# Copyright The Royal Society of Chemistry, 1999 # CCDC Number: 186/1406 data_global #==================================================================== # 1. SUBMISSION DETAILS _publ_contact_author ; Mark Thornton-Pett School of Chemistry University of Leeds Leeds LS2 9JT UK ; _publ_contact_author_phone '+44 113 2336423' _publ_contact_author_fax '+44 113 2336565' _publ_contact_author_email marktp@chem.leeds.ac.uk _publ_requested_journal 'J. Chem. Soc., Dalton Trans.' _publ_contact_letter ; This following two sets of data are for the two complexes included in manuscript 9/01347D which has been submitted to you. Compound 12a = s92; 13b = mb19 ; #======================================================================= # 2. TITLE AND AUTHOR LIST _publ_section_title ; Reaction of B(C~6~F~5~)~3~ with Zirconium and hafnium half-sandwich Benzyl Complexes. The crystal and molecular structures of Cp"Zr(C~6~F~5~){\e^4^CH~2~CMeCHCHB(C~6~F~5~)~2~} and [Cp"Hf(2,3-Me~2~C~4~H~4~)(OEt~2~)][PhCH~2~B(C~6~F~5~)~3~] [Cp" = 1,3-C~5~H~3~(SiMe~3~)~2~] ; loop_ _publ_author_name _publ_author_address 'Gerardo Jimen\'ez Pindado' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Mark Thornton-Pett' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Manfred Bochmann' ; School of Chemistry University of Leeds Leeds LS2 9JT UK ; 'Michael B. Hursthouse' ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; 'Simon Coles' ; Department of Chemistry University of Southampton Highfield Southampton SO17 1BJ UK ; #================================================================= data_MB19 _audit_creation_date 97-05-23 _audit_creation_method 'STADI4, X-RED' _audit_author_name 'J. Richter' _audit_contact_author 'J. Richter' _audit_contact_author_address ; STOE & CIE GmbH Hilpertstr. 10 D-64295 Darmstadt Germany ; _audit_contact_author_email 100066.3306@compuserve.com _audit_contact_author_fax '+49 6151 891293 ' _audit_contact_author_phone '+49 6151 891225 / 899174' _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C46 H48 B F15 Hf O Si2' _chemical_formula_weight 1147.32 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' 'Hf' 'Hf' -0.5830 6.1852 '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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.1910(15) _cell_length_b 13.1465(15) _cell_length_c 17.506(2) _cell_angle_alpha 104.763(10) _cell_angle_beta 94.315(11) _cell_angle_gamma 103.276(10) _cell_volume 2399.3(5) _cell_formula_units_Z 2 _cell_measurement_temperature 160(2) _cell_measurement_reflns_used 120 _cell_measurement_theta_min 14.9 _cell_measurement_theta_max 17.4 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.570 _exptl_crystal_size_mid 0.417 _exptl_crystal_size_min 0.300 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1144 _exptl_absorpt_coefficient_mu 2.317 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.2493 _exptl_absorpt_correction_T_max 0.4930 _exptl_absorpt_process_details ; Psi Scan Reflections used Mu * R = 0.49 H K L 2Theta Chi Imin/Imax -2 -3 1 13.5 -84.5 0.504 2 3 -1 13.5 84.5 0.491 3 5 -3 21.7 86.4 0.534 -3 -5 3 21.7 -86.4 0.555 -3 -6 4 24.6 -81.8 0.564 3 6 -4 24.6 81.8 0.539 -4 -7 4 29.9 -86.6 0.533 4 7 -4 29.9 86.6 0.526 5 8 -4 35.5 89.8 0.519 -5 -8 4 35.5 -89.8 0.523 -6 -8 3 38.5 -84.0 0.525 6 8 -3 38.5 84.0 0.527 ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 160(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_collimation '0.8 mm' _diffrn_radiation_detector 'NaI(Tl) scintillation counter' _diffrn_radiation_monochromator 'planar graphite' _diffrn_radiation_polarisn_norm 90 _diffrn_measurement_device 'STOE STADI4 4-circle-diffractometer' _diffrn_measurement_method ; Scan width (omega) = 2.05 - 2.20, scan ratio 2theta:omega = 1.00 I(Net) and sigma(I) calculated according to Blessing (1987) ; _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% 5.0 _diffrn_reflns_number 8418 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0133 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 24.97 _reflns_number_total 8418 _reflns_number_gt 7965 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'STADI4 (STOE, 1996)' _computing_cell_refinement 'STADI4 (STOE, 1996)' _computing_data_reduction 'X-RED (STOE, 1996)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 (Farrugia, 1997)' _computing_publication_material 'local program' _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 w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+2.4073P] 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 8418 _refine_ls_number_parameters 621 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0229 _refine_ls_R_factor_gt 0.0202 _refine_ls_wR_factor_ref 0.0483 _refine_ls_wR_factor_gt 0.0465 _refine_ls_goodness_of_fit_ref 1.084 _refine_ls_restrained_S_all 1.095 _refine_ls_shift/su_max 0.003 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Hf1 Hf 0.712845(10) 0.731029(8) 0.735750(6) 0.02491(4) Uani 1 d . . . C1 C 0.5366(2) 0.7166(2) 0.63434(15) 0.0302(5) Uani 1 d . . . C2 C 0.6499(2) 0.7499(2) 0.60457(14) 0.0273(5) Uani 1 d . . . H2 H 0.6788 0.8192 0.5957 0.033 Uiso 1 calc R . . C3 C 0.7144(2) 0.6669(2) 0.58972(14) 0.0265(5) Uani 1 d . . . C4 C 0.6376(2) 0.5788(2) 0.61124(15) 0.0293(5) Uani 1 d . . . H4 H 0.6554 0.5108 0.6082 0.035 Uiso 1 calc R . . C5 C 0.5318(2) 0.6084(2) 0.63755(15) 0.0308(6) Uani 1 d . . . H5 H 0.4667 0.5631 0.6549 0.037 Uiso 1 calc R . . C6 C 0.6894(3) 0.8895(2) 0.80280(18) 0.0357(6) Uani 1 d . . . H6A H 0.715(3) 0.931(2) 0.7682(17) 0.032(7) Uiso 1 d . . . H6B H 0.622(3) 0.904(3) 0.8258(19) 0.047(9) Uiso 1 d . . . C7 C 0.7896(3) 0.8825(2) 0.85861(16) 0.0352(6) Uani 1 d . . . C71 C 0.7667(4) 0.8959(3) 0.94433(18) 0.0555(9) Uani 1 d . . . H71A H 0.8208 0.8622 0.9706 0.083 Uiso 1 calc R . . H71B H 0.6798 0.8607 0.9454 0.083 Uiso 1 calc R . . H71C H 0.7846 0.9736 0.9725 0.083 Uiso 1 calc R . . C8 C 0.8933(3) 0.8543(2) 0.83151(16) 0.0341(6) Uani 1 d . . . C81 C 0.9940(3) 0.8364(3) 0.88553(19) 0.0497(8) Uani 1 d . . . H81A H 1.0579 0.9049 0.9081 0.075 Uiso 1 calc R . . H81B H 1.0312 0.7815 0.8546 0.075 Uiso 1 calc R . . H81C H 0.9580 0.8111 0.9288 0.075 Uiso 1 calc R . . C9 C 0.9048(3) 0.8295(2) 0.74614(17) 0.0326(6) Uani 1 d . . . H9A H 0.884(2) 0.881(2) 0.7235(14) 0.016(6) Uiso 1 d . . . H9B H 0.977(3) 0.808(3) 0.7321(19) 0.050(9) Uiso 1 d . . . Si1 Si 0.40736(7) 0.78584(6) 0.64357(5) 0.03567(17) Uani 1 d . . . C11 C 0.3104(3) 0.7377(3) 0.5431(2) 0.0470(7) Uani 1 d . . . H11A H 0.2815 0.6581 0.5274 0.071 Uiso 1 calc R . . H11B H 0.3602 0.7608 0.5039 0.071 Uiso 1 calc R . . H11C H 0.2388 0.7690 0.5455 0.071 Uiso 1 calc R . . C12 C 0.4703(3) 0.9362(2) 0.6708(2) 0.0467(8) Uani 1 d . . . H12A H 0.4019 0.9713 0.6771 0.070 Uiso 1 calc R . . H12B H 0.5152 0.9560 0.6286 0.070 Uiso 1 calc R . . H12C H 0.5271 0.9605 0.7211 0.070 Uiso 1 calc R . . C13 C 0.3114(3) 0.7470(3) 0.7190(2) 0.0537(8) Uani 1 d . . . H13A H 0.2829 0.6675 0.7057 0.081 Uiso 1 calc R . . H13B H 0.2396 0.7778 0.7190 0.081 Uiso 1 calc R . . H13C H 0.3613 0.7753 0.7719 0.081 Uiso 1 calc R . . Si3 Si 0.85248(6) 0.66100(6) 0.53655(4) 0.03024(15) Uani 1 d . . . C31 C 0.7911(3) 0.5695(2) 0.43434(16) 0.0382(6) Uani 1 d . . . H31A H 0.7375 0.6022 0.4066 0.057 Uiso 1 calc R . . H31B H 0.7431 0.4989 0.4378 0.057 Uiso 1 calc R . . H31C H 0.8604 0.5593 0.4047 0.057 Uiso 1 calc R . . C32 C 0.9587(3) 0.6001(3) 0.58745(18) 0.0461(8) Uani 1 d . . . H32A H 0.9137 0.5273 0.5888 0.069 Uiso 1 calc R . . H32B H 0.9888 0.6464 0.6421 0.069 Uiso 1 calc R . . H32C H 1.0292 0.5945 0.5582 0.069 Uiso 1 calc R . . C33 C 0.9300(3) 0.7989(3) 0.5298(2) 0.0493(8) Uani 1 d . . . H33A H 0.9979 0.7942 0.4979 0.074 Uiso 1 calc R . . H33B H 0.9632 0.8472 0.5835 0.074 Uiso 1 calc R . . H33C H 0.8697 0.8281 0.5043 0.074 Uiso 1 calc R . . O1 O 0.6915(2) 0.61246(18) 0.80181(13) 0.0571(6) Uani 1 d . . . C14 C 0.8027(4) 0.5720(3) 0.8038(3) 0.0767(14) Uani 1 d . . . H14A H 0.8424 0.5911 0.8598 0.092 Uiso 1 calc R . . H14B H 0.8624 0.6086 0.7741 0.092 Uiso 1 calc R . . C15 C 0.7748(5) 0.4511(3) 0.7682(3) 0.105(2) Uani 1 d . . . H15A H 0.7227 0.4142 0.8008 0.158 Uiso 1 calc R . . H15B H 0.8526 0.4288 0.7669 0.158 Uiso 1 calc R . . H15C H 0.7309 0.4312 0.7138 0.158 Uiso 1 calc R . . C16 C 0.5996(5) 0.5771(4) 0.8504(3) 0.100(2) Uani 1 d . . . H16A H 0.5704 0.4967 0.8329 0.120 Uiso 1 calc R . . H16B H 0.6386 0.5992 0.9068 0.120 Uiso 1 calc R . . C17 C 0.4942(5) 0.6230(4) 0.8447(3) 0.0931(17) Uani 1 d . . . H17A H 0.5223 0.7026 0.8636 0.140 Uiso 1 calc R . . H17B H 0.4341 0.5966 0.8777 0.140 Uiso 1 calc R . . H17C H 0.4549 0.6009 0.7891 0.140 Uiso 1 calc R . . B1 B 0.7944(3) 0.7936(2) 1.18616(17) 0.0297(6) Uani 1 d D . . C111 C 0.8218(2) 0.6730(2) 1.15602(15) 0.0294(5) Uani 1 d D . . C112 C 0.8559(3) 0.6139(2) 1.20538(17) 0.0363(6) Uani 1 d D . . C113 C 0.8851(3) 0.5156(2) 1.17826(19) 0.0422(7) Uani 1 d D . . C114 C 0.8858(3) 0.4723(2) 1.09870(19) 0.0406(7) Uani 1 d D . . C115 C 0.8572(2) 0.5287(2) 1.04668(17) 0.0334(6) Uani 1 d D . . C116 C 0.8275(2) 0.6259(2) 1.07650(16) 0.0304(6) Uani 1 d D . . C121 C 0.7483(2) 0.8189(2) 1.27590(15) 0.0307(6) Uani 1 d D . . C122 C 0.7843(2) 0.9162(2) 1.33602(16) 0.0330(6) Uani 1 d D . . C123 C 0.7330(3) 0.9368(2) 1.40630(16) 0.0357(6) Uani 1 d D . . C124 C 0.6385(3) 0.8592(2) 1.41922(16) 0.0370(6) Uani 1 d D . . C125 C 0.5989(3) 0.7599(2) 1.36225(17) 0.0378(6) Uani 1 d D . . C126 C 0.6542(3) 0.7430(2) 1.29408(17) 0.0349(6) Uani 1 d D . . C131 C 0.6720(2) 0.8056(2) 1.13161(15) 0.0304(6) Uani 1 d D . . C132 C 0.6533(3) 0.9073(2) 1.13275(16) 0.0344(6) Uani 1 d D . . C133 