# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_coden_Cambridge 222 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Fu-Chen Liu.' 'Shou-Chon Chen.' 'Gene-Hsian Lee.' 'Shie-Ming Peng.' 'Chien-Chan Yang.' _publ_contact_author_name 'Fu-Chen Liu' _publ_contact_author_address ; Department of Chemistry National Dong Hwa University 1, Sec. 2, Da Hsueh Rd. Shoufeng Hualien 974 TAIWAN ; _publ_contact_author_email FCLIU@MAIL.NDHU.EDU.TW _publ_section_title ; Novel u3-oxo complexes prepared from Cp*Zr(BH3R) (R = H, CH3) and B(C6F5)3 in ether ; # Attachment 'a.cif' data_ic9573 _database_code_depnum_ccdc_archive 'CCDC 672315' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H33 B3 Zr' _chemical_formula_weight 313.04 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P4(3) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y, x, z+3/4' 'y, -x, z+1/4' _cell_length_a 7.8250(3) _cell_length_b 7.8250(3) _cell_length_c 28.7350(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1759.46(12) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6320 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 25.67 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.182 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.605 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8394 _exptl_absorpt_correction_T_max 0.8394 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17156 _diffrn_reflns_av_R_equivalents 0.0366 _diffrn_reflns_av_sigmaI/netI 0.0339 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -37 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 2.60 _diffrn_reflns_theta_max 27.50 _reflns_number_total 4028 _reflns_number_gt 3828 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0344P)^2^+0.2734P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.04(4) _refine_ls_number_reflns 4028 _refine_ls_number_parameters 181 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0278 _refine_ls_R_factor_gt 0.0257 _refine_ls_wR_factor_ref 0.0643 _refine_ls_wR_factor_gt 0.0632 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _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 0.33118(2) 0.90785(2) 0.220270(8) 0.02016(6) Uani 1 1 d . . . B1 B 0.1099(4) 0.7000(4) 0.22851(11) 0.0325(7) Uani 1 1 d . . . H1A H 0.132(5) 0.805(4) 0.2567(13) 0.049 Uiso 1 1 d . . . H1B H 0.125(5) 0.780(5) 0.1928(12) 0.049 Uiso 1 1 d . . . H1C H 0.230(4) 0.633(4) 0.2339(12) 0.049 Uiso 1 1 d . . . B2 B 0.5042(4) 0.7974(4) 0.15975(13) 0.0374(7) Uani 1 1 d . . . H2A H 0.364(5) 0.830(5) 0.1536(14) 0.056 Uiso 1 1 d . . . H2B H 0.549(5) 0.919(5) 0.1779(14) 0.056 Uiso 1 1 d . . . H2C H 0.488(5) 0.688(5) 0.1898(14) 0.056 Uiso 1 1 d . . . B3 B 0.4989(4) 0.8757(4) 0.28855(12) 0.0363(7) Uani 1 1 d . . . H3A H 0.557(4) 0.972(5) 0.2614(13) 0.055 Uiso 1 1 d . . . H3B H 0.339(4) 0.916(4) 0.2908(16) 0.055 Uiso 1 1 d . . . H3C H 0.492(5) 0.754(5) 0.2729(13) 0.055 Uiso 1 1 d . . . C1 C -0.0616(4) 0.5945(5) 0.23161(14) 0.0577(10) Uani 1 1 d . . . H1D H -0.0357 0.4759 0.2399 0.087 Uiso 1 1 calc R . . H1E H -0.1198 0.5974 0.2014 0.087 Uiso 1 1 calc R . . H1F H -0.1358 0.6448 0.2554 0.087 Uiso 1 1 calc R . . C2 C 0.6122(5) 0.7382(6) 0.11593(15) 0.0627(10) Uani 1 1 d . . . H2D H 0.6827 0.6394 0.1244 0.094 Uiso 1 1 calc R . . H2E H 0.6861 0.8320 0.1057 0.094 Uiso 1 1 calc R . . H2F H 0.5345 0.7064 0.0906 0.094 Uiso 1 1 calc R . . C3 C 0.6115(5) 0.8814(5) 0.33500(13) 0.0586(11) Uani 1 1 d . . . H3D H 0.6408 0.7647 0.3444 0.088 Uiso 1 1 calc R . . H3E H 0.5462 0.9370 0.3599 0.088 Uiso 1 1 calc R . . H3F H 0.7166 0.9461 0.3291 0.088 Uiso 1 1 calc R . . C4 C 0.2848(4) 1.1606(4) 0.16845(11) 0.0428(8) Uani 1 1 d . . . C5 C 0.1239(4) 1.1126(4) 0.18480(10) 0.0319(6) Uani 1 1 d . . . C6 C 0.1174(3) 1.1419(3) 0.23272(8) 0.0280(6) Uani 1 1 d . . . C7 C 0.2742(4) 1.2078(3) 0.24671(10) 0.0363(7) Uani 1 1 d . . . C8 C 0.3800(4) 1.2200(3) 0.20737(14) 0.0448(9) Uani 1 1 d . . . C9 C 0.3440(8) 1.1658(6) 0.11871(16) 0.102(2) Uani 1 1 d . . . H9A H 0.3133 1.2761 0.1049 0.153 Uiso 1 1 calc R . . H9B H 0.2890 1.0734 0.1012 0.153 Uiso 1 1 calc R . . H9C H 0.4683 1.1511 0.1176 0.153 Uiso 1 1 calc R . . C10 C -0.0246(6) 1.0568(6) 0.15501(15) 0.0721(14) Uani 1 1 d . . . H10A H -0.0891 1.1574 0.1448 0.108 Uiso 1 1 calc R . . H10B H -0.0995 0.9816 0.1731 0.108 Uiso 1 1 calc R . . H10C H 0.0183 0.9950 0.1277 0.108 Uiso 1 1 calc R . . C11 C -0.0400(5) 1.1175(5) 0.26268(14) 0.0594(10) Uani 1 1 d . . . H11A H -0.1063 1.2238 0.2633 0.089 Uiso 1 1 calc R . . H11B H -0.0053 1.0875 0.2944 0.089 Uiso 1 1 calc R . . H11C H -0.1104 1.0255 0.2497 0.089 Uiso 1 1 calc R . . C12 C 0.3151(7) 1.2771(5) 0.29431(16) 0.0803(16) Uani 1 1 d . . . H12A H 0.2821 1.3978 0.2959 0.120 Uiso 1 1 calc R . . H12B H 0.4380 1.2664 0.3002 0.120 Uiso 1 1 calc R . . H12C H 0.2518 1.2123 0.3179 0.120 Uiso 1 1 calc R . . C13 C 0.5550(5) 1.2976(4) 0.2054(3) 0.111(3) Uani 1 1 d . . . H13A H 0.5452 1.4209 0.2001 0.167 Uiso 1 1 calc R . . H13B H 0.6201 1.2455 0.1800 0.167 Uiso 1 1 calc R . . H13C H 0.6142 1.2772 0.2350 0.167 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01923(11) 0.01834(11) 0.02291(10) 0.00302(9) -0.00318(9) -0.00009(8) B1 0.0299(14) 0.0298(14) 0.0378(19) 0.0061(13) -0.0068(13) -0.0081(11) B2 0.0323(17) 0.0341(18) 0.0458(19) -0.0051(15) 0.0062(14) 0.0048(14) B3 0.0377(17) 0.0332(17) 0.0381(17) 0.0115(14) -0.0141(14) -0.0076(13) C1 0.0452(18) 0.060(2) 0.068(3) 0.0107(19) -0.0047(16) -0.0279(16) C2 0.055(2) 0.070(3) 0.063(2) -0.018(2) 0.0252(18) 0.0030(19) C3 0.073(3) 0.058(2) 0.044(2) 0.0192(17) -0.0349(18) -0.0271(18) C4 0.0495(18) 0.0403(16) 0.0387(16) 0.0227(13) 0.0162(14) 0.0254(14) C5 0.0319(14) 0.0320(14) 0.0318(14) -0.0017(11) -0.0093(11) 0.0144(11) C6 0.0286(12) 0.0272(12) 0.0282(14) 0.0023(9) 0.0014(10) 0.0103(10) C7 0.0479(17) 0.0193(12) 0.0418(16) -0.0067(11) -0.0158(13) 0.0087(11) C8 0.0263(13) 0.0173(11) 0.091(3) 0.0167(14) -0.0014(14) 0.0015(10) C9 0.165(5) 0.091(3) 0.051(3) 0.050(2) 0.060(3) 0.077(4) C10 0.071(3) 0.073(3) 0.073(3) -0.024(2) -0.052(2) 0.034(2) C11 0.062(2) 0.053(2) 0.064(2) 0.0121(18) 0.0320(19) 0.0209(18) C12 0.127(4) 0.047(2) 0.067(3) -0.0266(19) -0.059(3) 0.025(2) C13 0.0320(17) 0.0284(16) 0.273(9) 0.043(3) 0.002(3) -0.0047(13) _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 B2 2.367(3) . ? Zr B3 2.374(3) . ? Zr B1 2.387(3) . ? Zr C5 2.498(2) . ? Zr C8 2.500(3) . ? Zr C4 2.502(3) . ? Zr C6 2.506(2) . ? Zr C7 2.507(3) . ? Zr H1A 2.04(4) . ? Zr H1B 2.06(4) . ? Zr H1C 2.33(3) . ? Zr H2A 2.02(4) . ? Zr H2B 2.10(4) . ? Zr H2C 2.29(4) . ? Zr H3A 2.18(4) . ? Zr H3B 2.03(5) . ? Zr H3C 2.31(4) . ? B1 C1 1.578(4) . ? B1 H1A 1.17(4) . ? B1 H1B 1.21(4) . ? B1 H1C 1.09(3) . ? B2 C2 1.586(5) . ? B2 H2A 1.14(4) . ? B2 H2B 1.14(4) . ? B2 H2C 1.22(4) . ? B3 C3 1.600(4) . ? B3 H3A 1.17(4) . ? B3 H3B 1.29(3) . ? B3 H3C 1.06(4) . ? C1 H1D 0.9800 . ? C1 H1E 0.9800 . ? C1 H1F 0.9800 . ? C2 H2D 0.9800 . ? C2 H2E 0.9800 . ? C2 H2F 0.9800 . ? C3 H3D 0.9800 . ? C3 H3E 0.9800 . ? C3 H3F 0.9800 . ? C4 C5 1.395(4) . ? C4 C8 1.422(5) . ? C4 C9 1.503(5) . ? C5 C6 1.397(4) . ? C5 C10 1.508(4) . ? C6 C7 1.390(4) . ? C6 C11 1.515(4) . ? C7 C8 1.404(5) . ? C7 C12 1.506(4) . ? C8 C13 1.499(5) . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? 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 B2 Zr B3 104.61(13) . . ? B2 Zr B1 103.83(12) . . ? B3 Zr B1 104.29(11) . . ? B2 Zr C5 107.82(11) . . ? B3 Zr C5 139.85(11) . . ? B1 Zr C5 90.37(10) . . ? B2 Zr C8 99.22(12) . . ? B3 Zr C8 98.13(12) . . ? B1 Zr C8 142.31(10) . . ? C5 Zr C8 53.98(10) . . ? B2 Zr C4 86.24(11) . . ? B3 Zr C4 130.99(12) . . ? B1 Zr C4 119.49(11) . . ? C5 Zr C4 32.41(10) . . ? C8 Zr C4 33.04(12) . . ? B2 Zr C6 138.89(11) . . ? B3 Zr C6 109.17(11) . . ? B1 Zr C6 89.98(10) . . ? C5 Zr C6 32.42(9) . . ? C8 Zr C6 53.79(9) . . ? C4 Zr C6 53.88(9) . . ? B2 Zr C7 131.76(12) . . ? B3 Zr C7 86.96(11) . . ? B1 Zr C7 118.62(11) . . ? C5 Zr C7 53.67(9) . . ? C8 Zr C7 32.58(11) . . ? C4 Zr C7 54.16(11) . . ? C6 Zr C7 32.21(9) . . ? B2 Zr H1A 132.0(10) . . ? B3 Zr H1A 87.5(10) . . ? B1 Zr H1A 29.2(10) . . ? C5 Zr H1A 88.1(10) . . ? C8 Zr H1A 125.3(10) . . ? C4 Zr H1A 120.4(10) . . ? C6 Zr H1A 72.9(10) . . ? C7 Zr H1A 94.5(10) . . ? B2 Zr H1B 89.4(10) . . ? B3 Zr H1B 134.3(10) . . ? B1 Zr H1B 30.3(10) . . ? C5 Zr H1B 69.3(10) . . ? C8 Zr H1B 122.6(10) . . ? C4 Zr H1B 92.5(10) . . ? C6 Zr H1B 83.5(10) . . ? C7 Zr H1B 115.6(10) . . ? H1A Zr H1B 53.5(13) . . ? B2 Zr H1C 88.8(8) . . ? B3 Zr H1C 87.2(8) . . ? B1 Zr H1C 26.7(8) . . ? C5 Zr H1C 116.2(8) . . ? C8 Zr H1C 168.8(8) . . ? C4 Zr H1C 141.5(8) . . ? C6 Zr H1C 115.2(8) . . ? C7 Zr H1C 139.0(8) . . ? H1A Zr H1C 44.8(12) . . ? H1B Zr H1C 49.3(13) . . ? B2 Zr H2A 28.9(11) . . ? B3 Zr H2A 132.9(11) . . ? B1 Zr H2A 88.9(10) . . ? C5 Zr H2A 83.5(11) . . ? C8 Zr H2A 97.7(11) . . ? C4 Zr H2A 72.1(11) . . ? C6 Zr H2A 115.9(11) . . ? C7 Zr H2A 126.1(11) . . ? H1A Zr H2A 117.5(14) . . ? H1B Zr H2A 65.8(14) . . ? H1C Zr H2A 85.7(14) . . ? B2 Zr H2B 28.8(11) . . ? B3 Zr H2B 92.0(11) . . ? B1 Zr H2B 132.5(11) . . ? C5 Zr H2B 105.4(10) . . ? C8 Zr H2B 75.5(11) . . ? C4 Zr H2B 75.0(10) . . ? C6 Zr H2B 126.6(11) . . ? C7 Zr H2B 106.4(11) . . ? H1A Zr H2B 159.0(14) . . ? H1B Zr H2B 115.9(15) . . ? H1C Zr H2B 114.3(13) . . ? H2A Zr H2B 50.3(14) . . ? B2 Zr H2C 30.4(10) . . ? B3 Zr H2C 86.5(10) . . ? B1 Zr H2C 85.1(10) . . ? C5 Zr H2C 132.5(10) . . ? C8 Zr H2C 126.6(10) . . ? C4 Zr H2C 116.4(10) . . ? C6 Zr H2C 164.3(10) . . ? C7 Zr H2C 156.3(10) . . ? H1A Zr H2C 108.0(14) . . ? H1B Zr H2C 84.8(13) . . ? H1C Zr H2C 63.3(13) . . ? H2A Zr H2C 49.2(14) . . ? H2B Zr H2C 51.1(15) . . ? B2 Zr H3A 91.0(10) . . ? B3 Zr H3A 29.5(10) . . ? B1 Zr H3A 133.6(10) . . ? C5 Zr H3A 126.9(10) . . ? C8 Zr H3A 74.5(10) . . ? C4 Zr H3A 105.0(10) . . ? C6 Zr H3A 107.2(10) . . ? C7 Zr H3A 76.5(10) . . ? H1A Zr H3A 115.5(15) . . ? H1B Zr H3A 162.5(14) . . ? H1C Zr H3A 113.3(13) . . ? H2A Zr H3A 118.6(14) . . ? H2B Zr H3A 69.3(13) . . ? H2C Zr H3A 86.8(13) . . ? B2 Zr H3B 136.7(9) . . ? B3 Zr H3B 32.9(9) . . ? B1 Zr H3B 86.8(9) . . ? C5 Zr H3B 114.1(9) . . ? C8 Zr H3B 96.5(10) . . ? C4 Zr H3B 125.0(10) . . ? C6 Zr H3B 81.7(9) . . ? C7 Zr H3B 70.9(10) . . ? H1A Zr H3B 61.6(13) . . ? H1B Zr H3B 115.0(13) . . ? H1C Zr H3B 82.6(12) . . ? H2A Zr H3B 161.9(15) . . ? H2B Zr H3B 123.6(14) . . ? H2C Zr H3B 112.9(14) . . ? H3A Zr H3B 55.0(14) . . ? B2 Zr H3C 88.8(9) . . ? B3 Zr H3C 26.0(10) . . ? B1 Zr H3C 88.5(10) . . ? C5 Zr H3C 163.1(9) . . ? C8 Zr H3C 121.6(10) . . ? C4 Zr H3C 151.9(10) . . ? C6 Zr H3C 130.7(9) . . ? C7 Zr H3C 112.8(10) . . ? H1A Zr H3C 82.7(13) . . ? H1B Zr H3C 115.1(15) . . ? H1C Zr H3C 65.9(13) . . ? H2A Zr H3C 113.3(15) . . ? H2B Zr H3C 87.6(13) . . ? H2C Zr H3C 64.2(14) . . ? H3A Zr H3C 47.4(15) . . ? H3B Zr H3C 49.0(12) . . ? C1 B1 Zr 168.2(2) . . ? C1 B1 H1A 117.0(18) . . ? Zr B1 H1A 58.8(18) . . ? C1 B1 H1B 113.5(17) . . ? Zr B1 H1B 59.6(17) . . ? H1A B1 H1B 102(2) . . ? C1 B1 H1C 118.3(18) . . ? Zr B1 H1C 73.6(18) . . ? H1A B1 H1C 97(2) . . ? H1B B1 H1C 107(3) . . ? C2 B2 Zr 174.2(3) . . ? C2 B2 H2A 117(2) . . ? Zr B2 H2A 59(2) . . ? C2 B2 H2B 116.2(19) . . ? Zr B2 H2B 62.4(19) . . ? H2A B2 H2B 100(3) . . ? C2 B2 H2C 114.1(18) . . ? Zr B2 H2C 71.4(18) . . ? H2A B2 H2C 100(3) . . ? H2B B2 H2C 107(3) . . ? C3 B3 Zr 172.3(3) . . ? C3 B3 H3A 108.9(18) . . ? Zr B3 H3A 66.2(18) . . ? C3 B3 H3B 119(2) . . ? Zr B3 H3B 59(2) . . ? H3A B3 H3B 105(2) . . ? C3 B3 H3C 114(2) . . ? Zr B3 H3C 73(2) . . ? H3A B3 H3C 108(3) . . ? H3B B3 H3C 101(2) . . ? B1 C1 H1D 109.5 . . ? B1 C1 H1E 109.5 . . ? H1D C1 H1E 109.5 . . ? B1 C1 H1F 109.5 . . ? H1D C1 H1F 109.5 . . ? H1E C1 H1F 109.5 . . ? B2 C2 H2D 109.5 . . ? B2 C2 H2E 109.5 . . ? H2D C2 H2E 109.5 . . ? B2 C2 H2F 109.5 . . ? H2D C2 H2F 109.5 . . ? H2E C2 H2F 109.5 . . ? B3 C3 H3D 109.5 . . ? B3 C3 H3E 109.5 . . ? H3D C3 H3E 109.5 . . ? B3 C3 H3F 109.5 . . ? H3D C3 H3F 109.5 . . ? H3E C3 H3F 109.5 . . ? C5 C4 C8 107.2(3) . . ? C5 C4 C9 127.3(4) . . ? C8 C4 C9 125.3(4) . . ? C5 C4 Zr 73.61(15) . . ? C8 C4 Zr 73.39(15) . . ? C9 C4 Zr 122.8(2) . . ? C4 C5 C6 108.7(3) . . ? C4 C5 C10 125.6(3) . . ? C6 C5 C10 125.4(3) . . ? C4 C5 Zr 73.98(15) . . ? C6 C5 Zr 74.12(15) . . ? C10 C5 Zr 123.1(2) . . ? C7 C6 C5 108.3(3) . . ? C7 C6 C11 126.9(3) . . ? C5 C6 C11 124.7(3) . . ? C7 C6 Zr 73.92(14) . . ? C5 C6 Zr 73.46(15) . . ? C11 C6 Zr 122.13(19) . . ? C6 C7 C8 108.2(3) . . ? C6 C7 C12 125.7(3) . . ? C8 C7 C12 125.6(3) . . ? C6 C7 Zr 73.87(14) . . ? C8 C7 Zr 73.44(16) . . ? C12 C7 Zr 125.1(2) . . ? C7 C8 C4 107.6(2) . . ? C7 C8 C13 126.6(4) . . ? C4 C8 C13 125.6(4) . . ? C7 C8 Zr 73.98(15) . . ? C4 C8 Zr 73.57(16) . . ? C13 C8 Zr 122.8(2) . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C6 C11 H11A 109.5 . . ? C6 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C6 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C7 C12 H12A 109.5 . . ? C7 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C7 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C8 C13 H13A 109.5 . . ? C8 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C8 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.308 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.052 data_ic9221 _database_code_depnum_ccdc_archive 'CCDC 672316' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H39 B3 Zr' _chemical_formula_weight 499.24 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' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.88680(10) _cell_length_b 14.7203(2) _cell_length_c 20.4718(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.1669(5) _cell_angle_gamma 90.00 _cell_volume 2677.49(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used all _cell_measurement_theta_min 1.70 _cell_measurement_theta_max 27.50 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.940 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'NONIUS KappaCCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20179 _diffrn_reflns_av_R_equivalents 0.0712 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.70 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6152 _reflns_number_gt 4159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'NONIUS COLLECT' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _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^)+(0.0576P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0086(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6152 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1152 _refine_ls_wR_factor_gt 0.0861 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.077 _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 0.88736(3) 0.296664(17) 0.299495(13) 0.02198(12) Uani 1 1 d . . . B1 B 1.0909(4) 0.4015(2) 0.32156(18) 0.0292(8) Uani 1 1 d . . . H1A H 0.988(3) 0.4282(19) 0.2928(14) 0.029(8) Uiso 1 1 d . . . H1B H 1.043(3) 0.3583(19) 0.3589(14) 0.028(8) Uiso 1 1 d . . . H1C H 1.146(3) 0.356(2) 0.2880(15) 0.040(9) Uiso 1 1 d . . . B2 B 0.9962(4) 0.1540(2) 0.32706(18) 0.0268(7) Uani 1 1 d . . . H2A H 0.875(3) 0.1407(19) 0.3037(12) 0.021(7) Uiso 1 1 d . . . H2B H 1.063(4) 0.190(2) 0.2909(16) 0.037(9) Uiso 1 1 d . . . H2C H 0.982(4) 0.208(2) 0.3660(16) 0.041(9) Uiso 1 1 d . . . B3 B 0.8611(4) 0.2942(2) 0.18312(16) 0.0277(7) Uani 1 1 d . . . H3A H 0.838(3) 0.3667(18) 0.2095(13) 0.022(7) Uiso 1 1 d . . . H3B H 0.978(4) 0.282(2) 0.1975(15) 0.043(9) Uiso 1 1 d . . . H3C H 0.797(3) 0.246(2) 0.2145(14) 0.025(7) Uiso 1 1 d . . . C1 C 1.1897(3) 0.4813(2) 0.35005(14) 0.0296(7) Uani 1 1 d . . . C2 C 1.1485(4) 0.5719(2) 0.34212(17) 0.0424(8) Uani 1 1 d . . . H2D H 1.0575 0.5856 0.3190 0.051 Uiso 1 1 calc R . . C3 C 1.2348(5) 0.6427(3) 0.36648(18) 0.0527(10) Uani 1 1 d . . . H3D H 1.2037 0.7038 0.3594 0.063 Uiso 1 1 calc R . . C4 C 1.3647(4) 0.6249(3) 0.40065(17) 0.0484(10) Uani 1 1 d . . . H4A H 1.4246 0.6734 0.4173 0.058 Uiso 1 1 calc R . . C5 C 1.4088(4) 0.5366(3) 0.41095(17) 0.0470(9) Uani 1 1 d . . . H5A H 1.4984 0.5241 0.4354 0.056 Uiso 1 1 calc R . . C6 C 1.3219(4) 0.4650(2) 0.38552(16) 0.0384(8) Uani 1 1 d . . . H6A H 1.3540 0.4042 0.3926 0.046 Uiso 1 1 calc R . . C7 C 1.0662(3) 0.06232(19) 0.35182(14) 0.0248(6) Uani 1 1 d . . . C8 C 1.2034(3) 0.0329(2) 0.32836(15) 0.0298(7) Uani 1 1 d . . . H8A H 1.2501 0.0672 0.2951 0.036 Uiso 1 1 calc R . . C9 C 1.2748(4) -0.0448(2) 0.35190(15) 0.0342(8) Uani 1 1 d . . . H9A H 1.3691 -0.0629 0.3352 0.041 Uiso 1 1 calc R . . C10 C 1.2074(4) -0.0951(2) 0.39961(15) 0.0384(8) Uani 1 1 d . . . H10A H 1.2560 -0.1478 0.4165 0.046 Uiso 1 1 calc R . . C11 C 1.0688(4) -0.0693(2) 0.42317(15) 0.0361(8) Uani 1 1 d . . . H11A H 1.0213 -0.1049 0.4555 0.043 Uiso 1 1 calc R . . C12 C 0.9997(4) 0.0088(2) 0.39949(15) 0.0319(7) Uani 1 1 d . . . H12A H 0.9049 0.0262 0.4161 0.038 Uiso 1 1 calc R . . C13 C 0.8186(3) 0.29372(19) 0.10765(14) 0.0281(7) Uani 1 1 d . . . C14 C 0.7458(4) 0.2200(2) 0.07858(16) 0.0397(8) Uani 1 1 d . . . H14A H 0.7165 0.1704 0.1051 0.048 Uiso 1 1 calc R . . C15 C 0.7149(4) 0.2168(2) 0.01197(17) 0.0452(9) Uani 1 1 d . . . H15A H 0.6668 0.1650 -0.0066 0.054 Uiso 1 1 calc R . . C16 C 0.7538(4) 0.2885(2) -0.02715(16) 0.0439(9) Uani 1 1 d . . . H16A H 0.7333 0.2864 -0.0728 0.053 Uiso 1 1 calc R . . C17 C 0.8226(4) 0.3634(2) 0.00029(16) 0.0425(9) Uani 1 1 d . . . H17A H 0.8480 0.4135 -0.0265 0.051 Uiso 1 1 calc R . . C18 C 0.8549(4) 0.3661(2) 0.06639(15) 0.0361(8) Uani 1 1 d . . . H18A H 0.9029 0.4183 0.0844 0.043 Uiso 1 1 calc R . . C19 C 0.7222(3) 0.28955(19) 0.39699(14) 0.0268(7) Uani 1 1 d . . . C20 C 0.7510(3) 0.38312(19) 0.38620(14) 0.0259(6) Uani 1 1 d . . . C21 C 0.6846(3) 0.4078(2) 0.32457(14) 0.0279(7) Uani 1 1 d . . . C22 C 0.6115(3) 0.3295(2) 0.29867(14) 0.0287(7) Uani 1 1 d . . . C23 C 0.6361(3) 0.2562(2) 0.34260(14) 0.0280(7) Uani 1 1 d . . . C24 C 0.7569(4) 0.2361(2) 0.45832(15) 0.0381(8) Uani 1 1 d . . . H24A H 0.6752 0.2441 0.4892 0.057 Uiso 1 1 calc R . . H24B H 0.8515 0.2580 0.4782 0.057 Uiso 1 1 calc R . . H24C H 0.7667 0.1716 0.4474 0.057 Uiso 1 1 calc R . . C25 C 0.8270(4) 0.4467(2) 0.43404(15) 0.0359(8) Uani 1 1 d . . . H25A H 0.7519 0.4725 0.4631 0.054 Uiso 1 1 calc R . . H25B H 0.8764 0.4957 0.4102 0.054 Uiso 1 1 calc R . . H25C H 0.9024 0.4132 0.4600 0.054 Uiso 1 1 calc R . . C26 C 0.6812(4) 0.5004(2) 0.29408(16) 0.0372(8) Uani 1 1 d . . . H26A H 0.5938 0.5341 0.3097 0.056 Uiso 1 1 calc R . . H26B H 0.6740 0.4945 0.2464 0.056 Uiso 1 1 calc R . . H26C H 0.7736 0.5333 0.3062 0.056 Uiso 1 1 calc R . . C27 C 0.5112(4) 0.3278(2) 0.23855(16) 0.0404(8) Uani 1 1 d . . . H27A H 0.4081 0.3432 0.2505 0.061 Uiso 1 1 calc R . . H27B H 0.5128 0.2670 0.2192 0.061 Uiso 1 1 calc R . . H27C H 0.5475 0.3722 0.2068 0.061 Uiso 1 1 calc R . . C28 C 0.5663(4) 0.1626(2) 0.33732(17) 0.0418(8) Uani 1 1 d . . . H28A H 0.4673 0.1631 0.3576 0.063 Uiso 1 1 calc R . . H28B H 0.6314 0.1184 0.3598 0.063 Uiso 1 1 calc R . . H28C H 0.5549 0.1458 0.2912 0.063 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.02582(18) 0.01945(16) 0.02060(17) 0.00051(12) -0.00088(11) 0.00179(12) B1 0.0299(19) 0.0279(19) 0.030(2) 0.0010(16) 0.0022(16) 0.0010(15) B2 0.0291(19) 0.0225(18) 0.0285(19) -0.0020(15) -0.0043(15) 0.0034(15) B3 0.033(2) 0.0280(18) 0.0223(17) 0.0011(15) -0.0010(15) -0.0008(16) C1 0.0330(18) 0.0287(17) 0.0272(16) -0.0021(13) 0.0048(13) -0.0018(13) C2 0.049(2) 0.0296(18) 0.048(2) -0.0022(16) -0.0095(17) -0.0050(16) C3 0.069(3) 0.036(2) 0.053(2) -0.0059(18) -0.003(2) -0.0109(19) C4 0.053(2) 0.048(2) 0.045(2) -0.0168(18) 0.0122(18) -0.0214(18) C5 0.0295(19) 0.070(3) 0.041(2) -0.0130(19) -0.0003(16) -0.0101(18) C6 0.0339(19) 0.0430(19) 0.038(2) -0.0026(16) 0.0043(15) -0.0017(15) C7 0.0300(16) 0.0215(15) 0.0227(15) -0.0043(12) -0.0049(12) 0.0010(12) C8 0.0347(18) 0.0288(16) 0.0256(16) -0.0033(13) -0.0040(13) -0.0003(14) C9 0.0360(18) 0.0337(18) 0.0328(18) -0.0068(15) -0.0056(14) 0.0102(14) C10 0.056(2) 0.0286(17) 0.0301(18) -0.0013(14) -0.0126(16) 0.0120(15) C11 0.057(2) 0.0265(17) 0.0252(17) 0.0033(13) -0.0017(15) 0.0006(15) C12 0.0403(19) 0.0269(17) 0.0284(17) -0.0005(13) 0.0019(14) 0.0036(14) C13 0.0280(16) 0.0310(16) 0.0253(16) 0.0010(13) 0.0008(12) 0.0057(13) C14 0.051(2) 0.0366(19) 0.0311(18) 0.0033(14) -0.0051(16) -0.0006(16) C15 0.052(2) 0.049(2) 0.0342(19) -0.0072(17) -0.0113(17) -0.0072(17) C16 0.045(2) 0.061(2) 0.0252(17) 0.0029(17) -0.0073(15) 0.0047(18) C17 0.050(2) 0.049(2) 0.0284(18) 0.0123(16) -0.0003(16) -0.0020(17) C18 0.0379(19) 0.0397(19) 0.0306(18) 0.0030(15) -0.0024(14) -0.0016(15) C19 0.0304(16) 0.0280(16) 0.0221(15) 0.0013(13) 0.0038(12) 0.0032(13) C20 0.0299(16) 0.0246(15) 0.0232(15) -0.0004(12) 0.0041(12) 0.0058(12) C21 0.0288(16) 0.0276(16) 0.0275(16) 0.0029(13) 0.0031(13) 0.0090(13) C22 0.0230(15) 0.0373(17) 0.0259(16) 0.0037(14) 0.0020(12) 0.0049(13) C23 0.0263(16) 0.0323(17) 0.0255(16) 0.0015(14) 0.0055(12) -0.0003(13) C24 0.052(2) 0.0368(18) 0.0255(17) 0.0088(14) 0.0013(15) 0.0080(16) C25 0.044(2) 0.0329(18) 0.0307(18) -0.0073(14) 0.0026(15) 0.0059(15) C26 0.047(2) 0.0279(17) 0.0365(19) 0.0058(14) 0.0046(16) 0.0114(15) C27 0.0288(18) 0.055(2) 0.0370(19) 0.0025(16) -0.0045(15) 0.0047(16) C28 0.042(2) 0.0392(19) 0.045(2) -0.0003(16) 0.0050(16) -0.0124(16) _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 B2 2.375(3) . ? Zr B3 2.389(3) . ? Zr B1 2.413(4) . ? Zr C23 2.490(3) . ? Zr C21 2.495(3) . ? Zr C22 2.498(3) . ? Zr C19 2.503(3) . ? Zr C20 2.515(3) . ? Zr H1A 2.14(3) . ? Zr H1B 2.04(3) . ? Zr H2A 2.30(3) . ? Zr H2B 2.22(3) . ? Zr H2C 2.05(3) . ? Zr H3A 2.15(3) . ? Zr H3B 2.26(3) . ? Zr H3C 2.04(3) . ? B1 C1 1.572(4) . ? B1 H1A 1.15(3) . ? B1 H1B 1.09(3) . ? B1 H1C 1.08(3) . ? B2 C7 1.567(4) . ? B2 H2A 1.18(2) . ? B2 H2B 1.09(3) . ? B2 H2C 1.14(3) . ? B3 C13 1.583(4) . ? B3 H3A 1.22(3) . ? B3 H3B 1.09(3) . ? B3 H3C 1.12(3) . ? C1 C6 1.390(4) . ? C1 C2 1.392(4) . ? C2 C3 1.381(5) . ? C2 H2D 0.9500 . ? C3 C4 1.363(5) . ? C3 H3D 0.9500 . ? C4 C5 1.372(5) . ? C4 H4A 0.9500 . ? C5 C6 1.401(4) . ? C5 H5A 0.9500 . ? C6 H6A 0.9500 . ? C7 C8 1.388(4) . ? C7 C12 1.395(4) . ? C8 C9 1.390(4) . ? C8 H8A 0.9500 . ? C9 C10 1.373(5) . ? C9 H9A 0.9500 . ? C10 C11 1.385(5) . ? C10 H10A 0.9500 . ? C11 C12 1.385(4) . ? C11 H11A 0.9500 . ? C12 H12A 0.9500 . ? C13 