# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2008 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name "Paul O'Brien" _publ_contact_author_email PAUL.OBRIEN@MANCHESTER.AC.UK loop_ _publ_author_name M.Helliwell S.Mlondo D.Procter J.Raftery P.Thomas data_s2621m _database_code_depnum_ccdc_archive 'CCDC 674752' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H51 B2 O8 Zr' _chemical_formula_weight 820.69 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.793(5) _cell_length_b 12.420(5) _cell_length_c 20.562(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 115.439(5) _cell_angle_gamma 90.000(5) _cell_volume 8255(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1530 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 23.70 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3432 _exptl_absorpt_coefficient_mu 0.318 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24979 _diffrn_reflns_av_R_equivalents 0.1178 _diffrn_reflns_av_sigmaI/netI 0.1495 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 23.25 _reflns_number_total 5921 _reflns_number_gt 3352 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0300P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5921 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1208 _refine_ls_R_factor_gt 0.0609 _refine_ls_wR_factor_ref 0.1122 _refine_ls_wR_factor_gt 0.0962 _refine_ls_goodness_of_fit_ref 0.916 _refine_ls_restrained_S_all 0.916 _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 Zr1 Zr 0.86288(2) 0.12534(5) 0.21886(3) 0.02369(18) Uani 1 1 d . . . O1 O 0.87453(13) 0.0130(3) 0.1509(2) 0.0291(11) Uani 1 1 d . . . O2 O 0.92322(12) 0.0607(3) 0.2866(2) 0.0279(11) Uani 1 1 d . . . O3 O 0.80208(12) 0.0794(3) 0.1449(2) 0.0272(11) Uani 1 1 d . . . O4 O 0.85040(13) -0.0131(3) 0.2689(2) 0.0288(11) Uani 1 1 d . . . O5 O 0.87724(12) 0.1814(3) 0.33001(19) 0.0241(11) Uani 1 1 d . . . O6 O 0.82476(12) 0.2489(3) 0.2364(2) 0.0225(10) Uani 1 1 d . . . O7 O 0.90632(12) 0.2505(3) 0.2196(2) 0.0272(11) Uani 1 1 d . . . O8 O 0.84923(12) 0.2256(3) 0.12175(19) 0.0270(11) Uani 1 1 d . . . B1 B 0.8409(2) 0.2525(6) 0.3179(4) 0.028(2) Uani 1 1 d . . . B2 B 0.8881(2) 0.2970(7) 0.1444(4) 0.032(2) Uani 1 1 d . . . C1 C 0.89563(19) -0.1188(5) 0.0907(3) 0.0396(17) Uani 1 1 d . . . H1A H 0.8668 -0.1345 0.0636 0.059 Uiso 1 1 calc R . . H1B H 0.9110 -0.1849 0.1035 0.059 Uiso 1 1 calc R . . H1C H 0.9051 -0.0756 0.0621 0.059 Uiso 1 1 calc R . . C2 C 0.9019(2) -0.0585(5) 0.1579(4) 0.0328(18) Uani 1 1 d . . . C3 C 0.9354(2) -0.0791(6) 0.2221(4) 0.047(2) Uani 1 1 d . . . H3 H 0.9522 -0.1374 0.2243 0.056 Uiso 1 1 calc R . . C4 C 0.9455(2) -0.0184(6) 0.2837(4) 0.0362(19) Uani 1 1 d . . . C5 C 0.9837(2) -0.0380(6) 0.3509(4) 0.062(3) Uani 1 1 d . . . H5A H 1.0024 0.0212 0.3592 0.092 Uiso 1 1 calc R . . H5B H 0.9966 -0.1033 0.3460 0.092 Uiso 1 1 calc R . . H5C H 0.9766 -0.0447 0.3907 0.092 Uiso 1 1 calc R . . C6 C 0.74466(19) -0.0173(5) 0.0589(3) 0.0336(17) Uani 1 1 d . . . H6A H 0.7246 0.0358 0.0565 0.050 Uiso 1 1 calc R . . H6B H 0.7326 -0.0877 0.0533 0.050 Uiso 1 1 calc R . . H6C H 0.7531 -0.0047 0.0212 0.050 Uiso 1 1 calc R . . C7 C 0.78195(19) -0.0100(5) 0.1313(3) 0.0253(16) Uani 1 1 d . . . C8 C 0.79286(19) -0.0975(5) 0.1786(3) 0.0296(17) Uani 1 1 d . . . H8 H 0.7782 -0.1616 0.1637 0.035 Uiso 1 1 calc R . . C9 C 0.8249(2) -0.0909(5) 0.2469(3) 0.0282(17) Uani 1 1 d . . . C10 C 0.8314(2) -0.1772(5) 0.3020(3) 0.046(2) Uani 1 1 d . . . H10A H 0.8600 -0.1978 0.3239 0.069 Uiso 1 1 calc R . . H10B H 0.8147 -0.2386 0.2790 0.069 Uiso 1 1 calc R . . H10C H 0.8237 -0.1502 0.3383 0.069 Uiso 1 1 calc R . . C11 C 0.80711(19) 0.1984(5) 0.3415(3) 0.0232(16) Uani 1 1 d . . . C12 C 0.77469(18) 0.1355(5) 0.2962(3) 0.0265(15) Uani 1 1 d . . . H12 H 0.7717 0.1234 0.2496 0.032 Uiso 1 1 calc R . . C13 C 0.7462(2) 0.0893(5) 0.3170(3) 0.0314(17) Uani 1 1 d . . . H13 H 0.7242 0.0497 0.2841 0.038 Uiso 1 1 calc R . . C14 C 0.7508(2) 0.1025(5) 0.3874(3) 0.0352(18) Uani 1 1 d . . . H14 H 0.7325 0.0696 0.4023 0.042 Uiso 1 1 calc R . . C15 C 0.7832(2) 0.1654(5) 0.4351(3) 0.0327(18) Uani 1 1 d . . . H15 H 0.7864 0.1765 0.4819 0.039 Uiso 1 1 calc R . . C16 C 0.8110(2) 0.2119(5) 0.4113(3) 0.0326(18) Uani 1 1 d . . . H16 H 0.8327 0.2533 0.4434 0.039 Uiso 1 1 calc R . . C17 C 0.85502(19) 0.3719(5) 0.3527(3) 0.0259(15) Uani 1 1 d . . . C18 C 0.8264(2) 0.4481(5) 0.3522(3) 0.0281(17) Uani 1 1 d . . . H18 H 0.7984 0.4303 0.3322 0.034 Uiso 1 1 calc R . . C19 C 0.8388(2) 0.5512(5) 0.3814(3) 0.0328(18) Uani 1 1 d . . . H19 H 0.8191 0.6014 0.3792 0.039 Uiso 1 1 calc R . . C20 C 0.8801(2) 0.5784(5) 0.4131(3) 0.0343(18) Uani 1 1 d . . . H20 H 0.8882 0.6465 0.4329 0.041 Uiso 1 1 calc R . . C21 C 0.9095(2) 0.5035(6) 0.4155(3) 0.0389(19) Uani 1 1 d . . . H21 H 0.9375 0.5205 0.4373 0.047 Uiso 1 1 calc R . . C22 C 0.8964(2) 0.4034(5) 0.3851(3) 0.0310(17) Uani 1 1 d . . . H22 H 0.9163 0.3542 0.3862 0.037 Uiso 1 1 calc R . . C23 C 0.89810(18) 0.1306(5) 0.3983(3) 0.0366(17) Uani 1 1 d . . . H23A H 0.9027 0.1822 0.4358 0.055 Uiso 1 1 calc R . . H23B H 0.9242 0.1030 0.4031 0.055 Uiso 1 1 calc R . . H23C H 0.8815 0.0725 0.4022 0.055 Uiso 1 1 calc R . . C24 C 0.78974(18) 0.3099(5) 0.1899(3) 0.0306(17) Uani 1 1 d . . . H24A H 0.7738 0.3305 0.2153 0.046 Uiso 1 1 calc R . . H24B H 0.7729 0.2671 0.1488 0.046 Uiso 1 1 calc R . . H24C H 0.7989 0.3733 0.1742 0.046 Uiso 1 1 calc R . . C25 C 0.87592(18) 0.4233(5) 0.1448(3) 0.0246(16) Uani 1 1 d . . . C26 C 0.87546(19) 0.4709(5) 0.2056(3) 0.0345(18) Uani 1 1 d . . . H26 H 0.8828 0.4295 0.2470 0.041 Uiso 1 1 calc R . . C27 C 0.8646(2) 0.5761(5) 0.2070(4) 0.0387(19) Uani 1 1 d . . . H27 H 0.8649 0.6045 0.2491 0.046 Uiso 1 1 calc R . . C28 C 0.8532(2) 0.6411(6) 0.1469(4) 0.0428(19) Uani 1 1 d . . . H28 H 0.8456 0.7126 0.1476 0.051 Uiso 1 1 calc R . . C29 C 0.8536(2) 0.5954(5) 0.0857(3) 0.044(2) Uani 1 1 d . . . H29 H 0.8462 0.6371 0.0444 0.053 Uiso 1 1 calc R . . C30 C 0.86471(19) 0.4894(5) 0.0847(3) 0.0355(18) Uani 1 1 d . . . H30 H 0.8647 0.4614 0.0427 0.043 Uiso 1 1 calc R . . C31 C 0.9142(2) 0.2708(5) 0.1004(3) 