C 0.5508(3) 0.9242(2) 1.09376(17) 0.0403(7) Uani 1 d D . . C134 C 0.4572(3) 0.8368(3) 1.05114(18) 0.0445(7) Uani 1 d D . . C135 C 0.4691(3) 0.7342(3) 1.04843(17) 0.0420(7) Uani 1 d D . . C136 C 0.5734(3) 0.7207(2) 1.08701(16) 0.0347(6) Uani 1 d D . . C141 C 0.9234(2) 0.8787(2) 1.17659(16) 0.0320(6) Uani 1 d D . . H14C H 0.9231 0.8745 1.1193 0.038 Uiso 1 calc R . . H14D H 0.9215 0.9537 1.2049 0.038 Uiso 1 calc R . . C142 C 1.0432(3) 0.8595(2) 1.20724(17) 0.0356(6) Uani 1 d D . . C143 C 1.0862(3) 0.8852(3) 1.28804(19) 0.0476(7) Uani 1 d D . . H143 H 1.0380 0.9154 1.3257 0.057 Uiso 1 calc R . . C144 C 1.1975(3) 0.8682(3) 1.3155(2) 0.0596(9) Uani 1 d D . . H144 H 1.2247 0.8876 1.3713 0.072 Uiso 1 calc R . . C145 C 1.2683(3) 0.8236(3) 1.2628(3) 0.0600(10) Uani 1 d D . . H145 H 1.3444 0.8115 1.2813 0.072 Uiso 1 calc R . . C146 C 1.2277(3) 0.7969(3) 1.1828(3) 0.0603(10) Uani 1 d D . . H146 H 1.2761 0.7656 1.1458 0.072 Uiso 1 calc R . . C147 C 1.1171(3) 0.8145(2) 1.1548(2) 0.0469(8) Uani 1 d D . . H147 H 1.0913 0.7955 1.0989 0.056 Uiso 1 calc R . . F112 F 0.86311(18) 0.65203(15) 1.28563(10) 0.0502(4) Uani 1 d . . . F113 F 0.9149(2) 0.46211(17) 1.23060(13) 0.0632(6) Uani 1 d . . . F114 F 0.91384(19) 0.37641(14) 1.07122(13) 0.0571(5) Uani 1 d . . . F115 F 0.85797(15) 0.48837(13) 0.96799(10) 0.0430(4) Uani 1 d . . . F116 F 0.80183(15) 0.67696(12) 1.02084(9) 0.0369(4) Uani 1 d . . . F122 F 0.87118(16) 1.00215(13) 1.32842(10) 0.0442(4) Uani 1 d . . . F123 F 0.77314(18) 1.03422(14) 1.46110(10) 0.0516(5) Uani 1 d . . . F124 F 0.58435(18) 0.88047(16) 1.48542(10) 0.0509(4) Uani 1 d . . . F125 F 0.50638(17) 0.68170(16) 1.37356(11) 0.0553(5) Uani 1 d . . . F126 F 0.60783(17) 0.64340(14) 1.24110(11) 0.0505(5) Uani 1 d . . . F132 F 0.73811(16) 0.99909(13) 1.17641(10) 0.0445(4) Uani 1 d . . . F133 F 0.54289(19) 1.02639(16) 1.09848(12) 0.0558(5) Uani 1 d . . . F134 F 0.35550(17) 0.8508(2) 1.01390(12) 0.0640(6) Uani 1 d . . . F135 F 0.37597(16) 0.64706(17) 1.00865(11) 0.0570(5) Uani 1 d . . . F136 F 0.57385(15) 0.61547(13) 1.07904(10) 0.0443(4) 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 Hf1 0.02611(6) 0.02031(6) 0.02732(6) 0.00724(4) 0.00199(4) 0.00403(4) C1 0.0257(13) 0.0298(13) 0.0329(13) 0.0060(11) 0.0002(10) 0.0073(11) C2 0.0254(13) 0.0274(13) 0.0294(13) 0.0081(10) 0.0003(10) 0.0084(10) C3 0.0217(12) 0.0293(13) 0.0268(12) 0.0048(10) -0.0004(10) 0.0076(10) C4 0.0285(13) 0.0218(12) 0.0325(13) 0.0014(10) -0.0005(10) 0.0051(10) C5 0.0242(13) 0.0280(13) 0.0341(14) 0.0058(11) -0.0008(10) -0.0001(10) C6 0.0376(16) 0.0316(15) 0.0369(15) 0.0057(12) 0.0086(12) 0.0102(12) C7 0.0454(16) 0.0222(13) 0.0314(14) 0.0031(11) 0.0012(12) 0.0021(12) C71 0.074(2) 0.053(2) 0.0311(16) 0.0035(14) 0.0063(15) 0.0104(18) C8 0.0381(15) 0.0199(12) 0.0363(14) 0.0051(11) -0.0063(12) -0.0012(11) C81 0.0509(19) 0.0394(17) 0.0486(18) 0.0079(14) -0.0162(15) 0.0044(14) C9 0.0283(14) 0.0283(14) 0.0384(15) 0.0073(12) 0.0010(11) 0.0056(11) Si1 0.0236(4) 0.0335(4) 0.0506(5) 0.0100(3) 0.0052(3) 0.0108(3) C11 0.0308(15) 0.0448(18) 0.065(2) 0.0177(15) -0.0034(14) 0.0102(13) C12 0.0357(16) 0.0349(16) 0.070(2) 0.0113(15) 0.0007(15) 0.0158(13) C13 0.0426(18) 0.052(2) 0.066(2) 0.0109(17) 0.0226(16) 0.0138(15) Si3 0.0245(4) 0.0336(4) 0.0302(4) 0.0043(3) 0.0032(3) 0.0083(3) C31 0.0418(16) 0.0408(16) 0.0316(14) 0.0084(12) 0.0041(12) 0.0122(13) C32 0.0366(16) 0.063(2) 0.0405(16) 0.0036(14) 0.0020(13) 0.0293(15) C33 0.0397(17) 0.0469(18) 0.0544(19) 0.0115(15) 0.0109(14) -0.0006(14) O1 0.0771(17) 0.0385(12) 0.0498(13) 0.0270(10) -0.0122(12) -0.0061(11) C14 0.082(3) 0.047(2) 0.088(3) 0.034(2) -0.040(2) -0.008(2) C15 0.106(4) 0.040(2) 0.152(5) 0.028(3) -0.061(3) 0.006(2) C16 0.087(3) 0.110(4) 0.078(3) 0.068(3) -0.035(3) -0.055(3) C17 0.120(4) 0.088(3) 0.054(2) 0.016(2) 0.027(3) -0.008(3) B1 0.0302(15) 0.0244(14) 0.0317(15) 0.0069(12) 0.0046(12) 0.0026(12) C111 0.0256(13) 0.0273(13) 0.0344(14) 0.0101(11) 0.0064(10) 0.0030(10) C112 0.0338(15) 0.0409(16) 0.0381(15) 0.0171(12) 0.0098(12) 0.0089(12) C113 0.0395(16) 0.0431(17) 0.0571(19) 0.0298(15) 0.0149(14) 0.0164(13) C114 0.0356(15) 0.0297(15) 0.0619(19) 0.0163(14) 0.0136(14) 0.0131(12) C115 0.0248(13) 0.0308(14) 0.0417(15) 0.0056(12) 0.0082(11) 0.0051(11) C116 0.0253(13) 0.0275(13) 0.0382(14) 0.0117(11) 0.0040(11) 0.0036(10) C121 0.0275(13) 0.0307(14) 0.0332(14) 0.0092(11) 0.0051(11) 0.0058(11) C122 0.0323(14) 0.0330(14) 0.0338(14) 0.0100(11) 0.0049(11) 0.0079(11) C123 0.0429(16) 0.0367(15) 0.0285(13) 0.0061(11) 0.0021(12) 0.0167(13) C124 0.0411(16) 0.0508(17) 0.0314(14) 0.0197(13) 0.0112(12) 0.0247(14) C125 0.0330(15) 0.0421(16) 0.0447(16) 0.0222(13) 0.0108(12) 0.0094(12) C126 0.0319(14) 0.0317(14) 0.0390(15) 0.0085(12) 0.0052(12) 0.0053(11) C131 0.0320(14) 0.0309(14) 0.0289(13) 0.0079(11) 