# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2012 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email m.tamm@tu-bs.de _publ_contact_author_name 'Matthias Tamm' loop_ _publ_author_name 'Matthias Tamm' 'Andreas Glockner' 'Constantin Daniliuc' P.Jones 'Yaofeng Chen' data_andyg65 _database_code_depnum_ccdc_archive 'CCDC 864982' #TrackingRef 'andyg65.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C13 H15 B Zr' _chemical_formula_weight 273.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' 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' '-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 8.1970(8) _cell_length_b 12.44180(14) _cell_length_c 21.9418(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2237.7(2) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 30547 _cell_measurement_theta_min 3.5495 _cell_measurement_theta_max 75.6144 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.622 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 7.693 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.43888 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 42506 _diffrn_reflns_av_R_equivalents 0.0349 _diffrn_reflns_av_sigmaI/netI 0.0097 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 4.03 _diffrn_reflns_theta_max 74.48 _reflns_number_total 2266 _reflns_number_gt 2186 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. The hydrogens of the seven-membered ring and of the six-membered ring were refined freely. ; _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^)+(0.0271P)^2^+1.3205P] 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 2266 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0187 _refine_ls_R_factor_gt 0.0180 _refine_ls_wR_factor_ref 0.0480 _refine_ls_wR_factor_gt 0.0475 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.088 _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 0.549515(16) 0.685405(10) 0.395483(5) 0.01464(7) Uani 1 1 d . . . B B 0.6014(2) 0.54070(14) 0.30695(8) 0.0175(3) Uani 1 1 d . . . C1 C 0.2719(2) 0.65005(15) 0.38718(8) 0.0230(3) Uani 1 1 d . . . H1 H 0.218(3) 0.6050(17) 0.3580(10) 0.031(5) Uiso 1 1 d . . . C2 C 0.2979(2) 0.75856(14) 0.36899(8) 0.0232(3) Uani 1 1 d . . . H2 H 0.261(3) 0.7757(17) 0.3302(10) 0.030(5) Uiso 1 1 d . . . C3 C 0.3881(2) 0.84074(14) 0.39881(7) 0.0232(4) Uani 1 1 d . . . H3 H 0.404(3) 0.9028(17) 0.3770(10) 0.027(5) Uiso 1 1 d . . . C4 C 0.4755(2) 0.83471(14) 0.45478(8) 0.0221(3) Uani 1 1 d . . . H4 H 0.541(2) 0.8966(16) 0.4666(9) 0.021(5) Uiso 1 1 d . . . C5 C 0.4915(2) 0.74535(14) 0.49491(7) 0.0203(3) Uani 1 1 d . . . H5 H 0.566(2) 0.7526(16) 0.5260(9) 0.020(5) Uiso 1 1 d . . . C6 C 0.4257(2) 0.64025(13) 0.48876(7) 0.0202(3) Uani 1 1 d . . . H6 H 0.465(2) 0.5895(17) 0.5191(10) 0.025(5) Uiso 1 1 d . . . C7 C 0.3284(2) 0.59741(13) 0.44068(7) 0.0217(3) Uani 1 1 d . . . H7 H 0.307(3) 0.5246(17) 0.4425(9) 0.028(5) Uiso 1 1 d . . . C8 C 0.61699(19) 0.65585(13) 0.28297(7) 0.0178(3) Uani 1 1 d . . . H8 H 0.549(2) 0.6837(13) 0.2505(10) 0.016(5) Uiso 1 1 d . . . C9 C 0.73289(19) 0.72740(12) 0.30660(7) 0.0184(3) Uani 1 1 d . . . H9 H 0.744(3) 0.7999(15) 0.2916(9) 0.024(5) Uiso 1 1 d . . . C10 C 0.83431(19) 0.69845(12) 0.35607(7) 0.0180(3) Uani 1 1 d . . . H10 H 0.906(3) 0.7491(17) 0.3718(10) 0.026(5) Uiso 1 1 d . . . C11 C 0.8236(2) 0.59557(13) 0.38276(7) 0.0182(3) Uani 1 1 d . . . H11 H 0.889(2) 0.5814(15) 0.4169(9) 0.020(5) Uiso 1 1 d . . . C12 C 0.71028(19) 0.51914(12) 0.36216(7) 0.0173(3) Uani 1 1 d . . . H12 H 0.710(3) 0.4512(16) 0.3850(9) 0.022(5) Uiso 1 1 d . . . C13 C 0.4801(2) 0.45530(13) 0.27826(8) 0.0239(3) Uani 1 1 d . . . H13A H 0.5335 0.4190 0.2440 0.036 Uiso 1 1 calc R . . H13B H 0.3817 0.4920 0.2638 0.036 Uiso 1 1 calc R . . H13C H 0.4503 0.4021 0.3093 0.036 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 0.01639(10) 0.01578(9) 0.01176(9) -0.00077(4) 0.00147(4) 0.00146(4) B 0.0175(8) 0.0195(8) 0.0153(8) -0.0026(6) 0.0015(6) 0.0023(7) C1 0.0157(8) 0.0307(9) 0.0226(8) -0.0069(7) -0.0009(6) -0.0006(7) C2 0.0209(8) 0.0319(9) 0.0169(7) 0.0002(6) -0.0015(6) 0.0094(7) C3 0.0295(10) 0.0184(7) 0.0215(8) 0.0026(6) 0.0045(7) 0.0076(7) C4 0.0284(9) 0.0182(7) 0.0197(8) -0.0047(6) 0.0055(7) 0.0000(7) C5 0.0228(8) 0.0256(8) 0.0125(7) -0.0041(6) 0.0012(6) 0.0008(7) C6 0.0236(8) 0.0210(8) 0.0158(7) 0.0039(6) 0.0051(6) 0.0023(6) C7 0.0203(7) 0.0203(8) 0.0245(8) -0.0015(6) 0.0054(6) -0.0023(6) C8 0.0199(7) 0.0223(7) 0.0114(7) 0.0003(6) 0.0007(6) 0.0029(6) C9 0.0203(7) 0.0187(7) 0.0162(7) 0.0017(6) 0.0040(6) 0.0008(6) C10 0.0165(7) 0.0205(7) 0.0171(7) -0.0021(6) 0.0016(6) -0.0017(6) C11 0.0177(7) 0.0225(8) 0.0144(7) -0.0012(6) -0.0008(6) 0.0048(6) C12 0.0205(7) 0.0158(7) 0.0155(7) -0.0009(6) 0.0011(6) 0.0028(6) C13 0.0263(8) 0.0214(8) 0.0239(8) -0.0038(6) -0.0050(7) 0.0002(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr C1 2.3249(17) . ? Zr C2 2.3283(16) . ? Zr C7 2.3383(16) . ? Zr C3 2.3431(17) . ? Zr C4 2.3476(16) . ? Zr C6 2.3524(16) . ? Zr C5 2.3540(15) . ? Zr C10 2.4948(16) . ? Zr C9 2.5172(15) . ? Zr C11 2.5252(16) . ? Zr C8 2.5566(15) . ? Zr C12 2.5594(15) . ? B C12 1.528(2) . ? B C8 1.532(2) . ? B C13 1.585(2) . ? C1 C7 1.422(2) . ? C1 C2 1.424(3) . ? C2 C3 1.422(3) . ? C3 C4 1.424(2) . ? C4 C5 1.424(2) . ? C5 C6 1.421(2) . ? C6 C7 1.426(2) . ? C8 C9 1.401(2) . ? C9 C10 1.414(2) . ? C10 C11 1.410(2) . ? C11 C12 1.404(2) . ? 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 C1 Zr C2 35.64(6) . . ? C1 Zr C7 35.50(6) . . ? C2 Zr C7 66.56(6) . . ? C1 Zr C3 66.79(7) . . ? C2 Zr C3 35.43(6) . . ? C7 Zr C3 86.30(6) . . ? C1 Zr C4 86.58(6) . . ? C2 Zr C4 66.44(6) . . ? C7 Zr C4 86.29(6) . . ? C3 Zr C4 35.34(6) . . ? C1 Zr C6 66.47(6) . . ? C2 Zr C6 85.90(6) . . ? C7 Zr C6 35.40(6) . . ? C3 Zr C6 85.78(6) . . ? C4 Zr C6 66.13(6) . . ? C1 Zr C5 86.27(6) . . ? C2 Zr C5 85.91(6) . . ? C7 Zr C5 66.35(6) . . ? C3 Zr C5 66.16(6) . . ? C4 Zr C5 35.27(6) . . ? C6 Zr C5 35.15(6) . . ? C1 Zr C10 154.30(5) . . ? C2 Zr C10 135.81(6) . . ? C7 Zr C10 154.53(5) . . ? C3 Zr C10 119.04(6) . . ? C4 Zr C10 112.48(6) . . ? C6 Zr C10 136.11(6) . . ? C5 Zr C10 119.31(6) . . ? C1 Zr C9 124.27(6) . . ? C2 Zr C9 104.74(6) . . ? C7 Zr C9 152.71(5) . . ? C3 Zr C9 100.96(6) . . ? C4 Zr C9 114.80(6) . . ? C6 Zr C9 168.88(6) . . ? C5 Zr C9 140.61(6) . . ? C10 Zr C9 32.77(5) . . ? C1 Zr C11 141.13(6) . . ? C2 Zr C11 159.03(5) . . ? C7 Zr C11 121.97(6) . . ? C3 Zr C11 150.56(6) . . ? C4 Zr C11 129.90(6) . . ? C6 Zr C11 111.98(5) . . ? C5 Zr C11 114.98(6) . . ? C10 Zr C11 32.63(5) . . ? C9 Zr C11 58.32(5) . . ? C1 Zr C8 96.25(5) . . ? C2 Zr C8 90.39(5) . . ? C7 Zr C8 120.66(5) . . ? C3 Zr C8 105.72(5) . . ? C4 Zr C8 134.82(6) . . ? C6 Zr C8 154.04(6) . . ? C5 Zr C8 169.79(6) . . ? C10 Zr C8 58.14(5) . . ? C9 Zr C8 32.06(5) . . ? C11 Zr C8 68.72(5) . . ? C1 Zr C12 109.19(6) . . ? C2 Zr C12 134.49(6) . . ? C7 Zr C12 98.15(5) . . ? C3 Zr C12 165.07(5) . . ? C4 Zr C12 158.57(6) . . ? C6 Zr C12 106.12(5) . . ? C5 Zr C12 128.67(5) . . ? C10 Zr C12 58.11(5) . . ? C9 Zr C12 68.84(5) . . ? C11 Zr C12 32.06(5) . . ? C8 Zr C12 59.77(5) . . ? C12 B C8 112.83(14) . . ? C12 B C13 124.27(14) . . ? C8 B C13 122.87(14) . . ? C12 B Zr 68.68(8) . . ? C8 B Zr 68.54(8) . . ? C13 B Zr 129.62(11) . . ? C7 C1 C2 128.28(16) . . ? C7 C1 Zr 72.76(10) . . ? C2 C1 Zr 72.31(10) . . ? C3 C2 C1 129.10(16) . . ? C3 C2 Zr 72.85(10) . . ? C1 C2 Zr 72.05(9) . . ? C2 C3 C4 128.39(16) . . ? C2 C3 Zr 71.71(10) . . ? C4 C3 Zr 72.50(10) . . ? C3 C4 C5 128.37(16) . . ? C3 C4 Zr 72.16(10) . . ? C5 C4 Zr 72.61(9) . . ? C6 C5 C4 128.66(16) . . ? C6 C5 Zr 72.37(9) . . ? C4 C5 Zr 72.12(9) . . ? C5 C6 C7 128.80(15) . . ? C5 C6 Zr 72.49(9) . . ? C7 C6 Zr 71.76(9) . . ? C1 C7 C6 128.38(15) . . ? C1 C7 Zr 71.74(10) . . ? C6 C7 Zr 72.84(9) . . ? C9 C8 B 121.57(14) . . ? C9 C8 Zr 72.42(8) . . ? B C8 Zr 77.57(9) . . ? C8 C9 C10 121.39(14) . . ? C8 C9 Zr 75.52(9) . . ? C10 C9 Zr 72.75(9) . . ? C11 C10 C9 120.89(14) . . ? C11 C10 Zr 74.87(9) . . ? C9 C10 Zr 74.48(9) . . ? C12 C11 C10 121.47(14) . . ? C12 C11 Zr 75.32(9) . . ? C10 C11 Zr 72.50(9) . . ? C11 C12 B 121.50(14) . . ? C11 C12 Zr 72.63(9) . . ? B C12 Zr 77.53(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Zr B C12 -129.31(10) . . . . ? C2 Zr B C12 -162.13(9) . . . . ? C7 Zr B C12 -94.72(9) . . . . ? C3 Zr B C12 174.31(9) . . . . ? C4 Zr B C12 163.1(2) . . . . ? C6 Zr B C12 -68.78(11) . . . . ? C5 Zr B C12 -52.42(18) . . . . ? C10 Zr B C12 63.43(9) . . . . ? C9 Zr B C12 98.24(10) . . . . ? C11 Zr B C12 28.82(9) . . . . ? C8 Zr B C12 126.94(13) . . . . ? C1 Zr B C8 103.75(10) . . . . ? C2 Zr B C8 70.93(10) . . . . ? C7 Zr B C8 138.34(9) . . . . ? C3 Zr B C8 47.37(12) . . . . ? C4 Zr B C8 36.2(3) . . . . ? C6 Zr B C8 164.28(9) . . . . ? C5 Zr B C8 -179.36(13) . . . . ? C10 Zr B C8 -63.51(9) . . . . ? C9 Zr B C8 -28.70(9) . . . . ? C11 Zr B C8 -98.12(10) . . . . ? C12 Zr B C8 -126.94(14) . . . . ? C1 Zr B C13 -11.82(14) . . . . ? C2 Zr B C13 -44.64(15) . . . . ? C7 Zr B C13 22.77(15) . . . . ? C3 Zr B C13 -68.20(16) . . . . ? C4 Zr B C13 -79.4(3) . . . . ? C6 Zr B C13 48.71(16) . . . . ? C5 Zr B C13 65.1(2) . . . . ? C10 Zr B C13 -179.08(15) . . . . ? C9 Zr B C13 -144.27(16) . . . . ? C11 Zr B C13 146.31(16) . . . . ? C8 Zr B C13 -115.57(18) . . . . ? C12 Zr B C13 117.49(18) . . . . ? C2 Zr C1 C7 -141.24(15) . . . . ? C3 Zr C1 C7 -118.68(11) . . . . ? C4 Zr C1 C7 -88.40(10) . . . . ? C6 Zr C1 C7 -22.98(9) . . . . ? C5 Zr C1 C7 -53.06(10) . . . . ? C10 Zr C1 C7 132.23(12) . . . . ? C9 Zr C1 C7 153.72(9) . . . . ? C11 Zr C1 C7 73.35(12) . . . . ? C8 Zr C1 C7 136.87(10) . . . . ? C12 Zr C1 C7 76.75(10) . . . . ? C7 Zr C1 C2 141.24(15) . . . . ? C3 Zr C1 C2 22.56(9) . . . . ? C4 Zr C1 C2 52.84(10) . . . . ? C6 Zr C1 C2 118.26(11) . . . . ? C5 Zr C1 C2 88.18(10) . . . . ? C10 Zr C1 C2 -86.52(16) . . . . ? C9 Zr C1 C2 -65.04(11) . . . . ? C11 Zr C1 C2 -145.40(10) . . . . ? C8 Zr C1 C2 -81.89(10) . . . . ? C12 Zr C1 C2 -142.01(9) . . . . ? C7 C1 C2 C3 1.1(3) . . . . ? Zr C1 C2 C3 -48.49(17) . . . . ? C7 C1 C2 Zr 49.61(17) . . . . ? C1 Zr C2 C3 142.54(15) . . . . ? C7 Zr C2 C3 119.20(11) . . . . ? C4 Zr C2 C3 22.76(9) . . . . ? C6 Zr C2 C3 88.48(10) . . . . ? C5 Zr C2 C3 53.24(10) . . . . ? C10 Zr C2 C3 -75.85(12) . . . . ? C9 Zr C2 C3 -88.24(10) . . . . ? C11 Zr C2 C3 -122.04(16) . . . . ? C8 Zr C2 C3 -117.24(10) . . . . ? C12 Zr C2 C3 -162.88(9) . . . . ? C7 Zr C2 C1 -23.34(9) . . . . ? C3 Zr C2 C1 -142.54(15) . . . . ? C4 Zr C2 C1 -119.78(11) . . . . ? C6 Zr C2 C1 -54.06(10) . . . . ? C5 Zr C2 C1 -89.30(10) . . . . ? C10 Zr C2 C1 141.61(10) . . . . ? C9 Zr C2 C1 129.22(9) . . . . ? C11 Zr C2 C1 95.42(18) . . . . ? C8 Zr C2 C1 100.22(10) . . . . ? C12 Zr C2 C1 54.58(12) . . . . ? C1 C2 C3 C4 0.0(3) . . . . ? Zr C2 C3 C4 -48.25(17) . . . . ? C1 C2 C3 Zr 48.21(17) . . . . ? C1 Zr C3 C2 -22.68(10) . . . . ? C7 Zr C3 C2 -53.38(10) . . . . ? C4 Zr C3 C2 -142.18(16) . . . . ? C6 Zr C3 C2 -88.86(10) . . . . ? C5 Zr C3 C2 -119.12(11) . . . . ? C10 Zr C3 C2 129.37(10) . . . . ? C9 Zr C3 C2 100.07(10) . . . . ? C11 Zr C3 C2 141.88(11) . . . . ? C8 Zr C3 C2 67.46(10) . . . . ? C12 Zr C3 C2 54.6(3) . . . . ? C1 Zr C3 C4 119.50(11) . . . . ? C2 Zr C3 C4 142.18(16) . . . . ? C7 Zr C3 C4 88.80(11) . . . . ? C6 Zr C3 C4 53.32(11) . . . . ? C5 Zr C3 C4 23.06(10) . . . . ? C10 Zr C3 C4 -88.45(11) . . . . ? C9 Zr C3 C4 -117.75(10) . . . . ? C11 Zr C3 C4 -75.94(14) . . . . ? C8 Zr C3 C4 -150.36(10) . . . . ? C12 Zr C3 C4 -163.2(2) . . . . ? C2 C3 C4 C5 -1.1(3) . . . . ? Zr C3 C4 C5 -49.06(17) . . . . ? C2 C3 C4 Zr 47.97(17) . . . . ? C1 Zr C4 C3 -53.26(11) . . . . ? C2 Zr C4 C3 -22.82(10) . . . . ? C7 Zr C4 C3 -88.83(11) . . . . ? C6 Zr C4 C3 -119.00(12) . . . . ? C5 Zr C4 C3 -141.64(16) . . . . ? C10 Zr C4 C3 108.94(11) . . . . ? C9 Zr C4 C3 73.16(11) . . . . ? C11 Zr C4 C3 141.58(10) . . . . ? C8 Zr C4 C3 42.16(14) . . . . ? C12 Zr C4 C3 168.25(14) . . . . ? C1 Zr C4 C5 88.38(11) . . . . ? C2 Zr C4 C5 118.82(12) . . . . ? C7 Zr C4 C5 52.81(11) . . . . ? C3 Zr C4 C5 141.64(16) . . . . ? C6 Zr C4 C5 22.64(10) . . . . ? C10 Zr C4 C5 -109.42(10) . . . . ? C9 Zr C4 C5 -145.20(10) . . . . ? C11 Zr C4 C5 -76.78(12) . . . . ? C8 Zr C4 C5 -176.21(9) . . . . ? C12 Zr C4 C5 -50.1(2) . . . . ? C3 C4 C5 C6 0.6(3) . . . . ? Zr C4 C5 C6 -48.26(17) . . . . ? C3 C4 C5 Zr 48.90(17) . . . . ? C1 Zr C5 C6 52.96(10) . . . . ? C2 Zr C5 C6 88.68(10) . . . . ? C7 Zr C5 C6 22.52(10) . . . . ? C3 Zr C5 C6 119.20(12) . . . . ? C4 Zr C5 C6 142.31(16) . . . . ? C10 Zr C5 C6 -129.67(10) . . . . ? C9 Zr C5 C6 -162.96(9) . . . . ? C11 Zr C5 C6 -93.18(11) . . . . ? C8 Zr C5 C6 157.7(3) . . . . ? C12 Zr C5 C6 -58.73(12) . . . . ? C1 Zr C5 C4 -89.35(11) . . . . ? C2 Zr C5 C4 -53.63(11) . . . . ? C7 Zr C5 C4 -119.79(11) . . . . ? C3 Zr C5 C4 -23.11(10) . . . . ? C6 Zr C5 C4 -142.31(16) . . . . ? C10 Zr C5 C4 88.02(11) . . . . ? C9 Zr C5 C4 54.73(14) . . . . ? C11 Zr C5 C4 124.51(10) . . . . ? C8 