# Supplementary Material (ESI) for ChemComm # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 182/1520 # Reactions of Permethylmetallocene Alkyne Complexes of # Titanium and Zirconium with Tris(perfluorphenyl)borane data_207 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C38 H29 B F15 Ti' _chemical_formula_weight 829.32 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ti' 'Ti' 0.2776 0.4457 '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 37.705(8) _cell_length_b 10.990(2) _cell_length_c 18.178(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.48(3) _cell_angle_gamma 90.00 _cell_volume 7223.1(26) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _exptl_crystal_description PRISM _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.525 _exptl_crystal_density_method ? _exptl_crystal_F_000 3352 _exptl_absorpt_coefficient_mu 0.343 _exptl_absorpt_correction_type NO _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 STOE-IPDS _diffrn_measurement_method 'LASER SCANNED IMAGING PLATE' _diffrn_standards_number 50-200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 360 _diffrn_standards_decay_% ? _diffrn_reflns_number 10465 _diffrn_reflns_av_R_equivalents 0.0468 _diffrn_reflns_av_sigmaI/netI 0.1182 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.94 _diffrn_reflns_theta_max 24.32 _reflns_number_total 5758 _reflns_number_observed 2868 _reflns_observed_criterion >2sigma(I) _computing_data_collection STOE-EXPOSE _computing_cell_refinement STOE-CELL _computing_data_reduction STOE-INTEGRATE _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _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^)+(0.0502P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5758 _refine_ls_number_parameters 496 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1184 _refine_ls_R_factor_obs 0.0523 _refine_ls_wR_factor_all 0.1159 _refine_ls_wR_factor_obs 0.1027 _refine_ls_goodness_of_fit_all 0.845 _refine_ls_goodness_of_fit_obs 1.110 _refine_ls_restrained_S_all 0.845 _refine_ls_restrained_S_obs 1.110 _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 C1 C 0.39712(13) -0.0298(4) 0.6007(3) 0.0510(12) Uani 1 d . . C2 C 0.41932(12) 0.0615(4) 0.6466(3) 0.0516(13) Uani 1 d . . C3 C 0.40221(14) 0.0950(4) 0.7043(3) 0.0562(13) Uani 1 d . . C4 C 0.36997(13) 0.0246(5) 0.6930(3) 0.0577(14) Uani 1 d . . C5 C 0.36653(13) -0.0522(4) 0.6289(3) 0.0562(13) Uani 1 d . . C6 C 0.33907(14) -0.1545(5) 0.6015(3) 0.083(2) Uani 1 d . . H6A H 0.32071(14) -0.1517(5) 0.6288(3) 0.125 Uiso 1 calc R . H6B H 0.35177(14) -0.2311(5) 0.6109(3) 0.125 Uiso 1 calc R . H6C H 0.32731(14) -0.1455(5) 0.5476(3) 0.125 Uiso 1 calc R . C7 C 0.33044(10) 0.2488(4) 0.4836(2) 0.0310(10) Uani 1 d . . C8 C 0.31019(10) 0.1383(4) 0.4848(2) 0.0371(10) Uani 1 d . . C9 C 0.29571(10) 0.1444(4) 0.5479(2) 0.0439(11) Uani 1 d . . C10 C 0.30653(11) 0.2568(4) 0.5856(2) 0.0444(12) Uani 1 d . . C11 C 0.32662(10) 0.3228(4) 0.5453(2) 0.0366(11) Uani 1 d . . C12 C 0.33929(11) 0.4517(4) 0.5658(3) 0.0515(13) Uani 1 d . . H12A H 0.35256(11) 0.4802(4) 0.5313(3) 0.077 Uiso 1 calc R . H12B H 0.35520(11) 0.4540(4) 0.6174(3) 0.077 Uiso 1 calc R . H12C H 0.31818(11) 0.5028(4) 0.5618(3) 0.077 Uiso 1 calc R . C13 C 0.36206(10) 0.2438(4) 0.4477(2) 0.0371(10) Uani 1 d . . H13A H 0.35405(10) 0.1901(4) 0.4037(2) 0.045 Uiso 1 calc R . H13B H 0.38217(10) 0.2023(4) 0.4844(2) 0.045 Uiso 1 calc R . C14 C 0.31483(11) 0.4068(4) 0.3219(2) 0.0389(11) Uani 1 d . . C15 C 0.28216(12) 0.4674(4) 0.2897(3) 0.0473(12) Uani 1 d . . C16 C 0.27825(12) 0.5833(4) 0.3123(3) 0.0488(12) Uani 1 d . . C17 C 0.30703(13) 0.6374(4) 0.3656(3) 0.0496(12) Uani 1 d . . C18 C 0.33908(12) 0.5721(4) 0.3963(3) 0.0433(11) Uani 1 d . . C19 C 0.34490(11) 0.4537(4) 0.3776(2) 0.0381(11) Uani 1 d . . C20 C 0.42800(11) 0.2214(4) 0.3755(3) 0.0435(11) Uani 1 d . . C21 C 0.40185(11) 0.3130(4) 0.3552(3) 0.0382(11) Uani 1 d . . C22 C 0.39738(11) 0.3553(4) 0.2816(3) 0.0483(12) Uani 1 d . . C23 C 0.41620(13) 0.3117(5) 0.2324(3) 0.0509(13) Uani 1 d . . C24 C 0.44144(13) 0.2221(5) 0.2560(3) 0.0528(13) Uani 1 d . . C25 C 0.44733(11) 0.1752(4) 0.3273(3) 0.0506(13) Uani 1 d . . C26 C 0.40614(15) -0.0941(5) 0.5351(3) 0.075(2) Uani 1 d . . H26A H 0.42850(15) -0.0610(5) 0.5280(3) 0.113 Uiso 1 calc R . H26B H 0.38624(15) -0.0829(5) 0.4891(3) 0.113 Uiso 1 calc R . H26C H 0.40943(15) -0.1794(5) 0.5464(3) 0.113 Uiso 1 calc R . C27 C 0.30434(12) 0.0388(4) 0.4256(3) 0.0521(13) Uani 1 d . . H27A H 0.31749(12) 0.0582(4) 0.3890(3) 0.078 Uiso 1 calc R . H27B H 0.27843(12) 0.0314(4) 0.3998(3) 0.078 Uiso 1 calc R . H27C H 0.31338(12) -0.0368(4) 