# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1831 data_j _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C19 H20 Cl Si' _chemical_formula_weight 311.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9575(10) _cell_length_b 9.4809(11) _cell_length_c 11.2364(13) _cell_angle_alpha 98.377(2) _cell_angle_beta 112.958(2) _cell_angle_gamma 96.817(2) _cell_volume 853.00(17) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.214 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 330 _exptl_absorpt_coefficient_mu 0.286 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3754 _diffrn_reflns_av_R_equivalents 0.1995 _diffrn_reflns_av_sigmaI/netI 0.1164 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2724 _reflns_number_gt 1988 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+2.3558P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.012(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2724 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1135 _refine_ls_R_factor_gt 0.0696 _refine_ls_wR_factor_ref 0.1913 _refine_ls_wR_factor_gt 0.1520 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.12407(16) 0.04702(13) 0.72375(12) 0.0368(4) Uani 1 1 d . . . Cl1 Cl 0.36751(16) 0.04016(15) 0.83768(14) 0.0561(4) Uani 1 1 d . . . C1 C 0.0729(6) 0.2224(5) 0.7756(4) 0.0384(11) Uani 1 1 d . . . C2 C -0.0484(6) 0.1959(5) 0.8177(4) 0.0346(10) Uani 1 1 d . . . C3 C -0.0990(6) 0.0396(5) 0.8216(4) 0.0373(11) Uani 1 1 d . . . C4 C -0.0224(5) -0.0596(5) 0.7719(4) 0.0334(10) Uani 1 1 d . . . C5 C 0.1511(6) 0.3672(5) 0.7699(5) 0.0430(12) Uani 1 1 d . . . C6 C 0.1401(8) 0.3991(6) 0.6505(6) 0.0627(17) Uani 1 1 d . . . H6A H 0.0781 0.3308 0.5725 0.075 Uiso 1 1 calc R . . C7 C 0.2200(9) 0.5312(7) 0.6456(7) 0.080(2) Uani 1 1 d . . . H7A H 0.2080 0.5525 0.5645 0.096 Uiso 1 1 calc R . . C8 C 0.3165(8) 0.6304(6) 0.7601(8) 0.0701(19) Uani 1 1 d . . . H8A H 0.3738 0.7175 0.7574 0.084 Uiso 1 1 calc R . . C9 C 0.3281(8) 0.6008(6) 0.8777(8) 0.076(2) Uani 1 1 d . . . H9A H 0.3908 0.6693 0.9554 0.091 Uiso 1 1 calc R . . C10 C 0.2471(7) 0.4690(6) 0.8828(6) 0.0563(14) Uani 1 1 d . . . H10A H 0.2583 0.4495 0.9644 0.068 Uiso 1 1 calc R . . C11 C -0.1379(6) 0.3080(5) 0.8550(5) 0.0459(12) Uani 1 1 d . . . H11A H -0.0777 0.4042 0.8649 0.055 Uiso 1 1 calc R . . H11B H -0.1388 0.3001 0.9399 0.055 Uiso 1 1 calc R . . C12 C -0.3152(7) 0.2915(7) 0.7535(6) 0.0585(15) Uani 1 1 d . . . H12A H -0.3754 0.1961 0.7456 0.070 Uiso 1 1 calc R . . H12B H -0.3669 0.3629 0.7861 0.070 Uiso 1 1 calc R . . C13 C -0.3316(8) 0.3091(8) 0.6193(6) 0.080(2) Uani 1 1 d . . . H13A H -0.2721 0.2433 0.5895 0.096 Uiso 1 1 calc R . . H13B H -0.2798 0.4074 0.6257 0.096 Uiso 1 1 calc R . . C14 C -0.5101(10) 0.2797(12) 0.5160(8) 0.127(4) Uani 