3) . ? K4 C72 3.382(4) . ? K4 K5 3.9948(12) . ? K5 C4 3.132(5) . ? K5 C3 3.208(5) . ? K5 P6 3.2615(14) . ? K5 C5 3.273(4) . ? K5 C20 3.316(4) . ? K5 P4 3.4019(15) . ? K5 C2 3.494(4) . ? K5 P2 3.6646(14) . ? K5 K7 4.8253(14) . ? K6 C50 3.118(4) 1_455 ? K6 C79 3.163(4) 2_545 ? K6 C49 3.189(3) 1_455 ? K6 C80 3.218(4) 2_545 ? K6 P2 3.3205(15) . ? K6 P7 3.4352(14) 2_545 ? K6 P5 3.7025(15) 1_455 ? K6 P3 3.7339(16) . ? K6 K1 4.5311(13) 2_545 ? K7 C25 3.077(4) . ? K7 C66 3.168(5) . ? K7 C65 3.238(7) . ? K7 P3 3.2430(17) . ? K7 P4 3.2831(15) 3 ? K7 C26 3.385(5) . ? K7 C42 3.446(4) 3 ? K7 P4 3.4949(16) . ? K7 K7 4.368(2) 3 ? P1 C1 1.807(4) . ? P1 C7 1.819(4) . ? P2 C13 1.814(4) . ? P2 C19 1.815(4) . ? P3 C31 1.818(4) . ? P3 C25 1.819(4) . ? P4 C43 1.821(5) . ? P4 C37 1.822(5) . ? P4 K7 3.2832(15) 3 ? P5 C49 1.793(4) . ? P5 C55 1.815(4) . ? P5 K6 3.7023(15) 1_655 ? P6 C61 1.808(4) . ? P6 C67 1.817(4) . ? P7 C79 1.819(4) . ? P7 C73 1.819(4) . ? P7 K6 3.4355(14) 2 ? C1 C2 1.407(5) . ? C1 C6 1.407(5) . ? C2 C3 1.389(6) . ? C3 C4 1.366(6) . ? C4 C5 1.387(6) . ? C5 C6 1.390(5) . ? C7 C8 1.406(5) . ? C7 C12 1.415(5) . ? C8 C9 1.380(6) . ? C9 C10 1.378(7) . ? C10 C11 1.363(7) . ? C11 C12 1.376(6) . ? C13 C14 1.407(5) . ? C13 C18 1.411(5) . ? C13 K1 3.474(4) 2_545 ? C14 C15 1.378(6) . ? C14 K1 3.354(4) 2_545 ? C15 C16 1.388(6) . ? C15 K1 3.159(4) 2_545 ? C16 C17 1.381(5) . ? C16 K1 3.086(4) 2_545 ? C17 C18 1.379(5) . ? C17 K1 3.169(4) 2_545 ? C18 K1 3.328(4) 2_545 ? C19 C24 1.409(5) . ? C19 C20 1.410(5) . ? C20 C21 1.380(6) . ? C21 C22 1.374(7) . ? C22 C23 1.384(6) . ? C23 C24 1.377(5) . ? C25 C30 1.388(6) . ? C25 C26 1.406(6) . ? C26 C27 1.380(7) . ? C27 C28 1.374(7) . ? C28 C29 1.373(7) . ? C29 C30 1.390(6) . ? C31 C32 1.393(6) . ? C31 C36 1.413(6) . ? C32 C33 1.379(6) . ? C33 C34 1.327(7) . ? C34 C35 1.361(8) . ? C35 C36 1.413(7) . ? C37 C38 1.407(7) . ? C37 C42 1.412(6) . ? C38 C39 1.353(7) . ? C39 C40 1.378(8) . ? C40 C41 1.384(8) . ? C41 C42 1.375(7) . ? C42 K7 3.447(4) 3 ? C43 C48 1.406(6) . ? C43 C44 1.408(6) . ? C44 C45 1.383(7) . ? C45 C46 1.401(8) . ? C46 C47 1.388(7) . ? C47 C48 1.364(7) . ? C49 C54 1.405(5) . ? C49 C50 1.425(6) . ? C49 K6 3.189(3) 1_655 ? C50 C51 1.377(7) . ? C50 K6 3.118(4) 1_655 ? C51 C52 1.372(8) . ? C52 C53 1.377(7) . ? C53 C54 1.387(6) . ? C55 C56 1.404(5) . ? C55 C60 1.413(5) . ? C55 K1 3.197(3) 2_645 ? C56 C57 1.375(5) . ? C56 K1 3.138(4) 2_645 ? C57 C58 1.388(5) . ? C57 K1 3.200(4) 2_645 ? C58 C59 1.377(5) . ? C58 K1 3.315(4) 2_645 ? C59 C60 1.387(5) . ? C59 K1 3.334(4) 2_645 ? C60 K1 3.278(4) 2_645 ? C61 C62 1.403(6) . ? C61 C66 1.404(6) . ? C62 C63 1.375(6) . ? C63 C64 1.386(9) . ? C64 C65 1.351(9) . ? C65 C66 1.383(8) . ? C67 C68 1.405(5) . ? C67 C72 1.415(5) . ? C68 C69 1.380(5) . ? C69 C70 1.384(5) . ? C70 C71 1.385(5) . ? C71 C72 1.377(5) . ? C73 C78 1.407(5) . ? C73 C74 1.426(5) . ? C73 K4 3.226(3) 2 ? C74 C75 1.395(6) . ? C74 K4 3.290(4) 2 ? C75 C76 1.379(6) . ? C75 K4 3.251(4) 2 ? C76 C77 1.383(5) . ? C76 K4 3.146(4) 2 ? C77 C78 1.375(5) . ? C77 K4 3.086(4) 2 ? C78 K4 3.114(3) 2 ? C79 C80 1.402(5) . ? C79 C84 1.408(5) . ? C79 K6 3.163(4) 2 ? C80 C81 1.393(6) . ? C80 K6 3.218(4) 2 ? C81 C82 1.366(7) . ? C82 C83 1.376(7) . ? C83 C84 1.388(6) . ? C85 C87 1.65(2) 3_665 ? C85 C86 1.66(2) . ? C86 C87 1.45(2) . ? C87 C85 1.65(2) 3_665 ? 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 C16 K1 C56 138.73(11) 2 2_655 ? C16 K1 C15 25.65(11) 2 2 ? C56 K1 C15 155.95(10) 2_655 2 ? C16 K1 C17 25.46(10) 2 2 ? C56 K1 C17 114.85(10) 2_655 2 ? C15 K1 C17 44.17(11) 2 2 ? C16 K1 C55 113.18(11) 2 2_655 ? C56 K1 C55 25.59(9) 2_655 2_655 ? C15 K1 C55 132.52(10) 2 2_655 ? C17 K1 C55 89.44(10) 2 2_655 ? C16 K1 C57 145.73(11) 2 2_655 ? C56 K1 C57 25.03(9) 2_655 2_655 ? C15 K1 C57 170.96(12) 2 2_655 ? C17 K1 C57 129.86(10) 2 2_655 ? C55 K1 C57 44.64(9) 2_655 2_655 ? C16 K1 C60 98.51(11) 2 2_655 ? C56 K1 C60 43.43(10) 2_655 2_655 ? C15 K1 C60 123.17(11) 2 2_655 ? C17 K1 C60 80.02(10) 2 2_655 ? C55 K1 C60 25.16(9) 2_655 2_655 ? C57 K1 C60 49.90(10) 2_655 2_655 ? C16 K1 C58 124.11(11) 2 2_655 ? C56 K1 C58 43.82(10) 2_655 2_655 ? C15 K1 C58 146.84(12) 2 2_655 ? C17 K1 C58 116.78(10) 2 2_655 ? C55 K1 C58 51.82(10) 2_655 2_655 ? C57 K1 C58 24.53(9) 2_655 2_655 ? C60 K1 C58 42.67(10) 2_655 2_655 ? C16 K1 P7 135.39(9) 2 . ? C56 K1 P7 74.82(7) 2_655 . ? C15 K1 P7 110.81(9) 2 . ? C17 K1 P7 134.80(8) 2 . ? C55 K1 P7 94.79(7) 2_655 . ? C57 K1 P7 78.19(7) 2_655 . ? C60 K1 P7 117.90(7) 2_655 . ? C58 K1 P7 100.45(7) 2_655 . ? C16 K1 C18 43.83(10) 2 2 ? C56 K1 C18 105.72(9) 2_655 2 ? C15 K1 C18 50.24(10) 2 2 ? C17 K1 C18 24.35(9) 2 2 ? C55 K1 C18 83.66(9) 2_655 2 ? C57 K1 C18 128.30(10) 2_655 2 ? C60 K1 C18 84.67(10) 2_655 2 ? C58 K1 C18 127.09(9) 2_655 2 ? P7 K1 C18 111.59(7) . 2 ? C16 K1 C59 103.33(11) 2 2_655 ? C56 K1 C59 50.37(10) 2_655 2_655 ? C15 K1 C59 128.58(11) 2 2_655 ? C17 K1 C59 92.94(10) 2 2_655 ? C55 K1 C59 44.13(10) 2_655 2_655 ? C57 K1 C59 42.50(10) 2_655 2_655 ? C60 K1 C59 24.20(9) 2_655 2_655 ? C58 K1 C59 23.90(9) 2_655 2_655 ? P7 K1 C59 120.55(8) . 2_655 ? C18 K1 C59 104.54(10) 2 2_655 ? C16 K1 C14 43.53(11) 2 2 ? C56 K1 C14 137.97(10) 2_655 2 ? C15 K1 C14 24.18(10) 2 2 ? C17 K1 C14 49.69(10) 2 2 ? C55 K1 C14 122.85(10) 2_655 2 ? C57 K1 C14 162.29(11) 2_655 2 ? C60 K1 C14 126.25(10) 2_655 2 ? C58 K1 C14 166.39(10) 2_655 2 ? P7 K1 C14 92.32(7) . 2 ? C18 K1 C14 41.82(9) 2 2 ? C59 K1 C14 142.63(10) 2_655 2 ? C70 K2 C71 25.08(9) . . ? C70 K2 C69 25.05(9) . . ? C71 K2 C69 43.73(10) . . ? C70 K2 C72 43.94(10) . . ? C71 K2 C72 24.72(9) . . ? C69 K2 C72 50.68(10) . . ? C70 K2 C68 43.96(9) . . ? C71 K2 C68 50.71(9) . . ? C69 K2 C68 24.76(9) . . ? C72 K2 C68 43.29(9) . . ? C70 K2 C60 88.97(10) . . ? C71 K2 C60 113.59(10) . . ? C69 K2 C60 79.79(10) . . ? C72 K2 C60 130.10(10) . . ? C68 K2 C60 94.17(10) . . ? C70 K2 P1 132.19(8) . . ? C71 K2 P1 107.32(8) . . ? C69 K2 P1 137.65(8) . . ? C72 K2 P1 90.20(7) . . ? C68 K2 P1 116.11(7) . . ? C60 K2 P1 138.79(8) . . ? C70 K2 C67 52.04(9) . . ? C71 K2 C67 44.30(9) . . ? C69 K2 C67 44.19(9) . . ? C72 K2 C67 25.09(8) . . ? C68 K2 C67 24.90(9) . . ? C60 K2 C67 119.05(9) . . ? P1 K2 C67 93.62(7) . . ? C70 K2 C55 96.31(10) . . ? C71 K2 C55 120.66(10) . . ? C69 K2 C55 78.23(9) . . ? C72 K2 C55 125.97(9) . . ? C68 K2 C55 83.13(9) . . ? C60 K2 C55 24.89(9) . . ? P1 K2 C55 127.66(7) . . ? C67 K2 C55 105.87(9) . . ? C70 K2 P7 93.67(7) . . ? C71 K2 P7 93.05(7) . . ? C69 K2 P7 114.49(7) . . ? C72 K2 P7 112.32(7) . . ? C68 K2 P7 137.55(7) . . ? C60 K2 P7 80.00(7) . . ? P1 K2 P7 93.33(3) . . ? C67 K2 P7 136.70(7) . . ? C55 K2 P7 103.20(7) . . ? C70 K2 P5 126.39(7) . . ? C71 K2 P5 148.13(8) . . ? C69 K2 P5 104.57(7) . . ? C72 K2 P5 139.50(7) . . ? C68 K2 P5 99.69(7) . . ? C60 K2 P5 49.36(8) . . ? P1 K2 P5 96.02(3) . . ? C67 K2 P5 114.42(7) . . ? C55 K2 P5 31.68(7) . . ? P7 K2 P5 107.23(3) . . ? C70 K2 K1 136.86(7) . . ? C71 K2 K1 122.33(7) . . ? C69 K2 K1 161.49(7) . . ? C72 K2 K1 123.75(7) . . ? C68 K2 K1 164.77(7) . . ? C60 K2 K1 101.00(7) . . ? P1 K2 K1 50.14(2) . . ? C67 K2 K1 139.89(7) . . ? C55 K2 K1 110.27(7) . . ? P7 K2 K1 48.38(2) . . ? P5 K2 K1 89.26(3) . . ? C12 K3 C51 81.19(14) . . ? C12 K3 C46 83.67(14) . . ? C51 K3 C46 70.12(14) . . ? C12 K3 C52 104.85(15) . . ? C51 K3 C52 24.07(14) . . ? C46 K3 C52 77.54(16) . . ? C12 K3 C45 77.09(13) . . ? C51 K3 C45 92.61(15) . . ? C46 K3 C45 24.50(13) . . ? C52 K3 C45 102.04(15) . . ? C12 K3 C47 107.10(14) . . ? C51 K3 C47 68.78(14) . . ? C46 K3 C47 24.24(13) . . ? C52 K3 C47 65.99(14) . . ? C45 K3 C47 42.36(14) . . ? C12 K3 P6 135.46(9) . . ? C51 K3 P6 121.44(12) . . ? C46 K3 P6 138.08(11) . . ? C52 K3 P6 100.19(13) . . ? C45 K3 P6 132.31(11) . . ? C47 K3 P6 116.65(11) . . ? C12 