0.4504(3) 0.078 Uiso 1 calc R . C28 C 0.43516(12) 0.5206(5) 0.4670(3) 0.0561(13) Uani 1 d . . C29 C 0.41354(11) 0.4302(4) 0.4855(3) 0.0450(12) Uani 1 d . . C30 C 0.42532(11) 0.4015(4) 0.5625(3) 0.0471(12) Uani 1 d . . C31 C 0.45493(13) 0.4535(5) 0.6169(3) 0.066(2) Uani 1 d . . C32 C 0.47456(13) 0.5427(5) 0.5932(4) 0.074(2) Uani 1 d . . C33 C 0.46440(14) 0.5783(5) 0.5189(4) 0.072(2) Uani 1 d . . C34 C 0.29412(14) 0.3030(5) 0.6531(3) 0.076(2) Uani 1 d . . H34A H 0.28079(14) 0.2399(5) 0.6704(3) 0.114 Uiso 1 calc R . H34B H 0.27834(14) 0.3724(5) 0.6374(3) 0.114 Uiso 1 calc R . H34C H 0.31537(14) 0.3257(5) 0.6941(3) 0.114 Uiso 1 calc R . C35 C 0.45670(12) 0.1047(5) 0.6418(3) 0.070(2) Uani 1 d . . H35A H 0.46577(12) 0.1672(5) 0.6794(3) 0.106 Uiso 1 calc R . H35B H 0.45434(12) 0.1367(5) 0.5915(3) 0.106 Uiso 1 calc R . H35C H 0.47372(12) 0.0377(5) 0.6516(3) 0.106 Uiso 1 calc R . C36 C 0.4174(2) 0.1843(6) 0.7689(3) 0.099(2) Uani 1 d . . H36A H 0.4397(2) 0.2202(6) 0.7632(3) 0.149 Uiso 1 calc R . H36B H 0.4227(2) 0.1425(6) 0.8172(3) 0.149 Uiso 1 calc R . H36C H 0.3995(2) 0.2470(6) 0.7673(3) 0.149 Uiso 1 calc R . C37 C 0.26808(12) 0.0579(5) 0.5649(3) 0.070(2) Uani 1 d . . H37A H 0.26279(12) 0.0823(5) 0.6114(3) 0.106 Uiso 1 calc R . H37B H 0.27812(12) -0.0229(5) 0.5709(3) 0.106 Uiso 1 calc R . H37C H 0.24570(12) 0.0592(5) 0.5233(3) 0.106 Uiso 1 calc R . C38 C 0.3462(2) 0.0194(6) 0.7470(3) 0.100(2) Uani 1 d . . H38A H 0.3258(2) -0.0349(6) 0.7268(3) 0.150 Uiso 1 calc R . H38B H 0.3370(2) 0.0992(6) 0.7525(3) 0.150 Uiso 1 calc R . H38C H 0.3607(2) -0.0095(6) 0.7962(3) 0.150 Uiso 1 calc R . B B 0.38062(12) 0.3634(4) 0.4181(3) 0.0374(12) Uani 1 d . . F1 F 0.31682(6) 0.2924(2) 0.29476(14) 0.0567(7) Uani 1 d . . F7 F 0.25431(7) 0.4141(2) 0.2365(2) 0.0741(9) Uani 1 d . . F8 F 0.24641(7) 0.6428(3) 0.2825(2) 0.0825(9) Uani 1 d . . F6 F 0.30405(8) 0.7513(2) 0.3877(2) 0.0895(10) Uani 1 d . . F4 F 0.36594(7) 0.6339(2) 0.4488(2) 0.0686(8) Uani 1 d . . F2 F 0.43638(7) 0.1728(2) 0.4468(2) 0.0670(8) Uani 1 d . . F12 F 0.47222(8) 0.0868(3) 0.3518(2) 0.0873(10) Uani 1 d . . F5 F 0.46065(8) 0.1827(3) 0.2082(2) 0.0871(10) Uani 1 d . . F3 F 0.40987(8) 0.3598(3) 0.1617(2) 0.0814(9) Uani 1 d . . F11 F 0.37366(7) 0.4486(3) 0.2533(2) 0.0706(8) Uani 1 d . . F9 F 0.42629(8) 0.5615(2) 0.3935(2) 0.0777(9) Uani 1 d . . F10 F 0.48310(9) 0.6671(3) 0.4946(2) 0.1128(13) Uani 1 d . . F14 F 0.50314(9) 0.5962(3) 0.6448(2) 0.1308(15) Uani 1 d . . F13 F 0.46366(8) 0.4204(3) 0.6906(2) 0.0974(11) Uani 1 d . . F15 F 0.40667(6) 0.3167(2) 0.59464(14) 0.0563(7) Uani 1 d . . Ti Ti 0.36333(2) 0.15260(7) 0.58460(4) 0.0399(2) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.054(3) 0.046(3) 0.047(3) 0.007(3) 0.005(3) 0.014(2) C2 0.041(3) 0.054(3) 0.051(3) 0.012(3) -0.002(2) 0.020(2) C3 0.064(3) 0.062(3) 0.033(3) 0.006(3) -0.002(3) 0.019(3) C4 0.053(3) 0.077(4) 0.043(3) 0.022(3) 0.014(3) 0.018(3) C5 0.050(3) 0.049(3) 0.061(4) 0.022(3) 0.002(3) 0.012(2) C6 0.064(3) 0.067(4) 0.109(5) 0.029(4) 0.009(3) 0.001(3) C7 0.028(2) 0.039(2) 0.023(2) -0.001(2) 0.002(2) 0.007(2) C8 0.029(2) 0.038(3) 0.039(3) 0.001(2) 0.001(2) 0.002(2) C9 0.029(2) 0.059(3) 0.046(3) 0.013(3) 0.014(2) 0.009(2) C10 0.037(3) 0.060(3) 0.038(3) 0.001(3) 0.014(2) 0.019(2) C11 0.025(2) 0.043(3) 0.038(3) 0.001(2) 0.002(2) 0.013(2) C12 0.045(3) 0.051(3) 0.055(3) -0.013(3) 0.009(2) 0.011(2) C13 0.034(2) 0.044(3) 0.030(2) -0.006(2) 0.003(2) 0.000(2) C14 0.040(3) 0.028(2) 0.046(3) 0.004(2) 0.008(2) 0.001(2) C15 0.039(3) 0.050(3) 0.052(3) 0.010(3) 0.009(2) -0.003(2) C16 0.042(3) 0.051(3) 0.056(3) 0.022(3) 0.019(3) 0.018(3) C17 0.063(3) 0.028(3) 0.061(3) 0.004(2) 0.023(3) 0.018(3) C18 0.048(3) 0.031(3) 0.050(3) -0.005(2) 0.013(2) -0.004(2) C19 0.039(2) 0.037(3) 0.040(3) -0.001(2) 0.013(2) -0.002(2) C20 0.039(3) 0.044(3) 0.051(3) 0.005(2) 0.017(2) 0.000(2) C21 0.032(2) 0.037(3) 0.045(3) -0.005(2) 0.011(2) -0.008(2) C22 0.037(3) 0.049(3) 0.058(3) 0.002(3) 0.013(2) -0.003(2) C23 0.045(3) 0.069(4) 0.045(3) -0.008(3) 0.023(3) -0.019(3) C24 0.041(3) 0.066(4) 0.059(4) -0.024(3) 0.027(3) -0.017(3) C25 0.033(3) 0.048(3) 0.075(4) -0.013(3) 0.022(3) 0.005(2) C26 0.087(4) 0.060(3) 0.079(4) 0.001(3) 0.023(3) 0.025(3) C27 0.049(3) 0.045(3) 0.057(3) -0.002(2) 0.006(2) -0.012(2) C28 0.044(3) 0.056(3) 0.071(4) -0.010(3) 0.021(3) -0.008(3) C29 0.033(2) 0.042(3) 0.059(4) -0.009(3) 0.013(2) 0.005(2) C30 0.031(2) 0.043(3) 0.063(4) -0.014(3) 0.005(2) 0.000(2) C31 0.043(3) 0.074(4) 0.067(4) -0.022(3) -0.005(3) 0.006(3) C32 0.031(3) 0.074(4) 0.107(5) -0.038(4) 0.002(3) -0.014(3) C33 0.046(3) 0.057(4) 0.120(6) -0.032(4) 