Zr C5 C4 15.4(4) . . . . ? C12 Zr C5 C4 158.96(10) . . . . ? C4 C5 C6 C7 0.6(3) . . . . ? Zr C5 C6 C7 -47.56(16) . . . . ? C4 C5 C6 Zr 48.17(17) . . . . ? C1 Zr C6 C5 -119.68(11) . . . . ? C2 Zr C6 C5 -88.72(10) . . . . ? C7 Zr C6 C5 -142.73(15) . . . . ? C3 Zr C6 C5 -53.19(11) . . . . ? C4 Zr C6 C5 -22.71(10) . . . . ? C10 Zr C6 C5 75.52(12) . . . . ? C9 Zr C6 C5 74.6(3) . . . . ? C11 Zr C6 C5 102.59(10) . . . . ? C8 Zr C6 C5 -171.15(11) . . . . ? C12 Zr C6 C5 136.00(10) . . . . ? C1 Zr C6 C7 23.05(9) . . . . ? C2 Zr C6 C7 54.01(10) . . . . ? C3 Zr C6 C7 89.54(10) . . . . ? C4 Zr C6 C7 120.02(11) . . . . ? C5 Zr C6 C7 142.73(15) . . . . ? C10 Zr C6 C7 -141.75(9) . . . . ? C9 Zr C6 C7 -142.7(3) . . . . ? C11 Zr C6 C7 -114.68(10) . . . . ? C8 Zr C6 C7 -28.42(17) . . . . ? C12 Zr C6 C7 -81.27(10) . . . . ? C2 C1 C7 C6 -0.6(3) . . . . ? Zr C1 C7 C6 48.88(16) . . . . ? C2 C1 C7 Zr -49.45(17) . . . . ? C5 C6 C7 C1 -0.7(3) . . . . ? Zr C6 C7 C1 -48.48(16) . . . . ? C5 C6 C7 Zr 47.82(16) . . . . ? C2 Zr C7 C1 23.43(10) . . . . ? C3 Zr C7 C1 53.90(10) . . . . ? C4 Zr C7 C1 89.31(10) . . . . ? C6 Zr C7 C1 141.82(15) . . . . ? C5 Zr C7 C1 119.45(11) . . . . ? C10 Zr C7 C1 -131.68(13) . . . . ? C9 Zr C7 C1 -52.95(16) . . . . ? C11 Zr C7 C1 -134.87(10) . . . . ? C8 Zr C7 C1 -52.19(11) . . . . ? C12 Zr C7 C1 -111.77(10) . . . . ? C1 Zr C7 C6 -141.82(15) . . . . ? C2 Zr C7 C6 -118.40(11) . . . . ? C3 Zr C7 C6 -87.92(10) . . . . ? C4 Zr C7 C6 -52.51(10) . . . . ? C5 Zr C7 C6 -22.37(9) . . . . ? C10 Zr C7 C6 86.49(15) . . . . ? C9 Zr C7 C6 165.23(11) . . . . ? C11 Zr C7 C6 83.31(10) . . . . ? C8 Zr C7 C6 165.98(9) . . . . ? C12 Zr C7 C6 106.41(9) . . . . ? C12 B C8 C9 6.2(2) . . . . ? C13 B C8 C9 -175.71(15) . . . . ? Zr B C8 C9 60.11(13) . . . . ? C12 B C8 Zr -53.89(11) . . . . ? C13 B C8 Zr 124.18(15) . . . . ? C1 Zr C8 C9 153.17(10) . . . . ? C2 Zr C8 C9 117.94(10) . . . . ? C7 Zr C8 C9 -179.34(9) . . . . ? C3 Zr C8 C9 85.56(10) . . . . ? C4 Zr C8 C9 61.78(12) . . . . ? C6 Zr C8 C9 -160.65(12) . . . . ? C5 Zr C8 C9 49.3(3) . . . . ? C10 Zr C8 C9 -29.20(9) . . . . ? C11 Zr C8 C9 -63.90(9) . . . . ? C12 Zr C8 C9 -98.24(10) . . . . ? C1 Zr C8 B -77.62(10) . . . . ? C2 Zr C8 B -112.85(10) . . . . ? C7 Zr C8 B -50.13(11) . . . . ? C3 Zr C8 B -145.23(10) . . . . ? C4 Zr C8 B -169.01(10) . . . . ? C6 Zr C8 B -31.44(17) . . . . ? C5 Zr C8 B 178.5(3) . . . . ? C10 Zr C8 B 100.01(10) . . . . ? C9 Zr C8 B 129.21(14) . . . . ? C11 Zr C8 B 65.31(9) . . . . ? C12 Zr C8 B 30.97(9) . . . . ? B C8 C9 C10 -3.7(2) . . . . ? Zr C8 C9 C10 58.91(13) . . . . ? B C8 C9 Zr -62.64(13) . . . . ? C1 Zr C9 C8 -32.88(11) . . . . ? C2 Zr C9 C8 -65.99(10) . . . . ? C7 Zr C9 C8 1.23(17) . . . . ? C3 Zr C9 C8 -102.17(10) . . . . ? C4 Zr C9 C8 -136.49(9) . . . . ? C6 Zr C9 C8 131.2(3) . . . . ? C5 Zr C9 C8 -167.77(9) . . . . ? C10 Zr C9 C8 130.05(14) . . . . ? C11 Zr C9 C8 100.48(10) . . . . ? C12 Zr C9 C8 66.48(9) . . . . ? C1 Zr C9 C10 -162.93(9) . . . . ? C2 Zr C9 C10 163.96(9) . . . . ? C7 Zr C9 C10 -128.82(12) . . . . ? C3 Zr C9 C10 127.78(9) . . . . ? C4 Zr C9 C10 93.46(10) . . . . ? C6 Zr C9 C10 1.2(3) . . . . ? C5 Zr C9 C10 62.18(12) . . . . ? C11 Zr C9 C10 -29.57(9) . . . . ? C8 Zr C9 C10 -130.05(14) . . . . ? C12 Zr C9 C10 -63.57(9) . . . . ? C8 C9 C10 C11 0.9(2) . . . . ? Zr C9 C10 C11 61.20(13) . . . . ? C8 C9 C10 Zr -60.25(13) . . . . ? C1 Zr C10 C11 -94.83(15) . . . . ? C2 Zr C10 C11 -151.37(9) . . . . ? C7 Zr C10 C11 -5.01(18) . . . . ? C3 Zr C10 C11 168.61(9) . . . . ? C4 Zr C10 C11 129.87(9) . . . . ? C6 Zr C10 C11 51.50(12) . . . . ? C5 Zr C10 C11 91.23(10) . . . . ? C9 Zr C10 C11 -128.83(13) . . . . ? C8 Zr C10 C11 -100.26(10) . . . . ? C12 Zr C10 C11 -28.41(9) . . . . ? C1 Zr C10 C9 34.00(17) . . . . ? C2 Zr C10 C9 -22.54(13) . . . . ? C7 Zr C10 C9 123.82(13) . . . . ? C3 Zr C10 C9 -62.56(10) . . . . ? C4 Zr C10 C9 -101.29(10) . . . . ? C6 Zr C10 C9 -179.67(9) . . . . ? C5 Zr C10 C9 -139.93(9) . . . . ? C11 Zr C10 C9 128.83(13) . . . . ? C8 Zr C10 C9 28.58(8) . . . . ? C12 Zr C10 C9 100.42(10) . . . . ? C9 C10 C11 C12 -1.3(2) . . . . ? Zr C10 C11 C12 59.70(14) . . . . ? C9 C10 C11 Zr -61.01(13) . . . . ? C1 Zr C11 C12 6.05(14) . . . . ? C2 Zr C11 C12 -61.51(19) . . . . ? C7 Zr C11 C12 47.03(11) . . . . ? C3 Zr C11 C12 -151.00(11) . . . . ? C4 Zr C11 C12 162.01(9) . . . . ? C6 Zr C11 C12 85.38(10) . . . . ? C5 Zr C11 C12 123.68(9) . . . . ? C10 Zr C11 C12 -130.43(14) . . . . ? C9 Zr C11 C12 -100.73(10) . . . . ? C8 Zr C11 C12 -66.67(9) . . . . ? C1 Zr C11 C10 136.48(10) . . . . ? C2 Zr C11 C10 68.92(19) . . . . ? C7 Zr C11 C10 177.46(9) . . . . ? C3 Zr C11 C10 -20.57(15) . . . . ? C4 Zr C11 C10 -67.57(11) . . . . ? C6 Zr C11 C10 -144.19(9) . . . . ? C5 Zr C11 C10 -105.89(10) . . . . ? C9 Zr C11 C10 29.70(9) . . . . ? C8 Zr C11 C10 63.76(9) . . . . ? C12 Zr C11 C10 130.43(14) . . . . ? C10 C11 C12 B 4.5(2) . . . . ? Zr C11 C12 B 62.80(13) . . . . ? C10 C11 C12 Zr -58.34(13) . . . . ? C8 B C12 C11 -6.6(2) . . . . ? C13 B C12 C11 175.39(15) . . . . ? Zr B C12 C11 -60.38(13) . . . . ? C8 B C12 Zr 53.82(11) . . . . ? C13 B C12 Zr -124.22(15) . . . . ? C1 Zr C12 C11 -175.99(9) . . . . ? C2 Zr C12 C11 153.83(9) . . . . ? C7 Zr C12 C11 -141.16(10) . . . . ? C3 Zr C12 C11 112.3(2) . . . . ? C4 Zr C12 C11 -40.44(19) . . . . ? C6 Zr C12 C11 -105.83(10) . . . . ? C5 Zr C12 C11 -75.02(11) . . . . ? C10 Zr C12 C11 28.90(9) . . . . ? C9 Zr C12 C11 63.71(9) . . . . ? C8 Zr C12 C11 97.99(10) . . . . ? C1 Zr C12 B 54.97(10) . . . . ? C2 Zr C12 B 24.79(12) . . . . ? C7 Zr C12 B 89.80(10) . . . . ? C3 Zr C12 B -16.7(3) . . . . ? C4 Zr C12 B -169.49(14) . . . . ? C6 Zr C12 B 125.13(9) . . . . ? C5 Zr C12 B 155.94(9) . . . . ? C10 Zr C12 B -100.14(10) . . . . ? C9 Zr C12 B -65.33(9) . . . . ? C11 Zr C12 B -129.04(14) . . . . ? C8 Zr C12 B -31.05(9) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 74.48 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.328 _refine_diff_density_min -0.471 _refine_diff_density_rms 0.057 # Attachment 'andyg67.cif' data_andyg67 _database_code_depnum_ccdc_archive 'CCDC 864983' #TrackingRef 'andyg67.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H25 B N2 Zr' _chemical_formula_weight 395.45 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' N N 0.0061 0.0033 '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 'P 21 21 21' 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 10.5081(2) _cell_length_b 11.2379(4) _cell_length_c 14.8903(4) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1758.38(9) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 16849 _cell_measurement_theta_min 2.2659 _cell_measurement_theta_max 29.2318 _exptl_crystal_description needle _exptl_crystal_colour orange _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.494 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.628 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.97637 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Xcalibur, Eos' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1419 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 69260 _diffrn_reflns_av_R_equivalents 0.0617 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 27.87 _reflns_number_total 4176 _reflns_number_gt 3756 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET) (compiled Jan 20 2011,15:58:25) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. The hydrogens of the seven-membered ring and of the six-membered ring were refined freely. ; _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^)+(0.0157P)^2^+0.7788P] 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 0.02(4) _refine_ls_number_reflns 4176 _refine_ls_number_parameters 268 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0298 _refine_ls_R_factor_gt 0.0236 _refine_ls_wR_factor_ref 0.0466 _refine_ls_wR_factor_gt 0.0449 _refine_ls_goodness_of_fit_ref 1.060 _refine_ls_restrained_S_all 1.060 _refine_ls_shift/su_max 0.002 _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 0.771173(14) 0.50169(2) 0.217572(10) 0.00912(5) Uani 1 1 d . . . B B 1.0298(2) 0.4812(2) 0.19198(14) 0.0132(6) Uani 1 1 d . . . N1 N 0.58948(12) 0.4993(3) 0.11698(9) 0.0117(3) Uani 1 1 d . . . N2 N 0.23101(14) 0.4939(2) -0.00832(10) 0.0139(3) Uani 1 1 d . . . C1 C 0.57718(17) 0.5006(4) 0.30959(11) 0.0195(4) Uani 1 1 d . . . H1 H 0.4938(19) 0.507(3) 0.2880(13) 0.022(5) Uiso 1 1 d . . . C2 C 0.6247(3) 0.3824(3) 0.30621(18) 0.0174(6) Uani 1 1 d . . . H2 H 0.570(3) 0.330(2) 0.2855(19) 0.026(7) Uiso 1 1 d . . . C3 C 0.7512(3) 0.3419(2) 0.31985(15) 0.0190(6) Uani 1 1 d . . . H3 H 0.766(2) 0.265(2) 0.3110(16) 0.018(6) Uiso 1 1 d . . . C4 C 0.8552(3) 0.4113(2) 0.35023(16) 0.0178(5) Uani 1 1 d . . . H4 H 0.932(2) 0.373(2) 0.3590(16) 0.020(6) Uiso 1 1 d . . . C5 C 0.8617(3) 0.5345(2) 0.36497(16) 0.0170(6) Uani 1 1 d . . . H5 H 0.938(2) 0.566(2) 0.3760(17) 0.021(7) Uiso 1 1 d . . . C6 C 0.7713(3) 0.6244(2) 0.34592(15) 0.0175(5) Uani 1 1 d . . . H6 H 0.799(2) 0.706(2) 0.3504(16) 0.018(6) Uiso 1 1 d . . . C7 C 0.6421(3) 0.6088(3) 0.32229(18) 0.0186(6) Uani 1 1 d . . . H7 H 0.592(3) 0.677(2) 0.3120(18) 0.027(8) Uiso 1 1 d . . . C8 C 0.9563(2) 0.3960(2) 0.13221(16) 0.0149(5) Uani 1 1 d . . . H8 H 0.967(2) 0.316(2) 0.1337(15) 0.014(6) Uiso 1 1 d . . . C9 C 0.8715(3) 0.4379(3) 0.06767(18) 0.0151(6) Uani 1 1 d . . . H9 H 0.827(3) 0.387(2) 0.0305(17) 0.029(8) Uiso 1 1 d . . . C10 C 0.8429(3) 0.5599(3) 0.05914(18) 0.0147(6) Uani 1 1 d . . . H10 H 0.789(2) 0.5845(19) 0.0186(14) 0.008(6) Uiso 1 1 d . . . C11 C 0.8982(2) 0.6443(2) 0.11684(15) 0.0142(4) Uani 1 1 d . . . H11 H 0.875(2) 0.725(2) 0.1101(16) 0.021(6) Uiso 1 1 d . . . C12 C 0.9841(2) 0.6098(2) 0.18373(15) 0.0136(4) Uani 1 1 d . . . H12 H 1.013(2) 0.671(2) 0.2223(16) 0.018(6) Uiso 1 1 d . . . C13 C 1.1469(2) 0.4458(2) 0.25429(15) 0.0195(5) Uani 1 1 d . . . H13A H 1.2267 0.4665 0.2240 0.029 Uiso 1 1 calc R . . H13B H 1.1449 0.3600 0.2660 0.029 Uiso 1 1 calc R . . H13C H 1.1412 0.4891 0.3113 0.029 Uiso 1 1 calc R . . C14 C 0.5326(3) 0.3986(2) 0.09052(18) 0.0135(6) Uani 1 1 d . . . H14 H 0.5761 0.3260 0.1018 0.016 Uiso 1 1 calc R . . C15 C 0.4175(3) 0.3914(2) 0.04883(18) 0.0132(6) Uani 1 1 d . . . H15 H 0.3842 0.3160 0.0319 0.016 Uiso 1 1 calc R . . C16 C 0.34765(15) 0.4961(3) 0.03071(10) 0.0115(3) Uani 1 1 d . . . C17 C 0.4074(3) 0.6037(2) 0.05629(17) 0.0122(6) Uani 1 1 d . . . H17 H 0.3669 0.6779 0.0453 0.015 Uiso 1 1 calc R . . C18 C 0.5249(3) 0.6003(2) 0.09729(17) 0.0122(6) Uani 1 1 d . . . H18 H 0.5633 0.6740 0.1129 0.015 Uiso 1 1 calc R . . C19 C 0.1793(3) 0.3826(2) -0.04144(17) 0.0168(6) Uani 1 1 d . . . H19A H 0.2360 0.3500 -0.0876 0.025 Uiso 1 1 calc R . . H19B H 0.0950 0.3967 -0.0674 0.025 Uiso 1 1 calc R . . H19C H 0.1721 0.3259 0.0083 0.025 Uiso 1 1 calc R . . C20 C 0.1630(3) 0.6036(2) -0.02880(17) 0.0148(5) Uani 1 1 d . . . H20A H 0.1674 0.6573 0.0230 0.022 Uiso 1 1 calc R . . H20B H 0.0738 0.5853 -0.0421 0.022 Uiso 1 1 calc R . . H20C H 0.2021 0.6421 -0.0810 0.022 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 0.00888(8) 0.01109(8) 0.00739(7) -0.00003(12) 0.00049(6) -0.00020(14) B 0.0103(10) 0.0185(17) 0.0108(9) 0.0022(9) 0.0019(7) 0.0005(10) N1 0.0113(7) 0.0135(7) 0.0103(7) -0.0017(12) 0.0002(5) -0.0006(15) N2 0.0122(7) 0.0137(8) 0.0160(7) 0.0009(10) -0.0027(6) 0.0008(13) C1 0.0113(9) 0.0359(11) 0.0113(8) -0.0005(17) 0.0037(6) 0.004(2) C2 0.0172(14) 0.0223(14) 0.0128(12) 0.0027(10) 0.0021(10) -0.0108(11) C3 0.0267(16) 0.0173(12) 0.0130(11) 0.0033(9) 0.0065(10) 0.0004(11) C4 0.0161(13) 0.0263(14) 0.0110(11) 0.0067(11) 0.0015(10) 0.0078(12) C5 0.0131(11) 0.0302(17) 0.0076(10) -0.0018(9) -0.0012(8) -0.0039(10) C6 0.0240(13) 0.0192(12) 0.0092(10) -0.0041(9) 0.0035(11) -0.0045(11) C7 0.0223(14) 0.0230(14) 0.0104(12) -0.0013(10) 0.0040(10) 0.0095(12) C8 0.0139(12) 0.0160(12) 0.0148(12) -0.0025(10) 0.0039(10) 0.0022(10) C9 0.0120(14) 0.0244(14) 0.0091(12) -0.0065(10) 0.0031(10) -0.0041(10) C10 0.0123(13) 0.0248(14) 0.0071(12) 0.0030(10) -0.0012(10) -0.0002(10) C11 0.0139(11) 0.0150(12) 0.0138(11) 0.0036(9) 0.0038(9) -0.0024(9) C12 0.0105(11) 0.0175(12) 0.0127(10) 0.0013(9) 0.0019(9) -0.0046(9) C13 0.0130(11) 0.0262(12) 0.0193(11) 0.0017(9) -0.0023(9) 0.0013(9) C14 0.0133(14) 0.0143(13) 0.0129(13) 0.0006(11) 0.0001(11) 0.0022(12) C15 0.0166(14) 0.0106(12) 0.0124(12) -0.0005(11) -0.0013(10) -0.0003(11) C16 0.0111(8) 0.0150(9) 0.0085(7) -0.0028(14) 0.0019(6) 0.0002(15) C17 0.0119(13) 0.0121(12) 0.0126(12) 0.0027(11) 0.0037(10) 0.0020(10) C18 0.0162(14) 0.0090(12) 0.0115(13) 0.0006(11) 0.0018(11) -0.0018(12) C19 0.0125(13) 0.0192(13) 0.0187(13) -0.0003(10) -0.0037(10) -0.0061(11) C20 0.0122(12) 0.0168(12) 0.0154(12) -0.0012(10) -0.0008(10) 0.0003(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr C6 2.357(2) . ? Zr C3 2.364(2) . ? Zr C4 2.390(2) . ? Zr C7 2.392(3) . ? Zr C5 2.420(2) . ? Zr N1 2.4268(13) . ? Zr C2 2.430(3) . ? Zr C1 2.4562(17) . ? Zr C10 