data_global _publ_contact_author_name 'Martin Lutz' _publ_contact_author_address ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; _publ_contact_author_email 'm.lutz@chem.uu.nl' _publ_contact_author_fax '[+31] 30 2533940' _publ_contact_author_phone '[+31] 30 2533902' _publ_section_title ; Fluorous Zirconocene(IV) Complexes and their Olefin Polymerization Activity in Toluene and Fluorous Biphasic Solvent Systems ; loop_ _publ_author_name _publ_author_address 'Merle, Philippe G.' ; Debye Institute Department of Metal Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Cheron, Virginie' ; Debye Institute Department of Metal Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Hagen, Henk' ; Debye Institute Department of Metal Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Lutz, Martin' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Spek, Anthony L.' ; Bijvoet Center for Biomolecular Research Dep. Crystal and Structural Chemistry Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'Deelman, Berth-Jan' ; Debye Institute Department of Metal Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; 'van Koten, Gerard' ; Debye Institute Department of Metal Mediated Synthesis Utrecht University Padualaan 8 3584 CH Utrecht The Netherlands ; # Compound 2d data_s2248c _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H6 Br F15 Si' _chemical_formula_sum 'C21 H6 Br F15 Si' _chemical_formula_weight 651.26 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' 'Br' 'Br' -0.2901 2.4595 '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' _symmetry_cell_setting trigonal _symmetry_space_group_name_H-M 'R -3' _symmetry_space_group_name_Hall '-R 3' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' _cell_length_a 15.9230(12) _cell_length_b 15.9230(12) _cell_length_c 29.4013(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 6455.8(8) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 11.70 _cell_measurement_theta_max 13.89 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.010 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_absorpt_coefficient_mu 2.106 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf-Nonius CAD4T' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8882 _diffrn_reflns_av_R_equivalents 0.0638 _diffrn_reflns_av_sigmaI/netI 0.0540 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 26.47 _reflns_number_total 2966 _reflns_number_gt 2249 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'locally modified CAD4 software' _computing_cell_refinement 'SET4' _computing_data_reduction 'HELENA' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0240P)^2^+10.6650P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2966 _refine_ls_number_parameters 229 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0780 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Br1 Br 0.3333 0.6667 -0.043457(17) 0.03052(14) Uani 1 3 d S . . Si1 Si 0.3333 0.6667 0.03202(5) 0.0209(3) Uani 1 3 d S . . F13 F 0.43946(11) 0.52000(12) -0.02516(6) 0.0286(4) Uani 1 1 d . . . F14 F 0.35239(13) 0.33061(13) -0.04587(6) 0.0351(4) Uani 1 1 d . . . F15 F 0.19965(13) 0.19879(12) 0.00444(6) 0.0378(4) Uani 1 1 d . . . F16 F 0.13813(12) 0.25944(12) 0.07717(6) 0.0315(4) Uani 1 1 d . . . F17 F 0.23062(12) 0.44768(12) 0.10034(5) 0.0315(4) Uani 1 1 d . . . C11 C 0.3900(2) 0.5953(2) 0.05200(10) 0.0253(6) Uani 1 1 d . . . H11A H 0.4571 0.6260 0.0402 0.030 Uiso 1 1 calc R . . H11B H 0.3938 0.5984 0.0856 0.030 Uiso 1 1 calc R . . C12 C 0.33680(19) 0.49043(19) 0.03776(9) 0.0219(6) Uani 1 1 d . . . C13 C 0.36427(19) 0.4573(2) 0.00025(9) 0.0222(6) Uani 1 1 d . . . C14 C 0.3193(2) 0.3603(2) -0.01107(9) 0.0243(6) Uani 1 1 d . . . C15 C 0.2422(2) 0.2936(2) 0.01454(10) 0.0254(6) Uani 1 1 d . . . C16 C 0.21124(19) 0.3241(2) 0.05137(9) 0.0239(6) Uani 1 1 d . . . C17 C 0.2591(2) 0.4208(2) 0.06256(9) 0.0225(6) Uani 1 1 d . . . Br2 Br 0.0000 0.0000 0.067642(16) 0.02630(14) Uani 1 3 d S . . Si52 Si 0.0000 0.0000 0.14237(4) 0.0176(3) Uani 1 3 d S . . F23 F 0.16352(13) 0.19948(12) 0.21579(6) 0.0329(4) Uani 1 1 d . . . F24 F 0.30151(15) 0.38212(13) 0.19494(7) 0.0501(6) Uani 1 1 d . . . F25 F 0.42031(14) 0.41496(14) 0.12278(8) 0.0587(6) Uani 1 1 d . . . F26 F 0.39637(13) 0.26384(16) 0.07015(7) 0.0522(6) Uani 1 1 d . . . F27 F 0.25424(13) 0.08336(13) 0.08902(6) 0.0362(4) Uani 1 1 d . . . C21 C 0.12421(19) 0.03440(19) 0.16362(9) 0.0203(6) Uani 1 1 d . . . H21A H 0.1212 0.0266 0.1971 0.024 Uiso 1 1 calc R . . H21B H 0.1427 -0.0115 0.1508 0.024 Uiso 1 1 calc R . . C22 C 0.20253(19) 0.1361(2) 0.15226(9) 0.0206(6) Uani 1 1 d . . . C23 C 0.2186(2) 0.2146(2) 0.17865(9) 0.0243(6) Uani 1 1 d . . . C24 C 0.2902(2) 0.3079(2) 0.16888(11) 0.0331(8) Uani 1 1 d . . . C25 C 0.3499(2) 0.3245(2) 0.13231(12) 0.0373(9) Uani 1 1 d . . . C26 C 0.3373(2) 0.2485(2) 0.10565(11) 0.0346(8) Uani 1 1 d . . . C27 C 0.2638(2) 0.1563(2) 0.11543(10) 0.0259(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.0335(2) 0.0335(2) 0.0245(3) 0.000 0.000 0.01675(10) Si1 0.0188(4) 0.0188(4) 0.0250(7) 0.000 0.000 0.0094(2) F13 0.0225(9) 0.0304(9) 0.0321(9) 0.0057(7) 0.0050(7) 0.0125(8) F14 0.0374(10) 0.0363(10) 0.0358(10) -0.0061(8) 0.0024(8) 0.0216(9) F15 0.0377(11) 0.0219(9) 0.0502(11) -0.0044(8) -0.0047(9) 0.0121(8) F16 0.0237(9) 0.0272(9) 0.0402(10) 0.0118(8) 0.0040(7) 0.0100(8) F17 0.0364(10) 0.0332(10) 0.0296(9) 0.0033(7) 0.0076(8) 0.0209(9) C11 0.0216(15) 0.0234(15) 0.0305(15) -0.0018(12) -0.0037(12) 0.0110(13) C12 0.0186(14) 0.0198(14) 0.0305(15) 0.0013(12) -0.0048(12) 0.0119(12) C13 0.0146(14) 0.0262(15) 0.0265(14) 0.0040(12) -0.0005(11) 0.0107(12) C14 0.0248(15) 0.0298(16) 0.0251(14) -0.0028(12) -0.0029(12) 0.0188(14) C15 0.0232(15) 0.0164(14) 0.0351(16) -0.0002(12) -0.0076(13) 0.0089(12) C16 0.0186(14) 0.0232(15) 0.0301(15) 0.0084(12) -0.0012(12) 0.0106(12) C17 0.0230(15) 0.0275(16) 0.0231(14) 0.0025(12) -0.0016(12) 0.0173(13) Br2 0.02739(19) 0.02739(19) 0.0241(3) 0.000 0.000 0.01369(9) Si52 0.0144(4) 0.0144(4) 0.0240(7) 0.000 0.000 0.0072(2) F23 0.0362(10) 0.0334(10) 0.0296(9) -0.0072(8) -0.0029(8) 0.0178(9) F24 0.0570(13) 0.0227(10) 0.0643(14) -0.0135(9) -0.0274(11) 0.0151(10) F25 0.0279(11) 0.0347(11) 0.0892(16) 0.0289(11) -0.0135(11) -0.0026(9) F26 0.0271(10) 0.0738(15) 0.0534(13) 0.0326(11) 0.0153(9) 0.0235(10) F27 0.0324(10) 0.0491(12) 0.0342(10) -0.0047(9) 0.0038(8) 0.0256(9) C21 0.0184(14) 0.0200(14) 0.0240(14) 0.0015(11) -0.0004(11) 0.0105(12) C22 0.0169(14) 0.0219(15) 0.0238(14) 0.0009(11) -0.0054(11) 0.0102(12) C23 0.0196(14) 0.0253(16) 0.0262(15) -0.0005(12) -0.0079(12) 0.0098(12) C24 0.0316(17) 0.0193(15) 0.0428(18) 0.0000(14) -0.0213(15) 0.0085(14) C25 0.0165(16) 0.0222(16) 0.058(2) 0.0210(16) -0.0130(15) -0.0014(13) C26 0.0165(15) 0.048(2) 0.0373(18) 0.0208(16) 0.0027(13) 0.0150(15) C27 0.0208(15) 0.0328(17) 0.0287(15) 0.0014(13) -0.0029(12) 0.0168(14) _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 Br1 Si1 2.2192(15) . ? Si1 C11 1.864(3) 2_665 ? Si1 C11 1.864(3) 3_565 ? Si1 C11 1.864(3) . ? F13 C13 1.339(3) . ? F14 C14 1.341(3) . ? F15 C15 1.343(3) . ? F16 C16 1.339(3) . ? F17 C17 1.348(3) . ? C11 C12 1.506(4) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.384(4) . ? C12 