0.033(4) -0.022(3) C34 0.075(4) 0.104(4) 0.062(4) 0.001(3) 0.039(3) 0.029(3) C35 0.037(3) 0.077(4) 0.090(4) 0.008(3) 0.007(3) 0.018(3) C36 0.104(5) 0.126(5) 0.050(4) -0.016(4) -0.008(3) 0.012(4) C37 0.043(3) 0.089(4) 0.085(4) 0.027(3) 0.027(3) 0.000(3) C38 0.103(5) 0.133(6) 0.075(4) 0.039(4) 0.043(4) 0.028(4) B 0.034(3) 0.036(3) 0.043(3) -0.004(3) 0.013(2) 0.003(2) F1 0.056(2) 0.042(2) 0.061(2) -0.0099(13) -0.0026(13) 0.0021(12) F7 0.052(2) 0.074(2) 0.077(2) 0.007(2) -0.0136(15) -0.0010(15) F8 0.058(2) 0.079(2) 0.106(3) 0.026(2) 0.017(2) 0.031(2) F6 0.103(2) 0.045(2) 0.114(3) -0.010(2) 0.019(2) 0.028(2) F4 0.068(2) 0.041(2) 0.086(2) -0.021(2) 0.005(2) -0.0014(14) F2 0.058(2) 0.078(2) 0.069(2) 0.022(2) 0.0254(14) 0.0253(15) F12 0.068(2) 0.080(2) 0.124(3) -0.003(2) 0.045(2) 0.028(2) F5 0.069(2) 0.119(3) 0.092(2) -0.044(2) 0.052(2) -0.012(2) F3 0.080(2) 0.116(3) 0.057(2) 0.003(2) 0.035(2) -0.013(2) F11 0.071(2) 0.084(2) 0.064(2) 0.028(2) 0.032(2) 0.020(2) F9 0.082(2) 0.060(2) 0.099(3) 0.002(2) 0.038(2) -0.021(2) F10 0.084(2) 0.088(2) 0.180(4) -0.041(2) 0.058(2) -0.049(2) F14 0.066(2) 0.134(3) 0.165(4) -0.061(3) -0.012(2) -0.036(2) F13 0.076(2) 0.116(3) 0.070(2) -0.021(2) -0.028(2) -0.006(2) F15 0.0470(15) 0.062(2) 0.049(2) -0.0030(14) -0.0037(12) 0.0011(13) Ti 0.0309(4) 0.0494(5) 0.0371(5) 0.0049(4) 0.0060(3) 0.0080(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 C1 C5 1.410(6) . ? C1 C2 1.417(6) . ? C1 C26 1.506(6) . ? C1 Ti 2.348(4) . ? C2 C3 1.426(6) . ? C2 C35 1.513(6) . ? C2 Ti 2.319(4) . ? C3 C4 1.406(7) . ? C3 C36 1.513(7) . ? C3 Ti 2.339(4) . ? C4 C5 1.415(7) . ? C4 C38 1.506(7) . ? C4 Ti 2.376(5) . ? C5 C6 1.514(7) . ? C5 Ti 2.381(5) . ? C7 C11 1.427(5) . ? C7 C8 1.437(5) . ? C7 C13 1.514(5) . ? C7 Ti 2.176(4) . ? C8 C9 1.405(5) . ? C8 C27 1.505(6) . ? C8 Ti 2.296(4) . ? C9 C10 1.416(6) . ? C9 C37 1.506(6) . ? C9 Ti 2.447(4) . ? C10 C11 1.397(6) . ? C10 C34 1.518(6) . ? C10 Ti 2.434(4) . ? C11 C12 1.507(5) . ? C11 Ti 2.316(4) . ? C13 B 1.649(6) . ? C13 Ti 2.671(4) . ? C14 F1 1.360(4) . ? C14 C15 1.376(5) . ? C14 C19 1.388(5) . ? C15 F7 1.344(5) . ? C15 C16 1.360(6) . ? C16 F8 1.339(5) . ? C16 C17 1.369(6) . ? C17 F6 1.329(5) . ? C17 C18 1.380(6) . ? C18 F4 1.360(5) . ? C18 C19 1.378(5) . ? C19 B 1.667(6) . ? C20 F2 1.353(5) . ? C20 C21 1.384(5) . ? C20 C25 1.385(6) . ? C21 C22 1.381(6) . ? C21 B 1.666(6) . ? C22 F11 1.362(5) . ? C22 C23 1.375(6) . ? C23 F3 1.347(5) . ? C23 C24 1.352(6) . ? C24 F5 1.350(5) . ? C24 C25 1.353(6) . ? C25 F12 1.337(5) . ? C28 F9 1.358(6) . ? C28 C33 1.384(7) . ? C28 C29 1.386(6) . ? C29 C30 1.380(6) . ? C29 B 1.649(6) . ? C30 C31 1.387(6) . ? C30 F15 1.391(5) . ? C31 F13 1.335(6) . ? C31 C32 1.370(7) . ? C32 F14 1.346(5) . ? C32 C33 1.354(8) . ? C33 F10 1.350(6) . ? F15 Ti 2.406(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C5 C1 C2 108.5(4) . . ? C5 C1 C26 126.7(5) . . ? C2 C1 C26 124.8(5) . . ? C5 C1 Ti 73.9(3) . . ? C2 C1 Ti 71.2(2) . . ? C26 C1 Ti 122.6(3) . . ? C1 C2 C3 107.5(4) . . ? C1 C2 C35 126.3(5) . . ? C3 C2 C35 125.8(5) . . ? C1 C2 Ti 73.4(2) . . ? C3 C2 Ti 73.0(2) . . ? C35 C2 Ti 124.8(3) . . ? C4 C3 C2 107.7(4) . . ? C4 C3 C36 126.3(5) . . ? C2 C3 C36 126.0(5) . . ? C4 C3 Ti 74.1(3) . . ? C2 C3 Ti 71.4(2) . . ? C36 C3 Ti 123.1(3) . . ? C3 C4 C5 108.8(4) . . ? C3 C4 C38 125.1(5) . . ? C5 C4 C38 125.6(5) . . ? C3 C4 Ti 71.2(3) . . ? C5 C4 Ti 72.9(3) . . ? C38 C4 Ti 128.4(3) . . ? C1 C5 C4 107.6(4) . . ? C1 C5 C6 124.4(5) . . ? C4 C5 C6 127.4(5) . . ? C1 C5 Ti 71.4(3) . . ? C4 C5 Ti 72.5(3) . . ? C6 C5 Ti 128.8(3) . . ? C11 C7 C8 107.3(3) . . ? C11 C7 C13 128.9(4) . . ? C8 C7 C13 117.6(3) . . ? C11 C7 Ti 76.9(2) . . ? C8 C7 Ti 75.8(2) . . ? C13 C7 Ti 90.9(2) . . ? C9 C8 C7 107.6(4) . . ? C9 C8 C27 127.3(4) . . ? C7 C8 C27 125.0(4) . . ? C9 C8 Ti 78.8(2) . . ? C7 C8 Ti 66.8(2) . . ? C27 C8 Ti 122.2(3) . . ? C8 C9 C10 108.2(4) . . ? C8 C9 C37 126.1(4) . . ? C10 C9 C37 124.9(4) . . ? C8 C9 Ti 66.9(2) . . ? C10 C9 Ti 72.6(2) . . ? C37 C9 Ti 134.1(3) . . ? C11 C10 C9 108.9(4) . . ? C11 C10 C34 126.0(4) . . ? C9 C10 C34 124.8(4) . . ? C11 C10 Ti 68.3(2) . . ? C9 C10 Ti 73.7(2) . . ? C34 C10 Ti 129.6(3) . . ? C10 C11 C7 107.9(4) . . ? C10 C11 C12 122.6(4) . . ? C7 C11 C12 129.4(4) . . ? C10 C11 Ti 77.6(2) . . ? C7 C11 Ti 66.2(2) . . ? C12 C11 Ti 124.3(3) . . ? C7 C13 B 124.8(3) . . ? C7 C13 Ti 54.5(2) . . ? B C13 Ti 134.9(3) . . ? F1 C14 C15 115.3(4) . . ? F1 C14 C19 119.3(3) . . ? C15 C14 C19 125.3(4) . . ? F7 C15 C16 119.8(4) . . ? F7 C15 C14 121.2(4) . . ? C16 C15 C14 119.1(4) . . ? F8 C16 C15 119.8(5) . . ? F8 C16 C17 121.0(4) . . ? C15 C16 