data_1 _audit_creation_method 'APEX2 v2014.5-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common 'TiOBut OBc 1:4' _chemical_formula_moiety ? _chemical_formula_sum 'C19 H36 O7 Ti' _chemical_formula_iupac ? _chemical_formula_weight 424.38 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system orthorhombic _space_group_name_H-M_alt 'P m n 21' _space_group_name_Hall 'P 2ac -2' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y, z+1/2' '-x, y, z' _cell_length_a 15.9892(11) _cell_length_b 8.1331(6) _cell_length_c 9.2864(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 1207.62(14) _cell_formula_units_Z 2 _cell_measurement_reflns_used 1832 _cell_measurement_theta_min 2.5363 _cell_measurement_theta_max 20.1599 _cell_measurement_temperature 173.(2) _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.167 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 456 _exptl_absorpt_coefficient_mu 0.386 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min .924 _exptl_absorpt_correction_T_max .955 _exptl_special_details ; ; _diffrn_ambient_temperature 173.(2) _diffrn_source 'fine-focus tube' _diffrn_source_type ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 11242 _diffrn_reflns_av_R_equivalents 0.1432 _diffrn_reflns_av_unetI/netI 0.1147 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.25 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measured_fraction_theta_full 1.000 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _refine_special_details ; ; _reflns_number_total 2273 _reflns_number_gt 1402 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1242 _refine_ls_R_factor_gt 0.0617 _refine_ls_wR_factor_gt 0.1438 _refine_ls_wR_factor_ref 0.1892 _refine_ls_goodness_of_fit_ref 0.934 _refine_ls_restrained_S_all 0.934 _refine_ls_number_reflns 2273 _refine_ls_number_parameters 136 _refine_ls_number_restraints 1 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment noref _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1114P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.018 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.600 _refine_diff_density_min -0.596 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details ; Flack x determined using 485 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.46(4) 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti 0.2776 0.4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'Bruker XT Intrinsic Solution Method' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Ti Ti1 0.5 0.3775(3) 0.6379(2) 0.0334(6) Uani d T P S 1 . . O O1 0.5 0.4553(11) 0.4234(8) 0.043(2) Uani d T P S 1 . . O O2 0.5 0.1974(10) 0.4804(9) 0.039(2) Uani d T P S 1 . . O O3 0.5808(3) 0.2519(8) 0.7705(6) 0.0404(15) Uani d . . . 1 . . O O4 0.6301(4) 0.3870(8) 0.5911(6) 0.0453(18) Uani d . . . 1 . . O O5 0.5 0.5716(9) 0.7121(9) 0.040(2) Uani d T P S 1 . . C C1 0.5 0.3066(17) 0.3824(14) 0.034(3) Uani d T P S 1 . . C C2 0.5 0.2612(18) 0.2245(14) 0.049(4) Uani d T P S 1 . . C C3 0.5 0.414(2) 0.132(2) 0.093(6) Uani d T P S 1 . . H H3A 0.4786 0.3874 0.0361 0.139 Uiso calc U P . 0.5 . . H H3B 0.5572 0.4566 0.124 0.139 Uiso calc U P . 0.5 . . H H3C 0.4642 0.4979 0.1765 0.139 Uiso calc U P . 0.5 . . C C4 0.4223(10) 0.163(2) 0.1945(16) 0.120(6) Uani d . . . 1 . . H H4A 0.4226 0.1268 0.094 0.18 Uiso calc U . . 1 . . H H4B 0.373 0.232 0.2118 0.18 Uiso calc U . . 1 . . H H4C 0.4206 0.0673 0.2582 0.18 Uiso calc U . . 1 . . C C5 0.6443(6) 0.3012(11) 0.7030(11) 0.038(2) Uani d . . . 1 . . C C6 0.7321(5) 0.2646(12) 0.7511(10) 0.042(2) Uani d . . . 1 . . C C7 0.7884(8) 0.2356(17) 0.6236(15) 0.091(4) Uani d . . . 1 . . H H7A 0.7667 0.1435 0.5666 0.136 Uiso calc U . . 1 . . H H7B 0.8449 0.2095 0.6574 0.136 Uiso calc U . . 1 . . H H7C 0.7901 0.3348 0.5638 0.136 Uiso calc U . . 1 . . C C8 0.7350(7) 0.1178(19) 0.8509(16) 0.104(6) Uani d . . . 1 . . H H8A 0.7166 0.0194 0.7989 0.155 Uiso calc U . . 1 . . H H8B 0.6978 0.1371 0.9332 0.155 Uiso calc U . . 1 . . H H8C 0.7923 0.1019 0.8855 0.155 Uiso calc U . . 1 . . C C9 0.7600(9) 0.4189(19) 0.832(2) 0.140(8) Uani d . . . 1 . . H H9A 0.7711 0.5072 0.7624 0.21 Uiso calc U . . 1 . . H H9B 0.8111 0.395 0.8862 0.21 Uiso calc U . . 1 . . H H9C 0.7158 0.4535 0.8981 0.21 Uiso calc U . . 1 . . C C10 0.5 0.7511(15) 0.7086(15) 0.043(3) Uani d T P S 1 . . C C11 0.4230(7) 0.8045(13) 0.626(2) 0.094(4) Uani d . . . 1 . . H H11A 0.4227 0.9245 0.6172 0.141 Uiso calc U . . 1 . . H H11B 0.3728 0.7688 0.678 0.141 Uiso calc U . . 1 . . H H11C 0.4237 0.7547 0.5301 0.141 Uiso calc U . . 1 . . C C12 0.5 0.810(2) 0.8618(19) 0.108(8) Uani d T P S 1 . . H H12A 0.455 0.8901 0.8753 0.162 Uiso calc U P . 0.5 . . H H12B 0.5539 0.8615 0.8837 0.162 Uiso calc U P . 0.5 . . H H12C 0.4911 0.7162 0.9264 0.162 Uiso calc U P . 0.5 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ti1 0.0386(11) 0.0338(12) 0.0280(11) 0 0 0.0028(12) O1 0.062(6) 0.040(6) 0.026(5) 0 0 0.000(4) O2 0.053(5) 0.030(5) 0.035(5) 0 0 0.003(5) O3 0.039(3) 0.047(4) 0.035(4) -0.002(3) 0.001(3) 0.007(3) O4 0.043(4) 0.054(4) 0.039(5) -0.004(3) 0.001(3) 0.007(3) O5 0.050(5) 0.032(5) 0.038(5) 0 0 -0.004(4) C1 0.030(6) 0.036(8) 0.038(7) 0 0 -0.007(7) C2 0.055(8) 0.064(10) 0.028(8) 0 0 -0.013(7) C3 0.151(16) 0.099(14) 0.028(7) 0 0 -0.010(12) C4 0.140(14) 0.173(15) 0.048(8) -0.078(11) -0.021(8) -0.012(9) C5 0.056(6) 0.031(5) 0.027(5) -0.005(5) 0.004(5) -0.002(5) C6 0.040(5) 0.049(6) 0.036(5) 0.002(4) -0.003(4) -0.002(4) C7 0.078(7) 0.139(11) 0.055(8) 0.048(7) 0.017(7) 0.012(10) C8 0.048(6) 0.141(13) 0.122(13) -0.004(8) -0.019(7) 0.089(10) C9 0.100(11) 0.107(12) 0.21(2) 0.018(10) -0.090(12) -0.089(13) C10 0.048(8) 0.035(7) 0.047(8) 0 0 -0.002(7) C11 0.088(9) 0.049(6) 0.144(12) 0.003(5) -0.048(10) 0.001(11) C12 0.22(3) 0.050(11) 0.059(13) 0 0 -0.017(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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Ti1 O5 . 1.723(8) ? Ti1 O3 4_655 2.057(6) ? Ti1 O3 . 2.057(6) ? Ti1 O2 . 2.070(8) ? Ti1 O1 . 2.090(8) ? Ti1 O4 . 2.126(6) ? Ti1 O4 4_655 2.126(6) ? Ti1 C1 . 2.441(13) ? Ti1 C5 . 2.465(9) ? Ti1 C5 4_655 2.465(9) ? O1 C1 . 1.267(14) ? O2 C1 . 1.271(14) ? O3 C5 . 1.259(10) ? O4 C5 . 1.272(10) ? O5 C10 . 1.460(14) ? C1 C2 . 1.512(17) ? C2 C4 . 1.502(14) ? C2 C4 4_655 1.502(14) ? C2 C3 . 1.51(2) ? C5 C6 . 1.504(12) ? C6 C7 . 1.505(15) ? C6 C8 . 1.512(15) ? C6 C9 . 1.528(16) ? C10 C12 . 1.50(2) ? C10 C11 4_655 1.513(14) ? C10 C11 . 1.513(14) ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O5 Ti1 O3 . 4_655 102.4(3) ? O5 Ti1 O3 . . 102.4(3) ? O3 Ti1 O3 4_655 . 77.8(3) ? O5 Ti1 O2 . . 158.6(4) ? O3 Ti1 O2 4_655 . 94.1(3) ? O3 Ti1 O2 . . 94.1(3) ? O5 Ti1 O1 . . 96.0(4) ? O3 Ti1 O1 4_655 . 136.1(2) ? O3 Ti1 O1 . . 136.1(2) ? O2 Ti1 O1 . . 62.7(3) ? O5 Ti1 O4 . . 92.78(19) ? O3 Ti1 O4 4_655 . 139.0(2) ? O3 Ti1 O4 . . 61.7(2) ? O2 Ti1 O4 . . 83.19(18) ? O1 Ti1 O4 . . 78.14(16) ? O5 Ti1 O4 . 4_655 92.78(19) ? O3 Ti1 O4 4_655 4_655 61.7(2) ? O3 Ti1 O4 . 4_655 139.0(2) ? O2 Ti1 O4 . 4_655 83.19(18) ? O1 Ti1 O4 . 4_655 78.14(16) ? O4 Ti1 O4 . 4_655 156.1(3) ? O5 Ti1 C1 . . 127.3(4) ? O3 Ti1 C1 4_655 . 117.7(3) ? O3 Ti1 C1 . . 117.7(3) ? O2 Ti1 C1 . . 31.4(4) ? O1 Ti1 C1 . . 31.3(4) ? O4 Ti1 C1 . . 79.06(17) ? O4 Ti1 C1 4_655 . 79.06(17) ? O5 Ti1 C5 . . 97.6(2) ? O3 Ti1 C5 4_655 . 108.4(3) ? O3 Ti1 C5 . . 30.7(3) ? O2 Ti1 C5 . . 89.7(2) ? O1 Ti1 C5 . . 108.1(2) ? O4 Ti1 C5 . . 31.1(2) ? O4 Ti1 C5 4_655 . 167.2(3) ? C1 Ti1 C5 . . 100.3(3) ? O5 Ti1 C5 . 4_655 97.6(2) ? O3 Ti1 C5 4_655 4_655 30.7(3) ? O3 Ti1 C5 . 4_655 108.4(3) ? O2 Ti1 C5 . 4_655 89.7(2) ? O1 Ti1 C5 . 4_655 108.1(2) ? O4 Ti1 C5 . 4_655 167.2(3) ? O4 Ti1 C5 4_655 4_655 31.1(2) ? C1 Ti1 C5 . 4_655 100.3(3) ? C5 Ti1 C5 . 4_655 138.8(5) ? C1 O1 Ti1 . . 89.8(7) ? C1 O2 Ti1 . . 90.6(7) ? C5 O3 Ti1 . . 92.8(6) ? C5 O4 Ti1 . . 89.3(5) ? C10 O5 Ti1 . . 155.1(8) ? O1 C1 O2 . . 116.9(11) ? O1 C1 C2 . . 121.6(12) ? O2 C1 C2 . . 121.5(11) ? O1 C1 Ti1 . . 58.9(6) ? O2 C1 Ti1 . . 58.0(6) ? C2 C1 Ti1 . . 179.5(10) ? C4 C2 C4 . 4_655 111.6(19) ? C4 C2 C3 . . 109.3(10) ? C4 C2 C3 4_655 . 109.3(10) ? C4 C2 C1 . . 108.0(8) ? C4 C2 C1 4_655 . 108.0(8) ? C3 C2 C1 . . 110.4(12) ? O3 C5 O4 . . 116.0(8) ? O3 C5 C6 . . 122.8(9) ? O4 C5 C6 . . 121.2(9) ? O3 C5 Ti1 . . 56.5(5) ? O4 C5 Ti1 . . 59.6(5) ? C6 C5 Ti1 . . 175.7(7) ? C5 C6 C7 . . 110.8(9) ? C5 C6 C8 . . 111.5(8) ? C7 C6 C8 . . 109.9(9) ? C5 C6 C9 . . 104.8(8) ? C7 C6 C9 . . 109.8(12) ? C8 C6 C9 . . 109.8(11) ? O5 C10 C12 . . 107.3(11) ? O5 C10 C11 . 4_655 107.3(8) ? C12 C10 C11 . 4_655 112.8(9) ? O5 C10 C11 . . 107.3(8) ? C12 C10 C11 . . 112.8(9) ? C11 C10 C11 4_655 . 108.9(16) ? #===END data_dyjn212a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H84 O26 Zr4' _chemical_formula_weight 1442.03 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' '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.0666(4) _cell_length_b 12.2893(3) _cell_length_c 19.4521(5) _cell_angle_alpha 90.00 _cell_angle_beta 91.102(2) _cell_angle_gamma 90.00 _cell_volume 3123.03(15) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5072 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 25.21 _exptl_crystal_description colourless _exptl_crystal_colour prism _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1480 _exptl_absorpt_coefficient_mu 0.726 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8608 _exptl_absorpt_correction_T_max 0.9161 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 20534 _diffrn_reflns_av_R_equivalents 0.0430 _diffrn_reflns_av_sigmaI/netI 0.0405 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.23 _reflns_number_total 5637 _reflns_number_gt 4544 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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 5637 _refine_ls_number_parameters 366 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0491 _refine_ls_R_factor_gt 0.0344 _refine_ls_wR_factor_ref 0.1316 _refine_ls_wR_factor_gt 0.1129 _refine_ls_goodness_of_fit_ref 0.959 _refine_ls_restrained_S_all 0.959 _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 0.52267(3) 0.05614(3) 0.338750(18) 0.02077(14) Uani 1 1 d . . . Zr2 Zr 0.53342(3) -0.12642(3) 0.476287(18) 0.01860(14) Uani 1 1 d . . . O1 O 0.5578(2) 0.2240(2) 0.35668(14) 0.0273(6) Uani 1 1 d . . . O2 O 0.3720(2) 0.1388(2) 0.34490(14) 0.0287(7) Uani 1 1 d . . . O3 O 0.4830(3) 0.1207(3) 0.23143(15) 0.0387(8) Uani 1 1 d . . . O4 O 0.6203(3) 0.0274(3) 0.24788(15) 0.0389(8) Uani 1 1 d . . . O5 O 0.4061(2) -0.0625(2) 0.31384(14) 0.0301(7) Uani 1 1 d . . . O6 O 0.4004(2) -0.1648(2) 0.40924(14) 0.0297(7) Uani 1 1 d . . . O7 O 0.5855(2) -0.1164(2) 0.35855(14) 0.0257(6) Uani 1 1 d . . . O8 O 0.6011(2) -0.2673(2) 0.41588(14) 0.0309(7) Uani 1 1 d . . . O9 O 0.4324(2) -0.2406(2) 0.52895(14) 0.0287(7) Uani 1 1 d . . . O10 O 0.6309(2) -0.2127(2) 0.55009(14) 0.0274(6) Uani 1 1 d . . . O11 O 0.5060(2) -0.0286(2) 0.56091(13) 0.0189(6) Uani 1 1 d . . . O12 O 0.6835(2) -0.0494(2) 0.47322(15) 0.0271(7) Uani 1 1 d . . . O13 O 0.6815(2) 0.0647(2) 0.38284(14) 0.0269(7) Uani 1 1 d . . . C1 C 0.5756(3) 0.2788(3) 0.4111(2) 0.0280(9) Uani 1 1 d . . . C2 C 0.6081(5) 0.3958(4) 0.4019(3) 0.0452(13) Uani 1 1 d . . . H2 H 0.6663 0.3950 0.3693 0.054 Uiso 1 1 calc R . . C3 C 0.6475(5) 0.4484(4) 0.4666(3) 0.0531(15) Uani 1 1 d . . . H3A H 0.6686 0.5232 0.4566 0.080 Uiso 1 1 calc R . . H3B H 0.7063 0.4072 0.4847 0.080 Uiso 1 1 calc R . . H3C H 0.5933 0.4493 0.5007 0.080 Uiso 1 1 calc R . . C4 C 0.5233(6) 0.4546(5) 0.3668(5) 0.084(2) Uani 1 1 d . . . H4A H 0.4605 0.4458 0.3930 0.125 Uiso 1 1 calc R . . H4B H 0.5128 0.4249 0.3205 0.125 Uiso 1 1 calc R . . H4C H 0.5405 0.5321 0.3638 0.125 Uiso 1 1 calc R . . C5 C 0.3306(3) 0.1948(3) 0.3908(2) 0.0261(9) Uani 1 1 d . . . C6 C 0.2278(4) 0.2470(4) 0.3746(2) 0.0353(11) Uani 1 1 d . . . H6 H 0.2057 0.2225 0.3276 0.042 Uiso 1 1 calc R . . C7 C 0.1482(5) 0.2094(8) 0.4242(4) 0.106(3) Uani 1 1 d . . . H7A H 0.1680 0.2320 0.4709 0.158 Uiso 1 1 calc R . . H7B H 0.1428 0.1299 0.4224 0.158 Uiso 1 1 calc R . . H7C H 0.0819 0.2417 0.4116 0.158 Uiso 1 1 calc R . . C8 C 0.2359(6) 0.3667(5) 0.3730(5) 0.083(2) Uani 1 1 d . . . H8A H 0.1732 0.3975 0.3525 0.125 Uiso 1 1 calc R . . H8B H 0.2947 0.3878 0.3455 0.125 Uiso 1 1 calc R . . H8C H 0.2453 0.3943 0.4200 0.125 Uiso 1 1 calc R . . C9 C 0.5608(4) 0.0777(3) 0.2068(2) 0.0286(10) Uani 1 1 d . . . C10 C 0.5839(4) 0.0820(4) 0.1311(2) 0.0353(11) Uani 1 1 d . . . H10 H 0.6554 0.1100 0.1268 0.042 Uiso 1 1 calc R . . C11 C 0.5138(5) 0.1598(5) 0.0918(3) 0.0640(18) Uani 1 1 d . . . H11A H 0.4436 0.1316 0.0917 0.096 Uiso 1 1 calc R . . H11B H 0.5369 0.1665 0.0443 0.096 Uiso 1 1 calc R . . H11C H 0.5156 0.2314 0.1140 0.096 Uiso 1 1 calc R . . C12 C 0.5816(5) -0.0323(5) 0.1010(3) 0.0544(15) Uani 1 1 d . . . H12A H 0.6303 -0.0785 0.1264 0.082 Uiso 1 1 calc R . . H12B H 0.6004 -0.0294 0.0525 0.082 Uiso 1 1 calc R . . H12C H 0.5125 -0.0626 0.1048 0.082 Uiso 1 1 calc R . . C13 C 0.3686(4) -0.1374(4) 0.3503(2) 0.0305(10) Uani 1 1 d . . . C14 C 0.2784(4) -0.1991(5) 0.3189(2) 0.0461(13) Uani 1 1 d . . . H14 H 0.2903 -0.2032 0.2683 0.055 Uiso 1 1 calc R . . C15 C 0.1819(5) -0.1325(6) 0.3280(4) 0.073(2) Uani 1 1 d . . . H15A H 0.1249 -0.1669 0.3028 0.109 Uiso 1 1 calc R . . H15B H 0.1925 -0.0588 0.3102 0.109 Uiso 1 1 calc R . . H15C H 0.1658 -0.1287 0.3770 0.109 Uiso 1 1 calc R . . C16 C 0.2699(5) -0.3137(5) 0.3439(3) 0.0613(16) Uani 1 1 d . . . H16A H 0.3353 -0.3511 0.3380 0.092 Uiso 1 1 calc R . . H16B H 0.2161 -0.3515 0.3174 0.092 Uiso 1 1 calc R . . H16C H 0.2525 -0.3135 0.3927 0.092 Uiso 1 1 calc R . . C17 C 0.6119(3) -0.2169(3) 0.3605(2) 0.0274(9) Uani 1 1 d . . . C18 C 0.6512(4) -0.2710(4) 0.2971(2) 0.0421(12) Uani 1 1 d . . . H18 H 0.6723 -0.3468 0.3095 0.050 Uiso 1 1 calc R . . C19 C 0.7446(5) -0.2112(4) 0.2707(3) 0.0567(16) Uani 1 1 d . . . H19A H 0.7245 -0.1382 0.2551 0.085 Uiso 1 1 calc R . . H19B H 0.7733 -0.2517 0.2322 0.085 Uiso 1 1 calc R . . H19C H 0.7962 -0.2050 0.3077 0.085 Uiso 1 1 calc R . . C20 C 0.5644(6) -0.2777(5) 0.2438(3) 0.0670(18) Uani 1 1 d . . . H20A H 0.5064 -0.3168 0.2634 0.100 Uiso 1 1 calc R . . H20B H 0.5881 -0.3166 0.2032 0.100 Uiso 1 1 calc R . . H20C H 0.5429 -0.2041 0.2307 0.100 Uiso 1 1 calc R . . C21 C 0.7229(3) 0.0226(3) 0.4356(2) 0.0259(9) Uani 1 1 d . . . C22 C 0.8311(4) 0.0596(4) 0.4552(3) 0.0401(12) Uani 1 1 d . . . H22 H 0.8444 0.0374 0.5040 0.048 Uiso 1 1 calc R . . C23 C 0.9066(4) -0.0002(5) 0.4116(3) 0.0556(15) Uani 1 1 d . . . H23A H 0.8929 0.0164 0.3630 0.083 Uiso 1 1 calc R . . H23B H 0.8996 -0.0787 0.4191 0.083 Uiso 1 1 calc R . . H23C H 0.9762 0.0227 0.4242 0.083 Uiso 1 1 calc R . . C24 C 0.8415(4) 0.1810(4) 0.4518(3) 0.0459(13) Uani 1 1 d . . . H24A H 0.8279 0.2056 0.4046 0.069 Uiso 1 1 calc R . . H24B H 0.9112 0.2019 0.4660 0.069 Uiso 1 1 calc R . . H24C H 0.7923 0.2147 0.4827 0.069 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 0.0251(2) 0.0222(2) 0.0151(2) 0.00049(14) 0.00310(16) -0.00032(16) Zr2 0.0229(2) 0.0173(2) 0.0157(2) -0.00128(13) 0.00251(15) -0.00107(15) O1 0.0347(17) 0.0250(15) 0.0223(15) 0.0022(12) 0.0044(12) -0.0016(13) O2 0.0289(16) 0.0355(17) 0.0217(15) -0.0006(12) -0.0001(12) 0.0036(13) O3 0.042(2) 0.054(2) 0.0205(16) 0.0077(14) 0.0039(14) 0.0130(16) O4 0.046(2) 0.0475(19) 0.0231(16) 0.0103(14) 0.0094(14) 0.0189(16) O5 0.0356(18) 0.0324(17) 0.0222(15) -0.0005(12) -0.0045(13) -0.0047(14) O6 0.0327(17) 0.0334(16) 0.0228(15) -0.0003(12) -0.0036(12) -0.0110(14) O7 0.0301(16) 0.0205(15) 0.0268(16) -0.0017(11) 0.0065(12) -0.0010(12) O8 0.0457(19) 0.0227(15) 0.0245(16) -0.0016(12) 0.0084(13) 0.0031(14) O9 0.0375(17) 0.0278(15) 0.0209(15) 0.0018(12) 0.0032(12) -0.0086(13) O10 0.0346(17) 0.0257(15) 0.0220(15) 0.0014(12) 0.0009(12) 0.0060(13) O11 0.0211(14) 0.0195(13) 0.0162(13) -0.0017(11) 0.0019(10) -0.0009(11) O12 0.0231(16) 0.0294(16) 0.0289(16) 0.0041(12) 0.0016(12) -0.0009(12) O13 0.0257(16) 0.0284(16) 0.0268(16) 0.0024(12) 0.0039(12) -0.0024(12) C1 0.030(2) 0.023(2) 0.031(2) 0.0004(18) 0.0044(18) -0.0035(18) C2 0.067(4) 0.030(3) 0.039(3) 0.004(2) 0.007(2) -0.011(3) C3 0.068(4) 0.030(3) 0.061(4) -0.007(2) 0.005(3) -0.011(3) C4 0.093(6) 0.030(3) 0.126(7) 0.014(3) -0.041(5) -0.003(3) C5 0.024(2) 0.029(2) 0.025(2) 0.0082(18) 0.0038(17) -0.0022(18) C6 0.035(3) 0.044(3) 0.027(2) 0.006(2) 0.0034(19) 0.007(2) C7 0.036(4) 0.153(8) 0.129(7) 0.080(6) 0.030(4) 0.035(4) C8 0.057(4) 0.053(4) 0.138(7) 0.001(4) -0.029(4) 0.013(3) C9 0.036(3) 0.027(2) 0.024(2) 0.0002(18) 0.0052(19) 0.000(2) C10 0.038(3) 0.047(3) 0.022(2) 0.003(2) 0.0057(19) -0.001(2) C11 0.086(5) 0.075(4) 0.031(3) 0.018(3) 0.011(3) 0.025(4) C12 0.078(4) 0.053(3) 0.032(3) -0.014(2) 0.008(3) -0.001(3) C13 0.033(3) 0.034(2) 0.025(2) -0.0036(18) -0.0002(19) -0.008(2) C14 0.048(3) 0.062(3) 0.029(3) -0.004(2) -0.009(2) -0.020(3) C15 0.043(4) 0.076(5) 0.099(5) 0.001(4) -0.020(4) -0.012(3) C16 0.054(4) 0.053(4) 0.076(4) -0.008(3) -0.008(3) -0.025(3) C17 0.035(2) 0.023(2) 0.025(2) -0.0036(17) 0.0063(18) 0.0003(18) C18 0.067(4) 0.032(2) 0.028(3) -0.004(2) 0.015(2) 0.009(2) C19 0.069(4) 0.046(3) 0.056(3) 0.015(3) 0.036(3) 0.020(3) C20 0.099(5) 0.065(4) 0.036(3) -0.020(3) -0.006(3) 0.009(4) C21 0.024(2) 0.028(2) 0.026(2) -0.0019(18) 0.0013(17) 0.0014(18) C22 0.030(3) 0.046(3) 0.045(3) 0.008(2) -0.006(2) -0.009(2) C23 0.030(3) 0.048(3) 0.089(4) 0.004(3) 0.009(3) -0.001(2) C24 0.038(3) 0.044(3) 0.055(3) -0.006(2) -0.004(2) -0.013(2) _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 O11 2.023(2) 3_656 ? Zr1 O1 2.140(3) . ? Zr1 O5 2.156(3) . ? Zr1 O2 2.221(3) . ? Zr1 O4 2.228(3) . ? Zr1 O13 2.232(3) . ? Zr1 O3 2.283(3) . ? Zr1 O7 2.303(3) . ? Zr2 O11 2.075(2) . ? Zr2 O11 2.099(3) 3_656 ? Zr2 O10 2.176(3) . ? Zr2 O12 2.179(3) . ? Zr2 O9 2.194(3) . ? Zr2 O6 2.204(3) . ? Zr2 O8 2.280(3) . ? Zr2 O7 2.405(3) . ? Zr2 Zr2 3.3615(7) 3_656 ? O1 C1 1.272(5) . ? O2 C5 1.258(5) . ? O3 C9 1.249(5) . ? O4 C9 1.265(5) . ? O5 C13 1.267(5) . ? O6 C13 1.258(5) . ? O7 C17 1.283(5) . ? O8 C17 1.253(5) . ? O9 C1 1.263(5) 3_656 ? O10 C5 1.265(5) 3_656 ? O11 Zr1 2.023(2) 3_656 ? O11 Zr2 2.099(3) 3_656 ? O12 C21 1.265(5) . ? O13 C21 1.261(5) . ? C1 O9 1.263(5) 3_656 ? C1 C2 1.511(6) . ? C2 C4 1.478(8) . ? C2 C3 1.496(7) . ? C2 H2 1.0000 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 O10 1.265(5) 3_656 ? C5 C6 1.517(6) . ? C6 C8 1.475(8) . ? C6 C7 1.506(7) . ? C6 H6 1.0000 . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.510(6) . ? C10 C11 1.520(7) . ? C10 C12 1.522(7) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.519(6) . ? C14 C16 1.494(8) . ? C14 C15 1.518(9) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.500(6) . ? C18 C20 1.524(8) . ? C18 C19 1.524(7) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.527(6) . ? C22 C24 1.499(7) . ? C22 C23 1.505(7) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O11 Zr1 O1 92.70(10) 3_656 . ? O11 Zr1 O5 87.74(10) 3_656 . ? O1 Zr1 O5 146.75(12) . . ? O11 Zr1 O2 81.00(10) 3_656 . ? O1 Zr1 O2 74.79(11) . . ? O5 Zr1 O2 72.44(11) . . ? O11 Zr1 O4 149.15(11) 3_656 . ? O1 Zr1 O4 99.08(12) . . ? O5 Zr1 O4 97.32(12) . . ? O2 Zr1 O4 129.57(11) . . ? O11 Zr1 O13 79.94(10) 3_656 . ? O1 Zr1 O13 72.40(11) . . ? O5 Zr1 O13 139.92(11) . . ? O2 Zr1 O13 140.92(10) . . ? O4 Zr1 O13 76.70(11) . . ? O11 Zr1 O3 153.78(11) 3_656 . ? O1 Zr1 O3 81.85(11) . . ? O5 Zr1 O3 83.25(12) . . ? O2 Zr1 O3 72.81(11) . . ? O4 Zr1 O3 56.84(11) . . ? O13 Zr1 O3 121.86(11) . . ? O11 Zr1 O7 75.92(10) 3_656 . ? O1 Zr1 O7 141.76(11) . . ? O5 Zr1 O7 70.32(11) . . ? O2 Zr1 O7 136.51(10) . . ? O4 Zr1 O7 77.24(11) . . ? O13 Zr1 O7 69.72(10) . . ? O3 Zr1 O7 123.13(11) . . ? O11 Zr2 O11 72.70(11) . 