# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/1926 data_apr498 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[SiMe2{CHCHCH(SiMe3)Li(tmeda)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C26 H62 Li2 N4 Si3' _chemical_formula_weight 528.95 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Li' 'Li' -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 17.496(6) _cell_length_b 13.420(7) _cell_length_c 16.247(6) _cell_angle_alpha 90.00 _cell_angle_beta 99.78(3) _cell_angle_gamma 90.00 _cell_volume 3759.3(27) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.935 _exptl_crystal_density_method ? _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.144 _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 3397 _diffrn_reflns_av_R_equivalents 0.0721 _diffrn_reflns_av_sigmaI/netI 0.1363 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 24.97 _reflns_number_total 3293 _reflns_number_observed 1591 _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 ; Allyl H atoms were freely refined; others were in riding mode. Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1184P)^2^+4.8934P] 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 3292 _refine_ls_number_parameters 171 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1909 _refine_ls_R_factor_obs 0.0899 _refine_ls_wR_factor_all 0.2726 _refine_ls_wR_factor_obs 0.2103 _refine_ls_goodness_of_fit_all 1.023 _refine_ls_goodness_of_fit_obs 1.150 _refine_ls_restrained_S_all 1.024 _refine_ls_restrained_S_obs 1.150 _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 -0.1136(5) -0.0971(7) 0.3667(6) 0.045(2) Uani 1 d . . Si1 Si 0.0000 0.0570(2) 0.2500 0.0379(6) Uani 1 d S . Si2 Si 0.01235(11) -0.29715(13) 0.45811(11) 0.0534(6) Uani 1 d . . N1 N -0.1946(3) -0.0357(4) 0.4334(3) 0.0503(13) Uani 1 d . . N2 N -0.2065(3) -0.1502(5) 0.2809(4) 0.066(2) Uani 1 d . . C1 C -0.0100(3) -0.0153(4) 0.3424(4) 0.0393(14) Uani 1 d . . H1 H -0.0261(25) 0.0194(33) 0.3861(27) 0.023(12) Uiso 1 d . . C2 C 0.0070(3) -0.1142(4) 0.3634(3) 0.0381(13) Uani 1 d . . H2 H 0.0229(29) -0.1559(39) 0.3144(31) 0.048(15) Uiso 1 d . . C3 C -0.0068(3) -0.1668(4) 0.4334(4) 0.0434(14) Uani 1 d . . H3 H -0.0184(28) -0.1287(37) 0.4750(28) 0.034(15) Uiso 1 d . . C4 C 0.0844(4) 0.1452(5) 0.2689(4) 0.063(2) Uani 1 d . . H4A H 0.0873(4) 0.1822(5) 0.2175(4) 0.095 Uiso 1 calc R . H4B H 0.1324(4) 0.1075(5) 0.2857(4) 0.095 Uiso 1 calc