0.0104(11) 0.0079(11) C132 0.0353(15) 0.0357(15) 0.0326(14) 0.0086(12) 0.0113(11) 0.0091(12) C133 0.0466(17) 0.0453(17) 0.0401(16) 0.0181(13) 0.0192(13) 0.0231(14) C134 0.0333(16) 0.068(2) 0.0398(16) 0.0185(15) 0.0115(13) 0.0226(15) C135 0.0291(15) 0.0546(19) 0.0369(15) 0.0068(14) 0.0080(12) 0.0057(13) C136 0.0317(14) 0.0344(15) 0.0366(14) 0.0077(12) 0.0094(11) 0.0066(12) C141 0.0326(14) 0.0270(13) 0.0337(14) 0.0075(11) 0.0074(11) 0.0027(11) C142 0.0309(14) 0.0241(13) 0.0476(16) 0.0092(12) 0.0105(12) -0.0018(11) C143 0.0397(17) 0.0470(18) 0.0502(18) 0.0066(14) 0.0022(14) 0.0091(14) C144 0.047(2) 0.052(2) 0.072(2) 0.0106(18) -0.0103(17) 0.0111(16) C145 0.0349(18) 0.0410(19) 0.103(3) 0.0227(19) 0.0011(19) 0.0085(14) C146 0.046(2) 0.048(2) 0.099(3) 0.029(2) 0.037(2) 0.0181(16) C147 0.0430(18) 0.0396(17) 0.061(2) 0.0152(15) 0.0244(15) 0.0102(14) F112 0.0640(12) 0.0603(12) 0.0387(9) 0.0244(8) 0.0131(8) 0.0266(9) F113 0.0800(14) 0.0669(13) 0.0731(13) 0.0477(11) 0.0260(11) 0.0427(11) F114 0.0629(12) 0.0377(10) 0.0830(14) 0.0212(9) 0.0238(10) 0.0279(9) F115 0.0439(10) 0.0376(9) 0.0446(9) 0.0020(7) 0.0111(7) 0.0136(7) F116 0.0457(9) 0.0349(8) 0.0329(8) 0.0099(7) 0.0065(7) 0.0150(7) F122 0.0473(10) 0.0314(9) 0.0429(9) 0.0020(7) 0.0116(8) -0.0034(7) F123 0.0697(12) 0.0434(10) 0.0362(9) 0.0000(8) 0.0101(8) 0.0155(9) F124 0.0627(12) 0.0660(12) 0.0392(9) 0.0237(9) 0.0246(8) 0.0308(10) F125 0.0487(11) 0.0584(12) 0.0618(12) 0.0268(10) 0.0244(9) 0.0029(9) F126 0.0497(10) 0.0354(9) 0.0513(10) 0.0024(8) 0.0163(8) -0.0100(8) F132 0.0502(10) 0.0284(8) 0.0528(10) 0.0062(7) 0.0066(8) 0.0119(7) F133 0.0651(12) 0.0560(12) 0.0645(12) 0.0272(10) 0.0209(10) 0.0363(10) F134 0.0421(11) 0.0996(17) 0.0631(12) 0.0341(12) 0.0043(9) 0.0319(11) F135 0.0288(9) 0.0703(13) 0.0569(11) 0.0051(10) 0.0000(8) -0.0004(9) F136 0.0344(9) 0.0312(9) 0.0575(10) 0.0039(8) 0.0032(8) 0.0002(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 Hf1 O1 2.148(2) . ? Hf1 C6 2.199(3) . ? Hf1 C9 2.207(3) . ? Hf1 C2 2.441(2) . ? Hf1 C7 2.466(3) . ? Hf1 C8 2.473(3) . ? Hf1 C3 2.482(2) . ? Hf1 C4 2.488(2) . ? Hf1 C1 2.491(3) . ? Hf1 C5 2.495(2) . ? C1 C2 1.425(4) . ? C1 C5 1.427(4) . ? C1 Si1 1.874(3) . ? C2 C3 1.423(3) . ? C2 H2 0.9500 . ? C3 C4 1.426(4) . ? C3 Si3 1.870(3) . ? C4 C5 1.403(4) . ? C6 C7 1.466(4) . ? C6 H6A 0.93(3) . ? C6 H6B 0.91(3) . ? C7 C8 1.377(4) . ? C7 C71 1.514(4) . ? C8 C9 1.469(4) . ? C8 C81 1.515(4) . ? C9 H9A 0.93(3) . ? C9 H9B 0.94(3) . ? Si1 C12 1.860(3) . ? Si1 C13 1.860(3) . ? Si1 C11 1.871(3) . ? Si3 C33 1.859(3) . ? Si3 C31 1.860(3) . ? Si3 C32 1.868(3) . ? O1 C16 1.453(5) . ? O1 C14 1.462(5) . ? C14 C15 1.501(5) . ? C16 C17 1.451(7) . ? B1 C111 1.646(4) . ? B1 C141 1.659(4) . ? B1 C121 1.667(4) . ? B1 C131 1.670(4) . ? C111 C116 1.385(4) . ? C111 C112 1.388(4) . ? C112 F112 1.355(3) . ? C112 C113 1.381(4) . ? C113 F113 1.354(3) . ? C113 C114 1.365(4) . ? C114 F114 1.347(3) . ? C114 C115 1.375(4) . ? C115 F115 1.346(3) . ? C115 C116 1.377(4) . ? C116 F116 1.365(3) . ? C121 C122 1.385(4) . ? C121 C126 1.391(4) . ? C122 F122 1.353(3) . ? C122 C123 1.387(4) . ? C123 F123 1.345(3) . ? C123 C124 1.367(4) . ? C124 F124 1.344(3) . ? C124 C125 1.378(4) . ? C125 F125 1.347(3) . ? C125 C126 1.377(4) . ? C126 F126 1.357(3) . ? C131 C136 1.391(4) . ? C131 C132 1.396(4) . ? C132 F132 1.355(3) . ? C132 C133 1.381(4) . ? C133 F133 1.349(3) . ? C133 C134 1.366(5) . ? C134 F134 1.341(3) . ? C134 C135 1.375(5) . ? C135 F135 1.349(3) . ? C135 C136 1.374(4) . ? C136 F136 1.356(3) . ? C141 C142 1.505(4) . ? C142 C143 1.388(4) . ? C142 C147 1.392(4) . ? C143 C144 1.388(5) . ? C144 C145 1.368(5) . ? C145 C146 1.367(5) . ? C146 C147 1.387(5) . ? 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 O1 Hf1 C6 113.86(11) . . ? O1 Hf1 C9 114.59(10) . . ? C6 Hf1 C9 81.38(11) . . ? O1 Hf1 C2 141.06(9) . . ? C6 Hf1 C2 95.13(10) . . ? C9 Hf1 C2 94.23(10) . . ? O1 Hf1 C7 91.88(9) . . ? C6 Hf1 C7 36.05(10) . . ? C9 Hf1 C7 63.64(10) . . ? C2 Hf1 C7 125.38(9) . . ? O1 Hf1 C8 92.32(9) . . ? C6 Hf1 C8 63.50(10) . . ? C9 Hf1 C8 36.01(10) . . ? C2 Hf1 C8 124.77(9) . . ? C7 Hf1 C8 32.39(10) . . ? O1 Hf1 C3 117.97(9) . . ? C6 Hf1 C3 126.70(10) . . ? C9 Hf1 C3 88.05(9) . . ? C2 Hf1 C3 33.58(8) . . ? C7 Hf1 C3 146.12(9) . . ? C8 Hf1 C3 123.98(9) . . ? O1 Hf1 C4 88.43(9) . . ? C6 Hf1 C4 144.17(10) . . ? C9 Hf1 C4 115.72(10) . . ? C2 Hf1 C4 54.44(9) . . ? C7 Hf1 C4 179.36(9) . . ? C8 Hf1 C4 147.04(9) . . ? C3 Hf1 C4 33.35(8) . . ? O1 Hf1 C1 118.00(9) . . ? C6 Hf1 C1 88.88(10) . . ? C9 Hf1 C1 125.84(10) . . ? C2 Hf1 C1 33.57(8) . . ? C7 Hf1 C1 124.88(9) . . ? C8 Hf1 C1 146.06(9) . . ? C3 Hf1 C1 56.63(8) . . ? C4 Hf1 C1 55.39(8) . . ? O1 Hf1 C5 88.57(9) . . ? C6 Hf1 C5 116.33(10) . . ? C9 Hf1 C5 143.21(10) . . ? C2 Hf1 C5 54.30(9) . . ? C7 Hf1 C5 