3_656 ? O11 Zr2 O10 82.34(10) . . ? O11 Zr2 O10 143.75(11) 3_656 . ? O11 Zr2 O12 86.51(10) . . ? O11 Zr2 O12 79.12(10) 3_656 . ? O10 Zr2 O12 73.40(11) . . ? O11 Zr2 O9 83.43(10) . . ? O11 Zr2 O9 126.55(11) 3_656 . ? O10 Zr2 O9 74.34(11) . . ? O12 Zr2 O9 147.19(11) . . ? O11 Zr2 O6 116.56(11) . . ? O11 Zr2 O6 78.72(11) 3_656 . ? O10 Zr2 O6 136.97(11) . . ? O12 Zr2 O6 140.94(11) . . ? O9 Zr2 O6 70.41(11) . . ? O11 Zr2 O8 157.40(11) . . ? O11 Zr2 O8 127.34(10) 3_656 . ? O10 Zr2 O8 75.07(11) . . ? O12 Zr2 O8 87.58(11) . . ? O9 Zr2 O8 89.88(11) . . ? O6 Zr2 O8 80.90(12) . . ? O11 Zr2 O7 141.45(9) . . ? O11 Zr2 O7 72.37(9) 3_656 . ? O10 Zr2 O7 118.72(10) . . ? O12 Zr2 O7 71.37(10) . . ? O9 Zr2 O7 131.40(10) . . ? O6 Zr2 O7 71.44(10) . . ? O8 Zr2 O7 55.15(9) . . ? O11 Zr2 Zr2 36.59(7) . 3_656 ? O11 Zr2 Zr2 36.11(7) 3_656 3_656 ? O10 Zr2 Zr2 114.91(7) . 3_656 ? O12 Zr2 Zr2 81.06(7) . 3_656 ? O9 Zr2 Zr2 107.53(8) . 3_656 ? O6 Zr2 Zr2 98.85(8) . 3_656 ? O8 Zr2 Zr2 161.54(7) . 3_656 ? O7 Zr2 Zr2 107.08(6) . 3_656 ? C1 O1 Zr1 132.9(3) . . ? C5 O2 Zr1 133.0(3) . . ? C9 O3 Zr1 91.8(3) . . ? C9 O4 Zr1 94.0(3) . . ? C13 O5 Zr1 130.2(3) . . ? C13 O6 Zr2 136.5(3) . . ? C17 O7 Zr1 170.4(3) . . ? C17 O7 Zr2 90.2(2) . . ? Zr1 O7 Zr2 95.74(10) . . ? C17 O8 Zr2 96.8(2) . . ? C1 O9 Zr2 136.8(3) 3_656 . ? C5 O10 Zr2 137.0(3) 3_656 . ? Zr1 O11 Zr2 134.95(13) 3_656 . ? Zr1 O11 Zr2 115.83(12) 3_656 3_656 ? Zr2 O11 Zr2 107.30(11) . 3_656 ? C21 O12 Zr2 134.2(3) . . ? C21 O13 Zr1 132.4(3) . . ? O9 C1 O1 123.7(4) 3_656 . ? O9 C1 C2 119.4(4) 3_656 . ? O1 C1 C2 117.0(4) . . ? C4 C2 C3 114.8(5) . . ? C4 C2 C1 108.1(5) . . ? C3 C2 C1 113.9(4) . . ? C4 C2 H2 106.5 . . ? C3 C2 H2 106.5 . . ? C1 C2 H2 106.5 . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O2 C5 O10 124.8(4) . 3_656 ? O2 C5 C6 118.3(4) . . ? O10 C5 C6 116.8(4) 3_656 . ? C8 C6 C7 111.8(6) . . ? C8 C6 C5 111.3(5) . . ? C7 C6 C5 110.9(4) . . ? C8 C6 H6 107.6 . . ? C7 C6 H6 107.6 . . ? C5 C6 H6 107.6 . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C6 C8 H8A 109.5 . . ? C6 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C6 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O4 117.4(4) . . ? O3 C9 C10 122.6(4) . . ? O4 C9 C10 120.1(4) . . ? C9 C10 C11 112.5(4) . . ? C9 C10 C12 109.8(4) . . ? C11 C10 C12 112.3(5) . . ? C9 C10 H10 107.3 . . ? C11 C10 H10 107.3 . . ? C12 C10 H10 107.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O6 C13 O5 125.4(4) . . ? O6 C13 C14 118.2(4) . . ? O5 C13 C14 116.4(4) . . ? C16 C14 C15 113.7(5) . . ? C16 C14 C13 113.7(4) . . ? C15 C14 C13 108.9(4) . . ? C16 C14 H14 106.7 . . ? C15 C14 H14 106.7 . . ? C13 C14 H14 106.7 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O8 C17 O7 117.8(3) . . ? O8 C17 C18 122.2(4) . . ? O7 C17 C18 119.9(4) . . ? C17 C18 C20 108.7(4) . . ? C17 C18 C19 110.7(4) . . ? C20 C18 C19 112.8(5) . . ? C17 C18 H18 108.2 . . ? C20 C18 H18 108.2 . . ? C19 C18 H18 108.2 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O13 C21 O12 125.7(4) . . ? O13 C21 C22 117.6(4) . . ? O12 C21 C22 116.7(4) . . ? C24 C22 C23 113.6(4) . . ? C24 C22 C21 111.7(4) . . ? C23 C22 C21 109.1(4) . . ? C24 C22 H22 107.4 . . ? C23 C22 H22 107.4 . . ? C21 C22 H22 107.4 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.23 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.683 _refine_diff_density_min -0.648 _refine_diff_density_rms 0.115 #===END data_12ja051_0m _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H54 O12 Zr' _chemical_formula_weight 697.95 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 11.3570(8) _cell_length_b 19.3700(13) _cell_length_c 35.211(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7745.8(9) _cell_formula_units_Z 8 _cell_measurement_temperature 193(2) _cell_measurement_reflns_used 5719 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 20.36 _exptl_crystal_description Prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.197 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2960 _exptl_absorpt_coefficient_mu 0.334 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9125 _exptl_absorpt_correction_T_max 0.9264 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 193(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 53618 _diffrn_reflns_av_R_equivalents 0.0703 _diffrn_reflns_av_sigmaI/netI 0.0433 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.29 _reflns_number_total 7023 _reflns_number_gt 4756 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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 7023 _refine_ls_number_parameters 406 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0600 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1655 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _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 Zr1 Zr 0.86770(4) 0.34467(2) 0.124001(11) 0.04305(18) Uani 1 1 d . . . O1 O 0.8717(3) 0.44528(16) 0.09258(9) 0.0549(8) Uani 1 1 d . . . O2 O 0.7073(3) 0.38866(16) 0.09560(9) 0.0578(8) Uani 1 1 d . . . O3 O 0.8050(3) 0.41256(16) 0.16664(9) 0.0590(8) Uani 1 1 d . . . O4 O 0.9249(3) 0.47456(18) 0.20240(9) 0.0670(9) Uani 1 1 d . . . O5 O 0.7304(3) 0.27304(17) 0.13523(9) 0.0611(9) Uani 1 1 d . . . O6 O 0.6616(3) 0.2047(2) 0.09090(10) 0.0843(13) Uani 1 1 d . . . O7 O 0.9281(3) 0.29986(16) 0.17925(9) 0.0609(9) Uani 1 1 d . . . O8 O 0.9704(3) 0.24605(15) 0.12702(8) 0.0591(9) Uani 1 1 d . . . O9 O 1.0450(3) 0.38162(16) 0.12703(9) 0.0576(8) Uani 1 1 d . . . O10 O 1.0867(3) 0.47771(18) 0.15834(10) 0.0688(10) Uani 1 1 d . . . O11 O 0.8927(3) 0.31100(17) 0.06667(9) 0.0613(9) Uani 1 1 d . . . O12 O 0.8171(3) 0.21512(19) 0.04472(10) 0.0797(12) Uani 1 1 d . . . C1 C 0.7647(4) 0.4404(2) 0.08388(13) 0.0517(11) Uani 1 1 d . . . C2 C 0.7042(5) 0.4969(3) 0.06105(16) 0.0689(14) Uani 1 1 d . . . C3 C 0.7931(6) 0.5386(3) 0.03938(19) 0.103(2) Uani 1 1 d . . . H3A H 0.8521 0.5570 0.0570 0.155 Uiso 1 1 calc R . . H3B H 0.7534 0.5769 0.0265 0.155 Uiso 1 1 calc R . . H3C H 0.8319 0.5091 0.0205 0.155 Uiso 1 1 calc R . . C4 C 0.6481(7) 0.5447(4) 0.0902(3) 0.151(4) Uani 1 1 d . . . H4A H 0.6023 0.5173 0.1083 0.226 Uiso 1 1 calc R . . H4B H 0.5960 0.5774 0.0772 0.226 Uiso 1 1 calc R . . H4C H 0.7098 0.5700 0.1037 0.226 Uiso 1 1 calc R . . C5 C 0.6134(10) 0.4641(5) 0.0358(3) 0.231(8) Uani 1 1 d . . . H5A H 0.6528 0.4353 0.0167 0.347 Uiso 1 1 calc R . . H5B H 0.5677 0.5002 0.0230 0.347 Uiso 1 1 calc R . . H5C H 0.5607 0.4354 0.0511 0.347 Uiso 1 1 calc R . . C6 C 0.8278(4) 0.4462(2) 0.19652(12) 0.0457(10) Uani 1 1 d . . . C7 C 0.7322(4) 0.4526(2) 0.22643(13) 0.0526(11) Uani 1 1 d . . . C8 C 0.6113(5) 0.4561(4) 0.20779(17) 0.088(2) Uani 1 1 d . . . H8A H 0.6074 0.4966 0.1912 0.133 Uiso 1 1 calc R . . H8B H 0.5505 0.4596 0.2275 0.133 Uiso 1 1 calc R . . H8C H 0.5982 0.4142 0.1927 0.133 Uiso 1 1 calc R . . C9 C 0.7412(6) 0.3867(3) 0.25087(16) 0.092(2) Uani 1 1 d . . . H9A H 0.7252 0.3462 0.2350 0.138 Uiso 1 1 calc R . . H9B H 0.6834 0.3889 0.2715 0.138 Uiso 1 1 calc R . . H9C H 0.8205 0.3832 0.2616 0.138 Uiso 1 1 calc R . . C10 C 0.7518(5) 0.5154(2) 0.25146(15) 0.0712(15) Uani 1 1 d . . . H10A H 0.8257 0.5100 0.2656 0.107 Uiso 1 1 calc R . . H10B H 0.6863 0.5199 0.2694 0.107 Uiso 1 1 calc R . . H10C H 0.7563 0.5569 0.2356 0.107 Uiso 1 1 calc R . . C11 C 0.6569(4) 0.2302(2) 0.12333(13) 0.0495(11) Uani 1 1 d . . . C12 C 0.5599(4) 0.2065(3) 0.14955(14) 0.0610(13) Uani 1 1 d . . . C13 C 0.5143(6) 0.2651(4) 0.1729(2) 0.121(3) Uani 1 1 d . . . H13A H 0.5788 0.2849 0.1879 0.182 Uiso 1 1 calc R . . H13B H 0.4526 0.2483 0.1900 0.182 Uiso 1 1 calc R . . H13C H 0.4816 0.3007 0.1561 0.182 Uiso 1 1 calc R . . C14 C 0.4638(7) 0.1707(6) 0.1273(2) 0.165(5) Uani 1 1 d . . . H14A H 0.4067 0.1504 0.1449 0.248 Uiso 1 1 calc R . . H14B H 0.4985 0.1342 0.1116 0.248 Uiso 1 1 calc R . . H14C H 0.4240 0.2043 0.1109 0.248 Uiso 1 1 calc R . . C15 C 0.6151(8) 0.1530(4) 0.1758(3) 0.146(4) Uani 1 1 d . . . H15A H 0.6703 0.1758 0.1931 0.219 Uiso 1 1 calc R . . H15B H 0.6573 0.1185 0.1606 0.219 Uiso 1 1 calc R . . H15C H 0.5532 0.1301 0.1905 0.219 Uiso 1 1 calc R . . C16 C 0.9778(4) 0.2494(2) 0.16289(13) 0.0516(11) Uani 1 1 d . . . C17 C 1.0434(5) 0.1947(2) 0.18570(15) 0.0661(14) Uani 1 1 d . . . C18 C 0.9669(9) 0.1719(5) 0.2178(3) 0.184(5) Uani 1 1 d . . . H18A H 0.8933 0.1529 0.2077 0.276 Uiso 1 1 calc R . . H18B H 0.9493 0.2115 0.2342 0.276 Uiso 1 1 calc R . . H18C H 1.0079 0.1364 0.2326 0.276 Uiso 1 1 calc R . . C19 C 1.0699(15) 0.1352(4) 0.1611(3) 0.254(8) Uani 1 1 d . . . H19A H 1.1367 0.1464 0.1446 0.381 Uiso 1 1 calc R . . H19B H 1.0009 0.1244 0.1455 0.381 Uiso 1 1 calc R . . H19C H 1.0898 0.0952 0.1768 0.381 Uiso 1 1 calc R . . C20 C 1.1492(7) 0.2265(4) 0.2029(4) 0.187(6) Uani 1 1 d . . . H20A H 1.1894 0.1924 0.2189 0.280 Uiso 1 1 calc R . . H20B H 1.1258 0.2661 0.2185 0.280 Uiso 1 1 calc R . . H20C H 1.2027 0.2419 0.1828 0.280 Uiso 1 1 calc R . . C21 C 1.1101(4) 0.4327(2) 0.13382(13) 0.0507(11) Uani 1 1 d . . . C22 C 1.2226(4) 0.4413(3) 0.11130(15) 0.0660(14) Uani 1 1 d . . . C23 C 1.3212(7) 0.4581(7) 0.1382(3) 0.215(7) Uani 1 1 d . . . H23A H 1.3940 0.4364 0.1292 0.323 Uiso 1 1 calc R . . H23B H 1.3019 0.4406 0.1635 0.323 Uiso 1 1 calc R . . H23C H 1.3319 0.5082 0.1393 0.323 Uiso 1 1 calc R . . C24 C 1.2554(8) 0.3765(5) 0.0925(4) 0.220(7) Uani 1 1 d . . . H24A H 1.3199 0.3851 0.0746 0.330 Uiso 1 1 calc R . . H24B H 1.1873 0.3582 0.0786 0.330 Uiso 1 1 calc R . . H24C H 1.2808 0.3428 0.1116 0.330 Uiso 1 1 calc R . . C25 C 1.2087(11) 0.4960(8) 0.0846(4) 0.299(10) Uani 1 1 d . . . H25A H 1.1270 0.4970 0.0757 0.449 Uiso 1 1 calc R . . H25B H 1.2616 0.4885 0.0630 0.449 Uiso 1 1 calc R . . H25C H 1.2278 0.5400 0.0968 0.449 Uiso 1 1 calc R . . C26 C 0.8906(4) 0.2630(2) 0.04326(12) 0.0503(11) Uani 1 1 d . . . C27 C 0.9801(5) 0.2616(3) 0.01144(14) 0.0655(14) Uani 1 1 d . . . C28 C 1.0931(5) 0.2319(5) 0.0296(2) 0.130(3) Uani 1 1 d . . . H28A H 1.1194 0.2625 0.0501 0.195 Uiso 1 1 calc R . . H28B H 1.1549 0.2285 0.0103 0.195 Uiso 1 1 calc R . . H28C H 1.0767 0.1859 0.0399 0.195 Uiso 1 1 calc R . . C29 C 0.9994(8) 0.3333(3) -0.0032(2) 0.135(4) Uani 1 1 d . . . H29A H 0.9258 0.3511 -0.0139 0.202 Uiso 1 1 calc R . . H29B H 1.0602 0.3325 -0.0230 0.202 Uiso 1 1 calc R . . H29C H 1.0250 0.3632 0.0176 0.202 Uiso 1 1 calc R . . C30 C 0.9430(5) 0.2137(3) -0.02014(15) 0.0854(18) Uani 1 1 d . . . H30A H 0.9240 0.1682 -0.0096 0.128 Uiso 1 1 calc R . . H30B H 1.0074 0.2091 -0.0385 0.128 Uiso 1 1 calc R . . H30C H 0.8734 0.2326 -0.0329 0.128 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 0.0478(3) 0.0406(3) 0.0407(3) -0.00592(17) 0.00395(18) -0.00818(18) O1 0.053(2) 0.0535(19) 0.059(2) 0.0018(15) -0.0024(15) -0.0118(15) O2 0.053(2) 0.062(2) 0.059(2) 0.0070(16) -0.0031(15) -0.0104(16) O3 0.057(2) 0.065(2) 0.055(2) -0.0147(17) 0.0051(16) 0.0031(16) O4 0.061(2) 0.083(2) 0.057(2) -0.0240(18) 0.0066(17) -0.0112(19) O5 0.068(2) 0.063(2) 0.0525(19) -0.0016(16) 0.0030(16) -0.0237(18) O6 0.082(3) 0.112(3) 0.059(2) -0.025(2) 0.0141(19) -0.052(2) O7 0.077(2) 0.058(2) 0.0476(19) -0.0078(15) -0.0001(17) 0.0021(18) O8 0.076(2) 0.0470(18) 0.054(2) -0.0090(15) 0.0040(16) -0.0006(16) O9 0.0469(18) 0.0503(19) 0.076(2) -0.0102(16) 0.0057(16) -0.0074(15) O10 0.060(2) 0.075(2) 0.072(2) -0.0311(19) 0.0137(18) -0.0192(18) O11 0.084(2) 0.056(2) 0.0441(18) -0.0088(15) 0.0124(16) -0.0165(17) O12 0.089(3) 0.085(3) 0.065(2) -0.028(2) 0.021(2) -0.047(2) C1 0.055(3) 0.049(3) 0.051(3) 0.000(2) -0.002(2) -0.014(2) C2 0.072(4) 0.058(3) 0.076(4) 0.013(3) -0.012(3) -0.002(3) C3 0.112(6) 0.098(5) 0.099(5) 0.047(4) 0.017(4) 0.008(4) C4 0.136(7) 0.095(6) 0.221(11) 0.053(6) 0.073(7) 0.056(5) C5 0.277(13) 0.139(8) 0.278(13) 0.102(8) -0.236(12) -0.087(8) C6 0.058(3) 0.038(2) 0.041(3) 0.0011(19) 0.002(2) 0.007(2) C7 0.060(3) 0.048(3) 0.049(3) -0.003(2) 0.010(2) 0.001(2) C8 0.062(4) 0.121(5) 0.083(4) -0.024(4) 0.017(3) 0.006(3) C9 0.137(6) 0.064(3) 0.074(4) 0.016(3) 0.040(4) 0.007(4) C10 0.087(4) 0.069(3) 0.058(3) -0.010(3) 0.021(3) -0.004(3) C11 0.049(3) 0.049(3) 0.051(3) 0.010(2) -0.005(2) -0.007(2) C12 0.056(3) 0.069(3) 0.058(3) 0.003(2) 0.012(2) -0.017(3) C13 0.084(5) 0.114(6) 0.165(8) -0.018(5) 0.055(5) -0.010(4) C14 0.115(7) 0.272(12) 0.108(7) -0.052(7) 0.047(5) -0.131(8) C15 0.159(8) 0.144(7) 0.135(7) 0.088(6) 0.069(6) 0.025(6) C16 0.064(3) 0.040(2) 0.051(3) -0.007(2) -0.001(2) -0.005(2) C17 0.083(4) 0.048(3) 0.068(3) -0.005(2) -0.016(3) -0.003(3) C18 0.164(9) 0.222(11) 0.166(9) 0.135(9) 0.029(7) 0.061(8) C19 0.53(2) 0.099(6) 0.130(8) -0.056(6) -0.131(11) 0.177(10) C20 0.121(7) 0.106(6) 0.334(16) 0.066(8) -0.122(9) -0.020(5) C21 0.047(3) 0.053(3) 0.051(3) -0.001(2) 0.000(2) -0.004(2) C22 0.058(3) 0.078(4) 0.062(3) -0.019(3) 0.021(3) -0.019(3) C23 0.088(6) 0.393(19) 0.164(9) -0.143(11) 0.050(6) -0.122(9) C24 0.115(7) 0.171(9) 0.373(17) -0.163(11) 0.140(9) -0.053(6) C25 0.213(13) 0.375(18) 0.309(16) 0.260(15) 0.200(13) 0.156(13) C26 0.063(3) 0.051(3) 0.037(2) -0.008(2) 0.001(2) -0.012(2) C27 0.067(3) 0.075(3) 0.054(3) -0.022(3) 0.014(2) -0.026(3) C28 0.061(4) 0.229(10) 0.100(5) -0.055(6) 0.007(4) 0.002(5) C29 0.218(9) 0.084(4) 0.103(5) -0.026(4) 0.102(6) -0.056(5) C30 0.091(4) 0.102(4) 0.063(3) -0.036(3) 0.018(3) -0.021(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 Zr1 O3 2.119(3) . ? Zr1 O5 2.124(3) . ? Zr1 O9 2.140(3) . ? Zr1 O11 2.140(3) . ? Zr1 O7 2.238(3) . ? Zr1 O8 2.241(3) . ? Zr1 O1 2.241(3) . ? Zr1 O2 2.246(3) . ? Zr1 C1 2.608(5) . ? Zr1 C16 2.616(5) . ? O1 C1 1.257(5) . ? O2 C1 1.265(5) . ? O3 C6 1.265(5) . ? O4 C6 1.249(5) . ? O5 C11 1.249(5) . ? O6 C11 1.246(5) . ? O7 C16 1.267(5) . ? O8 C16 1.267(5) . ? O9 C21 1.257(5) . ? O10 C21 1.256(5) . ? O11 C26 1.243(5) . ? O12 C26 1.248(5) . ? C1 C2 1.522(7) . ? C2 C5 1.502(9) . ? C2 C3 1.502(7) . ? C2 C4 1.521(9) . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 C7 1.517(6) . ? C7 C10 1.519(6) . ? C7 C8 1.524(7) . ? C7 C9 1.542(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.509(6) . ? C12 C13 1.495(8) . ? C12 C14 1.512(8) . ? C12 C15 1.523(8) . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.523(7) . ? C17 C19 1.474(8) . ? C17 C20 1.480(9) . ? C17 C18 1.493(10) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.513(6) . ? C22 C25 1.424(11) . ? C22 C24 1.468(9) . ? C22 C23 1.501(10) . ? 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 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.513(6) . ? C27 C29 1.499(7) . ? C27 C30 1.508(6) . ? C27 C28 1.544(9) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 Zr1 O5 91.55(13) . . ? O3 Zr1 O9 94.20(12) . . ? O5 Zr1 O9 154.16(13) . . ? O3 Zr1 O11 154.42(13) . . ? O5 Zr1 O11 94.23(12) . . ? O9 Zr1 O11 91.38(12) . . ? O3 Zr1 O7 74.21(12) . . ? O5 Zr1 O7 79.05(12) . . ? O9 Zr1 O7 78.34(12) . . ? O11 Zr1 O7 131.37(13) . . ? O3 Zr1 O8 132.09(12) . . ? O5 Zr1 O8 79.42(13) . . ? O9 Zr1 O8 78.05(12) . . ? O11 Zr1 O8 73.49(12) . . ? O7 Zr1 O8 57.89(11) . . ? O3 Zr1 O1 79.45(12) . . ? O5 Zr1 O1 132.43(12) . . ? O9 Zr1 O1 73.41(11) . . ? O11 Zr1 O1 78.27(12) . . ? O7 Zr1 O1 139.46(11) . . ? O8 Zr1 O1 138.94(12) . . ? O3 Zr1 O2 78.91(12) . . ? O5 Zr1 O2 74.64(12) . . ? O9 Zr1 O2 131.19(12) . . ? O11 Zr1 O2 78.66(13) . . ? O7 Zr1 O2 141.52(12) . . ? O8 Zr1 O2 140.05(12) . . ? O1 Zr1 O2 57.79(11) . . ? O3 Zr1 C1 77.99(14) . . ? O5 Zr1 C1 103.64(14) . . ? O9 Zr1 C1 102.20(13) . . ? O11 Zr1 C1 76.43(14) . . ? O7 Zr1 C1 152.14(13) . . ? O8 Zr1 C1 149.91(13) . . ? O1 Zr1 C1 28.80(11) . . ? O2 Zr1 C1 29.00(12) . . ? O3 Zr1 C16 103.16(13) . . ? O5 Zr1 C16 78.02(13) . . ? O9 Zr1 C16 76.14(13) . . ? O11 Zr1 C16 102.42(14) . . ? O7 Zr1 C16 28.95(12) . . ? O8 Zr1 C16 28.95(11) . . ? O1 Zr1 C16 149.55(13) . . ? O2 Zr1 C16 152.64(13) . . ? C1 Zr1 C16 178.00(15) . . ? C1 O1 Zr1 92.0(3) . . ? C1 O2 Zr1 91.6(3) . . ? C6 O3 Zr1 147.3(3) . . ? C11 O5 Zr1 149.5(3) . . ? C16 O7 Zr1 92.3(3) . . ? C16 O8 Zr1 92.2(3) . . ? C21 O9 Zr1 145.7(3) . . ? C26 O11 Zr1 148.3(3) . . ? O1 C1 O2 118.6(4) . . ? O1 C1 C2 120.8(4) . . ? O2 C1 C2 120.6(4) . . ? O1 C1 Zr1 59.2(2) . . ? O2 C1 Zr1 59.4(2) . . ? C2 C1 Zr1 179.1(4) . . ? C5 C2 C3 112.8(7) . . ? C5 C2 C4 111.7(8) . . ? C3 C2 C4 107.3(5) . . ? C5 C2 C1 108.6(5) . . ? C3 C2 C1 110.6(5) . . ? C4 C2 C1 105.7(5) . . ? C2 C3 H3A 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C2 C4 H4A 109.5 . . ? C2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C2 C5 H5A 109.5 . . ? C2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 O3 123.0(4) . . ? O4 C6 C7 118.7(4) . . ? O3 C6 C7 118.2(4) . . ? C6 C7 C10 111.3(4) . . ? C6 C7 C8 110.4(4) . . ? C10 C7 C8 110.3(4) . . ? C6 C7 C9 105.9(4) . . ? C10 C7 C9 109.2(4) . . ? C8 C7 C9 109.6(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O6 C11 O5 122.9(4) . . ? O6 C11 C12 118.1(4) . . ? O5 C11 C12 119.0(4) . . ? C13 C12 C11 111.0(4) . . ? C13 C12 C14 112.5(6) . . ? C11 C12 C14 110.4(4) . . ? C13 C12 C15 109.1(6) . . ? C11 C12 C15 106.2(5) . . ? C14 C12 C15 107.4(6) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 117.6(4) . . ? O8 C16 C17 121.5(4) . . ? O7 C16 C17 120.9(4) . . ? O8 C16 Zr1 58.9(2) . . ? O7 C16 Zr1 58.7(2) . . ? C17 C16 Zr1 179.0(3) . . ? C19 C17 C20 113.6(9) . . ? C19 C17 C18 109.4(8) . . ? C20 C17 C18 106.6(7) . . ? C19 C17 C16 109.5(5) . . ? C20 C17 C16 109.0(5) . . ? C18 C17 C16 108.7(5) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O10 C21 O9 123.5(4) . . ? O10 C21 C22 117.5(4) . . ? O9 C21 C22 119.0(4) . . ? C25 C22 C24 111.5(9) . . ? C25 C22 C23 109.8(9) . . ? C24 C22 C23 106.3(8) . . ? C25 C22 C21 109.5(6) . . ? C24 C22 C21 110.8(5) . . ? C23 C22 C21 108.9(5) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? O11 C26 O12 122.8(4) . . ? O11 C26 C27 119.5(4) . . ? O12 C26 C27 117.8(4) . . ? C29 C27 C30 110.9(5) . . ? C29 C27 C26 109.7(4) . . ? C30 C27 C26 111.7(4) . . ? C29 C27 C28 111.4(6) . . ? C30 C27 C28 108.0(5) . . ? C26 C27 C28 105.0(4) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 O3 Zr1 O1 C1 -84.2(3) . . . . ? O5 Zr1 O1 C1 -1.9(3) . . . . ? O9 Zr1 O1 C1 178.1(3) . . . . ? O11 Zr1 O1 C1 83.1(3) . . . . ? O7 Zr1 O1 C1 -134.2(3) . . . . ? O8 Zr1 O1 C1 130.3(3) . . . . ? O2 Zr1 O1 C1 -0.8(3) . . . . ? C16 Zr1 O1 C1 177.7(3) . . . . ? O3 Zr1 O2 C1 85.2(3) . . . . ? O5 Zr1 O2 C1 179.9(3) . . . . ? O9 Zr1 O2 C1 -0.6(3) . . . . ? O11 Zr1 O2 C1 -82.4(3) . . . . ? O7 Zr1 O2 C1 131.4(3) . . . . ? O8 Zr1 O2 C1 -128.7(3) . . . . ? O1 Zr1 O2 C1 0.8(3) . . . . ? C16 Zr1 O2 C1 -177.6(3) . . . . ? O5 Zr1 O3 C6 124.9(5) . . . . ? O9 Zr1 O3 C6 -29.9(6) . . . . ? O11 Zr1 O3 C6 -132.0(5) . . . . ? O7 Zr1 O3 C6 46.7(5) . . . . ? O8 Zr1 O3 C6 47.8(6) . . . . ? O1 Zr1 O3 C6 -102.2(6) . . . . ? O2 Zr1 O3 C6 -161.1(6) . . . . ? C1 Zr1 O3 C6 -131.5(6) . . . . ? C16 Zr1 O3 C6 46.8(6) . . . . ? O3 Zr1 O5 C11 142.4(7) . . . . ? O9 Zr1 O5 C11 -114.6(7) . . . . ? O11 Zr1 O5 C11 -12.6(7) . . . . ? O7 Zr1 O5 C11 -144.0(7) . . . . ? O8 Zr1 O5 C11 -84.9(7) . . . . ? O1 Zr1 O5 C11 65.3(7) . . . . ? O2 Zr1 O5 C11 64.4(7) . . . . ? C1 Zr1 O5 C11 64.4(7) . . . . ? C16 Zr1 O5 C11 -114.4(7) . . . . ? O3 Zr1 O7 C16 179.8(3) . . . . ? O5 Zr1 O7 C16 85.0(3) . . . . ? O9 Zr1 O7 C16 -82.4(3) . . . . ? O11 Zr1 O7 C16 -1.0(3) . . . . ? O8 Zr1 O7 C16 0.7(3) . . . . ? O1 Zr1 O7 C16 -128.8(3) . . . . ? O2 Zr1 O7 C16 132.4(3) . . . . ? C1 Zr1 O7 C16 -176.5(3) . . . . ? O3 Zr1 O8 C16 -1.9(3) . . . . ? O5 Zr1 O8 C16 -84.3(3) . . . . ? O9 Zr1 O8 C16 82.9(3) . . . . ? O11 Zr1 O8 C16 178.0(3) . . . . ? O7 Zr1 O8 C16 -0.7(3) . . . . ? O1 Zr1 O8 C16 129.5(3) . . . . ? O2 Zr1 O8 C16 -134.4(3) . . . . ? C1 Zr1 O8 C16 176.7(3) . . . . ? O3 Zr1 O9 C21 -30.3(6) . . . . ? O5 Zr1 O9 C21 -132.6(5) . . . . ? O11 Zr1 O9 C21 124.7(6) . . . . ? O7 Zr1 O9 C21 -103.2(6) . . . . ? O8 Zr1 O9 C21 -162.5(6) . . . . ? O1 Zr1 O9 C21 47.4(5) . . . . ? O2 Zr1 O9 C21 48.6(6) . . . . ? C1 Zr1 O9 C21 48.3(6) . . . . ? C16 Zr1 O9 C21 -132.8(6) . . . . ? O3 Zr1 O11 C26 -135.0(6) . . . . ? O5 Zr1 O11 C26 -32.4(6) . . . . ? O9 Zr1 O11 C26 122.3(6) . . . . ? O7 Zr1 O11 C26 46.7(7) . . . . ? O8 Zr1 O11 C26 45.2(6) . . . . ? O1 Zr1 O11 C26 -164.9(6) . . . . ? O2 Zr1 O11 C26 -105.8(6) . . . . ? C1 Zr1 O11 C26 -135.4(6) . . . . ? C16 Zr1 O11 C26 46.2(6) . . . . ? Zr1 O1 C1 O2 1.3(4) . . . . ? Zr1 O1 C1 C2 178.9(4) . . . . ? Zr1 O2 C1 O1 -1.3(4) . . . . ? Zr1 O2 C1 C2 -178.9(4) . . . . ? O3 Zr1 C1 O1 89.9(3) . . . . ? O5 Zr1 C1 O1 178.6(3) . . . . ? O9 