C17 1.385(4) . ? C13 C14 1.380(4) . ? C14 C15 1.378(4) . ? C15 C16 1.375(4) . ? C16 C17 1.374(4) . ? Br2 Si52 2.1971(14) . ? Si52 C21 1.876(3) . ? Si52 C21 1.876(3) 3 ? Si52 C21 1.876(3) 2 ? F23 C23 1.344(3) . ? F24 C24 1.343(4) . ? F25 C25 1.340(3) . ? F26 C26 1.343(4) . ? F27 C27 1.341(3) . ? C21 C22 1.506(4) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.383(4) . ? C22 C27 1.383(4) . ? C23 C24 1.377(4) . ? C24 C25 1.371(5) . ? C25 C26 1.370(5) . ? C26 C27 1.374(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C11 Si1 C11 110.55(9) 2_665 3_565 ? C11 Si1 C11 110.55(9) 2_665 . ? C11 Si1 C11 110.55(9) 3_565 . ? C11 Si1 Br1 108.37(10) 2_665 . ? C11 Si1 Br1 108.37(10) 3_565 . ? C11 Si1 Br1 108.37(10) . . ? C12 C11 Si1 114.41(19) . . ? C12 C11 H11A 108.7 . . ? Si1 C11 H11A 108.7 . . ? C12 C11 H11B 108.7 . . ? Si1 C11 H11B 108.7 . . ? H11A C11 H11B 107.6 . . ? C13 C12 C17 116.1(3) . . ? C13 C12 C11 122.3(3) . . ? C17 C12 C11 121.6(3) . . ? F13 C13 C14 118.0(2) . . ? F13 C13 C12 119.7(2) . . ? C14 C13 C12 122.2(3) . . ? F14 C14 C15 120.1(3) . . ? F14 C14 C13 120.2(3) . . ? C15 C14 C13 119.6(3) . . ? F15 C15 C16 120.2(3) . . ? F15 C15 C14 120.0(3) . . ? C16 C15 C14 119.8(3) . . ? F16 C16 C17 120.6(3) . . ? F16 C16 C15 120.2(3) . . ? C17 C16 C15 119.2(3) . . ? F17 C17 C16 117.8(2) . . ? F17 C17 C12 119.2(2) . . ? C16 C17 C12 123.0(3) . . ? C21 Si52 C21 109.48(9) . 3 ? C21 Si52 C21 109.48(9) . 2 ? C21 Si52 C21 109.48(9) 3 2 ? C21 Si52 Br2 109.46(9) . . ? C21 Si52 Br2 109.46(9) 3 . ? C21 Si52 Br2 109.46(9) 2 . ? C22 C21 Si52 115.18(18) . . ? C22 C21 H21A 108.5 . . ? Si52 C21 H21A 108.5 . . ? C22 C21 H21B 108.5 . . ? Si52 C21 H21B 108.5 . . ? H21A C21 H21B 107.5 . . ? C23 C22 C27 116.0(3) . . ? C23 C22 C21 121.8(3) . . ? C27 C22 C21 122.2(3) . . ? F23 C23 C24 118.5(3) . . ? F23 C23 C22 119.0(2) . . ? C24 C23 C22 122.5(3) . . ? F24 C24 C25 120.2(3) . . ? F24 C24 C23 120.3(3) . . ? C25 C24 C23 119.5(3) . . ? F25 C25 C26 120.3(3) . . ? F25 C25 C24 119.9(3) . . ? C26 C25 C24 119.9(3) . . ? F26 C26 C25 120.3(3) . . ? F26 C26 C27 120.2(3) . . ? C25 C26 C27 119.6(3) . . ? F27 C27 C26 118.1(3) . . ? F27 C27 C22 119.4(3) . . ? C26 C27 C22 122.5(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C11 Si1 C11 C12 179.56(17) 2_665 . . . ? C11 Si1 C11 C12 56.8(3) 3_565 . . . ? Br1 Si1 C11 C12 -61.8(2) . . . . ? Si1 C11 C12 C13 97.6(3) . . . . ? Si1 C11 C12 C17 -84.6(3) . . . . ? C17 C12 C13 F13 -179.2(2) . . . . ? C11 C12 C13 F13 -1.3(4) . . . . ? C17 C12 C13 C14 -2.1(4) . . . . ? C11 C12 C13 C14 175.8(3) . . . . ? F13 C13 C14 F14 1.7(4) . . . . ? C12 C13 C14 F14 -175.5(2) . . . . ? F13 C13 C14 C15 179.5(2) . . . . ? C12 C13 C14 C15 2.3(4) . . . . ? F14 C14 C15 F15 -0.5(4) . . . . ? C13 C14 C15 F15 -178.3(2) . . . . ? F14 C14 C15 C16 177.2(2) . . . . ? C13 C14 C15 C16 -0.6(4) . . . . ? F15 C15 C16 F16 -0.4(4) . . . . ? C14 C15 C16 F16 -178.1(2) . . . . ? F15 C15 C16 C17 176.5(2) . . . . ? C14 C15 C16 C17 -1.2(4) . . . . ? F16 C16 C17 F17 0.6(4) . . . . ? C15 C16 C17 F17 -176.3(2) . . . . ? F16 C16 C17 C12 178.3(2) . . . . ? C15 C16 C17 C12 1.4(4) . . . . ? C13 C12 C17 F17 177.9(2) . . . . ? C11 C12 C17 F17 0.0(4) . . . . ? C13 C12 C17 C16 0.2(4) . . . . ? C11 C12 C17 C16 -177.7(3) . . . . ? C21 Si52 C21 C22 -175.22(16) 3 . . . ? C21 Si52 C21 C22 -55.2(3) 2 . . . ? Br2 Si52 C21 C22 64.8(2) . . . . ? Si52 C21 C22 C23 83.8(3) . . . . ? Si52 C21 C22 C27 -97.4(3) . . . . ? C27 C22 C23 F23 -177.9(2) . . . . ? C21 C22 C23 F23 0.9(4) . . . . ? C27 C22 C23 C24 0.8(4) . . . . ? C21 C22 C23 C24 179.6(3) . . . . ? F23 C23 C24 F24 -2.8(4) . . . . ? C22 C23 C24 F24 178.5(3) . . . . ? F23 C23 C24 C25 177.2(2) . . . . ? C22 C23 C24 C25 -1.5(4) . . . . ? F24 C24 C25 F25 0.6(4) . . . . ? C23 C24 C25 F25 -179.4(3) . . . . ? F24 C24 C25 C26 -179.5(3) . . . . ? C23 C24 C25 C26 0.6(4) . . . . ? F25 C25 C26 F26 1.0(4) . . . . ? C24 C25 C26 F26 -179.0(3) . . . . ? F25 C25 C26 C27 -179.0(3) . . . . ? C24 C25 C26 C27 1.0(4) . . . . ? F26 C26 C27 F27 0.9(4) . . . . ? C25 C26 C27 F27 -179.2(3) . . . . ? F26 C26 C27 C22 178.2(2) . . . . ? C25 C26 C27 C22 -1.8(4) . . . . ? C23 C22 C27 F27 178.2(2) . . . . ? C21 C22 C27 F27 -0.7(4) . . . . ? C23 C22 C27 C26 0.9(4) . . . . ? C21 C22 C27 C26 -178.0(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.47 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.676 _refine_diff_density_min -0.313 _refine_diff_density_rms 0.073 #===END # Compound 4a data_s2505a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H28 Cl2 F26 Si2 Zr' _chemical_formula_sum 'C30 H28 Cl2 F26 Si2 Zr' _chemical_formula_weight 1100.82 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' 'Cl' 'Cl' 0.1484 0.1585 '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 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' 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 46.3678(10) _cell_length_b 6.5983(2) _cell_length_c 14.2962(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.4326(14) _cell_angle_gamma 90.00 _cell_volume 4195.2(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 28622 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.743 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.586 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17051 _diffrn_reflns_av_R_equivalents 0.0648 _diffrn_reflns_av_sigmaI/netI 0.1063 _diffrn_reflns_limit_h_min -60 _diffrn_reflns_limit_h_max 57 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.47 _reflns_number_total 4790 _reflns_number_gt 2810 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000+SORTAV' _computing_structure_solution 'SIR-97 (Altomare et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4790 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0331 _refine_ls_wR_factor_ref 0.0892 _refine_ls_wR_factor_gt 0.0710 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.0000 0.08932(6) 0.2500 0.02133(11) Uani 1 2 d S . . Cl Cl -0.018718(17) -0.15817(10) 0.34679(5) 0.03106(18) Uani 1 1 d . . . Si Si 0.077228(18) 0.26339(12) 0.20523(5) 0.02692(19) Uani 1 1 d . . . F1 F 0.15561(4) 0.6900(3) 0.37725(12) 0.0560(6) Uani 1 1 d . . . F2 F 0.11719(4) 0.7425(3) 0.43267(14) 0.0593(6) Uani 1 1 d . . . F3 F 0.13944(4) 0.4946(3) 0.58226(12) 0.0577(6) Uani 1 1 d . . . F4 F 0.17637(4) 0.4058(3) 0.52606(14) 0.0556(5) Uani 1 1 d . . . F5 F 0.20040(4) 0.7629(3) 0.54859(13) 0.0614(6) Uani 1 1 d . . . F6 F 0.16045(5) 0.9070(3) 0.56793(14) 0.0635(6) Uani 1 1 d . . . F7 F 0.16613(4) 0.7266(4) 0.73468(14) 0.0657(6) Uani 1 1 d . . . F8 F 0.20003(5) 0.5219(3) 0.71466(13) 0.0625(6) Uani 1 1 d . . . F9 F 0.23906(5) 0.8147(4) 0.72619(16) 0.0818(8) Uani 1 1 d . . . F10 F 0.20535(6) 1.0451(4) 0.71809(16) 0.0874(8) Uani 1 1 d . . . F11 F 0.19881(7) 0.9228(6) 0.88950(19) 0.1280(13) Uani 1 1 d . . . F12 F 0.24441(6) 0.9777(5) 0.89783(16) 0.1067(10) Uani 1 1 d . . . F13 F 0.22706(8) 0.6763(5) 0.89495(18) 0.1223(12) Uani 1 1 d . . . C1 C 0.05226(6) 0.2318(4) 0.28758(18) 0.0238(6) Uani 1 1 d . . . C2 C 0.05324(6) 0.0777(4) 0.35795(18) 0.0287(6) Uani 1 1 d . . . H2 H 0.0641 -0.0458 0.3629 0.034 Uiso 1 1 calc R . . C3 C 0.03584(6) 0.1353(4) 0.41871(19) 0.0304(7) Uani 1 1 d . . . H3 H 0.0333 0.0604 0.4725 0.037 