C17 119.3(4) . . ? F6 C17 C16 120.3(4) . . ? F6 C17 C18 120.5(4) . . ? C16 C17 C18 119.2(4) . . ? F4 C18 C19 120.4(4) . . ? F4 C18 C17 114.6(4) . . ? C19 C18 C17 125.0(4) . . ? C18 C19 C14 112.1(4) . . ? C18 C19 B 128.2(4) . . ? C14 C19 B 119.5(4) . . ? F2 C20 C21 119.9(4) . . ? F2 C20 C25 116.0(4) . . ? C21 C20 C25 124.1(5) . . ? C22 C21 C20 112.7(4) . . ? C22 C21 B 127.1(4) . . ? C20 C21 B 120.2(4) . . ? F11 C22 C23 114.9(4) . . ? F11 C22 C21 120.4(4) . . ? C23 C22 C21 124.7(5) . . ? F3 C23 C24 120.4(4) . . ? F3 C23 C22 119.9(5) . . ? C24 C23 C22 119.6(5) . . ? F5 C24 C23 119.2(5) . . ? F5 C24 C25 121.4(5) . . ? C23 C24 C25 119.4(4) . . ? F12 C25 C24 120.3(4) . . ? F12 C25 C20 120.1(5) . . ? C24 C25 C20 119.6(4) . . ? F9 C28 C33 116.4(5) . . ? F9 C28 C29 118.5(4) . . ? C33 C28 C29 124.9(6) . . ? C30 C29 C28 111.6(4) . . ? C30 C29 B 127.6(4) . . ? C28 C29 B 120.6(4) . . ? C29 C30 C31 126.3(5) . . ? C29 C30 F15 121.5(4) . . ? C31 C30 F15 112.2(5) . . ? F13 C31 C32 120.6(5) . . ? F13 C31 C30 121.5(5) . . ? C32 C31 C30 117.9(6) . . ? F14 C32 C33 120.8(6) . . ? F14 C32 C31 119.4(7) . . ? C33 C32 C31 119.7(5) . . ? F10 C33 C32 120.6(5) . . ? F10 C33 C28 119.8(6) . . ? C32 C33 C28 119.5(5) . . ? C29 B C13 114.3(4) . . ? C29 B C21 104.6(3) . . ? C13 B C21 106.9(3) . . ? C29 B C19 114.0(3) . . ? C13 B C19 104.7(3) . . ? C21 B C19 112.4(3) . . ? C30 F15 Ti 152.1(2) . . ? C7 Ti C8 37.37(14) . . ? C7 Ti C11 36.86(14) . . ? C8 Ti C11 60.02(14) . . ? C7 Ti C2 147.4(2) . . ? C8 Ti C2 145.6(2) . . ? C11 Ti C2 151.7(2) . . ? C7 Ti C3 166.6(2) . . ? C8 Ti C3 153.2(2) . . ? C11 Ti C3 131.8(2) . . ? C2 Ti C3 35.6(2) . . ? C7 Ti C1 132.7(2) . . ? C8 Ti C1 111.2(2) . . ? C11 Ti C1 169.6(2) . . ? C2 Ti C1 35.34(15) . . ? C3 Ti C1 58.6(2) . . ? C7 Ti C4 152.6(2) . . ? C8 Ti C4 118.6(2) . . ? C11 Ti C4 130.3(2) . . ? C2 Ti C4 58.3(2) . . ? C3 Ti C4 34.7(2) . . ? C1 Ti C4 57.7(2) . . ? C7 Ti C5 134.9(2) . . ? C8 Ti C5 98.7(2) . . ? C11 Ti C5 146.7(2) . . ? C2 Ti C5 58.4(2) . . ? C3 Ti C5 58.1(2) . . ? C1 Ti C5 34.7(2) . . ? C4 Ti C5 34.6(2) . . ? C7 Ti F15 84.96(12) . . ? C8 Ti F15 122.21(12) . . ? C11 Ti F15 75.61(12) . . ? C2 Ti F15 77.40(13) . . ? C3 Ti F15 84.23(14) . . ? C1 Ti F15 107.32(14) . . ? C4 Ti F15 118.1(2) . . ? C5 Ti F15 135.62(13) . . ? C7 Ti C10 59.05(14) . . ? C8 Ti C10 57.69(15) . . ? C11 Ti C10 34.10(14) . . ? C2 Ti C10 151.8(2) . . ? C3 Ti C10 116.2(2) . . ? C1 Ti C10 148.0(2) . . ? C4 Ti C10 99.1(2) . . ? C5 Ti C10 113.7(2) . . ? F15 Ti C10 103.12(14) . . ? C7 Ti C9 59.17(14) . . ? C8 Ti C9 34.28(14) . . ? C11 Ti C9 57.35(15) . . ? C2 Ti C9 148.3(2) . . ? C3 Ti C9 125.0(2) . . ? C1 Ti C9 119.3(2) . . ? C4 Ti C9 93.5(2) . . ? C5 Ti C9 90.4(2) . . ? F15 Ti C9 132.93(13) . . ? C10 Ti C9 33.73(14) . . ? C7 Ti C13 34.52(12) . . ? C8 Ti C13 60.53(13) . . ? C11 Ti C13 63.80(14) . . ? C2 Ti C13 112.9(2) . . ? C3 Ti C13 144.0(2) . . ? C1 Ti C13 107.57(15) . . ? C4 Ti C13 164.8(2) . . ? C5 Ti C13 130.9(2) . . ? F15 Ti C13 67.77(10) . . ? C10 Ti C13 92.72(14) . . ? C9 Ti C13 91.02(13) . . ? _refine_diff_density_max 0.294 _refine_diff_density_min -0.257 _refine_diff_density_rms 0.053 #===END data_202 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C49 H44 B F15 Si Zr' _chemical_formula_weight 1047.96 _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' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 '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 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 12.827(3) _cell_length_b 18.862(4) _cell_length_c 19.499(4) _cell_angle_alpha 90.00 _cell_angle_beta 94.26(3) _cell_angle_gamma 90.00 _cell_volume 4704.6(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 4 _cell_measurement_theta_max 20 _exptl_crystal_description PRISM _exptl_crystal_colour RED _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.480 _exptl_crystal_density_method ? _exptl_crystal_F_000 2128 _exptl_absorpt_coefficient_mu 0.353 _exptl_absorpt_correction_type 'MEAN IMAGING PLATE INTENSITY METHOD' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 STOE-IPDS _diffrn_measurement_method 'LASER SCANNED IMAGING PLATE' _diffrn_standards_number 50-200 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 360 _diffrn_standards_decay_% ? _diffrn_reflns_number 13886 _diffrn_reflns_av_R_equivalents 0.0766 _diffrn_reflns_av_sigmaI/netI 0.1836 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 24.29 _reflns_number_total 7099 _reflns_number_observed 3131 _reflns_observed_criterion >2sigma(I) _computing_data_collection STOE-EXPOSE _computing_cell_refinement STOE-CELL _computing_data_reduction