1 1 d . . . H14A H -0.5114 0.2918 0.4323 0.190 Uiso 1 1 calc R . . H14B H -0.5690 0.3468 0.5429 0.190 Uiso 1 1 calc R . . H14C H -0.5621 0.1821 0.5080 0.190 Uiso 1 1 calc R . . C15 C -0.2091(6) -0.0075(6) 0.8727(5) 0.0466(13) Uani 1 1 d . . . H15A H -0.2602 0.0579 0.9059 0.056 Uiso 1 1 calc R . . C16 C -0.2422(6) -0.1553(6) 0.8736(5) 0.0519(14) Uani 1 1 d . . . H16A H -0.3149 -0.1876 0.9090 0.062 Uiso 1 1 calc R . . C17 C -0.1701(7) -0.2531(6) 0.8238(5) 0.0549(15) Uani 1 1 d . . . H17A H -0.1959 -0.3511 0.8234 0.066 Uiso 1 1 calc R . . C18 C -0.0584(7) -0.2057(5) 0.7739(5) 0.0486(13) Uani 1 1 d . . . H18A H -0.0073 -0.2719 0.7417 0.058 Uiso 1 1 calc R . . C19 C 0.0899(6) -0.0001(5) 0.5468(4) 0.0431(12) Uani 1 1 d . . . H19A H 0.1644 0.0695 0.5305 0.052 Uiso 1 1 calc R . . H19C H 0.1148 -0.0956 0.5284 0.052 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0390(8) 0.0372(7) 0.0334(7) 0.0055(5) 0.0163(6) 0.0018(5) Cl1 0.0418(8) 0.0590(8) 0.0609(9) 0.0122(6) 0.0151(6) 0.0080(6) C1 0.041(3) 0.038(2) 0.029(2) 0.0068(19) 0.009(2) 0.000(2) C2 0.038(3) 0.037(2) 0.028(2) 0.0059(18) 0.013(2) 0.0079(19) C3 0.036(3) 0.043(2) 0.031(2) 0.0117(19) 0.011(2) 0.003(2) C4 0.034(2) 0.037(2) 0.030(2) 0.0084(18) 0.0144(19) 0.0078(19) C5 0.047(3) 0.034(2) 0.046(3) 0.009(2) 0.019(2) 0.002(2) C6 0.082(4) 0.052(3) 0.050(3) 0.011(3) 0.029(3) -0.008(3) C7 0.097(5) 0.065(4) 0.087(5) 0.035(4) 0.048(4) -0.003(4) C8 0.058(4) 0.045(3) 0.119(6) 0.027(4) 0.047(4) 0.006(3) C9 0.068(4) 0.047(3) 0.095(5) -0.004(3) 0.030(4) -0.012(3) C10 0.055(3) 0.051(3) 0.056(3) 0.004(3) 0.021(3) -0.001(3) C11 0.048(3) 0.047(3) 0.048(3) 0.011(2) 0.024(2) 0.010(2) C12 0.054(3) 0.067(4) 0.068(4) 0.024(3) 0.032(3) 0.027(3) C13 0.073(5) 0.106(5) 0.068(4) 0.030(4) 0.028(4) 0.031(4) C14 0.070(5) 0.215(11) 0.090(6) 0.062(7) 0.016(4) 0.032(6) C15 0.047(3) 0.054(3) 0.039(3) 0.016(2) 0.017(2) 0.004(2) C16 0.046(3) 0.061(3) 0.046(3) 0.021(3) 0.017(2) -0.005(3) C17 0.062(4) 0.042(3) 0.053(3) 0.017(2) 0.017(3) -0.005(3) C18 0.054(3) 0.040(3) 0.047(3) 0.010(2) 0.017(3) 0.005(2) C19 0.043(3) 0.049(3) 0.034(2) 0.004(2) 0.016(2) 0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.850(5) . ? Si1 C4 1.853(4) . ? Si1 C19 1.865(5) . ? Si1 Cl1 2.0684(19) . ? C1 C2 1.355(6) . ? C1 C5 1.487(6) . ? C2 C3 1.510(6) . ? C2 C11 1.511(7) . ? C3 C4 1.402(7) . ? C3 C15 1.384(7) . ? C4 C18 1.391(6) . ? C5 C10 1.370(7) . ? C5 C6 1.387(7) . ? C6 C7 1.387(7) . ? C7 C8 1.369(9) . ? C8 C9 1.357(10) . ? C9 C10 1.390(8) . ? C11 C12 1.525(7) . ? C12 C13 1.493(8) . ? C13 C14 1.528(9) . ? C15 C16 1.400(7) . ? C16 C17 1.365(8) . ? C17 C18 1.386(7) . ? C19 C19 1.542(9) 2_556 ? 