K3 P1 50.11(8) . . ? C51 K3 P1 124.58(12) . . ? C46 K3 P1 119.62(13) . . ? C52 K3 P1 141.79(11) . . ? C45 K3 P1 99.15(11) . . ? C47 K3 P1 141.52(10) . . ? P6 K3 P1 88.21(3) . . ? C12 K3 C7 24.88(9) . . ? C51 K3 C7 105.99(14) . . ? C46 K3 C7 90.24(14) . . ? C52 K3 C7 129.73(15) . . ? C45 K3 C7 74.30(12) . . ? C47 K3 C7 114.16(13) . . ? P6 K3 C7 119.43(7) . . ? P1 K3 C7 31.64(7) . . ? C12 K3 C44 93.72(11) . . ? C51 K3 C44 112.14(13) . . ? C46 K3 C44 42.20(13) . . ? C52 K3 C44 114.29(13) . . ? C45 K3 C44 23.77(12) . . ? C47 K3 C44 48.31(12) . . ? P6 K3 C44 108.71(9) . . ? P1 K3 C44 97.56(8) . . ? C7 K3 C44 82.58(10) . . ? C12 K3 C53 112.29(12) . . ? C51 K3 C53 41.62(14) . . ? C46 K3 C53 100.71(16) . . ? C52 K3 C53 23.65(13) . . ? C45 K3 C53 125.14(15) . . ? C47 K3 C53 85.99(13) . . ? P6 K3 C53 79.82(10) . . ? P1 K3 C53 129.19(9) . . ? C7 K3 C53 134.53(11) . . ? C44 K3 C53 133.11(12) . . ? C12 K3 C50 65.58(11) . . ? C51 K3 C50 23.64(12) . . ? C46 K3 C50 86.85(13) . . ? C52 K3 C50 41.62(14) . . ? C45 K3 C50 105.04(13) . . ? C47 K3 C50 90.96(13) . . ? P6 K3 C50 119.41(8) . . ? P1 K3 C50 102.10(9) . . ? C7 K3 C50 89.83(11) . . ? C44 K3 C50 128.05(12) . . ? C53 K3 C50 47.64(12) . . ? C77 K4 C78 25.62(9) 2_545 2_545 ? C77 K4 C76 25.61(10) 2_545 2_545 ? C78 K4 C76 45.02(10) 2_545 2_545 ? C77 K4 P2 106.58(8) 2_545 . ? C78 K4 P2 90.56(7) 2_545 . ? C76 K4 P2 132.17(8) 2_545 . ? C77 K4 C73 45.49(10) 2_545 2_545 ? C78 K4 C73 25.57(9) 2_545 2_545 ? C76 K4 C73 53.03(10) 2_545 2_545 ? P2 K4 C73 96.17(7) . 2_545 ? C77 K4 P3 148.45(8) 2_545 . ? C78 K4 P3 130.15(8) 2_545 . ? C76 K4 P3 133.06(9) 2_545 . ? P2 K4 P3 85.98(3) . . ? C73 K4 P3 105.54(7) 2_545 . ? C77 K4 C75 43.89(11) 2_545 2_545 ? C78 K4 C75 51.01(10) 2_545 2_545 ? C76 K4 C75 24.83(10) 2_545 2_545 ? P2 K4 C75 139.87(8) . 2_545 ? C73 K4 C75 44.45(10) 2_545 2_545 ? P3 K4 C75 108.94(9) . 2_545 ? C77 K4 C74 51.42(11) 2_545 2_545 ? C78 K4 C74 43.85(10) 2_545 2_545 ? C76 K4 C74 44.16(11) 2_545 2_545 ? P2 K4 C74 119.86(8) . 2_545 ? C73 K4 C74 25.26(9) 2_545 2_545 ? P3 K4 C74 97.12(8) . 2_545 ? C75 K4 C74 24.62(10) 2_545 2_545 ? C77 K4 P6 110.04(8) 2_545 . ? C78 K4 P6 134.51(7) 2_545 . ? C76 K4 P6 100.00(8) 2_545 . ? P2 K4 P6 103.44(3) . . ? C73 K4 P6 153.00(7) 2_545 . ? P3 K4 P6 94.30(4) . . ? C75 K4 P6 111.95(8) 2_545 . ? C74 K4 P6 135.76(8) 2_545 . ? C77 K4 C67 80.31(9) 2_545 . ? C78 K4 C67 103.28(9) 2_545 . ? C76 K4 C67 77.75(10) 2_545 . ? P2 K4 C67 102.44(7) . . ? C73 K4 C67 125.75(9) 2_545 . ? P3 K4 C67 126.04(7) . . ? C75 K4 C67 98.09(11) 2_545 . ? C74 K4 C67 121.50(10) 2_545 . ? P6 K4 C67 31.74(6) . . ? C77 K4 C72 76.37(10) 2_545 . ? C78 K4 C72 92.98(10) 2_545 . ? C76 K4 C72 84.59(11) 2_545 . ? P2 K4 C72 80.63(7) . . ? C73 K4 C72 118.49(10) 2_545 . ? P3 K4 C72 134.97(7) . . ? C75 K4 C72 108.86(11) 2_545 . ? C74 K4 C72 126.79(10) 2_545 . ? P6 K4 C72 48.73(7) . . ? C67 K4 C72 24.31(8) . . ? C77 K4 K5 145.96(8) 2_545 . ? C78 K4 K5 147.69(7) 2_545 . ? C76 K4 K5 150.87(9) 2_545 . ? P2 K4 K5 60.00(3) . . ? C73 K4 K5 154.01(7) 2_545 . ? P3 K4 K5 65.36(3) . . ? C75 K4 K5 160.11(7) 2_545 . ? C74 K4 K5 162.40(8) 2_545 . ? P6 K4 K5 52.02(2) . . ? C67 K4 K5 73.41(6) . . ? C72 K4 K5 70.73(7) . . ? C4 K5 C3 24.86(12) . . ? C4 K5 P6 129.94(9) . . ? C3 K5 P6 111.17(9) . . ? C4 K5 C5 24.89(11) . . ? C3 K5 C5 42.78(12) . . ? P6 K5 C5 119.44(8) . . ? C4 K5 C20 80.31(11) . . ? C3 K5 C20 84.06(11) . . ? P6 K5 C20 135.63(9) . . ? C5 K5 C20 100.28(11) . . ? C4 K5 P4 106.65(10) . . ? C3 K5 P4 127.04(10) . . ? P6 K5 P4 87.95(4) . . ? C5 K5 P4 84.49(9) . . ? C20 K5 P4 116.52(8) . . ? C4 K5 C2 42.13(11) . . ? C3 K5 C2 23.43(10) . . ? P6 K5 C2 89.07(8) . . ? C5 K5 C2 47.87(11) . . ? C20 K5 C2 105.66(10) . . ? P4 K5 C2 121.21(7) . . ? C4 K5 P2 92.46(10) . . ? C3 K5 P2 77.32(9) . . ? P6 K5 P2 95.00(3) . . ? C5 K5 P2 117.11(9) . . ? C20 K5 P2 46.23(8) . . ? P4 K5 P2 152.33(4) . . ? C2 K5 P2 86.39(7) . . ? C4 K5 K4 137.61(10) . . ? C3 K5 K4 115.02(10) . . ? P6 K5 K4 53.07(3) . . ? C5 K5 K4 156.12(8) . . ? C20 K5 K4 82.58(9) . . ? P4 K5 K4 115.69(4) . . ? C2 K5 K4 108.38(8) . . ? P2 K5 K4 49.26(2) . . ? C4 K5 K3 98.60(8) . . ? C3 K5 K3 94.55(8) . . ? P6 K5 K3 44.58(2) . . ? C5 K5 K3 78.92(8) . . ? C20 K5 K3 178.55(8) . . ? P4 K5 K3 64.67(3) . . ? C2 K5 K3 72.90(7) . . ? P2 K5 K3 133.06(3) . . ? K4 K5 K3 97.66(2) . . ? C4 K5 K7 151.55(10) . . ? C3 K5 K7 172.28(9) . . ? P6 K5 K7 66.89(3) . . ? C5 K5 K7 130.88(9) . . ? C20 K5 K7 102.55(8) . . ? P4 K5 K7 46.40(3) . . ? C2 K5 K7 151.34(7) . . ? P2 K5 K7 110.10(3) . . ? K4 K5 K7 70.26(2) . . ? K3 K5 K7 78.87(2) . . ? C50 K6 C79 125.71(12) 1_455 2_545 ? C50 K6 C49 26.09(10) 1_455 1_455 ? C79 K6 C49 106.44(10) 2_545 1_455 ? C50 K6 C80 128.17(13) 1_455 2_545 ? C79 K6 C80 25.37(10) 2_545 2_545 ? C49 K6 C80 119.37(11) 1_455 2_545 ? C50 K6 P2 108.42(10) 1_455 . ? C79 K6 P2 121.02(8) 2_545 . ? C49 K6 P2 114.28(8) 1_455 . ? C80 K6 P2 123.03(9) 2_545 . ? C50 K6 P7 137.47(9) 1_455 2_545 ? C79 K6 P7 31.66(7) 2_545 2_545 ? C49 K6 P7 111.54(8) 1_455 2_545 ? C80 K6 P7 51.48(8) 2_545 2_545 ? P2 K6 P7 92.41(3) . 2_545 ? C50 K6 P5 46.43(9) 1_455 1_455 ? C79 K6 P5 109.95(8) 2_545 1_455 ? C49 K6 P5 28.94(8) 1_455 1_455 ? C80 K6 P5 132.35(8) 2_545 1_455 ? P2 K6 P5 89.82(3) . 1_455 ? P7 K6 P5 99.00(3) 2_545 1_455 ? C50 K6 P3 118.32(9) 1_455 . ? C79 K6 P3 94.77(8) 2_545 . ? C49 K6 P3 143.56(8) 1_455 . ? C80 K6 P3 71.87(8) 2_545 . ? P2 K6 P3 76.68(3) . . ? P7 K6 P3 102.13(3) 2_545 . ? P5 K6 P3 155.28(4) 1_455 . ? C50 K6 K4 150.69(9) 1_455 . ? C79 K6 K4 83.38(7) 2_545 . ? C49 K6 K4 161.63(8) 1_455 . ? C80 K6 K4 75.96(8) 2_545 . ? P2 K6 K4 48.19(2) . . ? P7 K6 K4 68.78(2) 2_545 . ? P5 K6 K4 133.33(3) 1_455 . ? P3 K6 K4 47.16(2) . . ? C50 K6 K1 105.41(9) 1_455 2_545 ? C79 K6 K1 74.22(7) 2_545 2_545 ? C49 K6 K1 83.49(7) 1_455 2_545 ? C80 K6 K1 97.69(8) 2_545 2_545 ? P2 K6 K1 70.24(3) . 2_545 ? P7 K6 K1 46.86(2) 2_545 2_545 ? P5 K6 K1 59.03(2) 1_455 2_545 ? P3 K6 K1 131.51(3) . 2_545 ? K4 K6 K1 84.40(2) . 2_545 ? C25 K7 C66 109.41(12) . . ? C25 K7 C65 110.80(17) . . ? C66 K7 C65 24.90(14) . . ? C25 K7 P3 33.32(8) . . ? C66 K7 P3 104.56(9) . . ? C65 K7 P3 120.14(11) . . ? C25 K7 P4 117.93(9) . 3 ? C66 K7 P4 119.07(9) . 3 ? C65 K7 P4 99.65(10) . 3 ? P3 K7 P4 136.03(5) . 3 ? C25 K7 C26 24.54(11) . . ? C66 K7 C26 87.95(13) . . ? C65 K7 C26 86.31(17) . . ? P3 K7 C26 49.07(8) . . ? P4 K7 C26 123.48(9) 3 . ? C25 K7 C42 88.32(11) . 3 ? C66 K7 C42 97.97(13) . 3 ? C65 K7 C42 73.25(16) . 3 ? P3 K7 C42 121.50(9) . 3 ? P4 K7 C42 50.39(8) 3 3 ? C26 K7 C42 79.32(11) . 3 ? C25 K7 P4 126.21(9) . . ? C66 K7 P4 79.29(11) . . ? C65 K7 P4 97.82(16) . . ? P3 K7 P4 92.95(4) . . ? P4 K7 P4 99.82(4) 3 . ? C26 K7 P4 135.28(9) . . ? C42 K7 P4 144.55(9) 3 . ? C25 K7 K7 145.57(10) . 3 ? C66 K7 K7 102.50(10) . 3 ? C65 K7 K7 103.58(15) . 3 ? P3 K7 K7 125.60(5) . 3 ? P4 K7 K7 52.04(3) 3 3 ? C26 K7 K7 169.50(10) . 3 ? C42 K7 K7 99.94(8) 3 3 ? P4 K7 K7 47.79(3) . 3 ? C25 K7 K5 86.02(8) . . ? C66 K7 K5 72.23(9) . . ? C65 K7 K5 97.09(12) . . ? P3 K7 K5 54.50(3) . . ? P4 K7 K5 142.79(4) 3 . ? C26 K7 K5 90.47(8) . . ? C42 K7 K5 166.23(9) 3 . ? P4 K7 K5 44.82(2) . . ? K7 K7 K5 91.78(3) 3 . ? C1 P1 C7 105.23(17) . . ? C1 P1 K2 125.44(13) . . ? C7 P1 K2 126.75(13) . . ? C1 P1 K3 96.34(12) . . ? C7 P1 K3 74.25(12) . . ? K2 P1 K3 84.20(3) . . ? C1 P1 K1 120.26(12) . . ? C7 P1 K1 85.44(12) . . ? K2 P1 K1 82.75(3) . . ? K3 P1 K1 141.91(4) . . ? C13 P2 C19 108.04(17) . . ? C13 P2 K4 117.53(12) . . ? C19 P2 K4 134.43(12) . . ? C13 P2 K6 105.54(11) . . ? C19 P2 K6 86.70(12) . . ? K4 P2 K6 81.27(3) . . ? C13 P2 K5 144.57(12) . . ? C19 P2 K5 72.56(11) . . ? K4 P2 K5 70.74(3) . . ? K6 P2 K5 109.84(4) . . ? C31 P3 C25 104.08(19) . . ? C31 P3 K4 153.51(13) . . ? C25 P3 K4 99.43(14) . . ? C31 P3 K7 95.38(13) . . ? C25 P3 K7 68.32(14) . . ? K4 P3 K7 104.59(4) . . ? C31 P3 K6 85.11(13) . . ? C25 P3 K6 111.79(14) . . ? K4 P3 K6 74.87(3) . . ? K7 P3 K6 179.46(4) . . ? C43 P4 C37 102.2(2) . . ? C43 P4 K7 84.06(13) . 