2.562(3) . ? Zr C11 2.569(2) . ? Zr C9 2.570(3) . ? Zr C12 2.595(2) . ? B C8 1.518(3) . ? B C12 1.528(3) . ? B C13 1.591(3) . ? N1 C14 1.340(4) . ? N1 C18 1.354(4) . ? N2 C16 1.357(2) . ? N2 C19 1.450(3) . ? N2 C20 1.458(3) . ? C1 C7 1.407(5) . ? C1 C2 1.420(5) . ? C2 C3 1.419(4) . ? C3 C4 1.417(4) . ? C4 C5 1.404(4) . ? C5 C6 1.415(3) . ? C6 C7 1.414(4) . ? C8 C9 1.392(4) . ? C9 C10 1.410(3) . ? C10 C11 1.405(3) . ? C11 C12 1.398(3) . ? C14 C15 1.362(4) . ? C15 C16 1.413(4) . ? C16 C17 1.415(4) . ? C17 C18 1.377(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 C6 Zr C3 85.54(10) . . ? C6 Zr C4 65.07(9) . . ? C3 Zr C4 34.66(9) . . ? C6 Zr C7 34.64(10) . . ? C3 Zr C7 84.96(9) . . ? C4 Zr C7 83.38(9) . . ? C6 Zr C5 34.44(8) . . ? C3 Zr C5 64.30(9) . . ? C4 Zr C5 33.92(10) . . ? C7 Zr C5 63.58(10) . . ? C6 Zr N1 120.49(9) . . ? C3 Zr N1 108.63(9) . . ? C4 Zr N1 142.74(8) . . ? C7 Zr N1 87.80(8) . . ? C5 Zr N1 150.52(7) . . ? C6 Zr C2 83.27(9) . . ? C3 Zr C2 34.41(9) . . ? C4 Zr C2 63.29(10) . . ? C7 Zr C2 64.18(8) . . ? C5 Zr C2 80.81(9) . . ? N1 Zr C2 80.28(8) . . ? C6 Zr C1 63.33(10) . . ? C3 Zr C1 64.10(11) . . ? C4 Zr C1 80.99(9) . . ? C7 Zr C1 33.71(12) . . ? C5 Zr C1 79.69(8) . . ? N1 Zr C1 72.02(5) . . ? C2 Zr C1 33.78(12) . . ? C6 Zr C10 126.66(9) . . ? C3 Zr C10 144.44(9) . . ? C4 Zr C10 139.56(10) . . ? C7 Zr C10 129.69(9) . . ? C5 Zr C10 132.90(8) . . ? N1 Zr C10 70.47(8) . . ? C2 Zr C10 145.82(9) . . ? C1 Zr C10 139.39(9) . . ? C6 Zr C11 96.21(8) . . ? C3 Zr C11 153.65(9) . . ? C4 Zr C11 123.76(9) . . ? C7 Zr C11 111.19(9) . . ? C5 Zr C11 103.32(8) . . ? N1 Zr C11 93.17(7) . . ? C2 Zr C11 171.95(9) . . ? C1 Zr C11 139.48(11) . . ? C10 Zr C11 31.79(8) . . ? C6 Zr C9 150.13(9) . . ? C3 Zr C9 112.57(9) . . ? C4 Zr C9 116.58(9) . . ? C7 Zr C9 159.90(9) . . ? C5 Zr C9 131.97(10) . . ? N1 Zr C9 77.50(7) . . ? C2 Zr C9 125.26(9) . . ? C1 Zr C9 145.42(9) . . ? C10 Zr C9 31.89(7) . . ? C11 Zr C9 56.90(8) . . ? C6 Zr C12 83.28(8) . . ? C3 Zr C12 123.86(8) . . ? C4 Zr C12 92.36(8) . . ? C7 Zr C12 112.33(9) . . ? C5 Zr C12 76.47(8) . . ? N1 Zr C12 124.29(7) . . ? C2 Zr C12 155.43(8) . . ? C1 Zr C12 145.71(10) . . ? C10 Zr C12 56.49(8) . . ? C11 Zr C12 31.42(7) . . ? C9 Zr C12 66.95(8) . . ? C8 B C12 112.9(2) . . ? C8 B C13 125.3(2) . . ? C12 B C13 121.8(2) . . ? C8 B Zr 68.37(12) . . ? C12 B Zr 67.74(11) . . ? C13 B Zr 134.67(14) . . ? C14 N1 C18 114.86(14) . . ? C14 N1 Zr 122.82(18) . . ? C18 N1 Zr 121.26(18) . . ? C16 N2 C19 120.0(2) . . ? C16 N2 C20 121.1(2) . . ? C19 N2 C20 118.36(15) . . ? C7 C1 C2 129.99(19) . . ? C7 C1 Zr 70.64(14) . . ? C2 C1 Zr 72.11(14) . . ? C3 C2 C1 128.7(2) . . ? C3 C2 Zr 70.25(15) . . ? C1 C2 Zr 74.11(14) . . ? C4 C3 C2 126.2(2) . . ? C4 C3 Zr 73.67(14) . . ? C2 C3 Zr 75.34(15) . . ? C5 C4 C3 129.1(3) . . ? C5 C4 Zr 74.20(16) . . ? C3 C4 Zr 71.66(14) . . ? C4 C5 C6 129.8(3) . . ? C4 C5 Zr 71.87(16) . . ? C6 C5 Zr 70.33(13) . . ? C7 C6 C5 127.3(2) . . ? C7 C6 Zr 74.04(15) . . ? C5 C6 Zr 75.23(13) . . ? C1 C7 C6 127.3(3) . . ? C1 C7 Zr 75.65(14) . . ? C6 C7 Zr 71.32(15) . . ? C9 C8 B 121.2(2) . . ? C9 C8 Zr 72.87(15) . . ? B C8 Zr 78.89(12) . . ? C8 C9 C10 121.8(3) . . ? C8 C9 Zr 75.96(15) . . ? C10 C9 Zr 73.70(18) . . ? C11 C10 C9 120.8(3) . . ? C11 C10 Zr 74.39(14) . . ? C9 C10 Zr 74.40(19) . . ? C12 C11 C10 121.0(2) . . ? C12 C11 Zr 75.32(12) . . ? C10 C11 Zr 73.82(14) . . ? C11 C12 B 121.5(2) . . ? C11 C12 Zr 73.26(12) . . ? B C12 Zr 79.23(12) . . ? N1 C14 C15 125.5(3) . . ? C14 C15 C16 119.9(3) . . ? N2 C16 C15 122.4(3) . . ? N2 C16 C17 122.1(3) . . ? C15 C16 C17 115.48(15) . . ? C18 C17 C16 119.5(2) . . ? N1 C18 C17 124.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 Zr B C8 170.02(13) . . . . ? C3 Zr B C8 83.50(14) . . . . ? C4 Zr B C8 109.63(15) . . . . ? C7 Zr B C8 172.73(14) . . . . ? C5 Zr B C8 144.81(14) . . . . ? N1 Zr B C8 -40.06(19) . . . . ? C2 Zr B C8 80.95(16) . . . . ? C1 Zr B C8 124.1(3) . . . . ? C10 Zr B C8 -63.92(13) . . . . ? C11 Zr B C8 -98.52(14) . . . . ? C9 Zr B C8 -29.28(13) . . . . ? C12 Zr B C8 -127.9(2) . . . . ? C6 Zr B C12 -62.12(14) . . . . ? C3 Zr B C12 -148.63(13) . . . . ? C4 Zr B C12 -122.50(14) . . . . ? C7 Zr B C12 -59.41(17) . . . . ? C5 Zr B C12 -87.32(13) . . . . ? N1 Zr B C12 87.81(16) . . . . ? C2 Zr B C12 -151.18(14) . . . . ? C1 Zr B C12 -108.1(3) . . . . ? C10 Zr B C12 63.95(13) . . . . ? C11 Zr B C12 29.35(12) . . . . ? C9 Zr B C12 98.58(15) . . . . ? C6 Zr B C13 51.2(2) . . . . ? C3 Zr B C13 -35.4(2) . . . . ? C4 Zr B C13 -9.2(2) . . . . ? C7 Zr B C13 53.9(3) . . . . ? C5 Zr B C13 26.0(2) . . . . ? N1 Zr B C13 -158.9(2) . . . . ? C2 Zr B C13 -37.9(3) . . . . ? C1 Zr B C13 5.2(4) . . . . ? C10 Zr B C13 177.2(3) . . . . ? C11 Zr B C13 142.6(3) . . . . ? C9 Zr B C13 -148.1(3) . . . . ? C12 Zr B C13 113.3(3) . . . . ? C6 Zr N1 C14 -129.25(18) . . . . ? C3 Zr N1 C14 -33.32(19) . . . . ? C4 Zr N1 C14 -41.2(2) . . . . ? C7 Zr N1 C14 -117.25(19) . . . . ? C5 Zr N1 C14 -103.8(2) . . . . ? C2 Zr N1 C14 -53.07(18) . . . . ? C1 Zr N1 C14 -86.9(2) . . . . ? C10 Zr N1 C14 108.99(18) . . . . ? C11 Zr N1 C14 131.64(18) . . . . ? C9 Zr N1 C14 76.56(18) . . . . ? C12 Zr N1 C14 127.02(18) . . . . ? C6 Zr N1 C18 38.35(19) . . . . ? C3 Zr N1 C18 134.29(17) . . . . ? C4 Zr N1 C18 126.4(2) . . . . ? C7 Zr N1 C18 50.36(17) . . . . ? C5 Zr N1 C18 63.8(2) . . . . ? C2 Zr N1 C18 114.53(17) . . . . ? C1 Zr N1 C18 80.73(19) . . . . ? C10 Zr N1 C18 -83.41(18) . . . . ? C11 Zr N1 C18 -60.76(17) . . . . ? C9 Zr N1 C18 -115.83(17) . . . . ? C12 Zr N1 C18 -65.37(18) . . . . ? C6 Zr C1 C7 25.02(15) . . . . ? C3 Zr C1 C7 123.49(16) . . . . ? C4 Zr C1 C7 91.57(16) . . . . ? C5 Zr C1 C7 57.17(15) . . . . ? N1 Zr C1 C7 -114.44(19) . . . . ? C2 Zr C1 C7 146.0(2) . . . . ? C10 Zr C1 C7 -91.13(18) . . . . ? C11 Zr C1 C7 -41.31(18) . . . . ? C9 Zr C1 C7 -143.80(19) . . . . ? C12 Zr C1 C7 10.7(2) . . . . ? C6 Zr C1 C2 -121.00(16) . . . . ? C3 Zr C1 C2 -22.53(15) . . . . ? C4 Zr C1 C2 -54.45(15) . . . . ? C7 Zr C1 C2 -146.0(2) . . . . ? C5 Zr C1 C2 -88.85(15) . . . . ? N1 Zr C1 C2 99.54(17) . . . . ? C10 Zr C1 C2 122.85(18) . . . . ? C11 Zr C1 C2 172.66(15) . . . . ? C9 Zr C1 C2 70.2(2) . . . . ? C12 Zr C1 C2 -135.32(19) . . . . ? C7 C1 C2 C3 3.9(4) . . . . ? Zr C1 C2 C3 47.3(2) . . . . ? C7 C1 C2 Zr -43.5(2) . . . . ? C6 Zr C2 C3 -91.93(18) . . . . ? C4 Zr C2 C3 -26.51(15) . . . . ? C7 Zr C2 C3 -122.25(19) . . . . ? C5 Zr C2 C3 -57.24(16) . . . . ? N1 Zr C2 C3 145.48(16) . . . . ? C1 Zr C2 C3 -142.4(2) . . . . ? C10 Zr C2 C3 114.4(2) . . . . ? C11 Zr C2 C3 -178.7(5) . . . . ? C9 Zr C2 C3 78.43(18) . . . . ? C12 Zr C2 C3 -34.7(3) . . . . ? C6 Zr C2 C1 50.47(14) . . . . ? C3 Zr C2 C1 142.4(2) . . . . ? C4 Zr C2 C1 115.90(16) . . . . ? C7 Zr C2 C1 20.16(13) . . . . ? C5 Zr C2 C1 85.17(14) . . . . ? N1 Zr C2 C1 -72.12(15) . . . . ? C10 Zr C2 C1 -103.23(19) . . . . ? C11 Zr C2 C1 -36.3(7) . . . . ? C9 Zr C2 C1 -139.16(13) . . . . ? C12 Zr C2 C1 107.7(2) . . . . ? C1 C2 C3 C4 7.8(4) . . . . ? Zr C2 C3 C4 56.5(2) . . . . ? C1 C2 C3 Zr -48.7(2) . . . . ? C6 Zr C3 C4 -50.90(14) . . . . ? C7 Zr C3 C4 -85.65(15) . . . . ? C5 Zr C3 C4 -22.60(15) . . . . ? N1 Zr C3 C4 -171.62(13) . . . . ? C2 Zr C3 C4 -135.5(2) . . . . ? C1 Zr C3 C4 -113.34(16) . . . . ? C10 Zr C3 C4 106.14(19) . . . . ? C11 Zr C3 C4 44.1(2) . . . . ? C9 Zr C3 C4 104.54(15) . . . . ? C12 Zr C3 C4 27.94(17) . . . . ? C6 Zr C3 C2 84.60(17) . . . . ? C4 Zr C3 C2 135.5(2) . . . . ? C7 Zr C3 C2 49.84(16) . . . . ? C5 Zr C3 C2 112.89(18) . . . . ? N1 Zr C3 C2 -36.12(17) . . . . ? C1 Zr C3 C2 22.15(15) . . . . ? C10 Zr C3 C2 -118.36(19) . . . . ? C11 Zr C3 C2 179.59(17) . . . . ? C9 Zr C3 C2 -119.97(16) . . . . ? C12 Zr C3 C2 163.43(14) . . . . ? C2 C3 C4 C5 -6.9(4) . . . . ? Zr C3 C4 C5 50.3(3) . . . . ? C2 C3 C4 Zr -57.2(2) . . . . ? C6 Zr C4 C5 -20.20(16) . . . . ? C3 Zr C4 C5 -141.6(2) . . . . ? C7 Zr C4 C5 -50.94(18) . . . . ? N1 Zr C4 C5 -128.45(17) . . . . ? C2 Zr C4 C5 -115.3(2) . . . . ? C1 Zr C4 C5 -84.90(19) . . . . ? C10 Zr C4 C5 97.81(19) . . . . ? C11 Zr C4 C5 60.2(2) . . . . ? C9 Zr C4 C5 126.59(18) . . . . ? C12 Zr C4 C5 61.27(18) . . . . ? C6 Zr C4 C3 121.44(15) . . . . ? C7 Zr C4 C3 90.70(15) . . . . ? C5 Zr C4 C3 141.6(2) . . . . ? N1 Zr C4 C3 13.2(2) . . . . ? C2 Zr C4 C3 26.32(14) . . . . ? C1 Zr C4 C3 56.74(16) . . . . ? C10 Zr C4 C3 -120.55(17) . . . . ? C11 Zr C4 C3 -158.19(13) . . . . ? C9 Zr C4 C3 -91.77(15) . . . . ? C12 Zr C4 C3 -157.09(14) . . . . ? C3 C4 C5 C6 -6.6(5) . . . . ? Zr C4 C5 C6 42.8(3) . . . . ? C3 C4 C5 Zr -49.4(3) . . . . ? C6 Zr C5 C4 146.4(3) . . . . ? C3 Zr C5 C4 23.06(16) . . . . ? C7 Zr C5 C4 120.5(2) . . . . ? N1 Zr C5 C4 105.5(2) . . . . ? C2 Zr C5 C4 54.88(18) . . . . ? C1 Zr C5 C4 89.2(2) . . . . ? C10 Zr C5 C4 -118.68(18) . . . . ? C11 Zr C5 C4 -132.17(17) . . . . ? C9 Zr C5 C4 -75.0(2) . . . . ? C12 Zr C5 C4 -115.69(18) . . . . ? C3 Zr C5 C6 -123.32(16) . . . . ? C4 Zr C5 C6 -146.4(3) . . . . ? C7 Zr C5 C6 -25.84(15) . . . . ? N1 Zr C5 C6 -40.8(2) . . . . ? C2 Zr C5 C6 -91.50(16) . . . . ? C1 Zr C5 C6 -57.23(17) . . . . ? C10 Zr C5 C6 94.94(17) . . . . ? C11 Zr C5 C6 81.45(15) . . . . ? C9 Zr C5 C6 138.63(15) . . . . ? C12 Zr C5 C6 97.93(15) . . . . ? C4 C5 C6 C7 12.8(4) . . . . ? Zr C5 C6 C7 56.1(2) . . . . ? C4 C5 C6 Zr -43.2(3) . . . . ? C3 Zr C6 C7 -87.58(18) . . . . ? C4 Zr C6 C7 -116.70(18) . . . . ? C5 Zr C6 C7 -136.6(2) . . . . ? N1 Zr C6 C7 21.45(19) . . . . ? C2 Zr C6 C7 -53.08(16) . . . . ? C1 Zr C6 C7 -24.40(16) . . . . ? C10 Zr C6 C7 108.85(18) . . . . ? C11 Zr C6 C7 118.84(16) . . . . ? C9 Zr C6 C7 142.84(19) . . . . ? C12 Zr C6 C7 147.53(17) . . . . ? C3 Zr C6 C5 49.05(14) . . . . ? C4 Zr C6 C5 19.92(16) . . . . ? C7 Zr C6 C5 136.6(2) . . . . ? N1 Zr C6 C5 158.07(14) . . . . ? C2 Zr C6 C5 83.55(15) . . . . ? C1 Zr C6 C5 112.22(17) . . . . ? C10 Zr C6 C5 -114.53(15) . . . . ? C11 Zr C6 C5 -104.54(15) . . . . ? C9 Zr C6 C5 -80.5(2) . . . . ? C12 Zr C6 C5 -75.84(15) . . . . ? C2 C1 C7 C6 -8.4(4) . . . . ? Zr C1 C7 C6 -52.4(2) . . . . ? C2 C1 C7 Zr 44.0(2) . . . . ? C5 C6 C7 C1 -2.5(4) . . . . ? Zr C6 C7 C1 54.1(2) . . . . ? C5 C6 C7 Zr -56.6(2) . . . . ? C6 Zr C7 C1 -138.3(2) . . . . ? C3 Zr C7 C1 -48.86(15) . . . . ? C4 Zr C7 C1 -83.67(15) . . . . ? C5 Zr C7 C1 -112.61(16) . . . . ? N1 Zr C7 C1 60.07(16) . . . . ? C2 Zr C7 C1 -20.19(14) . . . . ? C10 Zr C7 C1 122.25(15) . . . . ? C11 Zr C7 C1 152.61(14) . . . . ? C9 Zr C7 C1 102.8(3) . . . . ? C12 Zr C7 C1 -173.51(13) . . . . ? C3 Zr C7 C6 89.45(18) . . . . ? C4 Zr C7 C6 54.64(17) . . . . ? C5 Zr C7 C6 25.70(14) . . . . ? N1 Zr C7 C6 -161.62(17) . . . . ? C2 Zr C7 C6 118.12(18) . . . . ? C1 Zr C7 C6 138.3(2) . . . . ? C10 Zr C7 C6 -99.43(18) . . . . ? C11 Zr C7 C6 -69.07(17) . . . . ? C9 Zr C7 C6 -118.9(3) . . . . ? C12 Zr C7 C6 -35.19(18) . . . . ? C12 B C8 C9 9.5(3) . . . . ? C13 B C8 C9 -167.8(2) . . . . ? Zr B C8 C9 62.0(2) . . . . ? C12 B C8 Zr -52.46(16) . . . . ? C13 B C8 Zr 130.2(2) . . . . ? C6 Zr C8 C9 -140.96(16) . . . . ? C3 Zr C8 C9 133.24(17) . . . . ? C4 Zr C8 C9 167.44(17) . . . . ? C7 Zr C8 C9 -149.6(3) . . . . ? C5 Zr C8 C9 -162.66(16) . . . . ? N1 Zr C8 C9 23.18(18) . . . . ? C2 Zr C8 C9 110.96(17) . . . . ? C1 Zr C8 C9 105.46(19) . . . . ? C10 Zr C8 C9 -29.15(15) . . . . ? C11 Zr C8 C9 -63.34(17) . . . . ? C12 Zr C8 C9 -97.43(17) . . . . ? C6 Zr C8 B -13.18(18) . . . . ? C3 Zr C8 B -98.97(14) . . . . ? C4 Zr C8 B -64.77(14) . . . . ? C7 Zr C8 B -21.8(4) . . . . ? C5 Zr C8 B -34.87(14) . . . . ? N1 Zr C8 B 150.97(13) . . . . ? C2 Zr C8 B -121.26(14) . . . . ? C1 Zr C8 B -126.75(16) . . . . ? C10 Zr C8 B 98.64(15) . . . . ? C11 Zr C8 B 64.45(13) . . . . ? C9 Zr C8 B 127.8(2) . . . . ? C12 Zr C8 B 30.35(13) . . . . ? B C8 C9 C10 -4.7(4) . . . . ? Zr C8 C9 C10 60.3(3) . . . . ? B C8 C9 Zr -65.0(2) . . . . ? C6 Zr C9 C8 71.6(3) . . . . ? C3 Zr C9 C8 -52.03(18) . . . . ? C4 Zr C9 C8 -14.04(19) . . . . ? C7 Zr C9 C8 158.8(3) . . . . ? C5 Zr C9 C8 23.0(2) . . . . ? N1 Zr C9 C8 -157.24(18) . . . . ? C2 Zr C9 C8 -88.87(18) . . . . ? C1 Zr C9 C8 -128.7(2) . . . . ? C10 Zr C9 C8 129.7(3) . . . . ? C11 Zr C9 C8 100.52(19) . . . . ? C12 Zr C9 C8 66.58(16) . . . . ? C6 Zr C9 C10 -58.1(3) . . . . ? C3 Zr C9 C10 178.23(18) . . . . ? C4 Zr C9 C10 -143.77(19) . . . . ? C7 Zr C9 C10 29.1(4) . . . . ? C5 Zr C9 C10 -106.71(19) . . . . ? N1 Zr C9 C10 73.03(19) . . . . ? C2 Zr C9 C10 141.40(18) . . . . ? C1 Zr C9 C10 101.6(2) . . . . ? C11 Zr C9 C10 -29.21(17) . . . . ? C12 Zr C9 C10 -63.15(18) . . . . ? C8 C9 C10 C11 -0.9(5) . . . . ? Zr C9 C10 C11 60.5(3) . . . . ? C8 C9 C10 Zr -61.4(3) . . . . ? C6 Zr C10 C11 19.1(2) . . . . ? C3 Zr C10 C11 -131.90(17) . . . . ? C4 Zr C10 C11 -74.5(2) . . . . ? C7 Zr C10 C11 63.4(2) . . . . ? C5 Zr C10 C11 -25.5(2) . . . . ? N1 Zr C10 C11 133.12(18) . . . . ? C2 Zr C10 C11 165.84(17) . . . . ? C1 Zr C10 C11 109.6(2) . . . . ? C9 Zr C10 C11 -129.1(3) . . . . ? C12 Zr C10 C11 -29.01(14) . . . . ? C6 Zr C10 C9 148.19(17) . . . . ? C3 Zr C10 C9 -2.8(3) . . . . ? C4 Zr C10 C9 54.6(2) . . . . ? C7 Zr C10 C9 -167.46(18) . . . . ? C5 Zr C10 C9 103.57(19) . . . . ? N1 Zr C10 C9 -97.78(19) . . . . ? C2 Zr C10 C9 -65.1(3) . . . . ? C1 Zr C10 C9 -121.3(2) . . . . ? C11 Zr C10 C9 129.1(3) . . . . ? C12 Zr C10 C9 100.1(2) . . . . ? C9 C10 C11 C12 0.6(4) . . . . ? Zr C10 C11 C12 61.1(2) . . . . ? C9 C10 C11 Zr -60.5(3) . . . . ? C6 Zr C11 C12 66.18(15) . . . . ? C3 Zr C11 C12 -26.3(2) . . . . ? C4 Zr C11 C12 2.11(17) . . . . ? C7 Zr C11 C12 98.46(15) . . . . ? C5 Zr C11 C12 31.95(15) . . . . ? N1 Zr C11 C12 -172.67(14) . . . . ? C2 Zr C11 C12 152.0(6) . . . . ? C1 Zr C11 C12 121.60(15) . . . . ? C10 Zr C11 C12 -129.1(2) . . . . ? C9 Zr C11 C12 -99.82(16) . . . . ? C6 Zr C11 C10 -164.69(17) . . . . ? C3 Zr C11 C10 102.8(2) . . . . ? C4 Zr C11 C10 131.24(16) . . . . ? C7 Zr C11 C10 -132.42(17) . . . . ? C5 Zr C11 C10 161.08(16) . . . . ? N1 Zr C11 C10 -43.55(17) . . . . ? C2 Zr C11 C10 -78.8(6) . . . . ? C1 Zr C11 C10 -109.27(17) . . . . ? C9 Zr C11 C10 29.31(17) . . . . ? C12 Zr C11 C10 129.1(2) . . . . ? C10 C11 C12 B 5.2(3) . . . . ? Zr C11 C12 B 65.60(18) . . . . ? C10 C11 C12 Zr -60.4(2) . . . . ? C8 B C12 C11 -9.8(3) . . . . ? C13 B C12 C11 167.61(19) . . . . ? Zr B C12 C11 -62.59(18) . . . . ? C8 B C12 Zr 52.79(16) . . . . ? C13 B C12 Zr -129.80(18) . . . . ? C6 Zr C12 C11 -113.69(15) . . . . ? C3 Zr C12 C11 166.29(13) . . . . ? C4 Zr C12 C11 -178.24(14) . . . . ? C7 Zr C12 C11 -94.43(15) . . . . ? C5 Zr C12 C11 -148.02(15) . . . . ? N1 Zr C12 C11 8.86(17) . . . . ? C2 Zr C12 C11 -170.9(2) . . . . ? C1 Zr C12 C11 -100.83(19) . . . . ? C10 Zr C12 C11 29.35(13) . . . . ? C9 Zr C12 C11 63.77(14) . . . . ? C6 Zr C12 B 118.54(13) . . . . ? C3 Zr C12 B 38.52(16) . . . . ? C4 Zr C12 B 53.99(13) . . . . ? C7 Zr C12 B 137.80(13) . . . . ? C5 Zr C12 B 84.21(13) . . . . ? N1 Zr C12 B -118.90(13) . . . . ? C2 Zr C12 B 61.3(2) . . . . ? C1 Zr C12 B 131.40(16) . . . . ? C10 Zr C12 B -98.42(15) . . . . ? C11 Zr C12 B -127.77(19) . . . . ? C9 Zr C12 B -63.99(13) . . . . ? C18 N1 C14 C15 -1.6(3) . . . . ? Zr N1 C14 C15 166.7(2) . . . . ? N1 C14 C15 C16 -0.4(4) . . . . ? C19 N2 C16 C15 -6.4(3) . . . . ? C20 N2 C16 C15 -178.0(2) . . . . ? C19 N2 C16 C17 173.8(2) . . . . ? C20 N2 C16 C17 2.2(3) . . . . ? C14 C15 C16 N2 -178.1(2) . . . . ? C14 C15 C16 C17 1.7(3) . . . . ? N2 C16 C17 C18 178.7(2) . . . . ? C15 C16 C17 C18 -1.1(3) . . . . ? C14 N1 C18 C17 2.3(3) . . . . ? Zr N1 C18 C17 -166.27(19) . . . . ? C16 C17 C18 N1 -1.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.317 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.056 # Attachment 'andyg68a.cif' data_andyg68a _database_code_depnum_ccdc_archive 'CCDC 864984' #TrackingRef 'andyg68a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H24 B P Zr' _chemical_formula_weight 349.35 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.0930(4) _cell_length_b 15.9788(2) _cell_length_c 12.2654(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.696(2) _cell_angle_gamma 90.00 _cell_volume 3173.22(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 26299 _cell_measurement_theta_min 3.7993 _cell_measurement_theta_max 75.7232 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.463 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 6.473 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.21575 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7641 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0230 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.89 _diffrn_reflns_theta_max 70.07 _reflns_number_total 7642 _reflns_number_gt 6922 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. The hydrogens of the seven-membered ring and of the six-membered ring were refined freely. The crystal was a non-merohedral twin, formed by 180 degree rotation about the c* axis. The structure was refined using the 'HKLF 5' option, whereby the scale factor refined to 0.2090(16). Because of overlapped reflections, the number of reflections is difficult to define and should be interpreted with caution; the untwinning routine merges all equivalent reflections and so R(int) is not defined. ; _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^)+(0.0508P)^2^+3.0032P] 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 7642 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0372 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0838 _refine_ls_wR_factor_gt 0.0809 _refine_ls_goodness_of_fit_ref 1.061 _refine_ls_restrained_S_all 1.061 _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 0.362763(14) 0.257202(14) 0.71017(2) 0.01535(7) Uani 1 1 d . . . P P 0.46551(5) 0.40267(5) 0.73835(7) 0.02250(16) Uani 1 1 d . . . B B 0.1969(2) 0.2335(2) 0.6025(3) 0.0221(7) Uani 1 1 d . . . C1 C 0.50715(19) 0.21384(19) 0.7875(3) 0.0225(6) Uani 1 1 d . . . H1 H 0.560(2) 0.249(2) 0.821(3) 0.024(9) Uiso 1 1 d . . . C2 C 0.4657(2) 0.1926(2) 0.8674(3) 0.0264(7) Uani 1 1 d . . . H2 H 0.487(3) 0.210(2) 0.942(4) 0.030(10) Uiso 1 1 d . . . C3 C 0.3919(2) 0.1448(2) 0.8428(3) 0.0296(7) Uani 1 1 d . . . H3 H 0.373(3) 0.139(3) 0.908(4) 0.047(12) Uiso 1 1 d . . . C4 C 0.3453(2) 0.10848(19) 0.7362(3) 0.0276(7) Uani 1 1 d . . . H4 H 0.292(2) 0.082(2) 0.739(3) 0.029(10) Uiso 1 1 d . . . C5 C 0.35044(19) 0.12164(18) 0.6254(3) 0.0244(6) Uani 1 1 d . . . H5 H 0.307(3) 0.103(2) 0.565(4) 0.031(10) Uiso 1 1 d . . . C6 C 0.41109(19) 0.16592(18) 0.5927(3) 0.0207(6) Uani 1 1 d . . . H6 H 0.405(2) 0.169(2) 0.516(3) 0.015(8) Uiso 1 1 d . . . C7 C 0.48321(19) 0.20235(18) 0.6680(3) 0.0198(6) Uani 1 1 d . . . H7 H 0.515(2) 0.230(2) 0.635(3) 0.026(10) Uiso 1 1 d . . . C8 C 0.21760(18) 0.2383(2) 0.7333(3) 0.0224(6) Uani 1 1 d . . . H8 H 0.204(3) 0.190(2) 0.772(4) 0.036(11) Uiso 1 1 d . . . C9 C 0.25375(19) 0.3089(2) 0.7965(3) 0.0246(7) Uani 1 1 d . . . H9 H 0.264(2) 0.309(2) 0.876(3) 0.017(8) Uiso 1 1 d . . . C10 C 0.27668(19) 0.37758(19) 0.7419(3) 0.0254(7) Uani 1 1 d . . . H10 H 0.303(2) 0.423(2) 0.790(3) 0.013(8) Uiso 1 1 d . . . C11 C 0.26211(19) 0.3773(2) 0.6213(3) 0.0260(7) Uani 1 1 d . . . H11 H 0.280(3) 0.428(3) 0.592(4) 0.037(11) Uiso 1 1 d . . . C12 C 0.2282(2) 0.3084(2) 0.5534(3) 0.0251(7) Uani 1 1 d . . . H12 H 0.222(3) 0.310(2) 0.474(4) 0.031(10) Uiso 1 1 d . . . C13 C 0.14460(19) 0.1588(2) 0.5287(3) 0.0274(7) Uani 1 1 d . . . H13A H 0.0856 0.1693 0.5141 0.041 Uiso 1 1 calc R . . H13B H 0.1603 0.1062 0.5713 0.041 Uiso 1 1 calc R . . H13C H 0.1556 0.1548 0.4553 0.041 Uiso 1 1 calc R . . C14 C 0.5540(2) 0.4008(2) 0.6854(3) 0.0283(7) Uani 1 1 d . . . H14A H 0.5347 0.3916 0.6020 0.043 Uiso 1 1 calc R . . H14B H 0.5914 0.3554 0.7232 0.043 Uiso 1 1 calc R . . H14C H 0.5833 0.4544 0.7026 0.043 Uiso 1 1 calc R . . C15 C 0.5163(2) 0.4286(2) 0.8898(3) 0.0376(9) Uani 1 1 d . . . H15A H 0.5491 0.3806 0.9291 0.056 Uiso 1 1 calc R . . H15B H 0.4745 0.4420 0.9262 0.056 Uiso 1 1 calc R . . H15C H 0.5526 0.4770 0.8954 0.056 Uiso 1 1 calc R . . C16 C 0.4236(3) 0.5041(2) 0.6815(5) 0.0471(11) Uani 1 1 d . . . H16A H 0.4676 0.5462 0.7034 0.071 Uiso 1 1 calc R . . H16B H 0.3798 0.5198 0.7130 0.071 Uiso 1 1 calc R . . H16C H 0.4010 0.5010 0.5974 0.071 Uiso 1 1 calc R . . Zr' Zr 0.165041(14) 0.696793(14) 0.87084(2) 0.01654(7) Uani 1 1 d . . . P' P 0.04566(5) 0.57507(5) 0.74995(7) 0.02077(16) Uani 1 1 d . . . B' B 0.1679(2) 0.8680(2) 0.8651(3) 0.0256(7) Uani 1 1 d . . . C1' C 0.22831(18) 0.55742(19) 0.9124(3) 0.0226(6) Uani 1 1 d . . . H1' H 0.206(2) 0.501(2) 0.900(3) 0.028(9) Uiso 1 1 d . . . C2' C 0.2272(2) 0.59467(19) 1.0163(3) 0.0241(6) Uani 1 1 d . . . H2' H 0.206(3) 0.566(3) 1.062(4) 0.036(11) Uiso 1 1 d . . . C3' C 0.25880(19) 0.6746(2) 1.0586(3) 0.0233(6) Uani 1 1 d . . . H3' H 0.249(2) 0.6908(19) 1.129(3) 0.013(8) Uiso 1 1 d . . . C4' C 0.29812(18) 0.73363(19) 1.0077(3) 0.0230(6) Uani 1 1 d . . . H4' H 0.309(2) 0.788(2) 1.050(3) 0.021(9) Uiso 1 1 d . . . C5' C 0.30414(18) 0.73442(18) 0.8952(3) 0.0235(6) Uani 1 1 d . . . H5' H 0.326(2) 0.783(2) 0.875(3) 0.021(9) Uiso 1 1 d . . . C6' C 0.28151(19) 0.6720(2) 0.8087(3) 0.0239(6) Uani 1 1 d . . . H6' H 0.286(3) 0.686(2) 0.737(4) 0.034(11) Uiso 1 1 d . . . C7' C 0.25068(18) 0.5910(2) 0.8202(3) 0.0236(6) Uani 1 1 d . . . H7' H 0.235(2) 0.559(2) 0.748(3) 0.015(8) Uiso 1 1 d . . . C8' C 0.1436(2) 0.8373(2) 0.9677(3) 0.0263(7) Uani 1 1 d . . . H8' H 0.177(2) 0.853(2) 1.044(3) 0.026(9) Uiso 1 1 d . . . C9' C 0.0735(2) 0.7876(2) 0.9540(3) 0.0250(6) Uani 1 1 d . . . H9' H 0.061(3) 0.768(2) 1.016(4) 0.033(11) Uiso 1 1 d . . . C10' C 0.02375(19) 0.76175(19) 0.8439(3) 0.0222(6) Uani 1 1 d . . . H10' H -0.025(2) 0.730(2) 0.834(3) 0.017(8) Uiso 1 1 d . . . C11' C 0.04345(19) 0.78539(19) 0.7449(3) 0.0213(6) Uani 1 1 d . . . H11' H 0.005(3) 0.763(2) 0.672(4) 0.035(11) Uiso 1 1 d . . . C12' C 0.11379(19) 0.83206(19) 0.7509(3) 0.0226(6) Uani 1 1 d . . . H12' H 0.123(2) 0.843(2) 0.686(3) 0.024(9) Uiso 1 1 d . . . C13' C 0.2397(2) 0.9342(2) 0.8748(4) 0.0356(8) Uani 1 1 d . . . H13D H 0.2185 0.9910 0.8774 0.053 Uiso 1 1 calc R . . H13E H 0.2587 0.9288 0.8078 0.053 Uiso 1 1 calc R . . H13F H 0.2858 0.9236 0.9452 0.053 Uiso 1 1 calc R . . C14' C 0.0740(2) 0.4883(2) 0.6729(3) 0.0302(7) Uani 1 1 d . . . H14D H 0.1212 0.4582 0.7250 0.045 Uiso 1 1 calc R . . H14E H 0.0889 0.5102 0.6076 0.045 Uiso 1 1 calc R . . H14F H 0.0270 0.4500 0.6447 0.045 Uiso 1 1 calc R . . C15' C 0.0075(2) 0.5204(2) 0.8534(3) 0.0295(7) Uani 1 1 d . . . H15D H -0.0183 0.5607 0.8915 0.044 Uiso 1 1 calc R . . H15E H 0.0537 0.4929 0.9111 0.044 Uiso 1 1 calc R . . H15F H -0.0332 0.4784 0.8132 0.044 Uiso 1 1 calc R . . C16' C -0.0519(2) 0.6047(2) 0.6407(3) 0.0302(7) Uani 1 1 d . . . H16D H -0.0876 0.5554 0.6188 0.045 Uiso 1 1 calc R . . H16E H -0.0406 0.6269 0.5728 0.045 Uiso 1 1 calc R . . H16F H -0.0796 0.6476 0.6722 0.045 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 0.01514(12) 0.01366(11) 0.01743(12) -0.00019(8) 0.00548(9) 0.00092(9) P 0.0210(4) 0.0160(3) 0.0327(4) -0.0032(3) 0.0117(3) -0.0021(3) B 0.0168(15) 0.0288(18) 0.0216(17) -0.0017(13) 0.0072(13) 0.0046(13) C1 0.0172(14) 0.0181(13) 0.0281(16) 0.0005(12) 0.0018(12) 0.0042(12) C2 0.0290(16) 0.0269(16) 0.0185(16) 0.0027(12) 0.0008(13) 0.0108(13) C3 0.0368(18) 0.0248(15) 0.0315(17) 0.0149(14) 0.0171(15) 0.0113(14) C4 0.0246(16) 0.0137(13) 0.045(2) 0.0048(13) 0.0119(14) 0.0010(12) C5 0.0193(14) 0.0154(13) 0.0353(18) -0.0081(12) 0.0044(13) 0.0003(11) C6 0.0223(14) 0.0201(14) 0.0194(15) -0.0052(11) 0.0063(12) 0.0061(12) C7 0.0175(14) 0.0183(14) 0.0256(15) 0.0010(11) 0.0097(12) 0.0036(11) C8 0.0176(14) 0.0287(16) 0.0215(15) -0.0003(12) 0.0071(12) -0.0024(12) C9 0.0172(14) 0.0351(17) 0.0239(17) -0.0046(13) 0.0100(12) 0.0035(12) C10 0.0175(14) 0.0206(14) 0.0374(18) -0.0067(13) 0.0079(13) 0.0040(12) C11 0.0192(14) 0.0223(14) 0.0367(18) 0.0080(13) 0.0090(13) 0.0062(12) C12 0.0201(15) 0.0305(16) 0.0232(16) 0.0038(13) 0.0050(12) 0.0066(12) C13 0.0211(15) 0.0373(18) 0.0218(15) -0.0071(13) 0.0041(12) -0.0052(13) C14 0.0268(16) 0.0284(16) 0.0346(18) -0.0066(14) 0.0166(14) -0.0084(13) C15 0.045(2) 0.0370(19) 0.038(2) -0.0198(16) 0.0234(17) -0.0234(17) C16 0.036(2) 0.0167(15) 0.090(3) 0.0052(18) 0.022(2) -0.0021(15) Zr' 0.01520(12) 0.01662(12) 0.01738(12) 0.00055(9) 0.00464(9) 0.00155(8) P' 0.0176(3) 0.0195(3) 0.0243(4) -0.0010(3) 0.0054(3) 0.0001(3) B' 0.0227(16) 0.0178(15) 0.0353(19) -0.0002(14) 0.0079(15) 0.0046(13) C1' 0.0184(14) 0.0192(14) 0.0276(16) 0.0012(12) 0.0037(12) 0.0036(11) C2' 0.0251(15) 0.0217(15) 0.0243(16) 0.0079(12) 0.0060(13) 0.0052(12) C3' 0.0222(15) 0.0260(15) 0.0170(15) 0.0007(12) -0.0002(12) 0.0035(12) C4' 0.0156(13) 0.0221(15) 0.0269(16) -0.0005(12) 0.0007(12) 0.0002(11) C5' 0.0155(14) 0.0202(15) 0.0345(17) 0.0030(13) 0.0075(13) 0.0018(11) C6' 0.0193(14) 0.0292(16) 0.0254(16) 0.0051(13) 0.0101(12) 0.0049(12) C7' 0.0183(14) 0.0255(15) 0.0271(16) -0.0007(13) 0.0073(12) 0.0096(12) C8' 0.0285(16) 0.0232(15) 0.0256(17) -0.0064(13) 0.0065(13) 0.0081(13) C9' 0.0268(16) 0.0268(15) 0.0250(16) 0.0031(13) 0.0133(13) 0.0117(13) C10' 0.0191(14) 0.0196(14) 0.0306(17) 0.0027(12) 0.0118(12) 0.0038(11) C11' 0.0213(14) 0.0202(13) 0.0207(15) 0.0004(11) 0.0045(12) 0.0058(12) C12' 0.0250(15) 0.0192(14) 0.0254(16) 0.0038(12) 0.0108(13) 0.0040(12) C13' 0.0301(17) 0.0225(16) 0.054(2) -0.0052(15) 0.0129(16) -0.0023(14) C14' 0.0277(16) 0.0276(16) 0.0344(18) -0.0077(14) 0.0089(14) 0.0005(13) C15' 0.0320(17) 0.0234(15) 0.0357(18) 0.0014(13) 0.0147(14) -0.0057(13) C16' 0.0199(15) 0.0297(16) 0.0348(18) -0.0038(14) 0.0002(13) -0.0031(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 C3 2.366(3) . ? Zr C6 2.377(3) . ? Zr C5 2.383(3) . ? Zr C2 2.388(3) . ? Zr C4 2.429(3) . ? Zr C7 2.441(3) . ? Zr C1 2.443(3) . ? Zr C10 2.527(3) . ? Zr C9 2.557(3) . ? Zr C11 2.575(3) . ? Zr C8 2.604(3) . ? Zr C12 2.612(3) . ? P C16 1.818(4) . ? P C14 1.828(3) . ? P C15 1.829(4) . ? B C12 1.512(5) . ? B