0.0291(17) Uani 1 1 d . . . C32 C 0.9460(2) 0.3361(6) 0.1023(3) 0.0388(19) Uani 1 1 d . . . H32 H 0.9511 0.3996 0.1287 0.047 Uiso 1 1 calc R . . C33 C 0.9705(2) 0.3137(6) 0.0679(4) 0.044(2) Uani 1 1 d . . . H33 H 0.9914 0.3612 0.0716 0.053 Uiso 1 1 calc R . . C34 C 0.9640(2) 0.2197(6) 0.0274(4) 0.049(2) Uani 1 1 d . . . H34 H 0.9807 0.2029 0.0044 0.059 Uiso 1 1 calc R . . C35 C 0.9322(2) 0.1522(6) 0.0224(4) 0.045(2) Uani 1 1 d . . . H35 H 0.9267 0.0903 -0.0056 0.054 Uiso 1 1 calc R . . C36 C 0.9084(2) 0.1761(5) 0.0588(3) 0.0389(19) Uani 1 1 d . . . H36 H 0.8878 0.1280 0.0557 0.047 Uiso 1 1 calc R . . C37 C 0.94797(19) 0.2755(5) 0.2671(3) 0.042(2) Uani 1 1 d . . . H37A H 0.9663 0.2401 0.2510 0.063 Uiso 1 1 calc R . . H37B H 0.9536 0.2513 0.3148 0.063 Uiso 1 1 calc R . . H37C H 0.9521 0.3519 0.2677 0.063 Uiso 1 1 calc R . . C38 C 0.81674(19) 0.2357(5) 0.0510(3) 0.0393(19) Uani 1 1 d . . . H38A H 0.8283 0.2402 0.0168 0.059 Uiso 1 1 calc R . . H38B H 0.8011 0.2997 0.0482 0.059 Uiso 1 1 calc R . . H38C H 0.7989 0.1741 0.0404 0.059 Uiso 1 1 calc R . . C1S C 0.9963(3) 0.6445(7) 0.2126(5) 0.079(3) Uani 1 1 d . . . C2S C 1.0297(3) 0.6626(9) 0.1973(6) 0.111(4) Uani 1 1 d . . . H2S H 1.0559 0.6727 0.2345 0.134 Uiso 1 1 calc R . . C3S C 1.0243(4) 0.6655(12) 0.1285(8) 0.174(7) Uani 1 1 d . . . H3S H 1.0470 0.6790 0.1190 0.209 Uiso 1 1 calc R . . C4S C 0.9849(4) 0.6488(8) 0.0696(6) 0.108(4) Uani 1 1 d . . . H4S H 0.9810 0.6506 0.0219 0.129 Uiso 1 1 calc R . . C5S C 0.9546(3) 0.6305(8) 0.0879(6) 0.095(3) Uani 1 1 d . . . H5S H 0.9283 0.6165 0.0519 0.114 Uiso 1 1 calc R . . C6S C 0.9603(3) 0.6314(8) 0.1581(5) 0.099(4) Uani 1 1 d . . . H6S H 0.9373 0.6222 0.1674 0.119 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 Zr1 0.0262(4) 0.0235(3) 0.0169(3) -0.0007(4) 0.0050(3) -0.0008(4) O1 0.037(3) 0.028(3) 0.027(3) 0.001(2) 0.017(2) 0.003(2) O2 0.027(3) 0.026(3) 0.028(3) -0.001(2) 0.008(2) 0.005(2) O3 0.030(3) 0.024(3) 0.023(3) -0.007(2) 0.007(2) -0.009(2) O4 0.034(3) 0.026(3) 0.022(3) -0.002(2) 0.009(2) -0.005(2) O5 0.027(3) 0.024(2) 0.015(2) 0.0029(19) 0.004(2) 0.003(2) O6 0.024(3) 0.021(2) 0.015(2) -0.0008(19) 0.002(2) 0.001(2) O7 0.021(3) 0.035(3) 0.019(2) 0.003(2) 0.003(2) -0.002(2) O8 0.033(3) 0.029(3) 0.014(2) -0.003(2) 0.004(2) -0.007(2) B1 0.035(5) 0.028(5) 0.014(4) 0.002(4) 0.003(4) -0.005(4) B2 0.028(5) 0.041(6) 0.019(5) 0.002(4) 0.002(4) -0.002(4) C1 0.042(4) 0.038(4) 0.040(4) -0.001(4) 0.018(4) 0.003(4) C2 0.038(5) 0.028(4) 0.043(5) -0.006(4) 0.028(4) -0.007(4) C3 0.038(5) 0.051(5) 0.035(5) -0.010(4) 0.001(4) 0.012(4) C4 0.033(5) 0.039(5) 0.035(5) -0.004(4) 0.014(4) 0.004(4) C5 0.051(6) 0.074(6) 0.041(5) -0.018(4) 0.001(4) 0.026(5) C6 0.041(5) 0.033(4) 0.031(4) -0.006(3) 0.020(4) -0.005(4) C7 0.023(4) 0.039(4) 0.016(4) -0.009(3) 0.010(3) 0.003(3) C8 0.039(4) 0.016(4) 0.031(4) -0.009(3) 0.013(4) -0.006(3) C9 0.032(4) 0.029(4) 0.027(4) -0.004(3) 0.016(4) 0.009(3) C10 0.060(6) 0.024(4) 0.043(5) 0.007(4) 0.011(4) -0.011(4) C11 0.027(4) 0.022(4) 0.016(4) 0.000(3) 0.004(3) 0.006(3) C12 0.033(4) 0.030(4) 0.020(3) 0.001(3) 0.015(3) 0.002(4) C13 0.036(4) 0.026(4) 0.024(4) -0.001(3) 0.006(3) -0.002(3) C14 0.046(5) 0.031(5) 0.027(4) 0.004(3) 0.013(4) -0.007(4) C15 0.033(5) 0.040(5) 0.022(4) 0.004(3) 0.010(4) 0.001(3) C16 0.036(5) 0.019(4) 0.035(4) -0.001(3) 0.008(4) -0.004(3) C17 0.034(4) 0.027(4) 0.017(3) 0.007(3) 0.011(3) 0.002(4) C18 0.027(4) 0.039(5) 0.018(4) 0.003(3) 0.010(3) -0.004(4) C19 0.058(5) 0.023(4) 0.021(4) 0.000(3) 0.021(4) 0.002(4) C20 0.056(5) 0.025(4) 0.020(4) -0.006(3) 0.015(4) -0.014(4) C21 0.036(5) 0.040(5) 0.033(4) -0.007(4) 0.009(4) -0.006(4) C22 0.036(4) 0.032(5) 0.024(4) 0.001(3) 0.012(3) -0.001(3) C23 0.040(4) 0.043(4) 0.023(4) 0.001(4) 0.010(3) 0.005(4) C24 0.039(5) 0.028(4) 0.024(4) -0.003(3) 0.014(4) -0.005(4) C25 0.024(4) 0.034(4) 0.015(4) -0.003(3) 0.008(3) -0.011(3) C26 0.042(5) 0.038(5) 0.023(4) 0.003(3) 0.013(4) -0.014(4) C27 0.052(5) 0.027(4) 0.040(5) -0.007(4) 0.024(4) -0.011(4) C28 0.053(5) 0.027(5) 0.046(5) -0.001(4) 0.020(4) 0.001(4) C29 0.076(6) 0.035(5) 0.022(4) 0.009(3) 0.020(4) -0.001(4) C30 0.048(5) 0.034(5) 0.024(4) -0.004(3) 0.015(4) -0.008(4) C31 0.029(4) 0.035(4) 0.019(4) 0.009(3) 0.006(3) 0.009(3) C32 0.032(5) 0.051(5) 0.029(4) 0.006(4) 0.009(4) 0.005(4) C33 0.031(5) 0.061(6) 0.038(5) 0.016(4) 0.014(4) 0.007(4) C34 0.048(6) 0.054(6) 0.047(5) 0.014(4) 0.021(4) 0.014(5) C35 0.059(6) 0.038(5) 0.044(5) 0.001(4) 0.028(4) 0.013(4) C36 0.052(5) 0.032(4) 0.031(4) 0.012(4) 0.017(4) 0.004(4) C37 0.034(5) 0.050(5) 0.033(4) 0.012(4) 0.006(4) -0.006(4) C38 0.040(5) 0.035(4) 0.028(4) 0.004(3) 0.000(4) -0.007(4) C1S 0.048(6) 0.079(7) 0.088(8) -0.016(6) 0.009(7) -0.011(6) C2S 0.065(8) 0.160(12) 0.099(9) -0.033(9) 0.025(7) -0.025(8) C3S 0.113(12) 0.266(19) 0.156(13) -0.130(14) 0.070(11) -0.041(12) C4S 0.113(10) 0.119(10) 0.115(10) -0.051(8) 0.072(9) -0.046(8) C5S 0.090(8) 0.088(8) 0.115(10) -0.029(8) 0.051(8) -0.016(7) C6S 0.075(8) 0.123(9) 0.067(7) -0.059(7) -0.002(6) 0.032(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr1 O3 2.129(4) . ? Zr1 O1 2.138(4) . ? Zr1 O4 2.147(4) . ? Zr1 O2 2.160(4) . ? Zr1 O6 2.183(4) . ? Zr1 O7 2.195(4) . ? Zr1 O8 2.223(4) . ? Zr1 O5 2.228(4) . ? O1 C2 1.283(7) . ? O2 C4 1.283(7) . ? O3 C7 1.287(7) . ? O4 C9 1.272(7) . ? O5 C23 1.424(6) . ? O5 B1 1.503(8) . ? O6 C24 1.425(6) . ? O6 B1 1.522(7) . ? O7 C37 1.422(6) . ? O7 B2 1.511(8) . ? O8 C38 1.425(6) . ? O8 B2 1.542(8) . ? B1 C11 1.628(9) . ? B1 C17 1.629(9) . ? B2 C31 1.588(10) . ? B2 C25 1.629(9) . ? C1 C2 1.501(8) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 C3 1.374(9) . ? C3 C4 1.382(8) . ? C3 H3 0.9300 . ? C4 C5 1.488(8) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.516(7) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.397(8) . ? C8 C9 1.383(8) . ? C8 H8 0.9300 . ? C9 C10 1.502(8) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.377(7) . ? C11 C16 1.392(8) . ? C12 C13 1.386(8) . ? C12 H12 0.9300 . ? C13 C14 1.393(8) . ? C13 H13 0.9300 . ? C14 C15 1.392(8) . ? C14 H14 0.9300 . ? C15 C16 