Zr1 C1 O1 -1.8(3) . . . . ? O11 Zr1 C1 O1 -90.3(3) . . . . ? O7 Zr1 C1 O1 86.2(4) . . . . ? O8 Zr1 C1 O1 -89.0(3) . . . . ? O2 Zr1 C1 O1 178.7(4) . . . . ? C16 Zr1 C1 O1 -35(4) . . . . ? O3 Zr1 C1 O2 -88.7(3) . . . . ? O5 Zr1 C1 O2 -0.1(3) . . . . ? O9 Zr1 C1 O2 179.5(2) . . . . ? O11 Zr1 C1 O2 91.0(3) . . . . ? O7 Zr1 C1 O2 -92.4(4) . . . . ? O8 Zr1 C1 O2 92.3(4) . . . . ? O1 Zr1 C1 O2 -178.7(4) . . . . ? C16 Zr1 C1 O2 146(4) . . . . ? O3 Zr1 C1 C2 3(22) . . . . ? O5 Zr1 C1 C2 91(22) . . . . ? O9 Zr1 C1 C2 -89(22) . . . . ? O11 Zr1 C1 C2 -177(100) . . . . ? O7 Zr1 C1 C2 -1(22) . . . . ? O8 Zr1 C1 C2 -176(100) . . . . ? O1 Zr1 C1 C2 -87(22) . . . . ? O2 Zr1 C1 C2 92(22) . . . . ? C16 Zr1 C1 C2 -122(22) . . . . ? O1 C1 C2 C5 146.2(7) . . . . ? O2 C1 C2 C5 -36.3(9) . . . . ? Zr1 C1 C2 C5 -127(22) . . . . ? O1 C1 C2 C3 21.9(7) . . . . ? O2 C1 C2 C3 -160.6(5) . . . . ? Zr1 C1 C2 C3 108(22) . . . . ? O1 C1 C2 C4 -93.9(6) . . . . ? O2 C1 C2 C4 83.7(6) . . . . ? Zr1 C1 C2 C4 -7(22) . . . . ? Zr1 O3 C6 O4 36.5(8) . . . . ? Zr1 O3 C6 C7 -143.7(4) . . . . ? O4 C6 C7 C10 23.0(6) . . . . ? O3 C6 C7 C10 -156.8(4) . . . . ? O4 C6 C7 C8 145.9(5) . . . . ? O3 C6 C7 C8 -33.9(6) . . . . ? O4 C6 C7 C9 -95.5(5) . . . . ? O3 C6 C7 C9 84.7(5) . . . . ? Zr1 O5 C11 O6 15.7(10) . . . . ? Zr1 O5 C11 C12 -166.2(5) . . . . ? O6 C11 C12 C13 -142.4(6) . . . . ? O5 C11 C12 C13 39.4(7) . . . . ? O6 C11 C12 C14 -16.8(8) . . . . ? O5 C11 C12 C14 165.0(6) . . . . ? O6 C11 C12 C15 99.3(6) . . . . ? O5 C11 C12 C15 -78.9(7) . . . . ? Zr1 O8 C16 O7 1.2(4) . . . . ? Zr1 O8 C16 C17 -179.0(4) . . . . ? Zr1 O7 C16 O8 -1.2(4) . . . . ? Zr1 O7 C16 C17 179.0(4) . . . . ? O3 Zr1 C16 O8 178.5(3) . . . . ? O5 Zr1 C16 O8 89.8(3) . . . . ? O9 Zr1 C16 O8 -90.3(3) . . . . ? O11 Zr1 C16 O8 -2.0(3) . . . . ? O7 Zr1 C16 O8 178.8(4) . . . . ? O1 Zr1 C16 O8 -89.9(3) . . . . ? O2 Zr1 C16 O8 87.3(4) . . . . ? C1 Zr1 C16 O8 -57(4) . . . . ? O3 Zr1 C16 O7 -0.2(3) . . . . ? O5 Zr1 C16 O7 -89.0(3) . . . . ? O9 Zr1 C16 O7 90.9(3) . . . . ? O11 Zr1 C16 O7 179.3(3) . . . . ? O8 Zr1 C16 O7 -178.8(4) . . . . ? O1 Zr1 C16 O7 91.3(4) . . . . ? O2 Zr1 C16 O7 -91.5(4) . . . . ? C1 Zr1 C16 O7 125(4) . . . . ? O3 Zr1 C16 C17 -70(23) . . . . ? O5 Zr1 C16 C17 -158(100) . . . . ? O9 Zr1 C16 C17 22(23) . . . . ? O11 Zr1 C16 C17 110(23) . . . . ? O7 Zr1 C16 C17 -69(23) . . . . ? O8 Zr1 C16 C17 112(23) . . . . ? O1 Zr1 C16 C17 22(23) . . . . ? O2 Zr1 C16 C17 -161(100) . . . . ? C1 Zr1 C16 C17 55(25) . . . . ? O8 C16 C17 C19 -11.9(10) . . . . ? O7 C16 C17 C19 167.9(8) . . . . ? Zr1 C16 C17 C19 -123(23) . . . . ? O8 C16 C17 C20 112.9(7) . . . . ? O7 C16 C17 C20 -67.3(8) . . . . ? Zr1 C16 C17 C20 1(23) . . . . ? O8 C16 C17 C18 -131.4(7) . . . . ? O7 C16 C17 C18 48.4(8) . . . . ? Zr1 C16 C17 C18 117(23) . . . . ? Zr1 O9 C21 O10 34.2(9) . . . . ? Zr1 O9 C21 C22 -145.4(5) . . . . ? O10 C21 C22 C25 -73.3(10) . . . . ? O9 C21 C22 C25 106.3(10) . . . . ? O10 C21 C22 C24 163.3(7) . . . . ? O9 C21 C22 C24 -17.1(9) . . . . ? O10 C21 C22 C23 46.7(8) . . . . ? O9 C21 C22 C23 -133.7(7) . . . . ? Zr1 O11 C26 O12 35.0(9) . . . . ? Zr1 O11 C26 C27 -145.0(5) . . . . ? O11 C26 C27 C29 -39.4(7) . . . . ? O12 C26 C27 C29 140.6(6) . . . . ? O11 C26 C27 C30 -162.7(5) . . . . ? O12 C26 C27 C30 17.2(7) . . . . ? O11 C26 C27 C28 80.5(6) . . . . ? O12 C26 C27 C28 -99.6(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.490 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.072 #===END data_tripdty-sr _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C48 H88 O16 Zr2' _chemical_formula_weight 1103.62 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' '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8579(13) _cell_length_b 14.5616(17) _cell_length_c 22.069(3) _cell_angle_alpha 72.483(2) _cell_angle_beta 78.790(2) _cell_angle_gamma 68.6880(10) _cell_volume 3369.9(7) _cell_formula_units_Z 2 _cell_measurement_temperature 194(2) _cell_measurement_reflns_used 4259 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 21.44 _exptl_crystal_description irregular _exptl_crystal_colour colourless _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.088 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1168 _exptl_absorpt_coefficient_mu 0.360 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8735 _exptl_absorpt_correction_T_max 0.9056 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 194(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 12166 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0711 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.55 _diffrn_reflns_theta_max 25.27 _reflns_number_total 12166 _reflns_number_gt 8025 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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^)+(0.1000P)^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 12166 _refine_ls_number_parameters 619 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0846 _refine_ls_R_factor_gt 0.0514 _refine_ls_wR_factor_ref 0.1543 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 0.881 _refine_ls_restrained_S_all 0.881 _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 O13 O 0.7729(2) 0.4237(2) 0.62866(13) 0.0469(7) Uani 1 1 d . . . Zr2 Zr 0.67163(3) 0.58727(3) 0.632758(17) 0.03572(13) Uani 1 1 d . . . Zr1 Zr 0.55804(3) 0.67912(3) 0.806069(18) 0.03604(13) Uani 1 1 d . . . O6 O 0.5649(2) 0.49825(19) 0.69856(12) 0.0387(6) Uani 1 1 d . . . O12 O 0.7679(2) 0.53019(19) 0.71538(13) 0.0390(6) Uani 1 1 d . . . O11 O 0.7289(2) 0.55210(19) 0.81349(12) 0.0389(6) Uani 1 1 d . . . O3 O 0.5273(3) 0.6009(2) 0.90712(13) 0.0560(8) Uani 1 1 d . . . O1 O 0.6807(3) 0.7188(2) 0.85428(15) 0.0589(9) Uani 1 1 d . . . O9 O 0.6692(2) 0.73792(19) 0.72604(13) 0.0408(6) Uani 1 1 d . . . O10 O 0.7407(2) 0.70807(19) 0.63034(13) 0.0413(6) Uani 1 1 d . . . O7 O 0.4300(2) 0.7772(2) 0.73519(13) 0.0406(6) Uani 1 1 d . . . O8 O 0.5098(2) 0.6997(2) 0.65695(13) 0.0416(7) Uani 1 1 d . . . O5 O 0.5181(2) 0.5635(2) 0.78262(12) 0.0400(6) Uani 1 1 d . . . O15 O 0.6270(3) 0.7011(2) 0.53708(13) 0.0545(8) Uani 1 1 d . . . O16 O 0.5706(3) 0.5666(2) 0.56722(13) 0.0490(7) Uani 1 1 d . . . O14 O 0.8446(3) 0.5443(2) 0.57355(14) 0.0516(8) Uani 1 1 d . . . C31 C 0.7975(3) 0.5108(3) 0.77092(19) 0.0340(9) Uani 1 1 d . . . O4 O 0.3702(2) 0.6941(2) 0.85593(14) 0.0534(8) Uani 1 1 d . . . C7 C 0.4126(4) 0.6367(4) 0.9075(2) 0.0509(11) Uani 1 1 d . . . C8 C 0.3342(5) 0.6163(5) 0.9677(2) 0.092(2) Uani 1 1 d . . . H8A H 0.3143 0.6743 0.9870 0.111 Uiso 1 1 calc R . . H8B H 0.3840 0.5554 0.9972 0.111 Uiso 1 1 calc R . . C9 C 0.2168(4) 0.5996(5) 0.9669(2) 0.0707(16) Uani 1 1 d . . . C10 C 0.1570(5) 0.5713(6) 1.0329(3) 0.110(3) Uani 1 1 d . . . H10A H 0.1374 0.6268 1.0535 0.166 Uiso 1 1 calc R . . H10B H 0.2123 0.5092 1.0579 0.166 Uiso 1 1 calc R . . H10C H 0.0820 0.5592 1.0305 0.166 Uiso 1 1 calc R . . C11 C 0.1330(6) 0.6733(9) 0.9221(4) 0.231(7) Uani 1 1 d . . . H11A H 0.0626 0.6514 0.9253 0.346 Uiso 1 1 calc R . . H11B H 0.1737 0.6786 0.8786 0.346 Uiso 1 1 calc R . . H11C H 0.1058 0.7398 0.9318 0.346 Uiso 1 1 calc R . . C1 C 0.6006(4) 0.8039(4) 0.8550(3) 0.0645(14) Uani 1 1 d . . . O2 O 0.5027(3) 0.8262(2) 0.83126(15) 0.0566(8) Uani 1 1 d . . . C2 C 0.6158(6) 0.8789(5) 0.8854(4) 0.135(4) Uani 1 1 d . . . H2A H 0.6059 0.9433 0.8517 0.163 Uiso 1 1 calc R . . H2B H 0.5454 0.8928 0.9178 0.163 Uiso 1 1 calc R . . C3 C 0.7176(9) 0.8618(5) 0.9147(5) 0.139(4) Uani 1 1 d . . . C5 C 0.7719(6) 0.7649(5) 0.9584(3) 0.110(2) Uani 1 1 d . . . H5A H 0.7140 0.7540 0.9959 0.165 Uiso 1 1 calc R . . H5B H 0.8459 0.7650 0.9718 0.165 Uiso 1 1 calc R . . H5C H 0.7924 0.7100 0.9371 0.165 Uiso 1 1 calc R . . C4 C 0.8270(10) 0.8580(8) 0.8513(5) 0.181(4) Uani 1 1 d . . . H4A H 0.8315 0.8044 0.8317 0.271 Uiso 1 1 calc R . . H4B H 0.9059 0.8434 0.8662 0.271 Uiso 1 1 calc R . . H4C H 0.8063 0.9239 0.8197 0.271 Uiso 1 1 calc R . . C25 C 0.7276(3) 0.7566(3) 0.6717(2) 0.0395(9) Uani 1 1 d . . . C26 C 0.7806(3) 0.8410(3) 0.6543(2) 0.0449(10) Uani 1 1 d . . . H26A H 0.8516 0.8260 0.6224 0.054 Uiso 1 1 calc R . . H26B H 0.8106 0.8422 0.6928 0.054 Uiso 1 1 calc R . . C27 C 0.6915(4) 0.9479(3) 0.6270(2) 0.0527(12) Uani 1 1 d . . . C29 C 0.7633(5) 1.0218(4) 0.6074(3) 0.090(2) Uani 1 1 d . . . H29A H 0.8308 1.0004 0.5756 0.135 Uiso 1 1 calc R . . H29B H 0.7956 1.0221 0.6449 0.135 Uiso 1 1 calc R . . H29C H 0.7099 1.0904 0.5890 0.135 Uiso 1 1 calc R . . C28 C 0.5884(5) 0.9781(4) 0.6781(3) 0.0861(19) Uani 1 1 d . . . H28A H 0.6226 0.9750 0.7160 0.129 Uiso 1 1 calc R . . H28B H 0.5415 0.9311 0.6896 0.129 Uiso 1 1 calc R . . H28C H 0.5351 1.0477 0.6615 0.129 Uiso 1 1 calc R . . C30 C 0.6382(5) 0.9476(4) 0.5689(3) 0.0874(18) Uani 1 1 d . . . H30A H 0.5880 1.0170 0.5495 0.131 Uiso 1 1 calc R . . H30B H 0.5880 0.9030 0.5826 0.131 Uiso 1 1 calc R . . H30C H 0.7045 0.9227 0.5376 0.131 Uiso 1 1 calc R . . C19 C 0.4310(3) 0.7689(3) 0.67986(19) 0.0368(9) Uani 1 1 d . . . C20 C 0.3306(3) 0.8442(3) 0.6398(2) 0.0425(10) Uani 1 1 d . . . H20A H 0.3640 0.8567 0.5945 0.051 Uiso 1 1 calc R . . H20B H 0.3037 0.9096 0.6519 0.051 Uiso 1 1 calc R . . C22 C 0.2195(4) 0.8107(3) 0.6461(2) 0.0474(11) Uani 1 1 d . . . C24 C 0.2577(5) 0.7120(4) 0.6248(3) 0.0886(19) Uani 1 1 d . . . H24A H 0.3053 0.6555 0.6568 0.133 Uiso 1 1 calc R . . H24B H 0.3073 0.7190 0.5837 0.133 Uiso 1 1 calc R . . H24C H 0.1851 0.6983 0.6204 0.133 Uiso 1 1 calc R . . C21 C 0.1614(5) 0.7950(6) 0.7140(3) 0.100(2) Uani 1 1 d . . . H21A H 0.1405 0.8575 0.7280 0.150 Uiso 1 1 calc R . . H21B H 0.2186 0.7390 0.7419 0.150 Uiso 1 1 calc R . . H21C H 0.0875 0.7782 0.7163 0.150 Uiso 1 1 calc R . . C23 C 0.1271(5) 0.8928(4) 0.6027(3) 0.0888(19) Uani 1 1 d . . . H23A H 0.0576 0.8704 0.6047 0.133 Uiso 1 1 calc R . . H23B H 0.1649 0.9052 0.5587 0.133 Uiso 1 1 calc R . . H23C H 0.0991 0.9559 0.6169 0.133 Uiso 1 1 calc R . . C13 C 0.5203(3) 0.4982(3) 0.75474(18) 0.0338(9) Uani 1 1 d . . . C14 C 0.4674(4) 0.4145(3) 0.7918(2) 0.0440(10) Uani 1 1 d . . . H14A H 0.4326 0.3959 0.7617 0.053 Uiso 1 1 calc R . . H14B H 0.4001 0.4414 0.8228 0.053 Uiso 1 1 calc R . . C15 C 0.5601(4) 0.3171(3) 0.8284(2) 0.0581(12) Uani 1 1 d . . . C17 C 0.4936(6) 0.2381(4) 0.8560(3) 0.099(2) Uani 1 1 d . . . H17A H 0.5500 0.1736 0.8781 0.149 Uiso 1 1 calc R . . H17B H 0.4635 0.2272 0.8213 0.149 Uiso 1 1 calc R . . H17C H 0.4250 0.2631 0.8863 0.149 Uiso 1 1 calc R . . C16 C 0.6028(5) 0.3371(4) 0.8826(2) 0.0821(17) Uani 1 1 d . . . H16A H 0.6542 0.2727 0.9077 0.123 Uiso 1 1 calc R . . H16B H 0.5321 0.3673 0.9101 0.123 Uiso 1 1 calc R . . H16C H 0.6496 0.3841 0.8648 0.123 Uiso 1 1 calc R . . C18 C 0.6693(5) 0.2752(4) 0.7839(3) 0.0777(16) Uani 1 1 d . . . H18A H 0.7168 0.3219 0.7693 0.117 Uiso 1 1 calc R . . H18B H 0.6414 0.2683 0.7470 0.117 Uiso 1 1 calc R . . H18C H 0.7201 0.2084 0.8066 0.117 Uiso 1 1 calc R . . C32 C 0.9211(3) 0.4371(3) 0.7870(2) 0.0425(10) Uani 1 1 d . . . H32A H 0.9434 0.3832 0.7641 0.051 Uiso 1 1 calc R . . H32B H 0.9174 0.4043 0.8334 0.051 Uiso 1 1 calc R . . C33 C 1.0210(4) 0.4879(4) 0.7695(2) 0.0550(12) Uani 1 1 d . . . C34 C 0.9860(5) 0.5740(4) 0.8027(3) 0.0755(16) Uani 1 1 d . . . H34A H 0.9654 0.5483 0.8484 0.113 Uiso 1 1 calc R . . H34B H 0.9155 0.6295 0.7843 0.113 Uiso 1 1 calc R . . H34C H 1.0545 0.5993 0.7967 0.113 Uiso 1 1 calc R . . C35 C 1.1393(4) 0.4060(5) 0.7917(4) 0.106(2) Uani 1 1 d . . . H35A H 1.2048 0.4358 0.7809 0.159 Uiso 1 1 calc R . . H35B H 1.1598 0.3511 0.7704 0.159 Uiso 1 1 calc R . . H35C H 1.1292 0.3785 0.8380 0.159 Uiso 1 1 calc R . . C36 C 1.0378(5) 0.5296(4) 0.6971(3) 0.0806(17) Uani 1 1 d . . . H36A H 1.0949 0.5679 0.6867 0.121 Uiso 1 1 calc R . . H36B H 0.9592 0.5747 0.6816 0.121 Uiso 1 1 calc R . . H36C H 1.0700 0.4728 0.6767 0.121 Uiso 1 1 calc R . . C43 C 0.5718(4) 0.6503(4) 0.5255(2) 0.0468(10) Uani 1 1 d . . . C44 C 0.5081(4) 0.6834(3) 0.46631(19) 0.0504(11) Uani 1 1 d . . . H44A H 0.4642 0.7576 0.4578 0.060 Uiso 1 1 calc R . . H44B H 0.4470 0.6485 0.4739 0.060 Uiso 1 1 calc R . . C45 C 0.5936(4) 0.6609(3) 0.40735(19) 0.0428(10) Uani 1 1 d . . . C46 C 0.5146(5) 0.6957(4) 0.3522(2) 0.0734(15) Uani 1 1 d . . . H46A H 0.4566 0.6581 0.3628 0.110 Uiso 1 1 calc R . . H46B H 0.5664 0.6825 0.3133 0.110 Uiso 1 1 calc R . . H46C H 0.4700 0.7688 0.3453 0.110 Uiso 1 1 calc R . . C48 C 0.6834(5) 0.7190(4) 0.3906(2) 0.0693(14) Uani 1 1 d . . . H48A H 0.6392 0.7914 0.3874 0.104 Uiso 1 1 calc R . . H48B H 0.7298 0.7106 0.3496 0.104 Uiso 1 1 calc R . . H48C H 0.7392 0.6925 0.4239 0.104 Uiso 1 1 calc R . . C47 C 0.6613(5) 0.5479(4) 0.4187(2) 0.0719(15) Uani 1 1 d . . . H47A H 0.7161 0.5267 0.4519 0.108 Uiso 1 1 calc R . . H47B H 0.7087 0.5332 0.3791 0.108 Uiso 1 1 calc R . . H47C H 0.6029 0.5105 0.4324 0.108 Uiso 1 1 calc R . . C40 C 0.8530(6) 0.2863(5) 0.5321(4) 0.137(3) Uani 1 1 d . . . H40A H 0.8458 0.2192 0.5377 0.206 Uiso 1 1 calc R . . H40B H 0.8639 0.3185 0.4865 0.206 Uiso 1 1 calc R . . H40C H 0.7790 0.3291 0.5516 0.206 Uiso 1 1 calc R . . C39 C 0.9600(4) 0.2742(3) 0.5635(2) 0.0471(10) Uani 1 1 d . . . C41 C 1.0780(5) 0.2187(4) 0.5279(3) 0.093(2) Uani 1 1 d . . . H41A H 1.1471 0.2035 0.5517 0.140 Uiso 1 1 calc R . . H41B H 1.0893 0.2621 0.4852 0.140 Uiso 1 1 calc R . . H41C H 1.0729 0.1550 0.5242 0.140 Uiso 1 1 calc R . . C42 C 0.9499(7) 0.2086(4) 0.6297(3) 0.129(3) Uani 1 1 d . . . H42A H 1.0176 0.2007 0.6523 0.194 Uiso 1 1 calc R . . H42B H 0.9525 0.1415 0.6277 0.194 Uiso 1 1 calc R . . H42C H 0.8728 0.2405 0.6526 0.194 Uiso 1 1 calc R . . C37 C 0.8556(4) 0.4497(3) 0.5904(2) 0.0467(10) Uani 1 1 d . . . C38 C 0.9649(5) 0.3753(4) 0.5641(3) 0.0784(18) Uani 1 1 d . . . H38A H 0.9859 0.4099 0.5196 0.094 Uiso 1 1 calc R . . H38B H 1.0334 0.3619 0.5886 0.094 Uiso 1 1 calc R . . C6 C 0.6994(9) 0.9505(6) 0.9436(5) 0.183(5) Uani 1 1 d . . . H6A H 0.6973 1.0120 0.9093 0.274 Uiso 1 1 calc R . . H6B H 0.7668 0.9332 0.9691 0.274 Uiso 1 1 calc R . . H6C H 0.6225 0.9628 0.9710 0.274 Uiso 1 1 calc R . . C12 C 0.2611(10) 0.5009(9) 0.9443(5) 0.211(6) Uani 1 1 d . . . H12A H 0.2240 0.5133 0.9053 0.316 Uiso 1 1 calc R . . H12B H 0.2376 0.4474 0.9777 0.316 Uiso 1 1 calc R . . H12C H 0.3498 0.4793 0.9354 0.316 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 O13 0.0396(16) 0.0429(16) 0.0613(19) -0.0211(14) 0.0140(14) -0.0203(14) Zr2 0.0318(2) 0.0391(2) 0.0388(2) -0.01347(17) 0.00085(16) -0.01377(17) Zr1 0.0250(2) 0.0415(2) 0.0428(2) -0.01718(18) -0.00496(16) -0.00589(17) O6 0.0349(15) 0.0448(16) 0.0397(16) -0.0144(12) 0.0012(12) -0.0160(12) O12 0.0308(14) 0.0429(16) 0.0460(17) -0.0133(13) -0.0023(12) -0.0142(12) O11 0.0279(14) 0.0434(16) 0.0452(16) -0.0139(13) -0.0024(12) -0.0098(12) O3 0.0346(17) 0.086(2) 0.0415(17) -0.0183(16) -0.0090(13) -0.0089(16) O1 0.0453(18) 0.0550(19) 0.086(2) -0.0364(17) -0.0270(17) -0.0022(15) O9 0.0337(15) 0.0389(15) 0.0502(18) -0.0140(13) -0.0044(13) -0.0102(12) O10 0.0342(15) 0.0378(15) 0.0539(17) -0.0148(13) -0.0009(13) -0.0133(12) O7 0.0306(15) 0.0436(16) 0.0476(17) -0.0153(13) -0.0089(12) -0.0065(12) O8 0.0330(15) 0.0441(16) 0.0504(17) -0.0191(13) -0.0048(13) -0.0094(13) O5 0.0329(15) 0.0440(16) 0.0452(16) -0.0146(13) -0.0058(12) -0.0113(12) O15 0.064(2) 0.062(2) 0.0464(18) -0.0072(15) -0.0076(15) -0.0348(17) O16 0.0506(18) 0.061(2) 0.0441(17) -0.0166(15) -0.0038(14) -0.0264(15) O14 0.0524(18) 0.0434(17) 0.0628(19) -0.0215(15) 0.0170(15) -0.0249(14) C31 0.0243(19) 0.032(2) 0.046(2) -0.0075(18) -0.0019(18) -0.0129(16) O4 0.0297(15) 0.072(2) 0.0468(18) -0.0125(16) 0.0008(13) -0.0076(14) C7 0.035(2) 0.081(3) 0.038(3) -0.028(2) 0.0007(19) -0.013(2) C8 0.048(3) 0.173(7) 0.049(3) -0.019(4) -0.002(2) -0.036(4) C9 0.043(3) 0.125(5) 0.034(3) -0.013(3) 0.001(2) -0.024(3) C10 0.066(4) 0.181(7) 0.055(4) -0.004(4) 0.009(3) -0.035(4) C11 0.057(5) 0.362(16) 0.149(8) 0.126(9) -0.022(5) -0.071(7) C1 0.056(3) 0.057(3) 0.090(4) -0.040(3) -0.031(3) 0.000(3) O2 0.0380(17) 0.0560(19) 0.079(2) -0.0375(17) -0.0203(16) 0.0051(14) C2 0.117(6) 0.086(5) 0.238(9) -0.103(6) -0.107(6) 0.023(4) C3 0.196(9) 0.077(5) 0.185(8) -0.050(5) -0.135(8) -0.017(5) C5 0.109(5) 0.129(6) 0.109(5) -0.045(5) -0.053(4) -0.023(5) C4 0.213(12) 0.217(11) 0.167(9) -0.024(8) -0.037(8) -0.143(10) C25 0.026(2) 0.032(2) 0.059(3) -0.013(2) -0.0103(19) -0.0043(17) C26 0.029(2) 0.041(2) 0.068(3) -0.019(2) -0.001(2) -0.0137(18) C27 0.040(2) 0.033(2) 0.081(3) -0.013(2) -0.001(2) -0.0102(19) C29 0.067(4) 0.040(3) 0.156(6) -0.004(3) -0.007(4) -0.029(3) C28 0.069(4) 0.038(3) 0.126(5) -0.021(3) 0.021(3) -0.004(3) C30 0.075(4) 0.061(3) 0.109(5) 0.000(3) -0.029(4) -0.009(3) C19 0.027(2) 0.037(2) 0.048(3) -0.0087(19) -0.0063(18) -0.0123(18) C20 0.035(2) 0.040(2) 0.050(3) -0.0074(19) -0.0119(19) -0.0090(18) C22 0.031(2) 0.053(3) 0.057(3) -0.012(2) -0.0083(19) -0.013(2) C24 0.057(3) 0.078(4) 0.152(6) -0.049(4) -0.031(4) -0.019(3) C21 0.060(4) 0.173(7) 0.083(4) -0.025(4) 0.006(3) -0.069(4) C23 0.053(3) 0.081(4) 0.126(5) -0.006(4) -0.048(3) -0.011(3) C13 0.0225(19) 0.041(2) 0.042(2) -0.0129(18) -0.0055(17) -0.0118(17) C14 0.042(2) 0.050(3) 0.049(3) -0.014(2) -0.0013(19) -0.026(2) C15 0.063(3) 0.052(3) 0.062(3) -0.006(2) -0.014(3) -0.025(2) C17 0.108(5) 0.065(4) 0.117(5) 0.020(4) -0.023(4) -0.049(4) C16 0.099(5) 0.085(4) 0.060(3) 0.000(3) -0.030(3) -0.031(4) C18 0.065(4) 0.062(3) 0.091(4) -0.015(3) -0.023(3) 0.002(3) C32 0.027(2) 0.040(2) 0.060(3) -0.015(2) -0.0058(19) -0.0075(18) C33 0.022(2) 0.061(3) 0.082(3) -0.020(3) -0.003(2) -0.014(2) C34 0.055(3) 0.084(4) 0.114(5) -0.044(3) 0.002(3) -0.043(3) C35 0.031(3) 0.097(5) 0.185(7) -0.024(5) -0.027(4) -0.016(3) C36 0.048(3) 0.102(4) 0.092(4) -0.023(3) 0.020(3) -0.037(3) C43 0.036(2) 0.060(3) 0.040(2) -0.016(2) 0.0040(19) -0.012(2) C44 0.042(2) 0.059(3) 0.046(3) -0.015(2) -0.009(2) -0.009(2) C45 0.047(2) 0.045(2) 0.037(2) -0.0115(19) -0.0011(19) -0.017(2) C46 0.091(4) 0.089(4) 0.053(3) -0.024(3) -0.021(3) -0.033(3) C48 0.078(4) 0.084(4) 0.062(3) -0.017(3) 0.005(3) -0.051(3) C47 0.070(4) 0.057(3) 0.080(4) -0.025(3) 0.008(3) -0.012(3) C40 0.112(6) 0.117(6) 0.218(9) -0.112(6) -0.086(6) 0.015(5) C39 0.041(2) 0.040(2) 0.063(3) -0.019(2) 0.000(2) -0.0135(19) C41 0.073(4) 0.071(4) 0.144(6) -0.067(4) 0.044(4) -0.030(3) C42 0.150(7) 0.059(4) 0.104(5) -0.012(4) 0.029(5) 0.022(4) C37 0.042(2) 0.052(3) 0.055(3) -0.026(2) 0.004(2) -0.020(2) C38 0.058(3) 0.067(3) 0.125(5) -0.061(3) 0.045(3) -0.035(3) C6 0.221(11) 0.117(6) 0.263(12) -0.101(7) -0.139(9) -0.016(7) C12 0.248(13) 0.261(13) 0.205(11) -0.131(10) 0.123(10) -0.191(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O13 C37 1.255(5) . ? O13 Zr2 2.265(3) . ? Zr2 O8 2.119(3) . ? Zr2 O12 2.128(3) . ? Zr2 O6 2.176(3) . ? Zr2 O10 2.177(3) . ? Zr2 O16 2.194(3) . ? Zr2 O14 2.196(3) . ? Zr2 O15 2.275(3) . ? Zr2 C37 2.609(4) . ? Zr2 C43 2.614(4) . ? Zr1 O5 2.128(3) . ? Zr1 O9 2.143(3) . ? Zr1 O11 2.185(2) . ? Zr1 O7 2.189(3) . ? Zr1 O3 2.205(3) . ? Zr1 O2 2.209(3) . ? Zr1 O4 2.249(3) . ? Zr1 O1 2.272(3) . ? Zr1 C1 2.605(4) . ? Zr1 C7 2.609(4) . ? O6 C13 1.249(4) . ? O12 C31 1.262(4) . ? O11 C31 1.262(4) . ? O3 C7 1.267(5) . ? O1 C1 1.260(5) . ? O9 C25 1.269(5) . ? O10 C25 1.269(5) . ? O7 C19 1.260(4) . ? O8 C19 1.258(4) . ? O5 C13 1.269(4) . ? O15 C43 1.254(5) . ? O16 C43 1.290(5) . ? O14 C37 1.277(5) . ? C31 C32 1.502(5) . ? O4 C7 1.261(5) . ? C7 C8 1.484(6) . ? C8 C9 1.502(7) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C11 1.445(8) . ? C9 C10 1.498(6) . ? C9 C12 1.540(10) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C1 O2 1.260(5) . ? C1 C2 1.519(7) . ? C2 C3 1.387(8) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C5 1.449(9) . ? C3 C6 1.538(8) . ? C3 C4 1.712(12) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C25 C26 1.496(5) . ? C26 C27 1.546(6) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C27 C29 1.520(6) . ? C27 C28 1.528(6) . ? C27 C30 1.537(7) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C19 C20 1.509(5) . ? C20 C22 1.533(5) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C22 C21 1.512(7) . ? C22 C23 1.521(6) . ? C22 C24 