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 Si1 C4 93.5(2) . . ? C1 Si1 C19 115.6(2) . . ? C4 Si1 C19 116.4(2) . . ? C1 Si1 Cl1 110.94(15) . . ? C4 Si1 Cl1 112.43(15) . . ? C19 Si1 Cl1 107.53(17) . . ? C2 C1 C5 126.2(5) . . ? C2 C1 Si1 108.5(3) . . ? C5 C1 Si1 125.3(4) . . ? C1 C2 C3 115.7(4) . . ? C1 C2 C11 125.3(4) . . ? C3 C2 C11 119.0(4) . . ? C4 C3 C15 120.3(4) . . ? C4 C3 C2 115.3(4) . . ? C15 C3 C2 124.4(5) . . ? C3 C4 C18 119.5(4) . . ? C3 C4 Si1 106.9(3) . . ? C18 C4 Si1 133.5(4) . . ? C10 C5 C6 117.7(5) . . ? C10 C5 C1 121.2(4) . . ? C6 C5 C1 120.9(4) . . ? C5 C6 C7 121.0(6) . . ? C8 C7 C6 120.0(6) . . ? C9 C8 C7 119.6(5) . . ? C8 C9 C10 120.5(6) . . ? C5 C10 C9 121.1(6) . . ? C2 C11 C12 113.1(4) . . ? C13 C12 C11 114.6(5) . . ? C12 C13 C14 113.9(6) . . ? C3 C15 C16 118.7(5) . . ? C17 C16 C15 121.5(5) . . ? C16 C17 C18 119.8(5) . . ? C17 C18 C4 120.2(5) . . ? C19 C19 Si1 111.5(4) 2_556 . ? _diffrn_measured_fraction_theta_max 0.901 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.901 _refine_diff_density_max 0.661 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.110 #===END data_j2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C47 H58 Li O5 Si2' _chemical_formula_weight 766.05 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2710(9) _cell_length_b 13.9844(9) _cell_length_c 14.0125(9) _cell_angle_alpha 64.6360(10) _cell_angle_beta 77.4500(10) _cell_angle_gamma 74.0300(10) _cell_volume 2244.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.134 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.121 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10702 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.0712 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.61 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7319 _reflns_number_gt 5692 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0664P)^2^+2.8822P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7319 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1085 _refine_ls_R_factor_gt 0.0838 _refine_ls_wR_factor_ref 0.2186 _refine_ls_wR_factor_gt 0.1967 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _refine_ls_shift/su_max 0.167 _refine_ls_shift/su_mean 0.016 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 Si1 Si 0.13905(8) 0.58511(8) 0.40266(8) 0.0451(3) Uani 1 1 d . . . Si2 Si 0.13051(8) 0.73888(8) 0.24230(8) 0.0460(3) Uani 1 1 d . . . Li1 Li 0.0742(8) 0.7561(6) 0.0648(6) 0.078(2) Uani 1 1 d . . . C1 C 0.1847(3) 0.6037(3) 0.5098(3) 0.0499(9) Uani 1 1 d . . . C2 C 0.1482(4) 0.6817(3) 0.5532(3) 0.0603(10) Uani 1 1 d . . . H2A H 0.0857 0.7319 0.5345 0.072 Uiso 1 1 calc R . . C3 C 0.2043(4) 0.6849(4) 0.6236(4) 0.0773(14) Uani 1 1 d . . . H3A H 0.1786 0.7360 0.6536 0.093 Uiso 1 1 calc R . . C4 C 0.2978(5) 0.6128(4) 0.6495(4) 0.0814(14) Uani 1 1 d . . . H4A