1.406(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C18 1.392(8) . ? C17 C22 1.394(8) . ? C18 C19 1.402(8) . ? C18 H18 0.9300 . ? C19 C20 1.376(8) . ? C19 H19 0.9300 . ? C20 C21 1.390(8) . ? C20 H20 0.9300 . ? C21 C22 1.380(8) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 C26 1.389(8) . ? C25 C30 1.391(8) . ? C26 C27 1.367(8) . ? C26 H26 0.9300 . ? C27 C28 1.382(8) . ? C27 H27 0.9300 . ? C28 C29 1.387(8) . ? C28 H28 0.9300 . ? C29 C30 1.378(8) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.386(8) . ? C31 C36 1.417(8) . ? C32 C33 1.370(8) . ? C32 H32 0.9300 . ? C33 C34 1.394(9) . ? C33 H33 0.9300 . ? C34 C35 1.383(9) . ? C34 H34 0.9300 . ? C35 C36 1.386(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C1S C6S 1.305(11) . ? C1S C2S 1.379(13) . ? C1S C1S 1.443(17) 2_755 ? C2S C3S 1.343(14) . ? C2S H2S 0.9300 . ? C3S C4S 1.425(13) . ? C3S H3S 0.9300 . ? C4S C5S 1.313(11) . ? C4S H4S 0.9300 . ? C5S C6S 1.367(11) . ? C5S H5S 0.9300 . ? C6S H6S 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zr1 O1 77.58(16) . . ? O3 Zr1 O4 76.59(15) . . ? O1 Zr1 O4 85.95(15) . . ? O3 Zr1 O2 142.49(15) . . ? O1 Zr1 O2 75.93(16) . . ? O4 Zr1 O2 75.50(15) . . ? O3 Zr1 O6 77.68(14) . . ? O1 Zr1 O6 151.32(15) . . ? O4 Zr1 O6 102.14(15) . . ? O2 Zr1 O6 132.66(15) . . ? O3 Zr1 O7 134.33(15) . . ? O1 Zr1 O7 97.49(16) . . ? O4 Zr1 O7 148.98(15) . . ? O2 Zr1 O7 75.50(15) . . ? O6 Zr1 O7 89.55(14) . . ? O3 Zr1 O8 75.28(15) . . ? O1 Zr1 O8 78.95(15) . . ? O4 Zr1 O8 150.31(15) . . ? O2 Zr1 O8 124.10(15) . . ? O6 Zr1 O8 80.94(14) . . ? O7 Zr1 O8 59.37(14) . . ? O3 Zr1 O5 122.08(15) . . ? O1 Zr1 O5 148.24(15) . . ? O4 Zr1 O5 76.26(14) . . ? O2 Zr1 O5 74.26(15) . . ? O6 Zr1 O5 59.76(14) . . ? O7 Zr1 O5 85.48(14) . . ? O8 Zr1 O5 127.69(15) . . ? C2 O1 Zr1 137.1(4) . . ? C4 O2 Zr1 136.4(4) . . ? C7 O3 Zr1 133.8(4) . . ? C9 O4 Zr1 134.7(4) . . ? C23 O5 B1 118.3(4) . . ? C23 O5 Zr1 131.8(3) . . ? B1 O5 Zr1 102.3(3) . . ? C24 O6 B1 122.1(5) . . ? C24 O6 Zr1 134.0(3) . . ? B1 O6 Zr1 103.6(4) . . ? C37 O7 B2 119.1(5) . . ? C37 O7 Zr1 133.6(4) . . ? B2 O7 Zr1 105.7(4) . . ? C38 O8 B2 119.5(5) . . ? C38 O8 Zr1 137.3(4) . . ? B2 O8 Zr1 103.3(3) . . ? O5 B1 O6 93.2(5) . . ? O5 B1 C11 114.1(5) . . ? O6 B1 C11 109.7(5) . . ? O5 B1 C17 112.3(5) . . ? O6 B1 C17 114.2(5) . . ? C11 B1 C17 112.0(5) . . ? O7 B2 O8 91.5(5) . . ? O7 B2 C31 113.7(6) . . ? O8 B2 C31 112.6(6) . . ? O7 B2 C25 111.2(6) . . ? O8 B2 C25 110.4(5) . . ? C31 B2 C25 115.1(6) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 123.1(6) . . ? O1 C2 C1 115.9(6) . . ? C3 C2 C1 121.0(6) . . ? C2 C3 C4 123.8(7) . . ? C2 C3 H3 118.1 . . ? C4 C3 H3 118.1 . . ? O2 C4 C3 122.5(7) . . ? O2 C4 C5 115.1(6) . . ? C3 C4 C5 122.4(6) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 123.8(6) . . ? O3 C7 C6 116.1(6) . . ? C8 C7 C6 120.1(6) . . ? C9 C8 C7 121.6(6) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? O4 C9 C8 124.1(6) . . ? O4 C9 C10 114.8(6) . . ? C8 C9 C10 121.1(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 116.5(6) . . ? C12 C11 B1 123.5(5) . . ? C16 C11 B1 120.0(6) . . ? C11 C12 C13 123.0(6) . . ? C11 C12 H12 118.5 . . ? C13 C12 H12 118.5 . . ? C12 C13 C14 119.7(6) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C15 C14 C13 119.3(6) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C16 118.9(6) . . ? C14 C15 H15 120.6 . . ? C16 C15 H15 120.6 . . ? C11 C16 C15 122.5(6) . . ? C11 C16 H16 118.7 . . ? C15 C16 H16 118.7 . . ? C18 C17 C22 116.2(6) . . ? C18 C17 B1 121.8(6) . . ? C22 C17 B1 122.0(6) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 120.4(6) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.7(6) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C22 C21 C20 118.8(7) . . ? C22 C21 H21 120.6 . . ? C20 C21 H21 120.6 . . ? C21 C22 C17 123.6(6) . . ? C21 C22 H22 118.2 . . ? C17 C22 H22 118.2 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C24 H24A 109.5 . . ? O6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 116.0(6) . . ? C26 C25 B2 121.4(6) . . ? C30 C25 B2 122.7(6) . . ? C27 C26 C25 122.6(6) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C28 121.1(7) . . ? C26 C27 H27 119.5 . . ? C28 C27 H27 119.5 . . ? C27 C28 C29 117.3(6) . . ? C27 C28 H28 121.4 . . ? C29 C28 H28 121.4 . . ? C30 C29 C28 121.4(6) . . ? C30 C29 H29 119.3 . . ? C28 C29 H29 119.3 . . ? C29 C30 C25 121.7(6) . . ? C29 C30 H30 119.2 . . ? C25 C30 H30 119.2 . . ? C32 C31 C36 114.0(6) . . ? C32 C31 B2 122.9(6) . . ? C36 C31 B2 123.0(6) . . ? C33 C32 C31 124.6(7) . . ? C33 C32 H32 117.7 . . ? C31 C32 H32 117.7 . . ? C32 C33 C34 119.9(7) . . ? C32 C33 H33 120.0 . . ? C34 C33 H33 120.0 . . ? C35 C34 C33 118.2(7) . . ? C35 C34 H34 120.9 . . ? C33 C34 H34 120.9 . . ? C34 C35 C36 120.5(7) . . ? C34 C35 H35 119.7 . . ? C36 C35 H35 119.7 . . ? C35 C36 C31 122.7(7) . . ? C35 C36 H36 118.7 . . ? C31 C36 H36 118.7 . . ? O7 C37 H37A 109.5 . . ? O7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C6S C1S C2S 117.2(10) . . ? C6S C1S C1S 125.2(13) . 2_755 ? C2S C1S C1S 117.5(12) . 2_755 ? C3S C2S C1S 119.8(11) . . ? C3S C2S H2S 120.1 . . ? C1S C2S H2S 120.1 . . ? C2S C3S C4S 122.3(12) . . ? C2S C3S H3S 118.8 . . ? C4S C3S H3S 118.8 . . ? C5S C4S C3S 114.8(11) . . ? C5S C4S H4S 122.6 . . ? C3S C4S H4S 122.6 . . ? C4S C5S C6S 122.3(11) . . ? C4S C5S H5S 118.9 . . ? C6S C5S H5S 118.9 . . ? C1S C6S C5S 123.5(11) . . ? C1S C6S H6S 118.2 . . ? C5S C6S H6S 118.