1.529(6) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C13 C14 1.518(5) . ? C14 C15 1.547(6) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C18 1.518(7) . ? C15 C16 1.526(6) . ? C15 C17 1.539(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C32 C33 1.544(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C35 1.526(6) . ? C33 C34 1.528(6) . ? C33 C36 1.531(7) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C43 C44 1.500(6) . ? C44 C45 1.527(5) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C47 1.511(6) . ? C45 C48 1.517(6) . ? C45 C46 1.531(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C40 C39 1.492(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C39 C42 1.496(7) . ? C39 C38 1.498(6) . ? C39 C41 1.537(6) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C37 C38 1.501(6) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C37 O13 Zr2 91.0(2) . . ? O8 Zr2 O12 104.34(10) . . ? O8 Zr2 O6 76.61(10) . . ? O12 Zr2 O6 78.50(9) . . ? O8 Zr2 O10 78.74(10) . . ? O12 Zr2 O10 76.07(10) . . ? O6 Zr2 O10 138.61(10) . . ? O8 Zr2 O16 87.71(10) . . ? O12 Zr2 O16 150.59(11) . . ? O6 Zr2 O16 78.41(10) . . ? O10 Zr2 O16 133.14(11) . . ? O8 Zr2 O14 150.36(11) . . ? O12 Zr2 O14 89.75(11) . . ? O6 Zr2 O14 132.43(10) . . ? O10 Zr2 O14 79.61(10) . . ? O16 Zr2 O14 92.52(11) . . ? O8 Zr2 O13 149.69(10) . . ? O12 Zr2 O13 78.56(10) . . ? O6 Zr2 O13 74.45(9) . . ? O10 Zr2 O13 130.14(10) . . ? O16 Zr2 O13 77.88(11) . . ? O14 Zr2 O13 58.01(10) . . ? O8 Zr2 O15 76.94(11) . . ? O12 Zr2 O15 150.24(10) . . ? O6 Zr2 O15 129.37(10) . . ? O10 Zr2 O15 75.07(10) . . ? O16 Zr2 O15 58.15(11) . . ? O14 Zr2 O15 78.09(11) . . ? O13 Zr2 O15 115.59(11) . . ? O8 Zr2 C37 172.19(12) . . ? O12 Zr2 C37 83.17(12) . . ? O6 Zr2 C37 103.19(12) . . ? O10 Zr2 C37 105.55(12) . . ? O16 Zr2 C37 84.62(12) . . ? O14 Zr2 C37 29.25(11) . . ? O13 Zr2 C37 28.76(11) . . ? O15 Zr2 C37 97.67(13) . . ? O8 Zr2 C43 80.57(12) . . ? O12 Zr2 C43 174.85(11) . . ? O6 Zr2 C43 104.44(12) . . ? O10 Zr2 C43 103.66(13) . . ? O16 Zr2 C43 29.50(12) . . ? O14 Zr2 C43 85.16(12) . . ? O13 Zr2 C43 98.03(12) . . ? O15 Zr2 C43 28.66(12) . . ? C37 Zr2 C43 91.99(13) . . ? O5 Zr1 O9 106.75(10) . . ? O5 Zr1 O11 75.87(9) . . ? O9 Zr1 O11 78.76(10) . . ? O5 Zr1 O7 81.67(10) . . ? O9 Zr1 O7 75.76(10) . . ? O11 Zr1 O7 139.24(10) . . ? O5 Zr1 O3 87.13(11) . . ? O9 Zr1 O3 152.12(10) . . ? O11 Zr1 O3 81.54(10) . . ? O7 Zr1 O3 131.12(10) . . ? O5 Zr1 O2 152.03(10) . . ? O9 Zr1 O2 87.80(11) . . ? O11 Zr1 O2 131.32(10) . . ? O7 Zr1 O2 78.94(10) . . ? O3 Zr1 O2 90.59(12) . . ? O5 Zr1 O4 78.25(11) . . ? O9 Zr1 O4 147.52(10) . . ? O11 Zr1 O4 132.46(10) . . ? O7 Zr1 O4 73.26(10) . . ? O3 Zr1 O4 57.88(10) . . ? O2 Zr1 O4 76.97(11) . . ? O5 Zr1 O1 147.46(10) . . ? O9 Zr1 O1 78.13(11) . . ? O11 Zr1 O1 73.62(10) . . ? O7 Zr1 O1 129.76(11) . . ? O3 Zr1 O1 77.51(12) . . ? O2 Zr1 O1 57.81(10) . . ? O4 Zr1 O1 115.28(11) . . ? O5 Zr1 C1 170.17(14) . . ? O9 Zr1 C1 82.21(15) . . ? O11 Zr1 C1 102.52(13) . . ? O7 Zr1 C1 104.89(13) . . ? O3 Zr1 C1 83.04(15) . . ? O2 Zr1 C1 28.87(12) . . ? O4 Zr1 C1 96.43(14) . . ? O1 Zr1 C1 28.94(12) . . ? O5 Zr1 C7 81.81(12) . . ? O9 Zr1 C7 170.58(13) . . ? O11 Zr1 C7 107.66(12) . . ? O7 Zr1 C7 102.15(12) . . ? O3 Zr1 C7 28.98(12) . . ? O2 Zr1 C7 82.79(14) . . ? O4 Zr1 C7 28.90(11) . . ? O1 Zr1 C7 96.83(13) . . ? C1 Zr1 C7 89.57(16) . . ? C13 O6 Zr2 131.0(2) . . ? C31 O12 Zr2 164.1(2) . . ? C31 O11 Zr1 129.8(2) . . ? C7 O3 Zr1 93.5(3) . . ? C1 O1 Zr1 90.3(3) . . ? C25 O9 Zr1 163.8(3) . . ? C25 O10 Zr2 130.6(3) . . ? C19 O7 Zr1 127.6(2) . . ? C19 O8 Zr2 165.3(3) . . ? C13 O5 Zr1 162.0(3) . . ? C43 O15 Zr2 90.9(3) . . ? C43 O16 Zr2 93.6(2) . . ? C37 O14 Zr2 93.6(2) . . ? O12 C31 O11 123.1(3) . . ? O12 C31 C32 118.8(3) . . ? O11 C31 C32 118.1(4) . . ? C7 O4 Zr1 91.6(2) . . ? O4 C7 O3 117.0(4) . . ? O4 C7 C8 122.7(4) . . ? O3 C7 C8 120.2(4) . . ? O4 C7 Zr1 59.5(2) . . ? O3 C7 Zr1 57.5(2) . . ? C8 C7 Zr1 175.4(4) . . ? C7 C8 C9 120.2(4) . . ? C7 C8 H8A 107.3 . . ? C9 C8 H8A 107.3 . . ? C7 C8 H8B 107.3 . . ? C9 C8 H8B 107.3 . . ? H8A C8 H8B 106.9 . . ? C11 C9 C10 113.3(5) . . ? C11 C9 C8 118.1(6) . . ? C10 C9 C8 111.9(4) . . ? C11 C9 C12 105.2(8) . . ? C10 C9 C12 104.2(6) . . ? C8 C9 C12 102.2(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 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? O2 C1 O1 118.6(4) . . ? O2 C1 C2 118.8(4) . . ? O1 C1 C2 122.5(4) . . ? O2 C1 Zr1 57.9(2) . . ? O1 C1 Zr1 60.7(2) . . ? C2 C1 Zr1 175.9(4) . . ? C1 O2 Zr1 93.2(3) . . ? C3 C2 C1 124.2(5) . . ? C3 C2 H2A 106.3 . . ? C1 C2 H2A 106.3 . . ? C3 C2 H2B 106.3 . . ? C1 C2 H2B 106.3 . . ? H2A C2 H2B 106.4 . . ? C2 C3 C5 121.0(7) . . ? C2 C3 C6 110.4(7) . . ? C5 C3 C6 110.7(6) . . ? C2 C3 C4 101.3(7) . . ? C5 C3 C4 100.9(7) . . ? C6 C3 C4 111.5(8) . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? O9 C25 O10 122.7(4) . . ? O9 C25 C26 119.3(4) . . ? O10 C25 C26 118.0(4) . . ? C25 C26 C27 114.7(3) . . ? C25 C26 H26A 108.6 . . ? C27 C26 H26A 108.6 . . ? C25 C26 H26B 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C29 C27 C28 110.1(4) . . ? C29 C27 C30 110.3(5) . . ? C28 C27 C30 109.4(4) . . ? C29 C27 C26 107.2(4) . . ? C28 C27 C26 109.7(4) . . ? C30 C27 C26 110.1(4) . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O8 C19 O7 123.3(4) . . ? O8 C19 C20 118.4(4) . . ? O7 C19 C20 118.2(4) . . ? C19 C20 C22 114.7(3) . . ? C19 C20 H20A 108.6 . . ? C22 C20 H20A 108.6 . . ? C19 C20 H20B 108.6 . . ? C22 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C21 C22 C23 109.0(4) . . ? C21 C22 C24 109.9(5) . . ? C23 C22 C24 108.5(4) . . ? C21 C22 C20 110.9(4) . . ? C23 C22 C20 108.9(4) . . ? C24 C22 C20 109.7(4) . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C21 H21A 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C22 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O6 C13 O5 123.6(3) . . ? O6 C13 C14 118.1(3) . . ? O5 C13 C14 118.3(3) . . ? C13 C14 C15 114.3(3) . . ? C13 C14 H14A 108.7 . . ? C15 C14 H14A 108.7 . . ? C13 C14 H14B 108.7 . . ? C15 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C18 C15 C16 109.5(4) . . ? C18 C15 C17 108.8(5) . . ? C16 C15 C17 109.5(4) . . ? C18 C15 C14 111.2(4) . . ? C16 C15 C14 111.3(4) . . ? C17 C15 C14 106.4(4) . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C18 H18A 109.5 . . ? C15 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C15 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C31 C32 C33 113.2(3) . . ? C31 C32 H32A 108.9 . . ? C33 C32 H32A 108.9 . . ? C31 C32 H32B 108.9 . . ? C33 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? C35 C33 C34 110.6(5) . . ? C35 C33 C36 108.9(4) . . ? C34 C33 C36 110.1(4) . . ? C35 C33 C32 107.5(4) . . ? C34 C33 C32 109.7(4) . . ? C36 C33 C32 110.0(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O15 C43 O16 117.4(4) . . ? O15 C43 C44 122.7(4) . . ? O16 C43 C44 119.9(4) . . ? O15 C43 Zr2 60.5(2) . . ? O16 C43 Zr2 56.9(2) . . ? C44 C43 Zr2 176.2(3) . . ? C43 C44 C45 113.7(3) . . ? C43 C44 H44A 108.8 . . ? C45 C44 H44A 108.8 . . ? C43 C44 H44B 108.8 . . ? C45 C44 H44B 108.8 . . ? H44A C44 H44B 107.7 . . ? C47 C45 C48 109.9(4) . . ? C47 C45 C44 110.1(4) . . ? C48 C45 C44 111.0(4) . . ? C47 C45 C46 109.6(4) . . ? C48 C45 C46 109.2(4) . . ? C44 C45 C46 107.0(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C45 C48 H48A 109.5 . . ? C45 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C45 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C47 H47A 109.5 . . ? C45 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C45 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C40 C39 C42 107.2(6) . . ? C40 C39 C38 111.4(4) . . ? C42 C39 C38 111.4(5) . . ? C40 C39 C41 109.9(5) . . ? C42 C39 C41 107.9(4) . . ? C38 C39 C41 108.9(4) . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O13 C37 O14 117.4(4) . . ? O13 C37 C38 123.1(4) . . ? O14 C37 C38 119.5(4) . . ? O13 C37 Zr2 60.3(2) . . ? O14 C37 Zr2 57.1(2) . . ? C38 C37 Zr2 176.7(3) . . ? C39 C38 C37 119.9(4) . . ? C39 C38 H38A 107.3 . . ? C37 C38 H38A 107.3 . . ? C39 C38 H38B 107.3 . . ? C37 C38 H38B 107.3 . . ? H38A C38 H38B 106.9 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? 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 C37 O13 Zr2 O8 164.4(2) . . . . ? C37 O13 Zr2 O12 -96.7(3) . . . . ? C37 O13 Zr2 O6 -177.8(3) . . . . ? C37 O13 Zr2 O10 -36.1(3) . . . . ? C37 O13 Zr2 O16 101.1(3) . . . . ? C37 O13 Zr2 O14 0.3(2) . . . . ? C37 O13 Zr2 O15 55.6(3) . . . . ? C37 O13 Zr2 C43 79.4(3) . . . . ? O8 Zr2 O6 C13 -57.2(3) . . . . ? O12 Zr2 O6 C13 50.7(3) . . . . ? O10 Zr2 O6 C13 -2.3(4) . . . . ? O16 Zr2 O6 C13 -147.6(3) . . . . ? O14 Zr2 O6 C13 129.6(3) . . . . ? O13 Zr2 O6 C13 131.9(3) . . . . ? O15 Zr2 O6 C13 -117.5(3) . . . . ? C37 Zr2 O6 C13 130.8(3) . . . . ? C43 Zr2 O6 C13 -133.6(3) . . . . ? O8 Zr2 O12 C31 9.9(9) . . . . ? O6 Zr2 O12 C31 -62.9(9) . . . . ? O10 Zr2 O12 C31 84.1(9) . . . . ? O16 Zr2 O12 C31 -101.8(9) . . . . ? O14 Zr2 O12 C31 163.5(9) . . . . ? O13 Zr2 O12 C31 -139.2(9) . . . . ? O15 Zr2 O12 C31 98.6(9) . . . . ? C37 Zr2 O12 C31 -167.9(9) . . . . ? C43 Zr2 O12 C31 171.8(13) . . . . ? O5 Zr1 O11 C31 64.1(3) . . . . ? O9 Zr1 O11 C31 -46.5(3) . . . . ? O7 Zr1 O11 C31 5.5(4) . . . . ? O3 Zr1 O11 C31 153.3(3) . . . . ? O2 Zr1 O11 C31 -123.4(3) . . . . ? O4 Zr1 O11 C31 123.1(3) . . . . ? O1 Zr1 O11 C31 -127.3(3) . . . . ? C1 Zr1 O11 C31 -125.8(3) . . . . ? C7 Zr1 O11 C31 140.6(3) . . . . ? O5 Zr1 O3 C7 -78.2(3) . . . . ? O9 Zr1 O3 C7 160.3(3) . . . . ? O11 Zr1 O3 C7 -154.4(3) . . . . ? O7 Zr1 O3 C7 -1.9(3) . . . . ? O2 Zr1 O3 C7 73.9(3) . . . . ? O4 Zr1 O3 C7 -0.3(3) . . . . ? O1 Zr1 O3 C7 130.6(3) . . . . ? C1 Zr1 O3 C7 101.8(3) . . . . ? O5 Zr1 O1 C1 -162.0(3) . . . . ? O9 Zr1 O1 C1 95.4(3) . . . . ? O11 Zr1 O1 C1 177.0(3) . . . . ? O7 Zr1 O1 C1 35.5(4) . . . . ? O3 Zr1 O1 C1 -98.3(3) . . . . ? O2 Zr1 O1 C1 0.5(3) . . . . ? O4 Zr1 O1 C1 -53.3(3) . . . . ? C7 Zr1 O1 C1 -76.6(3) . . . . ? O5 Zr1 O9 C25 7.2(9) . . . . ? O11 Zr1 O9 C25 78.6(9) . . . . ? O7 Zr1 O9 C25 -69.4(9) . . . . ? O3 Zr1 O9 C25 124.4(9) . . . . ? O2 Zr1 O9 C25 -148.5(9) . . . . ? O4 Zr1 O9 C25 -87.2(9) . . . . ? O1 Zr1 O9 C25 154.0(9) . . . . ? C1 Zr1 O9 C25 -176.9(9) . . . . ? C7 Zr1 O9 C25 -147.7(9) . . . . ? O8 Zr2 O10 C25 52.4(3) . . . . ? O12 Zr2 O10 C25 -55.6(3) . . . . ? O6 Zr2 O10 C25 -1.9(4) . . . . ? O16 Zr2 O10 C25 128.4(3) . . . . ? O14 Zr2 O10 C25 -147.9(3) . . . . ? O13 Zr2 O10 C25 -117.1(3) . . . . ? O15 Zr2 O10 C25 131.8(3) . . . . ? C37 Zr2 O10 C25 -134.3(3) . . . . ? C43 Zr2 O10 C25 129.7(3) . . . . ? O5 Zr1 O7 C19 -49.9(3) . . . . ? O9 Zr1 O7 C19 59.8(3) . . . . ? O11 Zr1 O7 C19 6.9(4) . . . . ? O3 Zr1 O7 C19 -128.7(3) . . . . ? O2 Zr1 O7 C19 150.4(3) . . . . ? O4 Zr1 O7 C19 -130.1(3) . . . . ? O1 Zr1 O7 C19 120.7(3) . . . . ? C1 Zr1 O7 C19 137.6(3) . . . . ? C7 Zr1 O7 C19 -129.6(3) . . . . ? O12 Zr2 O8 C19 30.6(11) . . . . ? O6 Zr2 O8 C19 104.8(10) . . . . ? O10 Zr2 O8 C19 -41.7(10) . . . . ? O16 Zr2 O8 C19 -176.6(10) . . . . ? O14 Zr2 O8 C19 -85.5(11) . . . . ? O13 Zr2 O8 C19 122.4(10) . . . . ? O15 Zr2 O8 C19 -118.8(11) . . . . ? C37 Zr2 O8 C19 -165.8(10) . . . . ? C43 Zr2 O8 C19 -147.8(11) . . . . ? O9 Zr1 O5 C13 12.4(8) . . . . ? O11 Zr1 O5 C13 -61.0(8) . . . . ? O7 Zr1 O5 C13 84.8(8) . . . . ? O3 Zr1 O5 C13 -143.0(8) . . . . ? O2 Zr1 O5 C13 131.2(8) . . . . ? O4 Zr1 O5 C13 159.3(8) . . . . ? O1 Zr1 O5 C13 -81.7(8) . . . . ? C1 Zr1 O5 C13 -142.7(9) . . . . ? C7 Zr1 O5 C13 -171.6(8) . . . . ? O8 Zr2 O15 C43 -94.2(3) . . . . ? O12 Zr2 O15 C43 169.7(2) . . . . ? O6 Zr2 O15 C43 -34.1(3) . . . . ? O10 Zr2 O15 C43 -175.8(3) . . . . ? O16 Zr2 O15 C43 1.3(2) . . . . ? O14 Zr2 O15 C43 101.9(3) . . . . ? O13 Zr2 O15 C43 56.4(3) . . . . ? C37 Zr2 O15 C43 80.0(3) . . . . ? O8 Zr2 O16 C43 74.8(2) . . . . ? O12 Zr2 O16 C43 -169.5(2) . . . . ? O6 Zr2 O16 C43 151.6(2) . . . . ? O10 Zr2 O16 C43 2.6(3) . . . . ? O14 Zr2 O16 C43 -75.5(2) . . . . ? O13 Zr2 O16 C43 -132.1(2) . . . . ? O15 Zr2 O16 C43 -1.2(2) . . . . ? C37 Zr2 O16 C43 -103.7(2) . . . . ? O8 Zr2 O14 C37 -164.1(2) . . . . ? O12 Zr2 O14 C37 76.4(3) . . . . ? O6 Zr2 O14 C37 2.3(3) . . . . ? O10 Zr2 O14 C37 152.3(3) . . . . ? O16 Zr2 O14 C37 -74.3(3) . . . . ? O13 Zr2 O14 C37 -0.3(2) . . . . ? O15 Zr2 O14 C37 -131.0(3) . . . . ? C43 Zr2 O14 C37 -102.9(3) . . . . ? Zr2 O12 C31 O11 -4.9(11) . . . . ? Zr2 O12 C31 C32 176.6(7) . . . . ? Zr1 O11 C31 O12 -9.6(5) . . . . ? Zr1 O11 C31 C32 169.0(2) . . . . ? O5 Zr1 O4 C7 94.3(3) . . . . ? O9 Zr1 O4 C7 -162.9(3) . . . . ? O11 Zr1 O4 C7 36.2(3) . . . . ? O7 Zr1 O4 C7 179.1(3) . . . . ? O3 Zr1 O4 C7 0.3(3) . . . . ? O2 Zr1 O4 C7 -98.8(3) . . . . ? O1 Zr1 O4 C7 -54.3(3) . . . . ? C1 Zr1 O4 C7 -77.3(3) . . . . ? Zr1 O4 C7 O3 -0.5(4) . . . . ? Zr1 O4 C7 C8 175.3(5) . . . . ? Zr1 O3 C7 O4 0.5(4) . . . . ? Zr1 O3 C7 C8 -175.4(5) . . . . ? O5 Zr1 C7 O4 -80.5(3) . . . . ? O9 Zr1 C7 O4 75.2(8) . . . . ? O11 Zr1 C7 O4 -152.8(2) . . . . ? O7 Zr1 C7 O4 -0.9(3) . . . . ? O3 Zr1 C7 O4 -179.5(4) . . . . ? O2 Zr1 C7 O4 76.1(3) . . . . ? O1 Zr1 C7 O4 132.3(3) . . . . ? C1 Zr1 C7 O4 104.2(3) . . . . ? O5 Zr1 C7 O3 98.9(3) . . . . ? O9 Zr1 C7 O3 -105.3(7) . . . . ? O11 Zr1 C7 O3 26.7(3) . . . . ? O7 Zr1 C7 O3 178.5(3) . . . . ? O2 Zr1 C7 O3 -104.5(3) . . . . ? O4 Zr1 C7 O3 179.5(4) . . . . ? O1 Zr1 C7 O3 -48.3(3) . . . . ? C1 Zr1 C7 O3 -76.3(3) . . . . ? O5 Zr1 C7 C8 160(5) . . . . ? O9 Zr1 C7 C8 -44(5) . . . . ? O11 Zr1 C7 C8 88(5) . . . . ? O7 Zr1 C7 C8 -120(5) . . . . ? O3 Zr1 C7 C8 61(5) . . . . ? O2 Zr1 C7 C8 -43(5) . . . . ? O4 Zr1 C7 C8 -119(5) . . . . ? O1 Zr1 C7 C8 13(5) . . . . ? C1 Zr1 C7 C8 -15(5) . . . . ? O4 C7 C8 C9 41.0(9) . . . . ? O3 C7 C8 C9 -143.4(5) . . . . ? Zr1 C7 C8 C9 158(5) . . . . ? C7 C8 C9 C11 -50.7(10) . . . . ? C7 C8 C9 C10 174.9(6) . . . . ? C7 C8 C9 C12 64.0(8) . . . . ? Zr1 O1 C1 O2 -0.8(5) . . . . ? Zr1 O1 C1 C2 177.1(6) . . . . ? O5 Zr1 C1 O2 -104.3(7) . . . . ? O9 Zr1 C1 O2 99.7(3) . . . . ? O11 Zr1 C1 O2 176.3(3) . . . . ? O7 Zr1 C1 O2 26.7(3) . . . . ? O3 Zr1 C1 O2 -104.1(3) . . . . ? O4 Zr1 C1 O2 -47.6(3) . . . . ? O1 Zr1 C1 O2 179.2(5) . . . . ? C7 Zr1 C1 O2 -75.7(3) . . . . ? O5 Zr1 C1 O1 76.5(8) . . . . ? O9 Zr1 C1 O1 -79.5(3) . . . . ? O11 Zr1 C1 O1 -3.0(3) . . . . ? O7 Zr1 C1 O1 -152.5(3) . . . . ? O3 Zr1 C1 O1 76.7(3) . . . . ? O2 Zr1 C1 O1 -179.2(5) . . . . ? O4 Zr1 C1 O1 133.2(3) . . . . ? C7 Zr1 C1 O1 105.0(3) . . . . ? O5 Zr1 C1 C2 -67(6) . . . . ? O9 Zr1 C1 C2 137(6) . . . . ? O11 Zr1 C1 C2 -146(6) . . . . ? O7 Zr1 C1 C2 64(6) . . . . ? O3 Zr1 C1 C2 -66(6) . . . . ? O2 Zr1 C1 C2 38(6) . . . . ? O4 Zr1 C1 C2 -10(6) . . . . ? O1 Zr1 C1 C2 -143(6) . . . . ? C7 Zr1 C1 C2 -38(6) . . . . ? O1 C1 O2 Zr1 0.8(5) . . . . ? C2 C1 O2 Zr1 -177.1(6) . . . . ? O5 Zr1 O2 C1 159.3(3) . . . . ? O9 Zr1 O2 C1 -77.8(3) . . . . ? O11 Zr1 O2 C1 -4.9(4) . . . . ? O7 Zr1 O2 C1 -153.7(3) . . . . ? O3 Zr1 O2 C1 74.4(3) . . . . ? O4 Zr1 O2 C1 131.1(3) . . . . ? O1 Zr1 O2 C1 -0.5(3) . . . . ? C7 Zr1 O2 C1 102.3(3) . . . . ? O2 C1 C2 C3 178.1(9) . . . . ? O1 C1 C2 C3 0.2(13) . . . . ? Zr1 C1 C2 C3 142(6) . . . . ? C1 C2 C3 C5 -45.1(15) . . . . ? C1 C2 C3 C6 -176.7(8) . . . . ? C1 C2 C3 C4 65.1(11) . . . . ? Zr1 O9 C25 O10 -7.6(11) . . . . ? Zr1 O9 C25 C26 170.5(7) . . . . ? Zr2 O10 C25 O9 1.9(5) . . . . ? Zr2 O10 C25 C26 -176.3(2) . . . . ? O9 C25 C26 C27 -84.7(5) . . . . ? O10 C25 C26 C27 93.6(4) . . . . ? C25 C26 C27 C29 -175.6(4) . . . . ? C25 C26 C27 C28 64.8(5) . . . . ? C25 C26 C27 C30 -55.6(5) . . . . ? Zr2 O8 C19 O7 -33.3(13) . . . . ? Zr2 O8 C19 C20 148.4(9) . . . . ? Zr1 O7 C19 O8 0.0(5) . . . . ? Zr1 O7 C19 C20 178.3(2) . . . . ? O8 C19 C20 C22 87.0(5) . . . . ? O7 C19 C20 C22 -91.3(4) . . . . ? C19 C20 C22 C21 60.8(5) . . . . ? C19 C20 C22 C23 -179.3(4) . . . . ? C19 C20 C22 C24 -60.7(5) . . . . ? Zr2 O6 C13 O5 9.0(5) . . . . ? Zr2 O6 C13 C14 -170.2(2) . . . . ? Zr1 O5 C13 O6 -19.3(10) . . . . ? Zr1 O5 C13 C14 159.8(6) . . . . ? O6 C13 C14 C15 88.9(4) . . . . ? O5 C13 C14 C15 -90.3(4) . . . . ? C13 C14 C15 C18 -55.3(5) . . . . ? C13 C14 C15 C16 67.2(5) . . . . ? C13 C14 C15 C17 -173.6(4) . . . . ? O12 C31 C32 C33 86.3(4) . . . . ? O11 C31 C32 C33 -92.3(4) . . . . ? C31 C32 C33 C35 177.0(4) . . . . ? C31 C32 C33 C34 56.7(5) . . . . ? C31 C32 C33 C36 -64.6(5) . . . . ? Zr2 O15 C43 O16 -2.1(4) . . . . ? Zr2 O15 C43 C44 177.6(4) . . . . ? Zr2 O16 C43 O15 2.2(4) . . . . ? Zr2 O16 C43 C44 -177.6(3) . . . . ? O8 Zr2 C43 O15 80.0(2) . . . . ? O12 Zr2 C43 O15 -82.3(14) . . . . ? O6 Zr2 C43 O15 153.4(2) . . . . ? O10 Zr2 C43 O15 4.1(3) . . . . ? O16 Zr2 C43 O15 -177.8(4) . . . . ? O14 Zr2 C43 O15 -73.9(2) . . . . ? O13 Zr2 C43 O15 -130.6(2) . . . . ? C37 Zr2 C43 O15 -102.4(3) . . . . ? O8 Zr2 C43 O16 -102.2(2) . . . . ? O12 Zr2 C43 O16 95.5(14) . . . . ? O6 Zr2 C43 O16 -28.8(2) . . . . ? O10 Zr2 C43 O16 -178.1(2) . . . . ? O14 Zr2 C43 O16 103.9(2) . . . . ? O13 Zr2 C43 O16 47.2(2) . . . . ? O15 Zr2 C43 O16 177.8(4) . . . . ? C37 Zr2 C43 O16 75.4(2) . . . . ? O8 Zr2 C43 C44 -68(5) . . . . ? O12 Zr2 C43 C44 130(4) . . . . ? O6 Zr2 C43 C44 5(5) . . . . ? O10 Zr2 C43 C44 -144(5) . . . . ? O16 Zr2 C43 C44 34(5) . . . . ? O14 Zr2 C43 C44 138(5) . . . . ? O13 Zr2 C43 C44 81(5) . . . . ? O15 Zr2 C43 C44 -148(5) . . . . ? C37 Zr2 C43 C44 110(5) . . . . ? O15 C43 C44 C45 79.5(5) . . . . ? O16 C43 C44 C45 -100.8(5) . . . . ? Zr2 C43 C44 C45 -134(5) . . . . ? C43 C44 C45 C47 59.0(5) . . . . ? C43 C44 C45 C48 -62.9(5) . . . . ? C43 C44 C45 C46 178.1(4) . . . . ? Zr2 O13 C37 O14 -0.4(4) . . . . ? Zr2 O13 C37 C38 179.5(4) . . . . ? Zr2 O14 C37 O13 0.5(4) . . . . ? Zr2 O14 C37 C38 -179.5(4) . . . . ? O8 Zr2 C37 O13 -85.4(9) . . . . ? O12 Zr2 C37 O13 78.6(2) . . . . ? O6 Zr2 C37 O13 2.2(3) . . . . ? O10 Zr2 C37 O13 152.1(2) . . . . ? O16 Zr2 C37 O13 -74.5(2) . . . . ? O14 Zr2 C37 O13 -179.5(4) . . . . ? O15 Zr2 C37 O13 -131.3(2) . . . . ? C43 Zr2 C37 O13 -103.1(3) . . . . ? O8 Zr2 C37 O14 94.1(9) . . . . ? O12 Zr2 C37 O14 -101.8(2) . . . . ? O6 Zr2 C37 O14 -178.3(2) . . . . ? O10 Zr2 C37 O14 -28.4(3) . . . . ? O16 Zr2 C37 O14 105.0(3) . . . . ? O13 Zr2 C37 O14 179.5(4) . . . . ? O15 Zr2 C37 O14 48.2(3) . . . . ? C43 Zr2 C37 O14 76.4(3) . . . . ? O8 Zr2 C37 C38 101(6) . . . . ? O12 Zr2 C37 C38 -95(6) . . . . ? O6 Zr2 C37 C38 -171(6) . . . . ? O10 Zr2 C37 C38 -21(6) . . . . ? O16 Zr2 C37 C38 112(6) . . . . ? O14 Zr2 C37 C38 7(6) . . . . ? O13 Zr2 C37 C38 -173(6) . . . . ? O15 Zr2 C37 C38 55(6) . . . . ? C43 Zr2 C37 C38 84(6) . . . . ? C40 C39 C38 C37 52.7(7) . . . . ? C42 C39 C38 C37 -67.0(7) . . . . ? C41 C39 C38 C37 174.0(5) . . . . ? O13 C37 C38 C39 21.8(8) . . . . ? O14 C37 C38 C39 -158.2(5) . . . . ? Zr2 C37 C38 C39 -165(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.845 _refine_diff_density_min -0.567 _refine_diff_density_rms 0.075 # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 0.000 0.000 854 132 ' ' 2 0.238 0.583 0.802 11 0 ' ' 3 0.761 0.416 0.198 11 0 ' ' _platon_squeeze_details ; ; #===END data_5 _audit_creation_method 'APEX2 v2014.5-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common AMLJA061AJMcc _chemical_formula_moiety ? _chemical_formula_sum 'C32 H56 Hf2 O16' _chemical_formula_iupac ? _chemical_formula_weight 1053.74 _chemical_absolute_configuration ? _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall 'C -2yc' loop_ _space_group_symop_operation_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' _cell_length_a 13.9140(4) _cell_length_b 14.3509(4) _cell_length_c 20.4398(6) _cell_angle_alpha 90 _cell_angle_beta 94.1728(15) _cell_angle_gamma 90 _cell_volume 4070.5(3) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9906 _cell_measurement_theta_min 2.8387 _cell_measurement_theta_max 25.2768 _cell_measurement_temperature 173.(2) _exptl_crystal_description irregular _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.160 _exptl_crystal_size_mid 0.120 _exptl_crystal_size_min 0.100 _exptl_crystal_density_diffrn 1.720 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 5.161 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_T_max 0.597 _exptl_special_details ; ; _diffrn_ambient_temperature 173.