C8 1.530(5) . ? B C13 1.590(5) . ? C1 C7 1.402(4) . ? C1 C2 1.421(5) . ? C2 C3 1.423(5) . ? C3 C4 1.419(5) . ? C4 C5 1.405(5) . ? C5 C6 1.415(5) . ? C6 C7 1.408(4) . ? C8 C9 1.396(5) . ? C9 C10 1.405(5) . ? C10 C11 1.419(5) . ? C11 C12 1.390(5) . ? Zr' C3' 2.373(3) . ? Zr' C5' 2.376(3) . ? Zr' C6' 2.382(3) . ? Zr' C2' 2.400(3) . ? Zr' C4' 2.427(3) . ? Zr' C7' 2.444(3) . ? Zr' C1' 2.457(3) . ? Zr' C10' 2.551(3) . ? Zr' C9' 2.572(3) . ? Zr' C11' 2.579(3) . ? Zr' C12' 2.603(3) . ? Zr' C8' 2.620(3) . ? P' C15' 1.824(3) . ? P' C14' 1.828(3) . ? P' C16' 1.835(3) . ? B' C12' 1.523(5) . ? B' C8' 1.526(5) . ? B' C13' 1.595(5) . ? C1' C7' 1.411(5) . ? C1' C2' 1.412(5) . ? C2' C3' 1.419(5) . ? C3' C4' 1.414(5) . ? C4' C5' 1.416(5) . ? C5' C6' 1.417(5) . ? C6' C7' 1.422(5) . ? C8' C9' 1.404(5) . ? C9' C10' 1.407(5) . ? C10' C11' 1.411(4) . ? C11' C12' 1.397(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 C3 Zr C6 85.03(11) . . ? C3 Zr C5 65.14(12) . . ? C6 Zr C5 34.59(11) . . ? C3 Zr C2 34.83(12) . . ? C6 Zr C2 85.12(11) . . ? C5 Zr C2 84.19(11) . . ? C3 Zr C4 34.39(12) . . ? C6 Zr C4 63.92(11) . . ? C5 Zr C4 33.95(12) . . ? C2 Zr C4 63.97(12) . . ? C3 Zr C7 82.37(11) . . ? C6 Zr C7 33.95(10) . . ? C5 Zr C7 62.85(10) . . ? C2 Zr C7 64.06(11) . . ? C4 Zr C7 79.86(11) . . ? C3 Zr C1 63.53(11) . . ? C6 Zr C1 63.72(10) . . ? C5 Zr C1 81.29(10) . . ? C2 Zr C1 34.19(11) . . ? C4 Zr C1 79.80(11) . . ? C7 Zr C1 33.36(11) . . ? C3 Zr C10 118.47(12) . . ? C6 Zr C10 153.29(11) . . ? C5 Zr C10 141.72(11) . . ? C2 Zr C10 121.30(11) . . ? C4 Zr C10 128.50(11) . . ? C7 Zr C10 151.46(10) . . ? C1 Zr C10 136.20(10) . . ? C3 Zr C9 88.93(11) . . ? C6 Zr C9 152.89(11) . . ? C5 Zr C9 120.01(11) . . ? C2 Zr C9 104.57(11) . . ? C4 Zr C9 97.19(11) . . ? C7 Zr C9 168.46(11) . . ? C1 Zr C9 135.26(11) . . ? C10 Zr C9 32.09(11) . . ? C3 Zr C11 145.25(11) . . ? C6 Zr C11 121.04(11) . . ? C5 Zr C11 122.63(11) . . ? C2 Zr C11 152.05(11) . . ? C4 Zr C11 133.74(11) . . ? C7 Zr C11 132.25(10) . . ? C1 Zr C11 146.14(10) . . ? C10 Zr C11 32.29(11) . . ? C9 Zr C11 57.18(11) . . ? C3 Zr C8 80.50(11) . . ? C6 Zr C8 121.56(10) . . ? C5 Zr C8 89.32(10) . . ? C2 Zr C8 110.08(11) . . ? C4 Zr C8 73.18(11) . . ? C7 Zr C8 151.58(10) . . ? C1 Zr C8 143.52(10) . . ? C10 Zr C8 56.58(10) . . ? C9 Zr C8 31.36(10) . . ? C11 Zr C8 66.55(10) . . ? C3 Zr C12 133.27(12) . . ? C6 Zr C12 98.11(10) . . ? C5 Zr C12 91.70(11) . . ? C2 Zr C12 167.65(11) . . ? C4 Zr C12 106.67(11) . . ? C7 Zr C12 124.06(11) . . ? C1 Zr C12 156.37(11) . . ? C10 Zr C12 57.04(10) . . ? C9 Zr C12 67.48(11) . . ? C11 Zr C12 31.08(11) . . ? C8 Zr C12 58.10(10) . . ? C16 P C14 98.45(18) . . ? C16 P C15 100.9(2) . . ? C14 P C15 100.78(17) . . ? C16 P Zr 121.74(14) . . ? C14 P Zr 119.25(11) . . ? C15 P Zr 112.30(12) . . ? C12 B C8 112.7(3) . . ? C12 B C13 125.0(3) . . ? C8 B C13 122.2(3) . . ? C12 B Zr 68.90(17) . . ? C8 B Zr 68.45(17) . . ? C13 B Zr 133.1(2) . . ? C7 C1 C2 130.3(3) . . ? C7 C1 Zr 73.22(17) . . ? C2 C1 Zr 70.79(18) . . ? C1 C2 C3 125.9(3) . . ? C1 C2 Zr 75.02(18) . . ? C3 C2 Zr 71.74(18) . . ? C4 C3 C2 127.8(3) . . ? C4 C3 Zr 75.21(18) . . ? C2 C3 Zr 73.43(18) . . ? C5 C4 C3 129.7(3) . . ? C5 C4 Zr 71.23(17) . . ? C3 C4 Zr 70.40(18) . . ? C4 C5 C6 128.8(3) . . ? C4 C5 Zr 74.82(18) . . ? C6 C5 Zr 72.47(16) . . ? C7 C6 C5 126.0(3) . . ? C7 C6 Zr 75.52(17) . . ? C5 C6 Zr 72.94(17) . . ? C1 C7 C6 129.9(3) . . ? C1 C7 Zr 73.42(17) . . ? C6 C7 Zr 70.53(17) . . ? C9 C8 B 122.3(3) . . ? C9 C8 Zr 72.48(17) . . ? B C8 Zr 78.42(18) . . ? C8 C9 C10 120.5(3) . . ? C8 C9 Zr 76.16(18) . . ? C10 C9 Zr 72.75(17) . . ? C9 C10 C11 120.8(3) . . ? C9 C10 Zr 75.16(17) . . ? C11 C10 Zr 75.74(17) . . ? C12 C11 C10 121.8(3) . . ? C12 C11 Zr 75.93(18) . . ? C10 C11 Zr 71.97(17) . . ? C11 C12 B 121.4(3) . . ? C11 C12 Zr 72.99(18) . . ? B C12 Zr 78.40(18) . . ? C3' Zr' C5' 65.06(12) . . ? C3' Zr' C6' 84.95(12) . . ? C5' Zr' C6' 34.65(11) . . ? C3' Zr' C2' 34.59(11) . . ? C5' Zr' C2' 83.77(11) . . ? C6' Zr' C2' 84.73(11) . . ? C3' Zr' C4' 34.24(11) . . ? C5' Zr' C4' 34.26(12) . . ? C6' Zr' C4' 64.38(11) . . ? C2' Zr' C4' 63.72(11) . . ? C3' Zr' C7' 82.55(11) . . ? C5' Zr' C7' 63.28(10) . . ? C6' Zr' C7' 34.24(11) . . ? C2' Zr' C7' 63.88(11) . . ? C4' Zr' C7' 80.72(11) . . ? C3' Zr' C1' 63.12(11) . . ? C5' Zr' C1' 81.20(10) . . ? C6' Zr' C1' 63.78(11) . . ? C2' Zr' C1' 33.77(11) . . ? C4' Zr' C1' 79.85(10) . . ? C7' Zr' C1' 33.46(11) . . ? C3' Zr' C10' 120.21(11) . . ? C5' Zr' C10' 141.33(10) . . ? C6' Zr' C10' 151.63(11) . . ? C2' Zr' C10' 123.25(11) . . ? C4' Zr' C10' 129.00(10) . . ? C7' Zr' C10' 150.23(11) . . ? C1' Zr' C10' 136.99(10) . . ? C3' Zr' C9' 90.40(11) . . ? C5' Zr' C9' 121.24(11) . . ? C6' Zr' C9' 153.87(11) . . ? C2' Zr' C9' 105.65(11) . . ? C4' Zr' C9' 98.25(11) . . ? C7' Zr' C9' 168.89(11) . . ? C1' Zr' C9' 135.43(11) . . ? C10' Zr' C9' 31.87(11) . . ? C3' Zr' C11' 145.79(10) . . ? C5' Zr' C11' 121.21(10) . . ? C6' Zr' C11' 119.70(10) . . ? C2' Zr' C11' 153.94(11) . . ? C4' Zr' C11' 132.67(10) . . ? C7' Zr' C11' 131.38(10) . . ? C1' Zr' C11' 146.99(10) . . ? C10' Zr' C11' 31.93(10) . . ? C9' Zr' C11' 56.75(10) . . ? C3' Zr' C12' 132.27(11) . . ? C5' Zr' C12' 90.17(10) . . ? C6' Zr' C12' 96.98(10) . . ? C2' Zr' C12' 166.72(11) . . ? C4' Zr' C12' 105.10(10) . . ? C7' Zr' C12' 123.45(11) . . ? C1' Zr' C12' 156.32(11) . . ? C10' Zr' C12' 57.05(10) . . ? C9' Zr' C12' 67.58(10) . . ? C11' Zr' C12' 31.27(10) . . ? C3' Zr' C8' 80.62(11) . . ? C5' Zr' C8' 90.31(11) . . ? C6' Zr' C8' 122.68(11) . . ? C2' Zr' C8' 109.80(11) . . ? C4' Zr' C8' 73.42(10) . . ? C7' Zr' C8' 152.92(11) . . ? C1' Zr' C8' 143.03(11) . . ? C10' Zr' C8' 56.37(10) . . ? C9' Zr' C8' 31.34(11) . . ? C11' Zr' C8' 66.31(10) . . ? C12' Zr' C8' 58.27(10) . . ? C15' P' C14' 102.11(16) . . ? C15' P' C16' 100.83(17) . . ? C14' P' C16' 98.47(16) . . ? C15' P' Zr' 108.60(11) . . ? C14' P' Zr' 121.31(11) . . ? C16' P' Zr' 122.18(11) . . ? C12' B' C8' 113.1(3) . . ? C12' B' C13' 123.0(3) . . ? C8' B' C13' 123.9(3) . . ? C12' B' Zr' 68.64(17) . . ? C8' B' Zr' 69.26(17) . . ? C13' B' Zr' 132.9(2) . . ? C7' C1' C2' 130.4(3) . . ? C7' C1' Zr' 72.76(17) . . ? C2' C1' Zr' 70.90(17) . . ? C1' C2' C3' 126.6(3) . . ? C1' C2' Zr' 75.33(18) . . ? C3' C2' Zr' 71.67(17) . . ? C4' C3' C2' 128.1(3) . . ? C4' C3' Zr' 74.98(18) . . ? C2' C3' Zr' 73.74(17) . . ? C3' C4' C5' 129.0(3) . . ? C3' C4' Zr' 70.78(17) . . ? C5' C4' Zr' 70.91(17) . . ? C4' C5' C6' 129.5(3) . . ? C4' C5' Zr' 74.83(18) . . ? C6' C5' Zr' 72.89(17) . . ? C5' C6' C7' 126.0(3) . . ? C5' C6' Zr' 72.45(18) . . ? C7' C6' Zr' 75.25(17) . . ? C1' C7' C6' 129.0(3) . . ? C1' C7' Zr' 73.78(17) . . ? C6' C7' Zr' 70.51(17) . . ? C9' C8' B' 122.1(3) . . ? C9' C8' Zr' 72.44(17) . . ? B' C8' Zr' 77.73(18) . . ? C8' C9' C10' 120.8(3) . . ? C8' C9' Zr' 76.22(18) . . ? C10' C9' Zr' 73.23(17) . . ? C9' C10' C11' 120.6(3) . . ? C9' C10' Zr' 74.90(18) . . ? C11' C10' Zr' 75.12(17) . . ? C12' C11' C10' 122.5(3) . . ? C12' C11' Zr' 75.33(18) . . ? C10' C11' Zr' 72.95(17) . . ? C11' C12' B' 120.5(3) . . ? C11' C12' Zr' 73.40(17) . . ? B' C12' Zr' 78.36(18) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C3 Zr P C16 -151.0(2) . . . . ? C6 Zr P C16 115.3(2) . . . . ? C5 Zr P C16 119.8(2) . . . . ? C2 Zr P C16 -159.9(2) . . . . ? C4 Zr P C16 177.6(3) . . . . ? C7 Zr P C16 136.5(2) . . . . ? C1 Zr P C16 170.5(2) . . . . ? C10 Zr P C16 -37.0(2) . . . . ? C9 Zr P C16 -55.2(2) . . . . ? C11 Zr P C16 -3.5(2) . . . . ? C8 Zr P C16 -43.7(2) . . . . ? C12 Zr P C16 13.8(2) . . . . ? C3 Zr P C14 85.99(17) . . . . ? C6 Zr P C14 -7.64(16) . . . . ? C5 Zr P C14 -3.22(19) . . . . ? C2 Zr P C14 77.14(16) . . . . ? C4 Zr P C14 54.6(2) . . . . ? C7 Zr P C14 13.56(16) . . . . ? C1 Zr P C14 47.53(16) . . . . ? C10 Zr P C14 -159.97(16) . . . . ? C9 Zr P C14 -178.15(16) . . . . ? C11 Zr P C14 -126.50(16) . . . . ? C8 Zr P C14 -166.65(16) . . . . ? C12 Zr P C14 -109.22(16) . . . . ? C3 Zr P C15 -31.48(18) . . . . ? C6 Zr P C15 -125.11(16) . . . . ? C5 Zr P C15 -120.69(19) . . . . ? C2 Zr P C15 -40.33(17) . . . . ? C4 Zr P C15 -62.9(2) . . . . ? C7 Zr P C15 -103.91(17) . . . . ? C1 Zr P C15 -69.94(17) . . . . ? C10 Zr P C15 82.56(17) . . . . ? C9 Zr P C15 64.38(17) . . . . ? C11 Zr P C15 116.03(17) . . . . ? C8 Zr P C15 75.88(17) . . . . ? C12 Zr P C15 133.31(16) . . . . ? C3 Zr B C12 -179.71(19) . . . . ? C6 Zr B C12 -93.40(19) . . . . ? C5 Zr B C12 -119.4(2) . . . . ? C2 Zr B C12 176.02(18) . . . . ? C4 Zr B C12 -154.4(2) . . . . ? C7 Zr B C12 -90.6(2) . . . . ? C1 Zr B C12 -132.2(3) . . . . ? C10 Zr B C12 63.70(19) . . . . ? C9 Zr B C12 98.4(2) . . . . ? C11 Zr B C12 29.00(18) . . . . ? C8 Zr B C12 126.7(3) . . . . ? C3 Zr B C8 53.6(2) . . . . ? C6 Zr B C8 139.92(18) . . . . ? C5 Zr B C8 113.9(2) . . . . ? C2 Zr B C8 49.3(2) . . . . ? C4 Zr B C8 78.92(19) . . . . ? C7 Zr B C8 142.70(18) . . . . ? C1 Zr B C8 101.1(3) . . . . ? C10 Zr B C8 -62.98(18) . . . . ? C9 Zr B C8 -28.33(17) . . . . ? C11 Zr B C8 -97.7(2) . . . . ? C12 Zr B C8 -126.7(3) . . . . ? C3 Zr B C13 -60.9(3) . . . . ? C6 Zr B C13 25.4(3) . . . . ? C5 Zr B C13 -0.7(3) . . . . ? C2 Zr B C13 -65.2(3) . . . . ? C4 Zr B C13 -35.6(3) . . . . ? C7 Zr B C13 28.2(4) . . . . ? C1 Zr B C13 -13.4(5) . . . . ? C10 Zr B C13 -177.5(3) . . . . ? C9 Zr B C13 -142.9(3) . . . . ? C11 Zr B C13 147.8(3) . . . . ? C8 Zr B C13 -114.5(4) . . . . ? C12 Zr B C13 118.8(4) . . . . ? C3 Zr C1 C7 119.1(2) . . . . ? C6 Zr C1 C7 21.19(17) . . . . ? C5 Zr C1 C7 52.63(19) . . . . ? C2 Zr C1 C7 145.1(3) . . . . ? C4 Zr C1 C7 87.02(19) . . . . ? C10 Zr C1 C7 -136.40(19) . . . . ? C9 Zr C1 C7 176.97(17) . . . . ? C11 Zr C1 C7 -86.0(3) . . . . ? C8 Zr C1 C7 129.5(2) . . . . ? C12 Zr C1 C7 -21.4(4) . . . . ? C3 Zr C1 C2 -25.99(19) . . . . ? C6 Zr C1 C2 -123.9(2) . . . . ? C5 Zr C1 C2 -92.5(2) . . . . ? C4 Zr C1 C2 -58.1(2) . . . . ? C7 Zr C1 C2 -145.1(3) . . . . ? C10 Zr C1 C2 78.5(2) . . . . ? C9 Zr C1 C2 31.9(3) . . . . ? C11 Zr C1 C2 128.9(2) . . . . ? C8 Zr C1 C2 -15.6(3) . . . . ? C12 Zr C1 C2 -166.5(2) . . . . ? C7 C1 C2 C3 7.7(5) . . . . ? Zr C1 C2 C3 53.6(3) . . . . ? C7 C1 C2 Zr -45.9(3) . . . . ? C3 Zr C2 C1 136.6(3) . . . . ? C6 Zr C2 C1 48.31(19) . . . . ? C5 Zr C2 C1 83.04(19) . . . . ? C4 Zr C2 C1 111.6(2) . . . . ? C7 Zr C2 C1 20.47(18) . . . . ? C10 Zr C2 C1 -127.47(19) . . . . ? C9 Zr C2 C1 -157.42(18) . . . . ? C11 Zr C2 C1 -112.2(3) . . . . ? C8 Zr C2 C1 170.18(18) . . . . ? C12 Zr C2 C1 154.1(5) . . . . ? C6 Zr C2 C3 -88.3(2) . . . . ? C5 Zr C2 C3 -53.6(2) . . . . ? C4 Zr C2 C3 -25.02(19) . . . . ? C7 Zr C2 C3 -116.2(2) . . . . ? C1 Zr C2 C3 -136.6(3) . . . . ? C10 Zr C2 C3 95.9(2) . . . . ? C9 Zr C2 C3 66.0(2) . . . . ? C11 Zr C2 C3 111.1(3) . . . . ? C8 Zr C2 C3 33.6(2) . . . . ? C12 Zr C2 C3 17.5(6) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? Zr C2 C3 C4 55.4(3) . . . . ? C1 C2 C3 Zr -55.0(3) . . . . ? C6 Zr C3 C4 -49.1(2) . . . . ? C5 Zr C3 C4 -19.64(18) . . . . ? C2 Zr C3 C4 -137.7(3) . . . . ? C7 Zr C3 C4 -83.2(2) . . . . ? C1 Zr C3 C4 -112.2(2) . . . . ? C10 Zr C3 C4 117.49(19) . . . . ? C9 Zr C3 C4 104.4(2) . . . . ? C11 Zr C3 C4 92.4(3) . . . . ? C8 Zr C3 C4 74.0(2) . . . . ? C12 Zr C3 C4 47.3(3) . . . . ? C6 Zr C3 C2 88.6(2) . . . . ? C5 Zr C3 C2 118.1(2) . . . . ? C4 Zr C3 C2 137.7(3) . . . . ? C7 Zr C3 C2 54.5(2) . . . . ? C1 Zr C3 C2 25.54(19) . . . . ? C10 Zr C3 C2 -104.8(2) . . . . ? C9 Zr C3 C2 -117.9(2) . . . . ? C11 Zr C3 C2 -129.9(2) . . . . ? C8 Zr C3 C2 -148.2(2) . . . . ? C12 Zr C3 C2 -174.94(18) . . . . ? C2 C3 C4 C5 -12.4(6) . . . . ? Zr C3 C4 C5 42.3(3) . . . . ? C2 C3 C4 Zr -54.7(3) . . . . ? C3 Zr C4 C5 -146.9(3) . . . . ? C6 Zr C4 C5 -23.91(18) . . . . ? C2 Zr C4 C5 -121.6(2) . . . . ? C7 Zr C4 C5 -55.62(19) . . . . ? C1 Zr C4 C5 -89.53(19) . . . . ? C10 Zr C4 C5 127.91(19) . . . . ? C9 Zr C4 C5 135.67(19) . . . . ? C11 Zr C4 C5 85.1(2) . . . . ? C8 Zr C4 C5 115.3(2) . . . . ? C12 Zr C4 C5 67.1(2) . . . . ? C6 Zr C4 C3 123.0(2) . . . . ? C5 Zr C4 C3 146.9(3) . . . . ? C2 Zr C4 C3 25.3(2) . . . . ? C7 Zr C4 C3 91.3(2) . . . . ? C1 Zr C4 C3 57.4(2) . . . . ? C10 Zr C4 C3 -85.2(2) . . . . ? C9 Zr C4 C3 -77.4(2) . . . . ? C11 Zr C4 C3 -128.0(2) . . . . ? C8 Zr C4 C3 -97.8(2) . . . . ? C12 Zr C4 C3 -146.01(19) . . . . ? C3 C4 C5 C6 9.7(6) . . . . ? Zr C4 C5 C6 51.7(3) . . . . ? C3 C4 C5 Zr -42.0(3) . . . . ? C3 Zr C5 C4 19.87(19) . . . . ? C6 Zr C5 C4 140.1(3) . . . . ? C2 Zr C5 C4 50.30(19) . . . . ? C7 Zr C5 C4 114.1(2) . . . . ? C1 Zr C5 C4 84.65(19) . . . . ? C10 Zr C5 C4 -85.3(2) . . . . ? C9 Zr C5 C4 -53.2(2) . . . . ? C11 Zr C5 C4 -121.26(19) . . . . ? C8 Zr C5 C4 -59.96(19) . . . . ? C12 Zr C5 C4 -118.02(19) . . . . ? C3 Zr C5 C6 -120.2(2) . . . . ? C2 Zr C5 C6 -89.81(19) . . . . ? C4 Zr C5 C6 -140.1(3) . . . . ? C7 Zr C5 C6 -26.05(17) . . . . ? C1 Zr C5 C6 -55.46(19) . . . . ? C10 Zr C5 C6 134.6(2) . . . . ? C9 Zr C5 C6 166.70(17) . . . . ? C11 Zr C5 C6 98.63(19) . . . . ? C8 