H 0.3358 0.6164 0.6959 0.098 Uiso 1 1 calc R . . C5 C 0.3361(4) 0.5353(4) 0.6076(4) 0.0734(13) Uani 1 1 d . . . H5A H 0.3997 0.4870 0.6258 0.088 Uiso 1 1 calc R . . C6 C 0.2799(3) 0.5286(3) 0.5379(3) 0.0548(9) Uani 1 1 d . . . C7 C 0.3116(3) 0.4483(3) 0.4873(3) 0.0562(10) Uani 1 1 d . . . C8 C 0.2500(3) 0.4636(3) 0.4150(3) 0.0518(9) Uani 1 1 d . . . C9 C 0.2659(3) 0.3941(3) 0.3555(3) 0.0594(10) Uani 1 1 d . . . C10 C 0.3559(4) 0.3831(4) 0.2840(4) 0.0804(14) Uani 1 1 d . . . H10A H 0.4089 0.4194 0.2739 0.097 Uiso 1 1 calc R . . C11 C 0.3670(5) 0.3192(4) 0.2284(4) 0.0977(19) Uani 1 1 d . . . H11A H 0.4274 0.3135 0.1812 0.117 Uiso 1 1 calc R . . C12 C 0.2922(6) 0.2645(5) 0.2409(5) 0.105(2) Uani 1 1 d . . . H12A H 0.3014 0.2210 0.2034 0.126 Uiso 1 1 calc R . . C13 C 0.2022(5) 0.2740(5) 0.3098(5) 0.1027(19) Uani 1 1 d . . . H13A H 0.1499 0.2373 0.3189 0.123 Uiso 1 1 calc R . . C14 C 0.1900(4) 0.3385(4) 0.3657(4) 0.0807(14) Uani 1 1 d . . . H14A H 0.1286 0.3446 0.4116 0.097 Uiso 1 1 calc R . . C15 C 0.4061(4) 0.3574(4) 0.5231(4) 0.0902(16) Uani 1 1 d . . . H15A H 0.4241 0.3197 0.4756 0.108 Uiso 1 1 calc R . . H15B H 0.4656 0.3887 0.5159 0.108 Uiso 1 1 calc R . . C16 C 0.3914(8) 0.2761(6) 0.6354(6) 0.139(3) Uani 1 1 d . . . H16A H 0.4601 0.2346 0.6573 0.167 Uiso 1 1 calc R . . H16B H 0.3597 0.3146 0.6816 0.167 Uiso 1 1 calc R . . C17 C 0.3337(7) 0.2104(9) 0.6483(8) 0.171(4) Uani 1 1 d . . . H17A H 0.3591 0.1796 0.5951 0.206 Uiso 1 1 calc R . . H17B H 0.2619 0.2503 0.6373 0.206 Uiso 1 1 calc R . . C18 C 0.3337(7) 0.1099(7) 0.7696(7) 0.171(4) Uani 1 1 d . . . H18A H 0.2895 0.0633 0.7751 0.256 Uiso 1 1 calc R . . H18B H 0.3072 0.1398 0.8226 0.256 Uiso 1 1 calc R . . H18C H 0.4044 0.0691 0.7804 0.256 Uiso 1 1 calc R . . C19 C 0.0429(3) 0.8314(3) 0.3078(3) 0.0511(9) Uani 1 1 d . . . C20 C -0.0644(3) 0.8441(3) 0.3460(3) 0.0624(11) Uani 1 1 d . . . H20A H -0.1038 0.7994 0.3439 0.075 Uiso 1 1 calc R . . C21 C -0.1128(4) 0.9220(4) 0.3866(4) 0.0815(14) Uani 1 1 d . . . H21A H -0.1839 0.9284 0.4128 0.098 Uiso 1 1 calc R . . C22 C -0.0559(4) 0.9905(4) 0.3887(4) 0.0856(15) Uani 1 1 d . . . H22A H -0.0890 1.0431 0.4157 0.103 Uiso 1 1 calc R . . C23 C 0.0496(4) 0.9807(4) 0.3510(4) 0.0744(13) Uani 1 1 d . . . H23A H 0.0871 1.0276 0.3516 0.089 Uiso 1 1 calc R . . C24 C 0.1006(3) 0.9013(3) 0.3119(3) 0.0558(10) Uani 1 1 d . . . C25 C 0.2138(3) 0.8818(3) 0.2698(3) 0.0569(10) Uani 1 1 d . . . C26 C 0.2439(3) 0.8018(3) 0.2332(3) 0.0509(9) Uani 1 1 d . . . C27 C 0.3514(3) 0.7746(3) 0.1796(3) 0.0567(10) Uani 1 1 d . . . C28 C 0.3921(4) 0.8519(4) 0.0872(4) 0.0849(15) Uani 1 1 d . . . H28A H 0.3533 0.9224 0.0614 0.102 Uiso 1 1 calc R . . C29 C 0.4893(5) 0.8253(6) 0.0333(5) 0.108(2) Uani 1 1 d . . . H29A H 0.5155 