STOE-INTEGRATE _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics XP _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^)+(0.0029P)^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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7099 _refine_ls_number_parameters 608 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1292 _refine_ls_R_factor_obs 0.0452 _refine_ls_wR_factor_all 0.0744 _refine_ls_wR_factor_obs 0.0607 _refine_ls_goodness_of_fit_all 0.717 _refine_ls_goodness_of_fit_obs 0.936 _refine_ls_restrained_S_all 0.717 _refine_ls_restrained_S_obs 0.936 _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 C1 C 1.2750(5) 0.3433(3) 0.5170(3) 0.047(2) Uani 1 d . . H1 H 1.2404(33) 0.3347(25) 0.4767(26) 0.047(18) Uiso 1 d . . C2 C 1.3337(4) 0.2979(3) 0.5516(3) 0.0468(15) Uani 1 d . . C3 C 1.4043(4) 0.3088(3) 0.6131(3) 0.056(2) Uani 1 d . . C4 C 1.4452(5) 0.2500(4) 0.6485(4) 0.077(2) Uani 1 d . . H4 H 1.4265(5) 0.2049(4) 0.6328(4) 0.092 Uiso 1 calc R . C5 C 1.5130(5) 0.2568(5) 0.7067(4) 0.097(3) Uani 1 d . . H5 H 1.5386(5) 0.2164(5) 0.7294(4) 0.116 Uiso 1 calc R . C6 C 1.5427(5) 0.3217(6) 0.7309(5) 0.114(3) Uani 1 d . . H6 H 1.5868(5) 0.3260(6) 0.7708(5) 0.137 Uiso 1 calc R . C7 C 1.5054(5) 0.3832(5) 0.6947(4) 0.107(3) Uani 1 d . . H7 H 1.5267(5) 0.4281(5) 0.7097(4) 0.128 Uiso 1 calc R . C8 C 1.4367(5) 0.3756(4) 0.6365(3) 0.078(2) Uani 1 d . . H8 H 1.4121(5) 0.4157(4) 0.6128(3) 0.094 Uiso 1 calc R . C9 C 1.0919(3) 0.1928(3) 0.4683(3) 0.0375(14) Uani 1 d . . C10 C 1.0451(3) 0.2384(2) 0.4119(3) 0.0408(14) Uani 1 d . . H10A H 1.0819(3) 0.2281(2) 0.3714(3) 0.049 Uiso 1 calc R . H10B H 1.0616(3) 0.2871(2) 0.4246(3) 0.049 Uiso 1 calc R . C11 C 1.1175(3) 0.2124(3) 0.5379(3) 0.0366(12) Uani 1 d . . C12 C 1.1827(4) 0.1598(3) 0.5701(3) 0.049(2) Uani 1 d . . C13 C 1.1998(4) 0.1063(3) 0.5203(3) 0.050(2) Uani 1 d . . C14 C 1.1420(4) 0.1244(3) 0.4586(3) 0.0419(14) Uani 1 d . . C15 C 1.1179(4) 0.0768(3) 0.3984(3) 0.061(2) Uani 1 d . . H15A H 1.0774(4) 0.1023(3) 0.3630(3) 0.091 Uiso 1 calc R . H15B H 1.0788(4) 0.0366(3) 0.4124(3) 0.091 Uiso 1 calc R . H15C H 1.1820(4) 0.0610(3) 0.3809(3) 0.091 Uiso 1 calc R . C16 C 1.3766(5) 0.2629(3) 0.3760(3) 0.064(2) Uani 1 d . . C17 C 1.3423(4) 0.1937(3) 0.3565(3) 0.054(2) Uani 1 d . . C18 C 1.3957(4) 0.1445(3) 0.4020(3) 0.056(2) Uani 1 d . . C19 C 1.4628(4) 0.1851(4) 0.4489(3) 0.060(2) Uani 1 d . . C20 C 1.4527(4) 0.2575(4) 0.4330(3) 0.058(2) Uani 1 d . . C21 C 1.5213(4) 0.3155(4) 0.4635(3) 0.104(3) Uani 1 d . . H21A H 1.4984(4) 0.3603(4) 0.4443(3) 0.157 Uiso 1 calc R . H21B H 1.5923(4) 0.3070(4) 0.4533(3) 0.157 Uiso 1 calc R . H21C H 1.5172(4) 0.3165(4) 0.5125(3) 0.157 Uiso 1 calc R . C22 C 1.1193(4) 0.4508(3) 0.4544(3) 0.081(2) Uani 1 d . . H22A H 1.1394(4) 0.4390(3) 0.4094(3) 0.122 Uiso 1 calc R . H22B H 1.0952(4) 0.4990(3) 0.4547(3) 0.122 Uiso 1 calc R . H22C H 1.0641(4) 0.4198(3) 0.4664(3) 0.122 Uiso 1 calc R . C23 C 1.3429(4) 0.4974(3) 0.4924(4) 0.097(2) Uani 1 d . . H23A H 1.3613(4) 0.4836(3) 0.4474(4) 0.145 Uiso 1 calc R . H23B H 1.4025(4) 0.4919(3) 0.5247(4) 0.145 Uiso 1 calc R . H23C H 1.3209(4) 0.5460(3) 0.4914(4) 0.145 Uiso 1 calc R . C24 C 1.1938(5) 0.4635(3) 0.6051(3) 0.092(2) Uani 1 d . . H24A H 1.1379(5) 0.4328(3) 0.6164(3) 0.138 Uiso 1 calc R . H24B H 1.1705(5) 0.5118(3) 0.6052(3) 0.138 Uiso 1 calc R . H24C H 1.2521(5) 0.4577(3) 0.6385(3) 0.138 Uiso 1 calc R . C25 C 0.7925(4) 0.1245(3) 0.3412(3) 0.0398(14) Uani 1 d . . C26 C 0.8794(4) 0.1690(3) 0.3363(3) 0.0358(13) Uani 1 d . . C27 C 0.9298(4) 0.1551(3) 0.2767(3) 0.0427(14) Uani 1 d . . C28 C 0.9018(5) 0.1018(3) 0.2304(3) 0.055(2) Uani 1 d . . C29 C 0.8170(5) 0.0592(3) 0.2398(4) 0.059(2) Uani 1 d . . C30 C 0.7628(5) 0.0718(3) 0.2952(3) 0.052(2) Uani 1 d . . C31 C 0.8639(3) 0.1736(3) 0.5023(3) 0.0369(13) Uani 1 d . . C32 C 0.8633(3) 0.2346(3) 0.4625(2) 0.0329(13) Uani 1 d . . C33 C 0.8279(3) 0.2936(3) 0.4957(3) 0.0414(13) Uani 1 d . . C34 C 0.7918(4) 0.2919(3) 0.5611(3) 0.050(2) Uani 1 d . . C35 C 0.7928(4) 0.2296(4) 0.5968(3) 0.051(2) Uani 1 d . . C36 C 0.8281(4) 0.1705(3) 0.5676(3) 0.051(2) Uani 1 d . . C37 C 0.7754(4) 0.3220(3) 0.3269(3) 0.0448(15) Uani 1 d . . C38 C 0.8805(4) 0.3055(3) 0.3398(3) 0.0392(14) Uani 1 d . . C39 C 0.9449(4) 0.3506(3) 0.3064(3) 0.0482(15) Uani 1 d . . C40 C 0.9100(6) 0.4076(3) 0.2666(3) 0.060(2) Uani 1 d . . C41 C 0.8069(6) 0.4219(3) 0.2581(3) 0.059(2) Uani 1 d . . C42 C 0.7378(5) 0.3791(3) 0.2886(3) 0.055(2) Uani 1 d . . C43 C 1.0777(3) 0.2748(3) 0.5749(3) 0.058(2) Uani 1 d . . H43A H 1.0351(3) 0.3035(3) 0.5432(3) 0.087 Uiso 1 calc R . H43B H 1.1357(3) 