(2) _diffrn_source 'fine-focus tube' _diffrn_source_type ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3333 _diffrn_reflns_number 17841 _diffrn_reflns_av_R_equivalents 0.0139 _diffrn_reflns_av_unetI/netI 0.0251 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.28 _diffrn_reflns_theta_full 25.28 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.998 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _refine_special_details 'Refined as a 2-component inversion twin.' _reflns_number_total 6874 _reflns_number_gt 6796 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_gt 0.0539 _refine_ls_wR_factor_ref 0.0667 _refine_ls_goodness_of_fit_ref 1.177 _refine_ls_restrained_S_all 1.177 _refine_ls_number_reflns 6874 _refine_ls_number_parameters 416 _refine_ls_number_restraints 2 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0390P)^2^+7.5165P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.364 _refine_diff_density_min -0.915 _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Refined as an inversion twin.' _refine_ls_abs_structure_Flack 0.129(14) 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' 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' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'Bruker XT Intrinsic Solution Method' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf1 0.49600(2) 0.79001(2) 1.10117(2) 0.02183(10) Uani d . . . 1 . . Hf Hf2 0.49900(2) 0.72989(2) 0.89817(2) 0.02122(10) Uani d . . . 1 . . O O1 0.4426(8) 0.7011(8) 1.1791(5) 0.068(3) Uani d . . . 1 . . O O2 0.5906(8) 0.7281(6) 1.1832(5) 0.059(3) Uani d . . . 1 . . O O3 0.3977(6) 0.8834(6) 1.1517(4) 0.050(2) Uani d . . . 1 . . O O4 0.5485(5) 0.9150(5) 1.1553(4) 0.0416(19) Uani d . . . 1 . . O O5 0.4667(5) 0.8877(4) 1.0245(3) 0.0298(15) Uani d . . . 1 . . O O6 0.6377(4) 0.8138(5) 1.0674(3) 0.0288(14) Uani d . . . 1 . . O O7 0.5251(5) 0.6615(4) 1.0564(3) 0.0283(14) Uani d . . . 1 . . O O8 0.3544(5) 0.7470(5) 1.0611(3) 0.0331(15) Uani d . . . 1 . . O O9 0.5381(5) 0.6070(4) 0.9553(3) 0.0292(14) Uani d . . . 1 . . O O10 0.3801(5) 0.7123(5) 0.9569(3) 0.0321(15) Uani d . . . 1 . . O O11 0.6168(5) 0.7795(4) 0.9604(4) 0.0269(15) Uani d . . . 1 . . O O12 0.4590(5) 0.8708(4) 0.9157(3) 0.0311(14) Uani d . . . 1 . . O O13 0.5691(6) 0.8037(5) 0.8204(4) 0.0358(17) Uani d . . . 1 . . O O14 0.6229(5) 0.6687(5) 0.8498(4) 0.0380(17) Uani d . . . 1 . . O O15 0.3758(8) 0.7617(6) 0.8248(5) 0.052(3) Uani d . . . 1 . . O O16 0.4276(7) 0.6232(6) 0.8349(4) 0.056(2) Uani d . . . 1 . . C C1 0.5196(9) 0.6886(7) 1.2080(5) 0.042(3) Uani d . . . 1 . . C C2 0.5299(15) 0.6312(14) 1.2694(7) 0.091(4) Uani d . . . 1 . . H H2 0.4801 0.5812 1.2625 0.109 Uiso calc U . R 1 . . C C3 0.6162(14) 0.5834(13) 1.2817(6) 0.091(4) Uani d . . . 1 . . H H3A 0.6703 0.6261 1.2771 0.137 Uiso calc U . . 1 . . H H3B 0.6195 0.5322 1.2502 0.137 Uiso calc U . . 1 . . H H3C 0.6196 0.5582 1.3264 0.137 Uiso calc U . . 1 . . C C4 0.4968(15) 0.6884(14) 1.3247(7) 0.091(4) Uani d . . . 1 . . H H4A 0.4886 0.6481 1.3626 0.137 Uiso calc U . . 1 . . H H4B 0.4353 0.7182 1.3109 0.137 Uiso calc U . . 1 . . H H4C 0.545 0.7364 1.3367 0.137 Uiso calc U . . 1 . . C C5 0.4648(7) 0.9378(6) 1.1711(4) 0.0282(19) Uani d . . . 1 . . C C6 0.4499(7) 1.0247(7) 1.2096(5) 0.034(2) Uani d . . . 1 . . H H6 0.5033 1.0299 1.2448 0.04 Uiso calc U . R 1 . . C C7 0.3551(9) 1.0229(8) 1.2414(5) 0.049(3) Uani d . . . 1 . . H H7A 0.3018 1.0212 1.2073 0.074 Uiso calc U . . 1 . . H H7B 0.3496 1.0789 1.2683 0.074 Uiso calc U . . 1 . . H H7C 0.3524 0.9675 1.2692 0.074 Uiso calc U . . 1 . . C C8 0.4544(11) 1.1082(8) 1.1645(7) 0.062(4) Uani d . . . 1 . . H H8A 0.5203 1.1156 1.1514 0.093 Uiso calc U . . 1 . . H H8B 0.4352 1.1643 1.1875 0.093 Uiso calc U . . 1 . . H H8C 0.4104 1.0985 1.1254 0.093 Uiso calc U . . 1 . . C C9 0.4473(6) 0.9177(6) 0.9668(4) 0.0243(18) Uani d . . . 1 . . C C10 0.4056(7) 1.0143(6) 0.9569(5) 0.030(2) Uani d . . . 1 . . H H10 0.4047 1.0459 1.0005 0.035 Uiso calc U . R 1 . . C C11 0.4662(9) 1.0718(8) 0.9124(6) 0.050(3) Uani d . . . 1 . . H H11A 0.534 1.0695 0.929 0.074 Uiso calc U . . 1 . . H H11B 0.4439 1.1366 0.9117 0.074 Uiso calc U . . 1 . . H H11C 0.4595 1.0463 0.8678 0.074 Uiso calc U . . 1 . . C C12 0.3009(8) 1.0037(8) 0.9266(5) 0.041(2) Uani d . . . 1 . . H H12A 0.3016 0.9767 0.8826 0.061 Uiso calc U . . 1 . . H H12B 0.2699 1.0651 0.9237 0.061 Uiso calc U . . 1 . . H H12C 0.2648 0.9627 0.9543 0.061 Uiso calc U . . 1 . . C C13 0.6664(7) 0.8093(6) 1.0110(4) 0.0251(19) Uani d . . . 1 . . C C14 0.7684(10) 0.8415(12) 1.0024(8) 0.069(2) Uani d . . . 1 . . H H14 0.7801 0.89 1.0372 0.083 Uiso calc U . R 1 . . C C15 0.8329(10) 0.7593(13) 1.0275(8) 0.069(2) Uani d . . . 1 . . H H15A 0.7926 0.71 1.0443 0.104 Uiso calc U . . 1 . . H H15B 0.8791 0.781 1.0627 0.104 Uiso calc U . . 1 . . H H15C 0.8679 0.7347 0.9913 0.104 Uiso calc U . . 1 . . C C16 0.7681(10) 0.8980(12) 0.9375(8) 0.069(2) Uani d . . . 1 . . H H16A 0.8335 0.9199 0.9313 0.104 Uiso calc U . . 1 . . H H16B 0.7248 0.9516 0.9397 0.104 Uiso calc U . . 1 . . H H16C 0.7458 0.858 0.9006 0.104 Uiso calc U . . 1 . . C C17 0.5453(6) 0.5982(6) 1.0169(5) 0.0243(19) Uani d . . . 1 . . C C18 0.5795(7) 0.5067(6) 1.0453(5) 0.029(2) Uani d . . . 1 . . H H18 0.5905 0.4627 1.0087 0.035 Uiso calc U . R 1 . . C C19 0.5042(9) 0.4652(8) 1.0875(6) 0.052(3) Uani d . . . 1 . . H H19A 0.5 0.5031 1.127 0.078 Uiso calc U . . 1 . . H H19B 0.5228 0.4014 1.1 0.078 Uiso calc U . . 1 . . H H19C 0.4414 0.4643 1.0625 0.078 Uiso calc U . . 1 . . C C20 0.6739(8) 0.5210(7) 1.0864(5) 0.040(2) Uani d . . . 1 . . H H20A 0.7198 0.5534 1.0602 0.059 Uiso calc U . . 1 . . H H20B 0.7005 0.4604 1.1004 0.059 Uiso calc U . . 1 . . H H20C 0.6623 0.5585 1.1251 0.059 Uiso calc U . . 1 . . C C21 0.3289(7) 0.7147(6) 1.0057(5) 0.024(2) Uani d . . . 1 . . C C22 0.2269(9) 0.6760(9) 0.9961(6) 0.0493(16) Uani d . . . 1 . . H H22 0.2166 0.6426 0.9532 0.059 Uiso calc U . R 1 . . C C23 0.1589(9) 0.7571(9) 0.9994(6) 0.0493(16) Uani d . . . 1 . . H H23A 0.1755 0.793 1.0394 0.074 Uiso calc U . . 1 . . H H23B 0.0927 0.7339 0.9999 0.074 Uiso calc U . . 1 . . H H23C 0.1642 0.797 0.9609 0.074 Uiso calc U . . 1 . . C C24 0.2037(8) 0.6131(9) 1.0528(6) 0.0493(16) Uani d . . . 1 . . H H24A 0.2595 0.5737 1.0653 0.074 Uiso calc U . . 1 . . H H24B 0.1483 0.5737 1.0392 0.074 Uiso calc U . . 1 . . H H24C 0.1884 0.6515 1.0903 0.074 Uiso calc U . . 1 . . C C25 0.6311(7) 0.7401(6) 0.8136(5) 0.029(2) Uani d . . . 1 . . C C26 0.7057(7) 0.7458(7) 0.7649(5) 0.033(2) Uani d . . . 1 . . H H26 0.766 0.7161 0.7847 0.039 Uiso calc U . R 1 . . C C27 0.7290(8) 0.8456(8) 0.7476(7) 0.048(3) Uani d . . . 1 . . H H27A 0.6724 0.8745 0.7246 0.072 Uiso calc U . . 1 . . H H27B 0.7829 0.8464 0.7193 0.072 Uiso calc U . . 1 . . H H27C 0.7468 0.8805 0.7879 0.072 Uiso calc U . . 1 . . C C28 0.6693(9) 0.6876(8) 0.7058(5) 0.045(3) Uani d . . . 1 . . H H28A 0.6526 0.6251 0.7204 0.067 Uiso calc U . . 1 . . H H28B 0.7198 0.6831 0.675 0.067 Uiso calc U . . 1 . . H H28C 0.6121 0.7173 0.6841 0.067 Uiso calc U . . 1 . . C C29 0.3668(8) 0.6802(10) 0.8085(5) 0.043(3) Uani d . . . 1 . . C C30 0.2871(9) 0.6468(11) 0.7614(5) 0.060(4) Uani d . . . 1 . . H H30 0.2576 0.7056 0.7428 0.072 Uiso calc U . R 1 . . C C31 0.2101(8) 0.6048(10) 0.7966(6) 0.053(3) Uani d . . . 1 . . H H31A 0.159 0.5823 0.765 0.08 Uiso calc U . . 1 . . H H31B 0.1836 0.6514 0.8253 0.08 Uiso calc U . . 1 . . H H31C 0.2361 0.5524 0.8231 0.08 Uiso calc U . . 1 . . C C32 0.3207(11) 0.6002(15) 0.7054(7) 0.081(5) Uani d . . . 1 . . H H32A 0.3435 0.5378 0.7182 0.122 Uiso calc U . . 1 . . H H32B 0.3737 0.6359 0.6886 0.122 Uiso calc U . . 1 . . H H32C 0.2679 0.5951 0.6712 0.122 Uiso calc U . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hf1 0.0246(2) 0.02493(15) 0.01555(18) 0.00117(14) -0.00122(13) -0.00317(14) Hf2 0.0242(2) 0.02406(15) 0.01517(18) 0.00009(15) 0.00004(13) -0.00239(14) O1 0.057(7) 0.101(8) 0.045(6) 0.005(5) 0.009(5) 0.040(5) O2 0.061(7) 0.068(6) 0.042(6) 0.002(5) -0.029(5) 0.009(4) O3 0.042(4) 0.055(5) 0.057(5) -0.015(4) 0.022(4) -0.034(4) O4 0.027(4) 0.047(4) 0.050(5) 0.004(3) -0.007(3) -0.027(4) O5 0.035(4) 0.032(3) 0.022(4) 0.006(3) -0.001(3) 0.002(3) O6 0.029(4) 0.037(3) 0.020(3) -0.001(3) 0.001(3) -0.005(3) O7 0.042(4) 0.021(3) 0.022(3) 0.007(3) 0.000(3) -0.006(2) O8 0.028(4) 0.037(3) 0.034(4) -0.004(3) 0.000(3) -0.017(3) O9 0.039(4) 0.026(3) 0.022(3) -0.002(3) 0.003(3) 0.003(2) O10 0.029(4) 0.045(4) 0.023(4) -0.001(3) 0.005(3) 0.003(3) O11 0.026(4) 0.034(4) 0.021(4) -0.006(3) -0.001(3) 0.000(3) O12 0.047(4) 0.026(3) 0.020(3) 0.006(3) 0.000(3) 0.001(3) O13 0.043(4) 0.036(4) 0.031(4) 0.010(3) 0.019(3) 0.008(3) O14 0.046(4) 0.031(3) 0.039(4) 0.008(3) 0.017(3) 0.002(3) O15 0.064(6) 0.058(6) 0.031(5) -0.017(4) -0.021(4) 0.009(4) O16 0.061(6) 0.054(5) 0.054(5) -0.010(4) 0.002(4) -0.031(4) C1 0.064(8) 0.035(5) 0.030(6) 0.011(5) 0.022(6) 0.001(4) C2 0.130(9) 0.114(8) 0.030(4) 0.060(7) 0.016(5) 0.018(5) C3 0.130(9) 0.114(8) 0.030(4) 0.060(7) 0.016(5) 0.018(5) C4 0.130(9) 0.114(8) 0.030(4) 0.060(7) 0.016(5) 0.018(5) C5 0.035(5) 0.033(5) 0.016(4) 0.000(4) -0.004(4) -0.007(4) C6 0.030(5) 0.040(5) 0.030(5) 0.004(4) -0.002(4) -0.012(4) C7 0.058(7) 0.058(7) 0.033(6) 0.008(6) 0.007(5) -0.024(5) C8 0.094(11) 0.034(6) 0.057(7) -0.002(6) -0.002(7) -0.007(6) C9 0.025(5) 0.029(4) 0.019(4) 0.002(3) 0.000(3) -0.001(3) C10 0.034(5) 0.025(4) 0.029(5) 0.008(4) 0.000(4) -0.003(4) C11 0.051(7) 0.039(6) 0.059(8) -0.010(5) 0.005(5) 0.012(5) C12 0.035(6) 0.047(6) 0.039(6) 0.012(5) 0.002(4) 0.003(5) C13 0.028(5) 0.023(4) 0.023(5) 0.003(4) -0.009(4) -0.011(4) C14 0.044(5) 0.093(6) 0.072(5) -0.017(4) 0.005(4) -0.007(5) C15 0.044(5) 0.093(6) 0.072(5) -0.017(4) 0.005(4) -0.007(5) C16 0.044(5) 0.093(6) 0.072(5) -0.017(4) 0.005(4) -0.007(5) C17 0.019(5) 0.026(4) 0.028(5) -0.002(3) 0.000(4) 0.000(4) C18 0.038(6) 0.021(4) 0.029(5) 0.003(4) 0.001(4) -0.001(4) C19 0.046(7) 0.041(5) 0.069(9) -0.007(5) -0.002(6) 0.017(6) C20 0.033(6) 0.042(5) 0.044(6) 0.005(4) 0.000(4) 0.004(5) C21 0.028(5) 0.023(4) 0.020(5) 0.001(3) 0.001(4) 0.000(3) C22 0.034(4) 0.064(4) 0.050(4) -0.009(3) 0.000(3) -0.008(3) C23 0.034(4) 0.064(4) 0.050(4) -0.009(3) 0.000(3) -0.008(3) C24 0.034(4) 0.064(4) 0.050(4) -0.009(3) 0.000(3) -0.008(3) C25 0.036(5) 0.033(5) 0.018(5) -0.003(4) 0.003(4) -0.003(4) C26 0.033(6) 0.039(5) 0.027(5) 0.001(4) 0.010(4) -0.009(4) C27 0.044(8) 0.047(6) 0.056(6) -0.002(5) 0.023(6) -0.001(5) C28 0.057(7) 0.049(6) 0.030(5) -0.007(5) 0.015(5) -0.019(5) C29 0.037(6) 0.077(8) 0.016(5) 0.002(6) -0.002(4) 0.000(5) C30 0.048(7) 0.105(11) 0.027(6) -0.024(7) -0.001(5) -0.011(6) C31 0.034(7) 0.083(9) 0.041(6) -0.002(6) -0.006(5) -0.006(6) C32 0.054(9) 0.144(16) 0.043(8) -0.005(9) -0.008(6) -0.037(9) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hf1 O7 . 2.111(5) ? Hf1 O5 . 2.119(6) ? Hf1 O6 . 2.163(6) ? Hf1 O8 . 2.167(7) ? Hf1 O4 . 2.203(7) ? Hf1 O1 . 2.211(9) ? Hf1 O3 . 2.222(7) ? Hf1 O2 . 2.239(9) ? Hf1 C5 . 2.611(9) ? Hf1 C1 . 2.625(11) ? Hf2 O11 . 2.123(7) ? Hf2 O10 . 2.128(7) ? Hf2 O12 . 2.135(6) ? Hf2 O9 . 2.163(6) ? Hf2 O16 . 2.195(8) ? Hf2 O13 . 2.196(7) ? Hf2 O14 . 2.229(7) ? Hf2 O15 . 2.241(10) ? Hf2 C29 . 2.599(11) ? Hf2 C25 . 2.616(10) ? O1 C1 . 1.198(15) ? O2 C1 . 1.276(16) ? O3 C5 . 1.260(12) ? O4 C5 . 1.273(12) ? O5 C9 . 1.267(10) ? O6 C13 . 1.248(11) ? O7 C17 . 1.260(11) ? O8 C21 . 1.251(12) ? O9 C17 . 1.263(11) ? O10 C21 . 1.267(12) ? O11 C13 . 1.276(11) ? O12 C9 . 1.262(10) ? O13 C25 . 1.270(12) ? O14 C25 . 1.273(11) ? O15 C29 . 1.221(16) ? O16 C29 . 1.268(15) ? C1 C2 . 1.499(17) ? C2 C3 . 1.39(2) ? C2 C4 . 1.50(2) ? C2 H2 . 1.0 ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 H4A . 0.98 ? C4 H4B . 0.98 ? C4 H4C . 0.98 ? C5 C6 . 1.497(12) ? C6 C7 . 1.513(15) ? C6 C8 . 1.515(16) ? C6 H6 . 1.0 ? C7 H7A . 0.98 ? C7 H7B . 0.98 ? C7 H7C . 0.98 ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 C10 . 1.510(12) ? C10 C11 . 1.527(14) ? C10 C12 . 1.549(15) ? C10 H10 . 1.0 ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? C12 H12A . 0.98 ? C12 H12B . 0.98 ? C12 H12C . 0.98 ? C13 C14 . 1.515(17) ? C14 C15 . 1.55(2) ? C14 C16 . 1.55(2) ? C14 H14 . 1.0 ? C15 H15A . 0.98 ? C15 H15B . 0.98 ? C15 H15C . 0.98 ? C16 H16A . 0.98 ? C16 H16B . 0.98 ? C16 H16C . 0.98 ? C17 C18 . 1.500(12) ? C18 C20 . 1.521(15) ? C18 C19 . 1.526(15) ? C18 H18 . 1.0 ? C19 H19A . 0.98 ? C19 H19B . 0.98 ? C19 H19C . 0.98 ? C20 H20A . 0.98 ? C20 H20B . 0.98 ? C20 H20C . 0.98 ? C21 C22 . 1.524(15) ? C22 C23 . 1.504(18) ? C22 C24 . 1.521(18) ? C22 H22 . 1.0 ? C23 H23A . 0.98 ? C23 H23B . 0.98 ? C23 H23C . 0.98 ? C24 H24A . 0.98 ? C24 H24B . 0.98 ? C24 H24C . 0.98 ? C25 C26 . 1.493(13) ? C26 C27 . 1.516(15) ? C26 C28 . 1.523(14) ? C26 H26 . 1.0 ? C27 H27A . 0.98 ? C27 H27B . 0.98 ? C27 H27C . 0.98 ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 C30 . 1.495(15) ? C30 C32 . 1.433(18) ? C30 C31 . 1.463(17) ? C30 H30 . 1.0 ? C31 H31A . 0.98 ? C31 H31B . 0.98 ? C31 H31C . 0.98 ? C32 H32A . 0.98 ? C32 H32B . 0.98 ? C32 H32C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O7 Hf1 O5 . . 106.9(2) ? O7 Hf1 O6 . . 78.0(3) ? O5 Hf1 O6 . . 77.9(3) ? O7 Hf1 O8 . . 77.6(3) ? O5 Hf1 O8 . . 77.8(3) ? O6 Hf1 O8 . . 138.5(2) ? O7 Hf1 O4 . . 149.5(3) ? O5 Hf1 O4 . . 82.6(3) ? O6 Hf1 O4 . . 75.8(3) ? O8 Hf1 O4 . . 132.9(3) ? O7 Hf1 O1 . . 83.8(4) ? O5 Hf1 O1 . . 149.1(3) ? O6 Hf1 O1 . . 133.1(3) ? O8 Hf1 O1 . . 76.4(4) ? O4 Hf1 O1 . . 103.0(4) ? O7 Hf1 O3 . . 150.7(3) ? O5 Hf1 O3 . . 81.5(3) ? O6 Hf1 O3 . . 131.2(3) ? O8 Hf1 O3 . . 76.9(3) ? O4 Hf1 O3 . . 57.9(3) ? O1 Hf1 O3 . . 76.3(4) ? O7 Hf1 O2 . . 81.8(3) ? O5 Hf1 O2 . . 152.5(3) ? O6 Hf1 O2 . . 78.6(3) ? O8 Hf1 O2 . . 129.7(3) ? O4 Hf1 O2 . . 78.0(3) ? O1 Hf1 O2 . . 56.0(4) ? O3 Hf1 O2 . . 103.9(4) ? O7 Hf1 C5 . . 172.5(3) ? O5 Hf1 C5 . . 80.6(3) ? O6 Hf1 C5 . . 103.7(3) ? O8 Hf1 C5 . . 104.8(3) ? O4 Hf1 C5 . . 29.1(3) ? O1 Hf1 C5 . . 89.8(4) ? O3 Hf1 C5 . . 28.8(3) ? O2 Hf1 C5 . . 91.4(3) ? O7 Hf1 C1 . . 81.9(3) ? O5 Hf1 C1 . . 170.8(3) ? O6 Hf1 C1 . . 106.9(3) ? O8 Hf1 C1 . . 102.2(4) ? O4 Hf1 C1 . . 91.0(3) ? O1 Hf1 C1 . . 27.0(4) ? O3 Hf1 C1 . . 89.5(3) ? O2 Hf1 C1 . . 29.0(4) ? C5 Hf1 C1 . . 90.6(3) ? O11 Hf2 O10 . . 107.4(3) ? O11 Hf2 O12 . . 77.3(3) ? O10 Hf2 O12 . . 78.1(3) ? O11 Hf2 O9 . . 78.3(3) ? O10 Hf2 O9 . . 77.0(3) ? O12 Hf2 O9 . . 137.8(2) ? O11 Hf2 O16 . . 152.1(3) ? O10 Hf2 O16 . . 85.0(3) ? O12 Hf2 O16 . . 130.4(3) ? O9 Hf2 O16 . . 80.4(3) ? O11 Hf2 O13 . . 84.7(3) ? O10 Hf2 O13 . . 150.4(3) ? O12 Hf2 O13 . . 78.5(2) ? O9 Hf2 O13 . . 132.5(3) ? O16 Hf2 O13 . . 96.7(3) ? O11 Hf2 O14 . . 79.0(3) ? O10 Hf2 O14 . . 149.5(3) ? O12 Hf2 O14 . . 131.9(3) ? O9 Hf2 O14 . . 75.3(3) ? O16 Hf2 O14 . . 78.2(3) ? O13 Hf2 O14 . . 58.0(3) ? O11 Hf2 O15 . . 148.4(3) ? O10 Hf2 O15 . . 79.3(3) ? O12 Hf2 O15 . . 73.9(3) ? O9 Hf2 O15 . . 132.7(3) ? O16 Hf2 O15 . . 57.1(3) ? O13 Hf2 O15 . . 77.1(3) ? O14 Hf2 O15 . . 111.2(3) ? O11 Hf2 C29 . . 171.9(3) ? O10 Hf2 C29 . . 80.0(3) ? O12 Hf2 C29 . . 101.5(3) ? O9 Hf2 C29 . . 107.1(4) ? O16 Hf2 C29 . . 29.1(4) ? O13 Hf2 C29 . . 87.2(3) ? O14 Hf2 C29 . . 96.3(3) ? O15 Hf2 C29 . . 28.0(4) ? O11 Hf2 C25 . . 80.1(3) ? O10 Hf2 C25 . . 172.4(3) ? O12 Hf2 C25 . . 105.2(3) ? O9 Hf2 C25 . . 103.9(3) ? O16 Hf2 C25 . . 87.7(3) ? O13 Hf2 C25 . . 29.0(3) ? O14 Hf2 C25 . . 29.1(3) ? O15 Hf2 C25 . . 95.0(3) ? C29 Hf2 C25 . . 92.6(3) ? C1 O1 Hf1 . . 96.1(8) ? C1 O2 Hf1 . . 92.5(8) ? C5 O3 Hf1 . . 93.0(6) ? C5 O4 Hf1 . . 93.5(5) ? C9 O5 Hf1 . . 158.4(6) ? C13 O6 Hf1 . . 130.3(6) ? C17 O7 Hf1 . . 165.0(6) ? C21 O8 Hf1 . . 129.6(6) ? C17 O9 Hf2 . . 128.1(6) ? C21 O10 Hf2 . . 160.9(7) ? C13 O11 Hf2 . . 161.3(7) ? C9 O12 Hf2 . . 134.0(6) ? C25 O13 Hf2 . . 94.2(6) ? C25 O14 Hf2 . . 92.6(6) ? C29 O15 Hf2 . . 92.6(7) ? C29 O16 Hf2 . . 93.4(7) ? O1 C1 O2 . . 115.3(10) ? O1 C1 C2 . . 121.5(13) ? O2 C1 C2 . . 123.2(13) ? O1 C1 Hf1 . . 56.9(6) ? O2 C1 Hf1 . . 58.4(6) ? C2 C1 Hf1 . . 178.2(10) ? C3 C2 C4 . . 116.3(15) ? C3 C2 C1 . . 116.8(14) ? C4 C2 C1 . . 108.3(13) ? C3 C2 H2 . . 104.6 ? C4 C2 H2 . . 104.6 ? C1 C2 H2 . . 104.6 ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C2 C4 H4A . . 109.5 ? C2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? O3 C5 O4 . . 115.6(8) ? O3 C5 C6 . . 123.6(9) ? O4 C5 C6 . . 120.8(8) ? O3 C5 Hf1 . . 58.2(5) ? O4 C5 Hf1 . . 57.4(5) ? C6 C5 Hf1 . . 177.6(7) ? C5 C6 C7 . . 111.8(8) ? C5 C6 C8 . . 109.0(8) ? C7 C6 C8 . . 110.5(9) ? C5 C6 H6 . . 108.5 ? C7 C6 H6 . . 108.5 ? C8 C6 H6 . . 108.5 ? C6 C7 H7A . . 109.5 ? C6 C7 H7B . . 109.5 ? H7A C7 H7B . . 109.5 ? C6 C7 H7C . . 109.5 ? H7A C7 H7C . . 109.5 ? H7B C7 H7C . . 109.5 ? C6 C8 H8A . . 109.5 ? C6 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C6 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? O12 C9 O5 . . 123.9(8) ? O12 C9 C10 . . 116.8(8) ? O5 C9 C10 . . 119.3(8) ? C9 C10 C11 . . 110.7(8) ? C9 C10 C12 . . 107.7(8) ? C11 C10 C12 . . 111.0(8) ? C9 C10 H10 . . 109.2 ? C11 C10 H10 . . 109.2 ? C12 C10 H10 . . 109.2 ? C10 C11 H11A . . 109.5 ? C10 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C10 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C10 C12 H12A . . 109.5 ? C10 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C10 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? O6 C13 O11 . . 125.2(9) ? O6 C13 C14 . . 117.1(9) ? O11 C13 C14 . . 117.7(10) ? C13 C14 C15 . . 104.8(12) ? C13 C14 C16 . . 108.3(11) ? C15 C14 C16 . . 130.2(14) ? C13 C14 H14 . . 103.6 ? C15 C14 H14 . . 103.6 ? C16 C14 H14 . . 103.6 ? C14 C15 H15A . . 109.5 ? C14 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C14 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? C14 C16 H16A . . 109.5 ? C14 C16 H16B . . 109.5 ? H16A C16 H16B . . 109.5 ? C14 C16 H16C . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? O7 C17 O9 . . 124.2(8) ? O7 C17 C18 . . 117.6(8) ? O9 C17 C18 . . 118.2(8) ? C17 C18 C20 . . 109.4(8) ? C17 C18 C19 . . 110.4(8) ? C20 C18 C19 . . 110.0(9) ? C17 C18 H18 . . 109.0 ? C20 C18 H18 . . 109.0 ? C19 C18 H18 . . 109.0 ? C18 C19 H19A . . 109.5 ? C18 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C18 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? C18 C20 H20A . . 109.5 ? C18 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C18 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? O8 C21 O10 . . 125.7(9) ? O8 C21 C22 . . 116.8(9) ? O10 C21 C22 . . 117.5(9) ? C23 C22 C24 . . 104.8(10) ? C23 C22 C21 . . 107.2(10) ? C24 C22 C21 . . 111.5(10) ? C23 C22 H22 . . 111.0 ? C24 C22 H22 . . 111.0 ? C21 C22 H22 . . 111.0 ? C22 C23 H23A . . 109.5 ? C22 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? C22 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? C22 C24 H24A . . 109.5 ? C22 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C22 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? O13 C25 O14 . . 115.1(9) ? O13 C25 C26 . . 122.9(9) ? O14 C25 C26 . . 121.9(9) ? O13 C25 Hf2 . . 56.9(5) ? O14 C25 Hf2 . . 58.3(5) ? C26 C25 Hf2 . . 179.5(7) ? C25 C26 C27 . . 112.2(8) ? C25 C26 C28 . . 106.9(8) ? C27 C26 C28 . . 113.4(9) ? C25 C26 H26 . . 108.0 ? C27 C26 H26 . . 108.0 ? C28 C26 H26 . . 108.0 ? C26 C27 H27A . . 109.5 ? C26 C27 H27B . . 109.5 ? H27A C27 H27B . . 109.5 ? C26 C27 H27C . . 109.5 ? H27A C27 H27C . . 109.5 ? H27B C27 H27C . . 109.5 ? C26 C28 H28A . . 109.5 ? C26 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C26 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? O15 C29 O16 . . 116.8(10) ? O15 C29 C30 . . 122.6(12) ? O16 C29 C30 . . 120.6(13) ? O15 C29 Hf2 . . 59.5(6) ? O16 C29 Hf2 . . 57.4(5) ? C30 C29 Hf2 . . 175.1(8) ? C32 C30 C31 . . 119.6(13) ? C32 C30 C29 . . 113.2(11) ? C31 C30 C29 . . 110.5(9) ? C32 C30 H30 . . 103.9 ? C31 C30 H30 . . 103.9 ? C29 C30 H30 . . 103.9 ? C30 C31 H31A . . 109.5 ? C30 C31 H31B . . 109.5 ? H31A C31 H31B . . 109.5 ? C30 C31 H31C . . 109.5 ? H31A C31 H31C . . 109.5 ? H31B C31 H31C . . 