Zr C5 C6 159.92(19) . . . . ? C12 Zr C5 C6 101.87(19) . . . . ? C4 C5 C6 C7 4.2(5) . . . . ? Zr C5 C6 C7 56.9(3) . . . . ? C4 C5 C6 Zr -52.6(3) . . . . ? C3 Zr C6 C7 -83.7(2) . . . . ? C5 Zr C6 C7 -135.6(3) . . . . ? C2 Zr C6 C7 -48.75(19) . . . . ? C4 Zr C6 C7 -112.1(2) . . . . ? C1 Zr C6 C7 -20.85(17) . . . . ? C10 Zr C6 C7 123.2(2) . . . . ? C9 Zr C6 C7 -161.5(2) . . . . ? C11 Zr C6 C7 120.75(18) . . . . ? C8 Zr C6 C7 -159.36(17) . . . . ? C12 Zr C6 C7 143.25(18) . . . . ? C3 Zr C6 C5 51.9(2) . . . . ? C2 Zr C6 C5 86.9(2) . . . . ? C4 Zr C6 C5 23.50(18) . . . . ? C7 Zr C6 C5 135.6(3) . . . . ? C1 Zr C6 C5 114.8(2) . . . . ? C10 Zr C6 C5 -101.2(3) . . . . ? C9 Zr C6 C5 -25.9(3) . . . . ? C11 Zr C6 C5 -103.6(2) . . . . ? C8 Zr C6 C5 -23.8(2) . . . . ? C12 Zr C6 C5 -81.15(19) . . . . ? C2 C1 C7 C6 -0.4(5) . . . . ? Zr C1 C7 C6 -45.5(3) . . . . ? C2 C1 C7 Zr 45.1(3) . . . . ? C5 C6 C7 C1 -9.4(5) . . . . ? Zr C6 C7 C1 46.4(3) . . . . ? C5 C6 C7 Zr -55.8(3) . . . . ? C3 Zr C7 C1 -52.09(19) . . . . ? C6 Zr C7 C1 -144.5(3) . . . . ? C5 Zr C7 C1 -118.0(2) . . . . ? C2 Zr C7 C1 -20.94(18) . . . . ? C4 Zr C7 C1 -86.82(19) . . . . ? C10 Zr C7 C1 87.4(3) . . . . ? C9 Zr C7 C1 -10.7(6) . . . . ? C11 Zr C7 C1 131.33(19) . . . . ? C8 Zr C7 C1 -105.4(3) . . . . ? C12 Zr C7 C1 169.83(17) . . . . ? C3 Zr C7 C6 92.4(2) . . . . ? C5 Zr C7 C6 26.51(18) . . . . ? C2 Zr C7 C6 123.6(2) . . . . ? C4 Zr C7 C6 57.71(19) . . . . ? C1 Zr C7 C6 144.5(3) . . . . ? C10 Zr C7 C6 -128.1(2) . . . . ? C9 Zr C7 C6 133.8(5) . . . . ? C11 Zr C7 C6 -84.1(2) . . . . ? C8 Zr C7 C6 39.1(3) . . . . ? C12 Zr C7 C6 -45.6(2) . . . . ? C12 B C8 C9 6.2(4) . . . . ? C13 B C8 C9 -171.2(3) . . . . ? Zr B C8 C9 60.4(3) . . . . ? C12 B C8 Zr -54.2(2) . . . . ? C13 B C8 Zr 128.3(3) . . . . ? C3 Zr C8 C9 103.8(2) . . . . ? C6 Zr C8 C9 -178.10(19) . . . . ? C5 Zr C8 C9 168.7(2) . . . . ? C2 Zr C8 C9 85.1(2) . . . . ? C4 Zr C8 C9 138.3(2) . . . . ? C7 Zr C8 C9 157.5(2) . . . . ? C1 Zr C8 C9 94.4(2) . . . . ? C10 Zr C8 C9 -29.81(19) . . . . ? C11 Zr C8 C9 -64.9(2) . . . . ? C12 Zr C8 C9 -98.9(2) . . . . ? C3 Zr C8 B -126.6(2) . . . . ? C6 Zr C8 B -48.5(2) . . . . ? C5 Zr C8 B -61.75(19) . . . . ? C2 Zr C8 B -145.32(18) . . . . ? C4 Zr C8 B -92.08(19) . . . . ? C7 Zr C8 B -73.0(3) . . . . ? C1 Zr C8 B -136.0(2) . . . . ? C10 Zr C8 B 99.8(2) . . . . ? C9 Zr C8 B 129.6(3) . . . . ? C11 Zr C8 B 64.62(19) . . . . ? C12 Zr C8 B 30.68(17) . . . . ? B C8 C9 C10 -3.3(5) . . . . ? Zr C8 C9 C10 60.0(3) . . . . ? B C8 C9 Zr -63.3(3) . . . . ? C3 Zr C9 C8 -73.3(2) . . . . ? C6 Zr C9 C8 3.6(3) . . . . ? C5 Zr C9 C8 -13.1(2) . . . . ? C2 Zr C9 C8 -104.8(2) . . . . ? C4 Zr C9 C8 -39.9(2) . . . . ? C7 Zr C9 C8 -114.3(5) . . . . ? C1 Zr C9 C8 -122.6(2) . . . . ? C10 Zr C9 C8 128.7(3) . . . . ? C11 Zr C9 C8 98.5(2) . . . . ? C12 Zr C9 C8 65.23(19) . . . . ? C3 Zr C9 C10 158.0(2) . . . . ? C6 Zr C9 C10 -125.1(3) . . . . ? C5 Zr C9 C10 -141.75(19) . . . . ? C2 Zr C9 C10 126.6(2) . . . . ? C4 Zr C9 C10 -168.5(2) . . . . ? C7 Zr C9 C10 117.1(5) . . . . ? C1 Zr C9 C10 108.7(2) . . . . ? C11 Zr C9 C10 -30.12(19) . . . . ? C8 Zr C9 C10 -128.7(3) . . . . ? C12 Zr C9 C10 -63.42(19) . . . . ? C8 C9 C10 C11 1.3(4) . . . . ? Zr C9 C10 C11 63.0(3) . . . . ? C8 C9 C10 Zr -61.7(3) . . . . ? C3 Zr C10 C9 -25.2(2) . . . . ? C6 Zr C10 C9 123.9(3) . . . . ? C5 Zr C10 C9 59.9(3) . . . . ? C2 Zr C10 C9 -65.5(2) . . . . ? C4 Zr C10 C9 14.6(3) . . . . ? C7 Zr C10 C9 -158.1(2) . . . . ? C1 Zr C10 C9 -105.6(2) . . . . ? C11 Zr C10 C9 127.9(3) . . . . ? C8 Zr C10 C9 29.14(18) . . . . ? C12 Zr C10 C9 100.1(2) . . . . ? C3 Zr C10 C11 -153.07(19) . . . . ? C6 Zr C10 C11 -3.9(3) . . . . ? C5 Zr C10 C11 -67.9(3) . . . . ? C2 Zr C10 C11 166.68(19) . . . . ? C4 Zr C10 C11 -113.3(2) . . . . ? C7 Zr C10 C11 74.0(3) . . . . ? C1 Zr C10 C11 126.6(2) . . . . ? C9 Zr C10 C11 -127.9(3) . . . . ? C8 Zr C10 C11 -98.7(2) . . . . ? C12 Zr C10 C11 -27.79(18) . . . . ? C9 C10 C11 C12 -2.8(5) . . . . ? Zr C10 C11 C12 59.8(3) . . . . ? C9 C10 C11 Zr -62.7(3) . . . . ? C3 Zr C11 C12 -86.4(3) . . . . ? C6 Zr C11 C12 47.2(2) . . . . ? C5 Zr C11 C12 6.3(2) . . . . ? C2 Zr C11 C12 -155.6(2) . . . . ? C4 Zr C11 C12 -35.1(3) . . . . ? C7 Zr C11 C12 87.6(2) . . . . ? C1 Zr C11 C12 135.4(2) . . . . ? C10 Zr C11 C12 -130.7(3) . . . . ? C9 Zr C11 C12 -100.8(2) . . . . ? C8 Zr C11 C12 -66.7(2) . . . . ? C3 Zr C11 C10 44.3(3) . . . . ? C6 Zr C11 C10 177.94(18) . . . . ? C5 Zr C11 C10 137.01(19) . . . . ? C2 Zr C11 C10 -24.8(3) . . . . ? C4 Zr C11 C10 95.7(2) . . . . ? C7 Zr C11 C10 -141.64(19) . . . . ? C1 Zr C11 C10 -93.8(2) . . . . ? C9 Zr C11 C10 29.94(18) . . . . ? C8 Zr C11 C10 64.06(19) . . . . ? C12 Zr C11 C10 130.7(3) . . . . ? C10 C11 C12 B 6.4(5) . . . . ? Zr C11 C12 B 64.3(3) . . . . ? C10 C11 C12 Zr -58.0(3) . . . . ? C8 B C12 C11 -7.7(4) . . . . ? C13 B C12 C11 169.7(3) . . . . ? Zr B C12 C11 -61.6(3) . . . . ? C8 B C12 Zr 54.0(2) . . . . ? C13 B C12 Zr -128.7(3) . . . . ? C3 Zr C12 C11 128.6(2) . . . . ? C6 Zr C12 C11 -140.6(2) . . . . ? C5 Zr C12 C11 -174.7(2) . . . . ? C2 Zr C12 C11 115.0(5) . . . . ? C4 Zr C12 C11 154.3(2) . . . . ? C7 Zr C12 C11 -116.8(2) . . . . ? C1 Zr C12 C11 -102.8(3) . . . . ? C10 Zr C12 C11 28.85(19) . . . . ? C9 Zr C12 C11 63.3(2) . . . . ? C8 Zr C12 C11 97.2(2) . . . . ? C3 Zr C12 B 0.4(3) . . . . ? C6 Zr C12 B 91.20(19) . . . . ? C5 Zr C12 B 57.05(19) . . . . ? C2 Zr C12 B -13.2(6) . . . . ? C4 Zr C12 B 26.1(2) . . . . ? C7 Zr C12 B 114.98(19) . . . . ? C1 Zr C12 B 129.0(3) . . . . ? C10 Zr C12 B -99.4(2) . . . . ? C9 Zr C12 B -64.90(19) . . . . ? C11 Zr C12 B -128.2(3) . . . . ? C8 Zr C12 B -31.08(17) . . . . ? C3' Zr' P' C15' 36.05(15) . . . . ? C5' Zr' P' C15' 125.25(17) . . . . ? C6' Zr' P' C15' 129.57(14) . . . . ? C2' Zr' P' C15' 45.08(14) . . . . ? C4' Zr' P' C15' 66.7(2) . . . . ? C7' Zr' P' C15' 108.35(14) . . . . ? C1' Zr' P' C15' 74.12(14) . . . . ? C10' Zr' P' C15' -79.82(14) . . . . ? C9' Zr' P' C15' -60.74(14) . . . . ? C11' Zr' P' C15' -112.84(14) . . . . ? C12' Zr' P' C15' -129.70(14) . . . . ? C8' Zr' P' C15' -70.74(16) . . . . ? C3' Zr' P' C14' -81.57(17) . . . . ? C5' Zr' P' C14' 7.63(19) . . . . ? C6' Zr' P' C14' 11.95(16) . . . . ? C2' Zr' P' C14' -72.54(16) . . . . ? C4' Zr' P' C14' -50.9(2) . . . . ? C7' Zr' P' C14' -9.27(16) . . . . ? C1' Zr' P' C14' -43.50(16) . . . . ? C10' Zr' P' C14' 162.56(16) . . . . ? C9' Zr' P' C14' -178.37(16) . . . . ? C11' Zr' P' C14' 129.53(16) . . . . ? C12' Zr' P' C14' 112.68(16) . . . . ? C8' Zr' P' C14' 171.64(17) . . . . ? C3' Zr' P' C16' 152.53(17) . . . . ? C5' Zr' P' C16' -118.26(18) . . . . ? C6' Zr' P' C16' -113.94(16) . . . . ? C2' Zr' P' C16' 161.57(16) . . . . ? C4' Zr' P' C16' -176.8(2) . . . . ? C7' Zr' P' C16' -135.17(16) . . . . ? C1' Zr' P' C16' -169.39(17) . . . . ? C10' Zr' P' C16' 36.66(16) . . . . ? C9' Zr' P' C16' 55.74(16) . . . . ? C11' Zr' P' C16' 3.64(16) . . . . ? C12' Zr' P' C16' -13.22(16) . . . . ? C8' Zr' P' C16' 45.75(18) . . . . ? C3' Zr' B' C12' 177.06(19) . . . . ? C5' Zr' B' C12' 116.5(2) . . . . ? C6' Zr' B' C12' 90.94(19) . . . . ? C2' Zr' B' C12' -178.97(18) . . . . ? C4' Zr' B' C12' 152.0(2) . . . . ? C7' Zr' B' C12' 88.7(2) . . . . ? C1' Zr' B' C12' 132.7(3) . . . . ? C10' Zr' B' C12' -63.99(19) . . . . ? C9' Zr' B' C12' -98.4(2) . . . . ? C11' Zr' B' C12' -29.63(17) . . . . ? C8' Zr' B' C12' -126.7(3) . . . . ? C3' Zr' B' C8' -56.2(2) . . . . ? C5' Zr' B' C8' -116.8(2) . . . . ? C6' Zr' B' C8' -142.34(19) . . . . ? C2' Zr' B' C8' -52.3(2) . . . . ? C4' Zr' B' C8' -81.31(19) . . . . ? C7' Zr' B' C8' -144.54(18) . . . . ? C1' Zr' B' C8' -100.6(3) . . . . ? C10' Zr' B' C8' 62.73(19) . . . . ? C9' Zr' B' C8' 28.29(18) . . . . ? C11' Zr' B' C8' 97.1(2) . . . . ? C12' Zr' B' C8' 126.7(3) . . . . ? C3' Zr' B' C13' 61.3(4) . . . . ? C5' Zr' B' C13' 0.7(3) . . . . ? C6' Zr' B' C13' -24.9(4) . . . . ? C2' Zr' B' C13' 65.2(4) . . . . ? C4' Zr' B' C13' 36.2(3) . . . . ? C7' Zr' B' C13' -27.1(4) . . . . ? C1' Zr' B' C13' 16.9(5) . . . . ? C10' Zr' B' C13' -179.8(4) . . . . ? C9' Zr' B' C13' 145.8(4) . . . . ? C11' Zr' B' C13' -145.4(4) . . . . ? C12' Zr' B' C13' -115.8(4) . . . . ? C8' Zr' B' C13' 117.5(4) . . . . ? C3' Zr' C1' C7' -120.2(2) . . . . ? C5' Zr' C1' C7' -53.78(19) . . . . ? C6' Zr' C1' C7' -22.17(18) . . . . ? C2' Zr' C1' C7' -145.7(3) . . . . ? C4' Zr' C1' C7' -88.50(19) . . . . ? C10' Zr' C1' C7' 133.31(19) . . . . ? C9' Zr' C1' C7' -179.99(18) . . . . ? C11' Zr' C1' C7' 82.6(2) . . . . ? C12' Zr' C1' C7' 16.0(3) . . . . ? C8' Zr' C1' C7' -132.5(2) . . . . ? C3' Zr' C1' C2' 25.51(19) . . . . ? C5' Zr' C1' C2' 91.9(2) . . . . ? C6' Zr' C1' C2' 123.5(2) . . . . ? C4' Zr' C1' C2' 57.22(19) . . . . ? C7' Zr' C1' C2' 145.7(3) . . . . ? C10' Zr' C1' C2' -81.0(2) . . . . ? C9' Zr' C1' C2' -34.3(2) . . . . ? C11' Zr' C1' C2' -131.6(2) . . . . ? C12' Zr' C1' C2' 161.7(2) . . . . ? C8' Zr' C1' C2' 13.3(3) . . . . ? C7' C1' C2' C3' -8.2(5) . . . . ? Zr' C1' C2' C3' -53.2(3) . . . . ? C7' C1' C2' Zr' 45.0(3) . . . . ? C3' Zr' C2' C1' -137.4(3) . . . . ? C5' Zr' C2' C1' -83.48(19) . . . . ? C6' Zr' C2' C1' -48.66(19) . . . . ? C4' Zr' C2' C1' -112.6(2) . . . . ? C7' Zr' C2' C1' -20.24(18) . . . . ? C10' Zr' C2' C1' 126.33(18) . . . . ? C9' Zr' C2' C1' 155.77(18) . . . . ? C11' Zr' C2' C1' 112.1(3) . . . . ? C12' Zr' C2' C1' -146.8(4) . . . . ? C8' Zr' C2' C1' -171.56(18) . . . . ? C5' Zr' C2' C3' 53.9(2) . . . . ? C6' Zr' C2' C3' 88.7(2) . . . . ? C4' Zr' C2' C3' 24.77(19) . . . . ? C7' Zr' C2' C3' 117.2(2) . . . . ? C1' Zr' C2' C3' 137.4(3) . . . . ? C10' Zr' C2' C3' -96.3(2) . . . . ? C9' Zr' C2' C3' -66.8(2) . . . . ? C11' Zr' C2' C3' -110.5(3) . . . . ? C12' Zr' C2' C3' -9.3(6) . . . . ? C8' Zr' C2' C3' -34.2(2) . . . . ? C1' C2' C3' C4' -0.4(5) . . . . ? Zr' C2' C3' C4' -55.1(3) . . . . ? C1' C2' C3' Zr' 54.7(3) . . . . ? C5' Zr' C3' C4' 20.49(18) . . . . ? C6' Zr' C3' C4' 50.07(19) . . . . ? C2' Zr' C3' C4' 138.1(3) . . . . ? C7' Zr' C3' C4' 84.44(19) . . . . ? C1' Zr' C3' C4' 113.2(2) . . . . ? C10' Zr' C3' C4' -116.03(19) . . . . ? C9' Zr' C3' C4' -104.18(19) . . . . ? C11' Zr' C3' C4' -88.9(2) . . . . ? C12' Zr' C3' C4' -44.8(2) . . . . ? C8' Zr' C3' C4' -74.27(19) . . . . ? C5' Zr' C3' C2' -117.6(2) . . . . ? C6' Zr' C3' C2' -88.0(2) . . . . ? C4' Zr' C3' C2' -138.1(3) . . . . ? C7' Zr' C3' C2' -53.7(2) . . . . ? C1' Zr' C3' C2' -24.94(18) . . . . ? C10' Zr' C3' C2' 105.9(2) . . . . ? C9' Zr' C3' C2' 117.7(2) . . . . ? C11' Zr' C3' C2' 133.0(2) . . . . ? C12' Zr' C3' C2' 177.11(18) . . . . ? C8' Zr' C3' C2' 147.6(2) . . . . ? C2' C3' C4' C5' 11.3(5) . . . . ? Zr' C3' C4' C5' -43.3(3) . . . . ? C2' C3' C4' Zr' 54.6(3) . . . . ? C5' Zr' C4' C3' -145.7(3) . . . . ? C6' Zr' C4' C3' -122.1(2) . . . . ? C2' Zr' C4' C3' -25.01(18) . . . . ? C7' Zr' C4' C3' -90.38(19) . . . . ? C1' Zr' C4' C3' -56.42(19) . . . . ? C10' Zr' C4' C3' 87.8(2) . . . . ? C9' Zr' C4' C3' 78.43(19) . . . . ? C11' Zr' C4' C3' 130.13(18) . . . . ? C12' Zr' C4' C3' 147.32(18) . . . . ? C8' Zr' C4' C3' 97.8(2) . . . . ? C3' Zr' C4' C5' 145.7(3) . . . . ? C6' Zr' C4' C5' 23.58(17) . . . . ? C2' Zr' C4' C5' 120.7(2) . . . . ? C7' Zr' C4' C5' 55.30(18) . . . . ? C1' Zr' C4' C5' 89.25(18) . . . . ? C10' Zr' C4' C5' -126.57(18) . . . . ? C9' Zr' C4' C5' -135.89(18) . . . . ? C11' Zr' C4' C5' -84.2(2) . . . . ? C12' Zr' C4' C5' -67.00(19) . . . . ? C8' Zr' C4' C5' -116.56(19) . . . . ? C3' C4' C5' C6' -8.6(5) . . . . ? Zr' C4' C5' C6' -51.8(3) . . . . ? C3' C4' C5' Zr' 43.2(3) . . . . ? C3' Zr' C5' C4' -20.48(17) . . . . ? C6' Zr' C5' C4' -140.6(3) . . . . ? C2' Zr' C5' C4' -50.88(18) . . . . ? C7' Zr' C5' C4' -114.7(2) . . . . ? C1' Zr' C5' C4' -84.85(18) . . . . ? C10' Zr' C5' C4' 87.4(2) . . . . ? C9' Zr' C5' C4' 53.7(2) . . . . ? C11' Zr' C5' C4' 121.20(18) . . . . ? C12' Zr' C5' C4' 117.29(18) . . . . ? C8' Zr' C5' C4' 59.01(18) . . . . ? C3' Zr' C5' C6' 120.1(2) . . . . ? C2' Zr' C5' C6' 89.75(19) . . . . ? C4' Zr' C5' C6' 140.6(3) . . . . ? C7' Zr' C5' C6' 25.90(18) . . . . ? C1' Zr' C5' C6' 55.77(19) . . . . ? C10' Zr' C5' C6' -132.0(2) . . . . ? C9' Zr' C5' C6' -165.71(17) . . . . ? C11' Zr' C5' C6' -98.18(19) . . . . ? C12' Zr' C5' C6' -102.09(19) . . . . ? C8' Zr' C5' C6' -160.36(19) . . . . ? C4' C5' C6' C7' -3.5(5) . . . . ? Zr' C5' C6' C7' -56.0(3) . . . . ? C4' C5' C6' Zr' 52.5(3) . . . . ? C3' Zr' C6' C5' -51.92(19) . . . . ? C2' Zr' C6' C5' -86.66(19) . . . . ? C4' Zr' C6' C5' -23.33(18) . . . . ? C7' Zr' C6' C5' -136.1(3) . . . . ? C1' Zr' C6' C5' -114.4(2) . . . . ? C10' Zr' C6' C5' 102.2(3) . . . . ? C9' Zr' C6' C5' 28.6(3) . . . . ? C11' Zr' C6' C5' 102.95(19) . . . . ? C12' Zr' C6' C5' 80.10(19) . . . . ? C8' Zr' C6' C5' 23.5(2) . . . . ? C3' Zr' C6' C7' 84.17(19) . . . . ? C5' Zr' C6' C7' 136.1(3) . . . . ? C2' Zr' C6' C7' 49.43(19) . . . . ? C4' Zr' C6' C7' 112.8(2) . . . . ? C1' Zr' C6' C7' 