0.8780 -0.0275 0.129 Uiso 1 1 calc R . . C30 C 0.5467(4) 0.7212(6) 0.0695(5) 0.0976(19) Uani 1 1 d . . . H30A H 0.6113 0.7032 0.0327 0.117 Uiso 1 1 calc R . . C31 C 0.5090(4) 0.6440(5) 0.1597(4) 0.0854(15) Uani 1 1 d . . . H31A H 0.5479 0.5734 0.1846 0.103 Uiso 1 1 calc R . . C32 C 0.4120(3) 0.6714(4) 0.2142(3) 0.0668(11) Uani 1 1 d . . . H32A H 0.3874 0.6183 0.2758 0.080 Uiso 1 1 calc R . . C33 C 0.2849(4) 0.9431(4) 0.2821(4) 0.0741(13) Uani 1 1 d . . . H33A H 0.2511 1.0190 0.2600 0.089 Uiso 1 1 calc R . . H33B H 0.3506 0.9373 0.2363 0.089 Uiso 1 1 calc R . . C34 C 0.3086(4) 0.8988(4) 0.3977(4) 0.0723(12) Uani 1 1 d . . . H34A H 0.2424 0.8944 0.4435 0.087 Uiso 1 1 calc R . . H34B H 0.3502 0.8257 0.4156 0.087 Uiso 1 1 calc R . . C35 C 0.3662(5) 0.9628(5) 0.4222(5) 0.0949(17) Uani 1 1 d . . . H35A H 0.3232 1.0347 0.4089 0.114 Uiso 1 1 calc R . . H35B H 0.4312 0.9705 0.3745 0.114 Uiso 1 1 calc R . . C36 C 0.3922(5) 0.9115(6) 0.5356(5) 0.1052(19) Uani 1 1 d . . . H36A H 0.4286 0.9559 0.5467 0.158 Uiso 1 1 calc R . . H36B H 0.4365 0.8411 0.5489 0.158 Uiso 1 1 calc R . . H36C H 0.3282 0.9049 0.5834 0.158 Uiso 1 1 calc R . . O1 O -0.0499(5) 0.7043(4) 0.0715(3) 0.136(2) Uani 1 1 d . . . O2 O -0.1481(6) 0.5597(7) 0.0705(7) 0.214(4) Uani 1 1 d . . . O3 O 0.1852(4) 0.6979(4) -0.0207(3) 0.1171(15) Uani 1 1 d . . . O4 O 0.3859(4) 0.6339(6) -0.1152(4) 0.1406(18) Uani 1 1 d . . . O5 O 0.0285(3) 0.9074(3) -0.0241(3) 0.0831(10) Uani 1 1 d . . . C37 C -0.0867(11) 0.6207(8) 0.1651(7) 0.214(6) Uani 1 1 d . . . H37A H -0.0262 0.5779 0.2036 0.256 Uiso 1 1 calc R . . H37B H -0.1345 0.6558 0.2090 0.256 Uiso 1 1 calc R . . C38 C -0.1255(15) 0.5651(13) 0.1611(8) 0.339(13) Uani 1 1 d . . . H38A H -0.1930 0.5719 0.2041 0.407 Uiso 1 1 calc R . . H38B H -0.0852 0.4939 0.1996 0.407 Uiso 1 1 calc R . . C39 C -0.1138(12) 0.6429(12) -0.0208(8) 0.259(8) Uani 1 1 d . . . H39A H -0.0660 0.6078 -0.0648 0.311 Uiso 1 1 calc R . . H39B H -0.1752 0.6833 -0.0584 0.311 Uiso 1 1 calc R . . C40 C -0.0740(13) 0.7052(9) -0.0222(7) 0.271(9) Uani 1 1 d . . . H40A H -0.1180 0.7754 -0.0569 0.325 Uiso 1 1 calc R . . H40B H -0.0083 0.7019 -0.0684 0.325 Uiso 1 1 calc R . . C41 C 0.2475(5) 0.5916(5) 0.0252(5) 0.109(2) Uani 1 1 d . . . H41A H 0.2319 0.5643 0.1020 0.130 Uiso 1 1 calc R . . H41B H 0.2293 0.5437 0.0010 0.130 Uiso 1 1 calc R . . C42 C 0.3571(6) 0.5917(8) -0.0032(6) 0.142(3) Uani 1 1 d . . . H42A H 0.3761 0.6345 0.0267 0.171 Uiso 1 1 calc R . . H42B H 0.3968 0.5182 0.0277 0.171 Uiso 1 1 calc R . . C43 C 0.3274(10) 0.7384(9) -0.1579(7) 0.171(4) Uani 1 1 d . . . H43A H 0.3453 0.7681 -0.2344 0.205 Uiso 1 1 calc R . . H43B H 0.3456 0.7832 -0.1298 0.205 Uiso 1 1 calc R . . C44 C 0.2116(9) 0.7415(8) -0.1327(5) 0.170(4) Uani 1 1 d . . . H44A H 0.1730 0.8156 -0.1629 0.204 Uiso 1 1 calc R . . H44B H 0.1921 0.6998 -0.1635 0.204 Uiso 1 1 calc R . . C45 C -0.0791(4) 0.9680(4) -0.0212(4) 0.0873(16) Uani 1 1 d . . . H45A H -0.1274 0.9195 0.0006 0.105 Uiso 1 1 calc R . . H45B H -0.0921 1.0219 -0.0918 0.105 Uiso 1 1 calc R . . C46 C 0.0984(4) 0.9785(5) -0.0531(4) 0.0894(16) Uani 1 1 d . . . H46A H 0.0891 1.0327 -0.1244 0.107 Uiso 1 1 calc R . . H46B H 0.1706 0.9381 -0.0534 0.107 Uiso 1 1 calc R . . C47 C 0.0072(3) 0.5436(3) 0.4434(3) 0.0503(9) Uani 1 1 d . . . H47A H -0.0478 0.6073 0.4380 0.060 Uiso 1 1 calc R . . H47B H -0.0027 0.5170 0.3933 0.060 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0471(6) 0.0431(6) 0.0397(5) -0.0131(4) 0.0017(4) -0.0115(4) Si2 0.0498(6) 0.0430(6) 0.0399(5) -0.0121(4) -0.0002(4) -0.0124(4) Li1 0.113(7) 0.058(4) 0.060(4) -0.021(4) -0.014(4) -0.016(4) C1 0.056(2) 0.045(2) 0.0413(19) -0.0105(16) 0.0004(16) -0.0149(17) C2 0.076(3) 0.053(2) 0.046(2) -0.0155(18) -0.0087(19) -0.010(2) C3 0.115(4) 0.060(3) 0.060(3) -0.021(2) -0.017(3) -0.020(3) C4 0.104(4) 0.082(4) 0.068(3) -0.023(3) -0.027(3) -0.031(3) C5 0.067(3) 0.075(3) 0.072(3) -0.017(3) -0.020(2) -0.015(2) C6 0.055(2) 0.049(2) 0.049(2) -0.0087(17) -0.0027(17) -0.0138(18) C7 0.050(2) 0.046(2) 0.052(2) -0.0052(17) 0.0018(18) -0.0068(17) C8 0.052(2) 0.042(2) 0.048(2) -0.0119(17) 0.0069(17) -0.0106(17) C9 0.071(3) 0.040(2) 0.051(2) -0.0130(17) 0.0091(19) -0.0077(19) C10 0.086(3) 0.061(3) 0.081(3) -0.031(2) 0.021(3) -0.014(2) C11 0.125(5) 0.070(3) 0.084(4) -0.040(3) 0.035(3) -0.017(3) C12 0.159(6) 0.071(4) 0.084(4) -0.042(3) 0.013(4) -0.025(4) C13 0.133(5) 0.086(4) 0.106(4) -0.056(4) 0.024(4) -0.048(4) C14 0.098(4) 0.074(3) 0.077(3) -0.041(3) 0.018(3) -0.032(3) C15 0.082(3) 0.074(3) 0.084(3) -0.019(3) -0.012(3) 0.012(3) C16 0.180(8) 0.079(5) 0.113(5) -0.011(4) -0.027(5) 0.006(5) C17 0.147(8) 0.186(10) 0.164(8) -0.032(7) 0.019(6) -0.098(8) C18 0.164(8) 0.136(7) 0.165(8) -0.007(6) 0.018(6) -0.072(6) C19 0.057(2) 0.048(2) 0.0411(19) -0.0126(16) -0.0027(16) -0.0090(17) C20 0.056(2) 0.056(2) 0.062(2) -0.019(2) -0.0031(19) -0.0017(19) C21 0.065(3) 0.086(4) 0.077(3) -0.034(3) 0.005(2) 0.003(3) C22 0.087(4) 0.076(3) 0.093(4) -0.050(3) -0.002(3) 0.008(3) C23 0.088(3) 0.061(3) 0.080(3) -0.038(2) -0.010(3) -0.006(2) C24 0.067(3) 0.047(2) 0.050(2) -0.0177(18) -0.0074(18) -0.0063(19) C25 0.067(3) 0.046(2) 0.053(2) -0.0133(18) -0.0008(19) -0.0191(19) C26 0.055(2) 0.049(2) 0.0415(19) -0.0103(17) -0.0017(16) -0.0133(17) C27 0.053(2) 0.066(3) 0.051(2) -0.0203(19) 0.0012(18) -0.021(2) C28 0.076(3) 0.083(3) 0.072(3) -0.014(3) 0.018(3) -0.027(3) C29 0.094(4) 0.128(6) 0.081(4) -0.028(4) 0.035(3) -0.050(4) C30 0.054(3) 0.148(6) 0.087(4) -0.053(4) 0.016(3) -0.023(3) C31 