Uiso 1 1 calc R . . C4 C 0.02271(6) 0.3253(4) 0.38587(19) 0.0287(7) Uani 1 1 d . . . H4 H 0.0091 0.3986 0.4119 0.034 Uiso 1 1 calc R . . C5 C 0.03356(6) 0.3858(4) 0.30714(18) 0.0258(6) Uani 1 1 d . . . H5 H 0.0290 0.5104 0.2728 0.031 Uiso 1 1 calc R . . C6 C 0.09737(7) 0.0245(5) 0.1960(2) 0.0392(8) Uani 1 1 d . . . H6A H 0.1093 -0.0178 0.2612 0.059 Uiso 1 1 calc R . . H6B H 0.1107 0.0465 0.1546 0.059 Uiso 1 1 calc R . . H6C H 0.0827 -0.0815 0.1672 0.059 Uiso 1 1 calc R . . C7 C 0.05600(7) 0.3610(4) 0.08273(19) 0.0333(7) Uani 1 1 d . . . H7A H 0.0394 0.2684 0.0529 0.050 Uiso 1 1 calc R . . H7B H 0.0695 0.3705 0.0412 0.050 Uiso 1 1 calc R . . H7C H 0.0479 0.4956 0.0897 0.050 Uiso 1 1 calc R . . C8 C 0.10334(6) 0.4689(4) 0.26837(19) 0.0313(7) Uani 1 1 d . . . H8A H 0.1172 0.5017 0.2289 0.038 Uiso 1 1 calc R . . H8B H 0.0913 0.5920 0.2708 0.038 Uiso 1 1 calc R . . C9 C 0.12210(7) 0.4179(5) 0.37204(19) 0.0334(7) Uani 1 1 d . . . H9A H 0.1088 0.3598 0.4085 0.040 Uiso 1 1 calc R . . H9B H 0.1372 0.3138 0.3691 0.040 Uiso 1 1 calc R . . C10 C 0.13795(7) 0.6002(5) 0.4259(2) 0.0348(7) Uani 1 1 d . . . C11 C 0.15767(7) 0.5579(5) 0.5300(2) 0.0352(7) Uani 1 1 d . . . C12 C 0.17682(7) 0.7372(5) 0.5849(2) 0.0386(8) Uani 1 1 d . . . C13 C 0.18922(7) 0.7078(5) 0.6964(2) 0.0406(8) Uani 1 1 d . . . C14 C 0.21331(8) 0.8613(6) 0.7493(3) 0.0540(10) Uani 1 1 d . . . C15 C 0.22150(10) 0.8602(8) 0.8599(3) 0.0695(13) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.0321(2) 0.0144(2) 0.01819(18) 0.000 0.00824(15) 0.000 Cl 0.0482(5) 0.0200(4) 0.0297(4) 0.0029(3) 0.0187(3) -0.0027(3) Si 0.0325(5) 0.0227(4) 0.0259(4) 0.0022(3) 0.0088(3) 0.0005(4) F1 0.0614(13) 0.0662(14) 0.0367(10) 0.0040(10) 0.0078(9) -0.0318(11) F2 0.0527(13) 0.0531(13) 0.0579(13) -0.0163(10) -0.0076(10) 0.0183(11) F3 0.0594(13) 0.0821(15) 0.0338(10) -0.0025(10) 0.0169(9) -0.0308(12) F4 0.0539(13) 0.0505(12) 0.0509(11) -0.0042(10) -0.0039(9) 0.0155(11) F5 0.0531(13) 0.0937(17) 0.0381(11) -0.0033(11) 0.0138(9) -0.0291(12) F6 0.0681(15) 0.0419(12) 0.0594(13) -0.0061(10) -0.0163(11) 0.0068(12) F7 0.0468(13) 0.1075(19) 0.0468(12) -0.0196(12) 0.0199(10) -0.0140(13) F8 0.0740(15) 0.0558(14) 0.0439(12) 0.0066(10) -0.0060(10) 0.0072(12) F9 0.0460(14) 0.132(2) 0.0637(15) -0.0186(15) 0.0100(11) -0.0224(15) F10 0.106(2) 0.0498(15) 0.0745(16) -0.0021(13) -0.0256(14) -0.0187(14) F11 0.115(2) 0.199(4) 0.0741(18) -0.070(2) 0.0348(17) -0.028(2) F12 0.101(2) 0.145(3) 0.0529(14) -0.0110(16) -0.0119(13) -0.062(2) F13 0.180(3) 0.113(2) 0.0424(15) 0.0104(16) -0.0197(17) -0.028(2) C1 0.0265(15) 0.0214(15) 0.0220(13) -0.0006(12) 0.0046(11) -0.0016(12) C2 0.0342(17) 0.0217(15) 0.0277(15) 0.0052(13) 0.0048(12) 0.0037(14) C3 0.0351(17) 0.0366(19) 0.0161(13) 0.0012(12) 0.0018(12) -0.0044(14) C4 0.0329(17) 0.0276(16) 0.0240(14) -0.0093(12) 0.0055(12) -0.0026(14) C5 0.0308(16) 0.0185(15) 0.0245(14) -0.0013(12) 0.0022(12) -0.0048(13) C6 0.0384(19) 0.0350(19) 0.0476(19) 0.0050(15) 0.0174(15) 0.0065(15) C7 0.0432(19) 0.0296(18) 0.0280(15) -0.0008(13) 0.0116(14) 0.0007(14) C8 0.0356(17) 0.0330(17) 0.0264(14) 0.0038(13) 0.0103(12) -0.0026(14) C9 0.0339(17) 0.0325(17) 0.0330(16) 0.0011(14) 0.0086(13) -0.0040(15) C10 0.0339(17) 0.0360(18) 0.0350(16) 0.0042(15) 0.0107(13) 0.0013(16) C11 0.0317(17) 0.039(2) 0.0348(16) -0.0012(15) 0.0102(14) -0.0003(15) C12 0.0341(19) 0.044(2) 0.0345(17) -0.0015(15) 0.0043(14) -0.0012(16) C13 0.0369(19) 0.050(2) 0.0342(17) -0.0002(16) 0.0082(15) -0.0007(17) C14 0.046(2) 0.068(3) 0.042(2) -0.0039(19) 0.0025(17) -0.011(2) C15 0.064(3) 0.094(4) 0.046(2) -0.013(2) 0.007(2) -0.013(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 Zr Cl 2.4523(7) 2 ? Zr Cl 2.4524(7) . ? Zr C4 2.480(3) . ? Zr C4 2.480(3) 2 ? Zr C5 2.490(3) 2 ? Zr C5 2.490(3) . ? Zr C1 2.511(3) . ? Zr C1 2.512(3) 2 ? Zr C2 2.515(3) . ? Zr C2 2.515(3) 2 ? Zr C3 2.530(3) . ? Zr C3 2.530(3) 2 ? Si C6 1.856(3) . ? Si C7 1.864(3) . ? Si C8 1.871(3) . ? Si C1 1.882(3) . ? F1 C10 1.352(3) . ? F2 C10 1.368(3) . ? F3 C11 1.343(3) . ? F4 C11 1.338(3) . ? F5 C12 1.347(3) . ? F6 C12 1.337(4) . ? F7 C13 1.339(3) . ? F8 C13 1.323(4) . ? F9 C14 1.361(4) . ? F10 C14 1.308(4) . ? F11 C15 1.307(5) . ? F12 C15 1.303(5) . ? F13 C15 1.310(5) . ? C1 C5 1.414(4) . ? C1 C2 1.422(4) . ? C2 C3 1.395(4) . ? C2 H2 0.9500 . ? C3 C4 1.414(4) . ? C3 H3 0.9500 . ? C4 C5 1.414(4) . ? C4 H4 0.9500 . ? C5 H5 0.9500 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.529(4) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.503(4) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.536(4) . ? C11 C12 1.552(4) . ? C12 C13 1.547(4) . ? C13 C14 1.538(5) . ? C14 C15 1.519(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 Cl Zr Cl 96.50(3) 2 . ? Cl Zr C4 136.09(7) 2 . ? Cl Zr C4 96.65(7) . . ? Cl Zr C4 96.65(7) 2 2 ? Cl Zr C4 136.09(7) . 2 ? C4 Zr C4 102.22(13) . 2 ? Cl Zr C5 128.78(6) 2 2 ? Cl Zr C5 114.85(6) . 2 ? C4 Zr C5 81.44(9) . 2 ? C4 Zr C5 33.07(8) 2 2 ? Cl Zr C5 114.86(6) 2 . ? Cl Zr C5 128.78(6) . . ? C4 Zr C5 33.07(8) . . ? C4 Zr C5 81.44(9) 2 . ? C5 Zr C5 76.40(13) 2 . ? Cl Zr C1 84.03(6) 2 . ? Cl Zr C1 127.05(6) . . ? C4 Zr C1 55.05(9) . . ? C4 Zr C1 95.91(9) 2 . ? C5 Zr C1 104.58(9) 2 . ? C5 Zr C1 32.85(8) . . ? Cl Zr C1 127.05(6) 2 2 ? Cl Zr C1 84.02(6) . 2 ? C4 Zr C1 95.91(9) . 2 ? C4 Zr C1 55.05(9) 2 2 ? C5 Zr C1 32.85(8) 2 2 ? C5 Zr C1 104.59(9) . 2 ? C1 Zr C1 136.04(12) . 2 ? Cl Zr C2 83.30(7) 2 . ? Cl Zr C2 94.36(6) . . ? C4 Zr C2 54.04(9) . . ? C4 Zr C2 128.72(9) 2 . ? C5 Zr C2 129.74(9) 2 . ? C5 Zr C2 53.75(9) . . ? C1 Zr C2 32.86(8) . . ? C1 Zr C2 149.63(9) 2 . ? Cl Zr C2 94.36(6) 2 2 ? Cl Zr C2 83.30(7) . 2 ? C4 Zr C2 128.71(9) . 2 ? C4 Zr C2 54.04(9) 2 2 ? C5 Zr C2 53.75(9) 2 2 ? C5 Zr C2 129.73(9) . 2 ? C1 Zr C2 149.63(9) . 2 ? C1 Zr C2 32.86(8) 2 2 ? C2 Zr C2 176.51(13) . 2 ? Cl Zr C3 112.09(7) 2 . ? Cl Zr C3 77.52(7) . . ? C4 Zr C3 32.77(9) . . ? C4 Zr C3 133.64(10) 2 . ? C5 Zr C3 113.54(9) 2 . ? C5 Zr C3 53.98(9) . . ? C1 Zr C3 54.37(9) . . ? C1 Zr C3 119.52(9) 2 . ? C2 Zr C3 32.11(9) . . ? C2 Zr C3 148.69(8) 2 . ? Cl Zr C3 77.52(7) 2 2 ? Cl Zr C3 112.08(7) . 2 ? C4 Zr C3 133.64(10) . 2 ? C4 Zr C3 32.76(9) 2 2 ? C5 Zr C3 53.98(9) 2 2 ? C5 Zr C3 113.54(9) . 2 ? C1 Zr C3 119.52(9) . 2 ? C1 Zr C3 54.37(9) 2 2 ? C2 Zr C3 148.69(8) . 2 ? C2 Zr C3 32.11(9) 2 2 ? C3 Zr C3 166.21(13) . 