0.3024(3) 0.5940(3) 0.087 Uiso 1 calc R . H43C H 1.0368(3) 0.2588(3) 0.6111(3) 0.087 Uiso 1 calc R . C44 C 1.2125(4) 0.1556(3) 0.6467(3) 0.075(2) Uani 1 d . . H44A H 1.2573(4) 0.1154(3) 0.6561(3) 0.113 Uiso 1 calc R . H44B H 1.1505(4) 0.1505(3) 0.6710(3) 0.113 Uiso 1 calc R . H44C H 1.2486(4) 0.1981(3) 0.6616(3) 0.113 Uiso 1 calc R . C45 C 1.2522(5) 0.0362(3) 0.5356(3) 0.079(2) Uani 1 d . . H45A H 1.2864(5) 0.0371(3) 0.5811(3) 0.119 Uiso 1 calc R . H45B H 1.3030(5) 0.0275(3) 0.5028(3) 0.119 Uiso 1 calc R . H45C H 1.2008(5) -0.0009(3) 0.5327(3) 0.119 Uiso 1 calc R . C46 C 1.3456(5) 0.3315(4) 0.3398(4) 0.100(2) Uani 1 d . . H46A H 1.3800(5) 0.3705(4) 0.3637(4) 0.150 Uiso 1 calc R . H46B H 1.2713(5) 0.3376(4) 0.3393(4) 0.150 Uiso 1 calc R . H46C H 1.3660(5) 0.3300(4) 0.2934(4) 0.150 Uiso 1 calc R . C47 C 1.4005(5) 0.0652(3) 0.3914(3) 0.089(2) Uani 1 d . . H47A H 1.4413(5) 0.0439(3) 0.4293(3) 0.133 Uiso 1 calc R . H47B H 1.4324(5) 0.0553(3) 0.3494(3) 0.133 Uiso 1 calc R . H47C H 1.3311(5) 0.0460(3) 0.3888(3) 0.133 Uiso 1 calc R . C48 C 1.2751(4) 0.1784(3) 0.2914(3) 0.076(2) Uani 1 d . . H48A H 1.2610(4) 0.1285(3) 0.2882(3) 0.114 Uiso 1 calc R . H48B H 1.3110(4) 0.1932(3) 0.2523(3) 0.114 Uiso 1 calc R . H48C H 1.2103(4) 0.2039(3) 0.2921(3) 0.114 Uiso 1 calc R . C49 C 1.5399(4) 0.1505(4) 0.5031(3) 0.109(3) Uani 1 d . . H49A H 1.5294(4) 0.1001(4) 0.5029(3) 0.164 Uiso 1 calc R . H49B H 1.5282(4) 0.1690(4) 0.5478(3) 0.164 Uiso 1 calc R . H49C H 1.6102(4) 0.1608(4) 0.4925(3) 0.164 Uiso 1 calc R . B B 0.9156(4) 0.2357(3) 0.3875(3) 0.037(2) Uani 1 d . . F1 F 0.7283(2) 0.1334(2) 0.3925(2) 0.0548(8) Uani 1 d . . F2 F 0.6773(2) 0.0312(2) 0.3044(2) 0.0735(11) Uani 1 d . . F3 F 0.7891(3) 0.0087(2) 0.1944(2) 0.0948(12) Uani 1 d . . F4 F 0.9568(3) 0.0935(2) 0.1746(2) 0.0902(12) Uani 1 d . . F5 F 1.0108(2) 0.1962(2) 0.26197(15) 0.0651(9) Uani 1 d . . F6 F 0.9003(2) 0.11218(15) 0.47740(14) 0.0502(8) Uani 1 d . . F7 F 0.8300(3) 0.1082(2) 0.6016(2) 0.0796(11) Uani 1 d . . F8 F 0.7579(2) 0.2272(2) 0.6607(2) 0.0917(11) Uani 1 d . . F9 F 0.7563(2) 0.3517(2) 0.5896(2) 0.0752(10) Uani 1 d . . F10 F 0.8278(2) 0.3586(2) 0.46654(15) 0.0615(9) Uani 1 d . . F11 F 0.7031(2) 0.2800(2) 0.35458(15) 0.0593(8) Uani 1 d . . F12 F 0.6334(3) 0.3923(2) 0.2822(2) 0.0889(12) Uani 1 d . . F13 F 0.7700(3) 0.4781(2) 0.2207(2) 0.0974(13) Uani 1 d . . F14 F 0.9778(3) 0.4494(2) 0.2351(2) 0.0940(12) Uani 1 d . . F15 F 1.0512(3) 0.3417(2) 0.3098(2) 0.0710(10) Uani 1 d . . Si Si 1.23445(13) 0.44039(9) 0.51850(10) 0.0612(5) Uani 1 d . . Zr Zr 1.27716(4) 0.21818(3) 0.47231(3) 0.03924(15) Uani 1 d . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.043(4) 0.069(5) 0.032(5) -0.013(3) 0.007(3) -0.013(3) C2 0.037(3) 0.053(4) 0.051(4) -0.014(3) 0.007(3) -0.005(3) C3 0.045(4) 0.062(5) 0.061(5) 0.006(4) 0.012(3) 0.002(3) C4 0.057(4) 0.098(6) 0.077(6) 0.000(4) 0.008(4) 0.006(4) C5 0.068(5) 0.120(8) 0.100(8) 0.018(5) -0.007(5) -0.010(5) C6 0.054(5) 0.187(10) 0.096(8) 0.012(7) -0.023(4) -0.018(6) C7 0.086(6) 0.121(8) 0.108(8) -0.013(6) -0.023(5) -0.035(5) C8 0.076(5) 0.076(5) 0.078(6) 0.001(4) -0.032(4) -0.003(4) C9 0.017(3) 0.049(4) 0.046(4) -0.006(3) 0.000(2) -0.008(2) C10 0.043(3) 0.037(3) 0.043(4) -0.006(3) 0.007(3) -0.010(2) C11 0.029(3) 0.039(3) 0.041(4) -0.009(3) -0.001(2) -0.007(3) C12 0.057(4) 0.053(4) 0.035(4) 0.001(3) 0.003(3) -0.018(3) C13 0.063(4) 0.038(4) 0.047(5) 0.002(3) -0.010(3) -0.006(3) C14 0.043(3) 0.037(4) 0.044(4) -0.007(3) 0.000(3) -0.010(3) C15 0.061(4) 0.048(4) 0.070(5) -0.015(3) -0.010(3) -0.005(3) C16 0.069(4) 0.079(6) 0.048(5) -0.005(4) 0.032(3) -0.005(4) C17 0.058(4) 0.069(5) 0.038(4) -0.018(3) 0.021(3) -0.015(3) C18 0.045(4) 0.065(5) 0.059(5) -0.013(4) 0.010(3) 0.008(3) C19 0.033(4) 0.091(6) 0.058(5) -0.026(4) 0.012(3) 0.004(4) C20 0.041(4) 0.072(5) 0.067(5) -0.025(4) 0.032(3) -0.014(4) C21 0.072(4) 0.134(7) 0.113(7) -0.068(5) 0.051(4) -0.062(4) C22 0.069(4) 0.080(5) 0.093(6) 0.016(4) -0.006(4) 0.004(4) C23 0.076(5) 0.067(5) 0.147(8) 0.010(5) 0.013(4) -0.007(4) C24 0.111(5) 0.078(5) 0.089(6) -0.026(4) 0.017(4) 0.005(4) C25 0.050(4) 0.040(4) 0.029(4) -0.001(3) 0.000(3) 0.008(3) C26 0.043(3) 0.037(3) 0.027(4) 0.005(2) 0.001(3) 0.000(3) C27 0.044(4) 0.042(4) 0.041(4) 0.000(3) 0.000(3) 0.000(3) C28 0.059(4) 0.068(5) 0.038(5) -0.015(3) 0.000(3) 0.012(4) C29 0.081(5) 0.039(4) 0.053(5) -0.012(3) -0.019(4) 0.000(4) C30 0.052(4) 0.057(4) 0.045(5) 0.000(4) -0.014(3) -0.006(3) C31 0.035(3) 0.041(4) 0.034(4) 0.007(3) -0.003(3) 0.000(3) C32 0.031(3) 0.040(4) 0.027(4) 0.002(3) 0.000(2) -0.003(2) C33 0.044(3) 0.040(4) 0.040(4) 0.008(3) 0.005(3) 