147.86(9) . . ? C8 Hf1 C5 179.07(9) . . ? C3 Hf1 C5 55.29(8) . . ? C4 Hf1 C5 32.70(9) . . ? C1 Hf1 C5 33.25(9) . . ? C2 C1 C5 104.4(2) . . ? C2 C1 Si1 127.0(2) . . ? C5 C1 Si1 127.2(2) . . ? C2 C1 Hf1 71.28(14) . . ? C5 C1 Hf1 73.50(14) . . ? Si1 C1 Hf1 129.86(13) . . ? C3 C2 C1 111.8(2) . . ? C3 C2 Hf1 74.79(14) . . ? C1 C2 Hf1 75.15(14) . . ? C2 C3 C4 104.6(2) . . ? C2 C3 Si3 128.59(19) . . ? C4 C3 Si3 125.90(19) . . ? C2 C3 Hf1 71.63(14) . . ? C4 C3 Hf1 73.55(14) . . ? Si3 C3 Hf1 127.39(11) . . ? C5 C4 C3 109.4(2) . . ? C5 C4 Hf1 73.91(14) . . ? C3 C4 Hf1 73.10(14) . . ? C4 C5 C1 109.7(2) . . ? C4 C5 Hf1 73.38(14) . . ? C1 C5 Hf1 73.24(14) . . ? C7 C6 Hf1 81.94(16) . . ? C7 C6 H6A 114.9(18) . . ? Hf1 C6 H6A 100.3(17) . . ? C7 C6 H6B 114(2) . . ? Hf1 C6 H6B 128(2) . . ? H6A C6 H6B 114(3) . . ? C8 C7 C6 120.6(3) . . ? C8 C7 C71 122.5(3) . . ? C6 C7 C71 116.6(3) . . ? C8 C7 Hf1 74.09(15) . . ? C6 C7 Hf1 62.00(14) . . ? C71 C7 Hf1 132.6(2) . . ? C7 C8 C9 120.7(2) . . ? C7 C8 C81 122.6(3) . . ? C9 C8 C81 116.5(3) . . ? C7 C8 Hf1 73.53(15) . . ? C9 C8 Hf1 62.06(14) . . ? C81 C8 Hf1 133.78(19) . . ? C8 C9 Hf1 81.94(16) . . ? C8 C9 H9A 111.8(15) . . ? Hf1 C9 H9A 95.9(15) . . ? C8 C9 H9B 116(2) . . ? Hf1 C9 H9B 130(2) . . ? H9A C9 H9B 116(2) . . ? C12 Si1 C13 110.29(16) . . ? C12 Si1 C11 109.56(15) . . ? C13 Si1 C11 109.58(16) . . ? C12 Si1 C1 110.45(13) . . ? C13 Si1 C1 110.62(14) . . ? C11 Si1 C1 106.24(13) . . ? C33 Si3 C31 109.21(14) . . ? C33 Si3 C32 112.79(16) . . ? C31 Si3 C32 109.01(14) . . ? C33 Si3 C3 109.92(13) . . ? C31 Si3 C3 105.87(12) . . ? C32 Si3 C3 109.80(13) . . ? C16 O1 C14 116.7(3) . . ? C16 O1 Hf1 133.3(3) . . ? C14 O1 Hf1 109.6(2) . . ? O1 C14 C15 112.5(3) . . ? C17 C16 O1 112.1(3) . . ? C111 B1 C141 103.8(2) . . ? C111 B1 C121 113.7(2) . . ? C141 B1 C121 116.3(2) . . ? C111 B1 C131 112.9(2) . . ? C141 B1 C131 110.6(2) . . ? C121 B1 C131 99.8(2) . . ? C116 C111 C112 112.5(2) . . ? C116 C111 B1 121.5(2) . . ? C112 C111 B1 125.5(2) . . ? F112 C112 C113 115.7(2) . . ? F112 C112 C111 120.2(3) . . ? C113 C112 C111 124.1(3) . . ? F113 C113 C114 119.5(3) . . ? F113 C113 C112 120.2(3) . . ? C114 C113 C112 120.3(3) . . ? F114 C114 C113 121.0(3) . . ? F114 C114 C115 120.3(3) . . ? C113 C114 C115 118.6(3) . . ? F115 C115 C114 119.9(2) . . ? F115 C115 C116 121.1(2) . . ? C114 C115 C116 118.9(3) . . ? F116 C116 C115 115.0(2) . . ? F116 C116 C111 119.5(2) . . ? C115 C116 C111 125.5(2) . . ? C122 C121 C126 112.2(2) . . ? C122 C121 B1 126.8(2) . . ? C126 C121 B1 120.7(2) . . ? F122 C122 C121 121.3(2) . . ? F122 C122 C123 114.2(2) . . ? C121 C122 C123 124.4(3) . . ? F123 C123 C124 119.4(2) . . ? F123 C123 C122 120.3(3) . . ? C124 C123 C122 120.2(3) . . ? F124 C124 C123 120.5(3) . . ? F124 C124 C125 121.0(3) . . ? C123 C124 C125 118.5(2) . . ? F125 C125 C126 121.1(3) . . ? F125 C125 C124 119.8(3) . . ? C126 C125 C124 119.1(3) . . ? F126 C126 C125 114.7(2) . . ? F126 C126 C121 119.6(2) . . ? C125 C126 C121 125.6(3) . . ? C136 C131 C132 112.1(3) . . ? C136 C131 B1 126.2(2) . . ? C132 C131 B1 121.5(2) . . ? F132 C132 C133 115.0(3) . . ? F132 C132 C131 119.8(2) . . ? C133 C132 C131 125.1(3) . . ? F133 C133 C134 120.4(3) . . ? F133 C133 C132 120.1(3) . . ? C134 C133 C132 119.6(3) . . ? F134 C134 C133 120.9(3) . . ? F134 C134 C135 120.8(3) . . ? C133 C134 C135 118.3(3) . . ? F135 C135 C136 120.4(3) . . ? F135 C135 C134 119.1(3) . . ? C136 C135 C134 120.4(3) . . ? F136 C136 C135 114.5(2) . . ? F136 C136 C131 121.0(2) . . ? C135 C136 C131 124.5(3) . . ? C142 C141 B1 116.1(2) . . ? C143 C142 C147 116.5(3) . . ? C143 C142 C141 122.6(3) . . ? C147 C142 C141 120.9(3) . . ? C144 C143 C142 122.1(3) . . ? C145 C144 C143 120.3(4) . . ? C146 C145 C144 118.8(3) . . ? C145 C146 C147 121.2(3) . . ? C146 C147 C142 121.1(3) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.620 _refine_diff_density_min -0.486 _refine_diff_density_rms 0.057 #===END data_s92 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C34 H28 B F15 Si2 Zr' _chemical_formula_weightical 879.77 _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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.068(7) _cell_length_b 11.442(16) _cell_length_c 16.218(17) _cell_angle_alpha 96.79(3) _cell_angle_beta 105.19(5) _cell_angle_gamma 94.15(6) _cell_volume 1780(3) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Needle _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method ? _exptl_crystal_F_000 880 _exptl_absorpt_coefficient_mu 0.481 _exptl_absorpt_correction_type DIFABS _exptl_absorpt_correction_T_min 0.872 _exptl_absorpt_correction_T_max 1.171 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'FAST TV Area detector' _diffrn_measurement_method 'Omega scans' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 5906 _diffrn_reflns_av_R_equivalents 0.0778 _diffrn_reflns_av_sigmaI/netI 0.1976 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 25.11 _reflns_number_total 4532 _reflns_number_observed 2222 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'MADNES (Pflugrath, 1989)' _computing_cell_refinement MADNES _computing_data_reduction ABSURD _computing_structure_solution 'SHELXS-96 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-96 (Sheldrick, 1996)' _computing_molecular_graphics 'SNOOPI (Davies, Prout)' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. 