2 ? C6 Si C7 111.67(13) . . ? C6 Si C8 112.34(14) . . ? C7 Si C8 107.48(13) . . ? C6 Si C1 111.19(13) . . ? C7 Si C1 111.79(13) . . ? C8 Si C1 101.95(12) . . ? C5 C1 C2 105.8(2) . . ? C5 C1 Si 124.3(2) . . ? C2 C1 Si 128.3(2) . . ? C5 C1 Zr 72.73(15) . . ? C2 C1 Zr 73.71(15) . . ? Si C1 Zr 129.40(12) . . ? C3 C2 C1 109.7(2) . . ? C3 C2 Zr 74.55(16) . . ? C1 C2 Zr 73.42(15) . . ? C3 C2 H2 125.2 . . ? C1 C2 H2 125.2 . . ? Zr C2 H2 118.6 . . ? C2 C3 C4 107.8(2) . . ? C2 C3 Zr 73.34(15) . . ? C4 C3 Zr 71.64(15) . . ? C2 C3 H3 126.1 . . ? C4 C3 H3 126.1 . . ? Zr C3 H3 120.7 . . ? C3 C4 C5 107.3(2) . . ? C3 C4 Zr 75.59(15) . . ? C5 C4 Zr 73.85(15) . . ? C3 C4 H4 126.3 . . ? C5 C4 H4 126.3 . . ? Zr C4 H4 116.4 . . ? C1 C5 C4 109.3(2) . . ? C1 C5 Zr 74.43(15) . . ? C4 C5 Zr 73.08(15) . . ? C1 C5 H5 125.4 . . ? C4 C5 H5 125.4 . . ? Zr C5 H5 118.9 . . ? Si C6 H6A 109.5 . . ? Si C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si C7 H7A 109.5 . . ? Si C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 Si 114.9(2) . . ? C9 C8 H8A 108.5 . . ? Si C8 H8A 108.5 . . ? C9 C8 H8B 108.5 . . ? Si C8 H8B 108.5 . . ? H8A C8 H8B 107.5 . . ? C10 C9 C8 112.5(2) . . ? C10 C9 H9A 109.1 . . ? C8 C9 H9A 109.1 . . ? C10 C9 H9B 109.1 . . ? C8 C9 H9B 109.1 . . ? H9A C9 H9B 107.8 . . ? F1 C10 F2 106.0(2) . . ? F1 C10 C9 111.5(2) . . ? F2 C10 C9 109.5(2) . . ? F1 C10 C11 107.3(2) . . ? F2 C10 C11 107.1(2) . . ? C9 C10 C11 114.9(3) . . ? F4 C11 F3 107.9(3) . . ? F4 C11 C10 108.1(2) . . ? F3 C11 C10 107.4(2) . . ? F4 C11 C12 107.9(2) . . ? F3 C11 C12 108.4(2) . . ? C10 C11 C12 116.7(3) . . ? F6 C12 F5 107.8(3) . . ? F6 C12 C13 108.6(3) . . ? F5 C12 C13 107.9(2) . . ? F6 C12 C11 109.5(2) . . ? F5 C12 C11 108.2(3) . . ? C13 C12 C11 114.7(3) . . ? F8 C13 F7 107.9(3) . . ? F8 C13 C14 109.4(3) . . ? F7 C13 C14 107.0(3) . . ? F8 C13 C12 109.2(3) . . ? F7 C13 C12 107.6(3) . . ? C14 C13 C12 115.5(3) . . ? F10 C14 F9 108.0(3) . . ? F10 C14 C15 108.8(4) . . ? F9 C14 C15 105.9(3) . . ? F10 C14 C13 110.3(3) . . ? F9 C14 C13 107.3(3) . . ? C15 C14 C13 116.2(3) . . ? F12 C15 F11 108.3(4) . . ? F12 C15 F13 110.1(4) . . ? F11 C15 F13 105.0(4) . . ? F12 C15 C14 111.4(4) . . ? F11 C15 C14 110.4(4) . . ? F13 C15 C14 111.5(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Si C1 C5 -178.5(2) . . . . ? C7 Si C1 C5 -52.9(3) . . . . ? C8 Si C1 C5 61.6(2) . . . . ? C6 Si C1 C2 17.8(3) . . . . ? C7 Si C1 C2 143.3(2) . . . . ? C8 Si C1 C2 -102.2(3) . . . . ? C6 Si C1 Zr -82.97(19) . . . . ? C7 Si C1 Zr 42.6(2) . . . . ? C8 Si C1 Zr 157.11(16) . . . . ? Cl Zr C1 C5 160.25(15) 2 . . . ? Cl Zr C1 C5 -106.11(14) . . . . ? C4 Zr C1 C5 -36.64(15) . . . . ? C4 Zr C1 C5 64.15(16) 2 . . . ? C5 Zr C1 C5 31.7(2) 2 . . . ? C1 Zr C1 C5 20.40(13) 2 . . . ? C2 Zr C1 C5 -112.9(2) . . . . ? C2 Zr C1 C5 71.8(2) 2 . . . ? C3 Zr C1 C5 -77.07(16) . . . . ? C3 Zr C1 C5 88.24(17) 2 . . . ? Cl Zr C1 C2 -86.89(15) 2 . . . ? Cl Zr C1 C2 6.75(18) . . . . ? C4 Zr C1 C2 76.22(17) . . . . ? C4 Zr C1 C2 177.01(16) 2 . . . ? C5 Zr C1 C2 144.54(16) 2 . . . ? C5 Zr C1 C2 112.9(2) . . . . ? C1 Zr C1 C2 133.26(16) 2 . . . ? C2 Zr C1 C2 -175.33(18) 2 . . . ? C3 Zr C1 C2 35.79(15) . . . . ? C3 Zr C1 C2 -158.90(15) 2 . . . ? Cl Zr C1 Si 39.65(15) 2 . . . ? Cl Zr C1 Si 133.30(13) . . . . ? C4 Zr C1 Si -157.2(2) . . . . ? C4 Zr C1 Si -56.45(17) 2 . . . ? C5 Zr C1 Si -88.92(17) 2 . . . ? C5 Zr C1 Si -120.6(2) . . . . ? C1 Zr C1 Si -100.19(16) 2 . . . ? C2 Zr C1 Si 126.5(3) . . . . ? C2 Zr C1 Si -48.8(3) 2 . . . ? C3 Zr C1 Si 162.3(2) . . . . ? C3 Zr C1 Si -32.4(2) 2 . . . ? C5 C1 C2 C3 -0.2(3) . . . . ? Si C1 C2 C3 166.0(2) . . . . ? Zr C1 C2 C3 -66.3(2) . . . . ? C5 C1 C2 Zr 66.15(18) . . . . ? Si C1 C2 Zr -127.7(2) . . . . ? Cl Zr C2 C3 -154.08(17) 2 . . . ? Cl Zr C2 C3 -58.04(17) . . . . ? C4 Zr C2 C3 37.02(16) . . . . ? C4 Zr C2 C3 112.75(18) 2 . . . ? C5 Zr C2 C3 69.7(2) 2 . . . ? C5 Zr C2 C3 78.26(18) . . . . ? C1 Zr C2 C3 116.6(2) . . . . ? C1 Zr C2 C3 27.6(3) 2 . . . ? C3 Zr C2 C3 153.6(3) 2 . . . ? Cl Zr C2 C1 89.36(15) 2 . . . ? Cl Zr C2 C1 -174.60(15) . . . . ? C4 Zr C2 C1 -79.55(17) . . . . ? C4 Zr C2 C1 -3.8(2) 2 . . . ? C5 Zr C2 C1 -46.9(2) 2 . . . ? C5 Zr C2 C1 -38.30(15) . . . . ? C1 Zr C2 C1 -89.0(3) 2 . . . ? C3 Zr C2 C1 -116.6(2) . . . . ? C3 Zr C2 C1 37.1(3) 2 . . . ? C1 C2 C3 C4 1.8(3) . . . . ? Zr C2 C3 C4 -63.82(19) . . . . ? C1 C2 C3 Zr 65.58(19) . . . . ? Cl Zr C3 C2 27.93(18) 2 . . . ? Cl Zr C3 C2 119.96(17) . . . . ? C4 Zr C3 C2 -115.8(2) . . . . ? C4 Zr C3 C2 -96.10(19) 2 . . . ? C5 Zr C3 C2 -128.14(17) 2 . . . ? C5 Zr C3 C2 -77.48(18) . . . . ? C1 Zr C3 C2 -36.67(16) . . . . ? C1 Zr C3 C2 -164.40(16) 2 . . . ? C2 Zr C3 C2 173.5(2) 2 . . . ? C3 Zr C3 C2 -104.51(16) 2 . . . ? Cl Zr C3 C4 143.72(15) 2 . . . ? Cl Zr C3 C4 -124.26(17) . . . . ? C4 Zr C3 C4 19.7(3) 2 . . . ? C5 Zr C3 C4 -12.4(2) 2 . . . ? C5 Zr C3 C4 38.30(16) . . . . ? C1 Zr C3 C4 79.12(18) . . . . ? C1 Zr C3 C4 -48.61(19) 2 . . . ? C2 Zr C3 C4 115.8(2) . . . . ? C2 Zr C3 C4 -70.7(2) 2 . . . ? C3 Zr C3 C4 11.28(16) 2 . . . ? C2 C3 C4 C5 -2.7(3) . . . . ? Zr C3 C4 C5 -67.60(18) . . . . ? C2 C3 C4 Zr 64.94(19) . . . . ? Cl Zr C4 C3 -52.2(2) 2 . . . ? Cl Zr C4 C3 54.33(16) . . . . ? C4 Zr C4 C3 -165.6(2) 2 . . . ? C5 Zr C4 C3 168.56(18) 2 . . . ? C5 Zr C4 C3 -113.3(2) . . . . ? C1 Zr C4 C3 -76.87(17) . . . . ? C1 Zr C4 C3 138.98(17) 2 . . . ? C2 Zr C4 C3 -36.24(16) . . . . ? C2 Zr C4 C3 141.06(16) 2 . . . ? C3 Zr C4 C3 -176.31(6) 2 . . . ? Cl Zr C4 C5 61.01(19) 2 . . . ? Cl Zr C4 C5 167.59(15) . . . . ? C4 Zr C4 C5 -52.30(14) 2 . . . ? C5 Zr C4 C5 -78.18(19) 2 . . . ? C1 Zr C4 C5 36.39(15) . . . . ? C1 Zr C4 C5 -107.77(17) 2 . . . ? C2 Zr C4 C5 77.01(17) . . . . ? C2 Zr C4 C5 -105.69(17) 2 . . . ? C3 Zr C4 C5 113.3(2) . . . . ? C3 Zr C4 C5 -63.1(2) 2 . . . ? C2 C1 C5 C4 -1.5(3) . . . . ? Si C1 C5 C4 -168.34(19) . . . . ? Zr C1 C5 C4 65.32(19) . . . . ? C2 C1 C5 Zr -66.83(18) . . . . ? Si C1 C5 Zr 126.34(19) . . . . ? C3 C4 C5 C1 2.6(3) . . . . ? Zr C4 C5 C1 -66.19(19) . . . . ? C3 C4 C5 Zr 68.79(19) . . . . ? Cl Zr C5 C1 -21.75(16) 2 . . . ? Cl Zr C5 C1 100.41(15) . . . . ? C4 Zr C5 C1 116.3(2) . . . . ? C4 Zr C5 C1 -115.14(16) 2 . . . ? C5 Zr C5 C1 -148.5(2) 2 . . . ? C1 Zr C5 C1 -165.52(10) 2 . . . ? C2 Zr C5 C1 38.32(14) . . . . ? C2 Zr C5 C1 -141.35(14) 2 . . . ? C3 Zr C5 C1 78.36(16) . . . . ? C3 Zr C5 C1 -108.42(16) 2 . . . ? Cl Zr C5 C4 -138.04(15) 2 . . . ? Cl Zr C5 C4 -15.89(19) . . . . ? C4 Zr C5 C4 128.56(16) 2 . . . ? C5 Zr C5 C4 95.23(18) 2 . . . ? C1 Zr C5 C4 -116.3(2) . . . . ? C1 Zr C5 C4 78.18(17) 2 . . . ? C2 Zr C5 C4 -77.98(17) . . . . ? C2 Zr C5 C4 102.35(17) 2 . . . ? C3 Zr C5 C4 -37.93(16) . . . . ? C3 Zr C5 C4 135.28(16) 2 . . . ? C6 Si C8 C9 -58.5(2) . . . . ? C7 Si C8 C9 178.2(2) . . . . ? C1 Si C8 C9 60.6(2) . . . . ? Si C8 C9 C10 -168.7(2) . . . . ? C8 C9 C10 F1 -56.5(3) . . . . ? C8 C9 C10 F2 60.5(3) . . . . ? C8 C9 C10 C11 -178.9(2) . . . . ? F1 C10 C11 F4 -72.1(3) . . . . ? F2 C10 C11 F4 174.4(2) . . . . ? C9 C10 C11 F4 52.5(3) . . . . ? F1 C10 C11 F3 171.7(2) . . . . ? F2 C10 C11 F3 58.2(3) . . . . ? C9 C10 C11 F3 -63.7(3) . . . . ? F1 C10 C11 C12 49.8(3) . . . . ? F2 C10 C11 C12 -63.7(3) . . . . ? C9 C10 C11 C12 174.4(3) . . . . ? F4 C11 C12 F6 163.6(2) . . . . ? F3 C11 C12 F6 -79.8(3) . . . . ? C10 C11 C12 F6 41.6(4) . . . . ? F4 C11 C12 F5 46.3(3) . . . . ? F3 C11 C12 F5 163.0(2) . . . . ? C10 C11 C12 F5 -75.6(3) . . . . ? F4 C11 C12 C13 -74.2(3) . . . . ? F3 C11 C12 C13 42.5(4) . . . . ? C10 C11 C12 C13 163.9(3) . . . . ? F6 C12 C13 F8 167.1(3) . . . . ? F5 C12 C13 F8 -76.3(3) . . . . ? C11 C12 C13 F8 44.3(4) . . . . ? F6 C12 C13 F7 50.1(3) . . . . ? F5 C12 C13 F7 166.7(3) . . . . ? C11 C12 C13 F7 -72.6(3) . . . . ? F6 C12 C13 C14 -69.2(4) . . . . ? F5 C12 C13 C14 47.4(4) . . . . ? C11 C12 C13 C14 168.0(3) . . . . ? F8 C13 C14 F10 168.2(3) . . . . ? F7 C13 C14 F10 -75.2(4) . . . . ? C12 C13 C14 F10 44.5(4) . . . . ? F8 C13 C14 F9 50.7(4) . . . . ? F7 C13 C14 F9 167.4(3) . . . . ? C12 C13 C14 F9 -72.9(4) . . . . ? F8 C13 C14 C15 -67.4(4) . . . . ? F7 C13 C14 