3 ? C37 P4 K7 82.75(14) . 3 ? C43 P4 K5 112.98(13) . . ? C37 P4 K5 96.25(14) . . ? K7 P4 K5 162.62(5) 3 . ? C43 P4 K7 116.02(15) . . ? C37 P4 K7 135.82(15) . . ? K7 P4 K7 80.18(4) 3 . ? K5 P4 K7 88.79(4) . . ? C49 P5 C55 106.29(18) . . ? C49 P5 K2 96.27(12) . . ? C55 P5 K2 72.84(11) . . ? C49 P5 K6 59.42(11) . 1_655 ? C55 P5 K6 97.75(12) . 1_655 ? K2 P5 K6 151.11(4) . 1_655 ? C61 P6 C67 106.74(17) . . ? C61 P6 K5 126.79(13) . . ? C67 P6 K5 117.83(12) . . ? C61 P6 K4 91.08(13) . . ? C67 P6 K4 74.96(11) . . ? K5 P6 K4 74.90(3) . . ? C61 P6 K3 96.75(13) . . ? C67 P6 K3 112.48(11) . . ? K5 P6 K3 91.95(4) . . ? K4 P6 K3 166.85(4) . . ? C79 P7 C73 108.57(18) . . ? C79 P7 K1 133.93(13) . . ? C73 P7 K1 112.19(12) . . ? C79 P7 K2 120.51(12) . . ? C73 P7 K2 86.45(11) . . ? K1 P7 K2 82.95(3) . . ? C79 P7 K6 65.87(12) . 2 ? C73 P7 K6 103.74(11) . 2 ? K1 P7 K6 84.18(3) . 2 ? K2 P7 K6 165.92(4) . 2 ? C2 C1 C6 115.6(3) . . ? C2 C1 P1 117.5(3) . . ? C6 C1 P1 126.7(3) . . ? C3 C2 C1 121.7(4) . . ? C3 C2 K5 66.6(2) . . ? C1 C2 K5 87.8(2) . . ? C4 C3 C2 121.6(4) . . ? C4 C3 K5 74.5(3) . . ? C2 C3 K5 89.9(3) . . ? C3 C4 C5 118.3(4) . . ? C3 C4 K5 80.7(3) . . ? C5 C4 K5 83.2(3) . . ? C4 C5 C6 120.7(4) . . ? C4 C5 K5 71.9(3) . . ? C6 C5 K5 89.7(2) . . ? C5 C6 C1 122.0(4) . . ? C8 C7 C12 115.7(4) . . ? C8 C7 P1 126.8(3) . . ? C12 C7 P1 117.3(3) . . ? C8 C7 K3 126.4(3) . . ? C12 C7 K3 72.1(2) . . ? P1 C7 K3 74.12(12) . . ? C9 C8 C7 121.9(4) . . ? C10 C9 C8 120.2(5) . . ? C11 C10 C9 119.5(5) . . ? C10 C11 C12 121.1(4) . . ? C11 C12 C7 121.4(4) . . ? C11 C12 K3 120.3(3) . . ? C7 C12 K3 83.0(2) . . ? C14 C13 C18 115.6(3) . . ? C14 C13 P2 117.1(3) . . ? C18 C13 P2 127.1(3) . . ? C14 C13 K1 73.4(2) . 2_545 ? C18 C13 K1 72.3(2) . 2_545 ? P2 C13 K1 118.55(14) . 2_545 ? C15 C14 C13 122.4(4) . . ? C15 C14 K1 69.9(2) . 2_545 ? C13 C14 K1 82.9(2) . 2_545 ? C14 C15 C16 120.5(4) . . ? C14 C15 K1 85.9(2) . 2_545 ? C16 C15 K1 74.2(2) . 2_545 ? C17 C16 C15 118.5(4) . . ? C17 C16 K1 80.6(2) . 2_545 ? C15 C16 K1 80.1(2) . 2_545 ? C18 C17 C16 121.2(4) . . ? C18 C17 K1 84.3(2) . 2_545 ? C16 C17 K1 73.9(2) . 2_545 ? C17 C18 C13 121.7(3) . . ? C17 C18 K1 71.3(2) . 2_545 ? C13 C18 K1 83.9(2) . 2_545 ? C24 C19 C20 115.9(4) . . ? C24 C19 P2 126.7(3) . . ? C20 C19 P2 117.1(3) . . ? C21 C20 C19 121.6(4) . . ? C21 C20 K5 107.8(3) . . ? C19 C20 K5 88.5(2) . . ? C22 C21 C20 121.3(4) . . ? C21 C22 C23 118.3(4) . . ? C24 C23 C22 121.2(4) . . ? C23 C24 C19 121.6(4) . . ? C30 C25 C26 115.4(4) . . ? C30 C25 P3 127.8(4) . . ? C26 C25 P3 116.8(3) . . ? C30 C25 K7 100.6(3) . . ? C26 C25 K7 90.1(3) . . ? P3 C25 K7 78.36(15) . . ? C27 C26 C25 122.8(5) . . ? C27 C26 K7 115.5(3) . . ? C25 C26 K7 65.4(3) . . ? C28 C27 C26 120.0(5) . . ? C29 C28 C27 118.9(5) . . ? C28 C29 C30 120.8(5) . . ? C25 C30 C29 121.9(5) . . ? C32 C31 C36 115.3(4) . . ? C32 C31 P3 120.3(3) . . ? C36 C31 P3 124.1(3) . . ? C33 C32 C31 123.1(5) . . ? C34 C33 C32 120.1(5) . . ? C33 C34 C35 121.3(5) . . ? C34 C35 C36 119.7(5) . . ? C31 C36 C35 120.5(5) . . ? C38 C37 C42 114.5(5) . . ? C38 C37 P4 120.8(4) . . ? C42 C37 P4 124.6(4) . . ? C39 C38 C37 124.0(5) . . ? C38 C39 C40 119.9(6) . . ? C39 C40 C41 119.0(6) . . ? C42 C41 C40 120.7(5) . . ? C41 C42 C37 121.9(5) . . ? C41 C42 K7 127.6(3) . 3 ? C37 C42 K7 82.4(3) . 3 ? C48 C43 C44 115.7(4) . . ? C48 C43 P4 119.9(3) . . ? C44 C43 P4 124.3(4) . . ? C48 C43 K3 76.6(3) . . ? C44 C43 K3 75.7(3) . . ? P4 C43 K3 113.43(16) . . ? C45 C44 C43 122.7(5) . . ? C45 C44 K3 75.2(3) . . ? C43 C44 K3 80.6(3) . . ? C44 C45 C46 119.5(5) . . ? C44 C45 K3 81.1(3) . . ? C46 C45 K3 76.4(3) . . ? C47 C46 C45 118.7(5) . . ? C47 C46 K3 79.4(3) . . ? C45 C46 K3 79.1(3) . . ? C48 C47 C46 121.2(5) . . ? C48 C47 K3 82.1(3) . . ? C46 C47 K3 76.3(3) . . ? C47 C48 C43 122.3(5) . . ? C47 C48 K3 74.6(3) . . ? C43 C48 K3 79.7(2) . . ? C54 C49 C50 114.6(4) . . ? C54 C49 P5 128.9(3) . . ? C50 C49 P5 116.4(3) . . ? C54 C49 K6 104.0(2) . 1_655 ? C50 C49 K6 74.2(2) . 1_655 ? P5 C49 K6 91.64(14) . 1_655 ? C51 C50 C49 122.4(5) . . ? C51 C50 K6 102.4(3) . 1_655 ? C49 C50 K6 79.7(2) . 1_655 ? C51 C50 K3 72.7(3) . . ? C49 C50 K3 84.1(2) . . ? K6 C50 K3 156.99(17) 1_655 . ? C52 C51 C50 120.5(5) . . ? C52 C51 K3 78.7(3) . . ? C50 C51 K3 83.6(3) . . ? C51 C52 C53 119.7(5) . . ? C51 C52 K3 77.2(3) . . ? C53 C52 K3 82.4(3) . . ? C52 C53 C54 120.1(5) . . ? C52 C53 K3 74.0(3) . . ? C54 C53 K3 82.5(3) . . ? C53 C54 C49 122.7(4) . . ? C53 C54 K3 74.4(3) . . ? C49 C54 K3 80.9(2) . . ? C56 C55 C60 115.1(3) . . ? C56 C55 P5 127.7(3) . . ? C60 C55 P5 116.7(3) . . ? C56 C55 K1 74.9(2) . 2_645 ? C60 C55 K1 80.6(2) . 2_645 ? P5 C55 K1 107.33(14) . 2_645 ? C56 C55 K2 124.6(2) . . ? C60 C55 K2 75.5(2) . . ? P5 C55 K2 75.48(12) . . ? K1 C55 K2 154.14(13) 2_645 . ? C57 C56 C55 121.9(4) . . ? C57 C56 K1 80.0(2) . 2_645 ? C55 C56 K1 79.5(2) . 2_645 ? C56 C57 C58 121.7(3) . . ? C56 C57 K1 75.0(2) . 2_645 ? C58 C57 K1 82.4(2) . 2_645 ? C59 C58 C57 118.1(4) . . ? C59 C58 K1 78.8(2) . 2_645 ? C57 C58 K1 73.1(2) . 2_645 ? C58 C59 C60 120.5(4) . . ? C58 C59 K1 77.3(2) . 2_645 ? C60 C59 K1 75.7(2) . 2_645 ? C59 C60 C55 122.7(4) . . ? C59 C60 K2 123.4(3) . . ? C55 C60 K2 79.6(2) . . ? C59 C60 K1 80.2(2) . 2_645 ? C55 C60 K1 74.2(2) . 2_645 ? K2 C60 K1 151.98(14) . 2_645 ? C62 C61 C66 115.8(4) . . ? C62 C61 P6 127.2(3) . . ? C66 C61 P6 116.9(3) . . ? C63 C62 C61 122.0(5) . . ? C62 C63 C64 120.7(6) . . ? C65 C64 C63 118.2(6) . . ? C64 C65 C66 122.4(6) . . ? C64 C65 K7 113.7(5) . . ? C66 C65 K7 74.7(3) . . ? C65 C66 C61 120.9(5) . . ? C65 C66 K7 80.4(3) . . ? C61 C66 K7 109.4(3) . . ? C68 C67 C72 115.7(3) . . ? C68 C67 P6 127.3(3) . . ? C72 C67 P6 116.8(3) . . ? C68 C67 K2 76.0(2) . . ? C72 C67 K2 75.79(19) . . ? P6 C67 K2 112.63(14) . . ? C68 C67 K4 121.2(2) . . ? C72 C67 K4 79.7(2) . . ? P6 C67 K4 73.29(11) . . ? K2 C67 K4 154.71(12) . . ? C69 C68 C67 122.1(3) . . ? C69 C68 K2 76.0(2) . . ? C67 C68 K2 79.1(2) . . ? C68 C69 C70 120.9(4) . . ? C68 C69 K2 79.3(2) . . ? C70 C69 K2 77.0(2) . . ? C69 C70 C71 118.5(4) . . ? C69 C70 K2 77.9(2) . . ? C71 C70 K2 77.7(2) . . ? C72 C71 C70 120.9(3) . . ? C72 C71 K2 79.4(2) . . ? C70 C71 K2 77.2(2) . . ? C71 C72 C67 121.9(3) . . ? C71 C72 K2 75.9(2) . . ? C67 C72 K2 79.1(2) . . ? C71 C72 K4 123.2(2) . . ? C67 C72 K4 75.98(19) . . ? K2 C72 K4 154.34(12) . . ? C78 C73 C74 115.5(3) . . ? C78 C73 P7 115.9(3) . . ? C74 C73 P7 128.5(3) . . ? C78 C73 K4 72.75(19) . 2 ? C74 C73 K4 79.8(2) . 2 ? P7 C73 K4 118.43(15) . 2 ? C75 C74 C73 120.6(4) . . ? C75 C74 K4 76.2(2) . 2 ? C73 C74 K4 74.9(2) . 2 ? C76 C75 C74 121.7(4) . . ? C76 C75 K4 73.3(2) . 2 ? C74 C75 K4 79.2(2) . 2 ? C75 C76 C77 118.5(4) . . ? C75 C76 K4 81.9(2) . 2 ? C77 C76 K4 74.8(2) . 2 ? C78 C77 C76 120.7(4) . . ? C78 C77 K4 78.3(2) . 2 ? C76 C77 K4 79.6(2) . 2 ? C77 C78 C73 122.9(4) . . ? C77 C78 K4 76.0(2) . 2 ? C73 C78 K4 81.7(2) . 2 ? C80 C79 C84 115.3(4) . . ? C80 C79 P7 127.7(3) . . ? C84 C79 P7 116.6(3) . . ? C80 C79 K6 79.5(2) . 2 ? C84 C79 K6 103.7(2) . 2 ? P7 C79 K6 82.47(13) . 2 ? C81 C80 C79 122.1(4) . . ? C81 C80 K6 107.1(3) . 2 ? C79 C80 K6 75.1(2) . 2 ? C82 C81 C80 120.6(4) . . ? C81 C82 C83 119.6(4) . . ? C82 C83 C84 120.0(4) . . ? C83 C84 C79 122.5(4) . . ? C87 C85 C86 88.1(13) 3_665 . ? C87 C86 C85 145.5(15) . . ? C86 C87 C85 126.4(16) . 