109.5 ? C30 C32 H32A . . 109.5 ? C30 C32 H32B . . 109.5 ? H32A C32 H32B . . 109.5 ? C30 C32 H32C . . 109.5 ? H32A C32 H32C . . 109.5 ? H32B C32 H32C . . 109.5 ? 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_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion _geom_torsion_publ_flag Hf1 O1 C1 O2 . . . . -0.1(12) ? Hf1 O1 C1 C2 . . . . 179.2(11) ? Hf1 O2 C1 O1 . . . . 0.1(11) ? Hf1 O2 C1 C2 . . . . -179.2(11) ? O1 C1 C2 C3 . . . . 149.6(17) ? O2 C1 C2 C3 . . . . -31.(2) ? O1 C1 C2 C4 . . . . -77.(2) ? O2 C1 C2 C4 . . . . 102.6(18) ? Hf1 O3 C5 O4 . . . . -1.1(9) ? Hf1 O3 C5 C6 . . . . 178.2(8) ? Hf1 O4 C5 O3 . . . . 1.1(9) ? Hf1 O4 C5 C6 . . . . -178.2(8) ? O3 C5 C6 C7 . . . . 19.1(14) ? O4 C5 C6 C7 . . . . -161.6(9) ? O3 C5 C6 C8 . . . . -103.3(12) ? O4 C5 C6 C8 . . . . 76.0(12) ? Hf2 O12 C9 O5 . . . . 6.4(14) ? Hf2 O12 C9 C10 . . . . -172.3(6) ? Hf1 O5 C9 O12 . . . . -19.(2) ? Hf1 O5 C9 C10 . . . . 159.9(13) ? O12 C9 C10 C11 . . . . -55.4(12) ? O5 C9 C10 C11 . . . . 125.7(10) ? O12 C9 C10 C12 . . . . 66.0(11) ? O5 C9 C10 C12 . . . . -112.8(9) ? Hf1 O6 C13 O11 . . . . -7.4(14) ? Hf1 O6 C13 C14 . . . . 172.8(9) ? Hf2 O11 C13 O6 . . . . 7.(3) ? Hf2 O11 C13 C14 . . . . -173.1(16) ? O6 C13 C14 C15 . . . . 78.9(14) ? O11 C13 C14 C15 . . . . -100.9(13) ? O6 C13 C14 C16 . . . . -138.9(11) ? O11 C13 C14 C16 . . . . 41.3(16) ? Hf1 O7 C17 O9 . . . . -20.(3) ? Hf1 O7 C17 C18 . . . . 160.(2) ? Hf2 O9 C17 O7 . . . . 3.9(13) ? Hf2 O9 C17 C18 . . . . -176.4(6) ? O7 C17 C18 C20 . . . . -62.9(11) ? O9 C17 C18 C20 . . . . 117.4(9) ? O7 C17 C18 C19 . . . . 58.3(12) ? O9 C17 C18 C19 . . . . -121.4(9) ? Hf1 O8 C21 O10 . . . . -10.7(14) ? Hf1 O8 C21 C22 . . . . 170.1(7) ? Hf2 O10 C21 O8 . . . . 0.(3) ? Hf2 O10 C21 C22 . . . . 179.1(16) ? O8 C21 C22 C23 . . . . 67.8(12) ? O10 C21 C22 C23 . . . . -111.5(11) ? O8 C21 C22 C24 . . . . -46.4(13) ? O10 C21 C22 C24 . . . . 134.3(10) ? Hf2 O13 C25 O14 . . . . 2.0(9) ? Hf2 O13 C25 C26 . . . . 179.4(8) ? Hf2 O14 C25 O13 . . . . -2.0(9) ? Hf2 O14 C25 C26 . . . . -179.4(8) ? O13 C25 C26 C27 . . . . 25.5(14) ? O14 C25 C26 C27 . . . . -157.3(10) ? O13 C25 C26 C28 . . . . -99.5(11) ? O14 C25 C26 C28 . . . . 77.7(12) ? Hf2 O15 C29 O16 . . . . -3.4(10) ? Hf2 O15 C29 C30 . . . . 174.8(9) ? Hf2 O16 C29 O15 . . . . 3.5(11) ? Hf2 O16 C29 C30 . . . . -174.8(8) ? O15 C29 C30 C32 . . . . 122.8(15) ? O16 C29 C30 C32 . . . . -59.0(17) ? O15 C29 C30 C31 . . . . -100.0(15) ? O16 C29 C30 C31 . . . . 78.2(15) ? #===END data_6 _audit_creation_method 'APEX2 v2014.5-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common 'HfOBut OBc 1:4' _chemical_formula_moiety ? _chemical_formula_sum 'C40 H71 Hf2 O16' _chemical_formula_iupac ? _chemical_formula_weight 1164.94 _chemical_melting_point ? _space_group_crystal_system monoclinic _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.148(5) _cell_length_b 20.579(6) _cell_length_c 21.896(7) _cell_angle_alpha 90 _cell_angle_beta 110.520(2) _cell_angle_gamma 90 _cell_volume 6815.(4) _cell_formula_units_Z 4 _cell_measurement_reflns_used 5585 _cell_measurement_theta_min 2.1754 _cell_measurement_theta_max 21.8580 _cell_measurement_temperature 193.(2) _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.284 _exptl_crystal_size_mid 0.225 _exptl_crystal_size_min 0.110 _exptl_crystal_density_diffrn 1.135 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2332 _exptl_absorpt_coefficient_mu 3.089 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2012/1 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.47 _exptl_absorpt_correction_T_max 0.73 _exptl_special_details ; ; _diffrn_ambient_temperature 193.(2) _diffrn_source 'fine-focus tube' _diffrn_source_type ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean 8.3660 _diffrn_reflns_number 35654 _diffrn_reflns_av_R_equivalents 0.1192 _diffrn_reflns_av_unetI/netI 0.1936 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 25.33 _diffrn_reflns_theta_full 25.33 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measured_fraction_theta_full 0.972 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 24 _refine_special_details ; ; _reflns_number_total 12119 _reflns_number_gt 4914 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.1414 _refine_ls_R_factor_gt 0.0615 _refine_ls_wR_factor_gt 0.1343 _refine_ls_wR_factor_ref 0.1639 _refine_ls_goodness_of_fit_ref 0.794 _refine_ls_restrained_S_all 0.794 _refine_ls_number_reflns 12119 _refine_ls_number_parameters 536 _refine_ls_number_restraints 13 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0555P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.922 _refine_diff_density_min -1.101 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 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' _computing_data_collection ? _computing_cell_refinement 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_data_reduction 'SAINT V8.34A (Bruker AXS Inc., 2013)' _computing_structure_solution 'Bruker XT Intrinsic Solution Method' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf1 1.02938(3) 0.78161(3) 0.19717(3) 0.04859(18) Uani d . . . 1.0 . . Hf Hf2 0.75764(4) 0.80155(3) 0.17035(3) 0.05248(19) Uani d . . . 1.0 . . O O1 1.1397(6) 0.7679(5) 0.2927(5) 0.078(3) Uani d . . . 1.0 . . O O2 1.1146(6) 0.6924(5) 0.2196(5) 0.082(3) Uani d . . . 1.0 . . O O3 1.1267(6) 0.8564(5) 0.1947(4) 0.073(3) Uani d . . . 1.0 . . O O4 1.0903(6) 0.7835(5) 0.1201(5) 0.070(3) Uani d . . . 1.0 . . O O5 0.9358(5) 0.8442(4) 0.1292(4) 0.057(2) Uani d . . . 1.0 . . O O6 0.9512(5) 0.7138(4) 0.1249(4) 0.059(3) Uani d . . . 1.0 . . O O7 0.9576(5) 0.7312(4) 0.2473(4) 0.057(2) Uani d . . . 1.0 . . O O8 1.0086(5) 0.8558(4) 0.2572(4) 0.055(2) Uani d . . . 1.0 . . O O9 0.8630(5) 0.8507(4) 0.2392(4) 0.061(3) Uani d . . . 1.0 . . O O10 0.8175(5) 0.7257(4) 0.2402(4) 0.056(2) Uani d . . . 1.0 . . O O11 0.8151(5) 0.7389(4) 0.1180(4) 0.054(2) Uani d . . . 1.0 . . O O12 0.7980(5) 0.8700(4) 0.1120(4) 0.053(2) Uani d . . . 1.0 . . O O13 0.6454(6) 0.8045(5) 0.0764(5) 0.091(4) Uani d . . . 1.0 . . O O14 0.6529(6) 0.7277(5) 0.1445(5) 0.086(3) Uani d . . . 1.0 . . O O15 0.6868(7) 0.8915(5) 0.1753(5) 0.085(4) Uani d . . . 1.0 . . O O16 0.6952(6) 0.8171(5) 0.2454(5) 0.078(3) Uani d . . . 1.0 . . C C1 1.1607(9) 0.7149(8) 0.2738(8) 0.062(4) Uani d . . . 1.0 . . C C2 1.2409(11) 0.6786(9) 0.3205(9) 0.086(5) Uani d . . . 1.0 . . C C3 1.2574(11) 0.6940(10) 0.3912(8) 0.117(7) Uani d . . . 1.0 . . H H3A 1.2549 0.7412 0.3966 0.176 Uiso calc U . . 1.0 . . H H3B 1.316 0.6779 0.4181 0.176 Uiso calc U . . 1.0 . . H H3C 1.2121 0.673 0.4046 0.176 Uiso calc U . . 1.0 . . C C4 1.3191(11) 0.7012(9) 0.3039(8) 0.116(7) Uani d . . . 1.0 . . H H4A 1.3262 0.6733 0.2699 0.174 Uiso calc U . . 1.0 . . H H4B 1.3726 0.699 0.3429 0.174 Uiso calc U . . 1.0 . . H H4C 1.3095 0.7461 0.2882 0.174 Uiso calc U . . 1.0 . . C C5 1.2316(13) 0.6088(11) 0.3067(10) 0.140(8) Uani d . . . 1.0 . . H H5A 1.1892 0.5903 0.3247 0.21 Uiso calc U . . 1.0 . . H H5B 1.2891 0.5876 0.3266 0.21 Uiso calc U . . 1.0 . . H H5C 1.2102 0.6019 0.2594 0.21 Uiso calc U . . 1.0 . . C C6 1.1388(9) 0.8326(8) 0.1467(8) 0.061(4) Uani d . . . 1.0 . . C C7 1.2070(9) 0.8582(8) 0.1186(6) 0.077(5) Uani d . . D 1.0 . . C C8 1.2925(10) 0.8205(8) 0.1572(9) 0.108(6) Uani d . . . 1.0 . . H H8A 1.2806 0.7737 0.1531 0.162 Uiso calc U . . 1.0 . . H H8B 1.312 0.833 0.2033 0.162 Uiso calc U . . 1.0 . . H H8C 1.339 0.831 0.1396 0.162 Uiso calc U . . 1.0 . . C C9 1.1741(11) 0.8470(9) 0.0402(6) 0.105(6) Uani d . . D 1.0 . . H H9A 1.1138 0.8638 0.02 0.158 Uiso calc U . . 1.0 . . H H9B 1.1747 0.8004 0.031 0.158 Uiso calc U . . 1.0 . . H H9C 1.2138 0.8699 0.0224 0.158 Uiso calc U . . 1.0 . . C C10 1.2220(10) 0.9297(8) 0.1342(8) 0.093(5) Uani d . . . 1.0 . . H H10A 1.2818 0.9416 0.1366 0.14 Uiso calc U . . 1.0 . . H H10B 1.2152 0.9386 0.1761 0.14 Uiso calc U . . 1.0 . . H H10C 1.1787 0.9552 0.0999 0.14 Uiso calc U . . 1.0 . . C C11 0.8685(9) 0.8781(7) 0.1010(6) 0.050(3) Uani d . . . 1.0 . . C C12 0.8688(10) 0.9277(8) 0.0516(8) 0.073(4) Uani d U . . 1.0 . . C C13 0.9400(15) 0.9206(12) 0.0288(13) 0.255(18) Uani d U . . 1.0 . . H H13A 0.9732 0.9576 0.0253 0.306 Uiso calc U . R 1.0 . . H H13B 0.9546 0.8789 0.017 0.306 Uiso calc U . R 1.0 . . C C14 0.8327(19) 0.9857(10) 0.0728(15) 0.229(15) Uani d . . . 1.0 . . H H14A 0.7685 0.9872 0.0503 0.344 Uiso calc U . . 1.0 . . H H14B 0.8595 1.0248 0.062 0.344 Uiso calc U . . 1.0 . . H H14C 0.8461 0.9837 0.12 0.344 Uiso calc U . . 1.0 . . C C15 0.7939(17) 0.9113(11) -0.0159(10) 0.174(10) Uani d . . . 1.0 . . H H15A 0.7997 0.9403 -0.0498 0.262 Uiso calc U . . 1.0 . . H H15B 0.7358 0.9175 -0.0121 0.262 Uiso calc U . . 1.0 . . H H15C 0.8 0.8661 -0.0277 0.262 Uiso calc U . . 1.0 . . C C16 0.8706(9) 0.7069(6) 0.1000(6) 0.047(3) Uani d . . . 1.0 . . C C17 0.8320(10) 0.6636(8) 0.0425(8) 0.077(4) Uani d U . . 1.0 . . C C18 0.9021(12) 0.6146(9) 0.0409(9) 0.133(8) Uani d . . . 1.0 . . H H18A 0.9056 0.6137 -0.0029 0.199 Uiso calc U . . 1.0 . . H H18B 0.8862 0.5713 0.0519 0.199 Uiso calc U . . 1.0 . . H H18C 0.9596 0.6273 0.0726 0.199 Uiso calc U . . 1.0 . . C C19 0.794(2) 0.7028(11) -0.0160(10) 0.251(18) Uani d U . . 1.0 . . H H19A 0.8095 0.6837 -0.0516 0.377 Uiso calc U . . 1.0 . . H H19B 0.8178 0.7471 -0.0075 0.377 Uiso calc U . . 1.0 . . H H19C 0.7297 0.704 -0.0283 0.377 Uiso calc U . . 1.0 . . C C20 0.7620(16) 0.6188(12) 0.0543(13) 0.220(14) Uani d . . . 1.0 . . H H20A 0.7043 0.6263 0.0203 0.33 Uiso calc U . . 1.0 . . H H20B 0.7582 0.6284 0.0971 0.33 Uiso calc U . . 1.0 . . H H20C 0.7792 0.5733 0.053 0.33 Uiso calc U . . 1.0 . . C C21 0.8953(8) 0.7062(6) 0.2641(6) 0.045(3) Uani d . . . 1.0 . . C C22 0.9183(11) 0.6513(8) 0.3115(9) 0.084(5) Uani d . . . 1.0 . . C C23 1.0017(16) 0.6594(11) 0.3640(9) 0.182(12) Uani d . . . 1.0 . . H H23A 1.0479 0.6356 0.3539 0.274 Uiso calc U . . 1.0 . . H H23B 0.997 0.6425 0.4045 0.274 Uiso calc U . . 1.0 . . H H23C 1.017 0.7056 0.3694 0.274 Uiso calc U . . 1.0 . . C C24 0.934(2) 0.5932(11) 0.2695(12) 0.206(13) Uani d . . . 1.0 . . H H24A 0.9206 0.6076 0.2244 0.309 Uiso calc U . . 1.0 . . H H24B 0.8952 0.5569 0.2704 0.309 Uiso calc U . . 1.0 . . H H24C 0.9958 0.5792 0.2878 0.309 Uiso calc U . . 1.0 . . C C25 0.8415(15) 0.6226(11) 0.3195(12) 0.183(11) Uani d . . . 1.0 . . H H25A 0.7924 0.6228 0.2776 0.274 Uiso calc U . . 1.0 . . H H25B 0.8249 0.6477 0.3515 0.274 Uiso calc U . . 1.0 . . H H25C 0.8548 0.5777 0.3348 0.274 Uiso calc U . . 1.0 . . C C26 0.9420(10) 0.8715(6) 0.2709(6) 0.049(3) Uani d . . D 1.0 . . C C31 0.6127(9) 0.7552(8) 0.0890(7) 0.063(4) Uani d . . . 1.0 . . C C32 0.5220(10) 0.7251(9) 0.0452(9) 0.093(6) Uani d . . . 1.0 . . C C33 0.5127(11) 0.7406(10) -0.0264(9) 0.126(7) Uani d . . . 1.0 . . H H33A 0.4505 0.737 -0.0546 0.189 Uiso calc U . . 1.0 . . H H33B 0.5482 0.7097 -0.0409 0.189 Uiso calc U . . 1.0 . . H H33C 0.5337 0.7849 -0.0289 0.189 Uiso calc U . . 1.0 . . C C34 0.5157(11) 0.6518(9) 0.0529(9) 0.114(7) Uani d . . . 1.0 . . H H34A 0.4567 0.6368 0.0256 0.172 Uiso calc U . . 1.0 . . H H34B 0.5258 0.6415 0.0986 0.172 Uiso calc U . . 1.0 . . H H34C 0.5605 0.6301 0.0394 0.172 Uiso calc U . . 1.0 . . C C35 0.4496(9) 0.7615(8) 0.0667(8) 0.093(6) Uani d . . . 1.0 . . H H35A 0.3911 0.7555 0.0331 0.139 Uiso calc U . . 1.0 . . H H35B 0.4636 0.8079 0.0722 0.139 Uiso calc U . . 1.0 . . H H35C 0.4495 0.7433 0.108 0.139 Uiso calc U . . 1.0 . . C C36 0.6652(9) 0.8743(8) 0.2221(9) 0.071(5) Uani d . . . 1.0 . . C C37 0.6076(11) 0.9077(8) 0.2529(8) 0.082(5) Uani d U . . 1.0 . . C C38 0.6232(12) 0.9813(9) 0.2459(10) 0.132(8) Uani d U . . 1.0 . . H H38A 0.6391 0.9884 0.2072 0.198 Uiso calc U . . 1.0 . . H H38B 0.6713 0.9965 0.2847 0.198 Uiso calc U . . 1.0 . . H H38C 0.569 1.0054 0.2414 0.198 Uiso calc U . . 1.0 . . C C39 0.6318(12) 0.8895(10) 0.3243(8) 0.122(7) Uani d . . . 1.0 . . H H39A 0.614 0.8445 0.3277 0.184 Uiso calc U . . 1.0 . . H H39B 0.6012 0.9185 0.3449 0.184 Uiso calc U . . 1.0 . . H H39C 0.6958 0.8937 0.3465 0.184 Uiso calc U . . 1.0 . . C C40 0.5119(11) 0.8880(10) 0.2118(10) 0.134(8) Uani d . . . 1.0 . . H H40A 0.5046 0.8886 0.1654 0.201 Uiso calc U . . 1.0 . . H H40B 0.4704 0.9187 0.2197 0.201 Uiso calc U . . 1.0 . . H H40C 0.5001 0.8441 0.2241 0.201 Uiso calc U . . 1.0 . . C C27 0.958(4) 0.911(3) 0.342(3) 0.077(4) Uani d . P . 0.356(18) A 1 C C28A 0.921(5) 0.905(5) 0.373(4) 0.122(7) Uani d . P . 0.356(18) A 1 H H28A 0.956 0.8806 0.4116 0.184 Uiso calc U P . 0.356 A 1 H H28B 0.8661 0.8816 0.3498 0.184 Uiso calc U P . 0.356 A 1 H H28C 0.9067 0.948 0.386 0.184 Uiso calc U P . 0.356 A 1 C C29A 1.0354(16) 0.9366(18) 0.3699(17) 0.152(17) Uani d . P D 0.644(18) A 1 H H29A 1.0293 0.9771 0.3914 0.227 Uiso calc U P . 0.644 A 1 H H29B 1.0627 0.9456 0.3373 0.227 Uiso calc U P . 0.644 A 1 H H29C 1.0727 0.9062 0.4025 0.227 Uiso calc U P . 0.644 A 1 C C30A 0.886(4) 0.978(3) 0.285(3) 0.133(8) Uani d . P . 0.356(18) A 1 H H30A 0.9031 0.9832 0.2469 0.199 Uiso calc U P . 0.356 A 1 H H30B 0.8958 1.0196 0.3094 0.199 Uiso calc U P . 0.356 A 1 H H30C 0.8236 0.9664 0.2719 0.199 Uiso calc U P . 0.356 A 1 C C28 0.997(4) 0.880(3) 0.401(3) 0.27(3) Uani d . P . 0.644(18) A 2 H H28D 1.0597 0.8717 0.4115 0.399 Uiso calc U P . 0.644 A 2 H H28E 0.9653 0.839 0.3992 0.399 Uiso calc U P . 0.644 A 2 H H28F 0.9883 0.908 0.4348 0.399 Uiso calc U P . 0.644 A 2 C C29 0.979(4) 0.976(2) 0.308(3) 0.090(11) Uani d U P . 0.356(18) A 2 H H29D 1.0301 0.9693 0.2943 0.136 Uiso calc U P . 0.356 A 2 H H29E 0.9961 1.0032 0.347 0.136 Uiso calc U P . 0.356 A 2 H H29F 0.9321 0.9984 0.2724 0.136 Uiso calc U P . 0.356 A 2 C C30 0.864(3) 0.925(2) 0.345(2) 0.17(2) Uani d . P . 0.644(18) A 2 H H30D 0.8572 0.8825 0.363 0.255 Uiso calc U P . 0.644 A 2 H H30F 0.8103 0.9356 0.3086 0.255 Uiso calc U P . 0.644 A 2 H H30E 0.8749 0.9582 0.3791 0.255 Uiso calc U P . 0.644 A 2 C C27A 0.9506(17) 0.9224(9) 0.3191(9) 0.073(4) Uani d U P D 0.644(18) A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hf1 0.0406(3) 0.0609(4) 0.0458(4) -0.0003(3) 0.0170(3) 0.0031(3) Hf2 0.0408(3) 0.0651(4) 0.0530(4) 0.0000(3) 0.0182(3) 0.0062(3) O1 0.053(6) 0.086(8) 0.067(7) 0.003(6) -0.014(5) -0.002(6) O2 0.066(7) 0.089(8) 0.076(8) 0.031(6) 0.007(6) -0.007(6) O3 0.060(6) 0.112(9) 0.049(6) -0.016(6) 0.023(5) -0.008(6) O4 0.077(7) 0.077(7) 0.077(7) -0.013(6) 0.052(6) -0.014(6) O5 0.051(6) 0.066(6) 0.058(6) 0.002(5) 0.024(5) 0.021(5) O6 0.035(5) 0.071(7) 0.070(6) -0.012(5) 0.017(5) -0.022(5) O7 0.045(5) 0.070(7) 0.060(6) 0.006(5) 0.023(5) 0.018(5) O8 0.058(6) 0.064(6) 0.053(6) -0.005(5) 0.034(5) -0.011(5) O9 0.046(6) 0.073(7) 0.058(6) -0.008(5) 0.011(5) -0.004(5) O10 0.048(6) 0.061(6) 0.056(6) 0.008(5) 0.014(5) 0.020(5) O11 0.052(6) 0.063(6) 0.049(6) -0.002(5) 0.021(5) -0.009(5) O12 0.049(6) 0.057(6) 0.055(6) -0.005(5) 0.019(5) 0.002(5) O13 0.066(7) 0.096(9) 0.086(8) -0.015(6) -0.004(6) 0.024(7) O14 0.063(7) 0.133(10) 0.055(7) -0.042(6) 0.013(5) 0.013(7) O15 0.087(8) 0.092(9) 0.087(9) 0.031(6) 0.044(7) 0.011(7) O16 0.078(7) 0.089(8) 0.098(8) -0.004(6) 0.067(7) -0.007(7) C1 0.036(8) 0.088(13) 0.072(12) 0.010(9) 0.033(8) 0.012(10) C2 0.058(11) 0.106(15) 0.095(15) 0.025(11) 0.027(10) 0.028(12) C3 0.104(15) 0.17(2) 0.056(12) -0.011(13) 0.001(10) 0.016(12) C4 0.079(13) 0.17(2) 0.091(14) 0.012(13) 0.022(11) 0.024(13) C5 0.126(18) 0.135(19) 0.129(18) 0.058(15) 0.007(14) 0.031(15) C6 0.034(8) 0.078(12) 0.070(12) 0.011(8) 0.016(8) 0.013(9) C7 0.056(10) 0.078(12) 0.111(14) 0.003(9) 0.045(10) 0.016(10) C8 0.053(11) 0.094(13) 0.19(2) -0.007(10) 0.059(12) 0.034(13) C9 0.134(16) 0.141(17) 0.061(12) -0.026(13) 0.062(11) -0.009(11) C10 0.076(12) 0.081(13) 0.136(16) -0.013(10) 0.054(11) 0.009(11) C11 0.047(9) 0.061(10) 0.038(8) 0.005(7) 0.010(7) 0.007(7) C12 0.069(9) 0.076(10) 0.077(11) 0.016(8) 0.029(8) 0.029(8) C13 0.21(3) 0.27(3) 0.39(4) 0.13(2) 0.23(3) 0.25(3) C14 0.29(4) 0.072(16) 0.35(4) 0.06(2) 0.15(3) 0.10(2) C15 0.22(3) 0.18(2) 0.088(17) -0.03(2) 0.012(18) 0.010(16) C16 0.060(9) 0.049(9) 0.047(9) -0.001(7) 0.036(7) 0.000(7) C17 0.067(10) 0.096(13) 0.073(11) -0.008(9) 0.031(9) -0.035(9) C18 0.128(16) 0.129(16) 0.121(16) 0.006(13) 0.017(13) -0.087(13) C19 0.45(5) 0.13(2) 0.068(14) -0.01(2) -0.04(2) -0.043(11) C20 0.20(2) 0.22(3) 0.31(3) -0.17(2) 0.18(2) -0.17(3) C21 0.045(8) 0.049(9) 0.044(8) 0.001(7) 0.018(7) 0.005(7) C22 0.072(12) 0.078(13) 0.115(16) 0.019(10) 0.047(11) 0.052(11) C23 0.21(2) 0.17(2) 0.082(15) -0.068(19) -0.058(15) 0.064(15) C24 0.35(4) 0.099(19) 0.17(2) 0.03(2) 0.08(3) 0.034(17) C25 0.16(2) 0.19(2) 0.22(3) 0.009(18) 0.11(2) 0.14(2) C26 0.074(10) 0.036(8) 0.039(8) 0.006(7) 0.024(8) -0.001(6) C31 0.048(9) 0.082(12) 0.054(10) -0.002(9) 0.013(8) -0.009(9) C32 0.053(11) 0.124(16) 0.095(14) -0.038(11) 0.019(10) 0.008(12) C33 0.081(14) 0.17(2) 0.105(16) -0.037(13) 0.007(12) -0.010(15) C34 0.083(13) 0.102(15) 0.173(19) -0.044(11) 0.063(13) -0.019(14) C35 0.035(9) 0.125(15) 0.119(14) 0.000(9) 0.027(9) 0.010(12) C36 0.037(9) 0.059(11) 0.105(15) 0.007(8) 0.009(9) -0.021(10) C37 0.073(12) 0.097(11) 0.083(13) 0.015(10) 0.034(10) -0.002(11) C38 0.121(16) 0.096(11) 0.21(2) 0.020(12) 0.101(16) -0.034(15) C39 0.114(16) 0.18(2) 0.078(13) 0.047(14) 0.046(12) -0.017(13) C40 0.055(12) 0.18(2) 0.166(19) 0.004(12) 0.036(12) -0.061(16) C27 0.067(10) 0.096(13) 0.073(11) -0.008(9) 0.031(9) -0.035(9) C28A 0.114(16) 0.18(2) 0.078(13) 0.047(14) 0.046(12) -0.017(13) C29A 0.08(2) 0.16(4) 0.19(4) -0.06(2) 0.00(2) -0.03(3) C30A 0.128(16) 0.129(16) 0.121(16) 0.006(13) 0.017(13) -0.087(13) C28 0.15(5) 0.34(8) 0.25(6) 0.02(5) 0.02(4) 0.10(5) C29 0.092(12) 0.088(12) 0.091(12) -0.002(4) 0.031(6) -0.001(4) C30 0.15(4) 0.24(5) 0.16(4) -0.06(3) 0.10(3) -0.11(4) C27A 0.069(9) 0.076(10) 0.077(11) 0.016(8) 0.029(8) 0.029(8) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hf1 O8 . 2.117(8) ? Hf1 O7 . 2.125(8) ? Hf1 O5 . 2.140(8) ? Hf1 O6 . 2.156(8) ? Hf1 O3 . 2.214(9) ? Hf1 O4 . 2.233(8) ? Hf1 O1 . 2.240(8) ? Hf1 O2 . 2.243(9) ? Hf2 O9 . 2.095(8) ? Hf2 O11 . 2.140(8) ? Hf2 O12 . 2.150(8) ? Hf2 O10 . 2.162(8) ? Hf2 O14 . 2.196(9) ? Hf2 O15 . 2.199(10) ? Hf2 O13 . 2.215(9) ? Hf2 O16 . 2.232(8) ? O1 C1 . 1.255(15) ? O2 C1 . 1.248(16) ? O3 C6 . 1.235(15) ? O4 C6 . 1.285(15) ? O5 C11 . 1.257(13) ? O6 C16 . 1.229(13) ? O7 C21 . 1.293(13) ? O8 C26 . 1.255(13) ? O9 C26 . 1.293(14) ? O10 C21 . 1.246(13) ? O11 C16 . 1.282(13) ? O12 C11 . 1.255(13) ? O13 C31 . 1.221(15) ? O14 C31 . 1.291(15) ? O15 C36 . 1.244(18) ? O16 C36 . 1.308(16) ? C1 C2 . 1.534(19) ? C2 C5 . 1.46(2) ? C2 C4 . 1.51(2) ? C2 C3 . 1.51(2) ? C3 H3A . 0.98 ? C3 H3B . 0.98 ? C3 H3C . 0.98 ? C4 H4A . 0.98 ? C4 H4B . 0.98 ? C4 H4C . 0.98 ? C5 H5A . 0.98 ? C5 H5B . 0.98 ? C5 H5C . 0.98 ? C6 C7 . 1.532(17) ? C7 C10 . 1.510(19) ? C7 C8 . 1.552(19) ? C7 C9 . 1.6248(11) ? C8 H8A . 0.98 ? C8 H8B . 0.98 ? C8 H8C . 0.98 ? C9 H9A . 0.98 ? C9 H9B . 0.98 ? C9 H9C . 0.98 ? C10 H10A . 0.98 ? C10 H10B . 0.98 ? C10 H10C . 0.98 ? C11 C12 . 1.488(17) ? C12 C13 . 1.41(2) ? C12 C14 . 1.47(3) ? C12 C15 . 1.58(2) ? C13 H13A . 0.95 ? C13 H13B . 0.95 ? C14 H14A . 0.98 ? C14 H14B . 0.98 ? C14 H14C . 0.98 ? C15 H15A . 0.98 ? C15 H15B . 0.98 ? C15 H15C . 0.98 ? C16 C17 . 1.488(17) ? C17 C19 . 1.46(2) ? C17 C18 . 1.53(2) ? C17 C20 . 1.55(2) ? C18 H18A . 0.98 ? C18 H18B . 0.98 ? C18 H18C . 0.98 ? C19 H19A . 0.98 ? C19 H19B . 0.98 ? C19 H19C . 0.98 ? C20 H20A . 0.98 ? C20 H20B . 0.98 ? C20 H20C . 0.98 ? C21 C22 . 1.490(17) ? C22 C25 . 1.44(2) ? C22 C23 . 1.44(2) ? C22 C24 . 1.58(3) ? C23 H23A . 0.98 ? C23 H23B . 0.98 ? C23 H23C . 0.98 ? C24 H24A . 0.98 ? C24 H24B . 0.98 ? C24 H24C . 0.98 ? C25 H25A . 0.98 ? C25 H25B . 0.98 ? C25 H25C . 0.98 ? C26 C27A . 1.460(2) ? C26 C27 . 1.69(5) ? C31 C32 . 1.570(18) ? C32 C34 . 1.52(2) ? C32 C33 . 1.55(2) ? C32 C35 . 1.59(2) ? C33 H33A . 0.98 ? C33 H33B . 0.98 ? C33 H33C . 0.98 ? C34 H34A . 0.98 ? C34 H34B . 0.98 ? C34 H34C . 0.98 ? C35 H35A . 0.98 ? C35 H35B . 0.98 ? C35 H35C . 0.98 ? C36 C37 . 1.494(19) ? C37 C39 . 1.52(2) ? C37 C40 . 1.54(2) ? C37 C38 . 1.55(2) ? C38 H38A . 