C15 49.2(4) . . . . ? C12 C13 C14 C15 169.0(3) . . . . ? F10 C14 C15 F12 -62.3(5) . . . . ? F9 C14 C15 F12 53.5(5) . . . . ? C13 C14 C15 F12 172.5(4) . . . . ? F10 C14 C15 F11 58.0(5) . . . . ? F9 C14 C15 F11 173.9(4) . . . . ? C13 C14 C15 F11 -67.2(5) . . . . ? F10 C14 C15 F13 174.3(4) . . . . ? F9 C14 C15 F13 -69.9(5) . . . . ? C13 C14 C15 F13 49.1(5) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.451 _refine_diff_density_min -0.607 _refine_diff_density_rms 0.088 #===END # Compound 4c data_s2458a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C28 H24 Cl2 F10 Si2 Zr' _chemical_formula_sum 'C28 H24 Cl2 F10 Si2 Zr' _chemical_formula_weight 768.77 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' 'Cl' 'Cl' 0.1484 0.1585 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.8842(1) _cell_length_b 13.4155(2) _cell_length_c 15.1449(3) _cell_angle_alpha 73.4706(7) _cell_angle_beta 80.0282(8) _cell_angle_gamma 87.9965(7) _cell_volume 1512.31(4) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 32903 _cell_measurement_theta_min 1.02 _cell_measurement_theta_max 25.68 _exptl_crystal_description 'trigonal prism' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.688 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.701 _exptl_absorpt_correction_type refdelf _exptl_absorpt_correction_T_min 0.53 _exptl_absorpt_correction_T_max 0.85 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius KappaCCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12579 _diffrn_reflns_av_R_equivalents 0.0411 _diffrn_reflns_av_sigmaI/netI 0.0460 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 25.65 _reflns_number_total 5631 _reflns_number_gt 4883 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement 'HKL2000' _computing_data_reduction 'HKL2000' _computing_structure_solution 'DIRDIF-97 (Beurskens et al., 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0361P)^2^+0.4443P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5631 _refine_ls_number_parameters 392 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0390 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0745 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.25356(2) 0.495429(15) 0.259807(14) 0.02415(8) Uani 1 1 d . . . Cl1 Cl -0.05113(7) 0.45447(5) 0.32711(5) 0.03870(16) Uani 1 1 d . . . Cl2 Cl 0.22325(9) 0.59253(5) 0.10084(4) 0.04115(16) Uani 1 1 d . . . Si1 Si 0.16233(8) 0.30804(5) 0.11141(4) 0.02666(14) Uani 1 1 d . . . F11 F 0.37095(19) 0.15702(12) -0.05407(10) 0.0450(4) Uani 1 1 d . . . F21 F 0.7011(2) 0.10202(12) -0.08763(10) 0.0501(4) Uani 1 1 d . . . F31 F 0.88822(18) 0.04801(14) 0.05323(13) 0.0617(5) Uani 1 1 d . . . F41 F 0.7391(2) 0.04925(15) 0.22868(12) 0.0654(5) Uani 1 1 d . . . F51 F 0.4061(2) 0.10134(11) 0.26345(9) 0.0453(4) Uani 1 1 d . . . C11 C 0.2854(3) 0.33832(16) 0.19620(15) 0.0253(5) Uani 1 1 d . . . C21 C 0.4514(3) 0.38748(17) 0.17553(17) 0.0299(5) Uani 1 1 d . . . H21 H 0.5124 0.4199 0.1147 0.036 Uiso 1 1 calc R . . C31 C 0.5096(3) 0.38019(18) 0.25959(18) 0.0354(6) Uani 1 1 d . . . H31 H 0.6162 0.4065 0.2654 0.042 Uiso 1 1 calc R . . C41 C 0.3820(3) 0.32684(18) 0.33413(17) 0.0347(5) Uani 1 1 d . . . H41 H 0.3864 0.3118 0.3989 0.042 Uiso 1 1 calc R . . C51 C 0.2476(3) 0.30011(16) 0.29515(16) 0.0289(5) Uani 1 1 d . . . H51 H 0.1465 0.2621 0.3297 0.035 Uiso 1 1 calc R . . C61 C -0.0721(3) 0.3285(2) 0.14100(17) 0.0367(6) Uani 1 1 d . . . H61A H -0.0926 0.4018 0.1380 0.055 Uiso 1 1 calc R . . H61B H -0.1158 0.2849 0.2043 0.055 Uiso 1 1 calc R . . H61C H -0.1320 0.3096 0.0963 0.055 Uiso 1 1 calc R . . C71 C 0.2536(3) 0.38259(19) -0.01025(16) 0.0372(6) Uani 1 1 d . . . H71A H 0.1967 0.3602 -0.0542 0.056 Uiso 1 1 calc R . . H71B H 0.3775 0.3699 -0.0226 0.056 Uiso 1 1 calc R . . H71C H 0.2348 0.4570 -0.0182 0.056 Uiso 1 1 calc R . . C81 C 0.1930(3) 0.16379(17) 0.12489(17) 0.0308(5) Uani 1 1 d . . . H81A H 0.1420 0.1244 0.1894 0.037 Uiso 1 1 calc R . . H81B H 0.1295 0.1434 0.0816 0.037 Uiso 1 1 calc R . . C91 C 0.3780(3) 0.13371(16) 0.10573(15) 0.0260(5) Uani 1 1 d . . . C101 C 0.4595(3) 0.13259(17) 0.01756(16) 0.0305(5) Uani 1 1 d . . . C111 C 0.6290(3) 0.10420(17) -0.00058(17) 0.0334(5) Uani 1 1 d . . . C121 C 0.7234(3) 0.07701(19) 0.06990(19) 0.0387(6) Uani 1 1 d . . . C131 C 0.6481(3) 0.0775(2) 0.15857(19) 0.0406(6) Uani 1 1 d . . . C141 C 0.4781(3) 0.10545(17) 0.17511(16) 0.0308(5) Uani 1 1 d . . . Si2 Si 0.00236(8) 0.73788(5) 0.30938(4) 0.02651(14) Uani 1 1 d . . . F12 F -0.09472(17) 0.87785(11) 0.49407(10) 0.0427(4) Uani 1 1 d . . . F22 F 0.0800(2) 0.88574(13) 0.62869(10) 0.0580(4) Uani 1 1 d . . . F32 F 0.4322(2) 0.88863(13) 0.59477(13) 0.0696(5) Uani 1 1 d . . . F42 F 0.6026(2) 0.88562(14) 0.42438(16) 0.0733(6) Uani 1 1 d . . . F52 F 0.42844(19) 0.87746(12) 0.28905(12) 0.0525(4) Uani 1 1 d . . . C12 C 0.2030(3) 0.65813(16) 0.31488(15) 0.0268(5) Uani 1 1 d . . . C22 C 0.2342(3) 0.57504(17) 0.39366(16) 0.0294(5) Uani 1 1 d . . . H22 H 0.1527 0.5474 0.4488 0.035 Uiso 1 1 calc R . . C32 C 0.4033(3) 0.54079(18) 0.37679(17) 0.0352(6) Uani 1 1 d . . . H32 H 0.4560 0.4864 0.4179 0.042 Uiso 1 1 calc R . . C42 C 0.4816(3) 0.60200(18) 0.28729(19) 0.0383(6) Uani 1 1 d . . . H42 H 0.5959 0.5954 0.2573 0.046 Uiso 1 1 calc R . . C52 C 0.3607(3) 0.67407(18) 0.25083(17) 0.0324(5) Uani 1 1 d . . . H52 H 0.3811 0.7257 0.1922 0.039 Uiso 1 1 calc R . . C62 C -0.0889(3) 0.75391(19) 0.20120(17) 0.0358(5) Uani 1 1 d . . . H62A H -0.0045 0.7899 0.1468 0.054 Uiso 1 1 calc R . . H62B H -0.1940 0.7949 0.2038 0.054 Uiso 1 1 calc R . . H62C H -0.1163 0.6854 0.1959 0.054 Uiso 1 1 calc R . . C72 C -0.1574(3) 0.67715(18) 0.41556(17) 0.0351(5) Uani 1 1 d . . . H72A H -0.2610 0.7197 0.4162 0.053 Uiso 1 1 calc R . . H72B H -0.1075 0.6726 0.4715 0.053 Uiso 1 1 calc R . . H72C H -0.1879 0.6072 0.4149 0.053 Uiso 1 1 calc R . . C82 C 0.0627(3) 0.87312(17) 0.31062(16) 0.0297(5) Uani 1 1 d . . . H82A H 0.1335 0.9082 0.2496 0.036 Uiso 1 1 calc R . . H82B H -0.0440 0.9134 0.3172 0.036 Uiso 1 1 calc R . . C92 C 0.1597(3) 0.87613(16) 0.38653(16) 0.0274(5) Uani 1 1 d . . . C102 C 0.0787(3) 0.87756(17) 0.47480(16) 0.0310(5) Uani 1 1 d . . . C112 C 0.1666(3) 0.88178(18) 0.54495(18) 0.0389(6) Uani 1 1 d . . . C122 C 0.3435(4) 0.88352(19) 0.5282(2) 0.0466(7) Uani 1 1 d . . . C132 C 0.4296(3) 0.88160(19) 0.4421(2) 0.0459(7) Uani 1 1 d . . . C142 C 0.3385(3) 0.87750(17) 0.37321(19) 0.0357(6) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.02299(12) 0.02365(13) 0.02640(14) -0.00782(9) -0.00474(9) 0.00150(8) Cl1 0.0252(3) 0.0415(3) 0.0542(4) -0.0249(3) 0.0000(3) -0.0025(2) Cl2 0.0583(4) 0.0352(3) 0.0307(3) -0.0077(3) -0.0145(3) 0.0108(3) Si1 0.0263(3) 0.0268(3) 0.0273(3) -0.0081(3) -0.0053(3) 0.0022(2) F11 0.0591(9) 0.0506(9) 0.0320(8) -0.0163(7) -0.0199(7) 0.0121(7) F21 0.0573(9) 0.0477(9) 0.0395(9) -0.0158(7) 0.0139(7) -0.0007(7) F31 0.0302(8) 0.0741(12) 0.0948(14) -0.0480(11) -0.0103(8) 0.0112(8) F41 0.0668(11) 0.0828(12) 0.0692(12) -0.0407(10) -0.0472(9) 0.0395(9) F51 0.0655(10) 0.0440(8) 0.0285(8) -0.0132(7) -0.0126(7) 0.0202(7) C11 0.0255(11) 0.0219(11) 0.0283(12) -0.0082(9) -0.0026(9) 0.0033(8) C21 0.0245(11) 0.0300(12) 0.0353(13) -0.0126(10) 0.0004(10) 0.0028(9) C31 0.0287(12) 