3_665 ? data_sep1198 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Na{C(SiMe3)2(SiMe2PPh2)}]' _chemical_formula_analytical ? _chemical_formula_sum 'C21 H34 Na P Si3' _chemical_formula_weight 424.71 _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' 'Na' 'Na' 0.0362 0.0249 '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 orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 10.770(2) _cell_length_b 13.683(2) _cell_length_c 16.542(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2437.7(8) _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 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.157 _exptl_crystal_density_method ? _exptl_crystal_F_000 912 _exptl_absorpt_coefficient_mu 0.282 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.95 _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 4699 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0954 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.26 _diffrn_reflns_theta_max 24.97 _reflns_number_total 4284 _reflns_number_observed 3347 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; The positions of the H atoms were refined. Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(17) _refine_ls_number_reflns 4284 _refine_ls_number_parameters 337 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_obs 0.0494 _refine_ls_wR_factor_all 0.1086 _refine_ls_wR_factor_obs 0.0957 _refine_ls_goodness_of_fit_all 0.992 _refine_ls_goodness_of_fit_obs 0.999 _refine_ls_restrained_S_all 0.992 _refine_ls_restrained_S_obs 0.999 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Na Na 0.4861(2) 0.49527(14) 0.82396(12) 0.0356(5) Uani 1 d . . M1 C 0.6282 0.6017 0.7293 0.000 Uiso 0.00 d P . P P 0.41789(10) 0.77001(8) 0.72995(7) 0.0200(3) Uani 1 d . . Si1 Si 0.19962(11) 0.48957(9) 0.87170(7) 0.0228(3) Uani 1 d . . Si2 Si 0.35471(12) 0.65460(9) 0.95316(7) 0.0246(3) Uani 1 d . . Si3 Si 0.25096(11) 0.67594(8) 0.77734(7) 0.0205(3) Uani 1 d . . C1 C 0.2961(4) 0.5983(3) 0.8606(2) 0.0201(9) Uani 1 d . . C2 C 0.2303(6) 0.3932(4) 0.7944(4) 0.0421(14) Uani 1 d . . H2A H 0.1789(53) 0.3397(41) 0.7965(32) 0.063 Uiso 1 d . . H2B H 0.3094(57) 0.3782(42) 0.7942(34) 0.063 Uiso 1 d . . H2C H 0.2118(56) 0.4139(40) 0.7434(34) 0.063 Uiso 1 d . . C3 C 0.0285(5) 0.5109(5) 0.8679(4) 0.0424(13) Uani 1 d . . H3A H -0.0154(55) 0.4531(44) 0.8780(34) 0.064 Uiso 1 d . . H3B H -0.0043(53) 0.5356(42) 0.8168(34) 0.064 Uiso 1 d . . H3C H 0.0024(54) 0.5616(42) 0.9052(34) 0.064 Uiso 1 d . . C4 C 0.2255(6) 0.4242(4) 0.9695(4) 0.045(2) Uani 1 d . . H4A H 0.1911(56) 0.3643(44) 0.9673(34) 0.068 Uiso 1 d . . H4B H 0.1832(61) 0.4477(46) 1.0118(36) 0.068 Uiso 1 d . . H4C H 0.3058(60) 0.4308(44) 0.9902(35) 0.068 Uiso 1 d . . C5 C 0.3940(6) 0.7883(4) 0.9439(3) 0.0389(14) Uani 1 d . . H5A H 0.4363(50) 0.8076(40) 0.9920(33) 0.058 Uiso 1 d . . H5B H 0.3199(53) 0.8218(42) 0.9380(31) 0.058 Uiso 1 d . . H5C H 0.4496(53) 0.8010(43) 0.9086(32) 0.058 Uiso 1 d . . C6 C 0.5018(6) 0.5946(5) 0.9894(4) 0.0428(15) Uani 1 d . . H6A H 0.5237(54) 0.6156(44) 1.0390(35) 0.064 Uiso 1 d . . H6B H 0.5662(56) 0.6064(46) 0.9563(36) 0.064 Uiso 1 d . . H6C H 0.4878(54) 0.5285(46) 1.0034(34) 0.064 Uiso 1 d . . C7 C 0.2471(7) 0.6559(5) 1.0420(3) 0.048(2) Uani 1 d . . H7A H 0.2837(54) 0.6896(43) 1.0841(35) 0.073 Uiso 1 d . . H7B H 0.2303(60) 0.5970(45) 1.0601(35) 0.073 Uiso 1 d . . H7C H 0.1632(62) 0.6836(44) 1.0326(35) 0.073 Uiso 1 d . . C8 C 0.1279(5) 0.7696(4) 0.8000(3) 0.0352(13) Uani 1 d . . H8A H 0.1028(44) 0.8100(41) 0.7545(30) 0.053 Uiso 1 d . . H8B H 0.1558(48) 0.8153(39) 0.8364(31) 0.053 Uiso 1 d . . H8C H 0.0634(47) 0.7399(40) 0.8188(32) 0.053 Uiso 1 d . . C9 C 0.1938(5) 0.6091(4) 0.6852(3) 0.0327(12) Uani 1 d . . H9A H 0.1795(48) 0.6491(37) 0.6447(32) 0.049 Uiso 1 d . . H9B H 0.1154(50) 0.5781(38) 0.6956(31) 0.049 Uiso 1 d . . H9C H 0.2599(48) 0.5565(36) 0.6687(30) 0.049 Uiso 1 d . . C10 C 0.5370(4) 0.6748(3) 0.7257(2) 0.0190(9) Uani 1 d . . C11 C 0.6305(4) 0.6780(3) 0.7830(3) 0.0274(10) Uani 1 d . . H11 H 0.6363(40) 0.7351(34) 0.8184(26) 0.033 Uiso 1 d . . C12 C 0.7210(4) 0.6057(4) 0.7869(3) 0.0342(12) Uani 1 d . . H12 H 0.7916(46) 0.6153(33) 0.8280(28) 0.041 Uiso 1 d . . C13 C 0.7188(5) 0.5300(4) 0.7330(3) 0.0384(14) Uani 1 d . . H13 H 0.7776(45) 0.4838(36) 0.7412(29) 0.046 Uiso 1 d . . C14 C 0.6265(5) 0.5249(3) 0.6756(3) 0.0338(12) Uani 1 d . . H14 H 0.6244(45) 0.4735(35) 0.6403(28) 0.041 Uiso 1 d . . C15 C 0.5355(5) 0.5967(4) 0.6722(3) 0.0271(11) Uani 1 d . . H15 H 0.4791(44) 0.5949(35) 0.6371(27) 0.032 Uiso 1 d . . C16 C 0.3873(4) 0.7956(3) 0.6227(2) 0.0217(10) Uani 1 d . . C17 C 0.4768(5) 0.7834(4) 0.5629(3) 0.0289(11) Uani 1 d . . H17 H 0.5498(44) 0.7571(34) 0.5768(27) 0.035 Uiso 1 d . . C18 C 0.4533(5) 0.8111(4) 0.4839(3) 0.0341(12) Uani 1 d . . H18 H 0.5153(45) 0.7931(38) 0.4486(27) 0.041 Uiso 1 d . . C19 C 0.3428(5) 0.8531(4) 0.4625(3) 0.0345(12) Uani 1 d . . H19 H 0.3234(46) 0.8720(36) 0.4155(30) 0.041 Uiso 1 d . . C20 C 0.2538(5) 0.8683(3) 0.5213(3) 0.0331(12) Uani 1 d . . H20 H 0.1803(47) 0.8967(36) 0.5111(28) 0.040 Uiso 1 d . . C21 C 0.2763(4) 0.8407(4) 0.6003(3) 0.0296(11) Uani 1 d . . H21 H 0.2114(42) 0.8432(34) 0.6383(26) 0.036 Uiso 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 Na 0.0283(10) 0.0307(11) 0.0478(11) 0.0090(10) 0.0099(9) 0.0046(9) P 0.0222(6) 0.0190(6) 0.0189(5) -0.0007(5) 0.0002(5) 0.0029(5) Si1 0.0199(6) 0.0250(7) 0.0235(6) -0.0006(6) 0.0025(5) -0.0015(6) Si2 0.0306(7) 0.0258(7) 0.0173(6) -0.0011(5) -0.0016(5) 0.0023(6) Si3 0.0199(6) 0.0245(6) 0.0170(5) 0.0004(5) -0.0008(5) 0.0012(5) C1 0.017(2) 0.023(2) 0.020(2) 0.003(2) -0.002(2) 0.003(2) C2 0.042(3) 0.029(3) 0.055(4) -0.009(3) 0.007(3) -0.007(3) C3 0.024(3) 0.044(4) 0.059(4) -0.004(3) 0.005(3) -0.002(3) C4 0.059(4) 0.039(3) 0.038(3) 0.009(3) -0.002(3) -0.017(3) C5 0.053(4) 0.034(3) 0.030(3) -0.006(3) -0.009(3) -0.004(3) C6 0.046(4) 0.042(3) 0.040(3) -0.001(3) -0.019(3) 0.008(3) C7 0.075(4) 0.048(4) 0.022(3) -0.007(3) 0.016(3) 0.001(4) C8 0.025(3) 0.038(3) 0.042(3) 0.011(3) 0.007(2) 0.012(2) C9 0.034(3) 0.043(3) 0.021(2) 0.008(2) -0.006(2) -0.011(3) C10 0.021(2) 0.017(2) 0.019(2) 0.003(2) 0.004(2) -0.002(2) C11 0.025(2) 0.028(3) 0.029(2) 0.001(2) -0.001(2) 0.000(2) C12 0.024(3) 0.040(3) 0.038(3) 0.010(3) 0.003(2) 0.007(2) C13 0.029(3) 0.032(3) 0.054(3) 0.020(3) 0.012(3) 0.013(2) C14 0.042(3) 0.019(3) 0.041(3) 0.000(2) 0.021(3) 0.006(2) C15 0.032(3) 0.026(3) 0.023(3) -0.001(2) 0.004(2) -0.005(2) C16 0.025(2) 0.016(2) 0.023(2) -0.001(2) -0.002(2) -0.001(2) C17 0.029(3) 0.028(3) 0.030(2) 0.006(2) 0.002(2) 0.001(2) C18 0.036(3) 0.040(3) 0.026(2) 0.005(2) 0.006(2) -0.005(3) C19 0.044(3) 0.036(3) 0.024(3) 0.008(2) -0.004(2) -0.004(3) C20 0.033(3) 0.029(3) 0.037(3) 0.007(2) -0.009(2) 0.007(3) C21 0.033(3) 0.032(3) 0.024(2) 0.000(2) 0.000(2) 0.006(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 Na C1 2.558(4) . ? Na M1 2.630(2) . ? Na C14 2.911(5) . ? Na C15 2.918(5) . ? Na C13 2.961(5) . ? Na C10 2.996(4) . ? Na C12 3.010(5) . ? Na C11 3.021(5) . ? Na C6 3.060(6) . ? Na C2 3.128(6) . ? Na P 3.371(2) 4_646 ? M1 C11 1.371(5) . ? M1 C14 1.376(5) . ? M1 C15 1.376(5) . ? M1 C12 1.382(5) . ? M1 C13 1.385(5) . ? M1 C10 1.403(4) . ? P C10 1.830(4) . ? P C16 1.839(4) . ? P Si3 2.346(2) . ? P Na 3.371(2) 4_656 ? Si1 C1 1.823(4) . ? Si1 C2 1.867(6) . ? Si1 C3 1.867(5) . ? Si1 C4 1.870(6) . ? Si2 C1 1.827(4) . ? Si2 C7 1.871(6) . ? Si2 C6 1.883(6) . ? Si2 C5 1.883(6) . ? Si3 C1 1.807(4) . ? Si3 C8 1.881(5) . ? Si3 C9 1.881(5) . ? C10 C11 1.384(6) . ? C10 C15 1.388(6) . ? C11 C12 1.390(6) . ? C12 C13 1.366(7) . ? C13 C14 1.377(7) . ? C14 C15 1.388(7) . ? C16 C17 1.390(6) . ? C16 C21 1.396(6) . ? C17 C18 1.385(6) . ? C18 C19 1.368(7) . ? C19 C20 1.381(8) . ? C20 C21 1.381(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Na M1 107.56(11) . . ? C1 Na C14 122.58(15) . . ? M1 Na C14 28.17(10) . . ? C1 Na C15 95.04(14) . . ? M1 Na C15 28.11(10) . . ? C14 Na C15 27.55(13) . . ? C1 Na C13 135.16(15) . . ? M1 Na C13 27.88(9) . . ? C14 Na C13 27.10(15) . . ? C15 Na C13 48.09(14) . . ? C1 Na C10 79.82(13) . . ? M1 Na C10 27.91(8) . . ? C14 Na C10 48.18(12) . . ? C15 Na C10 27.11(12) . . ? C13 Na C10 55.79(12) . . ? C1 Na C12 116.37(15) . . ? M1 Na C12 27.31(10) . . ? C14 Na C12 47.29(15) . . ? C15 Na C12 55.42(14) . . ? C13 Na C12 26.44(14) . . ? C10 Na C12 47.46(12) . . ? C1 Na C11 90.53(14) . . ? M1 Na C11 26.96(9) . . ? C14 Na C11 55.13(14) . . ? C15 Na C11 47.13(13) . . ? C13 Na C11 46.97(14) . . ? C10 Na C11 26.58(11) . . ? C12 Na C11 26.64(12) . . ? C1 Na C6 65.65(15) . . ? M1 Na C6 104.75(14) . . ? C14 Na C6 131.6(2) . . ? C15 Na C6 123.3(2) . . ? C13 Na C6 109.7(2) . . ? C10 Na C6 96.4(2) . . ? C12 Na C6 85.0(2) . . ? C11 Na C6 78.7(2) . . ? C1 Na C2 65.05(15) . . ? M1 Na C2 131.82(13) . . ? C14 Na C2 112.8(2) . . ? C15 Na C2 103.8(2) . . ? C13 Na C2 137.5(2) . . ? C10 Na C2 116.26(15) . . ? C12 Na C2 158.9(2) . . ? C11 Na C2 142.0(2) . . ? C6 Na C2 112.8(2) . . ? C1 Na P 144.27(12) . 