R . H4C H 0.0775(4) 0.1921(5) 0.3133(4) 0.095 Uiso 1 calc R . C5 C 0.0241(7) -0.3706(6) 0.3652(5) 0.137(4) Uani 1 d . . H5A H 0.0344(7) -0.4403(6) 0.3812(5) 0.205 Uiso 1 calc R . H5B H 0.0677(7) -0.3440(6) 0.3412(5) 0.205 Uiso 1 calc R . H5C H -0.0234(7) -0.3664(6) 0.3236(5) 0.205 Uiso 1 calc R . C6 C -0.0663(6) -0.3521(7) 0.5049(8) 0.160(5) Uani 1 d . . H6A H -0.0548(6) -0.4224(7) 0.5178(8) 0.239 Uiso 1 calc R . H6B H -0.1152(6) -0.3468(7) 0.4656(8) 0.239 Uiso 1 calc R . H6C H -0.0709(6) -0.3163(7) 0.5565(8) 0.239 Uiso 1 calc R . C7 C 0.1024(6) -0.3197(6) 0.5360(7) 0.150(5) Uani 1 d . . H7A H 0.1089(6) -0.3914(6) 0.5461(7) 0.225 Uiso 1 calc R . H7B H 0.0981(6) -0.2858(6) 0.5884(7) 0.225 Uiso 1 calc R . H7C H 0.1473(6) -0.2936(6) 0.5142(7) 0.225 Uiso 1 calc R . C8 C -0.2679(4) -0.0499(7) 0.3771(5) 0.084(2) Uani 1 d . . H8A H -0.3096(4) -0.0557(7) 0.4111(5) 0.101 Uiso 1 calc R . H8B H -0.2786(4) 0.0105(7) 0.3421(5) 0.101 Uiso 1 calc R . C9 C -0.2721(4) -0.1334(7) 0.3238(6) 0.105(3) Uani 1 d . . H9A H -0.3194(4) -0.1268(7) 0.2811(6) 0.126 Uiso 1 calc R . H9B H -0.2786(4) -0.1935(7) 0.3573(6) 0.126 Uiso 1 calc R . C10 C -0.1920(4) -0.0886(6) 0.5127(4) 0.081(2) Uani 1 d . . H10A H -0.1418(4) -0.0769(6) 0.5484(4) 0.122 Uiso 1 calc R . H10B H -0.1989(4) -0.1602(6) 0.5019(4) 0.122 Uiso 1 calc R . H10C H -0.2336(4) -0.0641(6) 0.5408(4) 0.122 Uiso 1 calc R . C11 C -0.1829(4) 0.0705(6) 0.4516(5) 0.082(2) Uani 1 d . . H11A H -0.1335(4) 0.0801(6) 0.4895(5) 0.124 Uiso 1 calc R . H11B H -0.2254(4) 0.0956(6) 0.4780(5) 0.124 Uiso 1 calc R . H11C H -0.1819(4) 0.1069(6) 0.3995(5) 0.124 Uiso 1 calc R . C12 C -0.2024(5) -0.2561(7) 0.2639(6) 0.119(3) Uani 1 d . . H12A H -0.1972(5) -0.2934(7) 0.3164(6) 0.178 Uiso 1 calc R . H12B H -0.1574(5) -0.2695(7) 0.2369(6) 0.178 Uiso 1 calc R . H12C H -0.2498(5) -0.2770(7) 0.2268(6) 0.178 Uiso 1 calc R . C13 C -0.2141(5) -0.0964(8) 0.2041(5) 0.123(4) Uani 1 d . . H13A H -0.2169(5) -0.0248(8) 0.2154(5) 0.184 Uiso 1 calc R . H13B H -0.2615(5) -0.1174(8) 0.1671(5) 0.184 Uiso 1 calc R . H13C H -0.1691(5) -0.1099(8) 0.1772(5) 0.184 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 Li 0.033(5) 0.051(6) 0.051(5) 0.000(5) 0.007(4) -0.007(4) Si1 0.0336(12) 0.0317(12) 0.0486(13) 0.000 0.0074(10) 0.000 Si2 0.0579(12) 0.0438(10) 0.0587(11) 0.0097(9) 0.0104(9) 0.0024(9) N1 0.035(3) 0.064(4) 0.052(3) -0.003(3) 0.007(2) -0.003(2) N2 0.041(3) 0.077(4) 