C14 1.391(4) . ? C13 C18 1.402(4) . ? C14 C15 1.386(5) . ? C14 H14A 0.9500 . ? C15 C16 1.373(5) . ? C15 H15A 0.9500 . ? C16 C17 1.375(5) . ? C16 H16A 0.9500 . ? C17 C18 1.378(4) . ? C17 H17A 0.9500 . ? C18 H18A 0.9500 . ? C19 C20 1.419(4) . ? C19 C23 1.425(4) . ? C19 C24 1.508(4) . ? C20 C21 1.428(4) . ? C20 C25 1.505(4) . ? C21 C22 1.420(4) . ? C21 C26 1.500(4) . ? C22 C23 1.419(4) . ? C22 C27 1.505(4) . ? C23 C28 1.514(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 B2 Zr B3 104.75(12) . . ? B2 Zr B1 102.75(12) . . ? B3 Zr B1 104.72(13) . . ? B2 Zr C23 93.90(11) . . ? B3 Zr C23 106.24(11) . . ? B1 Zr C23 139.53(11) . . ? B2 Zr C21 145.40(11) . . ? B3 Zr C21 99.14(11) . . ? B1 Zr C21 94.82(11) . . ? C23 Zr C21 55.06(10) . . ? B2 Zr C22 124.58(11) . . ? B3 Zr C22 85.43(11) . . ? B1 Zr C22 127.52(11) . . ? C23 Zr C22 33.05(10) . . ? C21 Zr C22 33.04(10) . . ? B2 Zr C19 90.92(11) . . ? B3 Zr C19 138.36(11) . . ? B1 Zr C19 109.08(11) . . ? C23 Zr C19 33.17(9) . . ? C21 Zr C19 54.96(9) . . ? C22 Zr C19 54.72(9) . . ? B2 Zr C20 118.64(11) . . ? B3 Zr C20 132.26(11) . . ? B1 Zr C20 85.10(11) . . ? C23 Zr C20 54.71(10) . . ? C21 Zr C20 33.13(9) . . ? C22 Zr C20 54.54(9) . . ? C19 Zr C20 32.84(9) . . ? B2 Zr H1A 130.3(8) . . ? B3 Zr H1A 89.0(8) . . ? B1 Zr H1A 28.4(8) . . ? C23 Zr H1A 128.2(8) . . ? C21 Zr H1A 74.0(8) . . ? C22 Zr H1A 103.6(8) . . ? C19 Zr H1A 110.0(8) . . ? C20 Zr H1A 78.2(8) . . ? B2 Zr H1B 89.1(8) . . ? B3 Zr H1B 130.8(8) . . ? B1 Zr H1B 26.6(8) . . ? C23 Zr H1B 119.8(8) . . ? C21 Zr H1B 94.0(8) . . ? C22 Zr H1B 124.9(8) . . ? C19 Zr H1B 86.8(8) . . ? C20 Zr H1B 71.6(8) . . ? H1A Zr H1B 49.9(11) . . ? B2 Zr H2A 29.2(6) . . ? B3 Zr H2A 91.1(6) . . ? B1 Zr H2A 131.8(6) . . ? C23 Zr H2A 72.9(6) . . ? C21 Zr H2A 127.8(6) . . ? C22 Zr H2A 98.5(6) . . ? C19 Zr H2A 84.2(6) . . ? C20 Zr H2A 117.1(6) . . ? H1A Zr H2A 157.8(10) . . ? H1B Zr H2A 117.0(10) . . ? B2 Zr H2B 27.2(8) . . ? B3 Zr H2B 88.0(8) . . ? B1 Zr H2B 86.8(8) . . ? C23 Zr H2B 119.6(8) . . ? C21 Zr H2B 172.1(9) . . ? C22 Zr H2B 145.6(8) . . ? C19 Zr H2B 117.2(9) . . ? C20 Zr H2B 139.7(8) . . ? H1A Zr H2B 109.9(11) . . ? H1B Zr H2B 83.9(11) . . ? H2A Zr H2B 47.9(10) . . ? B2 Zr H2C 28.5(9) . . ? B3 Zr H2C 133.0(9) . . ? B1 Zr H2C 89.3(9) . . ? C23 Zr H2C 88.3(9) . . ? C21 Zr H2C 124.5(9) . . ? C22 Zr H2C 121.0(9) . . ? C19 Zr H2C 71.5(9) . . ? C20 Zr H2C 92.8(9) . . ? H1A Zr H2C 116.9(11) . . ? H1B Zr H2C 67.9(12) . . ? H2A Zr H2C 50.1(10) . . ? H2B Zr H2C 47.6(12) . . ? B2 Zr H3A 134.7(7) . . ? B3 Zr H3A 30.5(7) . . ? B1 Zr H3A 89.7(7) . . ? C23 Zr H3A 104.4(7) . . ? C21 Zr H3A 74.0(7) . . ? C22 Zr H3A 73.5(7) . . ? C19 Zr H3A 126.2(7) . . ? C20 Zr H3A 105.6(7) . . ? H1A Zr H3A 65.8(10) . . ? H1B Zr H3A 115.1(11) . . ? H2A Zr H3A 120.1(9) . . ? H2B Zr H3A 113.8(11) . . ? H2C Zr H3A 161.4(12) . . ? B2 Zr H3B 89.0(8) . . ? B3 Zr H3B 27.0(8) . . ? B1 Zr H3B 87.3(8) . . ? C23 Zr H3B 130.1(8) . . ? C21 Zr H3B 121.7(8) . . ? C22 Zr H3B 112.4(8) . . ? C19 Zr H3B 163.2(8) . . ? C20 Zr H3B 152.3(8) . . ? H1A Zr H3B 82.5(11) . . ? H1B Zr H3B 110.0(12) . . ? H2A Zr H3B 87.5(9) . . ? H2B Zr H3B 66.1(11) . . ? H2C Zr H3B 113.7(12) . . ? H3A Zr H3B 47.7(10) . . ? B2 Zr H3C 91.7(8) . . ? B3 Zr H3C 28.0(8) . . ? B1 Zr H3C 132.4(9) . . ? C23 Zr H3C 82.8(8) . . ? C21 Zr H3C 98.2(8) . . ? C22 Zr H3C 72.3(8) . . ? C19 Zr H3C 115.9(8) . . ? C20 Zr H3C 126.8(8) . . ? H1A Zr H3C 115.8(11) . . ? H1B Zr H3C 157.3(12) . . ? H2A Zr H3C 69.4(10) . . ? H2B Zr H3C 86.4(11) . . ? H2C Zr H3C 118.7(12) . . ? H3A Zr H3C 51.4(11) . . ? H3B Zr H3C 47.3(11) . . ? C1 B1 Zr 163.4(2) . . ? C1 B1 H1A 111.6(14) . . ? Zr B1 H1A 62.4(14) . . ? C1 B1 H1B 113.6(15) . . ? Zr B1 H1B 57.0(14) . . ? H1A B1 H1B 104(2) . . ? C1 B1 H1C 116.1(16) . . ? Zr B1 H1C 80.4(16) . . ? H1A B1 H1C 105(2) . . ? H1B B1 H1C 106(2) . . ? C7 B2 Zr 174.9(2) . . ? C7 B2 H2A 109.8(14) . . ? Zr B2 H2A 71.9(13) . . ? C7 B2 H2B 114.7(16) . . ? Zr B2 H2B 68.6(15) . . ? H2A B2 H2B 108(2) . . ? C7 B2 H2C 115.3(16) . . ? Zr B2 H2C 59.7(15) . . ? H2A B2 H2C 107(2) . . ? H2B B2 H2C 102(2) . . ? C13 B3 Zr 171.8(2) . . ? C13 B3 H3A 113.5(12) . . ? Zr B3 H3A 63.7(12) . . ? C13 B3 H3B 118.0(17) . . ? Zr B3 H3B 70.1(17) . . ? H3A B3 H3B 101(2) . . ? C13 B3 H3C 116.2(14) . . ? Zr B3 H3C 58.6(14) . . ? H3A B3 H3C 102.1(19) . . ? H3B B3 H3C 104(2) . . ? C6 C1 C2 116.4(3) . . ? C6 C1 B1 121.6(3) . . ? C2 C1 B1 122.0(3) . . ? C3 C2 C1 122.6(3) . . ? C3 C2 H2D 118.7 . . ? C1 C2 H2D 118.7 . . ? C4 C3 C2 119.9(4) . . ? C4 C3 H3D 120.1 . . ? C2 C3 H3D 120.1 . . ? C3 C4 C5 119.8(3) . . ? C3 C4 H4A 120.1 . . ? C5 C4 H4A 120.1 . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C1 C6 C5 121.2(3) . . ? C1 C6 H6A 119.4 . . ? C5 C6 H6A 119.4 . . ? C8 C7 C12 117.0(3) . . ? C8 C7 B2 120.2(3) . . ? C12 C7 B2 122.8(3) . . ? C7 C8 C9 122.3(3) . . ? C7 C8 H8A 118.8 . . ? C9 C8 H8A 118.8 . . ? C10 C9 C8 119.2(3) . . ? C10 C9 H9A 120.4 . . ? C8 C9 H9A 120.4 . . ? C9 C10 C11 120.2(3) . . ? C9 C10 H10A 119.9 . . ? C11 C10 H10A 119.9 . . ? C10 C11 C12 119.8(3) . . ? C10 C11 H11A 120.1 . . ? C12 C11 H11A 120.1 . . ? C11 C12 C7 121.4(3) . . ? C11 C12 H12A 119.3 . . ? C7 C12 H12A 119.3 . . ? C14 C13 C18 116.5(3) . . ? C14 C13 B3 121.4(3) . . ? C18 C13 B3 122.1(3) . . ? C15 C14 C13 121.9(3) . . ? C15 C14 H14A 119.1 . . ? C13 C14 H14A 119.1 . . ? C16 C15 C14 120.0(3) . . ? C16 C15 H15A 120.0 . . ? C14 C15 H15A 120.0 . . ? C15 C16 C17 119.5(3) . . ? C15 C16 H16A 120.2 . . ? C17 C16 H16A 120.2 . . ? C16 C17 C18 120.5(3) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C17 C18 C13 121.5(3) . . ? C17 C18 H18A 119.2 . . ? C13 C18 H18A 119.2 . . ? C20 C19 C23 107.9(2) . . ? C20 C19 C24 127.0(3) . . ? C23 C19 C24 124.6(3) . . ? C20 C19 Zr 74.04(16) . . ? C23 C19 Zr 72.89(16) . . ? C24 C19 Zr 124.9(2) . . ? C19 C20 C21 108.2(3) . . ? C19 C20 C25 125.6(3) . . ? C21 C20 C25 126.1(3) . . ? C19 C20 Zr 73.12(16) . . ? C21 C20 Zr 72.64(16) . . ? C25 C20 Zr 123.9(2) . . ? C22 C21 C20 107.5(3) . . ? C22 C21 C26 125.2(3) . . ? C20 C21 C26 127.1(3) . . ? C22 C21 Zr 73.62(16) . . ? C20 C21 Zr 74.23(16) . . ? C26 C21 Zr 121.3(2) . . ? C23 C22 C21 108.5(3) . . ? C23 C22 C27 125.9(3) . . ? C21 C22 C27 125.3(3) . . ? C23 C22 Zr 73.14(16) . . ? C21 C22 Zr 73.33(16) . . ? C27 C22 Zr 124.5(2) . . ? C22 C23 C19 107.9(3) . . ? C22 C23 C28 126.1(3) . . ? C19 C23 C28 125.6(3) . . ? C22 C23 Zr 73.81(16) . . ? C19 C23 Zr 73.95(16) . . ? C28 C23 Zr 124.2(2) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C21 C26 H26A 109.5 . . ? C21 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C21 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C22 C27 H27A 109.5 . . ? C22 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C22 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.791 _refine_diff_density_min -0.663 _refine_diff_density_rms 0.138 data_ic9572 _database_code_depnum_ccdc_archive 'CCDC 672317' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H27 B3 Zr' _chemical_formula_weight 270.97 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' 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 7.0619(8) _cell_length_b 8.4186(9) _cell_length_c 13.4982(15) _cell_angle_alpha 84.077(2) _cell_angle_beta 88.589(2) _cell_angle_gamma 66.427(2) _cell_volume 731.47(14) _cell_formula_units_Z 2 _cell_measurement_temperature 150(1) _cell_measurement_reflns_used 3588 _cell_measurement_theta_min 2.65 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.230 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 284 _exptl_absorpt_coefficient_mu 0.717 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8699 _exptl_absorpt_correction_T_max 0.9318 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART ApexCCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9665 _diffrn_reflns_av_R_equivalents 0.0351 _diffrn_reflns_av_sigmaI/netI 0.0404 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.52 _diffrn_reflns_theta_max 27.50 _reflns_number_total 3345 _reflns_number_gt 3150 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0425P)^2^+0.2317P] 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 3345 _refine_ls_number_parameters 175 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0364 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0857 _refine_ls_goodness_of_fit_ref 1.155 _refine_ls_restrained_S_all 1.155 _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 0.08876(4) 0.81208(3) 0.251287(18) 0.01869(9) Uani 1 1 d . . . B1 B 0.3057(5) 0.6033(5) 0.1484(3) 0.0338(7) Uani 1 1 d . . . H1A H 0.221(5) 0.558(4) 0.213(2) 0.033(9) Uiso 1 1 d . . . H1B H 0.399(6) 0.660(5) 0.181(3) 0.046(10) Uiso 1 1 d . . . H1C H 0.170(6) 0.736(5) 0.114(3) 0.044(10) Uiso 1 1 d . . . H1D H 0.380(6) 0.508(5) 0.099(3) 0.045(10) Uiso 1 1 d . . . B2 B 0.1499(6) 1.0639(5) 0.1980(3) 0.0352(8) Uani 1 1 d . . . H2A H 0.078(5) 1.013(5) 0.144(3) 0.043(10) Uiso 1 1 d . . . H2B H 0.294(6) 0.971(5) 0.215(3) 0.045(10) Uiso 1 1 d . . . H2C H 0.061(6) 1.067(5) 0.268(3) 0.050(11) Uiso 1 1 d . . . H2D H 0.144(6) 1.194(5) 0.176(3) 0.053(11) Uiso 1 1 d . . . B3 B 0.2536(6) 0.7188(6) 0.4109(3) 0.0407(9) Uani 1 1 d . . . H3A H 0.362(5) 0.734(4) 0.365(2) 0.027(8) Uiso 1 1 d . . . H3B H 0.120(6) 0.834(5) 0.398(3) 0.039(9) Uiso 1 1 d . . . H3C H 0.196(5) 0.633(5) 0.381(3) 0.039(9) Uiso 1 1 d . . . H3D H 0.304(6) 0.677(5) 0.490(3) 0.064(12) Uiso 1 1 d . . . C1 C -0.2001(4) 0.7606(3) 0.17746(19) 0.0211(5) Uani 1 1 d . . . C2 C -0.2650(4) 0.9437(3) 0.17379(19) 0.0208(5) Uani 1 1 d . . . C3 C -0.2870(4) 0.9886(3) 0.2732(2) 0.0209(5) Uani 1 1 d . . . C4 C -0.2364(4) 0.8344(3) 0.33807(19) 0.0215(5) Uani 1 1 d . . . C5 C -0.1807(4) 0.6924(3) 0.2792(2) 0.0203(5) Uani 1 1 d . . . C6 C -0.1761(5) 0.6579(4) 0.0900(2) 0.0313(6) Uani 1 1 d . . . H6A H -0.3092 0.6550 0.0739 0.047 Uiso 1 1 calc R . . H6B H -0.0738 0.5387 0.1066 0.047 Uiso 1 1 calc R . . H6C H -0.1298 0.7130 0.0324 0.047 Uiso 1 1 calc R . . C7 C -0.3242(5) 1.0696(4) 0.0817(2) 0.0324(6) Uani 1 1 d . . . H7A H -0.4707 1.1032 0.0658 0.049 Uiso 1 1 calc R . . H7B H -0.2402 1.0145 0.0261 0.049 Uiso 1 1 calc R . . H7C H -0.3006 1.1734 0.0930 0.049 Uiso 1 1 calc R . . C8 C -0.3772(5) 1.1706(4) 0.3030(2) 0.0334(7) Uani 1 1 d . . . H8A H -0.5283 1.2150 0.3006 0.050 Uiso 1 1 calc R . . H8B H -0.3314 1.2456 0.2571 0.050 Uiso 1 1 calc R . . H8C H -0.3307 1.1702 0.3709 0.050 Uiso 1 1 calc R . . C9 C -0.2576(5) 0.8221(4) 0.4494(2) 0.0324(7) Uani 1 1 d . . . H9A H -0.3984 0.8349 0.4662 0.049 Uiso 1 1 calc R . . H9B H -0.2294 0.9148 0.4757 0.049 Uiso 1 1 calc R . . H9C H -0.1588 0.7085 0.4788 0.049 Uiso 1 1 calc R . . C10 C -0.1334(5) 0.5069(4) 0.3176(2) 0.0325(6) Uani 1 1 d . . . H10A H -0.2620 0.4887 0.3229 0.049 Uiso 1 1 calc R . . H10B H -0.0661 0.4812 0.3834 0.049 Uiso 1 1 calc R . . H10C H -0.0410 0.4294 0.2716 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr 0.01611(13) 0.01847(14) 0.02178(14) -0.00244(9) 0.00192(9) -0.00722(10) B1 0.0266(16) 0.0305(18) 0.043(2) -0.0102(15) 0.0078(14) -0.0086(14) B2 0.0332(18) 0.0283(18) 0.050(2) -0.0061(15) 0.0125(16) -0.0183(15) B3 0.0345(19) 0.063(3) 0.0291(18) 0.0025(17) -0.0071(15) -0.0258(19) C1 0.0170(12) 0.0230(13) 0.0244(13) -0.0060(10) 0.0009(10) -0.0082(10) C2 0.0164(11) 0.0210(12) 0.0240(13) 0.0001(10) 0.0000(10) -0.0069(10) C3 0.0169(12) 0.0190(12) 0.0263(13) -0.0047(10) 0.0026(10) -0.0062(10) C4 0.0177(12) 0.0237(13) 0.0229(13) -0.0031(10) 0.0025(10) -0.0080(10) C5 0.0158(11) 0.0176(12) 0.0266(13) -0.0008(10) 0.0011(10) -0.0062(9) C6 0.0330(15) 0.0335(16) 0.0302(15) -0.0139(12) 0.0019(12) -0.0137(13) C7 0.0330(15) 0.0322(16) 0.0277(15) 0.0058(12) -0.0035(12) -0.0105(13) C8 0.0322(15) 0.0217(14) 0.0443(18) -0.0128(12) 0.0050(13) -0.0065(12) C9 0.0317(15) 0.0435(18) 0.0223(14) -0.0048(12) 0.0073(11) -0.0153(14) C10 0.0341(16) 0.0186(13) 0.0435(17) 0.0022(12) 0.0040(13) -0.0107(12) _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 B2 2.366(3) . ? Zr B1 2.369(4) . ? Zr B3 2.378(4) . ? Zr C5 2.489(3) . ? Zr C3 2.497(2) . ? Zr C1 2.498(3) . ? Zr C2 2.498(2) . ? Zr C4 2.500(3) . ? Zr H1A 2.08(3) . ? Zr H1B 2.29(4) . ? Zr H1C 2.02(3) . ? Zr H2A 2.09(4) . ? Zr H2B 2.34(4) . ? Zr H2C 2.11(4) . ? Zr H3A 2.33(3) . ? Zr H3B 2.03(3) . ? Zr H3C 2.13(3) . ? B1 H1A 1.16(3) . ? B1 H1B 1.08(4) . ? B1 H1C 1.20(4) . ? B1 H1D 1.06(4) . ? B2 H2A 1.11(4) . ? B2 H2B 1.02(4) . ? B2 H2C 1.12(4) . ? B2 H2D 1.09(4) . ? B3 H3A 1.02(3) . ? B3 H3B 1.05(4) . ? B3 H3C 1.07(4) . ? B3 H3D 1.11(4) . ? C1 C2 1.417(4) . ? C1 C5 1.421(4) . ? C1 C6 1.501(4) . ? C2 C3 1.420(4) . ? C2 C7 1.497(4) . ? C3 C4 1.411(4) . ? C3 C8 1.500(4) . ? C4 C5 1.421(4) . ? C4 C9 1.503(4) . ? C5 C10 1.498(4) . ? 