0.007(3) C34 0.045(3) 0.054(5) 0.052(5) -0.010(4) 0.003(3) 0.011(3) C35 0.051(3) 0.075(5) 0.029(4) 0.006(4) 0.014(3) -0.002(3) C36 0.060(4) 0.051(4) 0.040(5) 0.013(3) -0.001(3) -0.006(3) C37 0.061(4) 0.046(4) 0.027(4) 0.007(3) -0.001(3) 0.005(3) C38 0.053(4) 0.039(4) 0.025(4) 0.001(2) 0.007(3) -0.007(3) C39 0.057(4) 0.047(4) 0.041(4) 0.002(3) 0.003(3) -0.004(3) C40 0.089(5) 0.047(4) 0.045(5) 0.007(3) 0.007(4) -0.010(4) C41 0.114(6) 0.024(4) 0.037(4) 0.010(3) -0.006(4) 0.005(4) C42 0.079(5) 0.051(4) 0.034(4) -0.005(3) -0.008(3) 0.017(4) C43 0.051(3) 0.073(4) 0.051(4) -0.018(4) 0.009(3) -0.014(3) C44 0.090(5) 0.091(5) 0.044(5) 0.012(4) -0.001(3) -0.014(4) C45 0.116(6) 0.043(4) 0.077(5) 0.014(4) -0.014(4) 0.002(4) C46 0.133(6) 0.085(6) 0.088(7) 0.019(5) 0.050(5) -0.003(5) C47 0.096(5) 0.074(5) 0.099(6) -0.022(4) 0.017(4) 0.030(4) C48 0.077(4) 0.112(6) 0.041(5) -0.014(4) 0.013(3) -0.007(4) C49 0.052(4) 0.189(8) 0.085(6) -0.029(5) -0.008(4) 0.045(5) B 0.039(4) 0.033(4) 0.037(4) -0.001(3) 0.000(3) 0.001(3) F1 0.045(2) 0.070(2) 0.049(2) 0.002(2) -0.002(2) -0.016(2) F2 0.075(2) 0.069(2) 0.074(3) 0.006(2) -0.015(2) -0.031(2) F3 0.119(3) 0.080(3) 0.082(3) -0.039(2) -0.015(2) -0.012(2) F4 0.096(3) 0.113(3) 0.063(3) -0.036(2) 0.016(2) -0.001(2) F5 0.062(2) 0.087(3) 0.049(2) -0.009(2) 0.021(2) -0.020(2) F6 0.065(2) 0.037(2) 0.048(2) 0.006(2) 0.0011(15) -0.001(2) F7 0.122(3) 0.065(3) 0.052(3) 0.025(2) 0.017(2) -0.006(2) F8 0.114(3) 0.120(3) 0.045(3) 0.015(2) 0.032(2) 0.007(2) F9 0.097(3) 0.083(3) 0.048(3) -0.008(2) 0.016(2) 0.029(2) F10 0.097(2) 0.043(2) 0.045(2) 0.002(2) 0.014(2) 0.018(2) F11 0.046(2) 0.072(2) 0.060(2) 0.018(2) 0.0030(14) 0.005(2) F12 0.086(3) 0.091(3) 0.086(3) 0.013(2) -0.014(2) 0.038(2) F13 0.170(4) 0.055(2) 0.065(3) 0.021(2) -0.003(2) 0.025(2) F14 0.133(3) 0.075(3) 0.076(3) 0.029(2) 0.023(2) -0.031(2) F15 0.072(2) 0.073(3) 0.071(3) 0.016(2) 0.018(2) -0.020(2) Si 0.0583(11) 0.0526(11) 0.0731(15) -0.0040(10) 0.0064(9) -0.0022(9) Zr 0.0380(3) 0.0391(3) 0.0406(4) -0.0073(3) 0.0035(2) -0.0031(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.297(7) . ? C1 Si 1.904(6) . ? C1 Zr 2.518(6) . ? C2 C3 1.463(7) . ? C2 Zr 2.238(5) . ? C3 C4 1.389(8) . ? C3 C8 1.392(8) . ? C4 C5 1.382(8) . ? C5 C6 1.357(10) . ? C6 C7 1.422(10) . ? C7 C8 1.391(8) . ? C9 C11 1.420(6) . ? C9 C14 1.459(6) . ? C9 C10 1.487(6) . ? C9 Zr 2.419(4) . ? C10 B 1.694(6) . ? C11 C12 1.414(7) . ? C11 C43 1.491(7) . ? C11 Zr 2.496(4) . ? C12 C13 1.428(7) . ? C12 C44 1.517(7) . ? C12 Zr 2.580(5) . ? C13 C14 1.408(7) . ? C13 C45 1.504(7) . ? C13 Zr 2.541(5) . ? C14 C15 1.492(7) . ? C14 Zr 2.477(5) . ? C16 C17 1.421(7) . ? C16 C20 1.427(8) . ? C16 C46 1.513(8) . ? C16 Zr 2.494(6) . ? C17 C18 1.423(8) . ? C17 C48 1.510(7) . ? C17 Zr 2.507(6) . ? C18 C19 1.430(7) . ? C18 C47 1.512(8) . ? C18 Zr 2.536(5) . ? C19 C20 1.404(7) . ? C19 C49 1.538(8) . ? C19 Zr 2.535(5) . ? C20 C21 1.500(7) . ? C20 Zr 2.543(5) . ? C22 Si 1.873(6) . ? C23 Si 1.859(6) . ? C24 Si 1.856(6) . ? C25 F1 1.352(5) . ? C25 C30 1.373(7) . ? C25 C26 1.405(6) . ? C26 C27 1.394(7) . ? C26 B 1.652(7) . ? C27 F5 1.346(5) . ? C27 C28 1.381(7) . ? C28 F4 1.349(6) . ? C28 C29 1.375(8) . ? C29 F3 1.331(6) . ? C29 C30 1.348(8) . ? C30 F2 1.361(6) . ? C31 F6 1.352(5) . ? C31 C36 1.386(7) . ? C31 C32 1.388(6) . ? C32 C33 1.382(6) . ? C32 B 1.653(7) . ? C33 F10 1.351(5) . ? C33 C34 1.390(7) . ? C34 F9 1.350(6) . ? C34 C35 1.367(7) . ? C35 C36 1.346(7) . ? C35 F8 1.355(6) . ? C36 F7 1.349(6) . ? C37 F11 1.362(6) . ? C37 C42 1.377(7) . ? C37 C38 1.388(6) . ? C38 C39 1.383(7) . ? C38 B 1.655(7) . ? C39 F15 1.369(5) . ? C39 C40 1.382(7) . ? C40 C41 1.348(7) . ? C40 F14 1.355(6) . ? C41 F13 1.351(6) . ? C41 C42 1.367(8) . ? C42 F12 1.358(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 C2 C1 Si 140.9(5) . . ? C2 C1 Zr 62.6(3) . . ? Si C1 Zr 156.5(4) . . ? C1 C2 C3 129.3(5) . . ? C1 C2 Zr 86.5(4) . . ? C3 C2 Zr 144.1(4) . . ? C4 C3 C8 117.9(6) . . ? C4 C3 C2 118.9(6) . . ? C8 C3 C2 123.1(6) . . ? C5 C4 C3 121.6(7) . . ? C6 C5 C4 120.9(8) . . ? C5 C6 C7 119.2(8) . . ? C8 C7 C6 119.3(8) . . ? C7 C8 C3 121.1(7) . . ? C11 C9 C14 106.3(4) . . ? C11 C9 C10 127.4(5) . . ? C14 C9 C10 125.0(5) . . ? C11 C9 Zr 76.2(2) . . ? C14 C9 Zr 74.8(3) . . ? C10 C9 Zr 104.6(3) . . ? C9 C10 B 121.6(4) . . ? C12 C11 C9 109.2(5) . . ? C12 C11 C43 123.5(5) . . ? C9 C11 C43 127.2(5) . . ? C12 C11 Zr 77.1(3) . . ? C9 C11 Zr 70.3(2) . . ? C43 C11 Zr 122.4(3) . . ? C11 C12 C13 108.0(5) . . ? C11 C12 C44 124.9(5) . . ? C13 C12 C44 126.3(5) . . ? C11 C12 Zr 70.6(3) . . ? C13 C12 Zr 72.3(3) . . ? C44 C12 Zr 130.7(3) . . ? C14 