0.0383(13) 0.0472(15) -0.0220(12) -0.0130(11) 0.0094(10) C41 0.0432(14) 0.0322(13) 0.0308(13) -0.0094(11) -0.0135(11) 0.0121(11) C51 0.0332(12) 0.0211(11) 0.0289(13) -0.0039(9) -0.0021(10) 0.0036(9) C61 0.0320(13) 0.0421(14) 0.0378(14) -0.0128(12) -0.0093(11) 0.0064(11) C71 0.0436(14) 0.0361(13) 0.0306(13) -0.0074(11) -0.0069(11) 0.0008(11) C81 0.0287(12) 0.0277(12) 0.0370(14) -0.0107(10) -0.0054(10) -0.0011(9) C91 0.0315(12) 0.0178(10) 0.0289(12) -0.0063(9) -0.0058(9) -0.0005(9) C101 0.0396(13) 0.0233(11) 0.0300(13) -0.0078(10) -0.0090(10) -0.0004(10) C111 0.0353(13) 0.0281(12) 0.0343(14) -0.0112(10) 0.0055(11) -0.0039(10) C121 0.0283(12) 0.0366(14) 0.0563(17) -0.0232(13) -0.0045(11) 0.0034(10) C131 0.0427(14) 0.0405(14) 0.0487(16) -0.0207(13) -0.0243(12) 0.0131(11) C141 0.0398(13) 0.0270(12) 0.0276(13) -0.0112(10) -0.0069(10) 0.0061(10) Si2 0.0301(3) 0.0247(3) 0.0252(3) -0.0070(3) -0.0064(3) 0.0017(2) F12 0.0333(7) 0.0547(9) 0.0437(9) -0.0219(7) -0.0014(6) -0.0055(6) F22 0.0855(12) 0.0590(10) 0.0327(9) -0.0140(8) -0.0126(8) -0.0189(9) F32 0.0919(13) 0.0501(10) 0.0906(14) -0.0256(9) -0.0718(11) 0.0132(9) F42 0.0326(8) 0.0627(11) 0.1468(19) -0.0564(12) -0.0318(10) 0.0124(8) F52 0.0416(8) 0.0473(9) 0.0716(11) -0.0336(8) 0.0128(8) -0.0087(7) C12 0.0303(12) 0.0235(11) 0.0292(12) -0.0106(10) -0.0068(9) -0.0003(9) C22 0.0365(12) 0.0265(11) 0.0284(12) -0.0106(10) -0.0096(10) 0.0012(10) C32 0.0388(13) 0.0317(13) 0.0423(15) -0.0151(11) -0.0200(11) 0.0057(10) C42 0.0268(12) 0.0357(13) 0.0575(17) -0.0213(13) -0.0065(11) -0.0037(10) C52 0.0340(12) 0.0270(12) 0.0352(14) -0.0093(10) -0.0006(10) -0.0073(10) C62 0.0351(13) 0.0390(14) 0.0364(14) -0.0123(11) -0.0119(11) 0.0009(11) C72 0.0368(13) 0.0312(12) 0.0356(14) -0.0100(11) -0.0014(11) 0.0050(10) C82 0.0377(13) 0.0232(11) 0.0284(12) -0.0062(10) -0.0089(10) 0.0046(9) C92 0.0342(12) 0.0175(10) 0.0310(13) -0.0056(9) -0.0096(10) 0.0018(9) C102 0.0320(12) 0.0281(12) 0.0340(14) -0.0082(10) -0.0092(10) -0.0011(9) C112 0.0562(16) 0.0293(13) 0.0335(14) -0.0074(11) -0.0154(12) -0.0031(11) C122 0.0591(17) 0.0301(13) 0.0623(19) -0.0145(13) -0.0408(15) 0.0069(12) C132 0.0311(13) 0.0308(13) 0.085(2) -0.0236(14) -0.0246(14) 0.0077(10) C142 0.0327(13) 0.0247(12) 0.0514(16) -0.0152(11) -0.0042(11) 0.0007(10) _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 Cl2 2.4379(6) . ? Zr Cl1 2.4571(6) . ? Zr C41 2.489(2) . ? Zr C42 2.495(2) . ? Zr C31 2.499(2) . ? Zr C32 2.508(2) . ? Zr C51 2.521(2) . ? Zr C21 2.522(2) . ? Zr C22 2.527(2) . ? Zr C52 2.528(2) . ? Zr C11 2.543(2) . ? Zr C12 2.545(2) . ? Si1 C61 1.855(2) . ? Si1 C71 1.859(2) . ? Si1 C11 1.874(2) . ? Si1 C81 1.899(2) . ? F11 C101 1.347(3) . ? F21 C111 1.350(3) . ? F31 C121 1.346(3) . ? F41 C131 1.343(3) . ? F51 C141 1.346(3) . ? C11 C51 1.420(3) . ? C11 C21 1.430(3) . ? C21 C31 1.403(3) . ? C21 H21 0.9500 . ? C31 C41 1.413(4) . ? C31 H31 0.9500 . ? C41 C51 1.401(3) . ? C41 H41 0.9500 . ? C51 H51 0.9500 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C81 C91 1.501(3) . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C91 C101 1.382(3) . ? C91 C141 1.382(3) . ? C101 C111 1.380(3) . ? C111 C121 1.364(4) . ? C121 C131 1.373(4) . ? C131 C141 1.379(3) . ? Si2 C62 1.856(2) . ? Si2 C72 1.860(2) . ? Si2 C12 1.879(2) . ? Si2 C82 1.898(2) . ? F12 C102 1.348(3) . ? F22 C112 1.346(3) . ? F32 C122 1.340(3) . ? F42 C132 1.343(3) . ? F52 C142 1.347(3) . ? C12 C52 1.419(3) . ? C12 C22 1.432(3) . ? C22 C32 1.400(3) . ? C22 H22 0.9500 . ? C32 C42 1.416(4) . ? C32 H32 0.9500 . ? C42 C52 1.401(3) . ? C42 H42 0.9500 . ? C52 H52 0.9500 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C82 C92 1.497(3) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C92 C102 1.383(3) . ? C92 C142 1.389(3) . ? C102 C112 1.380(3) . ? C112 C122 1.374(4) . ? C122 C132 1.369(4) . ? C132 C142 1.379(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cl2 Zr Cl1 99.48(2) . . ? Cl2 Zr C41 135.61(6) . . ? Cl1 Zr C41 99.34(6) . . ? Cl2 Zr C42 100.33(6) . . ? Cl1 Zr C42 135.07(6) . . ? C41 Zr C42 93.91(8) . . ? Cl2 Zr C31 110.84(6) . . ? Cl1 Zr C31 130.66(6) . . ? C41 Zr C31 32.91(8) . . ? C42 Zr C31 77.21(8) . . ? Cl2 Zr C32 131.25(6) . . ? Cl1 Zr C32 109.61(6) . . ? C41 Zr C32 77.63(8) . . ? C42 Zr C32 32.87(8) . . ? C31 Zr C32 78.46(7) . . ? Cl2 Zr C51 115.86(5) . . ? Cl1 Zr C51 78.41(5) . . ? C41 Zr C51 32.46(7) . . ? C42 Zr C51 126.06(8) . . ? C31 Zr C51 53.74(8) . . ? C32 Zr C51 107.89(7) . . ? Cl2 Zr C21 82.35(6) . . ? Cl1 Zr C21 125.22(5) . . ? C41 Zr C21 54.10(8) . . ? C42 Zr C21 97.18(7) . . ? C31 Zr C21 32.45(7) . . ? C32 Zr C21 109.01(7) . . ? C51 Zr C21 53.49(7) . . ? Cl2 Zr C22 124.27(5) . . ? Cl1 Zr C22 81.83(5) . . ? C41 Zr C22 98.00(7) . . ? C42 Zr C22 53.78(8) . . ? C31 Zr C22 109.10(7) . . ? C32 Zr C22 32.29(7) . . ? C51 Zr C22 118.84(7) . . ? C21 Zr C22 140.92(7) . . ? Cl2 Zr C52 78.51(6) . . ? Cl1 Zr C52 116.58(5) . . ? C41 Zr C52 126.07(8) . . ? C42 Zr C52 32.38(8) . . ? C31 Zr C52 107.19(8) . . ? C32 Zr C52 53.78(8) . . ? C51 Zr C52 158.42(8) . . ? C21 Zr C52 117.35(7) . . ? C22 Zr C52 53.34(8) . . ? Cl2 Zr C11 84.78(5) . . ? Cl1 Zr C11 92.48(5) . . ? C41 Zr C11 54.59(7) . . ? C42 Zr C11 129.14(7) . . ? C31 Zr C11 54.45(7) . . ? C32 Zr C11 130.27(7) . . ? C51 Zr C11 32.56(7) . . ? C21 Zr C11 32.80(7) . . ? C22 Zr C11 150.91(7) . . ? C52 Zr C11 148.32(7) . . ? Cl2 Zr C12 91.48(5) . . ? Cl1 Zr C12 85.26(5) . . ? C41 Zr C12 129.88(7) . . ? C42 Zr C12 54.40(7) . . ? C31 Zr C12 129.93(7) . . ? C32 Zr C12 54.47(7) . . ? C51 Zr C12 149.94(7) . . ? C21 Zr C12 149.47(7) . . ? C22 Zr C12 32.80(7) . . ? C52 Zr C12 32.49(7) . . ? C11 Zr C12 175.26(7) . . ? C61 Si1 C71 112.34(11) . . ? C61 Si1 C11 112.10(10) . . ? C71 Si1 C11 110.40(11) . . ? C61 Si1 C81 107.11(11) . . ? C71 Si1 C81 109.14(11) . . ? C11 Si1 C81 105.43(10) . . ? C51 C11 C21 105.55(19) . . ? C51 C11 Si1 126.35(16) . . ? C21 C11 Si1 127.18(17) . . ? C51 C11 Zr 72.86(12) . . ? C21 C11 Zr 72.80(12) . . ? Si1 C11 Zr 127.55(10) . . ? C31 C21 C11 109.0(2) . . ? C31 C21 Zr 72.87(12) . . ? C11 C21 Zr 74.40(12) . . ? C31 C21 H21 125.5 . . ? C11 C21 H21 125.5 . . ? Zr C21 H21 119.0 . . ? C21 C31 C41 108.1(2) . . ? C21 C31 Zr 74.68(13) . . ? C41 C31 Zr 73.13(13) . . ? C21 C31 H31 126.0 . . ? C41 C31 H31 126.0 . . ? Zr C31 H31 118.2 . . ? C51 C41 C31 107.5(2) . . ? C51 C41 Zr 75.05(13) . . ? C31 C41 Zr 73.96(13) . . ? C51 C41 H41 126.2 . . ? C31 C41 H41 126.2 . . ? Zr C41 H41 116.9 . . ? C41 C51 C11 109.8(2) . . ? C41 C51 Zr 72.49(13) . . ? C11 C51 Zr 74.57(12) . . ? C41 C51 H51 125.1 . . ? C11 C51 H51 125.1 . . ? Zr C51 H51 119.5 . . ? Si1 C61 H61A 109.5 . . ? Si1 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? Si1 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? Si1 C71 H71A 109.5 . . ? Si1 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? Si1 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C91 C81 Si1 113.75(15) . . ? C91 C81 H81A 108.8 . . ? Si1 C81 H81A 108.8 . . ? C91 C81 H81B 108.8 . . ? Si1 C81 H81B 108.8 . . ? H81A C81 H81B 107.7 . . ? C101 C91 C141 115.6(2) . . ? C101 C91 C81 122.2(2) . . ? C141 C91 C81 122.2(2) . . ? F11 C101 C111 117.6(2) . . ? F11 C101 C91 119.7(2) . . ? C111 C101 C91 