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 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? 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 B2 Zr B1 103.26(13) . . ? B2 Zr B3 103.66(15) . . ? B1 Zr B3 104.02(15) . . ? B2 Zr C5 144.91(11) . . ? B1 Zr C5 97.72(11) . . ? B3 Zr C5 98.04(12) . . ? B2 Zr C3 91.90(11) . . ? B1 Zr C3 139.20(11) . . ? B3 Zr C3 108.85(12) . . ? C5 Zr C3 54.73(8) . . ? B2 Zr C1 121.03(12) . . ? B1 Zr C1 85.49(11) . . ? B3 Zr C1 130.97(12) . . ? C5 Zr C1 33.11(8) . . ? C3 Zr C1 54.69(8) . . ? B2 Zr C2 91.76(12) . . ? B1 Zr C2 107.81(11) . . ? B3 Zr C2 140.19(12) . . ? C5 Zr C2 54.81(8) . . ? C3 Zr C2 33.03(8) . . ? C1 Zr C2 32.97(8) . . ? B2 Zr C4 121.10(11) . . ? B1 Zr C4 130.71(11) . . ? B3 Zr C4 86.43(11) . . ? C5 Zr C4 33.09(8) . . ? C3 Zr C4 32.80(8) . . ? C1 Zr C4 54.72(8) . . ? C2 Zr C4 54.62(8) . . ? B2 Zr H1A 132.2(9) . . ? B1 Zr H1A 29.3(9) . . ? B3 Zr H1A 90.4(9) . . ? C5 Zr H1A 74.0(9) . . ? C3 Zr H1A 126.7(9) . . ? C1 Zr H1A 74.9(9) . . ? C2 Zr H1A 106.1(9) . . ? C4 Zr H1A 104.9(9) . . ? B2 Zr H1B 86.0(10) . . ? B1 Zr H1B 26.7(10) . . ? B3 Zr H1B 88.7(9) . . ? C5 Zr H1B 122.0(10) . . ? C3 Zr H1B 162.2(9) . . ? C1 Zr H1B 111.9(10) . . ? C2 Zr H1B 129.3(9) . . ? C4 Zr H1B 152.8(10) . . ? H1A Zr H1B 48.3(13) . . ? B2 Zr H1C 87.5(10) . . ? B1 Zr H1C 30.5(10) . . ? B3 Zr H1C 133.7(11) . . ? C5 Zr H1C 97.2(10) . . ? C3 Zr H1C 115.6(10) . . ? C1 Zr H1C 71.4(10) . . ? C2 Zr H1C 82.6(10) . . ? C4 Zr H1C 126.0(10) . . ? H1A Zr H1C 52.9(13) . . ? H1B Zr H1C 46.7(13) . . ? B2 Zr H2A 28.1(10) . . ? B1 Zr H2A 90.1(10) . . ? B3 Zr H2A 131.4(10) . . ? C5 Zr H2A 126.2(10) . . ? C3 Zr H2A 85.9(10) . . ? C1 Zr H2A 95.8(10) . . ? C2 Zr H2A 72.1(10) . . ? C4 Zr H2A 118.7(10) . . ? H1A Zr H2A 118.0(13) . . ? H1B Zr H2A 84.0(13) . . ? H1C Zr H2A 65.8(14) . . ? B2 Zr H2B 25.0(9) . . ? B1 Zr H2B 88.1(9) . . ? B3 Zr H2B 88.5(9) . . ? C5 Zr H2B 169.9(9) . . ? C3 Zr H2B 115.8(9) . . ? C1 Zr H2B 140.3(9) . . ? C2 Zr H2B 115.5(9) . . ? C4 Zr H2B 140.9(9) . . ? H1A Zr H2B 113.9(13) . . ? H1B Zr H2B 65.5(13) . . ? H1C Zr H2B 83.6(13) . . ? H2A Zr H2B 45.1(13) . . ? B2 Zr H2C 28.1(10) . . ? B1 Zr H2C 130.8(11) . . ? B3 Zr H2C 89.1(10) . . ? C5 Zr H2C 127.6(10) . . ? C3 Zr H2C 73.8(10) . . ? C1 Zr H2C 120.8(10) . . ? C2 Zr H2C 87.9(10) . . ? C4 Zr H2C 96.8(11) . . ? H1A Zr H2C 158.2(15) . . ? H1B Zr H2C 109.9(14) . . ? H1C Zr H2C 114.5(15) . . ? H2A Zr H2C 49.8(14) . . ? H2B Zr H2C 44.3(13) . . ? B2 Zr H3A 87.6(8) . . ? B1 Zr H3A 89.7(8) . . ? B3 Zr H3A 24.9(8) . . ? C5 Zr H3A 120.7(8) . . ? C3 Zr H3A 129.2(8) . . ? C1 Zr H3A 151.4(8) . . ? C2 Zr H3A 162.2(8) . . ? C4 Zr H3A 111.1(8) . . ? H1A Zr H3A 87.3(12) . . ? H1B Zr H3A 68.4(12) . . ? H1C Zr H3A 115.2(13) . . ? H2A Zr H3A 112.4(13) . . ? H2B Zr H3A 67.4(12) . . ? H2C Zr H3A 83.1(12) . . ? B2 Zr H3B 93.4(10) . . ? B1 Zr H3B 130.0(10) . . ? B3 Zr H3B 26.0(10) . . ? C5 Zr H3B 94.3(10) . . ? C3 Zr H3B 85.7(10) . . ? C1 Zr H3B 125.0(10) . . ? C2 Zr H3B 118.6(10) . . ? C4 Zr H3B 71.1(10) . . ? H1A Zr H3B 114.2(13) . . ? H1B Zr H3B 112.1(14) . . ? H1C Zr H3B 158.7(15) . . ? H2A Zr H3B 120.1(14) . . ? H2B Zr H3B 88.2(13) . . ? H2C Zr H3B 70.9(14) . . ? H3A Zr H3B 43.7(13) . . ? B2 Zr H3C 130.2(10) . . ? B1 Zr H3C 91.6(9) . . ? B3 Zr H3C 26.8(10) . . ? C5 Zr H3C 76.1(10) . . ? C3 Zr H3C 107.1(9) . . ? C1 Zr H3C 107.1(10) . . ? C2 Zr H3C 128.6(10) . . ? C4 Zr H3C 76.4(9) . . ? H1A Zr H3C 69.6(13) . . ? H1B Zr H3C 87.4(13) . . ? H1C Zr H3C 121.3(14) . . ? H2A Zr H3C 157.1(15) . . ? H2B Zr H3C 112.1(13) . . ? H2C Zr H3C 114.8(14) . . ? H3A Zr H3C 44.7(12) . . ? H3B Zr H3C 45.1(13) . . ? Zr B1 H1A 61.2(16) . . ? Zr B1 H1B 72(2) . . ? H1A B1 H1B 107(3) . . ? Zr B1 H1C 58.3(17) . . ? H1A B1 H1C 101(2) . . ? H1B B1 H1C 98(3) . . ? Zr B1 H1D 171(2) . . ? H1A B1 H1D 114(3) . . ? H1B B1 H1D 117(3) . . ? H1C B1 H1D 117(3) . . ? Zr B2 H2A 62.0(18) . . ? Zr B2 H2B 76(2) . . ? H2A B2 H2B 107(3) . . ? Zr B2 H2C 63(2) . . ? H2A B2 H2C 105(3) . . ? H2B B2 H2C 105(3) . . ? Zr B2 H2D 168(2) . . ? H2A B2 H2D 115(3) . . ? H2B B2 H2D 115(3) . . ? H2C B2 H2D 109(3) . . ? Zr B3 H3A 74.7(18) . . ? Zr B3 H3B 58.0(19) . . ? H3A B3 H3B 106(3) . . ? Zr B3 H3C 63.6(18) . . ? H3A B3 H3C 109(3) . . ? H3B B3 H3C 97(3) . . ? Zr B3 H3D 170(2) . . ? H3A B3 H3D 115(3) . . ? H3B B3 H3D 116(3) . . ? H3C B3 H3D 112(3) . . ? C2 C1 C5 107.9(2) . . ? C2 C1 C6 126.3(2) . . ? C5 C1 C6 125.5(2) . . ? C2 C1 Zr 73.52(14) . . ? C5 C1 Zr 73.13(14) . . ? C6 C1 Zr 123.66(18) . . ? C1 C2 C3 107.9(2) . . ? C1 C2 C7 126.0(2) . . ? C3 C2 C7 125.8(2) . . ? C1 C2 Zr 73.51(14) . . ? C3 C2 Zr 73.46(14) . . ? C7 C2 Zr 124.26(18) . . ? C4 C3 C2 108.2(2) . . ? C4 C3 C8 125.9(2) . . ? C2 C3 C8 125.4(2) . . ? C4 C3 Zr 73.69(14) . . ? C2 C3 Zr 73.51(14) . . ? C8 C3 Zr 125.21(19) . . ? C3 C4 C5 108.1(2) . . ? C3 C4 C9 126.4(2) . . ? C5 C4 C9 125.2(2) . . ? C3 C4 Zr 73.51(14) . . ? C5 C4 Zr 73.07(14) . . ? C9 C4 Zr 123.91(18) . . ? C4 C5 C1 107.8(2) . . ? C4 C5 C10 125.8(2) . . ? C1 C5 C10 126.0(2) . . ? C4 C5 Zr 73.84(15) . . ? C1 C5 Zr 73.76(14) . . ? C10 C5 Zr 123.37(18) . . ? C1 C6 H6A 109.5 . . ? C1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C2 C7 H7A 109.5 . . ? C2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C4 C9 H9A 109.5 . . ? C4 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C4 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C5 C10 H10A 109.5 . . ? C5 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C5 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.205 _refine_diff_density_min -0.785 _refine_diff_density_rms 0.086 data_ic11985 _database_code_depnum_ccdc_archive 'CCDC 672318' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H60 B2 F15 O7 Zr2' _chemical_formula_weight 1262.04 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' O O 0.0106 0.0060 '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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 14.6566(5) _cell_length_b 18.0175(6) _cell_length_c 20.3699(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5379.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7421 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 21.78 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.558 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2564 _exptl_absorpt_coefficient_mu 0.488 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8438 _exptl_absorpt_correction_T_max 0.8877 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'BRUKER SMART APEXCCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54149 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0517 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12348 _reflns_number_gt 11109 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0407P)^2^+1.3942P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 12348 _refine_ls_number_parameters 704 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0481 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.0899 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.005 _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 Zr1 Zr 0.65152(2) 0.918394(17) 0.138437(15) 0.02052(7) Uani 1 1 d . . . Zr2 Zr 0.80663(2) 1.051320(17) 0.169138(15) 0.02124(7) Uani 1 1 d . . . O1 O 0.77207(14) 0.93821(12) 0.19318(10) 0.0195(5) Uani 1 1 d . . . O2 O 0.73058(16) 1.00212(13) 0.08933(11) 0.0251(5) Uani 1 1 d . . . O3 O 0.54411(16) 0.97767(13) 0.13289(12) 0.0301(5) Uani 1 1 d . . . O4 O 0.63792(14) 0.91832(13) 0.24572(10) 0.0263(5) Uani 1 1 d . B . O5 O 0.73558(16) 1.03187(13) 0.26269(11) 0.0259(5) Uani 1 1 d . . . O6 O 0.74482(17) 1.14292(13) 0.15398(12) 0.0336(6) Uani 1 1 d . . . O7 O 0.77694(15) 0.91847(13) 0.31394(10) 0.0267(5) Uani 1 1 d . . . B1 B 0.7334(3) 0.9482(2) 0.25831(18) 0.0237(7) Uani 1 1 d . . . C1 C 0.6910(3) 1.0407(2) 0.03375(17) 0.0378(9) Uani 1 1 d . . . H1A H 0.6540 1.0816 0.0494 0.045 Uiso 1 1 calc R . . H1B H 0.6517 1.0070 0.0097 0.045 Uiso 1 1 calc R . . C2 C 0.7636(3) 1.0697(3) -0.0112(2) 0.0634(15) Uani 1 1 d . . . H2A H 0.7951 1.1100 0.0097 0.095 Uiso 1 1 calc R . . H2B H 0.7361 1.0870 -0.0512 0.095 Uiso 1 1 calc R . . H2C H 0.8061 1.0308 -0.0210 0.095 Uiso 1 1 calc R . . C3 C 0.4578(3) 1.0099(3) 0.1227(2) 0.0561(13) Uani 1 1 d . . . H3A H 0.4111 0.9727 0.1306 0.067 Uiso 1 1 calc R . . H3B H 0.4529 1.0254 0.0772 0.067 Uiso 1 1 calc R . . C4 C 0.4405(3) 1.0745(2) 0.1656(3) 0.0563(12) Uani 1 1 d . . . H4A H 0.4396 1.0587 0.2106 0.084 Uiso 1 1 calc R . . H4B H 0.3828 1.0963 0.1545 0.084 Uiso 1 1 calc R . . H4C H 0.4880 1.1106 0.1596 0.084 Uiso 1 1 calc R . . C5 C 0.5627(3) 0.9337(2) 0.2885(2) 0.0449(11) Uani 1 1 d D . . H5A H 0.5066 0.9247 0.2645 0.054 Uiso 0.65 1 calc PR A 1 H5B H 0.5642 0.9861 0.2996 0.054 Uiso 0.65 1 calc PR A 1 H5'A H 0.5855 0.9360 0.3332 0.054 Uiso 0.35 1 d PR A 2 H5'B H 0.5389 0.9824 0.2777 0.054 Uiso 0.35 1 d PR A 2 C6 C 0.5591(4) 0.8914(4) 0.3494(3) 0.0452(16) Uani 0.65 1 d PD B 1 H6A H 0.5066 0.9062 0.3743 0.068 Uiso 0.65 1 calc PR B 1 H6B H 0.6133 0.9007 0.3746 0.068 Uiso 0.65 1 calc PR B 1 H6C H 0.5551 0.8394 0.3395 0.068 Uiso 0.65 1 calc PR B 1 C6' C 0.4892(7) 0.8818(6) 0.2865(6) 0.047(3) Uiso 0.35 1 d PD B 2 H6'A H 0.4423 0.8972 0.3165 0.070 Uiso 0.35 1 calc PR B 2 H6'B H 0.5111 0.8336 0.2988 0.070 Uiso 0.35 1 calc PR B 2 H6'C H 0.4647 0.8799 0.2429 0.070 Uiso 0.35 1 calc PR B 2 C7 C 0.7221(3) 1.0715(2) 0.32387(17) 0.0385(9) Uani 1 1 d . . . H7A H 0.7788 1.0723 0.3484 0.046 Uiso 1 1 calc R . . H7B H 0.6767 1.0460 0.3502 0.046 Uiso 1 1 calc R . . C8 C 0.6916(3) 