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Zr1 O1 C2 -145.5(6) . . . . ? O4 Zr1 O1 C2 -68.4(6) . . . . ? O2 Zr1 O1 C2 7.7(6) . . . . ? O6 Zr1 O1 C2 -176.4(5) . . . . ? O7 Zr1 O1 C2 80.6(6) . . . . ? O8 Zr1 O1 C2 137.3(6) . . . . ? O5 Zr1 O1 C2 -12.9(7) . . . . ? O3 Zr1 O2 C4 34.1(7) . . . . ? O1 Zr1 O2 C4 -12.2(6) . . . . ? O4 Zr1 O2 C4 77.2(6) . . . . ? O6 Zr1 O2 C4 170.5(5) . . . . ? O7 Zr1 O2 C4 -113.9(6) . . . . ? O8 Zr1 O2 C4 -78.1(6) . . . . ? O5 Zr1 O2 C4 156.7(6) . . . . ? O1 Zr1 O3 C7 64.1(5) . . . . ? O4 Zr1 O3 C7 -24.7(5) . . . . ? O2 Zr1 O3 C7 18.2(7) . . . . ? O6 Zr1 O3 C7 -130.6(5) . . . . ? O7 Zr1 O3 C7 152.4(5) . . . . ? O8 Zr1 O3 C7 145.7(5) . . . . ? O5 Zr1 O3 C7 -88.7(5) . . . . ? O3 Zr1 O4 C9 19.3(5) . . . . ? O1 Zr1 O4 C9 -58.9(6) . . . . ? O2 Zr1 O4 C9 -135.4(6) . . . . ? O6 Zr1 O4 C9 93.3(5) . . . . ? O7 Zr1 O4 C9 -156.7(5) . . . . ? O8 Zr1 O4 C9 0.3(7) . . . . ? O5 Zr1 O4 C9 147.7(6) . . . . ? O3 Zr1 O5 C23 106.0(5) . . . . ? O1 Zr1 O5 C23 -16.0(6) . . . . ? O4 Zr1 O5 C23 41.8(5) . . . . ? O2 Zr1 O5 C23 -36.7(5) . . . . ? O6 Zr1 O5 C23 154.9(5) . . . . ? O7 Zr1 O5 C23 -112.9(5) . . . . ? O8 Zr1 O5 C23 -158.0(4) . . . . ? O3 Zr1 O5 B1 -41.5(4) . . . . ? O1 Zr1 O5 B1 -163.5(4) . . . . ? O4 Zr1 O5 B1 -105.7(4) . . . . ? O2 Zr1 O5 B1 175.8(4) . . . . ? O6 Zr1 O5 B1 7.5(3) . . . . ? O7 Zr1 O5 B1 99.6(4) . . . . ? O8 Zr1 O5 B1 54.5(4) . . . . ? O3 Zr1 O6 C24 -41.9(5) . . . . ? O1 Zr1 O6 C24 -11.0(7) . . . . ? O4 Zr1 O6 C24 -115.0(5) . . . . ? O2 Zr1 O6 C24 163.6(4) . . . . ? O7 Zr1 O6 C24 93.9(5) . . . . ? O8 Zr1 O6 C24 34.9(5) . . . . ? O5 Zr1 O6 C24 179.0(5) . . . . ? O3 Zr1 O6 B1 131.8(4) . . . . ? O1 Zr1 O6 B1 162.7(4) . . . . ? O4 Zr1 O6 B1 58.6(4) . . . . ? O2 Zr1 O6 B1 -22.8(4) . . . . ? O7 Zr1 O6 B1 -92.4(4) . . . . ? O8 Zr1 O6 B1 -151.5(4) . . . . ? O5 Zr1 O6 B1 -7.4(3) . . . . ? O3 Zr1 O7 C37 -174.8(5) . . . . ? O1 Zr1 O7 C37 -94.8(5) . . . . ? O4 Zr1 O7 C37 -0.2(7) . . . . ? O2 Zr1 O7 C37 -21.5(5) . . . . ? O6 Zr1 O7 C37 113.1(5) . . . . ? O8 Zr1 O7 C37 -167.2(6) . . . . ? O5 Zr1 O7 C37 53.4(5) . . . . ? O3 Zr1 O7 B2 -10.4(5) . . . . ? O1 Zr1 O7 B2 69.5(4) . . . . ? O4 Zr1 O7 B2 164.1(4) . . . . ? O2 Zr1 O7 B2 142.8(4) . . . . ? O6 Zr1 O7 B2 -82.6(4) . . . . ? O8 Zr1 O7 B2 -2.9(4) . . . . ? O5 Zr1 O7 B2 -142.3(4) . . . . ? O3 Zr1 O8 C38 -4.3(5) . . . . ? O1 Zr1 O8 C38 75.6(5) . . . . ? O4 Zr1 O8 C38 14.8(7) . . . . ? O2 Zr1 O8 C38 140.0(5) . . . . ? O6 Zr1 O8 C38 -83.8(5) . . . . ? O7 Zr1 O8 C38 -178.7(6) . . . . ? O5 Zr1 O8 C38 -123.7(5) . . . . ? O3 Zr1 O8 B2 177.2(4) . . . . ? O1 Zr1 O8 B2 -102.9(4) . . . . ? O4 Zr1 O8 B2 -163.7(4) . . . . ? O2 Zr1 O8 B2 -38.4(4) . . . . ? O6 Zr1 O8 B2 97.7(4) . . . . ? O7 Zr1 O8 B2 2.8(4) . . . . ? O5 Zr1 O8 B2 57.8(4) . . . . ? C23 O5 B1 O6 -162.2(4) . . . . ? Zr1 O5 B1 O6 -9.3(4) . . . . ? C23 O5 B1 C11 -48.9(7) . . . . ? Zr1 O5 B1 C11 104.0(5) . . . . ? C23 O5 B1 C17 79.9(6) . . . . ? Zr1 O5 B1 C17 -127.1(4) . . . . ? C24 O6 B1 O5 -175.9(4) . . . . ? Zr1 O6 B1 O5 9.5(4) . . . . ? C24 O6 B1 C11 67.0(7) . . . . ? Zr1 O6 B1 C11 -107.6(5) . . . . ? C24 O6 B1 C17 -59.7(8) . . . . ? Zr1 O6 B1 C17 125.7(5) . . . . ? C37 O7 B2 O8 170.6(5) . . . . ? Zr1 O7 B2 O8 3.6(5) . . . . ? C37 O7 B2 C31 55.0(8) . . . . ? Zr1 O7 B2 C31 -112.0(5) . . . . ? C37 O7 B2 C25 -76.8(7) . . . . ? Zr1 O7 B2 C25 116.1(5) . . . . ? C38 O8 B2 O7 177.7(5) . . . . ? Zr1 O8 B2 O7 -3.5(5) . . . . ? C38 O8 B2 C31 -65.7(7) . . . . ? Zr1 O8 B2 C31 113.1(5) . . . . ? C38 O8 B2 C25 64.4(7) . . . . ? Zr1 O8 B2 C25 -116.8(5) . . . . ? Zr1 O1 C2 C3 -1.2(10) . . . . ? Zr1 O1 C2 C1 179.7(4) . . . . ? O1 C2 C3 C4 -6.9(12) . . . . ? C1 C2 C3 C4 172.2(7) . . . . ? Zr1 O2 C4 C3 9.9(10) . . . . ? Zr1 O2 C4 C5 -171.6(5) . . . . ? C2 C3 C4 O2 2.8(12) . . . . ? C2 C3 C4 C5 -175.5(7) . . . . ? Zr1 O3 C7 C8 18.9(9) . . . . ? Zr1 O3 C7 C6 -160.7(4) . . . . ? O3 C7 C8 C9 5.0(10) . . . . ? C6 C7 C8 C9 -175.4(6) . . . . ? Zr1 O4 C9 C8 -7.9(9) . . . . ? Zr1 O4 C9 C10 173.2(4) . . . . ? C7 C8 C9 O4 -10.3(10) . . . . ? C7 C8 C9 C10 168.6(6) . . . . ? O5 B1 C11 C12 -87.8(7) . . . . ? O6 B1 C11 C12 15.2(9) . . . . ? C17 B1 C11 C12 143.2(6) . . . . ? O5 B1 C11 C16 90.1(7) . . . . ? O6 B1 C11 C16 -166.9(5) . . . . ? C17 B1 C11 C16 -38.9(8) . . . . ? C16 C11 C12 C13 1.7(9) . . . . ? B1 C11 C12 C13 179.6(6) . . . . ? C11 C12 C13 C14 -2.5(9) . . . . ? C12 C13 C14 C15 2.4(9) . . . . ? C13 C14 C15 C16 -1.5(9) . . . . ? C12 C11 C16 C15 -0.7(9) . . . . ? B1 C11 C16 C15 -178.8(6) . . . . ? C14 C15 C16 C11 0.7(9) . . . . ? O5 B1 C17 C18 -175.4(5) . . . . ? O6 B1 C17 C18 80.1(7) . . . . ? C11 B1 C17 C18 -45.4(8) . . . . ? O5 B1 C17 C22 4.2(8) . . . . ? O6 B1 C17 C22 -100.3(7) . . . . ? C11 B1 C17 C22 134.2(6) . . . . ? C22 C17 C18 C19 1.4(8) . . . . ? B1 C17 C18 C19 -179.0(5) . . . . ? C17 C18 C19 C20 -1.8(9) . . . . ? C18 C19 C20 C21 0.7(9) . . . . ? C19 C20 C21 C22 0.7(10) . . . . ? C20 C21 C22 C17 -1.1(10) . . . . ? C18 C17 C22 C21 0.1(9) . . . . ? B1 C17 C22 C21 -179.5(6) . . . . ? O7 B2 C25 C26 -11.7(9) . . . . ? O8 B2 C25 C26 88.4(7) . . . . ? C31 B2 C25 C26 -142.8(6) . . . . ? O7 B2 C25 C30 169.6(6) . . . . ? O8 B2 C25 C30 -90.3(7) . . . . ? C31 B2 C25 C30 38.5(9) . . . . ? C30 C25 C26 C27 0.1(9) . . . . ? B2 C25 C26 C27 -178.7(6) . . . . ? C25 C26 C27 C28 0.3(11) . . . . ? C26 C27 C28 C29 -0.5(11) . . . . ? C27 C28 C29 C30 0.2(10) . . . . ? C28 C29 C30 C25 0.2(11) . . . . ? C26 C25 C30 C29 -0.4(9) . . . . ? B2 C25 C30 C29 178.4(6) . . . . ? O7 B2 C31 C32 -89.1(8) . . . . ? O8 B2 C31 C32 168.5(5) . . . . ? C25 B2 C31 C32 40.8(9) . . . . ? O7 B2 C31 C36 87.7(7) . . . . ? O8 B2 C31 C36 -14.7(9) . . . . ? C25 B2 C31 C36 -142.4(6) . . . . ? C36 C31 C32 C33 -0.2(9) . . . . ? B2 C31 C32 C33 176.8(6) . . . . ? C31 C32 C33 C34 0.1(10) . . . . ? C32 C33 C34 C35 1.0(10) . . . . ? C33 C34 C35 C36 -2.2(10) . . . . ? C34 C35 C36 C31 2.2(10) . . . . ? C32 C31 C36 C35 -0.9(9) . . . . ? B2 C31 C36 C35 -177.9(6) . . . . ? C6S C1S C2S C3S -0.3(19) . . . . ? C1S C1S C2S C3S -178.7(11) 2_755 . . . ? C1S C2S C3S C4S -1(2) . . . . ? C2S C3S C4S C5S 0(2) . . . . ? C3S C4S C5S C6S 2.2(19) . . . . ? C2S C1S C6S C5S 2.7(17) . . . . ? C1S C1S C6S C5S -179.1(8) 2_755 . . . ? C4S C5S C6S C1S -3.8(19) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 23.