21.71(18) . . . . ? C10' Zr' C6' C7' -121.7(2) . . . . ? C9' Zr' C6' C7' 164.7(2) . . . . ? C11' Zr' C6' C7' -120.96(19) . . . . ? C12' Zr' C6' C7' -143.81(19) . . . . ? C8' Zr' C6' C7' 159.62(18) . . . . ? C2' C1' C7' C6' 2.5(5) . . . . ? Zr' C1' C7' C6' 46.9(3) . . . . ? C2' C1' C7' Zr' -44.4(3) . . . . ? C5' C6' C7' C1' 6.7(5) . . . . ? Zr' C6' C7' C1' -48.1(3) . . . . ? C5' C6' C7' Zr' 54.8(3) . . . . ? C3' Zr' C7' C1' 51.03(19) . . . . ? C5' Zr' C7' C1' 116.8(2) . . . . ? C6' Zr' C7' C1' 143.0(3) . . . . ? C2' Zr' C7' C1' 20.41(18) . . . . ? C4' Zr' C7' C1' 85.60(19) . . . . ? C10' Zr' C7' C1' -91.5(3) . . . . ? C9' Zr' C7' C1' 0.0(7) . . . . ? C11' Zr' C7' C1' -133.93(18) . . . . ? C12' Zr' C7' C1' -172.37(17) . . . . ? C8' Zr' C7' C1' 102.9(3) . . . . ? C3' Zr' C7' C6' -92.0(2) . . . . ? C5' Zr' C7' C6' -26.20(19) . . . . ? C2' Zr' C7' C6' -122.6(2) . . . . ? C4' Zr' C7' C6' -57.41(19) . . . . ? C1' Zr' C7' C6' -143.0(3) . . . . ? C10' Zr' C7' C6' 125.5(2) . . . . ? C9' Zr' C7' C6' -143.0(5) . . . . ? C11' Zr' C7' C6' 83.1(2) . . . . ? C12' Zr' C7' C6' 44.6(2) . . . . ? C8' Zr' C7' C6' -40.1(3) . . . . ? C12' B' C8' C9' -5.7(4) . . . . ? C13' B' C8' C9' 171.5(3) . . . . ? Zr' B' C8' C9' -60.0(3) . . . . ? C12' B' C8' Zr' 54.2(2) . . . . ? C13' B' C8' Zr' -128.5(3) . . . . ? C3' Zr' C8' C9' -106.6(2) . . . . ? C5' Zr' C8' C9' -171.2(2) . . . . ? C6' Zr' C8' C9' 175.68(18) . . . . ? C2' Zr' C8' C9' -87.7(2) . . . . ? C4' Zr' C8' C9' -141.0(2) . . . . ? C7' Zr' C8' C9' -158.8(2) . . . . ? C1' Zr' C8' C9' -95.5(2) . . . . ? C10' Zr' C8' C9' 29.70(19) . . . . ? C11' Zr' C8' C9' 64.50(19) . . . . ? C12' Zr' C8' C9' 98.8(2) . . . . ? C3' Zr' C8' B' 123.8(2) . . . . ? C5' Zr' C8' B' 59.1(2) . . . . ? C6' Zr' C8' B' 46.0(2) . . . . ? C2' Zr' C8' B' 142.61(19) . . . . ? C4' Zr' C8' B' 89.4(2) . . . . ? C7' Zr' C8' B' 71.5(3) . . . . ? C1' Zr' C8' B' 134.8(2) . . . . ? C10' Zr' C8' B' -100.0(2) . . . . ? C9' Zr' C8' B' -129.7(3) . . . . ? C11' Zr' C8' B' -65.18(19) . . . . ? C12' Zr' C8' B' -30.88(18) . . . . ? B' C8' C9' C10' 2.0(5) . . . . ? Zr' C8' C9' C10' -60.5(3) . . . . ? B' C8' C9' Zr' 62.5(3) . . . . ? C3' Zr' C9' C8' 71.0(2) . . . . ? C5' Zr' C9' C8' 10.3(2) . . . . ? C6' Zr' C9' C8' -8.3(4) . . . . ? C2' Zr' C9' C8' 102.5(2) . . . . ? C4' Zr' C9' C8' 37.6(2) . . . . ? C7' Zr' C9' C8' 121.4(5) . . . . ? C1' Zr' C9' C8' 121.5(2) . . . . ? C10' Zr' C9' C8' -128.6(3) . . . . ? C11' Zr' C9' C8' -98.8(2) . . . . ? C12' Zr' C9' C8' -65.4(2) . . . . ? C3' Zr' C9' C10' -160.3(2) . . . . ? C5' Zr' C9' C10' 138.93(19) . . . . ? C6' Zr' C9' C10' 120.3(3) . . . . ? C2' Zr' C9' C10' -128.89(19) . . . . ? C4' Zr' C9' C10' 166.20(19) . . . . ? C7' Zr' C9' C10' -109.9(6) . . . . ? C1' Zr' C9' C10' -109.9(2) . . . . ? C11' Zr' C9' C10' 29.83(18) . . . . ? C12' Zr' C9' C10' 63.20(19) . . . . ? C8' Zr' C9' C10' 128.6(3) . . . . ? C8' C9' C10' C11' 0.0(5) . . . . ? Zr' C9' C10' C11' -62.0(3) . . . . ? C8' C9' C10' Zr' 62.0(3) . . . . ? C3' Zr' C10' C9' 22.9(2) . . . . ? C5' Zr' C10' C9' -64.0(3) . . . . ? C6' Zr' C10' C9' -126.9(3) . . . . ? C2' Zr' C10' C9' 63.7(2) . . . . ? C4' Zr' C10' C9' -17.7(2) . . . . ? C7' Zr' C10' C9' 158.6(2) . . . . ? C1' Zr' C10' C9' 104.7(2) . . . . ? C11' Zr' C10' C9' -128.1(3) . . . . ? C12' Zr' C10' C9' -100.5(2) . . . . ? C8' Zr' C10' C9' -29.22(19) . . . . ? C3' Zr' C10' C11' 151.03(18) . . . . ? C5' Zr' C10' C11' 64.1(3) . . . . ? C6' Zr' C10' C11' 1.3(3) . . . . ? C2' Zr' C10' C11' -168.20(18) . . . . ? C4' Zr' C10' C11' 110.4(2) . . . . ? C7' Zr' C10' C11' -73.3(3) . . . . ? C1' Zr' C10' C11' -127.2(2) . . . . ? C9' Zr' C10' C11' 128.1(3) . . . . ? C12' Zr' C10' C11' 27.66(18) . . . . ? C8' Zr' C10' C11' 98.9(2) . . . . ? C9' C10' C11' C12' 2.5(5) . . . . ? Zr' C10' C11' C12' -59.4(3) . . . . ? C9' C10' C11' Zr' 61.9(3) . . . . ? C3' Zr' C11' C12' 83.3(3) . . . . ? C5' Zr' C11' C12' -7.6(2) . . . . ? C6' Zr' C11' C12' -47.9(2) . . . . ? C2' Zr' C11' C12' 154.3(2) . . . . ? C4' Zr' C11' C12' 33.4(2) . . . . ? C7' Zr' C11' C12' -88.0(2) . . . . ? C1' Zr' C11' C12' -134.7(2) . . . . ? C10' Zr' C11' C12' 131.4(3) . . . . ? C9' Zr' C11' C12' 101.6(2) . . . . ? C8' Zr' C11' C12' 67.43(19) . . . . ? C3' Zr' C11' C10' -48.1(3) . . . . ? C5' Zr' C11' C10' -138.92(19) . . . . ? C6' Zr' C11' C10' -179.31(18) . . . . ? C2' Zr' C11' C10' 22.9(3) . . . . ? C4' Zr' C11' C10' -98.0(2) . . . . ? C7' Zr' C11' C10' 140.68(18) . . . . ? C1' Zr' C11' C10' 93.9(2) . . . . ? C9' Zr' C11' C10' -29.78(18) . . . . ? C12' Zr' C11' C10' -131.4(3) . . . . ? C8' Zr' C11' C10' -63.93(19) . . . . ? C10' C11' C12' B' -6.9(5) . . . . ? Zr' C11' C12' B' -65.1(3) . . . . ? C10' C11' C12' Zr' 58.3(3) . . . . ? C8' B' C12' C11' 8.0(4) . . . . ? C13' B' C12' C11' -169.3(3) . . . . ? Zr' B' C12' C11' 62.6(3) . . . . ? C8' B' C12' Zr' -54.6(2) . . . . ? C13' B' C12' Zr' 128.1(3) . . . . ? C3' Zr' C12' C11' -131.01(19) . . . . ? C5' Zr' C12' C11' 173.54(19) . . . . ? C6' Zr' C12' C11' 139.48(19) . . . . ? C2' Zr' C12' C11' -123.9(5) . . . . ? C4' Zr' C12' C11' -155.25(18) . . . . ? C7' Zr' C12' C11' 116.01(19) . . . . ? C1' Zr' C12' C11' 105.5(3) . . . . ? C10' Zr' C12' C11' -28.24(17) . . . . ? C9' Zr' C12' C11' -62.41(19) . . . . ? C8' Zr' C12' C11' -96.2(2) . . . . ? C3' Zr' C12' B' -3.9(3) . . . . ? C5' Zr' C12' B' -59.4(2) . . . . ? C6' Zr' C12' B' -93.4(2) . . . . ? C2' Zr' C12' B' 3.2(6) . . . . ? C4' Zr' C12' B' -28.2(2) . . . . ? C7' Zr' C12' B' -116.9(2) . . . . ? C1' Zr' C12' B' -127.4(3) . . . . ? C10' Zr' C12' B' 98.8(2) . . . . ? C9' Zr' C12' B' 64.67(19) . . . . ? C11' Zr' C12' B' 127.1(3) . . . . ? C8' Zr' C12' B' 30.89(18) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 70.07 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.830 _refine_diff_density_min -0.534 _refine_diff_density_rms 0.079 # Attachment 'andyg76c.cif' data_andyg76c _database_code_depnum_ccdc_archive 'CCDC 864985' #TrackingRef 'andyg76c.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C17 H21 B Si Zr' _chemical_formula_weight 355.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 17.5992(6) _cell_length_b 8.0986(3) _cell_length_c 11.9967(5) _cell_angle_alpha 90.00 _cell_angle_beta 102.029(4) _cell_angle_gamma 90.00 _cell_volume 1672.33(10) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 7846 _cell_measurement_theta_min 3.7613 _cell_measurement_theta_max 75.5525 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.412 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_absorpt_coefficient_mu 5.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.15185 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'Nova (Cu) X-ray Source' _diffrn_radiation_monochromator mirror _diffrn_measurement_device_type 'Xcalibur, Atlas, Nova' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3543 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3635 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0216 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 5.14 _diffrn_reflns_theta_max 66.58 _reflns_number_total 3635 _reflns_number_gt 3239 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET) (compiled Aug 3 2011,13:03:54) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'BRUKER XP' _computing_publication_material SHELXL-97 _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. The crystal was a non-merohedral twin, formed by 180 degree rotation about the a axis. The structure was refined using the 'HKLF 5' option, whereby the scale factor refined to 0.217(2). Because of overlapped reflections, the number of reflections is difficult to define and should be interpreted with caution; the untwinning routine merges all equivalent reflections and so R(int) is not defined. The hydrogens of the seven-membered ring were refined freely. ; _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^)+(0.1037P)^2^+4.4581P] 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 3635 _refine_ls_number_parameters 206 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.0642 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1571 _refine_ls_wR_factor_gt 0.1505 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.061 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Zr Zr 0.14282(2) 0.70933(5) 0.29862(4) 0.02530(19) Uani 1 1 d . . . Si Si 0.41135(9) 0.31879(19) 0.60755(13) 0.0301(3) Uani 1 1 d . . . B B 0.2879(4) 0.7601(8) 0.4082(6) 0.0283(13) Uani 1 1 d . . . C1 C 0.1633(3) 0.4249(6) 0.3006(5) 0.0299(11) Uani 1 1 d D . . H1 H 0.213(2) 0.376(7) 0.308(5) 0.036 Uiso 1 1 d D . . C2 C 0.1391(4) 0.4668(7) 0.4022(5) 0.0333(12) Uani 1 1 d D . . H2 H 0.173(3) 0.426(8) 0.469(4) 0.040 Uiso 1 1 d D . . C3 C 0.0748(4) 0.5639(8) 0.4170(6) 0.0389(15) Uani 1 1 d D . . H3 H 0.073(4) 0.603(8) 0.491(4) 0.047 Uiso 1 1 d D . . C4 C 0.0197(4) 0.6444(8) 0.3312(8) 0.0503(19) Uani 1 1 d D . . H4 H -0.019(4) 0.705(9) 0.358(7) 0.060 Uiso 1 1 d D . . C5 C 0.0146(4) 0.6475(8) 0.2121(9) 0.059(2) Uani 1 1 d D . . H5 H -0.029(4) 0.715(9) 0.184(7) 0.071 Uiso 1 1 d D . . C6 C 0.0634(4) 0.5704(8) 0.1471(6) 0.0472(17) Uani 1 1 d D . . H6 H 0.056(4) 0.589(10) 0.068(3) 0.057 Uiso 1 1 d D . . C7 C 0.1302(4) 0.4696(7) 0.1875(5) 0.0340(13) Uani 1 1 d D . . H7 H 0.159(3) 0.439(8) 0.132(4) 0.041 Uiso 1 1 d D . . C8 C 0.2334(3) 0.8738(6) 0.4535(4) 0.0270(11) Uani 1 1 d . . . H8 H 0.2307 0.8676 0.5316 0.032 Uiso 1 1 calc R . . C9 C 0.1869(3) 0.9881(7) 0.3830(5) 0.0308(12) Uani 1 1 d . . . H9 H 0.1553 1.0616 0.4151 0.037 Uiso 1 1 calc R . . C10 C 0.1858(3) 0.9970(6) 0.2652(5) 0.0282(11) Uani 1 1 d . . . H10 H 0.1523 1.0735 0.2189 0.034 Uiso 1 1 calc R . . C11 C 0.2341(3) 0.8926(7) 0.2153(5) 0.0294(11) Uani 1 1 d . . . H11 H 0.2336 0.9024 0.1362 0.035 Uiso 1 1 calc R . . C12 C 0.2830(3) 0.7743(7) 0.2807(5) 0.0271(11) Uani 1 1 d . . . H12 H 0.3132 0.7028 0.2446 0.032 Uiso 1 1 calc R . . C13 C 0.3363(3) 0.6238(7) 0.4805(5) 0.0293(11) Uani 1 1 d . . . C14 C 0.3696(3) 0.5072(7) 0.5346(5) 0.0329(12) Uani 1 1 d . . . C15 C 0.5015(4) 0.3732(9) 0.7121(6) 0.0444(15) Uani 1 1 d . . . H15A H 0.5379 0.4282 0.6726 0.067 Uiso 1 1 calc R . . H15B H 0.5254 0.2725 0.7490 0.067 Uiso 1 1 calc R . . H15C H 0.4887 0.4477 0.7699 0.067 Uiso 1 1 calc R . . C16 C 0.3371(4) 0.2284(7) 0.6790(6) 0.0374(14) Uani 1 1 d . . . H16A H 0.3271 0.3046 0.7378 0.056 Uiso 1 1 calc R . . H16B H 0.3561 0.1230 0.7143 0.056 Uiso 1 1 calc R . . H16C H 0.2889 0.2100 0.6227 0.056 Uiso 1 1 calc R . . C17 C 0.4310(6) 0.1736(10) 0.4978(6) 0.058(2) Uani 1 1 d . . . H17A H 0.3824 0.1498 0.4434 0.087 Uiso 1 1 calc R . . H17B H 0.4525 0.0708 0.5344 0.087 Uiso 1 1 calc R . . H17C H 0.4683 0.2233 0.4575 0.087 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 0.0252(3) 0.0176(3) 0.0337(3) 0.00008(17) 0.0076(2) -0.00238(14) Si 0.0308(8) 0.0298(7) 0.0302(8) 0.0029(6) 0.0078(6) 0.0067(6) B 0.028(3) 0.023(3) 0.034(3) -0.001(2) 0.007(3) -0.005(3) C1 0.028(3) 0.016(2) 0.047(3) -0.002(2) 0.009(2) 0.001(2) C2 0.045(3) 0.024(3) 0.032(3) 0.004(2) 0.011(3) -0.005(2) C3 0.049(4) 0.028(3) 0.048(4) -0.007(3) 0.030(3) -0.014(3) C4 0.028(3) 0.034(3) 0.095(6) -0.021(4) 0.027(4) -0.011(3) C5 0.028(3) 0.025(3) 0.109(7) 0.008(4) -0.020(4) -0.003(3) C6 0.057(4) 0.036(3) 0.038(3) 0.008(3) -0.014(3) -0.018(3) C7 0.050(4) 0.023(3) 0.031(3) -0.004(2) 0.014(3) -0.012(2) C8 0.030(3) 0.023(3) 0.027(3) 0.000(2) 0.003(2) -0.004(2) C9 0.033(3) 0.019(2) 0.042(3) -0.001(2) 0.012(2) 0.001(2) C10 0.027(3) 0.016(2) 0.041(3) 0.003(2) 0.004(2) -0.001(2) C11 0.034(3) 0.027(3) 0.030(3) 0.003(2) 0.011(2) -0.006(2) C12 0.028(3) 0.027(3) 0.028(3) -0.002(2) 0.009(2) -0.001(2) C13 0.027(3) 0.031(3) 0.030(3) 0.005(2) 0.006(2) 0.003(2) C14 0.032(3) 0.034(3) 0.034(3) 0.003(2) 0.008(2) 0.002(2) C15 0.035(3) 0.049(4) 0.047(4) 0.010(3) 0.004(3) 0.002(3) C16 0.040(3) 0.029(3) 0.044(4) 0.004(3) 0.010(3) 0.000(3) C17 0.085(6) 0.051(4) 0.043(4) 0.008(3) 0.024(4) 0.031(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr C1 2.331(5) . ? Zr C2 2.332(5) . ? Zr C5 2.333(6) . ? Zr C6 2.338(6) . ? Zr C7 2.339(6) . ? Zr C4 2.341(6) . ? Zr C3 2.355(6) . ? Zr C10 2.507(5) . ? Zr C9 2.529(6) . ? Zr C11 2.540(5) . ? Zr C8 2.556(5) . ? Zr C12 2.575(5) . ? Si C14 1.834(6) . ? Si C17 1.850(7) . ? Si C16 1.857(6) . ? Si C15 1.859(7) . ? B C8 1.509(8) . ? B C12 1.519(8) . ? B C13 1.545(8) . ? C1 C7 1.408(8) . ? C1 C2 1.413(8) . ? C2 C3 1.419(9) . ? C3 C4 1.417(11) . ? C4 C5 1.414(12) . ? C5 C6 1.419(12) . ? C6 C7 1.431(10) . ? C8 C9 1.397(8) . ? C9 C10 1.411(8) . ? C10 C11 1.417(8) . ? C11 C12 1.411(8) . ? C13 C14 1.224(8) . ? 