4_646 ? M1 Na P 99.81(6) . 4_646 ? C14 Na P 75.24(10) . 4_646 ? C15 Na P 98.70(11) . 4_646 ? C13 Na P 75.70(11) . 4_646 ? C10 Na P 123.37(10) . 4_646 ? C12 Na P 98.48(11) . 4_646 ? C11 Na P 122.65(10) . 4_646 ? C6 Na P 128.72(13) . 4_646 ? C2 Na P 79.65(11) . 4_646 ? C11 M1 C14 179.7(3) . . ? C11 M1 C15 119.8(3) . . ? C14 M1 C15 60.6(3) . . ? C11 M1 C12 60.6(3) . . ? C14 M1 C12 119.0(3) . . ? C15 M1 C12 179.4(3) . . ? C11 M1 C13 119.8(3) . . ? C14 M1 C13 59.8(3) . . ? C15 M1 C13 120.4(3) . . ? C12 M1 C13 59.2(3) . . ? C11 M1 C10 59.8(2) . . ? C14 M1 C10 120.5(3) . . ? C15 M1 C10 59.9(3) . . ? C12 M1 C10 120.5(3) . . ? C13 M1 C10 179.6(3) . . ? C11 M1 Na 92.6(2) . . ? C14 M1 Na 87.4(2) . . ? C15 M1 Na 87.7(2) . . ? C12 M1 Na 91.9(2) . . ? C13 M1 Na 89.5(2) . . ? C10 M1 Na 90.7(2) . . ? C10 P C16 102.9(2) . . ? C10 P Si3 99.19(13) . . ? C16 P Si3 106.84(15) . . ? C10 P Na 115.19(13) . 4_656 ? C16 P Na 68.01(14) . 4_656 ? Si3 P Na 145.60(6) . 4_656 ? C1 Si1 C2 114.0(2) . . ? C1 Si1 C3 115.6(2) . . ? C2 Si1 C3 105.2(3) . . ? C1 Si1 C4 113.1(2) . . ? C2 Si1 C4 103.2(3) . . ? C3 Si1 C4 104.5(3) . . ? C1 Si2 C7 116.6(3) . . ? C1 Si2 C6 111.9(2) . . ? C7 Si2 C6 106.0(3) . . ? C1 Si2 C5 114.8(2) . . ? C7 Si2 C5 101.2(3) . . ? C6 Si2 C5 105.1(3) . . ? C1 Si3 C8 116.0(2) . . ? C1 Si3 C9 114.8(2) . . ? C8 Si3 C9 105.2(3) . . ? C1 Si3 P 111.81(15) . . ? C8 Si3 P 103.4(2) . . ? C9 Si3 P 104.3(2) . . ? Si3 C1 Si1 113.8(2) . . ? Si3 C1 Si2 118.9(2) . . ? Si1 C1 Si2 117.2(2) . . ? Si3 C1 Na 111.0(2) . . ? Si1 C1 Na 91.7(2) . . ? Si2 C1 Na 98.9(2) . . ? Si1 C2 Na 74.5(2) . . ? Si2 C6 Na 82.1(2) . . ? C11 C10 C15 118.0(4) . . ? C11 C10 M1 58.9(3) . . ? C15 C10 M1 59.1(3) . . ? C11 C10 P 117.5(3) . . ? C15 C10 P 124.4(3) . . ? M1 C10 P 175.4(3) . . ? C11 C10 Na 77.7(3) . . ? C15 C10 Na 73.3(2) . . ? M1 C10 Na 61.35(14) . . ? P C10 Na 115.8(2) . . ? M1 C11 C10 61.2(3) . . ? M1 C11 C12 60.1(3) . . ? C10 C11 C12 121.3(4) . . ? M1 C11 Na 60.4(2) . . ? C10 C11 Na 75.7(2) . . ? C12 C11 Na 76.2(3) . . ? C13 C12 M1 60.5(3) . . ? C13 C12 C11 119.8(5) . . ? M1 C12 C11 59.3(3) . . ? C13 C12 Na 74.8(3) . . ? M1 C12 Na 60.8(2) . . ? C11 C12 Na 77.1(3) . . ? C12 C13 C14 120.1(5) . . ? C12 C13 M1 60.3(3) . . ? C14 C13 M1 59.8(3) . . ? C12 C13 Na 78.8(3) . . ? C14 C13 Na 74.4(3) . . ? M1 C13 Na 62.6(2) . . ? M1 C14 C13 60.4(3) . . ? M1 C14 C15 59.7(3) . . ? C13 C14 C15 120.1(5) . . ? M1 C14 Na 64.5(2) . . ? C13 C14 Na 78.5(3) . . ? C15 C14 Na 76.5(3) . . ? M1 C15 C14 59.7(3) . . ? M1 C15 C10 61.0(3) . . ? C14 C15 C10 120.7(5) . . ? M1 C15 Na 64.2(2) . . ? C14 C15 Na 76.0(3) . . ? C10 C15 Na 79.6(3) . . ? C17 C16 C21 117.3(4) . . ? C17 C16 P 122.6(3) . . ? C21 C16 P 119.6(3) . . ? C18 C17 C16 120.8(5) . . ? C19 C18 C17 121.2(5) . . ? C18 C19 C20 119.0(5) . . ? C21 C20 C19 120.2(5) . . ? C20 C21 C16 121.5(4) . . ? _refine_diff_density_max 0.269 _refine_diff_density_min -0.225 _refine_diff_density_rms 0.057 data_aug1398 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Li{C(SiMe2CH2PPh2)3}].1.5(C6H6)' _chemical_formula_analytical ? _chemical_formula_sum 'C55 H63 Li P3 Si3' _chemical_formula_weight 908.17 _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' 'Li' 'Li' -0.0003 0.0001 '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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.967(3) _cell_length_b 13.981(2) _cell_length_c 16.707(5) _cell_angle_alpha 67.62(2) _cell_angle_beta 65.41(2) _cell_angle_gamma 60.030(10) _cell_volume 2507.2(10) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method ? _exptl_crystal_F_000 966 _exptl_absorpt_coefficient_mu 0.226 _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 6125 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1585 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.43 _diffrn_reflns_theta_max 21.97 _reflns_number_total 6125 _reflns_number_observed 3424 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'CAMERON (Watkin and Pearce,1993)' _computing_publication_material SHELXL-93 _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0131P)^2^+1.5824P] 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 6125 _refine_ls_number_parameters 530 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1475 _refine_ls_R_factor_obs 0.0706 _refine_ls_wR_factor_all 0.1450 _refine_ls_wR_factor_obs 0.1155 _refine_ls_goodness_of_fit_all 1.032 _refine_ls_goodness_of_fit_obs 1.137 _refine_ls_restrained_S_all 1.032 _refine_ls_restrained_S_obs 1.137 _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 Li Li 0.2564(10) 0.2707(10) 0.2224(8) 0.031(3) Uani 1 d . 1 P1 P 0.0799(2) 0.23157(15) 0.23987(13) 0.0242(5) Uani 1 d . 1 P2 P 0.45381(15) 0.09656(15) 0.23646(13) 0.0243(5) Uani 1 d . 1 P3 P 0.2178(2) 0.46783(15) 0.24168(13) 0.0245(5) Uani 1 d . 1 Si1 Si 0.2330(2) 0.2604(2) 0.04245(13) 0.0235(5) Uani 1 d . 1 Si2 Si 0.4630(2) 0.2389(2) 0.04096(13) 0.0233(5) Uani 1 d . 1 Si3 Si 0.2529(2) 0.4681(2) 0.04499(13) 0.0233(5) Uani 1 d . 1 C1 C 0.3060(5) 0.3141(5) 0.0725(4) 0.019(2) Uani 1 d . 1 C2 C 0.3033(6) 0.1037(5) 0.0463(5) 0.029(2) Uani 1 d . 1 H2C H 0.2573(6) 0.0842(5) 0.0291(5) 0.044 Uiso 1 calc R 1 H2B H 0.3082(6) 0.0614(5) 0.1076(5) 0.044 Uiso 1 calc R 1 H2A H 0.3810(6) 0.0843(5) 0.0042(5) 0.044 Uiso 1 calc R 1 C3 C 0.2155(6) 0.3262(6) -0.0748(5) 0.036(2) Uani 1 d . 1 H3C H 0.1758(6) 0.2929(6) -0.0855(5) 0.054 Uiso 1 calc R 1 H3B H 0.2915(6) 0.3120(6) -0.1190(5) 0.054 Uiso 1 calc R 1 H3A H 0.1701(6) 0.4080(6) -0.0808(5) 0.054 Uiso 1 calc R 1 C4 C 0.0826(5) 0.2867(5) 0.1219(4) 0.024(2) Uani 1 d . 1 H4B H 0.0350(5) 0.3692(5) 0.1121(4) 0.029 Uiso 1 calc R 1 H4A H 0.0476(5) 0.2512(5) 0.1072(4) 0.029 Uiso 1 calc R 1 C5 C 0.1162(6) 0.0810(5) 0.2583(5) 0.025(2) Uani 1 d . 1 C6 C 0.1992(6) 0.0021(6) 0.3015(5) 0.033(2) Uani 1 d . 1 H6 H 0.2341(6) 0.0264(6) 0.3237(5) 0.040 Uiso 1 calc R 1 C7 C 0.2323(6) -0.1127(6) 0.3127(5) 0.042(2) Uani 1 d . 1 H7 H 0.2911(6) -0.1667(6) 0.3412(5) 0.051 Uiso 1 calc R 1 C8 C 0.1805(7) -0.1478(6) 0.2829(5) 0.048(2) Uani 1 d . 1 H8 H 0.2018(7) -0.2264(6) 0.2921(5) 0.058 Uiso 1 calc R 1 C9 C 0.0974(7) -0.0697(6) 0.2396(5) 0.043(2) Uani 1 d . 1 H9 H 0.0622(7) -0.0945(6) 0.2180(5) 0.052 Uiso 1 calc R 1 C10 C 0.0653(6) 0.0441(6) 0.2275(5) 0.032(2) Uani 1 d . 1 H10 H 0.0077(6) 0.0977(6) 0.1978(5) 0.039 Uiso 1 calc R 1 C11 C -0.0738(5) 0.2817(5) 0.3010(4) 0.021(2) Uani 1 d . 1 C12 C -0.1136(6) 0.2175(6) 0.3825(5) 0.037(2) Uani 1 d . 1 H12 H -0.0609(6) 0.1457(6) 0.4057(5) 0.044 Uiso 1 calc R 1 C13 C -0.2294(7) 0.2560(7) 0.4311(5) 0.043(2) Uani 1 d . 1 H13 H -0.2550(7) 0.2110(7) 0.4874(5) 0.052 Uiso 1 calc R 1 C14 C -0.3061(6) 0.3582(7) 0.3979(5) 0.036(2) Uani 1 d . 