0.078(4) -0.021(3) 0.005(3) -0.025(3) C1 0.031(3) 0.041(3) 0.047(3) -0.008(3) 0.011(3) -0.005(3) C2 0.029(3) 0.040(3) 0.043(3) 0.000(3) 0.001(2) -0.001(2) C3 0.049(4) 0.041(3) 0.040(3) 0.001(3) 0.006(3) 0.002(3) C4 0.065(4) 0.056(4) 0.069(4) -0.002(3) 0.014(3) -0.023(4) C5 0.248(13) 0.073(6) 0.094(6) 0.015(5) 0.044(7) 0.052(7) C6 0.139(9) 0.085(7) 0.284(14) 0.093(8) 0.117(10) 0.033(6) C7 0.137(9) 0.068(6) 0.207(11) 0.031(7) -0.080(8) 0.012(6) C8 0.039(4) 0.132(7) 0.081(5) -0.022(5) 0.004(4) -0.008(5) C9 0.039(4) 0.132(8) 0.142(8) -0.061(7) 0.005(5) -0.028(5) C10 0.078(5) 0.102(6) 0.070(5) 0.011(4) 0.030(4) 0.006(5) C11 0.060(5) 0.078(6) 0.109(6) -0.006(5) 0.018(4) 0.008(4) C12 0.104(7) 0.102(7) 0.146(9) -0.048(7) 0.007(6) -0.043(6) C13 0.075(6) 0.197(11) 0.081(6) 0.021(7) -0.028(5) -0.049(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li N2 2.079(10) . ? Li N1 2.093(10) . ? Li C2 2.131(10) . ? Li C3 2.202(11) . ? Li C1 2.210(10) . ? Li C9 2.785(11) . ? Si1 C1 1.820(6) . ? Si1 C1 1.820(6) 6_556 ? Si1 C4 1.877(6) . ? Si1 C4 1.877(6) 6_556 ? Si2 C3 1.814(6) . ? Si2 C6 1.837(9) . ? Si2 C5 1.844(8) . ? Si2 C7 1.870(8) . ? N1 C8 1.456(8) . ? N1 C11 1.463(8) . ? N1 C10 1.465(8) . ? N2 C13 1.428(9) . ? N2 C12 1.452(10) . ? N2 C9 1.458(9) . ? C1 C2 1.390(8) . ? C2 C3 1.395(8) . ? C8 C9 1.410(10) . ? 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 N2 Li N1 87.7(4) . . ? N2 Li C2 127.6(5) . . ? N1 Li C2 144.6(5) . . ? N2 Li C3 133.3(5) . . ? N1 Li C3 120.3(5) . . ? C2 Li C3 37.5(3) . . ? N2 Li C1 128.5(5) . . ? N1 Li C1 123.0(5) . . ? C2 Li C1 37.3(2) . . ? C3 Li C1 69.3(3) . . ? N2 Li C9 30.7(2) . . ? N1 Li C9 57.7(3) . . ? C2 Li C9 157.3(5) . . ? C3 Li C9 140.7(5) . . ? C1 Li C9 148.6(5) . . ? C1 Si1 C1 115.7(4) . 6_556 ? C1 Si1 C4 112.6(3) . . ? C1 Si1 C4 106.7(3) 6_556 . ? C1 Si1 C4 106.7(3) . 6_556 ? C1 Si1 C4 112.6(3) 6_556 6_556 ? C4 Si1 C4 101.7(4) . 6_556 ? C3 Si2 C6 110.8(4) . . ? C3 Si2 C5 112.1(3) . . ? C6 Si2 C5 108.7(6) . . ? C3 Si2 C7 114.1(3) . . ? C6 Si2 C7 105.0(5) . . ? C5 Si2 C7 105.6(5) . . ? C8 N1 C11 109.4(6) . . ? C8 N1 C10 112.4(6) . . ? C11 N1 C10 108.2(6) . . ? C8 N1 Li 103.0(5) . . ? C11 N1 Li 113.9(5) . . ? C10 N1 Li 110.0(5) . . ? C13 N2 C12 109.2(7) . . ? C13 N2 C9 112.0(7) . . ? C12 N2 C9 108.1(6) . . ? C13 N2 Li 111.0(5) . . ? C12 N2 Li 113.9(6) . . ? C9 N2 Li 102.4(5) . . ? C2 C1 Si1 131.6(5) . . ? C2 C1 Li 68.3(4) . . ? Si1 