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^)+(0.0620P)^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 4532 _refine_ls_number_parameters 485 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_obs 0.0734 _refine_ls_wR_factor_all 0.1720 _refine_ls_wR_factor_obs 0.1534 _refine_ls_goodness_of_fit_all 0.831 _refine_ls_goodness_of_fit_obs 1.119 _refine_ls_restrained_S_all 0.831 _refine_ls_restrained_S_obs 1.119 _refine_ls_shift/esd_max 0.010 _refine_ls_shift/esd_mean 0.001 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 Zr1 Zr 0.02294(12) 0.20223(9) 0.24460(7) 0.0362(3) Uani 1 d . . Si1 Si -0.2799(3) -0.0539(3) 0.19438(19) 0.0381(8) Uani 1 d . . Si2 Si 0.0754(3) 0.2543(3) 0.49768(19) 0.0411(8) Uani 1 d . . F32 F 0.0993(6) 0.4122(5) 0.2938(3) 0.0419(15) Uani 1 d . . F42 F -0.2024(6) 0.5384(5) 0.2616(3) 0.0445(16) Uani 1 d . . F22 F 0.1925(6) -0.0141(5) 0.3389(4) 0.0469(16) Uani 1 d . . F23 F 0.4515(6) -0.0458(5) 0.4131(4) 0.0503(17) Uani 1 d . . F33 F 0.2987(7) 0.5945(5) 0.3599(4) 0.0557(18) Uani 1 d . . F44 F -0.6694(6) 0.4807(5) 0.1113(4) 0.0606(19) Uani 1 d . . F36 F -0.0696(7) 0.5985(5) 0.0497(4) 0.0534(17) Uani 1 d . . F46 F -0.3523(6) 0.2970(5) -0.0072(4) 0.0535(17) Uani 1 d . . F35 F 0.1351(7) 0.7767(5) 0.1139(5) 0.069(2) Uani 1 d . . F24 F 0.6585(7) 0.1304(6) 0.4336(4) 0.0644(19) Uani 1 d . . F26 F 0.3437(6) 0.3658(5) 0.2905(4) 0.0625(19) Uani 1 d . . F25 F 0.6003(6) 0.3374(6) 0.3730(5) 0.071(2) Uani 1 d . . F34 F 0.3169(7) 0.7757(5) 0.2687(5) 0.070(2) Uani 1 d . . F45 F -0.6109(7) 0.3377(5) -0.0154(4) 0.0605(19) Uani 1 d . . F43 F -0.4615(7) 0.5810(5) 0.2514(4) 0.0612(19) Uani 1 d . . C12 C -0.0656(11) 0.2745(9) 0.1153(6) 0.039(3) Uani 1 d . . H12 H -0.1385 0.2202 0.0733 0.046 Uiso 1 calc R . C31 C 0.0078(10) 0.5009(8) 0.1709(6) 0.027(2) Uani 1 d . . C22 C 0.2918(11) 0.0780(9) 0.3473(6) 0.035(3) Uani 1 d . . C2 C -0.0719(10) 0.0876(8) 0.3428(6) 0.034(3) Uani 1 d . . H2 H -0.0321 0.0224 0.3637 0.040 Uiso 1 calc R . C25 C 0.5005(11) 0.2505(10) 0.3664(7) 0.045(3) Uani 1 d . . C32 C 0.1051(11) 0.5058(8) 0.2460(7) 0.035(3) Uani 1 d . . C42 C -0.2987(11) 0.4893(9) 0.1896(7) 0.035(3) Uani 1 d . . C21 C 0.2522(10) 0.1810(9) 0.3165(6) 0.035(3) Uani 1 d . . C1 C -0.1779(11) 0.0781(8) 0.2646(6) 0.033(3) Uani 1 d . . C34 C 0.2159(12) 0.6877(8) 0.2345(8) 0.042(3) Uani 1 d . . C35 C 0.1248(13) 0.6870(9) 0.1574(8) 0.045(3) Uani 1 d . . C5 C -0.2133(10) 0.1999(8) 0.2629(6) 0.033(3) Uani 1 d . . H5 H -0.2808 0.2262 0.2202 0.040 Uiso 1 calc R . C4 C -0.1288(11) 0.2682(8) 0.3356(6) 0.038(3) Uani 1 d . . H4 H -0.1348 0.3484 0.3499 0.045 Uiso 1 calc R . C24 C 0.5270(13) 0.1456(10) 0.3936(7) 0.046(3) Uani 1 d . . C44 C -0.5389(12) 0.4593(10) 0.1165(8) 0.047(3) Uani 1 d . . C26 C 0.3645(12) 0.2644(9) 0.3251(7) 0.043(3) Uani 1 d . . C23 C 0.4225(11) 0.0578(10) 0.3854(7) 0.041(3) Uani 1 d . . C41 C -0.2641(11) 0.4167(8) 0.1275(7) 0.035(3) Uani 1 d . . C46 C -0.3723(12) 0.3676(9) 0.0586(7) 0.041(3) Uani 1 d . . C7 C -0.1703(12) -0.1756(8) 0.1910(8) 0.057(3) Uani 1 d . . H7A H -0.1145 -0.1632 0.1524 0.085 Uiso 1 calc R . H7B H -0.2280 -0.2495 0.1710 0.085 Uiso 1 calc R . H7C H -0.1115 -0.1776 0.2478 0.085 Uiso 1 calc R . C3 C -0.0314(11) 0.2036(9) 0.3865(6) 0.036(3) Uani 1 d . . C8 C -0.4286(11) -0.1010(9) 0.2368(7) 0.053(3) Uani 1 d . . H8A H -0.3937 -0.1248 0.2926 0.080 Uiso 1 calc R . H8B H -0.4855 -0.1663 0.1979 0.080 Uiso 1 calc R . H8C H -0.4826 -0.0360 0.2416 0.080 Uiso 1 calc R . C45 C -0.5094(12) 0.3881(9) 0.0545(7) 0.044(3) Uani 1 d . . C33 C 0.2111(12) 0.5951(9) 0.2832(8) 0.043(3) Uani 1 d . . C10 C -0.0442(12) 0.2679(9) 0.5664(6) 0.052(3) Uani 1 d . . H10A H 0.0069 0.3004 0.6243 0.078 Uiso 1 calc R . H10B H -0.0897 0.1912 0.5663 0.078 Uiso 1 calc R . H10C H -0.1122 0.3193 0.5443 0.078 Uiso 1 calc R . C36 C 0.0199(12) 0.5971(9) 0.1269(7) 0.039(3) Uani 1 d . . B1 B -0.1086(14) 0.3961(10) 0.1365(7) 0.037(3) Uani 1 d . . C6 C -0.3579(12) -0.0139(10) 0.0874(6) 0.057(3) Uani 1 d . . H6A H -0.4142 0.0492 0.0928 0.085 Uiso 1 calc R . H6B H -0.4143 -0.0815 0.0509 0.085 Uiso 1 calc R . H6C H -0.2861 0.0114 0.0624 0.085 Uiso 1 calc R . C11 C 0.1724(12) 0.4008(9) 0.5016(7) 0.060(4) Uani 1 d . . H11A H 0.2147 0.4343 0.5607 0.090 