1 H14 H -0.3853(6) 0.3843(7) 0.4308(5) 0.043 Uiso 1 calc R 1 C15 C -0.2690(6) 0.4223(6) 0.3179(6) 0.043(2) Uani 1 d . 1 H15 H -0.3225(6) 0.4936(6) 0.2948(6) 0.051 Uiso 1 calc R 1 C16 C -0.1542(6) 0.3851(6) 0.2695(5) 0.033(2) Uani 1 d . 1 H16 H -0.1298(6) 0.4313(6) 0.2136(5) 0.040 Uiso 1 calc R 1 C17 C 0.5333(6) 0.2131(6) -0.0764(4) 0.036(2) Uani 1 d . 1 H17C H 0.6169(6) 0.1725(6) -0.0863(4) 0.053 Uiso 1 calc R 1 H17B H 0.5161(6) 0.2857(6) -0.1202(4) 0.053 Uiso 1 calc R 1 H17A H 0.5037(6) 0.1676(6) -0.0841(4) 0.053 Uiso 1 calc R 1 C18 C 0.5456(5) 0.3081(6) 0.0470(5) 0.032(2) Uani 1 d . 1 H18C H 0.6284(5) 0.2612(6) 0.0289(5) 0.048 Uiso 1 calc R 1 H18B H 0.5227(5) 0.3159(6) 0.1089(5) 0.048 Uiso 1 calc R 1 H18A H 0.5287(5) 0.3831(6) 0.0063(5) 0.048 Uiso 1 calc R 1 C19 C 0.5077(5) 0.0926(5) 0.1180(4) 0.025(2) Uani 1 d . 1 H19B H 0.4787(5) 0.0471(5) 0.1085(4) 0.030 Uiso 1 calc R 1 H19A H 0.5928(5) 0.0544(5) 0.1013(4) 0.030 Uiso 1 calc R 1 C20 C 0.4923(5) -0.0524(6) 0.2969(5) 0.025(2) Uani 1 d . 1 C21 C 0.4813(7) -0.0792(7) 0.3873(5) 0.051(2) Uani 1 d . 1 H21 H 0.4561(7) -0.0203(7) 0.4160(5) 0.061 Uiso 1 calc R 1 C22 C 0.5053(8) -0.1883(7) 0.4381(6) 0.058(3) Uani 1 d . 1 H22 H 0.4979(8) -0.2038(7) 0.5004(6) 0.070 Uiso 1 calc R 1 C23 C 0.5396(6) -0.2735(7) 0.3991(5) 0.040(2) Uani 1 d . 1 H23 H 0.5547(6) -0.3488(7) 0.4337(5) 0.048 Uiso 1 calc R 1 C24 C 0.5518(7) -0.2495(6) 0.3100(6) 0.047(2) Uani 1 d . 1 H24 H 0.5774(7) -0.3089(6) 0.2818(6) 0.056 Uiso 1 calc R 1 C25 C 0.5274(6) -0.1385(6) 0.2585(5) 0.040(2) Uani 1 d . 1 H25 H 0.5354(6) -0.1235(6) 0.1961(5) 0.048 Uiso 1 calc R 1 C26 C 0.5569(6) 0.1273(5) 0.2520(4) 0.023(2) Uani 1 d . 1 C27 C 0.6755(6) 0.0703(6) 0.2175(5) 0.034(2) Uani 1 d . 1 H27 H 0.7047(6) 0.0089(6) 0.1903(5) 0.041 Uiso 1 calc R 1 C28 C 0.7514(6) 0.1039(7) 0.2230(5) 0.042(2) Uani 1 d . 1 H28 H 0.8320(6) 0.0657(7) 0.1985(5) 0.050 Uiso 1 calc R 1 C29 C 0.7110(7) 0.1905(6) 0.2632(5) 0.041(2) Uani 1 d . 1 H29 H 0.7630(7) 0.2124(6) 0.2670(5) 0.050 Uiso 1 calc R 1 C30 C 0.5933(7) 0.2464(6) 0.2983(5) 0.038(2) Uani 1 d . 1 H30 H 0.5645(7) 0.3069(6) 0.3264(5) 0.045 Uiso 1 calc R 1 C31 C 0.5175(6) 0.2144(6) 0.2928(4) 0.027(2) Uani 1 d . 1 H31 H 0.4371(6) 0.2532(6) 0.3175(4) 0.033 Uiso 1 calc R 1 C32 C 0.3213(6) 0.5323(5) -0.0725(4) 0.031(2) Uani 1 d . 1 H32C H 0.2873(6) 0.6148(5) -0.0807(4) 0.046 Uiso 1 calc R 1 H32B H 0.3079(6) 0.5128(5) -0.1162(4) 0.046 Uiso 1 calc R 1 H32A H 0.4043(6) 0.5029(5) -0.0818(4) 0.046 Uiso 1 calc R 1 C33 C 0.0947(5) 0.5485(5) 0.0552(5) 0.032(2) Uani 1 d . 1 H33C H 0.0752(5) 0.6300(5) 0.0391(5) 0.047 Uiso 1 calc R 1 H33B H 0.0506(5) 0.5279(5) 0.1175(5) 0.047 Uiso 1 calc R 1 H33A H 0.0758(5) 0.5297(5) 0.0145(5) 0.047 Uiso 1 calc R 1 C34 C 0.2786(5) 0.5168(5) 0.1228(4) 0.026(2) Uani 1 d . 1 H34B H 0.3627(5) 0.4900(5) 0.1107(4) 0.031 Uiso 1 calc R 1 H34A H 0.2454(5) 0.6006(5) 0.1084(4) 0.031 Uiso 1 calc R 1 C35 C 0.0675(6) 0.5694(6) 0.2644(4) 0.025(2) Uani 1 d . 1 C36 C -0.0203(6) 0.5325(6) 0.3008(5) 0.031(2) Uani 1 d . 1 H36 H -0.0018(6) 0.4537(6) 0.3170(5) 0.037 Uiso 1 calc R 1 C37 C -0.1345(6) 0.6082(6) 0.3141(5) 0.036(2) Uani 1 d . 1 H37 H -0.1941(6) 0.5819(6) 0.3386(5) 0.043 Uiso 1 calc R 1 C38 C -0.1604(7) 0.7225(7) 0.2912(5) 0.046(2) Uani 1 d . 1 H38 H -0.2386(7) 0.7753(7) 0.2997(5) 0.055 Uiso 1 calc R 1 C39 C -0.0759(7) 0.7607(6) 0.2569(6) 0.048(2) Uani 1 d . 1 H39 H -0.0951(7) 0.8396(6) 0.2423(6) 0.058 Uiso 1 calc R 1 C40 C 0.0379(6) 0.6848(6) 0.2431(5) 0.041(2) Uani 1 d . 1 H40 H 0.0967(6) 0.7120(6) 0.2186(5) 0.049 Uiso 1 calc R 1 C41 C 0.2726(6) 0.5092(5) 0.3006(5) 0.024(2) Uani 1 d . 1 C42 C 0.3724(6) 0.5270(6) 0.2604(5) 0.038(2) Uani 1 d . 1 H42 H 0.4128(6) 0.5214(6) 0.1994(5) 0.045 Uiso 1 calc R 1 C43 C 0.4148(7) 0.5528(6) 0.3075(6) 0.044(2) Uani 1 d . 1 H43 H 0.4842(7) 0.5641(6) 0.2786(6) 0.053 Uiso 1 calc R 1 C44 C 0.3578(7) 0.5623(6) 0.3948(5) 0.035(2) Uani 1 d . 1 H44 H 0.3873(7) 0.5797(6) 0.4270(5) 0.042 Uiso 1 calc R 1 C45 C 0.2576(7) 0.5463(6) 0.4360(5) 0.044(2) Uani 1 d . 1 H45 H 0.2169(7) 0.5530(6) 0.4968(5) 0.053 Uiso 1 calc R 1 C46 C 0.2157(6) 0.5204(6) 0.3883(5) 0.040(2) Uani 1 d . 1 H46 H 0.1458(6) 0.5100(6) 0.4171(5) 0.048 Uiso 1 calc R 1 C47 C 0.2661(9) 0.1175(13) 0.5288(12) 0.078(6) Uiso 0.57(2) d PG 2 H47 H 0.3408(9) 0.0837(13) 0.5366(12) 0.094 Uiso 0.57(2) calc PR 2 C48 C 0.2123(11) 0.2344(13) 0.5018(9) 0.057(5) Uiso 0.57(2) d PG 2 H48 H 0.2502(16) 0.2804(18) 0.4911(13) 0.069 Uiso 0.57(2) calc PR 2 C49 C 0.1030(13) 0.2838(8) 0.4903(9) 0.049(5) Uiso 0.57(2) d PG 2 H49 H 0.0663(20) 0.3637(8) 0.4718(14) 0.059 Uiso 0.57(2) calc PR 2 C50 C 0.0475(9) 0.2164(10) 0.5059(11) 0.074(6) Uiso 0.57(2) d PG 2 H50 H -0.0272(11) 0.2502(16) 0.4981(18) 0.089 Uiso 0.57(2) calc PR 2 C51 C 0.1013(12) 0.0996(10) 0.5329(9) 0.061(8) Uiso 0.57(2) d PG 2 H51 H 0.0633(18) 0.0535(15) 0.5436(14) 0.073 Uiso 0.57(2) calc PR 2 C52 C 0.2106(14) 0.0501(8) 0.5444(11) 0.077(6) Uiso 0.57(2) d PG 2 H52 H 0.2473(22) -0.0298(8) 0.5628(16) 0.093 Uiso 0.57(2) calc PR 2 C47A C 0.2509(10) 0.0773(12) 0.5639(10) 0.030(5) Uiso 0.43(2) d PG 3 H47A H 0.3092(10) 0.0277(12) 0.5937(10) 0.035 Uiso 0.43(2) calc PR 3 C48A C 0.2509(15) 0.1813(17) 0.5097(9) 0.065(7) Uiso 0.43(2) d PG 3 H48A H 0.3092(21) 0.2028(25) 0.5024(14) 0.078 Uiso 0.43(2) calc PR 3 C49A C 0.1656(20) 0.2539(12) 0.4660(10) 0.049(6) Uiso 0.43(2) d PG 3 H49A H 0.1656(29) 0.3250(16) 0.4290(14) 0.059 Uiso 0.43(2) calc PR 3 C50A C 0.0803(14) 0.2225(11) 0.4766(11) 0.059(7) Uiso 0.43(2) d PG 3 H50A H 0.0220(19) 0.2721(15) 0.4468(16) 0.071 Uiso 0.43(2) calc PR 3 C51A C 0.0802(12) 0.1185(14) 0.5309(11) 0.076(13) Uiso 0.43(2) d PG 3 H51A H 0.0219(18) 0.0971(22) 0.5381(16) 0.091 Uiso 0.43(2) calc PR 3 C52A C 0.1655(15) 0.0459(9) 0.5745(10) 0.039(6) Uiso 0.43(2) d PG 3 H52A H 0.1655(24) -0.0252(12) 0.6115(14) 0.047 Uiso 0.43(2) calc PR 3 C53 C 0.9277(9) 0.1105(7) -0.0158(6) 0.063(3) Uani 1 d . 3 H53 H 0.8773(9) 0.1882(7) -0.0277(6) 0.076 Uiso 1 calc R 3 C54 C 0.8930(7) 0.0301(9) -0.0057(6) 0.063(3) Uani 1 d . 3 H54 H 0.8185(7) 0.0511(9) -0.0089(6) 0.075 Uiso 1 calc R 3 C55 C 0.9680(9) -0.0819(8) 0.0091(6) 0.062(3) Uani 1 d . 3 H55 H 0.9462(9) -0.1390(8) 0.0146(6) 0.075 Uiso 1 calc R 3 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 Li 0.026(7) 0.029(7) 0.035(8) -0.019(6) -0.009(6) 0.000(6) P1 0.0216(11) 0.0219(11) 0.0316(12) -0.0063(9) -0.0086(9) -0.0093(9) P2 0.0204(11) 0.0213(11) 0.0323(12) -0.0095(9) -0.0076(9) -0.0066(9) P3 0.0231(11) 0.0221(11) 0.0297(12) -0.0086(9) -0.0056(9) -0.0096(9) Si1 0.0232(12) 0.0223(11) 0.0291(12) -0.0076(10) -0.0065(10) -0.0113(9) Si2 0.0201(11) 0.0226(12) 0.0293(12) -0.0091(10) -0.0054(9) -0.0090(9) Si3 0.0244(11) 0.0192(11) 0.0261(12) -0.0051(9) -0.0066(9) -0.0091(9) C1 0.028(4) 0.017(4) 0.014(4) 0.003(3) -0.004(3) -0.016(3) C2 0.027(4) 0.029(4) 0.042(5) -0.018(4) -0.008(4) -0.013(4) C3 0.025(4) 0.046(5) 0.043(5) -0.013(4) -0.009(4) -0.017(4) C4 0.026(4) 0.015(4) 0.038(5) -0.003(3) -0.018(4) -0.008(3) C5 0.024(4) 0.020(4) 0.033(5) -0.006(4) -0.008(4) -0.009(4) C6 0.035(5) 0.033(5) 0.034(5) -0.006(4) -0.014(4) -0.014(4) C7 0.037(5) 0.034(5) 0.044(5) 0.003(4) -0.019(4) -0.009(4) C8 0.052(6) 0.020(5) 0.056(6) 0.001(4) -0.012(5) -0.011(4) C9 0.052(6) 0.027(5) 0.061(6) -0.008(4) -0.028(5) -0.015(4) C10 0.033(5) 0.015(4) 0.048(5) 0.002(4) -0.023(4) -0.007(4) C11 0.026(4) 0.015(4) 0.026(4) -0.006(3) -0.006(3) -0.011(4) C12 0.029(5) 0.036(5) 0.041(5) -0.008(4) -0.016(4) -0.005(4) C13 0.047(6) 0.053(6) 0.032(5) -0.010(5) 0.002(5) -0.032(5) C14 0.027(5) 0.050(6) 0.041(6) -0.030(5) 0.003(4) -0.018(5) C15 0.012(5) 0.032(5) 0.069(7) -0.019(5) -0.008(4) 0.004(4) C16 0.025(5) 0.026(5) 0.048(5) -0.009(4) -0.012(4) -0.006(4) C17 0.033(5) 0.033(5) 0.036(5) -0.006(4) -0.006(4) -0.014(4) C18 0.017(4) 0.032(5) 