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.556 _refine_diff_density_min -0.566 _refine_diff_density_rms 0.075 # Attachment 's2635n.cif' data_s2635n _database_code_depnum_ccdc_archive 'CCDC 677357' #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C44 H51 B2 Hf O8' _chemical_formula_weight 907.96 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Hf Hf -0.5830 6.1852 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 35.841(3) _cell_length_b 12.4200(9) _cell_length_c 20.5810(14) _cell_angle_alpha 90.00 _cell_angle_beta 115.637(2) _cell_angle_gamma 90.00 _cell_volume 8259.6(10) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8582 _cell_measurement_theta_min 2.194 _cell_measurement_theta_max 27.7095 _exptl_crystal_description block _exptl_crystal_colour white _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.460 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3688 _exptl_absorpt_coefficient_mu 2.577 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.5119 _exptl_absorpt_correction_T_max 0.6985 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34953 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0694 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 28.32 _reflns_number_total 9822 _reflns_number_gt 6845 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9822 _refine_ls_number_parameters 504 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0567 _refine_ls_R_factor_gt 0.0343 _refine_ls_wR_factor_ref 0.0877 _refine_ls_wR_factor_gt 0.0758 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.935 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.002 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 Hf1 Hf 0.862992(5) 0.125493(16) 0.719099(9) 0.02436(6) Uani 1 1 d . . . O1 O 0.87392(9) 0.0141(2) 0.65058(15) 0.0293(7) Uani 1 1 d . . . O2 O 0.92319(9) 0.0619(2) 0.78637(15) 0.0293(7) Uani 1 1 d . . . O3 O 0.80191(9) 0.0794(2) 0.64556(14) 0.0281(7) Uani 1 1 d . . . O4 O 0.85076(9) -0.0116(2) 0.76905(15) 0.0296(7) Uani 1 1 d . . . O5 O 0.87753(8) 0.1818(2) 0.82959(14) 0.0254(6) Uani 1 1 d . . . O6 O 0.82481(8) 0.2484(2) 0.73590(14) 0.0245(6) Uani 1 1 d . . . O7 O 0.90582(8) 0.2507(2) 0.72013(14) 0.0279(7) Uani 1 1 d . . . O8 O 0.84885(8) 0.2251(2) 0.62190(13) 0.0263(7) Uani 1 1 d . . . C1 C 0.89433(15) -0.1189(4) 0.5907(2) 0.0404(11) Uani 1 1 d . . . H1A H 0.8646 -0.1307 0.5617 0.061 Uiso 1 1 calc R . . H1B H 0.9085 -0.1885 0.6042 0.061 Uiso 1 1 calc R . . H1C H 0.9056 -0.0776 0.5626 0.061 Uiso 1 1 calc R . . C2 C 0.90090(15) -0.0573(4) 0.6578(3) 0.0344(11) Uani 1 1 d . . . C3 C 0.93525(16) -0.0779(5) 0.7217(3) 0.0488(14) Uani 1 1 d . . . H3 H 0.9527 -0.1368 0.7238 0.059 Uiso 1 1 calc R . . C4 C 0.94521(14) -0.0147(4) 0.7834(3) 0.0386(12) Uani 1 1 d . . . C5 C 0.98414(16) -0.0361(5) 0.8501(3) 0.0600(17) Uani 1 1 d . . . H5A H 1.0028 0.0258 0.8601 0.090 Uiso 1 1 calc R . . H5B H 0.9978 -0.1004 0.8429 0.090 Uiso 1 1 calc R . . H5C H 0.9774 -0.0478 0.8909 0.090 Uiso 1 1 calc R . . C6 C 0.74514(13) -0.0169(4) 0.5604(2) 0.0333(11) Uani 1 1 d . . . H6A H 0.7249 0.0378 0.5583 0.050 Uiso 1 1 calc R . . H6B H 0.7327 -0.0885 0.5549 0.050 Uiso 1 1 calc R . . H6C H 0.7534 -0.0045 0.5215 0.050 Uiso 1 1 calc R . . C7 C 0.78225(13) -0.0101(4) 0.6313(2) 0.0282(10) Uani 1 1 d . . . C8 C 0.79326(14) -0.0969(3) 0.6789(2) 0.0322(11) Uani 1 1 d . . . H8 H 0.7781 -0.1622 0.6640 0.039 Uiso 1 1 calc R . . C9 C 0.82574(14) -0.0909(4) 0.7476(2) 0.0314(10) Uani 1 1 d . . . C10 C 0.83274(16) -0.1777(4) 0.8021(3) 0.0469(14) Uani 1 1 d . . . H10A H 0.8618 -0.2005 0.8226 0.070 Uiso 1 1 calc R . . H10B H 0.8148 -0.2393 0.7788 0.070 Uiso 1 1 calc R . . H10C H 0.8262 -0.1501 0.8406 0.070 Uiso 1 1 calc R . . C11 C 0.80806(13) 0.1965(3) 0.8420(2) 0.0281(10) Uani 1 1 d . . . C12 C 0.77483(13) 0.1343(3) 0.7957(2) 0.0299(10) Uani 1 1 d . . . H12 H 0.7713 0.1228 0.7477 0.036 Uiso 1 1 calc R . . C13 C 0.74656(14) 0.0885(4) 0.8173(2) 0.0348(11) Uani 1 1 d . . . H13 H 0.7240 0.0474 0.7841 0.042 Uiso 1 1 calc R . . C14 C 0.75116(14) 0.1025(4) 0.8870(2) 0.0363(11) Uani 1 1 d . . . H14 H 0.7321 0.0708 0.9021 0.044 Uiso 1 1 calc R . . C15 C 0.78404(15) 0.1635(4) 0.9348(2) 0.0365(11) Uani 1 1 d . . . H15 H 0.7877 0.1735 0.9829 0.044 Uiso 1 1 calc R . . C16 C 0.81157(14) 0.2098(4) 0.9120(2) 0.0312(10) Uani 1 1 d . . . H16 H 0.8337 0.2522 0.9452 0.037 Uiso 1 1 calc R . . C17 C 0.85524(13) 0.3702(4) 0.8528(2) 0.0258(9) Uani 1 1 d . . . C18 C 0.82651(14) 0.4470(4) 0.8525(2) 0.0293(10) Uani 1 1 d . . . H18 H 0.7980 0.4288 0.8321 0.035 Uiso 1 1 calc R . . C19 C 0.83877(15) 0.5494(4) 0.8813(2) 0.0332(11) Uani 1 1 d . . . H19 H 0.8185 0.6005 0.8789 0.040 Uiso 1 1 calc R . . C20 C 0.88008(15) 0.5773(4) 0.9134(2) 0.0349(11) Uani 1 1 d . . . H20 H 0.8885 0.6466 0.9341 0.042 Uiso 1 1 calc R . . C21 C 0.90879(14) 0.5031(4) 0.9148(2) 0.0336(11) Uani 1 1 d . . . H21 H 0.9373 0.5214 0.9366 0.040 Uiso 1 1 calc R . . C22 C 0.89686(14) 0.4027(4) 0.8851(2) 0.0303(10) Uani 1 1 d . . . H22 H 0.9175 0.3535 0.8865 0.036 Uiso 1 1 calc R . . C23 C 0.89890(14) 0.1302(4) 0.8984(2) 0.0363(11) Uani 1 1 d . . . H23A H 0.9039 0.1826 0.9369 0.054 Uiso 1 1 calc R . . H23B H 0.9254 0.1019 0.9028 0.054 Uiso 1 1 calc R . . H23C H 0.8820 0.0709 0.9024 0.054 Uiso 1 1 calc R . . C24 C 0.79028(13) 0.3099(4) 0.6897(2) 0.0285(10) Uani 1 1 d . . . H24A H 0.7733 0.3281 0.7147 0.043 Uiso 1 1 calc R . . H24B H 0.7738 0.2680 0.6463 0.043 Uiso 1 1 calc R . . H24C H 0.7999 0.3762 0.6760 0.043 Uiso 1 1 calc R . . C25 C 0.87551(13) 0.4225(4) 0.6448(2) 0.0281(10) Uani 1 1 d . . . C26 C 0.87539(14) 0.4711(4) 0.7059(2) 0.0339(11) Uani 1 1 d . . . H26 H 0.8835 0.4295 0.7486 0.041 Uiso 1 1 calc R . . C27 C 0.86405(13) 0.5771(4) 0.7068(2) 0.0327(11) Uani 1 1 d . . . H27 H 0.8643 0.6072 0.7495 0.039 Uiso 1 1 calc R . . C28 C 0.85226(14) 0.6393(4) 0.6454(3) 0.0385(11) Uani 1 1 d . . . H28 H 0.8445 0.7124 0.6454 0.046 Uiso 1 1 calc R . . C29 C 0.85193(14) 0.5938(4) 0.5843(2) 0.0368(11) Uani 1 1 d . . . H29 H 0.8436 0.6358 0.5418 0.044 Uiso 1 1 calc R . . C30 C 0.86343(14) 0.4882(4) 0.5839(2) 0.0333(11) Uani 1 1 d . . . H30 H 0.8632 0.4591 0.5411 0.040 Uiso 1 1 calc R . . C31 C 0.91374(14) 0.2705(4) 0.6008(2) 0.0309(10) Uani 1 1 d . . . C32 C 0.94522(13) 0.3374(4) 0.6036(2) 0.0327(11) Uani 1 1 d . . . H32 H 0.9502 0.4022 0.6306 0.039 Uiso 1 1 calc R . . C33 C 0.96997(14) 0.3138(4) 0.5688(2) 0.0376(11) Uani 1 1 d . . . H33 H 0.9914 0.3617 0.5723 0.045 Uiso 1 1 calc R . . C34 C 0.96301(15) 0.2199(4) 0.5289(3) 0.0414(13) Uani 1 1 d . . . H34 H 0.9797 0.2028 0.5050 0.050 Uiso 1 1 calc R . . C35 C 