0.057(3) 0.108(4) 0.083(3) -0.044(3) -0.008(3) 0.005(3) C32 0.061(3) 0.074(3) 0.057(2) -0.020(2) -0.006(2) -0.011(2) C33 0.088(3) 0.060(3) 0.079(3) -0.027(2) 0.000(3) -0.030(2) C34 0.072(3) 0.072(3) 0.080(3) -0.031(3) -0.005(2) -0.028(2) C35 0.104(4) 0.094(4) 0.100(4) -0.040(3) -0.006(3) -0.042(3) C36 0.115(5) 0.123(5) 0.096(4) -0.052(4) -0.021(4) -0.031(4) O1 0.230(5) 0.118(3) 0.085(3) 0.000(2) -0.067(3) -0.102(4) O2 0.274(8) 0.271(9) 0.194(7) -0.125(7) 0.049(6) -0.209(8) O3 0.167(4) 0.099(3) 0.064(2) -0.039(2) -0.012(2) 0.016(3) O4 0.138(4) 0.172(6) 0.105(4) -0.050(4) 0.022(3) -0.056(4) O5 0.093(2) 0.062(2) 0.076(2) -0.0074(16) -0.0141(18) -0.0174(18) C37 0.378(17) 0.190(10) 0.108(6) 0.022(6) -0.083(8) -0.201(11) C38 0.61(3) 0.45(2) 0.128(8) -0.117(12) 0.091(12) -0.46(3) C39 0.42(2) 0.354(18) 0.119(8) -0.100(10) 0.002(10) -0.276(18) C40 0.55(3) 0.217(11) 0.123(7) 0.013(7) -0.154(11) -0.246(15) C41 0.112(5) 0.098(5) 0.103(4) -0.044(4) 0.007(4) -0.011(4) C42 0.120(6) 0.171(8) 0.108(6) -0.025(5) -0.008(5) -0.042(6) C43 0.209(11) 0.149(9) 0.101(6) 0.000(6) 0.010(7) -0.060(9) C44 0.247(11) 0.159(8) 0.070(4) -0.051(5) -0.033(6) 0.033(8) C45 0.089(4) 0.067(3) 0.092(4) -0.004(3) -0.032(3) -0.023(3) C46 0.074(3) 0.081(4) 0.084(4) -0.008(3) -0.001(3) -0.016(3) C47 0.054(2) 0.047(2) 0.0399(19) -0.0082(16) 0.0025(16) -0.0150(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 C1 1.871(4) . ? Si1 C8 1.888(4) . ? Si1 C47 1.889(4) . ? Si1 Si2 2.3501(14) . ? Si2 C19 1.896(4) . ? Si2 C26 1.899(4) . ? Si2 Li1 2.645(8) . ? Li1 O3 1.917(10) . ? Li1 O5 1.939(8) . ? Li1 O1 1.944(10) . ? C1 C2 1.395(5) . ? C1 C6 1.410(5) . ? C2 C3 1.381(6) . ? C3 C4 1.372(7) . ? C4 C5 1.375(7) . ? C5 C6 1.397(6) . ? C6 C7 1.494(6) . ? C7 C8 1.349(6) . ? C7 C15 1.513(6) . ? C8 C9 1.480(6) . ? C9 C14 1.383(6) . ? C9 C10 1.402(6) . ? C10 C11 1.379(7) . ? C11 C12 1.352(8) . ? C12 C13 1.378(8) . ? C13 C14 1.386(7) . ? C15 C16 1.504(8) . ? C16 C17 1.283(10) . ? C17 C18 1.679(12) . ? C19 C20 1.400(5) . ? C19 C24 1.422(6) . ? C20 C21 1.383(6) . ? C21 C22 1.386(7) . ? C22 C23 1.375(7) . ? C23 C24 1.391(6) . ? C24 C25 1.486(6) . ? C25 C26 1.352(5) . ? C25 C33 1.515(6) . ? C26 C27 1.491(5) . ? C27 C32 1.377(6) . ? C27 C28 1.398(6) . ? C28 C29 1.388(7) . ? C29 C30 1.372(9) . ? C30 C31 1.366(8) . ? C31 C32 1.392(6) . ? C33 C34 1.536(6) . ? C34 C35 1.503(6) . ? C35 C36 1.512(8) . ? O1 C40 1.411(8) . ? O1 C37 1.431(8) . ? O2 C39 1.401(12) . ? O2 C38 1.402(11) . ? O3 C44 1.420(8) . ? O3 C41 1.429(7) . ? O4 C43 1.387(11) . ? O4 C42 1.424(8) . ? O5 C46 1.419(6) . ? O5 C45 1.448(6) . ? C37 C38 1.069(10) . ? C39 C40 1.127(11) . ? C41 C42 1.422(9) . ? C43 C44 1.493(13) . ? C45 C46 1.468(8) 2_575 ? C46 C45 1.468(8) 2_575 ? C47 C47 