0.044(5) -0.013(4) -0.002(4) -0.010(3) C19 0.021(4) 0.026(4) 0.036(5) -0.017(4) -0.012(3) -0.005(3) C20 0.015(4) 0.027(4) 0.028(5) -0.006(4) -0.005(3) -0.006(3) C21 0.086(7) 0.040(6) 0.031(6) -0.007(4) -0.001(5) -0.042(5) C22 0.097(8) 0.047(6) 0.028(5) 0.007(5) -0.011(5) -0.044(6) C23 0.035(5) 0.042(5) 0.036(6) 0.001(5) -0.004(4) -0.021(4) C24 0.055(6) 0.022(5) 0.057(7) -0.008(4) -0.018(5) -0.010(4) C25 0.060(6) 0.033(5) 0.035(5) -0.008(4) -0.022(4) -0.017(4) C26 0.023(4) 0.021(4) 0.031(4) -0.007(4) -0.009(3) -0.010(3) C27 0.030(5) 0.028(5) 0.052(6) -0.017(4) -0.017(4) -0.007(4) C28 0.025(5) 0.049(6) 0.059(6) -0.022(5) -0.012(4) -0.014(4) C29 0.047(6) 0.043(5) 0.052(6) -0.006(5) -0.023(5) -0.026(5) C30 0.051(6) 0.029(5) 0.042(5) -0.012(4) -0.020(4) -0.013(4) C31 0.033(4) 0.027(4) 0.028(5) -0.012(4) -0.007(4) -0.013(4) C32 0.036(5) 0.023(4) 0.034(5) -0.010(4) -0.010(4) -0.009(4) C33 0.030(4) 0.023(4) 0.041(5) -0.008(4) -0.010(4) -0.010(4) C34 0.022(4) 0.016(4) 0.038(5) -0.011(3) -0.005(3) -0.005(3) C35 0.026(4) 0.024(4) 0.031(5) -0.008(3) -0.009(4) -0.013(4) C36 0.032(5) 0.030(5) 0.034(5) -0.011(4) -0.004(4) -0.016(4) C37 0.028(5) 0.046(6) 0.043(5) -0.012(4) -0.009(4) -0.021(4) C38 0.028(5) 0.036(6) 0.063(6) -0.017(5) -0.011(4) -0.003(4) C39 0.030(5) 0.024(5) 0.084(7) -0.021(5) -0.007(5) -0.007(4) C40 0.025(5) 0.036(5) 0.058(6) -0.012(4) -0.003(4) -0.016(4) C41 0.022(4) 0.023(4) 0.025(5) -0.006(3) -0.005(3) -0.010(3) C42 0.029(5) 0.058(6) 0.038(5) -0.025(4) -0.003(4) -0.020(4) C43 0.036(5) 0.050(6) 0.059(6) -0.015(5) -0.016(5) -0.023(4) C44 0.043(5) 0.033(5) 0.037(5) -0.013(4) -0.014(4) -0.015(4) C45 0.061(6) 0.052(6) 0.022(5) -0.010(4) -0.006(4) -0.027(5) C46 0.044(5) 0.052(6) 0.038(5) -0.010(4) -0.007(4) -0.033(4) C53 0.061(7) 0.043(6) 0.075(7) -0.013(5) -0.017(6) -0.017(6) C54 0.040(6) 0.084(8) 0.071(7) -0.035(6) -0.013(5) -0.018(6) C55 0.065(7) 0.062(8) 0.072(7) -0.019(6) -0.013(6) -0.036(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 Li C1 2.222(13) . ? Li P2 2.642(11) . ? Li P3 2.652(11) . ? Li P1 2.663(12) . ? Li Si3 3.187(12) . ? Li Si2 3.190(12) . ? P1 C4 1.814(6) . ? P1 C5 1.831(6) . ? P1 C11 1.833(7) . ? P2 C19 1.814(6) . ? P2 C26 1.827(6) . ? P2 C20 1.837(7) . ? P3 C34 1.810(7) . ? P3 C35 1.827(7) . ? P3 C41 1.842(7) . ? Si1 C1 1.825(6) . ? Si1 C3 1.882(7) . ? Si1 C2 1.887(6) . ? Si1 C4 1.895(6) . ? Si2 C1 1.830(6) . ? Si2 C17 1.877(7) . ? Si2 C18 1.889(6) . ? Si2 C19 1.902(6) . ? Si3 C1 1.826(6) . ? Si3 C32 1.877(7) . ? Si3 C33 1.878(6) . ? Si3 C34 1.894(6) . ? C5 C6 1.376(9) . ? C5 C10 1.382(9) . ? C6 C7 1.387(9) . ? C7 C8 1.362(10) . ? C8 C9 1.377(10) . ? C9 C10 1.376(9) . ? C11 C12 1.380(9) . ? C11 C16 1.385(9) . ? C12 C13 1.391(10) . ? C13 C14 1.363(10) . ? C14 C15 1.354(10) . ? C15 C16 1.380(9) . ? C20 C25 1.357(9) . ? C20 C21 1.370(9) . ? C21 C22 1.379(10) . ? C22 C23 1.355(10) . ? C23 C24 1.349(10) . ? C24 C25 1.402(9) . ? C26 C31 1.379(8) . ? C26 C27 1.395(9) . ? C27 C28 1.402(9) . ? C28 C29 1.362(10) . ? C29 C30 1.386(10) . ? C30 C31 1.382(9) . ? C35 C36 1.383(9) . ? C35 C40 1.384(9) . ? C36 C37 1.382(9) . ? C37 C38 1.380(9) . ? C38 C39 1.356(10) . ? C39 C40 1.379(9) . ? C41 C46 1.372(9) . ? C41 C42 1.377(9) . ? C42 C43 1.385(9) . ? C43 C44 1.362(10) . ? C44 C45 1.369(10) . ? C45 C46 1.389(10) . ? C47 C48 1.39 . ? C47 C52 1.39 . ? C48 C49 1.39 . ? C49 C50 1.39 . ? C50 C51 1.39 . ? C51 C52 1.39 . ? C47A C48A 1.39 . ? C47A C52A 1.39 . ? C48A C49A 1.39 . ? C49A C50A 1.39 . ? C50A C51A 1.39 . ? C51A C52A 1.39 . ? C53 C55 1.348(11) 2_755 ? C53 C54 1.362(11) . ? C54 C55 1.375(11) . ? C55 C53 1.348(11) 2_755 ? 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 C1 Li P2 95.8(4) . . ? C1 Li P3 96.0(5) . . ? P2 Li P3 119.1(4) . . ? C1 Li P1 94.5(4) . . ? P2 Li P1 118.7(4) . . ? P3 Li P1 119.6(4) . . ? C1 Li Si3 33.9(2) . . ? P2 Li Si3 119.1(4) . . ? P3 Li Si3 63.6(3) . . ? P1 Li Si3 101.4(4) . . ? C1 Li Si2 33.9(2) . . ? P2 Li Si2 63.4(2) . . ? P3 Li Si2 102.5(4) . . ? P1 Li Si2 117.7(4) . . ? Si3 Li Si2 57.8(2) . . ? C4 P1 C5 103.9(3) . . ? C4 P1 C11 104.2(3) . . ? C5 P1 C11 100.5(3) . . ? C4 P1 Li 95.6(3) . . ? C5 P1 Li 112.9(3) . . ? C11 P1 Li 135.6(3) . . ? C19 P2 C26 103.4(3) . . ? C19 P2 C20 104.8(3) . . ? C26 P2 C20 100.6(3) . . ? C19 P2 Li 94.6(3) . . ? C26 P2 Li 115.3(3) . . ? C20 P2 Li 133.7(3) . . ? C34 P3 C35 103.8(3) . . ? C34 P3 C41 105.1(3) . . ? C35 P3 C41 100.2(3) . . ? C34 P3 Li 94.0(3) . . ? C35 P3 Li 115.7(3) . . ? C41 P3 Li 133.8(3) . . ? C1 Si1 C3 114.6(3) . . ? C1 Si1 C2 116.3(3) . . ? C3 Si1 C2 103.3(3) . . ? C1 Si1 C4 110.7(3) . . ? C3 Si1 C4 106.1(3) . . ? C2 Si1 C4 104.8(3) . . ? C1 Si2 C17 116.1(3) . . ? C1 Si2 C18 116.1(3) . . ? C17 Si2 C18 102.8(3) . . ? C1 Si2 C19 110.3(3) . . ? C17 Si2 C19 105.0(3) . . ? C18 Si2 C19 105.6(3) . . ? C1 Si2 Li 42.7(3) . . ? C17 Si2 Li 153.5(3) . . ? C18 Si2 Li 102.1(3) . . ? C19 Si2 Li 76.9(3) . . ? C1 Si3 C32 115.6(3) . . ? C1 Si3 C33 115.9(3) . . ? C32 Si3 C33 103.1(3) . . ? C1 Si3 C34 110.6(3) . . ? C32 Si3 C34 105.5(3) . . ? C33 Si3 C34 105.0(3) . . ? C1 Si3 Li 42.7(3) . . ? C32 Si3 Li 152.9(3) . . ? C33 Si3 Li 102.2(3) . . ? C34 Si3 Li 76.7(3) . . ? Si1 C1 Si3 114.5(3) . . ? Si1 C1 Si2 113.8(3) . . ? Si3 C1 Si2 114.9(3) . . ? Si1 C1 Li 104.9(4) . . ? Si3 C1 Li 103.4(4) . . ? Si2 C1 Li 103.4(4) . . ? P1 C4 Si1 113.3(3) . . ? C6 C5 C10 119.0(6) . . ? C6 C5 P1 119.1(5) . . ? C10 C5 P1 121.9(5) . . ? C5 C6 C7 120.4(7) . . ? C8 C7 C6 119.9(7) . . ? C7 C8 C9 120.2(7) . . ? C10 C9 C8 120.0(7) . . ? C9 C10 C5 120.5(7) . . ? C12 C11 C16 117.1(6) . . ? C12 C11 P1 120.5(5) . . ? C16 C11 P1 122.3(5) . . ? C11 C12 C13 121.2(7) . . ? C14 C13 C12 120.0(7) . . ? C15 C14 C13 119.8(7) . . ? C14 C15 C16 120.5(7) . . ? C15 C16 C11 121.3(7) . . ? P2 C19 Si2 113.0(3) . . ? C25 C20 C21 117.0(7) . . ? C25 C20 P2 124.1(6) . . ? C21 C20 P2 118.8(6) . . ? C20 C21 C22 122.5(8) . . ? C23 C22 C21 119.9(8) . . ? C24 C23 C22 118.7(8) . . ? C23 C24 C25 121.2(8) . . ? C20 C25 C24 120.6(7) . . ? C31 C26 C27 118.5(6) . . ? C31 C26 P2 119.7(5) . . ? C27 C26 P2 121.6(5) . . ? C26 C27 C28 119.9(7) . . ? C29 C28 C27 120.8(7) . . ? C28 C29 C30 119.4(7) . . ? C31 C30 C29 120.3(7) . . ? C26 C31 C30 121.1(7) . . ? P3 C34 Si3 114.3(3) . . ? C36 C35 C40 118.1(6) . . ? C36 C35 P3 120.2(5) . . ? C40 C35 P3 121.6(5) . . ? C37 C36 C35 121.3(7) . . ? C38 C37 C36 118.8(7) . . ? C39 C38 C37 121.0(7) . . ? C38 C39 C40 119.9(7) . . ? C39 C40 C35 120.9(7) . . ? C46 C41 C42 117.5(6) . . ? C46 C41 P3 120.4(5) . . ? C42 C41 P3 122.1(5) . . ? C41 C42 C43 121.1(7) . . ? C44 C43 C42 120.5(7) . . ? C43 C44 C45 119.5(7) . . ? C44 C45 C46 119.6(7) . . ? C41 C46 C45 121.8(7) . . ? C48 C47 C52 120.0 . . ? C47 C48 C49 120.0 . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C52 C51 C50 120.0 . . ? C51 C52 C47 120.0 . . ? C48A C47A C52A 120.0 . . ? C49A C48A C47A 120.0 . . ? C48A C49A C50A 120.0 . . ? C51A C50A C49A 120.0 . . ? C52A C51A C50A 120.0 . . ? C51A C52A C47A 120.0 . . ? C55 C53 C54 121.2(9) 2_755 . ? C53 C54 C55 118.8(8) . . ? C53 C55 C54 119.9(8) 2_755 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Li P1 C4 -9.8(4) . . . . ? P2 Li P1 C4 -108.9(5) . . . . ? P3 Li P1 C4 89.7(5) . . . . ? Si3 Li P1 C4 23.7(3) . . . . ? Si2 Li P1 C4 -35.8(4) . . . . ? C1 Li P1 C5 97.8(4) . . . . ? P2 Li P1 C5 -1.3(6) . . . . ? P3 Li P1 C5 -162.7(4) . . . . ? Si3 Li P1 C5 131.3(3) . . . . ? Si2 Li P1 C5 71.9(5) . . . . ? C1 Li P1 C11 -126.7(4) . . . . ? P2 Li P1 C11 134.1(4) . . . . ? P3 Li P1 C11 -27.2(8) . . . . ? Si3 Li P1 C11 -93.3(5) . . . . ? Si2 Li P1 C11 -152.7(4) . . . . ? C1 Li P2 C19 -10.7(4) . . . . ? P3 Li P2 C19 -110.9(5) . . . . ? P1 Li P2 C19 87.6(5) . . . . ? Si3 Li P2 C19 -36.7(4) . . . . ? Si2 Li P2 C19 -21.0(2) . . . . ? C1 Li P2 C26 96.4(4) . . . . ? P3 Li P2 C26 -3.8(6) . . . . ? P1 Li P2 C26 -165.2(4) . . . . ? Si3 Li P2 C26 70.5(5) . . . . ? Si2 Li P2 C26 86.2(3) . . . . ? C1 Li P2 C20 -126.4(5) . . . . ? P3 Li P2 C20 133.4(5) . . . . ? P1 Li P2 C20 -28.1(7) . . . . ? Si3 Li P2 C20 -152.4(4) . . . . ? Si2 Li P2 C20 -136.6(4) . . . . ? C1 Li P3 C34 -9.9(4) . . . . ? P2 Li P3 C34 90.2(5) . . . . ? P1 Li P3 C34 -108.5(5) . . . . ? Si3 Li P3 C34 -20.1(2) . . . . ? Si2 Li P3 C34 23.9(4) . . . . ? C1 Li P3 C35 97.5(4) . . . . ? P2 Li P3 C35 -162.5(4) . . . . ? P1 Li P3 C35 -1.2(6) . . . . ? Si3 Li P3 C35 87.3(3) . . . . ? Si2 Li P3 C35 131.2(3) . . . . ? C1 Li P3 C41 -125.2(4) . . . . ? P2 Li P3 C41 -25.2(7) . . . . ? P1 Li P3 C41 136.1(4) . . . . ? Si3 Li P3 C41 -135.4(4) . . . . ? Si2 Li P3 C41 -91.5(5) . . . . ? C1 Li Si2 C1 0.0 . . . . ? P2 Li Si2 C1 161.5(5) . . . . ? P3 Li Si2 C1 -82.0(4) . . . . ? P1 Li Si2 C1 51.5(4) . . . . ? Si3 Li Si2 C1 -34.7(3) . . . . ? C1 Li Si2 C17 -43.7(8) . . . . ? P2 Li Si2 C17 117.8(6) . . . . ? P3 Li Si2 C17 -125.8(6) . . . . ? P1 Li Si2 C17 7.7(9) . . . . ? Si3 Li Si2 C17 -78.4(7) . . . . ? C1 Li Si2 C18 115.5(4) . . . . ? P2 Li Si2 C18 -83.0(3) . . . . ? P3 Li Si2 C18 33.5(4) . . . . ? P1 Li Si2 C18 167.0(4) . . . . ? Si3 Li Si2 C18 80.8(3) . . . . ? C1 Li Si2 C19 -141.0(4) . . . . ? P2 Li Si2 C19 20.5(2) . . . . ? P3 Li Si2 C19 136.9(4) . . . . ? P1 Li Si2 C19 -89.6(4) . . . . ? Si3 Li Si2 C19 -175.8(3) . . . . ? C1 Li Si3 C1 0.0 . . . . ? P2 Li Si3 C1 51.4(4) . . . . ? P3 Li Si3 C1 161.6(5) . . . . ? P1 Li Si3 C1 -80.9(4) . . . . ? Si2 Li Si3 C1 34.8(3) . . . . ? C1 Li Si3 C32 -43.7(8) . . . . ? P2 Li Si3 C32 7.8(9) . . . . ? P3 Li Si3 C32 117.9(6) . . . . ? P1 Li Si3 C32 -124.5(6) . . . . ? Si2 Li Si3 C32 -8.9(7) . . . . ? C1 Li Si3 C33 115.2(4) . . . . ? P2 Li Si3 C33 166.6(4) . . . . ? P3 Li Si3 C33 -83.2(3) . . . . ? P1 Li Si3 C33 34.3(4) . . . . ? Si2 Li Si3 C33 150.0(2) . . . . ? C1 Li Si3 C34 -141.9(4) . . . . ? P2 Li Si3 C34 -90.5(4) . . . . ? P3 Li Si3 C34 19.6(2) . . . . ? P1 Li Si3 C34 137.2(4) . . . . ? Si2 Li Si3 C34 -107.2(2) . . . . ? C3 Si1 C1 Si3 47.1(5) . . . . ? C2 Si1 C1 Si3 167.6(3) . . . . ? C4 Si1 C1 Si3 -72.9(4) . . . . ? C3 Si1 C1 Si2 -87.8(4) . . . . ? C2 Si1 C1 Si2 32.7(4) . . . . ? C4 Si1 C1 Si2 152.2(3) . . . . ? C3 Si1 C1 Li 159.8(4) . . . . ? C2 Si1 C1 Li -79.7(5) . . . . ? C4 Si1 C1 Li 39.8(5) . . . . ? C32 Si3 C1 Si1 -86.8(4) . . . . ? C33 Si3 C1 Si1 34.0(5) . . . . ? C34 Si3 C1 Si1 153.4(3) . . . . ? Li Si3 C1 Si1 113.6(5) . . . . ? C32 Si3 C1 Si2 47.7(5) . . . . ? C33 Si3 C1 Si2 168.5(3) . . . . ? C34 Si3 C1 Si2 -72.1(4) . . . . ? Li Si3 C1 Si2 -112.0(5) . . . . ? C32 Si3 C1 Li 159.6(4) . . . . ? C33 Si3 C1 Li -79.5(5) . . . . ? C34 Si3 C1 Li 39.9(5) . . . . ? Li Si3 C1 Li 0.0 . . . . ? C17 Si2 C1 Si1 46.6(4) . . . . ? C18 Si2 C1 Si1 167.5(3) . . . . ? C19 Si2 C1 Si1 -72.5(4) . . . . ? Li Si2 C1 Si1 -113.3(5) . . . . ? C17 Si2 C1 Si3 -88.1(4) . . . . ? C18 Si2 C1 Si3 32.7(5) . . . . ? C19 Si2 C1 Si3 152.7(3) . . . . ? Li Si2 C1 Si3 112.0(5) . . . . ? C17 Si2 C1 Li 159.9(4) . . . . ? C18 Si2 C1 Li -79.2(5) . . . . ? C19 Si2 C1 Li 40.8(5) . . . . ? Li Si2 C1 Li 0.0 . . . . ? P2 Li C1 Si1 103.0(4) . . . . ? P3 Li C1 Si1 -136.9(3) . . . . ? P1 Li C1 Si1 -16.4(4) . . . . ? Si3 Li C1 Si1 -120.3(4) . . . . ? Si2 Li C1 Si1 119.6(4) . . . . ? P2 Li C1 Si3 -136.7(3) . . . . ? P3 Li C1 Si3 -16.5(4) . . . . ? P1 Li C1 Si3 103.9(4) . . . . ? Si3 Li C1 Si3 0.0 . . . . ? Si2 Li C1 Si3 -120.1(4) . . . . ? P2 Li C1 Si2 -16.6(4) . . . . ? P3 Li C1 Si2 103.6(4) . . . . ? P1 Li C1 Si2 -136.0(3) . . . . ? Si3 Li C1 Si2 120.1(4) . . . . ? Si2 Li C1 Si2 0.0 . . . . ? C5 P1 C4 Si1 -81.3(4) . . . . ? C11 P1 C4 Si1 173.9(3) . . . . ? Li P1 C4 Si1 33.9(4) . . . . ? C1 Si1 C4 P1 -54.0(4) . . . . ? C3 Si1 C4 P1 -178.9(3) . . . . ? C2 Si1 C4 P1 72.2(4) . . . . ? C4 P1 C5 C6 131.8(6) . . . . ? C11 P1 C5 C6 -120.5(6) . . . . ? Li P1 C5 C6 29.5(7) . . . . ? C4 P1 C5 C10 -46.1(7) . . . . ? C11 P1 C5 C10 61.6(6) . . . . ? Li P1 C5 C10 -148.4(6) . . . . ? C10 C5 C6 C7 0.9(11) . . . . ? P1 C5 C6 C7 -177.0(6) . . . . ? C5 C6 C7 C8 -1.6(12) . . . . ? C6 C7 C8 C9 1.7(12) . . . . ? C7 C8 C9 C10 -1.0(12) . . . . ? C8 C9 C10 C5 0.2(12) . . . . ? C6 C5 C10 C9 -0.2(11) . . . . ? P1 C5 C10 C9 177.7(6) . . . . ? C4 P1 C11 C12 147.5(6) . . . . ? C5 P1 C11 C12 40.2(6) . . . . ? Li P1 C11 C12 -98.7(7) . . . . ? C4 P1 C11 C16 -34.0(6) . . . . ? C5 P1 C11 C16 -141.3(6) . . . . ? Li P1 C11 C16 79.8(7) . . . . ? C16 C11 C12 C13 -0.7(10) . . . . ? P1 C11 C12 C13 177.9(6) . . . . ? C11 C12 C13 C14 0.8(11) . . . . ? C12 C13 C14 C15 -0.5(11) . . . . ? C13 C14 C15 C16 0.0(12) . . . . ? C14 C15 C16 C11 0.1(12) . . . . ? C12 C11 C16 C15 0.3(10) . . . . ? P1 C11 C16 C15 -178.3(6) . . . . ? C26 P2 C19 Si2 -81.7(4) . . . . ? C20 P2 C19 Si2 173.3(3) . . . . ? Li P2 C19 Si2 35.7(4) . . . . ? C1 Si2 C19 P2 -56.6(4) . . . . ? C17 Si2 C19 P2 177.7(3) . . . . ? C18 Si2 C19 P2 69.5(4) . . . . ? Li Si2 C19 P2 -29.6(3) . . . . ? C19 P2 C20 C25 -14.0(7) . . . . ? C26 P2 C20 C25 -121.1(6) . . . . ? Li P2 C20 C25 97.7(7) . . . . ? C19 P2 C20 C21 168.6(6) . . . . ? C26 P2 C20 C21 61.6(6) . . . . ? Li P2 C20 C21 -79.7(7) . . . . ? C25 C20 C21 C22 0.7(12) . . . . ? P2 C20 C21 C22 178.2(7) . . . . ? C20 C21 C22 C23 -1.1(14) . . . . ? C21 C22 C23 C24 1.4(13) . . . . ? C22 C23 C24 C25 -1.4(12) . . . . ? C21 C20 C25 C24 -0.6(11) . . . . ? P2 C20 C25 C24 -178.0(6) . . . . ? C23 C24 C25 C20 1.0(12) . . . . ? C19 P2 C26 C31 129.2(6) . . . . ? C20 P2 C26 C31 -122.6(6) . . . . ? Li P2 C26 C31 27.5(7) . . . . ? C19 P2 C26 C27 -45.8(6) . . . . ? C20 P2 C26 C27 62.4(6) . . . . ? Li P2 C26 C27 -147.6(6) . . . . ? C31 C26 C27 C28 -1.4(10) . . . . ? P2 C26 C27 C28 173.7(6) . . . . ? C26 C27 C28 C29 1.1(12) . . . . ? C27 C28 C29 C30 -0.4(12) . . . . ? C28 C29 C30 C31 0.0(11) . . . . ? C27 C26 C31 C30 1.0(10) . . . . ? P2 C26 C31 C30 -174.2(5) . . . . ? C29 C30 C31 C26 -0.4(11) . . . . ? C35 P3 C34 Si3 -83.1(4) . . . . ? C41 P3 C34 Si3 172.1(3) . . . . ? Li P3 C34 Si3 34.6(4) . . . . ? C1 Si3 C34 P3 -55.5(4) . . . . ? C32 Si3 C34 P3 178.9(3) . . . . ? C33 Si3 C34 P3 70.3(4) . . . . ? Li Si3 C34 P3 -29.0(3) . . . . ? C34 P3 C35 C36 123.7(6) . . . . ? C41 P3 C35 C36 -127.9(6) . . . . ? Li P3 C35 C36 22.3(7) . . . . ? C34 P3 C35 C40 -54.0(7) . . . . ? C41 P3 C35 C40 54.5(7) . . . . ? Li P3 C35 C40 -155.3(6) . . . . ? C40 C35 C36 C37 1.2(11) . . . . ? P3 C35 C36 C37 -176.5(5) . . . . ? C35 C36 C37 C38 -0.7(11) . . . . ? C36 C37 C38 C39 -0.5(12) . . . . ? C37 C38 C39 C40 1.0(13) . . . . ? C38 C39 C40 C35 -0.4(13) . . . . ? C36 C35 C40 C39 -0.7(11) . . . . ? P3 C35 C40 C39 177.0(6) . . . . ? C34 P3 C41 C46 157.9(6) . . . . ? C35 P3 C41 C46 50.5(6) . . . . ? Li P3 C41 C46 -91.1(7) . . . . ? C34 P3 C41 C42 -23.9(7) . . . . ? C35 P3 C41 C42 -131.3(6) . . . . ? Li P3 C41 C42 87.1(7) . . . . ? C46 C41 C42 C43 1.3(11) . . . . ? P3 C41 C42 C43 -177.0(6) . . . . ? C41 C42 C43 C44 -0.6(12) . . . . ? C42 C43 C44 C45 -0.3(12) . . . . ? C43 C44 C45 C46 0.3(11) . . . . ? C42 C41 C46 C45 -1.3(11) . . . . ? P3 C41 C46 C45 177.0(6) . . . . ? C44 C45 C46 C41 0.5(12) . . . . ? C52 C47 C48 C49 0.0 . . . . ? C47 C48 C49 C50 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? C49 C50 C51 C52 0.0 . . . . ? C50 C51 C52 C47 0.0 . . . . ? C48 C47 C52 C51 0.0 . . . . ? C52A C47A C48A C49A 0.0 . . . . ? C47A C48A C49A C50A 0.0 . . . . ? C48A C49A C50A C51A 0.0 . . . . ? C49A C50A C51A C52A 0.0 . . . . ? C50A C51A C52A C47A 0.0 . . . . ? C48A C47A C52A C51A 0.0 . . . . ? C55 C53 C54 C55 -1.8(16) 2_755 . . . ? C53 C54 C55 C53 1.8(16) . . . 2_755 ? _refine_diff_density_max 0.280 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.070