Uiso 1 calc R . H11B H 0.1097 0.4528 0.4742 0.090 Uiso 1 calc R . H11C H 0.2428 0.3907 0.4721 0.090 Uiso 1 calc R . C43 C -0.4326(13) 0.5108(9) 0.1881(7) 0.045(3) Uani 1 d . . C9 C 0.1946(12) 0.1417(10) 0.5346(7) 0.060(4) Uani 1 d . . H9A H 0.2773 0.1550 0.5165 0.091 Uiso 1 calc R . H9B H 0.1496 0.0639 0.5098 0.091 Uiso 1 calc R . H9C H 0.2183 0.1484 0.5964 0.091 Uiso 1 calc R . C14 C 0.1181(12) 0.1417(9) 0.1203(7) 0.045(3) Uani 1 d . . C13 C 0.0721(11) 0.2506(8) 0.1146(6) 0.037(3) Uani 1 d . . H13 H 0.1334 0.3126 0.1099 0.045 Uiso 1 calc R . C15 C 0.0299(12) 0.0520(9) 0.1395(7) 0.045(3) Uani 1 d . . H15A H 0.0749 -0.0151 0.1604 0.054 Uiso 1 calc R . H15B H -0.0569 0.0277 0.0956 0.054 Uiso 1 calc R . C16 C 0.2666(12) 0.1259(10) 0.1211(7) 0.060(4) Uani 1 d . . H16A H 0.3197 0.2020 0.1327 0.090 Uiso 1 calc R . H16B H 0.2689 0.0864 0.0659 0.090 Uiso 1 calc R . H16C H 0.3053 0.0793 0.1652 0.090 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 Zr1 0.0318(7) 0.0292(6) 0.0507(7) 0.0082(5) 0.0149(5) 0.0064(5) Si1 0.032(2) 0.0336(17) 0.0465(19) 0.0032(14) 0.0081(15) 0.0016(14) Si2 0.039(2) 0.0437(19) 0.0417(19) 0.0066(15) 0.0129(15) 0.0019(16) F32 0.028(4) 0.034(3) 0.065(4) 0.014(3) 0.014(3) -0.002(3) F42 0.042(4) 0.037(3) 0.050(4) -0.003(3) 0.009(3) 0.006(3) F22 0.039(4) 0.042(4) 0.069(4) 0.019(3) 0.025(3) 0.011(3) F23 0.042(4) 0.055(4) 0.055(4) 0.010(3) 0.010(3) 0.019(3) F33 0.041(4) 0.046(4) 0.072(5) -0.005(3) 0.009(4) -0.002(3) F44 0.029(4) 0.051(4) 0.106(5) 0.014(4) 0.022(4) 0.013(3) F36 0.057(5) 0.037(4) 0.073(5) 0.024(3) 0.021(4) 0.007(3) F46 0.049(5) 0.052(4) 0.054(4) -0.002(3) 0.007(3) 0.005(3) F35 0.068(5) 0.028(4) 0.130(6) 0.028(4) 0.054(5) 0.010(3) F24 0.027(4) 0.076(5) 0.089(5) 0.010(4) 0.013(4) 0.011(4) F26 0.040(5) 0.040(4) 0.118(6) 0.021(4) 0.035(4) 0.006(3) F25 0.023(4) 0.054(4) 0.139(6) 0.004(4) 0.031(4) -0.004(3) F34 0.042(5) 0.038(4) 0.132(6) -0.002(4) 0.038(4) -0.011(3) F45 0.037(5) 0.057(4) 0.078(5) 0.005(4) 0.002(4) 0.000(3) F43 0.051(5) 0.055(4) 0.084(5) -0.004(4) 0.032(4) 0.012(4) C12 0.021(6) 0.045(7) 0.046(7) -0.002(5) 0.010(5) -0.011(5) C31 0.028(7) 0.021(5) 0.034(6) 0.005(5) 0.010(5) 0.010(5) C22 0.035(8) 0.036(7) 0.035(6) -0.003(5) 0.018(5) 0.000(6) C2 0.028(7) 0.031(6) 0.045(7) 0.008(5) 0.012(5) 0.007(5) C25 0.020(7) 0.040(7) 0.077(9) -0.003(6) 0.020(6) -0.007(6) C32 0.037(7) 0.024(6) 0.048(7) 0.005(5) 0.019(6) -0.004(5) C42 0.028(7) 0.032(6) 0.042(7) 0.009(5) -0.001(5) 0.007(5) C21 0.019(6) 0.041(6) 0.046(7) -0.005(5) 0.014(5) 0.000(5) C1 0.039(7) 0.034(6) 0.031(6) 0.010(5) 0.014(5) 0.015(5) C34 0.027(7) 0.020(6) 0.085(9) -0.004(6) 0.035(7) -0.007(5) C35 0.047(9) 0.022(6) 0.076(9) 0.011(6) 0.033(7) 0.008(6) C5 0.017(6) 0.034(6) 0.045(7) 0.005(5) 0.001(5) 0.009(5) C4 0.037(7) 0.023(6) 0.054(7) 0.000(5) 0.018(6) 0.003(5) C24 0.039(8) 0.051(8) 0.048(7) -0.003(6) 0.011(6) 0.021(7) C44 0.026(8) 0.043(7) 0.072(9) 0.016(7) 0.012(7) 0.006(6) C26 0.037(8) 0.037(7) 0.063(8) 0.007(6) 0.024(6) 0.012(6) C23 0.027(7) 0.041(7) 0.054(8) 0.001(6) 0.009(6) 0.015(6) C41 0.045(8) 0.024(6) 0.043(7) 0.006(5) 0.023(6) 0.006(5) C46 0.040(8) 0.028(6) 0.048(7) 0.004(6) 0.003(6) -0.002(6) C7 0.051(9) 0.015(6) 0.104(10) 0.002(6) 0.025(7) -0.003(5) C3 0.038(7) 0.036(6) 0.042(7) 0.022(5) 0.016(5) 0.011(5) C8 0.040(8) 0.051(7) 0.065(8) 0.002(6) 0.016(6) -0.014(6) C45 0.039(8) 0.039(7) 0.047(7) 0.003(6) -0.001(6) 0.008(6) C33 0.045(8) 0.033(7) 0.060(8) 0.011(6) 0.028(7) 0.006(6) C10 0.054(9) 0.053(8) 0.044(7) -0.003(6) 0.011(6) 0.002(6) C36 0.041(8) 0.028(6) 0.055(8) 0.012(5) 0.023(6) 0.013(6) B1 0.046(9) 0.031(7) 0.035(7) 0.012(6) 0.013(6) -0.001(6) C6 0.052(9) 0.071(9) 0.043(7) -0.010(6) 0.013(6) 0.006(7) C11 0.058(9) 0.052(8) 0.070(9) -0.001(6) 0.024(7) -0.013(7) C43 0.059(9) 0.027(6) 0.058(8) 0.015(6) 0.025(7) 0.014(6) C9 0.043(9) 0.074(9) 0.066(8) 0.022(7) 0.009(7) 0.026(7) C14 0.048(8) 0.045(7) 0.045(7) 0.002(6) 0.018(6) 0.016(6) C13 0.035(7) 0.026(6) 0.058(7) 0.012(5) 0.024(6) 0.001(5) C15 0.055(9) 0.035(7) 0.053(8) 0.007(6) 0.025(6) 0.018(6) C16 0.058(9) 0.073(9) 0.067(8) 0.020(7) 0.038(7) 0.030(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 Zr1 C15 2.292(9) . ? Zr1 C12 2.327(10) . ? Zr1 C21 2.342(10) . ? Zr1 C13 2.405(10) . ? Zr1 C5 2.471(10) . ? Zr1 C4 2.483(10) . ? Zr1 C14 2.498(10) . ? Zr1 C1 2.499(11) . ? Zr1 C3 2.499(10) . ? Zr1 C2 2.505(10) . ? Si1 C6 1.834(11) . ? Si1 C1 1.840(10) . ? Si1 C7 1.843(10) . ? Si1 C8 1.874(10) . ? Si2 C3 1.842(11) . ? Si2 C10 1.846(10) . ? Si2 C11 1.863(11) . ? Si2 C9 1.868(10) . ? F32 C32 1.400(11) . ? F42 C42 1.338(11) . ? F22 C22 1.368(11) . ? F23 C23 1.342(11) . ? F33 C33 1.324(12) . ? F44 C44 1.336(12) . ? F36 C36 1.339(12) . ? F46 C46 1.328(11) . ? F35 C35 1.325(11) . ? F24 C24 1.347(12) . ? F26 C26 1.354(11) . ? F25 C25 