1.1487(2) 0.3111(2) 0.0489(11) Uani 1 1 d . . . H8A H 0.7358 1.1735 0.2842 0.073 Uiso 1 1 calc R . . H8B H 0.6853 1.1746 0.3521 0.073 Uiso 1 1 calc R . . H8C H 0.6338 1.1478 0.2889 0.073 Uiso 1 1 calc R . . C9 C 0.7239(3) 1.2187(2) 0.1433(3) 0.0604(14) Uani 1 1 d . . . H9A H 0.7599 1.2365 0.1066 0.072 Uiso 1 1 calc R . . H9B H 0.7421 1.2468 0.1818 0.072 Uiso 1 1 calc R . . C10 C 0.6295(3) 1.2333(3) 0.1302(3) 0.0781(19) Uani 1 1 d . . . H10A H 0.6136 1.2137 0.0879 0.117 Uiso 1 1 calc R . . H10B H 0.6190 1.2859 0.1306 0.117 Uiso 1 1 calc R . . H10C H 0.5925 1.2101 0.1633 0.117 Uiso 1 1 calc R . . C11 C 0.7881(3) 0.8396(2) 0.31636(18) 0.0365(9) Uani 1 1 d . . . H11A H 0.7905 0.8201 0.2720 0.044 Uiso 1 1 calc R . . H11B H 0.7360 0.8176 0.3383 0.044 Uiso 1 1 calc R . . C12 C 0.8732(3) 0.8189(2) 0.3519(2) 0.0503(11) Uani 1 1 d . . . H12A H 0.9250 0.8386 0.3290 0.075 Uiso 1 1 calc R . . H12B H 0.8779 0.7659 0.3542 0.075 Uiso 1 1 calc R . . H12C H 0.8714 0.8390 0.3956 0.075 Uiso 1 1 calc R . . C13 C 0.6942(3) 0.83340(18) 0.04635(16) 0.0277(7) Uani 1 1 d . . . C14 C 0.5980(3) 0.8404(2) 0.04424(17) 0.0287(8) Uani 1 1 d . . . C15 C 0.5629(2) 0.80752(19) 0.10237(18) 0.0278(8) Uani 1 1 d . . . C16 C 0.6375(2) 0.77937(17) 0.13947(18) 0.0267(7) Uani 1 1 d . . . C17 C 0.7186(2) 0.79527(18) 0.10491(16) 0.0245(7) Uani 1 1 d . . . C18 C 0.7598(3) 0.8547(2) -0.00705(19) 0.0407(10) Uani 1 1 d . . . H18A H 0.7820 0.8107 -0.0283 0.061 Uiso 1 1 calc R . . H18B H 0.8102 0.8815 0.0116 0.061 Uiso 1 1 calc R . . H18C H 0.7292 0.8855 -0.0386 0.061 Uiso 1 1 calc R . . C19 C 0.5412(3) 0.8722(2) -0.0104(2) 0.0410(10) Uani 1 1 d . . . H19A H 0.5764 0.9083 -0.0341 0.061 Uiso 1 1 calc R . . H19B H 0.4880 0.8956 0.0077 0.061 Uiso 1 1 calc R . . H19C H 0.5230 0.8331 -0.0396 0.061 Uiso 1 1 calc R . . C20 C 0.4637(3) 0.8000(2) 0.1195(2) 0.0394(10) Uani 1 1 d . . . H20A H 0.4389 0.7572 0.0978 0.059 Uiso 1 1 calc R . . H20B H 0.4315 0.8435 0.1054 0.059 Uiso 1 1 calc R . . H20C H 0.4573 0.7944 0.1661 0.059 Uiso 1 1 calc R . . C21 C 0.6302(3) 0.7351(2) 0.20175(17) 0.0334(9) Uani 1 1 d . . . H21A H 0.6008 0.7644 0.2349 0.050 Uiso 1 1 calc R . . H21B H 0.6902 0.7215 0.2164 0.050 Uiso 1 1 calc R . . H21C H 0.5951 0.6911 0.1937 0.050 Uiso 1 1 calc R . . C22 C 0.8149(3) 0.7722(2) 0.12255(19) 0.0359(9) Uani 1 1 d . . . H22A H 0.8294 0.7263 0.1009 0.054 Uiso 1 1 calc R . . H22B H 0.8195 0.7655 0.1692 0.054 Uiso 1 1 calc R . . H22C H 0.8569 0.8099 0.1088 0.054 Uiso 1 1 calc R . . C23 C 0.9630(2) 1.0373(2) 0.12203(19) 0.0328(9) Uani 1 1 d . . . C24 C 0.9655(2) 0.9999(2) 0.1836(2) 0.0362(9) Uani 1 1 d . . . C25 C 0.9537(2) 1.0531(3) 0.23346(18) 0.0367(9) Uani 1 1 d . . . C26 C 0.9448(3) 1.1242(2) 0.20328(19) 0.0326(8) Uani 1 1 d . . . C27 C 0.9509(2) 1.1137(2) 0.13486(19) 0.0302(8) Uani 1 1 d . . . C28 C 0.9817(3) 1.0031(3) 0.0563(2) 0.0551(13) Uani 1 1 d . . . H28A H 0.9651 1.0375 0.0224 0.083 Uiso 1 1 calc R . . H28B H 0.9465 0.9585 0.0517 0.083 Uiso 1 1 calc R . . H28C H 1.0454 0.9915 0.0528 0.083 Uiso 1 1 calc R . . C29 C 0.9857(3) 0.9189(2) 0.1933(3) 0.0630(15) Uani 1 1 d . . . H29A H 1.0401 0.9136 0.2190 0.094 Uiso 1 1 calc R . . H29B H 0.9942 0.8956 0.1513 0.094 Uiso 1 1 calc R . . H29C H 0.9355 0.8959 0.2157 0.094 Uiso 1 1 calc R . . C30 C 0.9577(3) 1.0370(3) 0.3060(2) 0.0603(14) Uani 1 1 d . . . H30A H 0.9160 0.9976 0.3163 0.090 Uiso 1 1 calc R . . H30B H 0.9410 1.0808 0.3300 0.090 Uiso 1 1 calc R . . H30C H 1.0185 1.0224 0.3177 0.090 Uiso 1 1 calc R . . C31 C 0.9388(3) 1.1969(3) 0.2384(2) 0.0522(12) Uani 1 1 d . . . H31A H 0.9972 1.2089 0.2570 0.078 Uiso 1 1 calc R . . H31B H 0.8942 1.1936 0.2727 0.078 Uiso 1 1 calc R . . H31C H 0.9213 1.2350 0.2079 0.078 Uiso 1 1 calc R . . C32 C 0.9551(3) 1.1748(2) 0.0843(2) 0.0442(11) Uani 1 1 d . . . H32A H 0.9166 1.2151 0.0978 0.066 Uiso 1 1 calc R . . H32B H 0.9345 1.1562 0.0428 0.066 Uiso 1 1 calc R . . H32C H 1.0168 1.1921 0.0803 0.066 Uiso 1 1 calc R . . B2 B 0.2989(3) 0.9766(2) 0.8956(2) 0.0293(9) Uani 1 1 d . . . C33 C 0.2138(2) 0.92803(18) 0.92617(16) 0.0259(7) Uani 1 1 d . . . C34 C 0.2267(2) 0.8850(2) 0.98132(18) 0.0301(8) Uani 1 1 d . . . C35 C 0.1590(3) 0.8442(2) 1.01239(17) 0.0334(8) Uani 1 1 d . . . C36 C 0.0722(3) 0.8470(2) 0.98693(19) 0.0330(9) Uani 1 1 d . . . C37 C 0.0553(3) 0.8885(2) 0.9326(2) 0.0356(9) Uani 1 1 d . . . C38 C 0.1244(2) 0.9272(2) 0.90396(17) 0.0292(8) Uani 1 1 d . . . C39 C 0.3121(3) 1.0534(2) 0.93901(16) 0.0310(8) Uani 1 1 d . . . C40 C 0.2420(3) 1.0949(2) 0.96677(19) 0.0362(9) Uani 1 1 d . . . C41 C 0.2548(3) 1.1568(2) 1.0061(2) 0.0412(10) Uani 1 1 d . . . C42 C 0.3417(3) 1.1806(2) 1.01791(18) 0.0386(9) Uani 1 1 d . . . C43 C 0.4137(3) 1.1431(2) 0.9902(2) 0.0397(10) Uani 1 1 d . . . C44 C 0.3972(3) 1.0812(2) 0.95248(18) 0.0330(8) Uani 1 1 d . . . C45 C 0.2880(2) 0.99216(19) 0.81640(17) 0.0287(8) Uani 1 1 d . . . C46 C 0.2601(3) 1.0573(2) 0.78647(19) 0.0360(9) Uani 1 1 d . . . C47 C 0.2573(3) 1.0686(2) 0.7195(2) 0.0409(10) Uani 1 1 d . . . C48 C 0.2816(3) 1.0126(3) 0.67855(18) 0.0401(10) Uani 1 1 d . . . C49 C 0.3081(3) 0.9454(2) 0.70428(18) 0.0353(8) Uani 1 1 d . . . C50 C 0.3113(2) 0.93712(18) 0.77198(18) 0.0299(8) Uani 1 1 d . . . F1 F 0.31081(16) 0.88066(13) 1.00906(10) 0.0422(5) Uani 1 1 d . . . F2 F 0.17647(18) 0.80404(13) 1.06640(11) 0.0493(6) Uani 1 1 d . . . F3 F 0.00402(16) 0.81024(13) 1.01780(13) 0.0494(6) Uani 1 1 d . . . F4 F -0.03043(15) 0.89274(15) 0.90907(13) 0.0536(7) Uani 1 1 d . . . F5 F 0.10120(15) 0.96762(13) 0.85045(11) 0.0453(6) Uani 1 1 d . . . F6 F 0.15356(16) 1.07589(13) 0.95541(13) 0.0514(6) Uani 1 1 d . . . F7 F 0.1833(2) 1.19355(14) 1.03100(14) 0.0628(8) Uani 1 1 d . . . F8 F 0.3567(2) 1.24066(13) 1.05550(12) 0.0602(8) Uani 1 1 d . . . F9 F 0.49951(19) 1.16600(14) 1.00214(14) 0.0571(7) Uani 1 1 d . . . F10 F 0.47269(14) 1.04692(13) 0.92888(11) 0.0431(5) Uani 1 1 d . . . F11 F 0.23337(19) 1.11541(13) 0.82413(13) 0.0560(7) Uani 1 1 d . . . F12 F 0.2305(2) 1.13433(15) 0.69508(14) 0.0642(8) Uani 1 1 d . . . F13 F 0.27972(18) 1.02181(16) 0.61285(11) 0.0586(7) Uani 1 1 d . . . F14 F 0.33053(18) 0.88935(14) 0.66427(12) 0.0550(7) Uani 1 1 d . . . F15 F 0.33922(17) 0.87040(11) 0.79347(11) 0.0440(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 Zr1 0.02100(15) 0.01995(14) 0.02060(14) 0.00118(13) -0.00111(13) -0.00159(13) Zr2 0.02255(15) 0.02031(15) 0.02086(15) 0.00069(13) -0.00169(13) -0.00198(13) O1 0.0169(10) 0.0221(12) 0.0197(10) -0.0006(9) 0.0003(8) 0.0002(9) O2 0.0295(14) 0.0260(12) 0.0198(11) 0.0046(10) -0.0045(10) -0.0035(10) O3 0.0236(12) 0.0319(13) 0.0349(14) 0.0019(11) -0.0055(11) 0.0030(10) O4 0.0198(12) 0.0341(12) 0.0250(11) 0.0035(10) 0.0039(9) 0.0015(11) O5 0.0341(13) 0.0237(12) 0.0200(11) -0.0047(9) -0.0010(10) 0.0038(10) O6 0.0385(15) 0.0232(12) 0.0390(16) 0.0039(11) -0.0039(11) 0.0019(11) O7 0.0307(12) 0.0295(12) 0.0199(11) 0.0045(10) -0.0023(9) 0.0034(11) B1 0.0222(18) 0.0262(19) 0.0226(17) 0.0006(16) 0.0011(15) 0.0019(16) C1 0.049(2) 0.036(2) 0.0282(18) 0.0123(16) -0.0161(18) -0.010(2) C2 0.073(3) 0.079(4) 0.039(2) 0.032(3) -0.014(2) -0.024(3) C3 0.041(3) 0.060(3) 0.066(3) 0.003(3) -0.015(2) 0.016(2) C4 0.039(2) 0.042(2) 0.087(3) 0.005(3) 0.008(2) 0.013(2) C5 0.038(2) 0.051(3) 0.046(2) 0.009(2) 0.0221(19) 0.0115(19) C6 0.038(3) 0.065(4) 0.033(3) 0.008(3) 0.007(3) -0.002(3) C7 0.054(2) 0.036(2) 0.0257(18) -0.0090(16) -0.0020(17) 0.0122(18) C8 0.076(3) 0.034(2) 0.037(2) -0.0084(18) 0.010(2) 0.014(2) C9 0.047(3) 0.024(2) 0.110(4) 0.021(3) -0.003(3) 0.0001(18) C10 0.055(3) 0.034(2) 0.145(6) 0.008(3) -0.031(4) 0.010(2) C11 0.046(2) 0.034(2) 0.030(2) 0.0074(16) -0.0036(17) -0.0010(17) C12 0.049(3) 0.045(2) 0.057(3) 0.012(2) -0.004(2) 0.014(2) C13 0.036(2) 0.0243(17) 0.0225(17) -0.0040(13) 0.0003(16) -0.0043(16) C14 0.033(2) 0.0274(19) 0.0253(18) -0.0036(15) -0.0021(15) -0.0065(15) C15 0.0277(19) 0.0235(18) 0.0322(19) -0.0051(15) 0.0002(15) -0.0040(14) C16 0.0317(19) 0.0191(15) 0.0294(16) -0.0050(14) -0.0014(16) -0.0030(13) C17 0.0280(19) 0.0199(16) 0.0257(17) -0.0047(13) -0.0026(14) -0.0013(13) C18 0.053(3) 0.040(2) 0.030(2) -0.0038(18) 0.0101(19) -0.002(2) C19 0.047(3) 0.043(2) 0.033(2) 0.0027(19) -0.0096(19) -0.009(2) C20 0.030(2) 0.036(2) 0.052(3) -0.0006(18) -0.0002(18) -0.0122(17) C21 0.043(2) 0.0282(19) 0.0289(19) 0.0007(15) 0.0005(17) -0.0046(16) C22 0.035(2) 0.0321(19) 0.040(2) -0.0044(16) -0.0014(17) 0.0033(17) C23 0.0205(17) 0.040(2) 0.038(2) -0.0032(17) 0.0011(15) -0.0012(15) C24 0.0215(18) 0.031(2) 0.056(3) 0.0104(18) -0.0085(17) -0.0028(15) C25 0.0227(18) 0.055(2) 0.0326(19) 0.0077(19) -0.0071(15) -0.0144(18) C26 0.0281(19) 0.035(2) 0.035(2) -0.0042(17) -0.0013(16) -0.0122(16) C27 0.0255(18) 0.0317(19) 0.0334(19) 0.0033(17) 0.0001(16) -0.0086(15) C28 0.039(3) 0.067(3) 0.059(3) -0.030(3) 0.007(2) -0.003(2) C29 0.028(2) 0.039(2) 0.122(5) 0.020(3) -0.008(2) 0.005(2) C30 0.037(2) 0.098(4) 0.047(3) 0.028(3) -0.015(2) -0.022(3) C31 0.046(3) 0.055(3) 0.056(3) -0.026(2) 0.003(2) -0.015(2) C32 0.040(2) 0.045(2) 0.048(3) 0.012(2) 0.000(2) -0.012(2) B2 0.033(2) 0.026(2) 0.029(2) -0.0042(16) 0.0051(18) -0.0033(17) C33 0.0301(18) 0.0214(17) 0.0262(16) -0.0023(13) 0.0023(14) 0.0009(14) C34 0.0236(18) 0.038(2) 0.0290(18) -0.0085(16) -0.0042(15) 0.0041(16) C35 0.049(2) 0.0278(18) 0.0233(17) -0.0003(14) 0.0064(17) 0.0048(17) C36 0.036(2) 0.0268(19) 0.036(2) -0.0109(16) 0.0154(17) -0.0071(16) C37 0.027(2) 0.037(2) 0.043(2) -0.0091(18) 0.0007(17) 0.0000(16) C38 0.0300(19) 0.0261(19) 0.0316(18) 0.0004(15) -0.0030(15) 0.0024(14) C39 0.0338(19) 0.0324(18) 0.0267(17) 0.0039(15) -0.0005(15) -0.0034(18) C40 0.036(2) 0.034(2) 0.039(2) 0.0014(17) 0.0045(17) -0.0061(17) C41 0.058(3) 0.030(2) 0.036(2) -0.0021(17) 0.019(2) 0.0020(19) C42 0.060(3) 0.0262(19) 0.0295(19) -0.0091(15) -0.001(2) -0.0033(19) C43 0.045(2) 0.035(2) 0.038(2) 0.0044(18) -0.0089(19) -0.0123(19) C44 0.033(2) 0.0316(19) 0.034(2) -0.0003(18) 0.0044(16) 0.0012(18) C45 0.0260(19) 0.0295(18) 0.0305(19) -0.0034(15) 0.0028(14) -0.0034(14) C46 0.039(2) 0.032(2) 0.038(2) -0.0046(17) 0.0038(17) 0.0031(17) C47 0.035(2) 0.040(2) 0.048(2) 0.0120(19) 0.0006(18) 0.0017(17) C48 0.029(2) 0.064(3) 0.0273(19) 0.0066(19) 0.0001(16) -0.0063(18) C49 0.0301(18) 0.041(2) 0.0351(19) -0.0138(17) 0.0036(16) -0.0047(18) C50 0.0284(18) 0.0226(18) 0.0388(19) 0.0003(14) -0.0032(16) -0.0028(15) F1 0.0333(12) 0.0595(15) 0.0338(12) 0.0064(11) -0.0072(10) 0.0057(12) F2 0.0673(18) 0.0483(14) 0.0321(12) 0.0107(11) 0.0059(11) 0.0015(13) F3 0.0456(14) 0.0457(14) 0.0569(16) -0.0042(12) 0.0222(13) -0.0133(12) F4 0.0282(13) 0.0666(18) 0.0659(17) 0.0024(14) -0.0061(12) -0.0073(11) F5 0.0344(12) 0.0540(15) 0.0476(14) 0.0127(11) -0.0093(10) 0.0021(11) F6 0.0368(12) 0.0427(13) 0.0748(17) -0.0114(13) 0.0086(12) 0.0046(12) F7 0.0702(19) 0.0466(15) 0.0718(19) -0.0125(13) 0.0336(16) 0.0071(14) F8 0.098(2) 0.0376(13) 0.0449(14) -0.0173(11) 0.0067(15) -0.0162(15) F9 0.0580(17) 0.0513(15) 0.0620(17) -0.0059(13) -0.0164(14) -0.0133(13) F10 0.0283(11) 0.0465(13) 0.0545(14) -0.0104(12) 0.0021(10) -0.0047(11) F11 0.0840(19) 0.0343(13) 0.0497(15) -0.0011(12) -0.0023(14) 