0.93202(16) 0.1521(4) 0.5243(3) 0.0416(13) Uani 1 1 d . . . H35 H 0.9269 0.0881 0.4965 0.050 Uiso 1 1 calc R . . C36 C 0.90816(15) 0.1762(4) 0.5598(2) 0.0372(11) Uani 1 1 d . . . H36 H 0.8871 0.1271 0.5564 0.045 Uiso 1 1 calc R . . C37 C 0.94755(13) 0.2762(4) 0.7676(2) 0.0367(12) Uani 1 1 d . . . H37A H 0.9663 0.2400 0.7512 0.055 Uiso 1 1 calc R . . H37B H 0.9535 0.2518 0.8164 0.055 Uiso 1 1 calc R . . H37C H 0.9516 0.3542 0.7679 0.055 Uiso 1 1 calc R . . C38 C 0.81631(14) 0.2342(4) 0.5511(2) 0.0380(12) Uani 1 1 d . . . H38A H 0.8281 0.2473 0.5168 0.057 Uiso 1 1 calc R . . H38B H 0.7982 0.2943 0.5494 0.057 Uiso 1 1 calc R . . H38C H 0.8003 0.1673 0.5383 0.057 Uiso 1 1 calc R . . B1 B 0.84079(15) 0.2526(4) 0.8181(2) 0.0256(11) Uani 1 1 d . . . B2 B 0.88668(16) 0.2971(4) 0.6439(3) 0.0302(12) Uani 1 1 d . . . C39 C 0.00325(16) 0.6464(4) 0.7871(3) 0.0437(13) Uani 1 1 d . . . C40 C 0.04115(17) 0.6280(5) 0.8434(3) 0.0535(14) Uani 1 1 d . . . H40 H 0.0642 0.6142 0.8334 0.064 Uiso 1 1 calc R . . C41 C 0.04698(18) 0.6289(5) 0.9140(3) 0.0555(14) Uani 1 1 d . . . H41 H 0.0737 0.6137 0.9511 0.067 Uiso 1 1 calc R . . C42 C 0.01638(18) 0.6502(5) 0.9316(3) 0.0566(16) Uani 1 1 d . . . H42 H 0.0210 0.6520 0.9806 0.068 Uiso 1 1 calc R . . C43 C -0.0227(2) 0.6699(5) 0.8766(3) 0.0675(18) Uani 1 1 d . . . H43 H -0.0450 0.6860 0.8882 0.081 Uiso 1 1 calc R . . C44 C -0.02945(18) 0.6664(5) 0.8050(3) 0.0627(17) Uani 1 1 d . . . H44 H -0.0565 0.6778 0.7679 0.075 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 Hf1 0.02754(10) 0.02609(9) 0.01640(9) 0.00007(8) 0.00665(7) -0.00163(9) O1 0.0318(17) 0.0313(18) 0.0240(16) 0.0015(13) 0.0112(14) -0.0007(14) O2 0.0314(17) 0.0286(17) 0.0254(16) -0.0014(13) 0.0099(14) 0.0013(14) O3 0.0316(17) 0.0286(16) 0.0226(15) 0.0000(13) 0.0103(13) -0.0038(14) O4 0.0371(18) 0.0261(17) 0.0221(15) 0.0015(13) 0.0096(14) -0.0018(14) O5 0.0320(16) 0.0257(16) 0.0132(13) -0.0001(12) 0.0049(12) 0.0010(13) O6 0.0267(16) 0.0266(16) 0.0160(14) 0.0006(12) 0.0051(12) 0.0004(13) O7 0.0270(16) 0.0365(18) 0.0165(14) 0.0043(13) 0.0060(12) -0.0039(14) O8 0.0282(16) 0.0325(17) 0.0132(14) 0.0018(12) 0.0043(12) -0.0017(13) C1 0.046(3) 0.041(3) 0.037(3) -0.008(2) 0.021(2) 0.001(3) C2 0.035(3) 0.036(3) 0.036(3) -0.007(2) 0.019(2) -0.006(2) C3 0.040(3) 0.050(3) 0.044(3) -0.013(3) 0.008(3) 0.012(3) C4 0.030(3) 0.046(3) 0.035(3) -0.002(2) 0.010(2) 0.004(2) C5 0.040(3) 0.074(4) 0.044(3) -0.018(3) -0.002(3) 0.017(3) C6 0.034(3) 0.040(3) 0.023(2) -0.004(2) 0.009(2) -0.008(2) C7 0.030(2) 0.038(3) 0.020(2) -0.0087(19) 0.0140(19) 0.000(2) C8 0.037(3) 0.025(2) 0.031(2) -0.0049(19) 0.011(2) -0.0051(19) C9 0.035(3) 0.028(2) 0.032(2) -0.0015(19) 0.014(2) 0.002(2) C10 0.058(3) 0.032(3) 0.039(3) 0.006(2) 0.010(3) -0.014(3) C11 0.034(3) 0.025(2) 0.022(2) 0.0015(18) 0.010(2) -0.0007(19) C12 0.038(2) 0.029(2) 0.022(2) 0.001(2) 0.0121(19) -0.003(2) C13 0.036(3) 0.033(3) 0.032(3) 0.002(2) 0.010(2) -0.007(2) C14 0.036(3) 0.039(3) 0.034(3) 0.009(2) 0.015(2) -0.002(2) C15 0.047(3) 0.036(3) 0.027(2) 0.003(2) 0.017(2) -0.001(2) C16 0.037(3) 0.032(3) 0.024(2) -0.0039(19) 0.012(2) -0.008(2) C17 0.035(2) 0.028(2) 0.0140(18) 0.0023(18) 0.0104(17) -0.002(2) C18 0.035(3) 0.033(3) 0.020(2) 0.0042(19) 0.0126(19) -0.003(2) C19 0.053(3) 0.028(2) 0.022(2) 0.0012(19) 0.020(2) 0.002(2) C20 0.053(3) 0.029(2) 0.020(2) -0.0040(19) 0.013(2) -0.013(2) C21 0.036(3) 0.036(3) 0.023(2) 0.001(2) 0.007(2) -0.009(2) C22 0.037(3) 0.033(3) 0.019(2) -0.0004(18) 0.0105(19) -0.004(2) C23 0.042(3) 0.041(3) 0.017(2) 0.004(2) 0.0037(19) 0.008(2) C24 0.031(2) 0.031(3) 0.020(2) -0.0010(18) 0.0078(19) 0.000(2) C25 0.029(2) 0.035(2) 0.021(2) -0.0016(19) 0.0115(19) -0.007(2) C26 0.042(3) 0.038(3) 0.025(2) 0.002(2) 0.017(2) -0.010(2) C27 0.037(3) 0.037(3) 0.030(3) -0.004(2) 0.020(2) -0.004(2) C28 0.039(3) 0.034(3) 0.047(3) 0.001(2) 0.022(2) -0.001(2) C29 0.039(3) 0.042(3) 0.028(2) 0.009(2) 0.013(2) 0.000(2) C30 0.038(3) 0.038(3) 0.024(2) -0.002(2) 0.014(2) -0.005(2) C31 0.036(3) 0.037(3) 0.018(2) 0.0092(19) 0.0100(19) 0.004(2) C32 0.031(2) 0.041(3) 0.023(2) 0.0054(19) 0.009(2) 0.003(2) C33 0.031(3) 0.049(3) 0.032(3) 0.011(2) 0.013(2) 0.003(2) C34 0.043(3) 0.052(3) 0.037(3) 0.014(2) 0.023(2) 0.017(3) C35 0.057(3) 0.034(3) 0.039(3) 0.007(2) 0.026(3) 0.011(2) C36 0.047(3) 0.038(3) 0.029(3) 0.005(2) 0.019(2) 0.003(2) C37 0.030(3) 0.046(3) 0.026(2) 0.005(2) 0.005(2) -0.007(2) C38 0.042(3) 0.044(3) 0.020(2) 0.003(2) 0.005(2) -0.007(2) B1 0.030(3) 0.029(3) 0.016(2) 0.001(2) 0.009(2) 0.000(2) B2 0.033(3) 0.036(3) 0.019(2) 0.004(2) 0.008(2) 0.000(2) C39 0.040(3) 0.037(3) 0.050(3) 0.002(2) 0.016(3) 0.002(2) C40 0.051(3) 0.059(4) 0.047(3) 0.014(3) 0.019(3) 0.002(3) C41 0.054(3) 0.062(4) 0.054(3) 0.009(3) 0.027(3) 0.007(3) C42 0.062(4) 0.061(4) 0.049(3) 0.012(3) 0.027(3) 0.010(3) C43 0.070(4) 0.080(5) 0.067(4) 0.009(4) 0.043(4) 0.006(4) C44 0.046(3) 0.092(5) 0.047(4) -0.007(3) 0.017(3) 0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Hf1 O1 2.129(3) . ? Hf1 O4 2.131(3) . ? Hf1 O3 2.132(3) . ? Hf1 O2 2.147(3) . ? Hf1 O6 2.175(3) . ? Hf1 O7 2.179(3) . ? Hf1 O5 2.215(3) . ? Hf1 O8 2.216(3) . ? O1 C2 1.273(5) . ? O2 C4 1.254(5) . ? O3 C7 1.280(5) . ? O4 C9 1.275(5) . ? O5 C23 1.436(5) . ? O5 B1 1.514(6) . ? O6 C24 1.415(5) . ? O6 B1 1.535(5) . ? O7 C37 1.424(5) . ? O7 B2 1.527(5) . ? O8 C38 1.424(5) . ? O8 B2 1.520(6) . ? C1 C2 1.506(6) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 C3 1.381(7) . ? C3 C4 1.403(7) . ? C3 H3 0.9500 . ? C4 C5 1.498(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.492(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.394(6) . ? C8 C9 1.391(6) . ? C8 H8 0.9500 . ? C9 C10 1.497(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.393(6) . ? C11 C16 1.402(5) . ? C11 B1 1.613(6) . ? C12 C13 1.393(6) . ? C12 H12 0.9500 . ? C13 C14 1.382(6) . ? C13 H13 0.9500 . ? C14 C15 1.388(6) . ? C14 H14 0.9500 . ? C15 C16 1.386(6) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 C22 1.405(6) . ? C17 C18 1.403(6) . ? C17 B1 1.609(6) . ? C18 C19 1.391(6) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C19 