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 C1 Zr C2 35.3(2) . . ? C1 Zr C5 85.7(2) . . ? C2 Zr C5 85.7(2) . . ? C1 Zr C6 66.3(2) . . ? C2 Zr C6 86.0(2) . . ? C5 Zr C6 35.4(3) . . ? C1 Zr C7 35.1(2) . . ? C2 Zr C7 66.10(19) . . ? C5 Zr C7 66.4(3) . . ? C6 Zr C7 35.6(2) . . ? C1 Zr C4 85.6(2) . . ? C2 Zr C4 65.9(3) . . ? C5 Zr C4 35.2(3) . . ? C6 Zr C4 66.2(3) . . ? C7 Zr C4 85.9(2) . . ? C1 Zr C3 66.2(2) . . ? C2 Zr C3 35.3(2) . . ? C5 Zr C3 66.1(3) . . ? C6 Zr C3 86.0(2) . . ? C7 Zr C3 85.9(2) . . ? C4 Zr C3 35.1(3) . . ? C1 Zr C10 150.32(18) . . ? C2 Zr C10 155.6(2) . . ? C5 Zr C10 115.1(2) . . ? C6 Zr C10 118.3(2) . . ? C7 Zr C10 132.52(19) . . ? C4 Zr C10 123.8(2) . . ? C3 Zr C10 140.3(2) . . ? C1 Zr C9 147.6(2) . . ? C2 Zr C9 125.4(2) . . ? C5 Zr C9 123.9(2) . . ? C6 Zr C9 145.6(2) . . ? C7 Zr C9 162.5(2) . . ? C4 Zr C9 110.6(2) . . ? C3 Zr C9 111.0(2) . . ? C10 Zr C9 32.53(18) . . ? C1 Zr C11 118.19(19) . . ? C2 Zr C11 142.3(2) . . ? C5 Zr C11 125.6(3) . . ? C6 Zr C11 107.5(2) . . ? C7 Zr C11 104.67(19) . . ? C4 Zr C11 151.7(2) . . ? C3 Zr C11 166.5(2) . . ? C10 Zr C11 32.61(18) . . ? C9 Zr C11 57.95(18) . . ? C1 Zr C8 115.84(19) . . ? C2 Zr C8 97.70(19) . . ? C5 Zr C8 146.5(3) . . ? C6 Zr C8 175.8(2) . . ? C7 Zr C8 144.8(2) . . ? C4 Zr C8 117.0(2) . . ? C3 Zr C8 98.1(2) . . ? C10 Zr C8 57.91(17) . . ? C9 Zr C8 31.90(18) . . ? C11 Zr C8 68.38(17) . . ? C1 Zr C12 93.10(18) . . ? C2 Zr C12 110.5(2) . . ? C5 Zr C12 149.5(3) . . ? C6 Zr C12 117.5(2) . . ? C7 Zr C12 95.8(2) . . ? C4 Zr C12 175.1(3) . . ? C3 Zr C12 140.2(2) . . ? C10 Zr C12 58.04(17) . . ? C9 Zr C12 68.37(18) . . ? C11 Zr C12 32.02(18) . . ? C8 Zr C12 59.39(17) . . ? C14 Si C17 107.8(3) . . ? C14 Si C16 107.3(3) . . ? C17 Si C16 109.4(4) . . ? C14 Si C15 109.0(3) . . ? C17 Si C15 111.8(4) . . ? C16 Si C15 111.5(3) . . ? C8 B C12 114.2(5) . . ? C8 B C13 123.5(5) . . ? C12 B C13 121.8(5) . . ? C8 B Zr 69.8(3) . . ? C12 B Zr 70.5(3) . . ? C13 B Zr 122.0(4) . . ? C7 C1 C2 129.1(5) . . ? C7 C1 Zr 72.8(3) . . ? C2 C1 Zr 72.4(3) . . ? C1 C2 C3 129.2(6) . . ? C1 C2 Zr 72.3(3) . . ? C3 C2 Zr 73.2(3) . . ? C4 C3 C2 127.4(6) . . ? C4 C3 Zr 71.9(4) . . ? C2 C3 Zr 71.5(3) . . ? C5 C4 C3 129.1(6) . . ? C5 C4 Zr 72.1(4) . . ? C3 C4 Zr 73.0(3) . . ? C4 C5 C6 129.0(6) . . ? C4 C5 Zr 72.7(4) . . ? C6 C5 Zr 72.5(4) . . ? C5 C6 C7 127.9(6) . . ? C5 C6 Zr 72.1(4) . . ? C7 C6 Zr 72.2(3) . . ? C1 C7 C6 128.2(6) . . ? C1 C7 Zr 72.1(3) . . ? C6 C7 Zr 72.1(4) . . ? C9 C8 B 121.5(5) . . ? C9 C8 Zr 73.0(3) . . ? B C8 Zr 76.5(3) . . ? C8 C9 C10 121.6(5) . . ? C8 C9 Zr 75.1(3) . . ? C10 C9 Zr 72.9(3) . . ? C9 C10 C11 120.5(5) . . ? C9 C10 Zr 74.6(3) . . ? C11 C10 Zr 75.0(3) . . ? C12 C11 C10 121.3(5) . . ? C12 C11 Zr 75.3(3) . . ? C10 C11 Zr 72.4(3) . . ? C11 C12 B 120.7(5) . . ? C11 C12 Zr 72.6(3) . . ? B C12 Zr 75.8(3) . . ? C14 C13 B 174.7(6) . . ? C13 C14 Si 174.0(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Zr B C8 -139.5(3) . . . . ? C2 Zr B C8 -104.3(3) . . . . ? C5 Zr B C8 -96(3) . . . . ? C6 Zr B C8 173.0(3) . . . . ? C7 Zr B C8 -168.2(3) . . . . ? C4 Zr B C8 -55.4(5) . . . . ? C3 Zr B C8 -74.5(4) . . . . ? C10 Zr B C8 63.1(3) . . . . ? C9 Zr B C8 28.6(3) . . . . ? C11 Zr B C8 97.7(4) . . . . ? C12 Zr B C8 126.4(5) . . . . ? C1 Zr B C12 94.1(4) . . . . ? C2 Zr B C12 129.4(4) . . . . ? C5 Zr B C12 138(3) . . . . ? C6 Zr B C12 46.6(5) . . . . ? C7 Zr B C12 65.4(4) . . . . ? C4 Zr B C12 178.2(3) . . . . ? C3 Zr B C12 159.1(3) . . . . ? C10 Zr B C12 -63.3(3) . . . . ? C9 Zr B C12 -97.8(4) . . . . ? C11 Zr B C12 -28.7(3) . . . . ? C8 Zr B C12 -126.4(5) . . . . ? C1 Zr B C13 -21.9(5) . . . . ? C2 Zr B C13 13.3(5) . . . . ? C5 Zr B C13 22(4) . . . . ? C6 Zr B C13 -69.4(6) . . . . ? C7 Zr B C13 -50.6(5) . . . . ? C4 Zr B C13 62.2(6) . . . . ? C3 Zr B C13 43.1(5) . . . . ? C10 Zr B C13 -179.3(5) . . . . ? C9 Zr B C13 146.2(5) . . . . ? C11 Zr B C13 -144.7(5) . . . . ? C8 Zr B C13 117.6(6) . . . . ? C12 Zr B C13 -116.0(6) . . . . ? C2 Zr C1 C7 142.3(5) . . . . ? C5 Zr C1 C7 53.8(4) . . . . ? C6 Zr C1 C7 23.1(4) . . . . ? C4 Zr C1 C7 89.1(4) . . . . ? C3 Zr C1 C7 119.5(4) . . . . ? C10 Zr C1 C7 -82.9(5) . . . . ? C9 Zr C1 C7 -148.5(4) . . . . ? C11 Zr C1 C7 -74.8(4) . . . . ? C8 Zr C1 C7 -152.9(3) . . . . ? C12 Zr C1 C7 -95.7(3) . . . . ? C5 Zr C1 C2 -88.5(4) . . . . ? C6 Zr C1 C2 -119.2(4) . . . . ? C7 Zr C1 C2 -142.3(5) . . . . ? C4 Zr C1 C2 -53.2(4) . . . . ? C3 Zr C1 C2 -22.8(4) . . . . ? C10 Zr C1 C2 134.7(4) . . . . ? C9 Zr C1 C2 69.1(5) . . . . ? C11 Zr C1 C2 142.9(3) . . . . ? C8 Zr C1 C2 64.7(4) . . . . ? C12 Zr C1 C2 122.0(3) . . . . ? C7 C1 C2 C3 0.6(10) . . . . ? Zr C1 C2 C3 49.4(6) . . . . ? C7 C1 C2 Zr -48.8(5) . . . . ? C5 Zr C2 C1 88.7(4) . . . . ? C6 Zr C2 C1 53.3(4) . . . . ? C7 Zr C2 C1 22.6(3) . . . . ? C4 Zr C2 C1 119.0(4) . . . . ? C3 Zr C2 C1 142.1(5) . . . . ? C10 Zr C2 C1 -121.7(5) . . . . ? C9 Zr C2 C1 -142.1(3) . . . . ? C11 Zr C2 C1 -60.5(5) . . . . ? C8 Zr C2 C1 -124.8(3) . . . . ? C12 Zr C2 C1 -64.6(4) . . . . ? C1 Zr C2 C3 -142.1(5) . . . . ? C5 Zr C2 C3 -53.3(4) . . . . ? C6 Zr C2 C3 -88.8(4) . . . . ? C7 Zr C2 C3 -119.5(4) . . . . ? C4 Zr C2 C3 -23.1(4) . . . . ? C10 Zr C2 C3 96.2(6) . . . . ? C9 Zr C2 C3 75.8(4) . . . . ? C11 Zr C2 C3 157.5(4) . . . . ? C8 Zr C2 C3 93.2(4) . . . . ? C12 Zr C2 C3 153.3(4) . . . . ? C1 C2 C3 C4 -1.0(10) . . . . ? Zr C2 C3 C4 48.1(6) . . . . ? C1 C2 C3 Zr -49.1(6) . . . . ? C1 Zr C3 C4 -118.7(4) . . . . ? C2 Zr C3 C4 -141.6(6) . . . . ? C5 Zr C3 C4 -22.6(4) . . . . ? C6 Zr C3 C4 -52.9(4) . . . . ? C7 Zr C3 C4 -88.6(4) . . . . ? C10 Zr C3 C4 78.5(5) . . . . ? C9 Zr C3 C4 96.3(4) . . . . ? C11 Zr C3 C4 129.4(9) . . . . ? C8 Zr C3 C4 126.6(4) . . . . ? C12 Zr C3 C4 177.3(3) . . . . ? C1 Zr C3 C2 22.8(3) . . . . ? C5 Zr C3 C2 119.0(4) . . . . ? C6 Zr C3 C2 88.7(4) . . . . ? C7 Zr C3 C2 53.0(4) . . . . ? C4 Zr C3 C2 141.6(6) . . . . ? C10 Zr C3 C2 -139.9(3) . . . . ? C9 Zr C3 C2 -122.2(4) . . . . ? C11 Zr C3 C2 -89.1(9) . . . . ? C8 Zr C3 C2 -91.9(4) . . . . ? C12 Zr C3 C2 -41.2(5) . . . . ? C2 C3 C4 C5 0.5(11) . . . . ? Zr C3 C4 C5 48.4(7) . . . . ? C2 C3 C4 Zr -47.9(6) . . . . ? C1 Zr C4 C5 -88.9(4) . . . . ? C2 Zr C4 C5 -119.3(4) . . . . ? C6 Zr C4 C5 -22.8(4) . . . . ? C7 Zr C4 C5 -53.7(4) . . . . ? C3 Zr C4 C5 -142.5(6) . . . . ? C10 Zr C4 C5 86.4(4) . . . . ? C9 Zr C4 C5 120.0(4) . . . . ? C11 Zr C4 C5 60.0(6) . . . . ? C8 Zr C4 C5 154.3(4) . . . . ? C12 Zr C4 C5 -163(2) . . . . ? C1 Zr C4 C3 53.6(4) . . . . ? C2 Zr C4 C3 23.1(3) . . . . ? C5 Zr C4 C3 142.5(6) . . . . ? C6 Zr C4 C3 119.6(4) . . . . ? C7 Zr C4 C3 88.8(4) . . . . ? C10 Zr C4 C3 -131.1(3) . . . . ? C9 Zr C4 C3 -97.5(4) . . . . ? C11 Zr C4 C3 -157.6(4) . . . . ? C8 Zr C4 C3 -63.2(4) . . . . ? C12 Zr C4 C3 -21(2) . . . . ? C3 C4 C5 C6 0.2(12) . . . . ? Zr C4 C5 C6 48.9(7) . . . . ? C3 C4 C5 Zr -48.7(6) . . . . ? C1 Zr C5 C4 88.4(4) . . . . ? C2 Zr C5 C4 53.0(4) . . . . ? C6 Zr C5 C4 142.2(6) . . . . ? C7 Zr C5 C4 118.8(4) . . . . ? C3 Zr C5 C4 22.5(4) . . . . ? C10 Zr C5 C4 -113.7(4) . . . . ? C9 Zr C5 C4 -77.4(5) . . . . ? C11 Zr C5 C4 -149.7(4) . . . . ? C8 Zr C5 C4 -44.5(6) . . . . ? C12 Zr C5 C4 177.2(4) . . . . ? C1 Zr C5 C6 -53.8(4) . . . . ? C2 Zr C5 C6 -89.2(4) . . . . ? C7 Zr C5 C6 -23.4(4) . . . . ? C4 Zr C5 C6 -142.2(6) . . . . ? C3 Zr C5 C6 -119.6(4) . . . . ? C10 Zr C5 C6 104.2(4) . . . . ? C9 Zr C5 C6 140.4(4) . . . . ? C11 Zr C5 C6 68.2(4) . . . . ? C8 Zr C5 C6 173.4(3) . . . . ? C12 Zr C5 C6 35.1(6) . . . . ? C4 C5 C6 C7 0.0(11) . . . . ? Zr C5 C6 C7 49.0(6) . . . . ? C4 C5 C6 Zr -48.9(7) . . . . ? C1 Zr C6 C5 118.5(4) . . . . ? C2 Zr C6 C5 88.2(4) . . . . ? C7 Zr C6 C5 141.3(6) . . . . ? C4 Zr C6 C5 22.7(4) . . . . ? C3 Zr C6 C5 52.8(4) . . . . ? C10 Zr C6 C5 -94.2(4) . . . . ? C9 Zr C6 C5 -69.4(6) . . . . ? C11 Zr C6 C5 -127.7(4) . . . . ? C8 Zr C6 C5 -119(3) . . . . ? C12 Zr C6 C5 -160.8(4) . . . . ? C1 Zr C6 C7 -22.8(3) . . . . ? C2 Zr C6 C7 -53.1(4) . . . . ? C5 Zr C6 C7 -141.3(6) . . . . ? C4 Zr C6 C7 -118.6(4) . . . . ? C3 Zr C6 C7 -88.5(4) . . . . ? C10 Zr C6 C7 124.5(3) . . . . ? C9 Zr C6 C7 149.3(4) . . . . ? C11 Zr C6 C7 91.0(4) . . . . ? C8 Zr C6 C7 99(3) . . . . ? C12 Zr C6 C7 57.9(4) . . . . ? C2 C1 C7 C6 0.3(10) . . . . ? Zr C1 C7 C6 -48.4(6) . . . . ? C2 C1 C7 Zr 48.7(5) . . . . ? C5 C6 C7 C1 -0.5(10) . . . . ? Zr C6 C7 C1 48.4(6) . . . . ? C5 C6 C7 Zr -48.9(6) . . . . ? C2 Zr C7 C1 -22.7(3) . . . . ? C5 Zr C7 C1 -118.6(4) . . . . ? C6 Zr C7 C1 -141.9(5) . . . . ? C4 Zr C7 C1 -88.2(4) . . . . ? C3 Zr C7 C1 -53.0(4) . . . . ? C10 Zr C7 C1 138.2(3) . . . . ? C9 Zr C7 C1 111.7(7) . . . . ? C11 Zr C7 C1 118.5(3) . . . . ? C8 Zr C7 C1 45.3(5) . . . . ? C12 Zr C7 C1 87.2(3) . . . . ? C1 Zr C7 C6 141.9(5) . . . . ? C2 Zr C7 C6 119.2(4) . . . . ? C5 Zr C7 C6 23.3(4) . . . . ? C4 Zr C7 C6 53.7(4) . . . . ? C3 Zr C7 C6 88.9(4) . . . . ? C10 Zr C7 C6 -79.9(4) . . . . ? C9 Zr C7 C6 -106.4(7) . . . . ? C11 Zr C7 C6 -99.6(4) . . . . ? C8 Zr C7 C6 -172.8(4) . . . . ? C12 Zr C7 C6 -130.9(4) . . . . ? C12 B C8 C9 -3.8(8) . . . . ? C13 B C8 C9 -175.7(5) . . . . ? Zr B C8 C9 -60.0(5) . . . . ? C12 B C8 Zr 56.3(4) . . . . ? C13 B C8 Zr -115.7(5) . . . . ? C1 Zr C8 C9 175.5(3) . . . . ? C2 Zr C8 C9 -152.6(3) . . . . ? C5 Zr C8 C9 -58.8(5) . . . . ? C6 Zr C8 C9 55(3) . . . . ? C7 Zr C8 C9 148.5(4) . . . . ? C4 Zr C8 C9 -85.8(4) . . . . ? C3 Zr C8 C9 -117.0(3) . . . . ? C10 Zr C8 C9 28.8(3) . . . . ? C11 Zr C8 C9 63.7(3) . . . . ? C12 Zr C8 C9 98.1(4) . . . . ? C1 Zr C8 B 46.2(4) . . . . ? C2 Zr C8 B 78.0(4) . . . . ? C5 Zr C8 B 171.8(4) . . . . ? C6 Zr C8 B -74(3) . . . . ? C7 Zr C8 B 19.1(5) . . . . ? C4 Zr C8 B 144.8(4) . . . . ? C3 Zr C8 B 113.6(4) . . . . ? C10 Zr C8 B -100.5(4) . . . . ? C9 Zr C8 B -129.4(5) . . . . ? C11 Zr C8 B -65.7(3) . . . . ? C12 Zr C8 B -31.3(3) . . . . ? B C8 C9 C10 3.2(8) . . . . ? Zr C8 C9 C10 -58.6(5) . . . . ? B C8 C9 Zr 61.8(5) . . . . ? C1 Zr C9 C8 -7.5(5) . . . . ? C2 Zr C9 C8 33.9(4) . . . . ? C5 Zr C9 C8 145.4(4) . . . . ? C6 Zr C9 C8 -173.9(4) . . . . ? C7 Zr C9 C8 -92.8(7) . . . . ? C4 Zr C9 C8 108.4(4) . . . . ? C3 Zr C9 C8 70.8(4) . . . . ? C10 Zr C9 C8 -130.5(5) . . . . ? C11 Zr C9 C8 -100.6(4) . . . . ? C12 Zr C9 C8 -66.4(3) . . . . ? C1 Zr C9 C10 123.0(4) . . . . ? C2 Zr C9 C10 164.5(3) . . . . ? C5 Zr C9 C10 -84.1(4) . . . . ? C6 Zr C9 C10 -43.4(6) . . . . ? C7 Zr C9 C10 37.7(8) . . . . ? C4 Zr C9 C10 -121.1(4) . . . . ? C3 Zr C9 C10 -158.7(3) . . . . ? C11 Zr C9 C10 30.0(3) . . . . ? C8 Zr C9 C10 130.5(5) . . . . ? C12 Zr C9 C10 64.1(3) . . . . ? C8 C9 C10 C11 -2.0(8) . . . . ? Zr C9 C10 C11 -61.7(5) . . . . ? C8 C9 C10 Zr 59.6(5) . . . . ? C1 Zr C10 C9 -114.8(5) . . . . ? C2 Zr C10 C9 -31.9(6) . . . . ? C5 Zr C10 C9 114.2(4) . . . . ? C6 Zr C10 C9 153.8(4) . . . . ? C7 Zr C10 C9 -165.5(3) . . . . ? C4 Zr C10 C9 74.8(4) . . . . ? C3 Zr C10 C9 32.1(5) . . . . ? C11 Zr C10 C9 -128.3(5) . . . . ? C8 Zr C10 C9 -28.3(3) . . . . ? C12 Zr C10 C9 -99.8(4) . . . . ? C1 Zr C10 C11 13.5(6) . . . . ? C2 Zr C10 C11 96.4(5) . . . . ? C5 Zr C10 C11 -117.5(4) . . . . ? C6 Zr C10 C11 -77.9(4) . . . . ? C7 Zr C10 C11 -37.3(4) . . . . ? C4 Zr C10 C11 -157.0(4) . . . . ? C3 Zr C10 C11 160.3(4) . . . . ? C9 Zr C10 C11 128.3(5) . . . . ? C8 Zr C10 C11 100.0(4) . . . . ? C12 Zr C10 C11 28.5(3) . . . . ? C9 C10 C11 C12 1.7(8) . . . . ? Zr C10 C11 C12 -59.7(5) . . . . ? C9 C10 C11 Zr 61.5(5) . . . . ? C1 Zr C11 C12 -42.2(4) . . . . ? C2 Zr C11 C12 -7.4(5) . . . . ? C5 Zr C11 C12 -148.5(4) . . . . ? C6 Zr C11 C12 -114.2(4) . . . . ? C7 Zr C11 C12 -77.2(4) . . . . ? C4 Zr C11 C12 173.6(5) . . . . ? C3 Zr C11 C12 63.4(10) . . . . ? C10 Zr C11 C12 130.3(5) . . . . ? C9 Zr C11 C12 100.4(4) . . . . ? C8 Zr C11 C12 66.5(3) . . . . ? C1 Zr C11 C10 -172.5(3) . . . . ? C2 Zr C11 C10 -137.7(4) . . . . ? C5 Zr C11 C10 81.2(4) . . . . ? C6 Zr C11 C10 115.5(4) . . . . ? C7 Zr C11 C10 152.5(3) . . . . ? C4 Zr C11 C10 43.3(6) . . . . ? C3 Zr C11 C10 -66.9(10) . . . . ? C9 Zr C11 C10 -29.9(3) . . . . ? C8 Zr C11 C10 -63.8(3) . . . . ? C12 Zr C11 C10 -130.3(5) . . . . ? C10 C11 C12 B -2.6(8) . . . . ? Zr C11 C12 B -60.9(5) . . . . ? C10 C11 C12 Zr 58.3(5) . . . . ? C8 B C12 C11 3.5(8) . . . . ? C13 B C12 C11 175.5(5) . . . . ? Zr B C12 C11 59.4(5) . . . . ? C8 B C12 Zr -55.9(4) . . . . ? C13 B C12 Zr 116.2(5) . . . . ? C1 Zr C12 C11 143.7(3) . . . . ? C2 Zr C12 C11 175.2(3) . . . . ? C5 Zr C12 C11 56.8(5) . . . . ? C6 Zr C12 C11 78.8(4) . . . . ? C7 Zr C12 C11 108.6(3) . . . . ? C4 Zr C12 C11 -142(2) . . . . ? C3 Zr C12 C11 -160.9(3) . . . . ? C10 Zr C12 C11 -29.0(3) . . . . ? C9 Zr C12 C11 -63.7(3) . . . . ? C8 Zr C12 C11 -98.0(4) . . . . ? C1 Zr C12 B -87.2(4) . . . . ? C2 Zr C12 B -55.6(4) . . . . ? C5 Zr C12 B -174.0(4) . . . . ? C6 Zr C12 B -152.0(4) . . . . ? C7 Zr C12 B -122.3(4) . . . . ? C4 Zr C12 B -13(2) . . . . ? C3 Zr C12 B -31.7(5) . . . . ? C10 Zr C12 B 100.2(4) . . . . ? C9 Zr C12 B 65.5(4) . . . . ? C11 Zr C12 B 129.2(5) . . . . ? C8 Zr C12 B 31.2(3) . . . . ? C8 B C13 C14 90(6) . . . . ? C12 B C13 C14 -81(6) . . . . ? Zr B C13 C14 4(7) . . . . ? B C13 C14 Si 11(11) . . . . ? C17 Si C14 C13 59(5) . . . . ? C16 Si C14 C13 -59(5) . . . . ? C15 Si C14 C13 -179(100) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 66.58 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.298 _refine_diff_density_min -1.081 _refine_diff_density_rms 0.129