1.335(12) . ? F34 C34 1.335(12) . ? F45 C45 1.347(11) . ? F43 C43 1.335(11) . ? C12 C13 1.435(13) . ? C12 B1 1.514(15) . ? C31 C32 1.341(13) . ? C31 C36 1.395(13) . ? C31 B1 1.555(15) . ? C22 C23 1.349(14) . ? C22 C21 1.378(14) . ? C2 C3 1.406(13) . ? C2 C1 1.415(13) . ? C25 C24 1.348(15) . ? C25 C26 1.387(14) . ? C32 C33 1.381(14) . ? C42 C41 1.362(13) . ? C42 C43 1.382(14) . ? C21 C26 1.392(14) . ? C1 C5 1.464(12) . ? C34 C35 1.341(15) . ? C34 C33 1.400(14) . ? C35 C36 1.366(15) . ? C5 C4 1.372(13) . ? C4 C3 1.419(13) . ? C24 C23 1.369(15) . ? C44 C45 1.327(14) . ? C44 C43 1.392(15) . ? C41 C46 1.370(14) . ? C41 B1 1.572(15) . ? C46 C45 1.402(14) . ? C14 C13 1.365(13) . ? C14 C15 1.423(14) . ? C14 C16 1.516(14) . ? 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 C15 Zr1 C12 75.3(4) . . ? C15 Zr1 C21 89.2(4) . . ? C12 Zr1 C21 129.8(4) . . ? C15 Zr1 C13 60.9(3) . . ? C12 Zr1 C13 35.3(3) . . ? C21 Zr1 C13 95.6(4) . . ? C15 Zr1 C5 110.0(4) . . ? C12 Zr1 C5 86.6(3) . . ? C21 Zr1 C5 142.9(3) . . ? C13 Zr1 C5 121.4(3) . . ? C15 Zr1 C4 140.2(4) . . ? C12 Zr1 C4 104.2(3) . . ? C21 Zr1 C4 116.9(3) . . ? C13 Zr1 C4 136.9(3) . . ? C5 Zr1 C4 32.2(3) . . ? C15 Zr1 C14 34.2(3) . . ? C12 Zr1 C14 61.4(3) . . ? C21 Zr1 C14 78.9(4) . . ? C13 Zr1 C14 32.3(3) . . ? C5 Zr1 C14 134.0(4) . . ? C4 Zr1 C14 164.1(3) . . ? C15 Zr1 C1 86.3(4) . . ? C12 Zr1 C1 104.4(3) . . ? C21 Zr1 C1 122.2(3) . . ? C13 Zr1 C1 130.1(3) . . ? C5 Zr1 C1 34.3(3) . . ? C4 Zr1 C1 54.8(3) . . ? C14 Zr1 C1 119.5(3) . . ? C15 Zr1 C3 132.5(3) . . ? C12 Zr1 C3 137.3(3) . . ? C21 Zr1 C3 87.6(3) . . ? C13 Zr1 C3 166.4(3) . . ? C5 Zr1 C3 55.8(3) . . ? C4 Zr1 C3 33.1(3) . . ? C14 Zr1 C3 160.3(3) . . ? C1 Zr1 C3 56.7(3) . . ? C15 Zr1 C2 100.4(4) . . ? C12 Zr1 C2 136.6(3) . . ? C21 Zr1 C2 92.7(3) . . ? C13 Zr1 C2 159.3(3) . . ? C5 Zr1 C2 53.7(3) . . ? C4 Zr1 C2 52.1(3) . . ? C14 Zr1 C2 132.9(3) . . ? C1 Zr1 C2 32.8(3) . . ? C3 Zr1 C2 32.6(3) . . ? C6 Si1 C1 108.8(5) . . ? C6 Si1 C7 112.9(5) . . ? C1 Si1 C7 110.1(5) . . ? C6 Si1 C8 105.7(5) . . ? C1 Si1 C8 109.5(5) . . ? C7 Si1 C8 109.6(5) . . ? C3 Si2 C10 106.9(5) . . ? C3 Si2 C11 109.2(5) . . ? C10 Si2 C11 110.4(5) . . ? C3 Si2 C9 109.9(5) . . ? C10 Si2 C9 108.7(5) . . ? C11 Si2 C9 111.7(6) . . ? C13 C12 B1 125.0(10) . . ? C13 C12 Zr1 75.3(6) . . ? B1 C12 Zr1 107.9(7) . . ? C32 C31 C36 114.5(10) . . ? C32 C31 B1 122.1(9) . . ? C36 C31 B1 123.3(9) . . ? C23 C22 F22 115.3(9) . . ? C23 C22 C21 125.8(11) . . ? F22 C22 C21 118.9(10) . . ? C3 C2 C1 114.7(9) . . ? C3 C2 Zr1 73.5(6) . . ? C1 C2 Zr1 73.4(6) . . ? F25 C25 C24 122.6(11) . . ? F25 C25 C26 119.5(10) . . ? C24 C25 C26 117.8(11) . . ? C31 C32 C33 127.0(10) . . ? C31 C32 F32 117.7(9) . . ? C33 C32 F32 115.3(9) . . ? F42 C42 C41 120.6(10) . . ? F42 C42 C43 114.8(9) . . ? C41 C42 C43 124.4(10) . . ? C22 C21 C26 112.5(10) . . ? C22 C21 Zr1 122.7(8) . . ? C26 C21 Zr1 124.4(8) . . ? C2 C1 C5 102.6(8) . . ? C2 C1 Si1 130.2(7) . . ? C5 C1 Si1 125.7(7) . . ? C2 C1 Zr1 73.8(6) . . ? C5 C1 Zr1 71.8(6) . . ? Si1 C1 Zr1 128.7(5) . . ? F34 C34 C35 122.1(11) . . ? F34 C34 C33 116.2(12) . . ? C35 C34 C33 121.8(11) . . ? F35 C35 C34 119.0(11) . . ? F35 C35 C36 121.2(12) . . ? C34 C35 C36 119.7(11) . . ? C4 C5 C1 107.8(9) . . ? C4 C5 Zr1 74.4(6) . . ? C1 C5 Zr1 73.9(6) . . ? C5 C4 C3 112.9(8) . . ? C5 C4 Zr1 73.4(5) . . ? C3 C4 Zr1 74.1(5) . . ? F24 C24 C25 118.6(11) . . ? F24 C24 C23 120.0(10) . . ? C25 C24 C23 121.3(11) . . ? C45 C44 F44 120.8(11) . . ? C45 C44 C43 119.4(11) . . ? F44 C44 C43 119.9(11) . . ? F26 C26 C25 116.2(10) . . ? F26 C26 C21 119.6(10) . . ? C25 C26 C21 124.2(10) . . ? F23 C23 C22 121.7(10) . . ? F23 C23 C24 120.2(10) . . ? C22 C23 C24 118.1(11) . . ? C42 C41 C46 115.4(10) . . ? C42 C41 B1 120.3(10) . . ? C46 C41 B1 124.3(9) . . ? F46 C46 C41 121.4(10) . . ? F46 C46 C45 116.8(9) . . ? C41 C46 C45 121.8(10) . . ? C2 C3 C4 101.8(9) . . ? C2 C3 Si2 129.3(8) . . ? C4 C3 Si2 126.0(7) . . ? C2 C3 Zr1 73.9(6) . . ? C4 C3 Zr1 72.8(5) . . ? Si2 C3 Zr1 131.3(5) . . ? C44 C45 F45 120.2(11) . . ? C44 C45 C46 120.9(10) . . ? F45 C45 C46 118.8(10) . . ? F33 C33 C32 122.5(10) . . ? F33 C33 C34 122.9(11) . . ? C32 C33 C34 114.6(11) . . ? F36 C36 C35 118.5(10) . . ? F36 C36 C31 119.1(10) . . ? C35 C36 C31 122.3(11) . . ? C12 B1 C31 117.5(10) . . ? C12 B1 C41 122.0(10) . . ? C31 B1 C41 120.4(9) . . ? F43 C43 C42 122.1(11) . . ? F43 C43 C44 119.8(11) . . ? C42 C43 C44 118.1(10) . . ? C13 C14 C15 117.3(10) . . ? C13 C14 C16 119.7(11) . . ? C15 C14 C16 122.2(9) . . ? C13 C14 Zr1 70.1(6) . . ? C15 C14 Zr1 64.9(5) . . ? C16 C14 Zr1 128.6(7) . . ? C14 C13 C12 123.7(10) . . ? C14 C13 Zr1 77.6(6) . . ? C12 C13 Zr1 69.4(5) . . ? C14 C15 Zr1 80.8(6) . . ? _refine_diff_density_max 1.510 _refine_diff_density_min -0.521 _refine_diff_density_rms 0.114