0.98 ? C38 H38B . 0.98 ? C38 H38C . 0.98 ? C39 H39A . 0.98 ? C39 H39B . 0.98 ? C39 H39C . 0.98 ? C40 H40A . 0.98 ? C40 H40B . 0.98 ? C40 H40C . 0.98 ? C27 C28A . 1.06(8) ? C27 C29A . 1.30(6) ? C27 C30A . 1.94(9) ? C28A C29A . 1.98(9) ? C28A H28A . 0.98 ? C28A H28B . 0.98 ? C28A H28C . 0.98 ? C29A H29A . 0.98 ? C29A H29B . 0.98 ? C29A H29C . 0.98 ? C30A H30A . 0.98 ? C30A H30B . 0.98 ? C30A H30C . 0.98 ? C28 C27A . 1.90(6) ? C28 H28D . 0.98 ? C28 H28E . 0.98 ? C28 H28F . 0.98 ? C29 C27A . 1.26(5) ? C29 H29D . 0.98 ? C29 H29E . 0.98 ? C29 H29F . 0.98 ? C30 C27A . 1.68(4) ? C30 H30D . 0.98 ? C30 H30F . 0.98 ? C30 H30E . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O8 Hf1 O7 . . 78.3(3) ? O8 Hf1 O5 . . 76.8(3) ? O7 Hf1 O5 . . 105.8(3) ? O8 Hf1 O6 . . 138.0(3) ? O7 Hf1 O6 . . 77.2(3) ? O5 Hf1 O6 . . 77.9(3) ? O8 Hf1 O3 . . 77.4(3) ? O7 Hf1 O3 . . 150.7(3) ? O5 Hf1 O3 . . 84.2(3) ? O6 Hf1 O3 . . 132.1(3) ? O8 Hf1 O4 . . 131.7(3) ? O7 Hf1 O4 . . 149.8(3) ? O5 Hf1 O4 . . 81.6(3) ? O6 Hf1 O4 . . 75.9(3) ? O3 Hf1 O4 . . 57.6(3) ? O8 Hf1 O1 . . 76.0(4) ? O7 Hf1 O1 . . 81.7(3) ? O5 Hf1 O1 . . 149.5(4) ? O6 Hf1 O1 . . 132.3(4) ? O3 Hf1 O1 . . 76.8(3) ? O4 Hf1 O1 . . 107.0(4) ? O8 Hf1 O2 . . 132.3(4) ? O7 Hf1 O2 . . 83.8(3) ? O5 Hf1 O2 . . 151.0(4) ? O6 Hf1 O2 . . 77.7(3) ? O3 Hf1 O2 . . 100.8(4) ? O4 Hf1 O2 . . 77.3(4) ? O1 Hf1 O2 . . 57.7(3) ? O9 Hf2 O11 . . 106.3(3) ? O9 Hf2 O12 . . 76.9(3) ? O11 Hf2 O12 . . 78.3(3) ? O9 Hf2 O10 . . 77.9(3) ? O11 Hf2 O10 . . 76.9(3) ? O12 Hf2 O10 . . 137.7(3) ? O9 Hf2 O14 . . 151.3(3) ? O11 Hf2 O14 . . 83.4(3) ? O12 Hf2 O14 . . 131.8(3) ? O10 Hf2 O14 . . 78.2(4) ? O9 Hf2 O15 . . 82.1(4) ? O11 Hf2 O15 . . 149.8(4) ? O12 Hf2 O15 . . 75.5(4) ? O10 Hf2 O15 . . 133.2(4) ? O14 Hf2 O15 . . 103.2(4) ? O9 Hf2 O13 . . 148.0(4) ? O11 Hf2 O13 . . 83.5(4) ? O12 Hf2 O13 . . 75.5(3) ? O10 Hf2 O13 . . 134.0(4) ? O14 Hf2 O13 . . 58.3(3) ? O15 Hf2 O13 . . 75.7(4) ? O9 Hf2 O16 . . 82.2(3) ? O11 Hf2 O16 . . 150.8(4) ? O12 Hf2 O16 . . 130.8(4) ? O10 Hf2 O16 . . 77.7(4) ? O14 Hf2 O16 . . 77.4(4) ? O15 Hf2 O16 . . 57.7(4) ? O13 Hf2 O16 . . 104.3(4) ? C1 O1 Hf1 . . 91.1(9) ? C1 O2 Hf1 . . 91.1(9) ? C6 O3 Hf1 . . 94.0(9) ? C6 O4 Hf1 . . 91.8(8) ? C11 O5 Hf1 . . 162.6(9) ? C16 O6 Hf1 . . 131.1(8) ? C21 O7 Hf1 . . 163.9(8) ? C26 O8 Hf1 . . 132.0(8) ? C26 O9 Hf2 . . 161.0(9) ? C21 O10 Hf2 . . 131.7(8) ? C16 O11 Hf2 . . 162.9(9) ? C11 O12 Hf2 . . 133.3(9) ? C31 O13 Hf2 . . 92.6(9) ? C31 O14 Hf2 . . 91.6(9) ? C36 O15 Hf2 . . 95.9(10) ? C36 O16 Hf2 . . 92.4(10) ? O2 C1 O1 . . 119.8(14) ? O2 C1 C2 . . 122.4(16) ? O1 C1 C2 . . 117.8(16) ? C5 C2 C4 . . 106.7(17) ? C5 C2 C3 . . 112.8(17) ? C4 C2 C3 . . 108.6(16) ? C5 C2 C1 . . 109.8(16) ? C4 C2 C1 . . 105.8(14) ? C3 C2 C1 . . 112.6(15) ? C2 C3 H3A . . 109.5 ? C2 C3 H3B . . 109.5 ? H3A C3 H3B . . 109.5 ? C2 C3 H3C . . 109.5 ? H3A C3 H3C . . 109.5 ? H3B C3 H3C . . 109.5 ? C2 C4 H4A . . 109.5 ? C2 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C2 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C2 C5 H5A . . 109.5 ? C2 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? C2 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? O3 C6 O4 . . 116.4(13) ? O3 C6 C7 . . 123.7(14) ? O4 C6 C7 . . 119.9(14) ? C10 C7 C6 . . 109.0(12) ? C10 C7 C8 . . 108.8(12) ? C6 C7 C8 . . 103.7(11) ? C10 C7 C9 . . 110.2(13) ? C6 C7 C9 . . 111.1(11) ? C8 C7 C9 . . 113.8(13) ? C7 C8 H8A . . 109.5 ? C7 C8 H8B . . 109.5 ? H8A C8 H8B . . 109.5 ? C7 C8 H8C . . 109.5 ? H8A C8 H8C . . 109.5 ? H8B C8 H8C . . 109.5 ? C7 C9 H9A . . 109.5 ? C7 C9 H9B . . 109.5 ? H9A C9 H9B . . 109.5 ? C7 C9 H9C . . 109.5 ? H9A C9 H9C . . 109.5 ? H9B C9 H9C . . 109.5 ? C7 C10 H10A . . 109.5 ? C7 C10 H10B . . 109.5 ? H10A C10 H10B . . 109.5 ? C7 C10 H10C . . 109.5 ? H10A C10 H10C . . 109.5 ? H10B C10 H10C . . 109.5 ? O12 C11 O5 . . 121.3(12) ? O12 C11 C12 . . 117.7(12) ? O5 C11 C12 . . 121.0(13) ? C13 C12 C14 . . 131.(2) ? C13 C12 C11 . . 113.4(14) ? C14 C12 C11 . . 103.0(15) ? C13 C12 C15 . . 95.6(18) ? C14 C12 C15 . . 102.1(17) ? C11 C12 C15 . . 109.7(14) ? C12 C13 H13A . . 120.0 ? C12 C13 H13B . . 120.0 ? H13A C13 H13B . . 120.0 ? C12 C14 H14A . . 109.5 ? C12 C14 H14B . . 109.5 ? H14A C14 H14B . . 109.5 ? C12 C14 H14C . . 109.5 ? H14A C14 H14C . . 109.5 ? H14B C14 H14C . . 109.5 ? C12 C15 H15A . . 109.5 ? C12 C15 H15B . . 109.5 ? H15A C15 H15B . . 109.5 ? C12 C15 H15C . . 109.5 ? H15A C15 H15C . . 109.5 ? H15B C15 H15C . . 109.5 ? O6 C16 O11 . . 123.3(12) ? O6 C16 C17 . . 120.6(12) ? O11 C16 C17 . . 115.9(12) ? C19 C17 C16 . . 109.6(15) ? C19 C17 C18 . . 115.5(18) ? C16 C17 C18 . . 108.7(13) ? C19 C17 C20 . . 112.(2) ? C16 C17 C20 . . 109.3(14) ? C18 C17 C20 . . 101.6(17) ? C17 C18 H18A . . 109.5 ? C17 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C17 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? C17 C19 H19A . . 109.5 ? C17 C19 H19B . . 109.5 ? H19A C19 H19B . . 109.5 ? C17 C19 H19C . . 109.5 ? H19A C19 H19C . . 109.5 ? H19B C19 H19C . . 109.5 ? C17 C20 H20A . . 109.5 ? C17 C20 H20B . . 109.5 ? H20A C20 H20B . . 109.5 ? C17 C20 H20C . . 109.5 ? H20A C20 H20C . . 109.5 ? H20B C20 H20C . . 109.5 ? O10 C21 O7 . . 121.5(12) ? O10 C21 C22 . . 120.4(12) ? O7 C21 C22 . . 118.1(12) ? C25 C22 C23 . . 123.7(18) ? C25 C22 C21 . . 112.4(14) ? C23 C22 C21 . . 113.8(15) ? C25 C22 C24 . . 94.6(18) ? C23 C22 C24 . . 104.8(18) ? C21 C22 C24 . . 102.7(15) ? C22 C23 H23A . . 109.5 ? C22 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? C22 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? C22 C24 H24A . . 109.5 ? C22 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C22 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? C22 C25 H25A . . 109.5 ? C22 C25 H25B . . 109.5 ? H25A C25 H25B . . 109.5 ? C22 C25 H25C . . 109.5 ? H25A C25 H25C . . 109.5 ? H25B C25 H25C . . 109.5 ? O8 C26 O9 . . 123.6(12) ? O8 C26 C27A . . 119.0(16) ? O9 C26 C27A . . 116.8(15) ? O8 C26 C27 . . 118.(2) ? O9 C26 C27 . . 117.(2) ? O13 C31 O14 . . 117.6(14) ? O13 C31 C32 . . 125.1(15) ? O14 C31 C32 . . 117.2(15) ? C34 C32 C33 . . 109.1(16) ? C34 C32 C31 . . 114.0(15) ? C33 C32 C31 . . 105.9(13) ? C34 C32 C35 . . 110.4(13) ? C33 C32 C35 . . 112.4(15) ? C31 C32 C35 . . 105.0(13) ? C32 C33 H33A . . 109.5 ? C32 C33 H33B . . 109.5 ? H33A C33 H33B . . 109.5 ? C32 C33 H33C . . 109.5 ? H33A C33 H33C . . 109.5 ? H33B C33 H33C . . 109.5 ? C32 C34 H34A . . 109.5 ? C32 C34 H34B . . 109.5 ? H34A C34 H34B . . 109.5 ? C32 C34 H34C . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? C32 C35 H35A . . 109.5 ? C32 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? C32 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? O15 C36 O16 . . 113.9(14) ? O15 C36 C37 . . 129.8(16) ? O16 C36 C37 . . 116.2(17) ? C36 C37 C39 . . 112.0(14) ? C36 C37 C40 . . 105.7(13) ? C39 C37 C40 . . 112.3(16) ? C36 C37 C38 . . 104.8(14) ? C39 C37 C38 . . 110.5(16) ? C40 C37 C38 . . 111.2(15) ? C37 C38 H38A . . 109.5 ? C37 C38 H38B . . 109.5 ? H38A C38 H38B . . 109.5 ? C37 C38 H38C . . 109.5 ? H38A C38 H38C . . 109.5 ? H38B C38 H38C . . 109.5 ? C37 C39 H39A . . 109.5 ? C37 C39 H39B . . 109.5 ? H39A C39 H39B . . 109.5 ? C37 C39 H39C . . 109.5 ? H39A C39 H39C . . 109.5 ? H39B C39 H39C . . 109.5 ? C37 C40 H40A . . 109.5 ? C37 C40 H40B . . 109.5 ? H40A C40 H40B . . 109.5 ? C37 C40 H40C . . 109.5 ? H40A C40 H40C . . 109.5 ? H40B C40 H40C . . 109.5 ? C28A C27 C29A . . 114.(7) ? C28A C27 C26 . . 127.(7) ? C29A C27 C26 . . 116.(4) ? C28A C27 C30A . . 98.(7) ? C29A C27 C30A . . 106.(4) ? C26 C27 C30A . . 84.(3) ? C27 C28A C29A . . 37.(5) ? C27 C28A H28A . . 109.5 ? C29A C28A H28A . . 86.2 ? C27 C28A H28B . . 109.5 ? C29A C28A H28B . . 146.1 ? H28A C28A H28B . . 109.5 ? C27 C28A H28C . . 109.5 ? C29A C28A H28C . . 92.0 ? H28A C28A H28C . . 109.5 ? H28B C28A H28C . . 109.5 ? C27 C29A C28A . . 29.(3) ? C27 C29A H29A . . 109.5 ? C28A C29A H29A . . 90.6 ? C27 C29A H29B . . 109.5 ? C28A C29A H29B . . 138.5 ? H29A C29A H29B . . 109.5 ? C27 C29A H29C . . 109.5 ? C28A C29A H29C . . 96.4 ? H29A C29A H29C . . 109.5 ? H29B C29A H29C . . 109.5 ? C27 C30A H30A . . 109.5 ? C27 C30A H30B . . 109.5 ? H30A C30A H30B . . 109.5 ? C27 C30A H30C . . 109.5 ? H30A C30A H30C . . 109.5 ? H30B C30A H30C . . 109.5 ? C27A C28 H28D . . 109.5 ? C27A C28 H28E . . 109.5 ? H28D C28 H28E . . 109.5 ? C27A C28 H28F . . 109.5 ? H28D C28 H28F . . 109.5 ? H28E C28 H28F . . 109.5 ? C27A C29 H29D . . 109.5 ? C27A C29 H29E . . 109.5 ? H29D C29 H29E . . 109.5 ? C27A C29 H29F . . 109.5 ? H29D C29 H29F . . 109.5 ? H29E C29 H29F . . 109.5 ? C27A C30 H30D . . 109.5 ? C27A C30 H30F . . 109.5 ? H30D C30 H30F . . 109.5 ? C27A C30 H30E . . 109.5 ? H30D C30 H30E . . 109.5 ? H30F C30 H30E . . 109.5 ? C29 C27A C26 . . 116.(3) ? C29 C27A C30 . . 116.(3) ? C26 C27A C30 . . 113.(2) ? C29 C27A C28 . . 123.(3) ? C26 C27A C28 . . 105.(2) ? C30 C27A C28 . . 78.(3) ? # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.069 0.012 0.491 3033 1106 ' ' 2 0.043 0.523 0.656 10 3 ' ' 3 0.043 0.977 0.156 10 3 ' ' 4 0.957 0.023 0.843 10 4 ' ' 5 0.957 0.477 0.343 10 3 ' ' _platon_squeeze_details ; ; #===END data_7 _audit_creation_method 'APEX2 v2014.5-0' _publ_requested_journal ? _publ_contact_author_name ? _publ_contact_author_address ; ; _publ_contact_author_email ? _publ_contact_author_fax ? _publ_contact_author_phone ? _publ_section_title ; ; _publ_section_abstract ; ; _publ_section_references ; ; _publ_section_comment ; ; data_I _chemical_name_systematic ? _chemical_name_common HfONc4 _chemical_formula_moiety ? _chemical_formula_sum 'C48 H88 Hf2 O16' _chemical_formula_iupac ? _chemical_formula_weight 1278.16 _chemical_melting_point ? _space_group_crystal_system triclinic _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3388(5) _cell_length_b 11.8903(6) _cell_length_c 43.709(2) _cell_angle_alpha 86.329(2) _cell_angle_beta 86.672(2) _cell_angle_gamma 87.272(2) _cell_volume 5865.2(5) _cell_formula_units_Z 4 _cell_measurement_reflns_used 3204 _cell_measurement_theta_min 1.9834 _cell_measurement_theta_max 25.0457 _cell_measurement_temperature 171.(2) _exptl_crystal_description prism _exptl_crystal_colour 'clear colourless' _exptl_crystal_size_max 0.230 _exptl_crystal_size_mid 0.160 _exptl_crystal_size_min 0.110 _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2592 _exptl_absorpt_coefficient_mu 3.596 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS V2014/2 (Bruker AXS Inc.)' _exptl_absorpt_correction_T_min 0.506 _exptl_absorpt_correction_T_max 0.673 _exptl_special_details ; ; _diffrn_ambient_temperature 171.(2) _diffrn_source 'fine-focus tube' _diffrn_source_type ? _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 42052 _diffrn_reflns_av_R_equivalents 0.0342 _diffrn_reflns_av_unetI/netI 0.0591 _diffrn_reflns_theta_min 0.94 _diffrn_reflns_theta_max 25.29 _diffrn_reflns_theta_full 25.29 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measured_fraction_theta_full 0.956 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 52 _refine_special_details ; ; _reflns_number_total 20405 _reflns_number_gt 17518 _reflns_threshold_expression 'I > 2\s(I)' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_R_factor_all 0.0966 _refine_ls_R_factor_gt 0.0837 _refine_ls_wR_factor_gt 0.2591 _refine_ls_wR_factor_ref 0.2670 _refine_ls_goodness_of_fit_ref 1.862 _refine_ls_restrained_S_all 1.862 _refine_ls_number_reflns 20405 _refine_ls_number_parameters 1142 _refine_ls_number_restraints 0 _refine_ls_number_constraints ? _refine_ls_hydrogen_treatment constr _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.4552P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 2.868 _refine_diff_density_min -3.928 _refine_ls_extinction_method none _refine_ls_extinction_coef ? 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' 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' _computing_data_collection ? _computing_cell_refinement 'APEX2 v2014.5-0 (Bruker AXS)' _computing_data_reduction ? _computing_structure_solution 'Bruker XT Intrinsic Solution Method' _computing_structure_refinement 'SHELXL-2014 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_refinement_flags_posn _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Hf Hf1 0.45523(5) 0.26727(5) 0.92568(2) 0.02144(18) Uani d . . . 1 . . Hf Hf2 0.36034(5) 0.27239(5) 0.83343(2) 0.02001(18) Uani d . . . 1 . . Hf Hf3 0.07045(5) 0.75913(5) 0.42424(2) 0.02126(18) Uani d . . . 1 . . Hf Hf4 0.18855(5) 0.79661(5) 0.33016(2) 0.01965(17) Uani d . . . 1 . . O O1 0.3204(10) 0.2454(9) 0.9655(2) 0.034(3) Uani d . . . 1 . . O O2 0.4747(10) 0.1325(9) 0.9610(2) 0.038(3) Uani d . . . 1 . . O O3 0.5014(9) 0.3967(9) 0.9557(2) 0.033(3) Uani d . . . 1 . . O O4 0.6445(9) 0.2866(9) 0.9375(3) 0.039(3) Uani d . . . 1 . . O O5 0.5281(8) 0.3678(8) 0.8877(2) 0.023(2) Uani d . . . 1 . . O O6 0.5603(9) 0.1407(8) 0.9011(2) 0.024(2) Uani d . . . 1 . . O O7 0.3264(9) 0.1708(8) 0.9076(2) 0.028(2) Uani d . . . 1 . . O O8 0.3173(9) 0.3949(8) 0.9171(2) 0.029(2) Uani d . . . 1 . . O O9 0.2464(8) 0.1633(7) 0.8621(2) 0.020(2) Uani d . . . 1 . . O O10 0.2874(8) 0.3786(8) 0.8673(2) 0.023(2) Uani d . . . 1 . . O O11 0.4896(8) 0.1663(8) 0.8546(2) 0.025(2) Uani d . . . 1 . . O O12 0.5066(9) 0.3798(8) 0.8371(2) 0.026(2) Uani d . . . 1 . . O O13 0.4557(9) 0.2510(8) 0.7890(2) 0.026(2) Uani d . . . 1 . . O O14 0.3534(10) 0.1113(8) 0.8081(2) 0.035(3) Uani d . . . 1 . . O O15 0.3133(9) 0.4356(8) 0.8061(2) 0.028(2) Uani d . . . 1 . . O O16 0.1958(9) 0.2969(8) 0.8104(2) 0.027(2) Uani d . . . 1 . . O O17 -0.1223(9) 0.7315(9) 0.4385(2) 0.035(3) Uani d . . . 1 . . O O18 0.0191(9) 0.6178(9) 0.4559(2) 0.030(2) Uani d . . . 1 . . O O19 0.0376(10) 0.8784(10) 0.4601(2) 0.039(3) Uani d . . . 1 . . O O20 0.1962(10) 0.7666(9) 0.4621(2) 0.037(3) Uani d . . . 1 . . O O21 0.2035(8) 0.8628(8) 0.4037(2) 0.020(2) Uani d . . . 1 . . O O22 0.2109(8) 0.6342(8) 0.4138(2) 0.020(2) Uani d . . . 1 . . O O23 -0.0291(8) 0.8935(8) 0.4011(2) 0.027(2) Uani d . . . 1 . . O O24 0.0054(8) 0.6731(8) 0.3874(2) 0.024(2) Uani d . . . 1 . . O O25 0.0451(8) 0.6826(8) 0.3368(2) 0.022(2) Uani d . . . 1 . . O O26 0.0489(8) 0.8943(7) 0.3526(2) 0.022(2) Uani d . . . 1 . . O O27 0.2559(8) 0.6753(7) 0.3638(2) 0.022(2) Uani d . . . 1 . . O O28 0.2923(8) 0.8966(7) 0.3577(2) 0.025(2) Uani d . . . 1 . . O O29 0.2412(9) 0.6478(8) 0.3020(2) 0.026(2) Uani d . . . 1 . . O O30 0.3625(10) 0.7780(8) 0.3063(3) 0.036(3) Uani d . . . 1 . . O O31 0.0923(10) 0.8369(8) 0.2881(2) 0.033(3) Uani d . . . 1 . . O O32 0.2018(11) 0.9659(8) 0.3031(3) 0.039(3) Uani d . . . 1 . . C C1 0.3776(15) 0.1601(15) 0.9761(4) 0.039(4) Uani d . . . 1 . . C C2 0.3355(18) 0.0846(15) 1.0025(4) 0.050(4) Uani d . . . 1 . . H H2A 0.3077 0.0159 0.994 0.059 Uiso calc U . R 1 . . H H2B 0.4051 0.0608 1.0144 0.059 Uiso calc U . R 1 . . C C3 0.2413(14) 0.1252(13) 1.0245(4) 0.032(3) Uani d . . . 1 . . C C4 0.130(2) 0.133(3) 1.0070(6) 0.114(8) Uani d . . . 1 . . H H4A 0.0621 0.1507 1.0211 0.171 Uiso calc U . . 1 . . H H4B 0.1196 0.0613 0.9981 0.171 Uiso calc U . . 1 . . H H4C 0.1366 0.1933 0.9907 0.171 Uiso calc U . . 1 . . C C5 0.2192(19) 0.0347(18) 1.0511(4) 0.057(4) Uani d . . . 1 . . H H5A 0.2893 0.0248 1.0633 0.086 Uiso calc U . . 1 . . H H5B 0.2032 -0.0371 1.0427 0.086 Uiso calc U . . 1 . . H H5C 0.151 0.0592 1.0643 0.086 Uiso calc U . . 1 . . C C6 0.268(3) 0.227(2) 1.0352(5) 0.110(8) Uani d . . . 1 . . H H6A 0.3158 0.2129 1.0532 0.165 Uiso calc U . . 1 . . H H6B 0.1944 0.2686 1.0411 0.165 Uiso calc U . . 1 . . H H6C 0.3121 0.2706 1.0191 0.165 Uiso calc U . . 1 . . C C7 0.6106(13) 0.3678(12) 0.9538(3) 0.025(3) Uani d . . . 1 . . C C8 0.6999(18) 0.4315(15) 0.9698(4) 0.050(4) Uani d . . . 1 . . H H8A 0.7693 0.4446 0.9554 0.059 Uiso calc U . R 1 . . H H8B 0.6638 0.506 0.9747 0.059 Uiso calc U . R 1 . . C C9 0.7418(13) 0.3712(12) 0.9990(3) 0.027(3) Uani d . . . 1 . . C C10 0.811(2) 0.2620(17) 0.9921(4) 0.063(6) Uani d . . . 1 . . H H10A 0.7561 0.2043 0.988 0.095 Uiso calc U . . 1 . . H H10B 0.8568 0.236 1.0097 0.095 Uiso calc U . . 1 . . H H10C 0.8651 0.2754 0.974 0.095 Uiso calc U . . 1 . . C C11 0.823(2) 0.4479(19) 1.0139(5) 0.067(7) Uani d . . . 1 . . H H11A 0.8161 0.4342 1.0363 0.101 Uiso calc U . . 1 . . H H11B 0.8009 0.527 1.0084 0.101 Uiso calc U . . 1 . . H H11C 0.9053 0.4319 1.0065 0.101 Uiso calc U . . 1 . . C C12 0.632(2) 0.341(3) 1.0217(6) 0.114(8) Uani d . . . 1 . . H H12A 0.5847 0.2867 1.0124 0.171 Uiso calc U . . 1 . . H H12B 0.5838 0.4095 1.0255 0.171 Uiso calc U . . 1 . . H H12C 0.6605 0.3075 1.0411 0.171 Uiso calc U . . 1 . . C C13 0.5549(12) 0.4093(11) 0.8607(3) 0.020(3) Uani d . . . 1 . . C C14 0.6486(13) 0.4950(12) 0.8559(3) 0.025(3) Uani d . . . 1 . . H H14A 0.6854 0.4917 0.8348 0.03 Uiso calc U . R 1 . . H H14B 0.7111 0.4768 0.8705 0.03 Uiso calc U . R 1 . . C C15 0.5957(16) 0.6161(13) 0.8604(4) 0.041(4) Uani d . . . 1 . . C C16 0.6924(18) 0.6966(14) 0.8499(5) 0.057(6) Uani d . . . 1 . . H H16A 0.7106 0.6915 0.8278 0.085 Uiso calc U . . 1 . . H H16B 0.7635 0.6762 0.8611 0.085 Uiso calc U . . 1 . . H H16C 0.6652 0.7739 0.854 0.085 Uiso calc U . . 1 . . C C17 0.564(2) 0.6254(15) 0.8952(6) 0.076(8) Uani d . . . 1 . . H H17A 0.6361 0.6362 0.9058 0.114 Uiso calc U . . 1 . . H H17B 0.5279 0.556 0.9036 0.114 Uiso calc U . . 1 . . H H17C 0.5082 0.6897 0.8981 0.114 Uiso calc U . . 1 . . C C18 0.4892(18) 0.6411(15) 0.8407(5) 0.060(6) Uani d . . . 1 . . H H18A 0.4755 0.7229 0.8375 0.089 Uiso calc U . . 1 . . H H18B 0.4189 0.6082 0.8511 0.089 Uiso calc U . . 1 . . H H18C 0.505 0.6082 0.8208 0.089 Uiso calc U . . 1 . . C C19 0.5627(12) 0.1179(11) 0.8733(3) 0.018(3) Uani d . . . 1 . . C C20 0.6539(13) 0.0341(11) 0.8624(3) 0.025(3) Uani d . . . 1 . . H H20A 0.6188 -0.0123 0.8475 0.03 Uiso calc U . R 1 . . H H20B 0.6771 -0.0167 0.88 0.03 Uiso calc U . R 1 . . C C21 0.7670(14) 0.0872(12) 0.8468(4) 0.037(4) Uani d . . . 1 . . C C22 0.8143(16) 0.1638(18) 0.8693(5) 0.058(6) Uani d . . . 1 . . H H22A 0.891 0.1908 0.8612 0.086 Uiso calc U . . 1 . . H H22B 0.8238 0.1216 0.8891 0.086 Uiso calc U . . 1 . . H H22C 0.7585 0.2283 0.8721 0.086 Uiso calc U . . 1 . . C C23 0.8597(18) -0.0097(18) 0.8418(5) 0.059(6) Uani d . . . 1 . . H H23A 0.8266 -0.0663 0.8298 0.089 Uiso calc U . . 1 . . H H23B 0.8812 -0.0446 0.8617 0.089 Uiso calc U . . 1 . . H H23C 0.9302 0.02 0.8307 0.089 Uiso calc U . . 1 . . C C24 0.7376(18) 0.1542(17) 0.8171(5) 0.060(6) Uani d . . . 1 . . H H24A 0.7343 0.235 0.8205 0.09 Uiso calc U . . 1 . . H H24B 0.6608 0.1327 0.8107 0.09 Uiso calc U . . 1 . . H H24C 0.7988 0.138 0.801 0.09 Uiso calc U . . 1 . . C C25 0.2509(12) 0.1363(10) 0.8896(3) 0.019(3) Uani d . . . 1 . . C C26 0.1679(12) 0.0508(11) 0.9043(3) 0.023(3) Uani d . . . 1 . . H H26A 0.0894 0.064 0.8956 0.027 Uiso calc U . R 1 . . H H26B 0.1581 0.0614 0.9266 0.027 Uiso calc U . R 1 . . C C27 0.2138(16) -0.0742(13) 0.8993(4) 0.040(4) Uani d . . . 1 . . C C28 0.1246(17) -0.1497(14) 0.9156(5) 0.061(6) Uani d . . . 1 . . H H28A 0.1305 -0.2236 0.9067 0.092 Uiso calc U . R 1 . . H H28B 0.0449 -0.1158 0.9132 0.092 Uiso calc U . R 1 . . H H28C 0.1401 -0.1591 0.9374 0.092 Uiso calc U . R 1 . . C C29 0.3332(19) -0.0992(18) 0.9131(8) 0.107(12) Uani d . . . 1 . . H H29A 0.3289 -0.0772 0.9343 0.16 Uiso calc U . . 1 . . H H29B 0.3937 -0.0564 0.9011 0.16 Uiso calc U . . 1 . . H H29C 0.3539 -0.1801 0.9126 0.16 Uiso calc U . . 1 . . C C30 0.218(2) -0.0945(15) 0.8641(5) 0.076(8) Uani d . . . 1 . . H H30A 0.2283 -0.1755 0.8613 0.114 Uiso calc U . . 1 . . H H30B 0.2849 -0.0554 0.8537 0.114 Uiso calc U . . 1 . . H H30C 0.1443 -0.0651 0.8555 0.114 Uiso calc U . . 1 . . C C31 0.2662(12) 0.4254(11) 0.8922(3) 0.020(3) Uani d . . . 1 . . C C32 0.1682(12) 0.5135(10) 0.8938(3) 0.019(3) Uani d . . . 1 . . H H32A 0.1769 0.5662 0.8754 0.023 Uiso calc U . R 1 . . H H32B 0.1779 0.5572 0.912 0.023 Uiso calc U . R 1 . . C C33 0.0407(12) 0.4710(12) 0.8958(3) 0.026(3) Uani d . . . 1 . . C C34 0.0273(17) 0.3708(14) 0.9200(5) 0.049(5) Uani d . . . 1 . . H H34A 0.0555 0.3914 0.9395 0.074 Uiso calc U . . 