H19 0.9500 . ? C20 C21 1.373(6) . ? C20 H20 0.9500 . ? C21 C22 1.372(6) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.396(6) . ? C25 C30 1.398(6) . ? C25 B2 1.610(7) . ? C26 C27 1.381(7) . ? C26 H26 0.9500 . ? C27 C28 1.382(6) . ? C27 H27 0.9500 . ? C28 C29 1.373(6) . ? C28 H28 0.9500 . ? C29 C30 1.376(6) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.381(6) . ? C31 C36 1.407(6) . ? C31 B2 1.608(7) . ? C32 C33 1.393(6) . ? C32 H32 0.9500 . ? C33 C34 1.385(7) . ? C33 H33 0.9500 . ? C34 C35 1.363(7) . ? C34 H34 0.9500 . ? C35 C36 1.376(6) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.371(7) . ? C39 C44 1.394(7) . ? C39 C39 1.442(10) 2_556 ? C40 C41 1.375(7) . ? C40 H40 0.9500 . ? C41 C42 1.321(7) . ? C41 H41 0.9500 . ? C42 C43 1.388(8) . ? C42 H42 0.9500 . ? C43 C44 1.388(8) . ? C43 H43 0.9500 . ? C44 H44 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Hf1 O4 86.31(11) . . ? O1 Hf1 O3 77.40(11) . . ? O4 Hf1 O3 76.42(11) . . ? O1 Hf1 O2 76.50(11) . . ? O4 Hf1 O2 75.76(11) . . ? O3 Hf1 O2 142.71(12) . . ? O1 Hf1 O6 150.44(10) . . ? O4 Hf1 O6 102.07(11) . . ? O3 Hf1 O6 77.17(11) . . ? O2 Hf1 O6 132.95(10) . . ? O1 Hf1 O7 98.00(11) . . ? O4 Hf1 O7 148.98(11) . . ? O3 Hf1 O7 134.56(10) . . ? O2 Hf1 O7 75.47(11) . . ? O6 Hf1 O7 89.25(11) . . ? O1 Hf1 O5 148.88(11) . . ? O4 Hf1 O5 76.28(10) . . ? O3 Hf1 O5 121.79(10) . . ? O2 Hf1 O5 74.32(10) . . ? O6 Hf1 O5 60.00(10) . . ? O7 Hf1 O5 85.02(10) . . ? O1 Hf1 O8 78.50(11) . . ? O4 Hf1 O8 150.15(11) . . ? O3 Hf1 O8 75.27(10) . . ? O2 Hf1 O8 124.12(11) . . ? O6 Hf1 O8 80.67(10) . . ? O7 Hf1 O8 59.69(10) . . ? O5 Hf1 O8 127.64(11) . . ? C2 O1 Hf1 136.3(3) . . ? C4 O2 Hf1 136.5(3) . . ? C7 O3 Hf1 133.7(3) . . ? C9 O4 Hf1 135.3(3) . . ? C23 O5 B1 118.0(3) . . ? C23 O5 Hf1 131.3(3) . . ? B1 O5 Hf1 102.8(2) . . ? C24 O6 B1 121.6(3) . . ? C24 O6 Hf1 134.4(2) . . ? B1 O6 Hf1 103.8(2) . . ? C37 O7 B2 119.5(3) . . ? C37 O7 Hf1 133.8(3) . . ? B2 O7 Hf1 104.9(2) . . ? C38 O8 B2 119.2(3) . . ? C38 O8 Hf1 137.3(3) . . ? B2 O8 Hf1 103.5(2) . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? C2 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? O1 C2 C3 124.1(4) . . ? O1 C2 C1 115.9(4) . . ? C3 C2 C1 120.0(5) . . ? C2 C3 C4 122.1(5) . . ? C2 C3 H3 119.0 . . ? C4 C3 H3 119.0 . . ? O2 C4 C3 123.3(4) . . ? O2 C4 C5 116.5(4) . . ? C3 C4 C5 120.1(5) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 H6A 109.5 . . ? C7 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C7 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C8 123.4(4) . . ? O3 C7 C6 116.3(4) . . ? C8 C7 C6 120.3(4) . . ? C9 C8 C7 122.0(4) . . ? C9 C8 H8 119.0 . . ? C7 C8 H8 119.0 . . ? O4 C9 C8 123.2(4) . . ? O4 C9 C10 115.5(4) . . ? C8 C9 C10 121.2(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C16 116.0(4) . . ? C12 C11 B1 123.4(4) . . ? C16 C11 B1 120.6(4) . . ? C11 C12 C13 122.2(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 120.3(4) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 119.9(4) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 122.5(4) . . ? C15 C16 H16 118.7 . . ? C11 C16 H16 118.7 . . ? C22 C17 C18 115.7(4) . . ? C22 C17 B1 122.9(4) . . ? C18 C17 B1 121.4(4) . . ? C19 C18 C17 121.6(4) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C20 C19 C18 120.6(5) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C21 C20 C19 118.8(4) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C22 120.9(4) . . ? C20 C21 H21 119.5 . . ? C22 C21 H21 119.5 . . ? C21 C22 C17 122.4(5) . . ? C21 C22 H22 118.8 . . ? C17 C22 H22 118.8 . . ? O5 C23 H23A 109.5 . . ? O5 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O5 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C24 H24A 109.5 . . ? O6 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O6 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C26 C25 C30 115.8(4) . . ? C26 C25 B2 121.7(4) . . ? C30 C25 B2 122.4(4) . . ? C27 C26 C25 122.7(4) . . ? C27 C26 H26 118.7 . . ? C25 C26 H26 118.7 . . ? C26 C27 C28 119.7(4) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C29 C28 C27 119.0(5) . . ? C29 C28 H28 120.5 . . ? C27 C28 H28 120.5 . . ? C28 C29 C30 120.9(4) . . ? C28 C29 H29 119.5 . . ? C30 C29 H29 119.5 . . ? C29 C30 C25 121.9(4) . . ? C29 C30 H30 119.0 . . ? C25 C30 H30 119.0 . . ? C32 C31 C36 115.4(4) . . ? C32 C31 B2 122.0(4) . . ? C36 C31 B2 122.6(4) . . ? C31 C32 C33 122.8(5) . . ? C31 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C34 C33 C32 119.4(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C35 C34 C33 119.6(5) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 120.2(5) . . ? C34 C35 H35 119.9 . . ? C36 C35 H35 119.9 . . ? C35 C36 C31 122.6(5) . . ? C35 C36 H36 118.7 . . ? C31 C36 H36 118.7 . . ? O7 C37 H37A 109.5 . . ? O7 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? O7 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O8 C38 H38A 109.5 . . ? O8 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O8 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O5 B1 O6 92.1(3) . . ? O5 B1 C17 111.5(4) . . ? O6 B1 C17 114.5(3) . . ? O5 B1 C11 113.5(4) . . ? O6 B1 C11 110.3(3) . . ? C17 B1 C11 113.2(4) . . ? O8 B2 O7 91.8(3) . . ? O8 B2 C31 112.9(4) . . ? O7 B2 C31 112.3(4) . . ? O8 B2 C25 112.2(4) . . ? O7 B2 C25 110.9(4) . . ? C31 B2 C25 114.7(4) . . ? C40 C39 C44 116.5(5) . . ? C40 C39 C39 122.9(6) . 2_556 ? C44 C39 C39 120.7(6) . 2_556 ? C39 C40 C41 122.3(5) . . ? C39 C40 H40 118.9 . . ? C41 C40 H40 118.9 . . ? C42 C41 C40 121.7(6) . . ? C42 C41 H41 119.1 . . ? C40 C41 H41 119.1 . . ? C41 C42 C43 118.4(6) . . ? C41 C42 H42 120.8 . . ? C43 C42 H42 120.8 . . ? C42 C43 C44 120.8(6) . . ? C42 C43 H43 119.6 . . ? C44 C43 H43 119.6 . . ? C39 C44 C43 120.3(6) . . ? C39 C44 H44 119.8 . . ? C43 C44 H44 119.8 . . ? 