122.6(2) . . ? F21 C111 C121 119.9(2) . . ? F21 C111 C101 120.2(2) . . ? C121 C111 C101 119.9(2) . . ? F31 C121 C111 120.4(2) . . ? F31 C121 C131 120.1(2) . . ? C111 C121 C131 119.5(2) . . ? F41 C131 C121 119.9(2) . . ? F41 C131 C141 120.5(2) . . ? C121 C131 C141 119.5(2) . . ? F51 C141 C131 118.1(2) . . ? F51 C141 C91 119.1(2) . . ? C131 C141 C91 122.8(2) . . ? C62 Si2 C72 111.36(11) . . ? C62 Si2 C12 114.05(10) . . ? C72 Si2 C12 107.85(10) . . ? C62 Si2 C82 106.61(11) . . ? C72 Si2 C82 109.64(10) . . ? C12 Si2 C82 107.20(10) . . ? C52 C12 C22 105.4(2) . . ? C52 C12 Si2 128.89(17) . . ? C22 C12 Si2 125.17(17) . . ? C52 C12 Zr 73.09(12) . . ? C22 C12 Zr 72.90(12) . . ? Si2 C12 Zr 124.94(10) . . ? C32 C22 C12 109.5(2) . . ? C32 C22 Zr 73.11(12) . . ? C12 C22 Zr 74.30(12) . . ? C32 C22 H22 125.3 . . ? C12 C22 H22 125.3 . . ? Zr C22 H22 119.1 . . ? C22 C32 C42 107.5(2) . . ? C22 C32 Zr 74.59(12) . . ? C42 C32 Zr 73.06(13) . . ? C22 C32 H32 126.2 . . ? C42 C32 H32 126.2 . . ? Zr C32 H32 118.1 . . ? C52 C42 C32 107.9(2) . . ? C52 C42 Zr 75.10(13) . . ? C32 C42 Zr 74.07(13) . . ? C52 C42 H42 126.0 . . ? C32 C42 H42 126.0 . . ? Zr C42 H42 116.9 . . ? C42 C52 C12 109.6(2) . . ? C42 C52 Zr 72.52(13) . . ? C12 C52 Zr 74.42(12) . . ? C42 C52 H52 125.2 . . ? C12 C52 H52 125.2 . . ? Zr C52 H52 119.6 . . ? Si2 C62 H62A 109.5 . . ? Si2 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? Si2 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? Si2 C72 H72A 109.5 . . ? Si2 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? Si2 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? C92 C82 Si2 114.96(15) . . ? C92 C82 H82A 108.5 . . ? Si2 C82 H82A 108.5 . . ? C92 C82 H82B 108.5 . . ? Si2 C82 H82B 108.5 . . ? H82A C82 H82B 107.5 . . ? C102 C92 C142 115.1(2) . . ? C102 C92 C82 122.7(2) . . ? C142 C92 C82 122.2(2) . . ? F12 C102 C112 117.2(2) . . ? F12 C102 C92 119.46(19) . . ? C112 C102 C92 123.3(2) . . ? F22 C112 C122 120.2(2) . . ? F22 C112 C102 120.4(2) . . ? C122 C112 C102 119.4(2) . . ? F32 C122 C132 119.9(3) . . ? F32 C122 C112 120.7(3) . . ? C132 C122 C112 119.4(2) . . ? F42 C132 C122 119.9(2) . . ? F42 C132 C142 120.2(3) . . ? C122 C132 C142 119.9(2) . . ? F52 C142 C132 117.9(2) . . ? F52 C142 C92 119.3(2) . . ? C132 C142 C92 122.8(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C61 Si1 C11 C51 50.6(2) . . . . ? C71 Si1 C11 C51 176.65(18) . . . . ? C81 Si1 C11 C51 -65.6(2) . . . . ? C61 Si1 C11 C21 -142.00(19) . . . . ? C71 Si1 C11 C21 -15.9(2) . . . . ? C81 Si1 C11 C21 101.8(2) . . . . ? C61 Si1 C11 Zr -45.41(16) . . . . ? C71 Si1 C11 Zr 80.65(15) . . . . ? C81 Si1 C11 Zr -161.60(12) . . . . ? Cl2 Zr C11 C51 -163.12(12) . . . . ? Cl1 Zr C11 C51 -63.82(12) . . . . ? C41 Zr C11 C51 35.89(13) . . . . ? C42 Zr C11 C51 97.80(15) . . . . ? C31 Zr C11 C51 76.60(14) . . . . ? C32 Zr C11 C51 54.67(16) . . . . ? C21 Zr C11 C51 112.90(19) . . . . ? C22 Zr C11 C51 13.8(2) . . . . ? C52 Zr C11 C51 138.81(16) . . . . ? Cl2 Zr C11 C21 83.98(13) . . . . ? Cl1 Zr C11 C21 -176.71(13) . . . . ? C41 Zr C11 C21 -77.01(14) . . . . ? C42 Zr C11 C21 -15.10(18) . . . . ? C31 Zr C11 C21 -36.30(13) . . . . ? C32 Zr C11 C21 -58.23(17) . . . . ? C51 Zr C11 C21 -112.90(19) . . . . ? C22 Zr C11 C21 -99.12(18) . . . . ? C52 Zr C11 C21 25.9(2) . . . . ? Cl2 Zr C11 Si1 -40.07(12) . . . . ? Cl1 Zr C11 Si1 59.24(12) . . . . ? C41 Zr C11 Si1 158.94(17) . . . . ? C42 Zr C11 Si1 -139.15(12) . . . . ? C31 Zr C11 Si1 -160.35(17) . . . . ? C32 Zr C11 Si1 177.72(11) . . . . ? C51 Zr C11 Si1 123.1(2) . . . . ? C21 Zr C11 Si1 -124.0(2) . . . . ? C22 Zr C11 Si1 136.83(14) . . . . ? C52 Zr C11 Si1 -98.14(17) . . . . ? C51 C11 C21 C31 -0.9(2) . . . . ? Si1 C11 C21 C31 -170.35(16) . . . . ? Zr C11 C21 C31 65.18(15) . . . . ? C51 C11 C21 Zr -66.03(14) . . . . ? Si1 C11 C21 Zr 124.47(16) . . . . ? Cl2 Zr C21 C31 151.65(14) . . . . ? Cl1 Zr C21 C31 -112.11(13) . . . . ? C41 Zr C21 C31 -37.51(14) . . . . ? C42 Zr C21 C31 52.12(15) . . . . ? C32 Zr C21 C31 20.55(16) . . . . ? C51 Zr C21 C31 -78.04(15) . . . . ? C22 Zr C21 C31 14.3(2) . . . . ? C52 Zr C21 C31 78.85(15) . . . . ? C11 Zr C21 C31 -116.1(2) . . . . ? C12 Zr C21 C31 71.8(2) . . . . ? Cl2 Zr C21 C11 -92.22(13) . . . . ? Cl1 Zr C21 C11 4.02(15) . . . . ? C41 Zr C21 C11 78.61(14) . . . . ? C42 Zr C21 C11 168.25(14) . . . . ? C31 Zr C21 C11 116.1(2) . . . . ? C32 Zr C21 C11 136.68(13) . . . . ? C51 Zr C21 C11 38.09(13) . . . . ? C22 Zr C21 C11 130.40(14) . . . . ? C52 Zr C21 C11 -165.03(13) . . . . ? C12 Zr C21 C11 -172.07(13) . . . . ? C11 C21 C31 C41 -0.1(3) . . . . ? Zr C21 C31 C41 66.06(16) . . . . ? C11 C21 C31 Zr -66.17(15) . . . . ? Cl2 Zr C31 C21 -30.24(15) . . . . ? Cl1 Zr C31 C21 93.77(14) . . . . ? C41 Zr C31 C21 114.8(2) . . . . ? C42 Zr C31 C21 -126.58(15) . . . . ? C32 Zr C31 C21 -160.20(15) . . . . ? C51 Zr C31 C21 77.20(14) . . . . ? C22 Zr C31 C21 -170.53(13) . . . . ? C52 Zr C31 C21 -114.19(14) . . . . ? C11 Zr C31 C21 36.71(13) . . . . ? C12 Zr C31 C21 -141.00(13) . . . . ? Cl2 Zr C31 C41 -145.01(12) . . . . ? Cl1 Zr C31 C41 -21.00(16) . . . . ? C42 Zr C31 C41 118.65(15) . . . . ? C32 Zr C31 C41 85.03(14) . . . . ? C51 Zr C31 C41 -37.57(13) . . . . ? C21 Zr C31 C41 -114.8(2) . . . . ? C22 Zr C31 C41 74.69(14) . . . . ? C52 Zr C31 C41 131.04(14) . . . . ? C11 Zr C31 C41 -78.06(14) . . . . ? C12 Zr C31 C41 104.22(15) . . . . ? C21 C31 C41 C51 1.1(2) . . . . ? Zr C31 C41 C51 68.15(15) . . . . ? C21 C31 C41 Zr -67.09(16) . . . . ? Cl2 Zr C41 C51 -63.63(16) . . . . ? Cl1 Zr C41 C51 50.37(14) . . . . ? C42 Zr C41 C51 -172.70(14) . . . . ? C31 Zr C41 C51 -113.6(2) . . . . ? C32 Zr C41 C51 158.56(15) . . . . ? C21 Zr C41 C51 -76.67(14) . . . . ? C22 Zr C41 C51 133.35(14) . . . . ? C52 Zr C41 C51 -176.71(13) . . . . ? C11 Zr C41 C51 -36.00(13) . . . . ? C12 Zr C41 C51 141.99(13) . . . . ? Cl2 Zr C41 C31 50.01(16) . . . . ? Cl1 Zr C41 C31 164.01(12) . . . . ? C42 Zr C41 C31 -59.07(14) . . . . ? C32 Zr C41 C31 -87.81(14) . . . . ? C51 Zr C41 C31 113.6(2) . . . . ? C21 Zr C41 C31 36.97(13) . . . . ? C22 Zr C41 C31 -113.02(14) . . . . ? C52 Zr C41 C31 -63.07(16) . . . . ? C11 Zr C41 C31 77.63(14) . . . . ? C12 Zr C41 C31 -104.37(14) . . . . ? C31 C41 C51 C11 -1.6(2) . . . . ? Zr C41 C51 C11 65.79(15) . . . . ? C31 C41 C51 Zr -67.41(16) . . . . ? C21 C11 C51 C41 1.5(2) . . . . ? Si1 C11 C51 C41 171.14(15) . . . . ? Zr C11 C51 C41 -64.46(15) . . . . ? C21 C11 C51 Zr 65.98(14) . . . . ? Si1 C11 C51 Zr -124.40(16) . . . . ? Cl2 Zr C51 C41 135.86(13) . . . . ? Cl1 Zr C51 C41 -129.12(14) . . . . ? C42 Zr C51 C41 9.02(18) . . . . ? C31 Zr C51 C41 38.12(14) . . . . ? C32 Zr C51 C41 -22.04(15) . . . . ? C21 Zr C51 C41 78.73(15) . . . . ? C22 Zr C51 C41 -55.29(16) . . . . ? C52 Zr C51 C41 7.3(3) . . . . ? C11 Zr C51 C41 117.11(19) . . . . ? C12 Zr C51 C41 -70.6(2) . . . . ? Cl2 Zr C51 C11 18.75(14) . . . . ? Cl1 Zr C51 C11 113.77(12) . . . . ? C41 Zr C51 C11 -117.11(19) . . . . ? C42 Zr C51 C11 -108.09(14) . . . . ? C31 Zr C51 C11 -78.99(14) . . . . ? C32 Zr C51 C11 -139.15(13) . . . . ? C21 Zr C51 C11 -38.38(12) . . . . ? C22 Zr C51 C11 -172.40(12) . . . . ? C52 Zr C51 C11 -109.9(2) . . . . ? C12 Zr C51 C11 172.25(12) . . . . ? C61 