0.0240(13) F12 0.078(2) 0.0553(17) 0.0592(17) 0.0246(14) -0.0048(15) 0.0147(15) F13 0.0606(18) 0.086(2) 0.0288(12) 0.0114(13) 0.0011(12) -0.0016(15) F14 0.0635(17) 0.0613(15) 0.0402(13) -0.0205(12) 0.0039(13) 0.0022(13) F15 0.0585(15) 0.0285(11) 0.0449(13) -0.0007(10) 0.0000(12) 0.0044(11) _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 O3 1.906(2) . ? Zr1 O1 2.120(2) . ? Zr1 O2 2.149(2) . ? Zr1 O4 2.194(2) . ? Zr1 C15 2.493(3) . ? Zr1 C13 2.501(3) . ? Zr1 C14 2.505(3) . ? Zr1 C16 2.513(3) . ? Zr1 C17 2.521(3) . ? Zr1 B1 2.773(4) . ? Zr1 Zr2 3.3608(4) . ? Zr2 O6 1.908(2) . ? Zr2 O1 2.156(2) . ? Zr2 O2 2.161(2) . ? Zr2 O5 2.200(2) . ? Zr2 C27 2.494(3) . ? Zr2 C23 2.498(4) . ? Zr2 C26 2.512(4) . ? Zr2 C24 2.523(4) . ? Zr2 C25 2.523(3) . ? Zr2 B1 2.811(4) . ? O1 B1 1.454(4) . ? O2 C1 1.449(4) . ? O3 C3 1.407(5) . ? O4 C5 1.433(4) . ? O4 B1 1.521(4) . ? O5 C7 1.450(4) . ? O5 B1 1.510(5) . ? O6 C9 1.417(4) . ? O7 B1 1.407(4) . ? O7 C11 1.431(4) . ? C1 C2 1.498(6) . ? C3 C4 1.478(6) . ? C5 C6' 1.427(8) . ? C5 C6 1.457(6) . ? C7 C8 1.483(5) . ? C9 C10 1.434(6) . ? C11 C12 1.490(5) . ? C13 C14 1.416(5) . ? C13 C17 1.422(5) . ? C13 C18 1.502(5) . ? C14 C15 1.420(5) . ? C14 C19 1.503(5) . ? C15 C16 1.423(5) . ? C15 C20 1.501(5) . ? C16 C17 1.411(5) . ? C16 C21 1.502(5) . ? C17 C22 1.515(5) . ? C23 C27 1.412(5) . ? C23 C24 1.423(5) . ? C23 C28 1.498(5) . ? C24 C25 1.407(6) . ? C24 C29 1.502(5) . ? C25 C26 1.427(6) . ? C25 C30 1.506(6) . ? C26 C27 1.410(5) . ? C26 C31 1.495(6) . ? C27 C32 1.509(5) . ? B2 C33 1.646(5) . ? B2 C45 1.646(5) . ? B2 C39 1.653(5) . ? C33 C34 1.378(5) . ? C33 C38 1.387(5) . ? C34 F1 1.358(4) . ? C34 C35 1.387(5) . ? C35 F2 1.342(4) . ? C35 C36 1.375(6) . ? C36 F3 1.354(4) . ? C36 C37 1.358(6) . ? C37 F4 1.348(4) . ? C37 C38 1.360(5) . ? C38 F5 1.354(4) . ? C39 C44 1.371(5) . ? C39 C40 1.391(5) . ? C40 F6 1.361(4) . ? C40 C41 1.385(6) . ? C41 F7 1.341(5) . ? C41 C42 1.366(6) . ? C42 F8 1.343(4) . ? C42 C43 1.375(6) . ? C43 F9 1.346(5) . ? C43 C44 1.376(5) . ? C44 F10 1.355(4) . ? C45 C46 1.385(5) . ? C45 C50 1.385(5) . ? C46 F11 1.356(4) . ? C46 C47 1.380(5) . ? C47 F12 1.344(5) . ? C47 C48 1.357(6) . ? C48 F13 1.349(4) . ? C48 C49 1.374(6) . ? C49 F14 1.339(4) . ? C49 C50 1.388(5) . ? C50 F15 1.343(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 O3 Zr1 O1 128.71(9) . . ? O3 Zr1 O2 91.40(10) . . ? O1 Zr1 O2 71.16(8) . . ? O3 Zr1 O4 89.10(10) . . ? O1 Zr1 O4 63.38(8) . . ? O2 Zr1 O4 120.85(9) . . ? O3 Zr1 C15 90.07(11) . . ? O1 Zr1 C15 136.40(10) . . ? O2 Zr1 C15 134.91(10) . . ? O4 Zr1 C15 104.22(11) . . ? O3 Zr1 C13 120.36(12) . . ? O1 Zr1 C13 106.81(11) . . ? O2 Zr1 C13 86.89(10) . . ? O4 Zr1 C13 140.29(10) . . ? C15 Zr1 C13 54.46(12) . . ? O3 Zr1 C14 90.60(12) . . ? O1 Zr1 C14 139.35(11) . . ? O2 Zr1 C14 101.91(10) . . ? O4 Zr1 C14 137.24(10) . . ? C15 Zr1 C14 33.01(12) . . ? C13 Zr1 C14 32.87(12) . . ? O3 Zr1 C16 119.44(11) . . ? O1 Zr1 C16 103.39(10) . . ? O2 Zr1 C16 138.37(10) . . ? O4 Zr1 C16 89.07(10) . . ? C15 Zr1 C16 33.01(11) . . ? C13 Zr1 C16 54.30(11) . . ? C14 Zr1 C16 54.65(11) . . ? O3 Zr1 C17 143.06(11) . . ? O1 Zr1 C17 88.04(9) . . ? O2 Zr1 C17 106.34(10) . . ? O4 Zr1 C17 107.74(10) . . ? C15 Zr1 C17 54.42(11) . . ? C13 Zr1 C17 32.90(11) . . ? C14 Zr1 C17 54.59(11) . . ? C16 Zr1 C17 32.54(11) . . ? O3 Zr1 B1 107.52(11) . . ? O1 Zr1 B1 31.07(9) . . ? O2 Zr1 B1 92.31(10) . . ? O4 Zr1 B1 33.14(10) . . ? C15 Zr1 B1 129.80(12) . . ? C13 Zr1 B1 132.12(12) . . ? C14 Zr1 B1 156.75(12) . . ? C16 Zr1 B1 102.78(12) . . ? C17 Zr1 B1 103.91(11) . . ? O3 Zr1 Zr2 99.81(7) . . ? O1 Zr1 Zr2 38.57(6) . . ? O2 Zr1 Zr2 38.89(6) . . ? O4 Zr1 Zr2 82.91(6) . . ? C15 Zr1 Zr2 167.98(8) . . ? C13 Zr1 Zr2 113.99(9) . . ? C14 Zr1 Zr2 138.97(8) . . ? C16 Zr1 Zr2 139.81(8) . . ? C17 Zr1 Zr2 114.45(8) . . ? B1 Zr1 Zr2 53.51(8) . . ? O6 Zr2 O1 137.97(9) . . ? O6 Zr2 O2 89.32(10) . . ? O1 Zr2 O2 70.25(8) . . ? O6 Zr2 O5 93.06(10) . . ? O1 Zr2 O5 62.71(8) . . ? O2 Zr2 O5 110.01(9) . . ? O6 Zr2 C27 88.14(11) . . ? O1 Zr2 C27 133.50(10) . . ? O2 Zr2 C27 114.29(11) . . ? O5 Zr2 C27 135.70(11) . . ? O6 Zr2 C23 117.47(12) . . ? O1 Zr2 C23 101.94(11) . . ? O2 Zr2 C23 98.21(11) . . ? O5 Zr2 C23 138.68(11) . . ? C27 Zr2 C23 32.87(12) . . ? O6 Zr2 C26 88.59(12) . . ? O1 Zr2 C26 128.36(11) . . ? O2 Zr2 C26 146.98(11) . . ? O5 Zr2 C26 103.00(11) . . ? C27 Zr2 C26 32.71(12) . . ? C23 Zr2 C26 54.52(12) . . ? O6 Zr2 C24 140.75(11) . . ? O1 Zr2 C24 81.01(10) . . ? O2 Zr2 C24 114.40(12) . . ? O5 Zr2 C24 106.12(11) . . ? C27 Zr2 C24 54.22(12) . . ? C23 Zr2 C24 32.91(12) . . ? C26 Zr2 C24 54.23(13) . . ? O6 Zr2 C25 118.61(13) . . ? O1 Zr2 C25 95.43(11) . . ? O2 Zr2 C25 146.77(12) . . ? O5 Zr2 C25 87.51(10) . . ? C27 Zr2 C25 54.22(12) . . ? C23 Zr2 C25 54.30(12) . . ? C26 Zr2 C25 32.94(13) . . ? C24 Zr2 C25 32.38(13) . . ? O6 Zr2 B1 119.67(11) . . ? O1 Zr2 B1 30.57(10) . . ? O2 Zr2 B1 91.04(10) . . ? O5 Zr2 B1 32.24(10) . . ? C27 Zr2 B1 143.34(12) . . ? C23 Zr2 B1 122.11(12) . . ? C26 Zr2 B1 118.32(12) . . ? C24 Zr2 B1 91.99(12) . . ? C25 Zr2 B1 89.95(12) . . ? O6 Zr2 Zr1 105.38(7) . . ? O1 Zr2 Zr1 37.80(6) . . ? O2 Zr2 Zr1 38.64(6) . . ? O5 Zr2 Zr1 74.19(6) . . ? C27 Zr2 Zr1 147.38(9) . . ? C23 Zr2 Zr1 118.49(9) . . ? C26 Zr2 Zr1 165.80(9) . . ? C24 Zr2 Zr1 112.62(9) . . ? C25 Zr2 Zr1 133.13(10) . . ? B1 Zr2 Zr1 52.49(8) . . ? B1 O1 Zr1 100.14(18) . . ? B1 O1 Zr2 100.5(2) . . ? Zr1 O1 Zr2 103.62(9) . . ? C1 O2 Zr1 119.0(2) . . ? C1 O2 Zr2 126.7(2) . . ? Zr1 O2 Zr2 102.47(9) . . ? C3 O3 Zr1 169.3(3) . . ? C5 O4 B1 122.5(3) . . ? C5 O4 Zr1 132.5(2) . . ? B1 O4 Zr1 94.82(17) . . ? C7 O5 B1 122.7(3) . . ? C7 O5 Zr2 136.9(2) . . ? B1 O5 Zr2 96.76(18) . . ? C9 O6 Zr2 164.1(3) . . ? B1 O7 C11 117.3(3) . . ? O7 B1 O1 120.7(3) . . ? O7 B1 O5 108.8(3) . . ? O1 B1 O5 99.8(3) . . ? O7 B1 O4 114.7(3) . . ? O1 B1 O4 99.3(3) . . ? O5 B1 O4 112.5(3) . . ? O7 B1 Zr1 146.3(3) . . ? O1 B1 Zr1 48.79(14) . . ? O5 B1 Zr1 104.8(2) . . ? O4 B1 Zr1 52.04(14) . . ? O7 B1 Zr2 126.8(2) . . ? O1 B1 Zr2 48.97(15) . . ? O5 B1 Zr2 51.00(15) . . ? O4 B1 Zr2 118.4(2) . . ? Zr1 B1 Zr2 74.00(9) . . ? O2 C1 C2 111.2(3) . . ? O3 C3 C4 113.0(4) . . ? C6' C5 O4 115.9(6) . . ? C6' C5 C6 69.8(6) . . ? O4 C5 C6 116.4(4) . . ? O5 C7 C8 110.6(3) . . ? O6 C9 C10 114.5(4) . . ? O7 C11 C12 111.2(3) . . ? C14 C13 C17 108.6(3) . . ? C14 C13 C18 126.4(3) . . ? C17 C13 C18 124.8(4) . . ? C14 C13 Zr1 73.7(2) . . ? C17 C13 Zr1 74.31(19) . . ? C18 C13 Zr1 123.2(2) . . ? C13 C14 C15 107.4(3) . . ? C13 C14 C19 127.4(3) . . ? C15 C14 C19 125.1(3) . . ? C13 C14 Zr1 73.4(2) . . ? C15 C14 Zr1 73.1(2) . . ? C19 C14 Zr1 121.7(3) . . ? C14 C15 C16 108.3(3) . . ? C14 C15 C20 125.6(3) . . ? C16 C15 C20 126.1(3) . . ? C14 C15 Zr1 73.93(19) . . ? C16 C15 Zr1 74.27(18) . . ? C20 C15 Zr1 120.6(2) . . ? C17 C16 C15 108.1(3) . . ? C17 C16 C21 126.1(3) . . ? C15 C16 C21 125.7(3) . . ? C17 C16 Zr1 74.01(18) . . ? C15 C16 Zr1 72.72(19) . . ? C21 C16 Zr1 122.8(2) . . ? C16 C17 C13 107.8(3) . . ? C16 C17 C22 127.6(3) . . ? C13 C17 C22 124.5(3) . . ? C16 C17 Zr1 73.44(19) . . ? C13 C17 Zr1 72.79(19) . . ? C22 C17 Zr1 122.7(2) . . ? C27 C23 C24 107.5(3) . . ? C27 C23 C28 126.0(4) . . ? C24 C23 C28 126.1(4) . . ? C27 C23 Zr2 73.4(2) . . ? C24 C23 Zr2 74.5(2) . . ? C28 C23 Zr2 123.5(3) . . ? C25 C24 C23 108.2(3) . . ? C25 C24 C29 126.2(4) . . ? C23 C24 C29 125.5(4) . . ? C25 C24 Zr2 73.8(2) . . ? C23 C24 Zr2 72.6(2) . . ? C29 C24 Zr2 123.6(3) . . ? C24 C25 C26 108.1(3) . . ? C24 C25 C30 125.0(4) . . ? C26 C25 C30 126.7(4) . . ? C24 C25 Zr2 73.8(2) . . ? C26 C25 Zr2 73.1(2) . . ? C30 C25 Zr2 122.6(3) . . ? C27 C26 C25 107.4(3) . . ? C27 C26 C31 126.5(4) . . ? C25 C26 C31 125.9(4) . . ? C27 C26 Zr2 73.0(2) . . ? C25 C26 Zr2 74.0(2) . . ? C31 C26 Zr2 122.9(3) . . ? C26 C27 C23 108.8(3) . . ? C26 C27 C32 125.3(4) . . ? C23 C27 C32 125.5(4) . . ? C26 C27 Zr2 74.3(2) . . ? C23 C27 Zr2 73.7(2) . . ? C32 C27 Zr2 123.7(3) . . ? C33 B2 C45 112.8(3) . . ? C33 B2 C39 109.4(3) . . ? C45 B2 C39 113.1(3) . . ? C34 C33 C38 112.9(3) . . ? C34 C33 B2 120.2(3) . . ? C38 C33 B2 126.8(3) . . ? F1 C34 C33 119.7(3) . . ? F1 C34 C35 115.4(3) . . ? C33 C34 C35 124.9(3) . . ? F2 C35 C36 120.4(4) . . ? F2 C35 C34 121.6(4) . . ? C36 C35 C34 118.1(3) . . ? F3 C36 C37 120.9(4) . . ? F3 C36 C35 119.3(4) . . ? C37 C36 C35 119.7(3) . . ? F4 C37 C36 119.4(4) . . ? F4 C37 C38 120.8(4) . . ? C36 C37 C38 119.8(4) . . ? F5 C38 C37 115.7(3) . . ? F5 C38 C33 119.6(3) . . ? C37 C38 C33 124.7(3) . . ? C44 C39 C40 113.2(3) . . ? C44 C39 B2 121.3(3) . . ? C40 C39 B2 125.5(3) . . ? F6 C40 C41 115.5(4) . . ? F6 C40 C39 120.0(3) . . ? C41 C40 C39 124.6(4) . . ? F7 C41 C42 120.5(4) . . ? F7 C41 C40 120.7(4) . . ? C42 C41 C40 118.8(4) . . ? F8 C42 C41 120.5(4) . . ? F8 C42 C43 120.3(4) . . ? C41 C42 C43 119.2(3) . . ? F9 C43 C42 119.5(4) . . ? F9 C43 C44 120.9(4) . . ? C42 C43 C44 119.6(4) . . ? F10 C44 C39 120.3(3) . . ? F10 C44 C43 115.1(3) . . ? C39 C44 C43 124.6(4) . . ? C46 C45 C50 113.1(3) . . ? C46 C45 B2 127.2(3) . . ? C50 C45 B2 119.6(3) . . ? F11 C46 C47 115.9(3) . . ? F11 C46 C45 119.4(3) . . ? C47 C46 C45 124.7(4) . . ? F12 C47 C48 120.3(4) . . ? F12 C47 C46 120.3(4) . . ? C48 C47 C46 119.4(4) . . ? F13 C48 C47 120.9(4) . . ? F13 C48 C49 119.5(4) . . ? C47 C48 C49 119.6(3) . . ? F14 C49 C48 120.1(3) . . ? F14 C49 C50 121.0(4) . . ? C48 C49 C50 118.9(3) . . ? F15 C50 C45 120.2(3) . . ? F15 C50 C49 115.5(3) . . ? C45 C50 C49 124.3(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.590 _refine_diff_density_min -0.294 _refine_diff_density_rms 0.071 data_ic11788 _database_code_depnum_ccdc_archive 'CCDC 672319' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H59 B2 F15 O6 Zr2' _chemical_formula_weight 1233.02 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' Zr Zr -2.9673 0.5597 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.5767(5) _cell_length_b 16.4862(8) _cell_length_c 32.1655(17) _cell_angle_alpha 90.00 _cell_angle_beta 93.389(1) _cell_angle_gamma 90.00 _cell_volume 5598.9(5) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5589 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 21.21 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas not_measured _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2504 _exptl_absorpt_coefficient_mu 0.466 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8005 _exptl_absorpt_correction_T_max 0.9126 _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 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49575 _diffrn_reflns_av_R_equivalents 0.0591 _diffrn_reflns_av_sigmaI/netI 0.0613 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 1.27 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12748 _reflns_number_gt 9142 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1010P)^2^+10.4174P] 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 12748 _refine_ls_number_parameters 689 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0997 _refine_ls_R_factor_gt 0.0695 _refine_ls_wR_factor_ref 0.2137 _refine_ls_wR_factor_gt 0.1928 _refine_ls_goodness_of_fit_ref 1.089 _refine_ls_restrained_S_all 1.089 _refine_ls_shift/su_max 0.011 _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 Zr1 Zr 0.16251(4) 0.70708(3) 0.190124(14) 0.02883(14) Uani 1 1 d . . . Zr2 Zr 0.05774(5) 0.69071(3) 0.089543(14) 0.03422(15) Uani 1 1 d . . . O1 O 0.2245(3) 0.7128(2) 0.12781(10) 0.0336(8) Uani 1 1 d . . . O2 O 0.0335(4) 0.6366(2) 0.14914(10) 0.0390(9) Uani 1 1 d . . . O3 O 0.0239(3) 0.7487(2) 0.21896(11) 0.0425(9) Uani 1 1 d . . . O4 O 0.2014(4) 0.8273(2) 0.16588(12) 0.0415(9) Uani 1 1 d . B . O5 O 0.1308(4) 0.8140(2) 0.09038(13) 0.0489(10) Uani 1 1 d . . . O6 O -0.1105(4) 0.7338(3) 0.08706(13) 0.0574(11) Uani 1 1 d D . . B1 B 0.2395(7) 0.8002(4) 0.1228(2) 0.0434(15) Uani 1 1 d . . . C1 C -0.0947(7) 0.6091(5) 0.1580(2) 0.0637(19) Uani 1 1 d . . . H1A H -0.1425 0.6558 0.1684 0.076 Uiso 1 1 calc R . . H1B H -0.1387 0.5907 0.1316 0.076 Uiso 1 1 calc R . . C2 C -0.0972(8) 0.5445(6) 0.1880(3) 0.096(3) Uani 1 1 d . . . H2A H -0.0511 0.4976 0.1779 0.144 Uiso 1 1 calc R . . H2B H -0.1852 0.5291 0.1919 0.144 Uiso 1 1 calc R . . H2C H -0.0570 0.5628 0.2146 0.144 Uiso 1 1 calc R . . C3 C -0.0661(6) 0.7786(4) 0.2466(2) 0.0573(17) Uani 1 1 d . . . H3A H -0.0256 0.8210 0.2647 0.069 Uiso 1 1 calc R . . H3B H -0.0924 0.7338 0.2647 0.069 Uiso 1 1 calc R . . C4 C -0.1788(7) 0.8129(5) 0.2240(3) 0.076(2) Uani 1 1 d . . . H4A H -0.1536 0.8587 0.2069 0.114 Uiso 1 1 calc R . . H4B H -0.2388 0.8316 0.2440 0.114 Uiso 1 1 calc R . . H4C H -0.2191 0.7712 0.2060 0.114 Uiso 1 1 calc R . . C5 C 0.2284(6) 0.9075(4) 0.1812(2) 0.0575(17) Uani 1 1 d D . . H5A H 0.2363 0.9447 0.1574 0.069 Uiso 0.50 1 calc PR A 1 H5B H 0.3104 0.9071 0.1977 0.069 Uiso 0.50 1 calc PR A 1 H5'A H 0.2752 0.9380 0.1606 0.069 Uiso 0.50 1 calc PR A 2 H5'B H 0.2823 0.9042 0.2074 0.069 Uiso 0.50 1 calc PR A 2 C6 C 0.129(3) 0.938(2) 0.2075(9) 0.088(11) Uani 0.50 1 d PD B 1 H6A H 0.1503 0.9925 0.2173 0.133 Uiso 0.50 1 calc PR B 1 H6B H 0.1216 0.9016 0.2314 0.133 Uiso 0.50 1 calc PR B 1 H6C H 0.0474 0.9391 0.1911 0.133 Uiso 0.50 1 calc PR B 1 C6' C 0.109(2) 0.950(2) 0.1890(9) 0.074(8) Uani 0.50 1 d PD B 2 H6'A H 0.1287 1.0050 0.1994 0.111 Uiso 0.50 1 calc PR B 2 H6'B H 0.0636 0.9203 0.2098 0.111 Uiso 0.50 1 calc PR B 2 H6'C H 0.0563 0.9539 0.1630 0.111 Uiso 0.50 1 calc PR B 2 C7 C 0.0839(8) 0.8928(4) 0.0796(2) 0.070(2) Uani 1 1 d . . . H7A H 0.1472 0.9339 0.0893 0.084 Uiso 1 1 calc R . . H7B H 0.0054 0.9029 0.0941 0.084 Uiso 1 1 calc R . . C8 C 0.0575(14) 0.9018(7) 0.0352(3) 0.149(6) Uani 1 1 d . . . H8A H 0.1372 0.9007 0.0211 0.223 Uiso 1 1 calc R . . H8B H 0.0145 0.9536 0.0295 0.223 Uiso 1 1 calc R . . H8C H 0.0031 0.8572 0.0248 0.223 Uiso 1 1 calc R . . C9 C -0.2362(8) 0.7638(6) 0.0816(3) 0.112(3) Uiso 1 1 d D . . H9A H -0.2670 0.7830 0.1083 0.134 Uiso 1 1 calc R . . H9B H -0.2944 0.7214 0.0699 0.134 Uiso 1 1 calc R . . C10 C -0.2259(9) 0.8329(6) 0.0515(3) 0.097(3) Uani 1 1 d D . . H10A H -0.3105 0.8543 0.0439 0.146 Uiso 1 1 calc R . . H10B H -0.1872 0.8135 0.0264 0.146 Uiso 1 1 calc R . . H10C H -0.1732 0.8759 0.0645 0.146 Uiso 1 1 calc R . . C11 C 0.3698(6) 0.8361(5) 0.1098(2) 0.0632(19) Uani 1 1 d . . . H11A H 0.4356 0.8250 0.1318 0.095 Uiso 1 1 calc R . . H11B H 0.3615 0.8949 0.1058 0.095 Uiso 1 1 calc R . . H11C H 0.3930 0.8108 0.0838 0.095 Uiso 1 1 calc R . . C12 C 0.2266(5) 0.6227(3) 0.25226(16) 0.0388(12) Uani 1 1 d . . . C13 C 0.2831(5) 0.6995(3) 0.25947(15) 0.0339(11) Uani 1 1 d . . . C14 C 0.3766(5) 0.7104(3) 0.23029(15) 0.0343(11) Uani 1 1 d . . . C15 C 0.3771(5) 0.6407(4) 0.20478(16) 0.0409(13) Uani 1 1 d . . . C16 C 0.2848(6) 0.5861(3) 0.21807(17) 0.0432(13) Uani 1 1 d . . . C17 C 0.1299(6) 0.5836(4) 0.2792(2) 0.0585(18) Uani 1 1 d . . . H17A H 0.1671 0.5769 0.3076 0.088 Uiso 1 1 calc R . . H17B H 0.1055 0.5305 0.2677 0.088 Uiso 1 1 calc R . . H17C H 0.0549 0.6184 0.2797 0.088 Uiso 1 1 calc R . . C18 C 0.2535(6) 0.7550(4) 0.29435(17) 0.0469(14) Uani 1 1 d . . . H18A H 0.3057 0.7403 0.3194 0.070 Uiso 1 1 calc R . . H18B H 0.1638 0.7499 0.2999 0.070 Uiso 1 1 calc R . . H18C H 0.2716 0.8111 0.2866 0.070 Uiso 1 1 calc R . . C19 C 0.4687(5) 0.7796(4) 0.22955(19) 0.0492(15) Uani 1 1 d . . . H19A H 0.5504 0.7627 0.2426 0.074 Uiso 1 1 calc R . . H19B H 0.4359 0.8257 0.2449 0.074 Uiso 1 1 calc R . . H19C H 0.4796 0.7957 0.2006 0.074 Uiso 1 1 calc R . . C20 C 0.4690(6) 0.6245(5) 0.1721(2) 0.0591(18) Uani 1 1 d . . . H20A H 0.4451 0.5744 0.1573 0.089 Uiso 1 1 calc R . . H20B H 0.5544 0.6186 0.1854 0.089 Uiso 1 1 calc R . . H20C H 0.4677 0.6698 0.1524 0.089 Uiso 1 1 calc R . . C21 C 0.2618(8) 0.5025(4) 0.2013(2) 0.067(2) Uani 1 1 d . . . H21A H 0.2555 0.5044 0.1708 0.101 Uiso 1 1 calc R . . H21B H 0.1826 0.4813 0.2113 0.101 Uiso 1 1 calc R . . H21C H 0.3321 0.4671 0.2107 0.101 Uiso 1 1 calc R . . C22 C 0.1960(6) 0.5999(4) 0.04871(17) 0.0484(15) Uani 1 1 d . . . C23 C 0.1529(6) 0.6600(4) 0.02140(17) 0.0477(14) Uani 1 1 d . . . C24 C 0.0205(6) 0.6525(4) 0.01456(16) 0.0515(16) Uani 1 1 d . . . C25 C -0.0178(7) 0.5854(5) 0.0383(2) 0.067(2) Uani 1 1 d . . . C26 C 0.0945(9) 0.5534(4) 0.05980(17) 0.063(2) Uani 1 1 d . . . C27 C 0.3351(8) 0.5859(6) 0.0620(2) 0.086(3) Uani 1 1 d . . . H27A H 0.3747 0.5532 0.0409 0.129 Uiso 1 1 calc R . . H27B H 0.3414 0.5573 0.0888 0.129 Uiso 1 1 calc R . . H27C H 0.3786 0.6383 0.0649 0.129 Uiso 1 1 calc R . . C28 C 0.2348(9) 0.7199(5) -0.0007(3) 0.082(3) Uani 1 1 d . . . H28A H 0.3075 0.7355 0.0180 0.122 Uiso 1 1 calc R . . H28B H 0.1848 0.7683 -0.0083 0.122 Uiso 1 1 calc R . . H28C H 0.2650 0.6948 -0.0258 0.122 Uiso 1 1 calc R . . C29 C -0.0661(10) 0.7023(6) -0.0142(2) 0.097(3) Uani 1 1 d . . . H29A H -0.0342 0.7580 -0.0152 0.146 Uiso 1 1 calc R . . H29B H -0.1515 0.7025 -0.0039 0.146 Uiso 1 1 calc R . . H29C H -0.0689 0.6788 -0.0422 0.146 Uiso 1 1 calc R . . C30 C -0.1504(9) 0.5517(7) 0.0379(3) 0.124(5) Uani 1 1 d . . . H30A H -0.1646 0.5151 0.0141 0.186 Uiso 1 1 calc R . . H30B H -0.2115 0.5964 0.0357 0.186 Uiso 1 1 calc R . . H30C H -0.1611 0.5217 0.0638 0.186 Uiso 1 1 calc R . . C31 C 0.1001(13) 0.4776(5) 0.0866(2) 0.121(5) Uani 1 1 d . . . H31A H 0.1189 0.4305 0.0694 0.181 Uiso 1 1 calc R . . H31B H 0.0183 0.4695 0.0988 0.181 Uiso 1 1 calc R . . H31C H 0.1667 0.4836 0.1089 0.181 Uiso 1 1 calc R . . B2 B 0.3289(6) 0.2407(4) 0.15466(19) 0.0403(14) Uani 1 1 d . . . H2 H 0.314(5) 0.269(4) 0.1833(19) 0.048 Uiso 1 1 d . . . C32 C 0.4082(5) 0.1568(4) 0.16586(19) 0.0448(13) Uani 1 1 d . . . C33 C 0.3876(6) 0.1153(4) 0.2022(2) 0.0494(15) Uani 1 1 d . . . C34 C 0.4528(6) 0.0464(4) 0.2151(2) 0.0544(17) Uani 1 1 d . . . C35 C 0.5434(6) 0.0166(4) 0.1910(2) 0.0581(18) Uani 1 1 d . . . C36 C 0.5682(6) 0.0543(4) 0.1547(2) 0.0592(17) Uani 1 1 d . . . C37 C 0.5011(6) 0.1233(4) 0.1428(2) 0.0544(16) Uani 1 1 d . . . C38 C 0.1814(5) 0.2230(3) 0.13802(16) 0.0376(12) Uani 1 1 d . . . C39 C 0.1333(6) 0.1519(4) 0.12047(18) 0.0445(13) Uani 1 1 d . . . C40 C 0.0078(6) 0.1410(4) 0.10715(19) 0.0490(14) Uani 1 1 d . . . C41 C -0.0761(5) 0.2039(4) 0.11089(17) 0.0440(14) Uani 1 1 d . . . C42 C -0.0334(6) 0.2757(3) 0.12736(16) 0.0410(13) Uani 1 1 d . . . C43 C 0.0916(5) 0.2828(3) 0.14038(16) 0.0386(12) Uani 1 1 d . . . C44 C 0.4002(5) 0.2995(3) 0.12232(18) 0.0412(13) Uani 1 1 d . . . C45 C 0.3864(6) 0.2934(4) 0.0797(2) 0.0500(15) Uani 1 1 d . . . C46 C 0.4476(6) 0.3420(5) 0.0526(2) 0.0575(17) Uani 1 1 d . . . C47 C 0.5270(6) 0.4013(4) 0.0680(2) 0.0555(17) Uani 1 1 d . . . C48 C 0.5449(6) 0.4115(4) 0.1102(2) 0.0547(16) Uani 1 1 d . . . C49 C 0.4810(5) 0.3616(4) 0.13640(18) 0.0427(13) Uani 1 1 d . . . F2 F 0.2972(4) 0.1412(2) 0.22725(11) 0.0591(9) Uani 1 1 d . . . F3 F 0.4248(4) 0.0083(2) 0.25048(12) 0.0696(11) Uani 1 1 d . . . F4 F 0.6081(4) -0.0508(2) 0.20317(16) 0.0832(14) Uani 1 1 d . . . F5 F 0.6571(4) 0.0240(3) 0.13076(17) 0.0866(14) Uani 1 1 d . . . F6 F 0.5304(4) 0.1564(3) 0.10641(14) 0.0733(12) Uani 1 1 d . . . F7 F 0.2105(3) 0.0875(2) 0.11485(13) 0.0649(11) Uani 1 1 d . . . F8 F -0.0321(4) 0.0696(2) 0.09044(15) 0.0767(12) Uani 1 1 d . . . F9 F -0.1989(3) 0.1943(3) 0.09821(13) 0.0650(11) Uani 1 1 d . . . F10 F -0.1148(3) 0.3381(2) 0.13064(12) 0.0587(10) Uani 1 1 d . . . F11 F 0.1259(3) 0.35513(19) 0.15779(11) 0.0497(8) Uani 1 1 d . . . F12 F 0.3132(4) 0.2342(3) 0.06211(11) 0.0634(10) Uani 1 1 d . . . F13 F 0.4296(4) 0.3322(3) 0.01080(13) 0.0810(13) Uani 1 1 d . . . F14 F 0.5877(4) 0.4499(3) 0.04140(15) 0.0819(13) Uani 1 1 d . . . F15 F 0.6240(4) 0.4694(3) 0.12554(16) 0.0807(13) Uani 1 1 d . . . F16 F 0.5029(3) 0.3753(2) 0.17748(11) 0.0562(9) 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 Zr1 0.0307(3) 0.0291(3) 0.0266(2) -0.00389(18) 0.00147(18) -0.00013(19) Zr2 0.0418(3) 0.0343(3) 0.0264(2) -0.00432(19) 0.0006(2) -0.0026(2) O1 0.0348(19) 0.0348(19) 0.0316(17) -0.0016(14) 0.0043(14) -0.0012(15) O2 0.050(2) 0.036(2) 0.0313(17) -0.0031(15) 0.0025(16) -0.0151(17) O3 0.037(2) 0.047(2) 0.044(2) -0.0047(17) 0.0076(16) 0.0027(17) O4 0.048(2) 0.030(2) 0.047(2) -0.0037(16) -0.0019(17) -0.0035(17) O5 0.055(3) 0.037(2) 0.053(2) 0.0068(18) -0.0117(19) -0.0024(19) O6 0.042(2) 0.075(3) 0.054(3) -0.007(2) -0.0043(19) 0.004(2) B1 0.045(4) 0.045(4) 0.040(3) 0.005(3) 0.001(3) -0.004(3) C1 0.063(4) 0.072(5) 0.056(4) -0.006(3) 0.004(3) -0.026(4) C2 0.078(6) 0.115(8) 0.095(6) 0.031(6) 0.012(5) -0.044(5) C3 0.051(4) 0.071(5) 0.052(4) -0.006(3) 0.021(3) 0.004(3) C4 0.049(4) 0.076(5) 0.104(6) -0.009(5) 0.017(4) 0.011(4) C5 0.060(4) 0.037(3) 0.074(4) -0.012(3) -0.004(3) -0.008(3) C6 0.086(15) 0.058(17) 0.13(3) -0.034(17) 0.054(17) -0.024(11) C6' 0.090(15) 0.031(10) 0.11(2) -0.025(13) 0.054(15) -0.007(8) C7 0.100(6) 0.044(4) 0.065(4) 0.011(3) -0.010(4) 0.014(4) C8 0.277(17) 0.098(8) 0.070(6) 0.019(6) -0.012(8) 0.081(10) C10 0.078(6) 0.103(7) 0.109(7) 0.000(6) -0.011(5) 0.018(5) C11 0.062(4) 0.072(5) 0.057(4) 0.015(3) 0.008(3) -0.023(4) C12 0.043(3) 0.038(3) 0.035(3) 0.007(2) -0.003(2) -0.003(2) C13 0.035(3) 0.038(3) 0.028(2) 0.001(2) -0.001(2) 0.000(2) C14 0.029(3) 0.039(3) 0.033(2) 0.002(2) -0.002(2) -0.002(2) C15 0.042(3) 0.045(3) 0.035(3) -0.002(2) 0.001(2) 0.011(3) C16 0.050(3) 0.032(3) 0.046(3) 0.000(2) -0.008(3) 0.007(3) C17 0.046(4) 0.068(5) 0.060(4) 0.023(3) -0.007(3) -0.017(3) C18 0.040(3) 0.062(4) 0.038(3) -0.012(3) 0.000(2) 0.001(3) C19 0.034(3) 0.063(4) 0.049(3) 0.011(3) -0.007(3) -0.011(3) C20 0.052(4) 0.072(5) 0.053(4) -0.008(3) 0.007(3) 0.023(3) C21 0.082(5) 0.035(3) 0.082(5) -0.012(3) -0.018(4) 0.007(3) C22 0.068(4) 0.043(3) 0.034(3) -0.007(2) 0.000(3) 0.018(3) C23 0.063(4) 0.046(3) 0.036(3) -0.002(2) 0.012(3) 0.004(3) C24 0.061(4) 0.066(4) 0.027(3) -0.009(3) 0.001(3) 0.009(3) C25 0.080(5) 0.076(5) 0.045(3) -0.037(3) 0.017(3) -0.034(4) C26 0.127(7) 0.039(3) 0.026(3) -0.010(2) 0.012(3) -0.006(4) C27 0.089(6) 0.111(7) 0.057(4) -0.024(4) -0.011(4) 0.056(5) C28 0.099(6) 0.082(6) 0.068(5) 0.005(4) 0.043(5) -0.003(5) C29 0.119(8) 0.131(9) 0.039(4) -0.015(4) -0.016(4) 0.056(6) C30 0.106(7) 0.179(11) 0.091(6) -0.091(7) 0.042(5) -0.081(7) C31 0.279(15) 0.037(4) 0.049(4) 0.000(3) 0.035(6) -0.009(6) B2 0.045(4) 0.038(3) 0.036(3) 0.003(3) -0.007(3) 0.002(3) C32 0.040(3) 0.038(3) 0.055(3) 