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 O4 Hf1 O1 C2 -67.6(4) . . . . ? O3 Hf1 O1 C2 -144.5(4) . . . . ? O2 Hf1 O1 C2 8.6(4) . . . . ? O6 Hf1 O1 C2 -175.7(4) . . . . ? O7 Hf1 O1 C2 81.5(4) . . . . ? O5 Hf1 O1 C2 -12.1(5) . . . . ? O8 Hf1 O1 C2 138.3(4) . . . . ? O1 Hf1 O2 C4 -11.7(4) . . . . ? O4 Hf1 O2 C4 77.9(4) . . . . ? O3 Hf1 O2 C4 35.1(5) . . . . ? O6 Hf1 O2 C4 171.3(4) . . . . ? O7 Hf1 O2 C4 -113.8(5) . . . . ? O5 Hf1 O2 C4 157.4(5) . . . . ? O8 Hf1 O2 C4 -77.4(5) . . . . ? O1 Hf1 O3 C7 62.7(4) . . . . ? O4 Hf1 O3 C7 -26.5(3) . . . . ? O2 Hf1 O3 C7 16.2(4) . . . . ? O6 Hf1 O3 C7 -132.5(4) . . . . ? O7 Hf1 O3 C7 151.5(3) . . . . ? O5 Hf1 O3 C7 -90.6(4) . . . . ? O8 Hf1 O3 C7 143.9(4) . . . . ? O1 Hf1 O4 C9 -57.0(4) . . . . ? O3 Hf1 O4 C9 20.9(4) . . . . ? O2 Hf1 O4 C9 -134.0(4) . . . . ? O6 Hf1 O4 C9 94.3(4) . . . . ? O7 Hf1 O4 C9 -156.4(4) . . . . ? O5 Hf1 O4 C9 149.0(4) . . . . ? O8 Hf1 O4 C9 2.1(5) . . . . ? O1 Hf1 O5 C23 -15.8(5) . . . . ? O4 Hf1 O5 C23 42.0(3) . . . . ? O3 Hf1 O5 C23 106.2(4) . . . . ? O2 Hf1 O5 C23 -36.7(3) . . . . ? O6 Hf1 O5 C23 155.0(4) . . . . ? O7 Hf1 O5 C23 -113.0(4) . . . . ? O8 Hf1 O5 C23 -158.0(3) . . . . ? O1 Hf1 O5 B1 -162.8(2) . . . . ? O4 Hf1 O5 B1 -105.0(2) . . . . ? O3 Hf1 O5 B1 -40.8(3) . . . . ? O2 Hf1 O5 B1 176.2(3) . . . . ? O6 Hf1 O5 B1 7.9(2) . . . . ? O7 Hf1 O5 B1 99.9(2) . . . . ? O8 Hf1 O5 B1 54.9(3) . . . . ? O1 Hf1 O6 C24 -12.0(5) . . . . ? O4 Hf1 O6 C24 -116.1(3) . . . . ? O3 Hf1 O6 C24 -43.2(3) . . . . ? O2 Hf1 O6 C24 162.2(3) . . . . ? O7 Hf1 O6 C24 93.0(3) . . . . ? O5 Hf1 O6 C24 177.7(4) . . . . ? O8 Hf1 O6 C24 33.7(3) . . . . ? O1 Hf1 O6 B1 162.5(3) . . . . ? O4 Hf1 O6 B1 58.4(2) . . . . ? O3 Hf1 O6 B1 131.2(2) . . . . ? O2 Hf1 O6 B1 -23.3(3) . . . . ? O7 Hf1 O6 B1 -92.5(2) . . . . ? O5 Hf1 O6 B1 -7.8(2) . . . . ? O8 Hf1 O6 B1 -151.9(2) . . . . ? O1 Hf1 O7 C37 -95.1(4) . . . . ? O4 Hf1 O7 C37 1.1(5) . . . . ? O3 Hf1 O7 C37 -175.3(3) . . . . ? O2 Hf1 O7 C37 -21.3(4) . . . . ? O6 Hf1 O7 C37 113.7(4) . . . . ? O5 Hf1 O7 C37 53.7(4) . . . . ? O8 Hf1 O7 C37 -166.7(4) . . . . ? O1 Hf1 O7 B2 69.1(3) . . . . ? O4 Hf1 O7 B2 165.3(3) . . . . ? O3 Hf1 O7 B2 -11.1(3) . . . . ? O2 Hf1 O7 B2 142.8(3) . . . . ? O6 Hf1 O7 B2 -82.1(3) . . . . ? O5 Hf1 O7 B2 -142.1(3) . . . . ? O8 Hf1 O7 B2 -2.5(2) . . . . ? O1 Hf1 O8 C38 74.6(4) . . . . ? O4 Hf1 O8 C38 13.7(5) . . . . ? O3 Hf1 O8 C38 -5.2(4) . . . . ? O2 Hf1 O8 C38 139.4(4) . . . . ? O6 Hf1 O8 C38 -84.3(4) . . . . ? O7 Hf1 O8 C38 -178.9(4) . . . . ? O5 Hf1 O8 C38 -124.2(4) . . . . ? O1 Hf1 O8 B2 -103.9(3) . . . . ? O4 Hf1 O8 B2 -164.8(3) . . . . ? O3 Hf1 O8 B2 176.2(3) . . . . ? O2 Hf1 O8 B2 -39.1(3) . . . . ? O6 Hf1 O8 B2 97.2(3) . . . . ? O7 Hf1 O8 B2 2.5(2) . . . . ? O5 Hf1 O8 B2 57.2(3) . . . . ? Hf1 O1 C2 C3 -3.1(8) . . . . ? Hf1 O1 C2 C1 178.7(3) . . . . ? O1 C2 C3 C4 -5.4(9) . . . . ? C1 C2 C3 C4 172.7(5) . . . . ? Hf1 O2 C4 C3 8.8(8) . . . . ? Hf1 O2 C4 C5 -172.0(4) . . . . ? C2 C3 C4 O2 2.8(9) . . . . ? C2 C3 C4 C5 -176.3(5) . . . . ? Hf1 O3 C7 C8 21.4(6) . . . . ? Hf1 O3 C7 C6 -160.4(3) . . . . ? O3 C7 C8 C9 3.0(7) . . . . ? C6 C7 C8 C9 -175.1(4) . . . . ? Hf1 O4 C9 C8 -9.9(7) . . . . ? Hf1 O4 C9 C10 171.7(3) . . . . ? C7 C8 C9 O4 -8.6(7) . . . . ? C7 C8 C9 C10 169.8(5) . . . . ? C16 C11 C12 C13 0.4(6) . . . . ? B1 C11 C12 C13 -178.7(4) . . . . ? C11 C12 C13 C14 -0.9(7) . . . . ? C12 C13 C14 C15 0.6(7) . . . . ? C13 C14 C15 C16 0.3(7) . . . . ? C14 C15 C16 C11 -0.9(7) . . . . ? C12 C11 C16 C15 0.6(7) . . . . ? B1 C11 C16 C15 179.7(4) . . . . ? C22 C17 C18 C19 1.2(6) . . . . ? B1 C17 C18 C19 -179.0(4) . . . . ? C17 C18 C19 C20 -2.1(6) . . . . ? C18 C19 C20 C21 1.5(6) . . . . ? C19 C20 C21 C22 -0.1(6) . . . . ? C20 C21 C22 C17 -0.7(7) . . . . ? C18 C17 C22 C21 0.2(6) . . . . ? B1 C17 C22 C21 -179.7(4) . . . . ? C30 C25 C26 C27 0.2(7) . . . . ? B2 C25 C26 C27 -176.9(4) . . . . ? C25 C26 C27 C28 -0.1(7) . . . . ? C26 C27 C28 C29 0.3(7) . . . . ? C27 C28 C29 C30 -0.5(7) . . . . ? C28 C29 C30 C25 0.6(7) . . . . ? C26 C25 C30 C29 -0.4(7) . . . . ? B2 C25 C30 C29 176.6(4) . . . . ? C36 C31 C32 C33 -0.1(6) . . . . ? B2 C31 C32 C33 177.6(4) . . . . ? C31 C32 C33 C34 0.3(7) . . . . ? C32 C33 C34 C35 0.1(7) . . . . ? C33 C34 C35 C36 -0.8(7) . . . . ? C34 C35 C36 C31 1.1(7) . . . . ? C32 C31 C36 C35 -0.6(7) . . . . ? B2 C31 C36 C35 -178.3(4) . . . . ? C23 O5 B1 O6 -162.1(3) . . . . ? Hf1 O5 B1 O6 -9.7(3) . . . . ? C23 O5 B1 C17 80.5(4) . . . . ? Hf1 O5 B1 C17 -127.1(3) . . . . ? C23 O5 B1 C11 -48.9(5) . . . . ? Hf1 O5 B1 C11 103.5(3) . . . . ? C24 O6 B1 O5 -174.7(3) . . . . ? Hf1 O6 B1 O5 10.0(3) . . . . ? C24 O6 B1 C17 -59.9(5) . . . . ? Hf1 O6 B1 C17 124.8(3) . . . . ? C24 O6 B1 C11 69.2(5) . . . . ? Hf1 O6 B1 C11 -106.1(3) . . . . ? C22 C17 B1 O5 3.8(5) . . . . ? C18 C17 B1 O5 -176.1(3) . . . . ? C22 C17 B1 O6 -99.1(4) . . . . ? C18 C17 B1 O6 81.1(5) . . . . ? C22 C17 B1 C11 133.3(4) . . . . ? C18 C17 B1 C11 -46.5(5) . . . . ? C12 C11 B1 O5 -89.5(5) . . . . ? C16 C11 B1 O5 91.5(5) . . . . ? C12 C11 B1 O6 12.3(6) . . . . ? C16 C11 B1 O6 -166.8(4) . . . . ? C12 C11 B1 C17 142.0(4) . . . . ? C16 C11 B1 C17 -37.0(6) . . . . ? C38 O8 B2 O7 178.0(3) . . . . ? Hf1 O8 B2 O7 -3.1(3) . . . . ? C38 O8 B2 C31 -66.8(5) . . . . ? Hf1 O8 B2 C31 112.1(3) . . . . ? C38 O8 B2 C25 64.6(5) . . . . ? Hf1 O8 B2 C25 -116.6(3) . . . . ? C37 O7 B2 O8 170.1(3) . . . . ? Hf1 O7 B2 O8 3.2(3) . . . . ? C37 O7 B2 C31 54.5(5) . . . . ? Hf1 O7 B2 C31 -112.5(3) . . . . ? C37 O7 B2 C25 -75.3(5) . . . . ? Hf1 O7 B2 C25 117.8(3) . . . . ? C32 C31 B2 O8 169.0(4) . . . . ? C36 C31 B2 O8 -13.5(6) . . . . ? C32 C31 B2 O7 -89.0(5) . . . . ? C36 C31 B2 O7 88.6(5) . . . . ? C32 C31 B2 C25 38.8(6) . . . . ? C36 C31 B2 C25 -143.6(4) . . . . ? C26 C25 B2 O8 88.1(5) . . . . ? C30 C25 B2 O8 -88.8(5) . . . . ? C26 C25 B2 O7 -12.9(6) . . . . ? C30 C25 B2 O7 170.2(4) . . . . ? C26 C25 B2 C31 -141.4(4) . . . . ? C30 C25 B2 C31 41.7(6) . . . . ? C44 C39 C40 C41 0.1(9) . . . . ? C39 C39 C40 C41 179.6(4) 2_556 . . . ? C39 C40 C41 C42 -1.7(10) . . . . ? C40 C41 C42 C43 1.3(10) . . . . ? C41 C42 C43 C44 0.5(10) . . . . ? C40 C39 C44 C43 1.7(9) . . . . ? C39 C39 C44 C43 -177.8(5) 2_556 . . . ? C42 C43 C44 C39 -2.1(10) . . . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 28.32 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 2.046 _refine_diff_density_min -1.191 _refine_diff_density_rms 0.111