Si1 C81 C91 -178.46(16) . . . . ? C71 Si1 C81 C91 59.69(19) . . . . ? C11 Si1 C81 C91 -58.90(19) . . . . ? Si1 C81 C91 C101 -90.2(2) . . . . ? Si1 C81 C91 C141 89.8(2) . . . . ? C141 C91 C101 F11 178.67(19) . . . . ? C81 C91 C101 F11 -1.4(3) . . . . ? C141 C91 C101 C111 0.7(3) . . . . ? C81 C91 C101 C111 -179.4(2) . . . . ? F11 C101 C111 F21 0.3(3) . . . . ? C91 C101 C111 F21 178.37(19) . . . . ? F11 C101 C111 C121 -178.9(2) . . . . ? C91 C101 C111 C121 -0.8(3) . . . . ? F21 C111 C121 F31 0.0(3) . . . . ? C101 C111 C121 F31 179.2(2) . . . . ? F21 C111 C121 C131 -178.7(2) . . . . ? C101 C111 C121 C131 0.5(4) . . . . ? F31 C121 C131 F41 0.2(4) . . . . ? C111 C121 C131 F41 179.0(2) . . . . ? F31 C121 C131 C141 -178.8(2) . . . . ? C111 C121 C131 C141 0.0(4) . . . . ? F41 C131 C141 F51 -1.4(3) . . . . ? C121 C131 C141 F51 177.5(2) . . . . ? F41 C131 C141 C91 -179.1(2) . . . . ? C121 C131 C141 C91 -0.1(4) . . . . ? C101 C91 C141 F51 -177.82(19) . . . . ? C81 C91 C141 F51 2.3(3) . . . . ? C101 C91 C141 C131 -0.2(3) . . . . ? C81 C91 C141 C131 179.9(2) . . . . ? C62 Si2 C12 C52 56.7(2) . . . . ? C72 Si2 C12 C52 -179.08(19) . . . . ? C82 Si2 C12 C52 -61.1(2) . . . . ? C62 Si2 C12 C22 -132.57(18) . . . . ? C72 Si2 C12 C22 -8.3(2) . . . . ? C82 Si2 C12 C22 109.67(18) . . . . ? C62 Si2 C12 Zr -39.51(16) . . . . ? C72 Si2 C12 Zr 84.73(14) . . . . ? C82 Si2 C12 Zr -157.27(12) . . . . ? Cl2 Zr C12 C52 -65.70(13) . . . . ? Cl1 Zr C12 C52 -165.10(13) . . . . ? C41 Zr C12 C52 96.69(15) . . . . ? C42 Zr C12 C52 35.96(14) . . . . ? C31 Zr C12 C52 53.35(17) . . . . ? C32 Zr C12 C52 76.67(15) . . . . ? C51 Zr C12 C52 137.98(16) . . . . ? C21 Zr C12 C52 11.7(2) . . . . ? C22 Zr C12 C52 112.63(19) . . . . ? Cl2 Zr C12 C22 -178.33(12) . . . . ? Cl1 Zr C12 C22 82.27(12) . . . . ? C41 Zr C12 C22 -15.95(17) . . . . ? C42 Zr C12 C22 -76.67(14) . . . . ? C31 Zr C12 C22 -59.28(16) . . . . ? C32 Zr C12 C22 -35.96(13) . . . . ? C51 Zr C12 C22 25.3(2) . . . . ? C21 Zr C12 C22 -100.94(18) . . . . ? C52 Zr C12 C22 -112.63(19) . . . . ? Cl2 Zr C12 Si2 60.32(12) . . . . ? Cl1 Zr C12 Si2 -39.07(12) . . . . ? C41 Zr C12 Si2 -137.29(12) . . . . ? C42 Zr C12 Si2 161.99(17) . . . . ? C31 Zr C12 Si2 179.38(11) . . . . ? C32 Zr C12 Si2 -157.30(17) . . . . ? C51 Zr C12 Si2 -96.00(17) . . . . ? C21 Zr C12 Si2 137.72(13) . . . . ? C22 Zr C12 Si2 -121.3(2) . . . . ? C52 Zr C12 Si2 126.0(2) . . . . ? C52 C12 C22 C32 -1.2(2) . . . . ? Si2 C12 C22 C32 -173.72(15) . . . . ? Zr C12 C22 C32 65.20(15) . . . . ? C52 C12 C22 Zr -66.38(14) . . . . ? Si2 C12 C22 Zr 121.08(15) . . . . ? Cl2 Zr C22 C32 -114.54(13) . . . . ? Cl1 Zr C22 C32 149.51(14) . . . . ? C41 Zr C22 C32 51.15(15) . . . . ? C42 Zr C22 C32 -37.84(14) . . . . ? C31 Zr C22 C32 19.20(16) . . . . ? C51 Zr C22 C32 77.61(16) . . . . ? C21 Zr C22 C32 11.2(2) . . . . ? C52 Zr C22 C32 -78.39(15) . . . . ? C11 Zr C22 C32 69.2(2) . . . . ? C12 Zr C22 C32 -116.6(2) . . . . ? Cl2 Zr C22 C12 2.01(15) . . . . ? Cl1 Zr C22 C12 -93.93(12) . . . . ? C41 Zr C22 C12 167.71(13) . . . . ? C42 Zr C22 C12 78.72(14) . . . . ? C31 Zr C22 C12 135.76(13) . . . . ? C32 Zr C22 C12 116.6(2) . . . . ? C51 Zr C22 C12 -165.83(12) . . . . ? C21 Zr C22 C12 127.71(14) . . . . ? C52 Zr C22 C12 38.17(13) . . . . ? C11 Zr C22 C12 -174.25(13) . . . . ? C12 C22 C32 C42 0.2(2) . . . . ? Zr C22 C32 C42 66.17(15) . . . . ? C12 C22 C32 Zr -65.97(15) . . . . ? Cl2 Zr C32 C22 90.81(15) . . . . ? Cl1 Zr C32 C22 -32.22(15) . . . . ? C41 Zr C32 C22 -127.86(15) . . . . ? C42 Zr C32 C22 114.2(2) . . . . ? C31 Zr C32 C22 -161.51(16) . . . . ? C51 Zr C32 C22 -115.96(14) . . . . ? C21 Zr C32 C22 -172.59(14) . . . . ? C52 Zr C32 C22 76.93(15) . . . . ? C11 Zr C32 C22 -143.44(13) . . . . ? C12 Zr C32 C22 36.54(13) . . . . ? Cl2 Zr C32 C42 -23.43(16) . . . . ? Cl1 Zr C32 C42 -146.46(12) . . . . ? C41 Zr C32 C42 117.90(15) . . . . ? C31 Zr C32 C42 84.25(14) . . . . ? C51 Zr C32 C42 129.79(14) . . . . ? C21 Zr C32 C42 73.17(15) . . . . ? C22 Zr C32 C42 -114.2(2) . . . . ? C52 Zr C32 C42 -37.32(13) . . . . ? C11 Zr C32 C42 102.32(15) . . . . ? C12 Zr C32 C42 -77.70(14) . . . . ? C22 C32 C42 C52 0.9(2) . . . . ? Zr C32 C42 C52 68.08(15) . . . . ? C22 C32 C42 Zr -67.20(15) . . . . ? Cl2 Zr C42 C52 48.28(15) . . . . ? Cl1 Zr C42 C52 -66.56(17) . . . . ? C41 Zr C42 C52 -173.95(15) . . . . ? C31 Zr C42 C52 157.51(16) . . . . ? C32 Zr C42 C52 -114.0(2) . . . . ? C51 Zr C42 C52 -178.79(13) . . . . ? C21 Zr C42 C52 131.77(15) . . . . ? C22 Zr C42 C52 -76.89(15) . . . . ? C11 Zr C42 C52 139.94(14) . . . . ? C12 Zr C42 C52 -36.09(13) . . . . ? Cl2 Zr C42 C32 162.31(12) . . . . ? Cl1 Zr C42 C32 47.47(17) . . . . ? C41 Zr C42 C32 -59.92(14) . . . . ? C31 Zr C42 C32 -88.46(14) . . . . ? C51 Zr C42 C32 -64.75(16) . . . . ? C21 Zr C42 C32 -114.20(14) . . . . ? C22 Zr C42 C32 37.14(13) . . . . ? C52 Zr C42 C32 114.0(2) . . . . ? C11 Zr C42 C32 -106.03(15) . . . . ? C12 Zr C42 C32 77.94(14) . . . . ? C32 C42 C52 C12 -1.6(2) . . . . ? Zr C42 C52 C12 65.74(15) . . . . ? C32 C42 C52 Zr -67.38(15) . . . . ? C22 C12 C52 C42 1.7(2) . . . . ? Si2 C12 C52 C42 173.89(16) . . . . ? Zr C12 C52 C42 -64.52(16) . . . . ? C22 C12 C52 Zr 66.24(14) . . . . ? Si2 C12 C52 Zr -121.59(17) . . . . ? Cl2 Zr C52 C42 -131.47(15) . . . . ? Cl1 Zr C52 C42 133.57(13) . . . . ? C41 Zr C52 C42 7.48(18) . . . . ? C31 Zr C52 C42 -22.99(16) . . . . ? C32 Zr C52 C42 37.92(14) . . . . ? C51 Zr C52 C42 2.7(3) . . . . ? C21 Zr C52 C42 -56.42(17) . . . . ? C22 Zr C52 C42 78.36(16) . . . . ? C11 Zr C52 C42 -71.9(2) . . . . ? C12 Zr C52 C42 116.9(2) . . . . ? Cl2 Zr C52 C12 111.61(13) . . . . ? Cl1 Zr C52 C12 16.65(15) . . . . ? C41 Zr C52 C12 -109.44(14) . . . . ? C42 Zr C52 C12 -116.9(2) . . . . ? C31 Zr C52 C12 -139.91(13) . . . . ? C32 Zr C52 C12 -79.00(14) . . . . ? C51 Zr C52 C12 -114.2(2) . . . . ? C21 Zr C52 C12 -173.34(12) . . . . ? C22 Zr C52 C12 -38.56(13) . . . . ? C11 Zr C52 C12 171.20(12) . . . . ? C62 Si2 C82 C92 -172.56(17) . . . . ? C72 Si2 C82 C92 66.77(19) . . . . ? C12 Si2 C82 C92 -50.05(19) . . . . ? Si2 C82 C92 C102 -87.6(2) . . . . ? Si2 C82 C92 C142 92.3(2) . . . . ? C142 C92 C102 F12 179.09(19) . . . . ? C82 C92 C102 F12 -1.0(3) . . . . ? C142 C92 C102 C112 1.0(3) . . . . ? C82 C92 C102 C112 -179.1(2) . . . . ? F12 C102 C112 F22 0.2(3) . . . . ? C92 C102 C112 F22 178.2(2) . . . . ? F12 C102 C112 C122 -178.9(2) . . . . ? C92 C102 C112 C122 -0.8(4) . . . . ? F22 C112 C122 F32 0.3(4) . . . . ? C102 C112 C122 F32 179.3(2) . . . . ? F22 C112 C122 C132 -178.7(2) . . . . ? C102 C112 C122 C132 0.3(4) . . . . ? F32 C122 C132 F42 -0.5(4) . . . . ? C112 C122 C132 F42 178.5(2) . . . . ? F32 C122 C132 C142 -179.3(2) . . . . ? C112 C122 C132 C142 -0.3(4) . . . . ? F42 C132 C142 F52 0.1(3) . . . . ? C122 C132 C142 F52 178.9(2) . . . . ? F42 C132 C142 C92 -178.2(2) . . . . ? C122 C132 C142 C92 0.6(4) . . . . ? C102 C92 C142 F52 -179.25(19) . . . . ? C82 C92 C142 F52 0.9(3) . . . . ? C102 C92 C142 C132 -1.0(3) . . . . ? C82 C92 C142 C132 179.2(2) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.65 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.637 _refine_diff_density_min -0.495 _refine_diff_density_rms 0.075 #===END