C13 C12 108.1(5) . . ? C14 C13 C45 125.6(5) . . ? C12 C13 C45 125.2(5) . . ? C14 C13 Zr 71.2(3) . . ? C12 C13 Zr 75.3(3) . . ? C45 C13 Zr 128.5(4) . . ? C13 C14 C9 108.2(5) . . ? C13 C14 C15 126.2(5) . . ? C9 C14 C15 124.5(5) . . ? C13 C14 Zr 76.2(3) . . ? C9 C14 Zr 70.5(2) . . ? C15 C14 Zr 128.1(4) . . ? C17 C16 C20 108.8(6) . . ? C17 C16 C46 126.6(7) . . ? C20 C16 C46 124.4(6) . . ? C17 C16 Zr 74.0(3) . . ? C20 C16 Zr 75.4(3) . . ? C46 C16 Zr 120.6(4) . . ? C16 C17 C18 107.9(5) . . ? C16 C17 C48 123.1(6) . . ? C18 C17 C48 128.2(6) . . ? C16 C17 Zr 73.0(3) . . ? C18 C17 Zr 74.7(3) . . ? C48 C17 Zr 125.8(4) . . ? C17 C18 C19 106.7(6) . . ? C17 C18 C47 125.6(6) . . ? C19 C18 C47 126.0(6) . . ? C17 C18 Zr 72.5(3) . . ? C19 C18 Zr 73.6(3) . . ? C47 C18 Zr 130.4(4) . . ? C20 C19 C18 109.8(6) . . ? C20 C19 C49 127.4(6) . . ? C18 C19 C49 122.5(7) . . ? C20 C19 Zr 74.2(3) . . ? C18 C19 Zr 73.7(3) . . ? C49 C19 Zr 123.0(4) . . ? C19 C20 C16 106.7(6) . . ? C19 C20 C21 125.5(7) . . ? C16 C20 C21 127.1(7) . . ? C19 C20 Zr 73.7(3) . . ? C16 C20 Zr 71.7(3) . . ? C21 C20 Zr 126.9(4) . . ? F1 C25 C30 114.8(5) . . ? F1 C25 C26 120.5(5) . . ? C30 C25 C26 124.7(5) . . ? C27 C26 C25 111.4(5) . . ? C27 C26 B 121.4(5) . . ? C25 C26 B 127.0(5) . . ? F5 C27 C28 116.6(5) . . ? F5 C27 C26 118.9(5) . . ? C28 C27 C26 124.5(5) . . ? F4 C28 C29 120.4(6) . . ? F4 C28 C27 119.0(6) . . ? C29 C28 C27 120.5(6) . . ? F3 C29 C30 122.0(6) . . ? F3 C29 C28 120.4(6) . . ? C30 C29 C28 117.6(6) . . ? C29 C30 F2 118.3(6) . . ? C29 C30 C25 121.1(6) . . ? F2 C30 C25 120.5(6) . . ? F6 C31 C36 116.1(5) . . ? F6 C31 C32 119.8(5) . . ? C36 C31 C32 124.1(5) . . ? C33 C32 C31 113.2(5) . . ? C33 C32 B 125.0(5) . . ? C31 C32 B 121.3(5) . . ? F10 C33 C32 121.6(5) . . ? F10 C33 C34 114.7(5) . . ? C32 C33 C34 123.7(5) . . ? F9 C34 C35 120.0(6) . . ? F9 C34 C33 120.2(5) . . ? C35 C34 C33 119.8(6) . . ? C36 C35 F8 120.5(6) . . ? C36 C35 C34 119.2(6) . . ? F8 C35 C34 120.3(6) . . ? C35 C36 F7 120.5(6) . . ? C35 C36 C31 119.9(5) . . ? F7 C36 C31 119.6(5) . . ? F11 C37 C42 116.6(5) . . ? F11 C37 C38 118.5(5) . . ? C42 C37 C38 124.8(6) . . ? C39 C38 C37 112.5(5) . . ? C39 C38 B 127.4(5) . . ? C37 C38 B 120.1(4) . . ? F15 C39 C40 113.7(5) . . ? F15 C39 C38 122.0(5) . . ? C40 C39 C38 124.3(6) . . ? C41 C40 F14 119.0(6) . . ? C41 C40 C39 119.9(6) . . ? F14 C40 C39 121.0(6) . . ? C40 C41 F13 121.6(6) . . ? C40 C41 C42 119.4(6) . . ? F13 C41 C42 119.0(7) . . ? F12 C42 C41 121.2(6) . . ? F12 C42 C37 119.8(6) . . ? C41 C42 C37 119.0(6) . . ? C26 B C32 114.3(4) . . ? C26 B C38 102.3(4) . . ? C32 B C38 113.3(4) . . ? C26 B C10 114.8(4) . . ? C32 B C10 101.9(4) . . ? C38 B C10 110.7(4) . . ? C24 Si C23 112.4(3) . . ? C24 Si C22 108.7(3) . . ? C23 Si C22 109.0(3) . . ? C24 Si C1 109.6(3) . . ? C23 Si C1 109.9(3) . . ? C22 Si C1 107.1(3) . . ? C2 Zr C9 115.0(2) . . ? C2 Zr C14 138.0(2) . . ? C9 Zr C14 34.66(15) . . ? C2 Zr C16 97.7(2) . . ? C9 Zr C16 126.8(2) . . ? C14 Zr C16 123.6(2) . . ? C2 Zr C11 85.0(2) . . ? C9 Zr C11 33.55(15) . . ? C14 Zr C11 55.2(2) . . ? C16 Zr C11 152.3(2) . . ? C2 Zr C17 129.3(2) . . ? C9 Zr C17 109.1(2) . . ? C14 Zr C17 92.8(2) . . ? C16 Zr C17 33.0(2) . . ? C11 Zr C17 142.6(2) . . ? C2 Zr C1 30.9(2) . . ? C9 Zr C1 99.2(2) . . ? C14 Zr C1 132.9(2) . . ? C16 Zr C1 87.9(2) . . ? C11 Zr C1 80.4(2) . . ? C17 Zr C1 119.8(2) . . ? C2 Zr C19 91.7(2) . . ? C9 Zr C19 151.5(2) . . ? C14 Zr C19 117.7(2) . . ? C16 Zr C19 53.7(2) . . ? C11 Zr C19 154.0(2) . . ? C17 Zr C19 54.0(2) . . ? C1 Zr C19 109.1(2) . . ? C2 Zr C18 124.4(2) . . ? C9 Zr C18 120.1(2) . . ? C14 Zr C18 89.6(2) . . ? C16 Zr C18 54.4(2) . . ? C11 Zr C18 143.2(2) . . ? C17 Zr C18 32.8(2) . . ? C1 Zr C18 136.3(2) . . ? C19 Zr C18 32.8(2) . . ? C2 Zr C13 114.8(2) . . ? C9 Zr C13 55.8(2) . . ? C14 Zr C13 32.6(2) . . ? C16 Zr C13 142.6(2) . . ? C11 Zr C13 54.3(2) . . ? C17 Zr C13 110.1(2) . . ? C1 Zr C13 129.6(2) . . ? C19 Zr C13 105.1(2) . . ? C18 Zr C13 90.6(2) . . ? C2 Zr C20 76.3(2) . . ? C9 Zr C20 159.7(2) . . ? C14 Zr C20 143.5(2) . . ? C16 Zr C20 32.9(2) . . ? C11 Zr C20 161.1(2) . . ? C17 Zr C20 54.6(2) . . ? C1 Zr C20 82.2(2) . . ? C19 Zr C20 32.1(2) . . ? C18 Zr C20 54.3(2) . . ? C13 Zr C20 137.1(2) . . ? C2 Zr C12 85.5(2) . . ? C9 Zr C12 54.9(2) . . ? C14 Zr C12 54.0(2) . . ? C16 Zr C12 174.3(2) . . ? C11 Zr C12 32.3(2) . . ? C17 Zr C12 142.4(2) . . ? C1 Zr C12 97.3(2) . . ? C19 Zr C12 121.8(2) . . ? C18 Zr C12 119.9(2) . . ? C13 Zr C12 32.4(2) . . ? C20 Zr C12 145.3(2) . . ? _refine_diff_density_max 0.343 _refine_diff_density_min -0.304 _refine_diff_density_rms 0.050 #===END