0.002(3) -0.008(3) 0.000(3) C33 0.050(4) 0.037(3) 0.059(4) 0.001(3) -0.016(3) -0.008(3) C34 0.059(4) 0.030(3) 0.071(4) 0.005(3) -0.020(3) -0.015(3) C35 0.046(4) 0.026(3) 0.098(5) 0.006(3) -0.027(4) -0.001(3) C36 0.045(4) 0.041(4) 0.090(5) -0.002(3) -0.006(3) 0.007(3) C37 0.050(4) 0.045(4) 0.067(4) 0.009(3) -0.005(3) 0.002(3) C38 0.037(3) 0.037(3) 0.039(3) 0.000(2) 0.001(2) -0.002(2) C39 0.043(3) 0.041(3) 0.050(3) -0.002(3) 0.003(3) 0.003(3) C40 0.050(4) 0.045(3) 0.051(3) -0.004(3) 0.001(3) -0.013(3) C41 0.032(3) 0.059(4) 0.040(3) 0.013(3) 0.000(2) 0.000(3) C42 0.049(3) 0.040(3) 0.035(3) 0.014(2) 0.011(2) 0.010(3) C43 0.044(3) 0.032(3) 0.040(3) 0.006(2) 0.001(2) -0.001(2) C44 0.035(3) 0.039(3) 0.050(3) 0.006(2) -0.005(2) 0.006(2) C45 0.037(3) 0.057(4) 0.055(4) 0.007(3) -0.003(3) 0.000(3) C46 0.041(4) 0.078(5) 0.054(4) 0.017(3) 0.008(3) 0.009(3) C47 0.049(4) 0.047(4) 0.073(4) 0.015(3) 0.026(3) 0.005(3) C48 0.037(3) 0.038(3) 0.089(5) -0.008(3) 0.011(3) 0.004(3) C49 0.035(3) 0.042(3) 0.051(3) -0.003(3) 0.000(2) 0.014(2) F2 0.071(3) 0.050(2) 0.056(2) 0.0087(17) 0.0028(19) -0.0028(19) F3 0.090(3) 0.043(2) 0.073(3) 0.0174(18) -0.022(2) -0.012(2) F4 0.070(3) 0.043(2) 0.131(4) 0.016(2) -0.033(3) 0.006(2) F5 0.065(3) 0.069(3) 0.126(4) 0.000(3) 0.009(3) 0.022(2) F6 0.071(3) 0.070(3) 0.081(3) 0.011(2) 0.020(2) 0.019(2) F7 0.054(2) 0.046(2) 0.094(3) -0.021(2) -0.008(2) 0.0129(17) F8 0.063(3) 0.055(2) 0.109(3) -0.023(2) -0.016(2) -0.010(2) F9 0.038(2) 0.080(3) 0.076(3) 0.015(2) -0.0055(18) -0.0076(18) F10 0.050(2) 0.054(2) 0.073(2) 0.0173(18) 0.0144(18) 0.0196(17) F11 0.063(2) 0.0293(17) 0.057(2) 0.0022(14) -0.0004(16) 0.0015(15) F12 0.055(2) 0.087(3) 0.048(2) -0.0062(19) -0.0050(17) -0.021(2) F13 0.074(3) 0.114(4) 0.055(2) 0.015(2) 0.010(2) -0.001(3) F14 0.085(3) 0.069(3) 0.096(3) 0.021(2) 0.041(3) -0.004(2) F15 0.063(3) 0.055(3) 0.126(4) -0.027(3) 0.029(2) -0.018(2) F16 0.049(2) 0.054(2) 0.065(2) -0.0149(17) -0.0033(17) 0.0004(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O3 1.908(4) . ? Zr1 O1 2.147(3) . ? Zr1 O2 2.177(3) . ? Zr1 O4 2.178(4) . ? Zr1 C12 2.496(5) . ? Zr1 C13 2.506(5) . ? Zr1 C16 2.514(5) . ? Zr1 C15 2.539(5) . ? Zr1 C14 2.541(5) . ? Zr1 B1 2.813(6) . ? Zr1 Zr2 3.3680(7) . ? Zr2 O6 1.914(4) . ? Zr2 O1 2.121(3) . ? Zr2 O2 2.144(3) . ? Zr2 O5 2.174(4) . ? Zr2 C25 2.493(6) . ? Zr2 C26 2.497(6) . ? Zr2 C24 2.501(5) . ? Zr2 C22 2.516(6) . ? Zr2 C23 2.517(5) . ? Zr2 B1 2.803(7) . ? O1 B1 1.460(7) . ? O2 C1 1.474(7) . ? O3 C3 1.428(7) . ? O4 C5 1.433(7) . ? O4 B1 1.532(8) . ? O5 C7 1.427(7) . ? O5 B1 1.523(8) . ? O6 C9 1.419(8) . ? B1 C11 1.578(9) . ? C1 C2 1.438(10) . ? C3 C4 1.472(10) . ? C5 C6 1.477(10) . ? C5 C6' 1.479(10) . ? C7 C8 1.449(11) . ? C9 C10 1.503(8) . ? C12 C13 1.414(7) . ? C12 C16 1.426(8) . ? C12 C17 1.522(8) . ? C13 C14 1.415(7) . ? C13 C18 1.495(7) . ? C14 C15 1.412(7) . ? C14 C19 1.501(7) . ? C15 C16 1.413(8) . ? C15 C20 1.497(8) . ? C16 C21 1.495(8) . ? C22 C23 1.383(8) . ? C22 C26 1.384(10) . ? C22 C27 1.525(10) . ? C23 C24 1.410(9) . ? C23 C28 1.518(9) . ? C24 C25 1.418(10) . ? C24 C29 1.506(10) . ? C25 C26 1.438(11) . ? C25 C30 1.507(10) . ? C26 C31 1.517(10) . ? B2 C44 1.638(9) . ? B2 C38 1.645(8) . ? B2 C32 1.647(9) . ? C32 C37 1.380(9) . ? C32 C33 1.383(8) . ? C33 F2 1.354(7) . ? C33 C34 1.380(9) . ? C34 F3 1.348(8) . ? C34 C35 1.359(10) . ? C35 F4 1.351(7) . ? C35 C36 1.361(10) . ? C36 F5 1.346(8) . ? C36 C37 1.383(9) . ? C37 F6 1.344(8) . ? C38 C43 1.374(8) . ? C38 C39 1.385(8) . ? C39 F7 1.359(7) . ? C39 C40 1.382(8) . ? C40 F8 1.350(7) . ? C40 C41 1.375(9) . ? C41 F9 1.348(6) . ? C41 C42 1.363(8) . ? C42 F10 1.349(6) . ? C42 C43 1.367(8) . ? C43 F11 1.358(6) . ? C44 C45 1.373(8) . ? C44 C49 1.392(8) . ? C45 F12 1.350(7) . ? C45 C46 1.373(9) . ? C46 F13 1.357(8) . ? C46 C47 1.363(10) . ? C47 F14 1.362(7) . ? C47 C48 1.370(10) . ? C48 F15 1.343(7) . ? C48 C49 1.382(9) . ? C49 F16 1.347(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zr1 O1 136.34(15) . . ? O3 Zr1 O2 90.82(15) . . ? O1 Zr1 O2 70.91(13) . . ? O3 Zr1 O4 90.78(16) . . ? O1 Zr1 O4 63.35(13) . . ? O2 Zr1 O4 113.20(13) . . ? O3 Zr1 C12 89.50(18) . . ? O1 Zr1 C12 133.51(16) . . ? O2 Zr1 C12 108.55(16) . . ? O4 Zr1 C12 138.24(16) . . ? O3 Zr1 C13 87.16(16) . . ? O1 Zr1 C13 131.73(15) . . ? O2 Zr1 C13 141.29(15) . . ? O4 Zr1 C13 105.48(15) . . ? C12 Zr1 C13 32.84(17) . . ? O3 Zr1 C16 120.35(18) . . ? O1 Zr1 C16 100.93(16) . . ? O2 Zr1 C16 94.79(16) . . ? O4 Zr1 C16 138.25(17) . . ? C12 Zr1 C16 33.06(18) . . ? C13 Zr1 C16 54.45(17) . . ? O3 Zr1 C15 140.26(17) . . ? O1 Zr1 C15 82.73(15) . . ? O2 Zr1 C15 113.80(17) . . ? O4 Zr1 C15 105.86(17) . . ? C12 Zr1 C15 54.09(18) . . ? C13 Zr1 C15 53.92(17) . . ? C16 Zr1 C15 32.47(19) . . ? O3 Zr1 C14 115.63(16) . . ? O1 Zr1 C14 99.30(15) . . ? O2 Zr1 C14 145.83(16) . . ? O4 Zr1 C14 88.91(15) . . ? C12 Zr1 C14 54.06(17) . . ? C13 Zr1 C14 32.55(16) . . ? C16 Zr1 C14 53.93(18) . . ? C15 Zr1 C14 32.29(17) . . ? O3 Zr1 B1 116.33(19) . . ? O1 Zr1 B1 30.65(16) . . ? O2 Zr1 B1 91.44(16) . . ? O4 Zr1 B1 32.70(17) . . ? C12 Zr1 B1 147.46(19) . . ? C13 Zr1 B1 123.82(18) . . ? C16 Zr1 B1 122.8(2) . . ? C15 Zr1 B1 94.69(19) . . ? C14 Zr1 B1 95.14(18) . . ? O3 Zr1 Zr2 106.08(12) . . ? O1 Zr1 Zr2 37.64(9) . . ? O2 Zr1 Zr2 38.43(9) . . ? O4 Zr1 Zr2 77.72(10) . . ? C12 Zr1 Zr2 141.53(13) . . ? C13 Zr1 Zr2 166.45(12) . . ? C16 Zr1 Zr2 114.38(13) . . ? C15 Zr1 Zr2 112.55(12) . . ? C14 Zr1 Zr2 136.30(12) . . ? B1 Zr1 Zr2 53.02(14) . . ? O6 Zr2 O1 134.39(16) . . ? O6 Zr2 O2 91.83(17) . . ? O1 Zr2 O2 72.05(13) . . ? O6 Zr2 O5 89.00(19) . . ? O1 Zr2 O5 63.23(14) . . ? O2 Zr2 O5 116.06(14) . . ? O6 Zr2 C25 88.3(2) . . ? O1 Zr2 C25 136.6(2) . . ? O2 Zr2 C25 104.5(2) . . ? O5 Zr2 C25 139.4(2) . . ? O6 Zr2 C26 119.1(2) . . ? O1 Zr2 C26 103.6(2) . . ? O2 Zr2 C26 89.70(17) . . ? O5 Zr2 C26 142.1(2) . . ? C25 Zr2 C26 33.5(3) . . ? O6 Zr2 C24 87.7(2) . . ? O1 Zr2 C24 132.91(18) . . ? O2 Zr2 C24 137.49(19) . . ? O5 Zr2 C24 106.4(2) . . ? C25 Zr2 C24 33.0(2) . . ? C26 Zr2 C24 54.7(2) . . ? O6 Zr2 C22 140.08(19) . . ? O1 Zr2 C22 85.18(17) . . ? O2 Zr2 C22 108.85(17) . . ? O5 Zr2 C22 110.2(2) . . ? C25 Zr2 C22 54.1(2) . . ? C26 Zr2 C22 32.0(2) . . ? C24 Zr2 C22 53.9(2) . . ? O6 Zr2 C23 117.2(2) . . ? O1 Zr2 C23 100.28(18) . . ? O2 Zr2 C23 140.36(18) . . ? O5 Zr2 C23 92.21(19) . . ? C25 Zr2 C23 54.1(2) . . ? C26 Zr2 C23 53.5(2) . . ? C24 Zr2 C23 32.6(2) . . ? C22 Zr2 C23 31.90(19) . . ? O6 Zr2 B1 113.1(2) . . ? O1 Zr2 B1 30.69(16) . . ? O2 Zr2 B1 92.41(16) . . ? O5 Zr2 B1 32.64(17) . . ? C25 Zr2 B1 152.5(2) . . ? C26 Zr2 B1 127.7(3) . . ? C24 Zr2 B1 126.6(2) . . ? C22 Zr2 B1 100.1(2) . . ? C23 Zr2 B1 99.3(2) . . ? O6 Zr2 Zr1 105.23(13) . . ? O1 Zr2 Zr1 38.18(9) . . ? O2 Zr2 Zr1 39.13(9) . . ? O5 Zr2 Zr1 79.43(11) . . ? C25 Zr2 Zr1 139.9(2) . . ? C26 Zr2 Zr1 113.01(16) . . ? C24 Zr2 Zr1 166.06(15) . . ? C22 Zr2 Zr1 112.38(13) . . ? C23 Zr2 Zr1 136.63(15) . . ? B1 Zr2 Zr1 53.29(13) . . ? B1 O1 Zr2 101.4(3) . . ? B1 O1 Zr1 100.8(3) . . ? Zr2 O1 Zr1 104.18(15) . . ? C1 O2 Zr2 117.4(3) . . ? C1 O2 Zr1 126.7(3) . . ? Zr2 O2 Zr1 102.44(14) . . ? C3 O3 Zr1 170.5(4) . . ? C5 O4 B1 121.5(5) . . ? C5 O4 Zr1 138.9(4) . . ? B1 O4 Zr1 97.1(3) . . ? C7 O5 B1 122.6(5) . . ? C7 O5 Zr2 136.9(4) . . ? B1 O5 Zr2 97.1(3) . . ? C9 O6 Zr2 175.1(6) . . ? O1 B1 O5 98.0(4) . . ? O1 B1 O4 98.8(4) . . ? O5 B1 O4 110.3(5) . . ? O1 B1 C11 120.2(6) . . ? O5 B1 C11 113.4(5) . . ? O4 B1 C11 114.2(5) . . ? O1 B1 Zr2 47.9(2) . . ? O5 B1 Zr2 50.3(2) . . ? O4 B1 Zr2 108.8(4) . . ? C11 B1 Zr2 136.9(5) . . ? O1 B1 Zr1 48.6(2) . . ? O5 B1 Zr1 111.6(4) . . ? O4 B1 Zr1 50.2(2) . . ? C11 B1 Zr1 134.9(4) . . ? Zr2 B1 Zr1 73.69(16) . . ? C2 C1 O2 114.2(7) . . ? O3 C3 C4 112.0(6) . . ? O4 C5 C6 111.9(18) . . ? O4 C5 C6' 110.1(16) . . ? C6 C5 C6' 25.4(19) . . ? O5 C7 C8 112.1(7) . . ? O6 C9 C10 104.0(7) . . ? C13 C12 C16 108.0(5) . . ? C13 C12 C17 125.3(5) . . ? C16 C12 C17 126.5(5) . . ? C13 C12 Zr1 74.0(3) . . ? C16 C12 Zr1 74.2(3) . . ? C17 C12 Zr1 122.2(4) . . ? C12 C13 C14 108.1(5) . . ? C12 C13 C18 124.5(5) . . ? C14 C13 C18 127.3(5) . . ? C12 C13 Zr1 73.2(3) . . ? C14 C13 Zr1 75.1(3) . . ? C18 C13 Zr1 121.3(4) . . ? C15 C14 C13 108.0(5) . . ? C15 C14 C19 125.8(5) . . ? C13 C14 C19 125.9(5) . . ? C15 C14 Zr1 73.8(3) . . ? C13 C14 Zr1 72.4(3) . . ? C19 C14 Zr1 124.6(4) . . ? C14 C15 C16 108.5(5) . . ? C14 C15 C20 125.3(6) . . ? C16 C15 C20 126.0(5) . . ? C14 C15 Zr1 73.9(3) . . ? C16 C15 Zr1 72.8(3) . . ? C20 C15 Zr1 123.9(4) . . ? C15 C16 C12 107.5(5) . . ? C15 C16 C21 125.3(6) . . ? C12 C16 C21 126.9(6) . . ? C15 C16 Zr1 74.7(3) . . ? C12 C16 Zr1 72.8(3) . . ? C21 C16 Zr1 122.2(4) . . ? C23 C22 C26 109.2(6) . . ? C23 C22 C27 124.3(7) . . ? C26 C22 C27 126.5(7) . . ? C23 C22 Zr2 74.1(3) . . ? C26 C22 Zr2 73.2(4) . . ? C27 C22 Zr2 121.6(4) . . ? C22 C23 C24 108.9(6) . . ? C22 C23 C28 126.0(7) . . ? C24 C23 C28 125.0(6) . . ? C22 C23 Zr2 74.0(3) . . ? C24 C23 Zr2 73.1(3) . . ? C28 C23 Zr2 123.0(5) . . ? C23 C24 C25 107.3(6) . . ? C23 C24 C29 127.6(7) . . ? C25 C24 C29 125.0(7) . . ? C23 C24 Zr2 74.3(3) . . ? C25 C24 Zr2 73.2(3) . . ? C29 C24 Zr2 120.7(4) . . ? C24 C25 C26 106.9(6) . . ? C24 C25 C30 125.3(9) . . ? C26 C25 C30 127.6(9) . . ? C24 C25 Zr2 73.8(3) . . ? C26 C25 Zr2 73.4(3) . . ? C30 C25 Zr2 121.6(5) . . ? C22 C26 C25 107.7(6) . . ? C22 C26 C31 126.8(9) . . ? C25 C26 C31 125.3(9) . . ? C22 C26 Zr2 74.7(3) . . ? C25 C26 Zr2 73.1(4) . . ? C31 C26 Zr2 122.1(4) . . ? C44 B2 C38 111.2(4) . . ? C44 B2 C32 112.8(5) . . ? C38 B2 C32 112.6(5) . . ? C37 C32 C33 114.2(6) . . ? C37 C32 B2 126.0(5) . . ? C33 C32 B2 119.7(6) . . ? F2 C33 C34 116.1(6) . . ? F2 C33 C32 119.9(5) . . ? C34 C33 C32 123.9(7) . . ? F3 C34 C35 120.7(6) . . ? F3 C34 C33 120.3(7) . . ? C35 C34 C33 118.9(6) . . ? F4 C35 C34 119.6(7) . . ? F4 C35 C36 120.3(7) . . ? C34 C35 C36 120.1(6) . . ? F5 C36 C35 119.8(6) . . ? F5 C36 C37 120.7(7) . . ? C35 C36 C37 119.4(7) . . ? F6 C37 C32 120.9(6) . . ? F6 C37 C36 115.7(6) . . ? C32 C37 C36 123.4(6) . . ? C43 C38 C39 113.0(5) . . ? C43 C38 B2 120.0(5) . . ? C39 C38 B2 126.9(5) . . ? F7 C39 C40 115.5(5) . . ? F7 C39 C38 120.4(5) . . ? C40 C39 C38 124.1(5) . . ? F8 C40 C41 120.2(5) . . ? F8 C40 C39 120.6(6) . . ? C41 C40 C39 119.2(6) . . ? F9 C41 C42 120.7(5) . . ? F9 C41 C40 120.0(6) . . ? C42 C41 C40 119.2(5) . . ? F10 C42 C41 119.6(5) . . ? F10 C42 C43 121.4(5) . . ? C41 C42 C43 119.0(5) . . ? F11 C43 C42 115.6(5) . . ? F11 C43 C38 118.9(5) . . ? C42 C43 C38 125.5(5) . . ? C45 C44 C49 113.9(5) . . ? C45 C44 B2 124.4(5) . . ? C49 C44 B2 121.7(5) . . ? F12 C45 C44 119.8(5) . . ? F12 C45 C46 115.8(6) . . ? C44 C45 C46 124.4(6) . . ? F13 C46 C47 119.5(6) . . ? F13 C46 C45 121.1(7) . . ? C47 C46 C45 119.4(6) . . ? F14 C47 C46 119.8(7) . . ? F14 C47 C48 120.6(6) . . ? C46 C47 C48 119.6(6) . . ? F15 C48 C47 119.8(6) . . ? F15 C48 C49 121.1(7) . . ? C47 C48 C49 119.1(6) . . ? F16 C49 C48 115.8(5) . . ? F16 C49 C44 120.6(5) . . ? C48 C49 C44 123.6(6) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 2.181 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.171