C1 Li 127.5(4) . . ? C1 C2 C3 128.6(6) . . ? C1 C2 Li 74.4(4) . . ? C3 C2 Li 74.0(4) . . ? C2 C3 Si2 128.1(5) . . ? C2 C3 Li 68.5(4) . . ? Si2 C3 Li 128.9(4) . . ? C9 C8 N1 115.9(7) . . ? C8 C9 N2 117.0(6) . . ? C8 C9 Li 76.2(4) . . ? N2 C9 Li 46.8(3) . . ? _refine_diff_density_max 0.482 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.063 #==END data_may898 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural '[Zr{Me3Si(CH)3SiMe2(CH)3SiMe3)}2]' _chemical_formula_analytical ? _chemical_formula_sum 'C28 H60 Si6 Zr' _chemical_formula_weight 656.52 _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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' '-x, -y, -z' '-x, y, -z-1/2' '-x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z-1/2' _cell_length_a 11.512(2) _cell_length_b 17.267(3) _cell_length_c 19.367(2) _cell_angle_alpha 90.00 _cell_angle_beta 103.39(2) _cell_angle_gamma 90.00 _cell_volume 3745.1(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method ? _exptl_crystal_F_000 1408 _exptl_absorpt_coefficient_mu 0.501 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.91 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 4830 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.1037 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.16 _diffrn_reflns_theta_max 28.34 _reflns_number_total 4622 _reflns_number_observed 2835 _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 allyl H atoms were freely refined isotropic; other H atoms were in riding mode. 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^)+(0.0650P)^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_number_reflns 4622 _refine_ls_number_parameters 183 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1216 _refine_ls_R_factor_obs 0.0627 _refine_ls_wR_factor_all 0.1661 _refine_ls_wR_factor_obs 0.1357 _refine_ls_goodness_of_fit_all 1.043 _refine_ls_goodness_of_fit_obs 1.096 _refine_ls_restrained_S_all 1.043 _refine_ls_restrained_S_obs 1.096 _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 Zr Zr 0.0000 0.17604(4) 0.2500 0.0312(2) Uani 1 d S . Si1 Si 0.16607(14) 0.05666(9) 0.11641(8) 0.0515(4) Uani 1 d . . Si2 Si -0.23226(13) 0.16099(9) 0.12958(8) 0.0502(4) Uani 1 d . . Si3 Si -0.17613(15) 0.32434(10) 0.34868(8) 0.0556(4) Uani 1 d . . C1 C 0.0353(4) 0.1020(3) 0.1401(3) 0.0405(11) Uani 1 d . . H1 H 0.0049(40) 0.1402(27) 0.1157(23) 0.034(13) Uiso 