1.541(7) 2_566 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Si1 C8 90.62(18) . . ? C1 Si1 C47 112.98(16) . . ? C8 Si1 C47 110.53(17) . . ? C1 Si1 Si2 113.20(12) . . ? C8 Si1 Si2 119.91(12) . . ? C47 Si1 Si2 108.74(12) . . ? C19 Si2 C26 87.84(17) . . ? C19 Si2 Si1 93.46(12) . . ? C26 Si2 Si1 105.26(12) . . ? C19 Si2 Li1 116.7(2) . . ? C26 Si2 Li1 118.8(2) . . ? Si1 Si2 Li1 125.90(18) . . ? O3 Li1 O5 106.0(4) . . ? O3 Li1 O1 106.8(4) . . ? O5 Li1 O1 98.9(4) . . ? O3 Li1 Si2 114.3(4) . . ? O5 Li1 Si2 109.8(3) . . ? O1 Li1 Si2 119.3(4) . . ? C2 C1 C6 119.3(4) . . ? C2 C1 Si1 131.9(3) . . ? C6 C1 Si1 108.4(3) . . ? C3 C2 C1 120.4(4) . . ? C4 C3 C2 120.2(5) . . ? C3 C4 C5 120.8(5) . . ? C4 C5 C6 120.3(5) . . ? C5 C6 C1 119.0(4) . . ? C5 C6 C7 126.0(4) . . ? C1 C6 C7 115.0(4) . . ? C8 C7 C6 115.5(3) . . ? C8 C7 C15 126.4(4) . . ? C6 C7 C15 118.0(4) . . ? C7 C8 C9 124.9(4) . . ? C7 C8 Si1 110.1(3) . . ? C9 C8 Si1 125.0(3) . . ? C14 C9 C10 116.3(4) . . ? C14 C9 C8 121.1(4) . . ? C10 C9 C8 122.6(4) . . ? C11 C10 C9 121.0(5) . . ? C12 C11 C10 121.6(5) . . ? C11 C12 C13 119.1(5) . . ? C12 C13 C14 119.8(6) . . ? C9 C14 C13 122.2(5) . . ? C16 C15 C7 115.3(5) . . ? C17 C16 C15 114.2(8) . . ? C16 C17 C18 112.8(8) . . ? C20 C19 C24 117.9(4) . . ? C20 C19 Si2 131.5(3) . . ? C24 C19 Si2 110.5(3) . . ? C21 C20 C19 121.0(4) . . ? C20 C21 C22 120.4(5) . . ? C23 C22 C21 120.0(5) . . ? C22 C23 C24 120.6(5) . . ? C23 C24 C19 120.0(4) . . ? C23 C24 C25 125.9(4) . . ? C19 C24 C25 114.1(3) . . ? C26 C25 C24 114.7(4) . . ? C26 C25 C33 126.8(4) . . ? C24 C25 C33 118.2(4) . . ? C25 C26 C27 123.7(4) . . ? C25 C26 Si2 112.8(3) . . ? C27 C26 Si2 123.1(3) . . ? C32 C27 C28 116.9(4) . . ? C32 C27 C26 122.0(4) . . ? C28 C27 C26 121.0(4) . . ? C29 C28 C27 121.2(5) . . ? C30 C29 C28 120.1(5) . . ? C29 C30 C31 120.0(5) . . ? C30 C31 C32 119.7(5) . . ? C27 C32 C31 122.1(5) . . ? C25 C33 C34 111.5(4) . . ? C35 C34 C33 116.0(4) . . ? C34 C35 C36 113.2(5) . . ? C40 O1 C37 112.3(6) . . ? C40 O1 Li1 118.9(7) . . ? C37 O1 Li1 121.9(5) . . ? C39 O2 C38 109.6(7) . . ? C44 O3 C41 110.1(5) . . ? C44 O3 Li1 128.9(5) . . ? C41 O3 Li1 120.7(4) . . ? C43 O4 C42 108.1(7) . . ? C46 O5 C45 109.0(4) . . ? C46 O5 Li1 118.8(4) . . ? C45 O5 Li1 124.8(4) . . ? C38 C37 O1 121.9(9) . . ? C37 C38 O2 128.3(10) . . ? C40 C39 O2 125.7(9) . . ? C39 C40 O1 122.1(10) . . ? C42 C41 O3 111.2(6) . . ? O4 C42 C41 112.9(6) . . ? O4 C43 C44 111.8(8) . . ? O3 C44 C43 109.4(7) . . ? O5 C45 C46 110.8(4) . 2_575 ? O5 C46 C45 111.1(4) . 2_575 ? C47 C47 Si1 115.3(3) 2_566 . ? _diffrn_measured_fraction_theta_max 0.925 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.925 _refine_diff_density_max 0.698 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.054