1 d . . C2 C -0.0426(5) 0.0598(3) 0.1698(3) 0.0409(11) Uani 1 d . . H2 H -0.0190(38) 0.0174(26) 0.1847(22) 0.029(12) Uiso 1 d . . C3 C -0.1488(5) 0.0843(3) 0.1841(3) 0.0440(12) Uani 1 d . . H3 H -0.1740(45) 0.0538(29) 0.2099(26) 0.047(16) Uiso 1 d . . C4 C -0.1379(5) 0.2477(3) 0.1532(3) 0.0458(12) Uani 1 d . . H4 H -0.1016(56) 0.2717(37) 0.1247(34) 0.091(23) Uiso 1 d . . C5 C -0.1383(5) 0.2896(3) 0.2123(3) 0.0457(12) Uani 1 d . . H5 H -0.1111(44) 0.3412(29) 0.2127(26) 0.048(15) Uiso 1 d . . C6 C -0.1564(5) 0.2612(3) 0.2757(3) 0.0454(12) Uani 1 d . . H6 H -0.2034(42) 0.2191(28) 0.2655(25) 0.046(14) Uiso 1 d . . C7 C 0.1702(6) -0.0473(3) 0.1392(3) 0.071(2) Uani 1 d . . H7C H 0.2382(6) -0.0710(3) 0.1269(3) 0.107 Uiso 1 calc R . H7B H 0.0985(6) -0.0718(3) 0.1133(3) 0.107 Uiso 1 calc R . H7A H 0.1762(6) -0.0530(3) 0.1892(3) 0.107 Uiso 1 calc R . C8 C 0.1492(6) 0.0660(4) 0.0190(3) 0.075(2) Uani 1 d . . H8C H 0.1469(6) 0.1198(4) 0.0063(3) 0.113 Uiso 1 calc R . H8B H 0.0763(6) 0.0414(4) -0.0053(3) 0.113 Uiso 1 calc R . H8A H 0.2156(6) 0.0415(4) 0.0056(3) 0.113 Uiso 1 calc R . C9 C 0.3145(5) 0.0965(4) 0.1601(4) 0.088(2) Uani 1 d . . H9C H 0.3167(5) 0.1508(4) 0.1498(4) 0.132 Uiso 1 calc R . H9B H 0.3753(5) 0.0701(4) 0.1427(4) 0.132 Uiso 1 calc R . H9A H 0.3282(5) 0.0893(4) 0.2105(4) 0.132 Uiso 1 calc R . C10 C -0.3850(5) 0.1734(4) 0.1457(4) 0.083(2) Uani 1 d . . H10C H -0.4258(5) 0.2142(4) 0.1160(4) 0.125 Uiso 1 calc R . H10B H -0.3787(5) 0.1864(4) 0.1946(4) 0.125 Uiso 1 calc R . H10A H -0.4290(5) 0.1260(4) 0.1347(4) 0.125 Uiso 1 calc R . C11 C -0.2501(6) 0.1399(4) 0.0330(3) 0.075(2) Uani 1 d . . H11C H -0.2943(6) 0.1810(4) 0.0054(3) 0.113 Uiso 1 calc R . H11B H -0.2925(6) 0.0919(4) 0.0215(3) 0.113 Uiso 1 calc R . H11A H -0.1729(6) 0.1358(4) 0.0225(3) 0.113 Uiso 1 calc R . C12 C -0.1268(6) 0.2814(4) 0.4383(3) 0.073(2) Uani 1 d . . H12C H -0.1688(6) 0.2338(4) 0.4404(3) 0.109 Uiso 1 calc R . H12B H -0.1433(6) 0.3169(4) 0.4730(3) 0.109 Uiso 1 calc R . H12A H -0.0425(6) 0.2714(4) 0.4481(3) 0.109 Uiso 1 calc R . C13 C -0.3389(6) 0.3463(4) 0.3342(4) 0.080(2) Uani 1 d . . H13C H -0.3824(6) 0.2990(4) 0.3347(4) 0.120 Uiso 1 calc R . H13B H -0.3661(6) 0.3715(4) 0.2892(4) 0.120 Uiso 1 calc R . H13A H -0.3518(6) 0.3797(4) 0.3714(4) 0.120 Uiso 1 calc R . C14 C -0.0930(7) 0.4151(4) 0.3478(4) 0.083(2) Uani 1 d . . H14C H -0.1037(7) 0.4477(4) 0.3860(4) 0.125 Uiso 1 calc R . H14B H -0.1222(7) 0.4411(4) 0.3034(4) 0.125 Uiso 1 calc R . H14A H -0.0097(7) 0.4037(4) 0.3535(4) 0.125 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 Zr 0.0301(3) 0.0298(3) 0.0339(3) 0.000 0.0080(2) 0.000 Si1 0.0514(9) 0.0528(9) 0.0559(9) -0.0047(7) 0.0241(7) 0.0032(7) Si2 0.0390(8) 0.0581(10) 0.0489(8) -0.0031(7) 0.0010(6) 0.0019(7) Si3 0.0653(10) 0.0501(9) 0.0547(9) -0.0070(8) 0.0207(7) 0.0134(8) C1 0.043(3) 0.037(3) 0.042(3) 0.000(2) 0.010(2) -0.002(2) C2 0.043(3) 0.033(3) 0.044(3) -0.006(2) 0.005(2) -0.001(2) C3 0.042(3) 0.048(3) 0.042(3) 0.002(2) 0.010(2) -0.005(2) C4 0.045(3) 0.052(3) 0.039(3) 0.006(2) 0.007(2) 0.013(2) C5 0.040(3) 0.046(3) 0.050(3) 0.008(3) 0.008(2) 0.013(2) C6 0.041(3) 0.042(3) 0.054(3) 0.002(2) 0.014(2) 0.005(2) C7 0.089(5) 0.061(4) 0.069(4) 0.004(3) 0.028(3) 0.023(3) C8 0.108(6) 0.071(4) 0.057(4) -0.001(3) 0.040(4) 0.000(4) C9 0.048(4) 0.105(6) 0.118(6) -0.027(5) 0.035(4) -0.007(4) C10 0.036(3) 0.100(5) 0.108(5) 0.008(4) 0.006(3) 0.003(4) C11 0.088(5) 0.074(4) 0.050(3) 0.000(3) -0.011(3) 0.004(4) C12 0.089(5) 0.080(5) 0.050(3) -0.003(3) 0.020(3) 0.022(4) C13 0.071(4) 0.091(5) 0.084(5) -0.010(4) 0.029(4) 0.030(4) C14 0.112(6) 0.053(4) 0.086(5) -0.010(3) 0.027(4) 0.009(4) _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 Zr C3 2.462(5) . ? Zr C3 2.462(5) 6_556 ? Zr C6 2.462(5) 6_556 ? Zr C6 2.462(5) . ? Zr C4 2.488(5) 6_556 ? Zr C4 2.488(5) . ? Zr C2 2.516(5) . ? Zr C2 2.516(5) 6_556 ? Zr C5 2.525(5) 6_556 ? Zr C5 2.525(5) . ? Zr C1 2.594(5) . ? Zr C1 2.594(5) 6_556 ? Si1 C7 1.846(6) . ? Si1 C1 1.846(5) . ? Si1 C9 1.854(6) . ? Si1 C8 1.859(6) . ? Si2 C3 1.822(6) . ? Si2 C4 1.844(6) . ? Si2 C10 1.868(6) . ? Si2 C11 1.870(6) . ? Si3 C14 1.838(7) . ? Si3 C6 1.841(5) . ? Si3 C12 1.852(6) . ? Si3 C13 1.868(6) . ? C1 C2 1.381(7) . ? C2 C3 1.381(7) . ? C4 C5 1.355(7) . ? C5 C6 1.382(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C3 Zr C3 99.9(3) . 6_556 ? C3 Zr C6 137.1(2) . 6_556 ? C3 Zr C6 92.0(2) 6_556 6_556 ? C3 Zr C6 92.0(2) . . ? C3 Zr C6 137.1(2) 6_556 . ? C6 Zr C6 106.7(3) 6_556 . ? C3 Zr C4 163.1(2) . 6_556 ? C3 Zr C4 71.5(2) 6_556 6_556 ? C6 Zr C4 59.1(2) 6_556 6_556 ? C6 Zr C4 85.4(2) . 6_556 ? C3 Zr C4 71.5(2) . . ? C3 Zr C4 163.1(2) 6_556 . ? C6 Zr C4 85.4(2) 6_556 . ? C6 Zr C4 59.1(2) . . ? C4 Zr C4 120.3(3) 6_556 . ? C3 Zr C2 32.2(2) . . ? C3 Zr C2 79.6(2) 6_556 . ? C6 Zr C2 113.5(2) 6_556 . ? C6 Zr C2 123.6(2) . . ? C4 Zr C2 149.5(2) 6_556 . ? C4 Zr C2 86.1(2) . . ? C3 Zr C2 79.6(2) . 6_556 ? C3 Zr C2 32.2(2) 6_556 6_556 ? C6 Zr C2 123.6(2) 6_556 6_556 ? C6 Zr C2 113.5(2) . 6_556 ? C4 Zr C2 86.1(2) 6_556 6_556 ? C4 Zr C2 149.5(2) . 6_556 ? C2 Zr C2 74.1(2) . 6_556 ? C3 Zr C5 165.0(2) . 6_556 ? C3 Zr C5 91.9(2) 6_556 6_556 ? C6 Zr C5 32.1(2) 6_556 6_556 ? C6 Zr C5 85.4(2) . 6_556 ? C4 Zr C5 31.4(2) 6_556 6_556 ? C4 Zr C5 94.6(2) . 6_556 ? C2 Zr C5 144.9(2) . 6_556 ? C2 Zr C5 114.9(2) 6_556 6_556 ? C3 Zr C5 91.9(2) . . ? C3 Zr C5 165.0(2) 6_556 . ? C6 Zr C5 85.4(2) 6_556 . ? C6 Zr C5 32.1(2) . . ? C4 Zr C5 94.6(2) 6_556 . ? C4 Zr C5 31.4(2) . . ? C2 Zr C5 114.9(2) . . ? C2 Zr C5 144.9(2) 6_556 . ? C5 Zr C5 78.1(3) 6_556 . ? C3 Zr C1 58.7(2) . . ? C3 Zr C1 83.5(2) 6_556 . ? C6 Zr C1 82.4(2) 6_556 . ? C6 Zr C1 136.1(2) . . ? C4 Zr C1 132.0(2) 6_556 . ? C4 Zr C1 79.7(2) . . ? C2 Zr C1 31.3(2) . . ? C2 Zr C1 93.9(2) 6_556 . ? C5 Zr C1 114.3(2) 6_556 . ? C5 Zr C1 110.7(2) . . ? C3 Zr C1 83.5(2) . 6_556 ? C3 Zr C1 58.7(2) 6_556 6_556 ? C6 Zr C1 136.1(2) 6_556 6_556 ? C6 Zr C1 82.4(2) . 6_556 ? C4 Zr C1 79.7(2) 6_556 6_556 ? C4 Zr C1 132.0(2) . 6_556 ? C2 Zr C1 93.9(2) . 6_556 ? C2 Zr C1 31.3(2) 6_556 6_556 ? C5 Zr C1 110.7(2) 6_556 6_556 ? C5 Zr C1 114.3(2) . 6_556 ? C1 Zr C1 120.9(2) . 6_556 ? C7 Si1 C1 109.3(3) . . ? C7 Si1 C9 106.3(3) . . ? C1 Si1 C9 116.6(3) . . ? C7 Si1 C8 108.5(3) . . ? C1 Si1 C8 108.4(3) . . ? C9 Si1 C8 107.5(3) . . ? C3 Si2 C4 104.2(2) . . ? C3 Si2 C10 112.2(3) . . ? C4 Si2 C10 112.8(3) . . ? C3 Si2 C11 111.0(3) . . ? C4 Si2 C11 109.2(3) . . ? C10 Si2 C11 107.4(3) . . ? C3 Si2 Zr 51.9(2) . . ? C4 Si2 Zr 52.7(2) . . ? C10 Si2 Zr 122.8(2) . . ? C11 Si2 Zr 129.8(2) . . ? C14 Si3 C6 109.9(3) . . ? C14 Si3 C12 107.6(3) . . ? C6 Si3 C12 114.7(3) . . ? C14 Si3 C13 109.4(3) . . ? C6 Si3 C13 107.7(3) . . ? C12 Si3 C13 107.5(3) . . ? C2 C1 Si1 121.7(4) . . ? C2 C1 Zr 71.2(3) . . ? Si1 C1 Zr 134.8(2) . . ? C3 C2 C1 127.7(5) . . ? C3 C2 Zr 71.8(3) . . ? C1 C2 Zr 77.5(3) . . ? C2 C3 Si2 118.7(4) . . ? C2 C3 Zr 76.1(3) . . ? Si2 C3 Zr 92.5(2) . . ? C5 C4 Si2 121.7(5) . . ? C5 C4 Zr 75.8(3) . . ? Si2 C4 Zr 91.1(2) . . ? C4 C5 C6 126.2(6) . . ? C4 C5 Zr 72.8(3) . . ? C6 C5 Zr 71.4(3) . . ? C5 C6 Si3 122.8(4) . . ? C5 C6 Zr 76.4(3) . . ? Si3 C6 Zr 137.3(3) . . ? _refine_diff_density_max 0.477 _refine_diff_density_min -0.357 _refine_diff_density_rms 0.091 #===END