1 . . H H34B 0.074 0.3051 0.9129 0.074 Uiso calc U . . 1 . . H H34C -0.0561 0.3525 0.9228 0.074 Uiso calc U . . 1 . . C C35 0.0115(16) 0.4390(18) 0.8640(5) 0.055(6) Uani d . . . 1 . . H H35A 0.0617 0.3735 0.8582 0.083 Uiso calc U . . 1 . . H H35B 0.026 0.5027 0.8491 0.083 Uiso calc U . . 1 . . H H35C -0.0718 0.4203 0.8643 0.083 Uiso calc U . . 1 . . C C36 -0.0417(15) 0.5691(17) 0.9056(5) 0.052(5) Uani d . . . 1 . . H H36A -0.1225 0.5434 0.9091 0.078 Uiso calc U . . 1 . . H H36B -0.0401 0.6299 0.8894 0.078 Uiso calc U . . 1 . . H H36C -0.0154 0.5971 0.9246 0.078 Uiso calc U . . 1 . . C C37 0.4236(14) 0.1525(12) 0.7865(3) 0.029(4) Uani d . . . 1 . . C C38 0.4584(16) 0.0931(12) 0.7579(3) 0.035(4) Uani d . . . 1 . . H H38A 0.5435 0.1046 0.7529 0.041 Uiso calc U . R 1 . . H H38B 0.4145 0.1314 0.741 0.041 Uiso calc U . R 1 . . C C39 0.4397(15) -0.0312(12) 0.7577(4) 0.034(4) Uani d . . . 1 . . C C40 0.497(2) -0.0706(16) 0.7264(4) 0.061(6) Uani d . . . 1 . . H H40A 0.4941 -0.1528 0.7262 0.092 Uiso calc U . . 1 . . H H40B 0.5791 -0.0486 0.7241 0.092 Uiso calc U . . 1 . . H H40C 0.4525 -0.0351 0.7095 0.092 Uiso calc U . . 1 . . C C41 0.307(2) -0.053(2) 0.7597(5) 0.077(8) Uani d . . . 1 . . H H41A 0.2816 -0.0755 0.7809 0.116 Uiso calc U . . 1 . . H H41B 0.2916 -0.1132 0.7463 0.116 Uiso calc U . . 1 . . H H41C 0.2622 0.0162 0.753 0.116 Uiso calc U . . 1 . . C C42 0.504(3) -0.0963(17) 0.7835(4) 0.083(9) Uani d . . . 1 . . H H42A 0.5739 -0.0559 0.7879 0.124 Uiso calc U . . 1 . . H H42B 0.5289 -0.1717 0.7771 0.124 Uiso calc U . . 1 . . H H42C 0.451 -0.103 0.8019 0.124 Uiso calc U . . 1 . . C C43 0.2179(13) 0.3948(12) 0.7979(3) 0.026(3) Uani d . . . 1 . . C C44 0.1378(14) 0.4637(12) 0.7785(3) 0.028(3) Uani d . . . 1 . . H H44A 0.1838 0.5219 0.7666 0.034 Uiso calc U . R 1 . . H H44B 0.0779 0.503 0.7918 0.034 Uiso calc U . R 1 . . C C45 0.0722(14) 0.3956(13) 0.7555(4) 0.032(3) Uani d . . . 1 . . C C46 0.1576(19) 0.3143(18) 0.7388(4) 0.057(4) Uani d . . . 1 . . H H46A 0.1133 0.2685 0.726 0.086 Uiso calc U . . 1 . . H H46B 0.1992 0.2648 0.7538 0.086 Uiso calc U . . 1 . . H H46C 0.2152 0.3572 0.7258 0.086 Uiso calc U . . 1 . . C C47 0.0117(18) 0.4775(15) 0.7340(4) 0.052(5) Uani d . . . 1 . . H H47A 0.069 0.5298 0.7243 0.078 Uiso calc U . . 1 . . H H47B -0.051 0.5199 0.7453 0.078 Uiso calc U . . 1 . . H H47C -0.0228 0.4369 0.7181 0.078 Uiso calc U . . 1 . . C C48 -0.025(3) 0.327(2) 0.7734(5) 0.110(8) Uani d . . . 1 . . H H48A -0.0797 0.3784 0.7845 0.165 Uiso calc U . . 1 . . H H48B 0.0118 0.2723 0.7881 0.165 Uiso calc U . . 1 . . H H48C -0.0681 0.2872 0.759 0.165 Uiso calc U . . 1 . . C C49 -0.0933(15) 0.6451(14) 0.4547(3) 0.035(4) Uani d . . . 1 . . C C50 -0.1786(18) 0.5737(17) 0.4733(4) 0.056(4) Uani d . . . 1 . . H H50A -0.1363 0.5037 0.481 0.068 Uiso calc U . R 1 . . H H50B -0.24 0.552 0.4598 0.068 Uiso calc U . R 1 . . C C51 -0.2406(14) 0.6341(13) 0.5014(4) 0.031(4) Uani d . . . 1 . . C C52 -0.3111(18) 0.7380(16) 0.4922(4) 0.056(6) Uani d . . . 1 . . H H52A -0.3822 0.7173 0.4825 0.084 Uiso calc U . . 1 . . H H52B -0.2635 0.7854 0.4776 0.084 Uiso calc U . . 1 . . H H52C -0.3341 0.7796 0.5104 0.084 Uiso calc U . . 1 . . C C53 -0.320(3) 0.550(3) 0.5191(6) 0.111(8) Uani d . . . 1 . . H H53A -0.3822 0.5914 0.531 0.167 Uiso calc U . . 1 . . H H53B -0.2729 0.5016 0.5331 0.167 Uiso calc U . . 1 . . H H53C -0.356 0.5043 0.5047 0.167 Uiso calc U . . 1 . . C C54 -0.1389(18) 0.6595(18) 0.5226(4) 0.056(6) Uani d . . . 1 . . H H54A -0.0884 0.7163 0.5121 0.084 Uiso calc U . . 1 . . H H54B -0.0913 0.5901 0.5271 0.084 Uiso calc U . . 1 . . H H54C -0.1734 0.6881 0.5418 0.084 Uiso calc U . . 1 . . C C55 0.1304(17) 0.8432(14) 0.4743(4) 0.041(4) Uani d . . . 1 . . C C56 0.1574(18) 0.9006(18) 0.5019(4) 0.056(4) Uani d . . . 1 . . H H56A 0.1708 0.9802 0.4951 0.068 Uiso calc U . R 1 . . H H56B 0.0841 0.9013 0.5154 0.068 Uiso calc U . R 1 . . C C57 0.2539(18) 0.8641(15) 0.5217(4) 0.048(5) Uani d . . . 1 . . C C58 0.237(4) 0.749(2) 0.5329(7) 0.149(12) Uani d . . . 1 . . H H58A 0.2974 0.7249 0.5474 0.224 Uiso calc U . . 1 . . H H58B 0.2434 0.6996 0.5157 0.224 Uiso calc U . . 1 . . H H58C 0.1583 0.7431 0.5433 0.224 Uiso calc U . . 1 . . C C59 0.262(4) 0.933(2) 0.5483(7) 0.149(12) Uani d . . . 1 . . H H59A 0.2563 0.8849 0.5673 0.224 Uiso calc U . . 1 . . H H59B 0.1969 0.9907 0.5485 0.224 Uiso calc U . . 1 . . H H59C 0.3376 0.9703 0.5468 0.224 Uiso calc U . . 1 . . C C60 0.363(3) 0.883(3) 0.5031(6) 0.111(8) Uani d . . . 1 . . H H60A 0.4123 0.8133 0.5028 0.167 Uiso calc U . . 1 . . H H60B 0.4068 0.9418 0.5119 0.167 Uiso calc U . . 1 . . H H60C 0.3444 0.9083 0.482 0.167 Uiso calc U . . 1 . . C C61 0.2793(12) 0.9097(11) 0.3871(3) 0.019(3) Uani d . . . 1 . . C C62 0.3619(12) 0.9890(11) 0.3996(3) 0.024(3) Uani d . . . 1 . . H H62A 0.441 0.9797 0.3891 0.029 Uiso calc U . R 1 . . H H62B 0.3699 0.9691 0.4218 0.029 Uiso calc U . R 1 . . C C63 0.3172(14) 1.1150(11) 0.3953(3) 0.027(3) Uani d . . . 1 . . C C64 0.1963(16) 1.1339(17) 0.4090(6) 0.066(7) Uani d . . . 1 . . H H64A 0.1791 1.215 0.4104 0.1 Uiso calc U . . 1 . . H H64B 0.1901 1.0959 0.4295 0.1 Uiso calc U . . 1 . . H H64C 0.1394 1.1032 0.396 0.1 Uiso calc U . . 1 . . C C65 0.4036(16) 1.1862(15) 0.4125(5) 0.058(6) Uani d . . . 1 . . H H65A 0.3714 1.264 0.4134 0.087 Uiso calc U . . 1 . . H H65B 0.4812 1.1859 0.4014 0.087 Uiso calc U . . 1 . . H H65C 0.4117 1.1529 0.4334 0.087 Uiso calc U . . 1 . . C C66 0.3267(17) 1.1580(14) 0.3616(4) 0.047(5) Uani d . . . 1 . . H H66A 0.2681 1.122 0.3503 0.071 Uiso calc U . . 1 . . H H66B 0.4062 1.1395 0.3528 0.071 Uiso calc U . . 1 . . H H66C 0.3117 1.24 0.3601 0.071 Uiso calc U . . 1 . . C C67 0.2722(12) 0.6176(11) 0.3894(3) 0.021(3) Uani d . . . 1 . . C C68 0.3689(12) 0.5260(11) 0.3912(3) 0.022(3) Uani d . . . 1 . . H H68A 0.3703 0.4828 0.3726 0.026 Uiso calc U . R 1 . . H H68B 0.3508 0.4734 0.4092 0.026 Uiso calc U . R 1 . . C C69 0.4929(13) 0.5732(13) 0.3941(3) 0.027(3) Uani d . . . 1 . . C C70 0.4879(16) 0.6618(14) 0.4199(4) 0.043(4) Uani d . . . 1 . . H H70A 0.5406 0.635 0.4361 0.065 Uiso calc U . . 1 . . H H70B 0.4068 0.6703 0.4288 0.065 Uiso calc U . . 1 . . H H70C 0.5133 0.7349 0.4109 0.065 Uiso calc U . . 1 . . C C71 0.5751(14) 0.4704(13) 0.4048(4) 0.040(4) Uani d . . . 1 . . H H71A 0.5873 0.4185 0.3882 0.059 Uiso calc U . . 1 . . H H71B 0.5379 0.4309 0.423 0.059 Uiso calc U . . 1 . . H H71C 0.6515 0.4973 0.4099 0.059 Uiso calc U . . 1 . . C C72 0.5426(14) 0.6266(15) 0.3641(4) 0.040(4) Uani d . . . 1 . . H H72A 0.6238 0.6481 0.3665 0.06 Uiso calc U . . 1 . . H H72B 0.4938 0.6938 0.3582 0.06 Uiso calc U . . 1 . . H H72C 0.5427 0.5725 0.3481 0.06 Uiso calc U . . 1 . . C C73 -0.0260(13) 0.9296(10) 0.3727(3) 0.023(3) Uani d . . . 1 . . C C74 -0.1177(13) 1.0166(12) 0.3635(3) 0.026(3) Uani d . . . 1 . . H H74A -0.0855 1.0634 0.3457 0.032 Uiso calc U . R 1 . . H H74B -0.1349 1.0665 0.3806 0.032 Uiso calc U . R 1 . . C C75 -0.2370(13) 0.9670(13) 0.3548(4) 0.032(4) Uani d . . . 1 . . C C76 -0.3180(17) 1.0673(15) 0.3475(4) 0.045(5) Uani d . . . 1 . . H H76A -0.3936 1.0417 0.3414 0.068 Uiso calc U . . 1 . . H H76B -0.2818 1.1146 0.3307 0.068 Uiso calc U . . 1 . . H H76C -0.3316 1.1111 0.3657 0.068 Uiso calc U . . 1 . . C C77 -0.2881(14) 0.8937(14) 0.3822(4) 0.036(4) Uani d . . . 1 . . H H77A -0.3126 0.9416 0.3991 0.054 Uiso calc U . . 1 . . H H77B -0.2277 0.8374 0.389 0.054 Uiso calc U . . 1 . . H H77C -0.3567 0.8553 0.376 0.054 Uiso calc U . . 1 . . C C78 -0.2149(16) 0.8939(16) 0.3264(4) 0.047(5) Uani d . . . 1 . . H H78A -0.2898 0.8643 0.3211 0.07 Uiso calc U . . 1 . . H H78B -0.1588 0.831 0.3314 0.07 Uiso calc U . . 1 . . H H78C -0.1823 0.9405 0.3089 0.07 Uiso calc U . . 1 . . C C79 -0.0070(11) 0.6432(10) 0.3607(3) 0.014(3) Uani d . . . 1 . . C C80 -0.0962(12) 0.5529(11) 0.3578(3) 0.021(3) Uani d . . . 1 . . H H80A -0.1218 0.5578 0.3365 0.026 Uiso calc U . R 1 . . H H80B -0.1667 0.5697 0.3715 0.026 Uiso calc U . R 1 . . C C81 -0.0511(14) 0.4318(11) 0.3657(3) 0.026(3) Uani d . . . 1 . . C C82 0.0696(14) 0.4101(14) 0.3489(4) 0.042(4) Uani d . . . 1 . . H H82A 0.1287 0.4549 0.3574 0.063 Uiso calc U . . 1 . . H H82B 0.064 0.4318 0.327 0.063 Uiso calc U . . 1 . . H H82C 0.093 0.3298 0.3514 0.063 Uiso calc U . . 1 . . C C83 -0.1424(17) 0.3538(14) 0.3558(6) 0.066(7) Uani d . . . 1 . . H H83A -0.1091 0.2762 0.3563 0.1 Uiso calc U . . 1 . . H H83B -0.1639 0.3772 0.3349 0.1 Uiso calc U . . 1 . . H H83C -0.213 0.3578 0.3698 0.1 Uiso calc U . . 1 . . C C84 -0.0380(18) 0.4147(14) 0.3995(4) 0.047(5) Uani d . . . 1 . . H H84A -0.1139 0.3946 0.4098 0.071 Uiso calc U . . 1 . . H H84B -0.0127 0.4845 0.4074 0.071 Uiso calc U . . 1 . . H H84C 0.0214 0.3538 0.4036 0.071 Uiso calc U . . 1 . . C C85 0.3413(14) 0.6820(12) 0.2961(4) 0.031(4) Uani d . . . 1 . . C C86 0.4442(14) 0.6209(12) 0.2803(4) 0.029(4) Uani d . . . 1 . . H H86A 0.5115 0.6171 0.2938 0.035 Uiso calc U . R 1 . . H H86B 0.4681 0.666 0.2613 0.035 Uiso calc U . R 1 . . C C87 0.4217(17) 0.4991(13) 0.2716(4) 0.042(4) Uani d . . . 1 . . C C88 0.3806(18) 0.4255(14) 0.2993(4) 0.054(6) Uani d . . . 1 . . H H88A 0.3134 0.4635 0.3101 0.081 Uiso calc U . . 1 . . H H88B 0.4454 0.4118 0.3131 0.081 Uiso calc U . . 1 . . H H88C 0.3563 0.3534 0.2926 0.081 Uiso calc U . . 1 . . C C89 0.5424(17) 0.4477(14) 0.2587(4) 0.048(5) Uani d . . . 1 . . H H89A 0.5312 0.3721 0.252 0.072 Uiso calc U . . 1 . . H H89B 0.5994 0.4429 0.2748 0.072 Uiso calc U . . 1 . . H H89C 0.5724 0.496 0.2412 0.072 Uiso calc U . . 1 . . C C90 0.3352(19) 0.4999(16) 0.2466(4) 0.055(5) Uani d . . . 1 . . H H90A 0.3065 0.4239 0.2455 0.082 Uiso calc U . . 1 . . H H90B 0.3747 0.5238 0.2269 0.082 Uiso calc U . . 1 . . H H90C 0.2683 0.5524 0.2512 0.082 Uiso calc U . . 1 . . C C91 0.1327(16) 0.9359(12) 0.2841(3) 0.034(4) Uani d . . . 1 . . C C92 0.096(2) 1.0120(14) 0.2553(4) 0.058(6) Uani d . . . 1 . . H H92A 0.1571 1.0012 0.2386 0.069 Uiso calc U . R 1 . . H H92B 0.0212 0.9846 0.2485 0.069 Uiso calc U . R 1 . . C C93 0.0787(16) 1.1358(13) 0.2595(4) 0.037(4) Uani d . . . 1 . . C C94 -0.012(2) 1.162(2) 0.2849(5) 0.078(8) Uani d . . . 1 . . H H94A -0.0028 1.1063 0.3023 0.117 Uiso calc U . . 1 . . H H94B -0.0916 1.1584 0.2774 0.117 Uiso calc U . . 1 . . H H94C -0.0012 1.2375 0.2916 0.117 Uiso calc U . . 1 . . C C95 0.184(2) 1.1968(17) 0.2650(7) 0.091(9) Uani d . . . 1 . . H H95A 0.1635 1.2779 0.2644 0.137 Uiso calc U . . 1 . . H H95B 0.2457 1.1812 0.2491 0.137 Uiso calc U . . 1 . . H H95C 0.2119 1.1721 0.2852 0.137 Uiso calc U . . 1 . . C C96 0.026(2) 1.1899(17) 0.2296(4) 0.073(7) Uani d . . . 1 . . H H96A 0.0131 1.2714 0.2314 0.109 Uiso calc U . . 1 . . H H96B -0.0494 1.1564 0.2266 0.109 Uiso calc U . . 1 . . H H96C 0.0813 1.176 0.2121 0.109 Uiso calc U . . 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Hf1 0.0214(3) 0.0268(3) 0.0160(3) 0.0048(2) -0.0044(3) -0.0017(2) Hf2 0.0242(3) 0.0207(3) 0.0152(3) -0.0026(2) -0.0034(3) 0.0014(2) Hf3 0.0195(3) 0.0263(3) 0.0170(3) 0.0034(2) 0.0020(3) -0.0003(2) Hf4 0.0228(3) 0.0173(3) 0.0183(3) -0.0016(2) 0.0038(3) -0.0008(2) O1 0.038(7) 0.035(6) 0.026(6) 0.014(5) 0.002(5) 0.010(5) O2 0.039(7) 0.048(7) 0.023(6) 0.015(5) 0.003(5) 0.004(5) O3 0.030(6) 0.036(6) 0.036(6) 0.010(5) -0.017(5) -0.012(5) O4 0.025(6) 0.049(7) 0.046(7) 0.010(5) -0.010(5) -0.023(6) O5 0.021(5) 0.027(5) 0.021(5) 0.000(4) -0.001(4) 0.003(4) O6 0.025(6) 0.025(5) 0.021(5) -0.001(4) -0.003(4) 0.010(4) O7 0.029(6) 0.033(6) 0.022(5) -0.001(5) 0.000(5) 0.000(4) O8 0.029(6) 0.034(6) 0.023(6) 0.008(5) -0.004(5) 0.006(5) O9 0.024(5) 0.023(5) 0.014(5) -0.006(4) -0.001(4) 0.006(4) O10 0.023(6) 0.026(5) 0.021(5) -0.002(4) -0.005(4) -0.002(4) O11 0.016(5) 0.034(6) 0.026(6) 0.002(4) -0.002(4) -0.004(5) O12 0.031(6) 0.026(5) 0.020(5) -0.004(4) 0.004(5) 0.003(4) O13 0.037(6) 0.023(5) 0.020(5) -0.004(4) -0.003(5) -0.002(4) O14 0.043(7) 0.030(6) 0.034(6) -0.010(5) 0.012(5) -0.010(5) O15 0.025(6) 0.032(6) 0.028(6) -0.005(5) -0.008(5) 0.009(5) O16 0.033(6) 0.032(6) 0.018(5) 0.000(5) -0.013(5) 0.005(4) O17 0.022(6) 0.048(7) 0.028(6) 0.005(5) 0.004(5) 0.026(5) O18 0.027(6) 0.039(6) 0.025(6) 0.001(5) -0.001(5) 0.005(5) O19 0.034(7) 0.063(8) 0.023(6) 0.022(6) -0.019(5) -0.025(5) O20 0.041(7) 0.046(7) 0.025(6) 0.009(5) -0.005(5) -0.014(5) O21 0.019(5) 0.027(5) 0.016(5) 0.007(4) -0.006(4) -0.002(4) O22 0.016(5) 0.031(5) 0.014(5) 0.003(4) -0.001(4) 0.001(4) O23 0.018(5) 0.031(5) 0.031(6) 0.006(4) 0.004(5) -0.001(5) O24 0.020(5) 0.027(5) 0.024(6) -0.002(4) -0.001(4) 0.006(4) O25 0.015(5) 0.026(5) 0.025(6) -0.005(4) 0.004(4) -0.002(4) O26 0.021(5) 0.023(5) 0.022(5) -0.001(4) 0.005(4) -0.003(4) O27 0.018(5) 0.021(5) 0.027(6) -0.006(4) 0.002(4) 0.000(4) O28 0.021(5) 0.021(5) 0.033(6) -0.006(4) 0.001(5) -0.006(4) O29 0.024(6) 0.031(6) 0.023(5) -0.004(5) 0.005(5) -0.009(4) O30 0.037(7) 0.022(5) 0.050(7) -0.012(5) 0.022(6) -0.016(5) O31 0.044(7) 0.026(6) 0.030(6) 0.001(5) -0.011(5) 0.001(5) O32 0.054(8) 0.027(6) 0.034(7) -0.009(5) -0.008(6) 0.010(5) C1 0.036(10) 0.057(11) 0.019(8) 0.021(8) 0.009(8) 0.010(8) C2 0.072(10) 0.043(7) 0.031(7) 0.010(7) 0.001(7) 0.014(6) C3 0.033(7) 0.036(6) 0.026(6) 0.006(5) 0.000(5) 0.007(5) C4 0.058(12) 0.21(2) 0.059(12) 0.004(14) 0.011(10) 0.055(14) C5 0.066(10) 0.074(10) 0.029(7) -0.007(8) 0.000(7) 0.014(7) C6 0.21(3) 0.073(12) 0.045(10) -0.051(14) 0.041(13) -0.015(9) C7 0.025(9) 0.032(8) 0.019(8) 0.006(7) -0.010(6) 0.001(6) C8 0.072(10) 0.043(7) 0.031(7) 0.010(7) 0.001(7) 0.014(6) C9 0.017(8) 0.033(8) 0.032(9) -0.001(6) -0.001(7) -0.007(7) C10 0.089(17) 0.069(14) 0.029(10) 0.043(12) -0.020(11) -0.003(9) C11 0.078(16) 0.085(16) 0.045(12) -0.013(13) -0.042(12) -0.001(11) C12 0.058(12) 0.21(2) 0.059(12) 0.004(14) 0.011(10) 0.055(14) C13 0.017(7) 0.017(7) 0.027(8) 0.001(6) -0.007(6) -0.005(6) C14 0.019(8) 0.031(8) 0.024(8) -0.009(6) 0.004(6) 0.010(6) C15 0.045(11) 0.030(9) 0.050(11) -0.002(8) -0.020(9) -0.002(8) C16 0.058(13) 0.031(9) 0.083(16) -0.021(9) -0.006(11) 0.009(10) C17 0.090(18) 0.027(10) 0.12(2) 0.021(10) -0.051(16) -0.030(12) C18 0.050(13) 0.031(10) 0.096(17) 0.000(9) -0.011(12) 0.017(10) C19 0.025(8) 0.021(7) 0.009(7) -0.003(6) 0.002(6) -0.004(5) C20 0.038(9) 0.019(7) 0.017(7) 0.007(6) -0.008(7) -0.002(6) C21 0.026(9) 0.025(8) 0.058(12) 0.003(7) 0.018(8) 0.000(8) C22 0.033(11) 0.078(14) 0.063(14) -0.030(10) 0.017(10) -0.011(11) C23 0.047(12) 0.081(15) 0.050(12) 0.008(11) 0.014(10) -0.024(11) C24 0.050(13) 0.065(13) 0.060(14) 0.010(10) 0.017(11) 0.013(11) C25 0.013(7) 0.011(6) 0.033(9) 0.002(5) 0.000(6) 0.001(6) C26 0.012(7) 0.030(8) 0.026(8) 0.001(6) -0.003(6) 0.000(6) C27 0.048(11) 0.028(8) 0.039(10) -0.010(8) 0.021(9) 0.013(7) C28 0.049(13) 0.031(10) 0.100(18) 0.004(9) 0.001(12) 0.020(11) C29 0.025(12) 0.051(13) 0.24(4) 0.014(10) -0.013(17) -0.014(18) C30 0.13(2) 0.027(10) 0.062(14) -0.004(12) 0.029(15) -0.012(10) C31 0.019(7) 0.017(7) 0.024(8) -0.011(6) 0.003(6) 0.003(6) C32 0.030(8) 0.012(6) 0.016(7) 0.003(6) -0.002(6) -0.001(5) C33 0.012(7) 0.032(8) 0.034(9) -0.004(6) 0.009(6) -0.010(7) C34 0.050(12) 0.037(10) 0.057(12) 0.004(8) 0.017(10) 0.013(9) C35 0.028(10) 0.079(14) 0.064(13) -0.003(9) -0.012(9) -0.038(11) C36 0.022(9) 0.074(13) 0.058(13) 0.022(9) 0.002(9) -0.005(10) C37 0.037(9) 0.033(9) 0.017(8) 0.005(7) -0.003(7) 0.000(6) C38 0.052(11) 0.029(8) 0.022(8) -0.001(8) -0.004(8) -0.003(7) C39 0.048(11) 0.027(8) 0.026(9) 0.013(7) -0.002(8) -0.007(7) C40 0.098(18) 0.055(12) 0.032(10) 0.026(12) -0.016(11) -0.017(9) C41 0.056(14) 0.12(2) 0.063(15) -0.042(14) 0.010(12) -0.035(14) C42 0.17(3) 0.053(12) 0.024(10) 0.058(15) -0.006(13) -0.007(9) C43 0.028(9) 0.034(8) 0.017(8) -0.001(7) 0.002(6) -0.008(6) C44 0.029(9) 0.030(8) 0.026(8) 0.000(7) -0.010(7) 0.002(7) C45 0.033(7) 0.036(6) 0.026(6) 0.006(5) 0.000(5) 0.007(5) C46 0.066(10) 0.074(10) 0.029(7) -0.007(8) 0.000(7) 0.014(7) C47 0.061(13) 0.047(11) 0.049(12) 0.006(10) -0.026(10) 0.002(9) C48 0.21(3) 0.073(12) 0.045(10) -0.051(14) 0.041(13) -0.015(9) C49 0.039(10) 0.047(10) 0.018(8) 0.018(8) -0.002(7) -0.010(7) C50 0.057(9) 0.077(10) 0.037(8) 0.019(8) -0.013(7) -0.021(7) C51 0.025(9) 0.040(9) 0.027(9) -0.005(7) 0.004(7) 0.010(7) C52 0.058(13) 0.057(12) 0.045(11) 0.027(10) 0.029(10) 0.000(9) C53 0.088(15) 0.17(2) 0.071(13) -0.022(15) 0.028(12) -0.016(14) C54 0.053(13) 0.096(16) 0.022(9) -0.003(11) -0.002(9) -0.025(10) C55 0.052(12) 0.045(10) 0.026(9) 0.013(9) 0.007(9) -0.009(8) C56 0.057(9) 0.077(10) 0.037(8) 0.019(8) -0.013(7) -0.021(7) C57 0.067(14) 0.044(10) 0.036(10) 0.012(9) -0.014(10) -0.018(8) C58 0.30(4) 0.077(13) 0.084(15) -0.013(17) -0.12(2) -0.011(11) C59 0.30(4) 0.077(13) 0.084(15) -0.013(17) -0.12(2) -0.011(11) C60 0.088(15) 0.17(2) 0.071(13) -0.022(15) 0.028(12) -0.016(14) C61 0.012(7) 0.021(7) 0.024(8) 0.008(6) 0.005(6) -0.006(6) C62 0.020(8) 0.024(7) 0.029(8) -0.002(6) 0.002(7) -0.005(6) C63 0.036(9) 0.015(7) 0.033(9) -0.003(6) -0.006(7) -0.015(6) C64 0.024(10) 0.056(12) 0.12(2) 0.021(9) -0.004(11) -0.020(13) C65 0.032(10) 0.039(10) 0.106(18) -0.019(8) -0.016(11) -0.014(11) C66 0.059(13) 0.038(10) 0.044(11) 0.015(9) -0.021(10) 0.008(8) C67 0.012(7) 0.016(7) 0.036(9) -0.011(5) -0.005(7) -0.002(6) C68 0.022(8) 0.029(8) 0.011(7) 0.009(6) 0.004(6) 0.008(6) C69 0.016(8) 0.039(9) 0.027(8) 0.005(6) -0.008(7) 0.003(7) C70 0.047(11) 0.044(10) 0.040(10) 0.005(8) 0.001(9) -0.016(8) C71 0.022(9) 0.032(9) 0.064(12) 0.011(7) -0.007(8) 0.001(8) C72 0.022(9) 0.055(11) 0.042(10) -0.016(8) 0.003(8) 0.008(8) C73 0.038(9) 0.009(6) 0.025(8) -0.009(6) -0.012(7) -0.006(6) C74 0.028(9) 0.028(8) 0.022(8) 0.005(6) 0.004(7) 0.003(6) C75 0.022(8) 0.042(9) 0.031(9) 0.014(7) -0.009(7) -0.005(7) C76 0.049(12) 0.048(11) 0.040(11) 0.012(9) -0.017(9) -0.004(9) C77 0.019(8) 0.049(10) 0.043(10) -0.009(7) -0.004(7) -0.006(8) C78 0.045(11) 0.070(13) 0.027(9) 0.010(9) -0.017(8) -0.008(9) C79 0.009(6) 0.014(6) 0.017(7) 0.005(5) -0.005(6) -0.002(5) C80 0.014(7) 0.029(8) 0.022(8) -0.012(6) 0.004(6) 0.000(6) C81 0.037(9) 0.018(7) 0.023(8) 0.000(6) 0.007(7) -0.005(6) C82 0.024(9) 0.038(9) 0.061(12) -0.003(7) 0.010(8) 0.010(9) C83 0.042(12) 0.019(8) 0.14(2) -0.007(8) 0.035(13) -0.016(11) C84 0.064(13) 0.029(9) 0.044(11) 0.012(8) -0.005(10) 0.016(8) C85 0.034(10) 0.026(8) 0.030(9) 0.002(7) 0.008(7) 0.007(7) C86 0.030(9) 0.024(8) 0.031(9) 0.006(6) 0.010(7) -0.005(7) C87 0.060(12) 0.023(8) 0.043(11) -0.007(8) 0.013(9) -0.006(7) C88 0.075(14) 0.034(9) 0.050(12) -0.014(9) 0.047(11) -0.018(9) C89 0.056(12) 0.034(9) 0.050(11) 0.003(8) 0.039(10) -0.004(8) C90 0.075(15) 0.048(11) 0.043(11) -0.007(10) 0.004(11) -0.022(9) C91 0.061(12) 0.018(8) 0.022(8) -0.006(7) 0.006(8) -0.005(6) C92 0.083(16) 0.035(10) 0.049(12) 0.011(10) 0.014(11) 0.021(9) C93 0.050(11) 0.037(9) 0.023(8) 0.002(8) -0.003(8) 0.003(7) C94 0.074(16) 0.091(17) 0.057(14) 0.051(14) 0.030(12) 0.026(13) C95 0.055(15) 0.039(12) 0.17(3) 0.008(11) 0.008(17) 0.024(15) C96 0.13(2) 0.052(12) 0.031(11) 0.015(13) -0.006(12) 0.016(9) _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_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Hf1 O7 . 2.118(10) ? Hf1 O5 . 2.134(9) ? Hf1 O8 . 2.158(10) ? Hf1 O2 . 2.165(10) ? Hf1 O6 . 2.174(10) ? Hf1 O3 . 2.186(10) ? Hf1 O1 . 2.258(11) ? Hf1 O4 . 2.262(11) ? Hf1 C7 . 2.585(15) ? Hf1 C1 . 2.604(16) ? Hf2 O11 . 2.105(9) ? Hf2 O10 . 2.114(9) ? Hf2 O12 . 2.160(10) ? Hf2 O9 . 2.164(9) ? Hf2 O16 . 2.171(9) ? Hf2 O13 . 2.191(10) ? Hf2 O15 . 2.271(9) ? Hf2 O14 . 2.280(10) ? Hf2 C37 . 2.618(15) ? Hf2 C43 . 2.629(15) ? Hf3 O21 . 2.116(10) ? Hf3 O24 . 2.144(10) ? Hf3 O23 . 2.146(10) ? Hf3 O22 . 2.174(9) ? Hf3 O19 . 2.184(10) ? Hf3 O18 . 2.186(10) ? Hf3 O20 . 2.255(10) ? Hf3 O17 . 2.270(10) ? Hf3 C55 . 2.600(17) ? Hf3 C49 . 2.605(18) ? Hf4 O27 . 2.141(9) ? Hf4 O26 . 2.146(9) ? Hf4 O25 . 2.162(9) ? Hf4 O28 . 2.175(9) ? Hf4 O30 . 2.186(10) ? Hf4 O31 . 2.205(10) ? Hf4 O29 . 2.258(9) ? Hf4 O32 . 2.276(10) ? Hf4 C85 . 2.608(15) ? Hf4 C91 . 2.612(16) ? O1 C1 . 1.257(18) ? O2 C1 . 1.291(19) ? O3 C7 . 1.269(18) ? O4 C7 . 1.268(17) ? O5 C13 . 1.273(17) ? O6 C19 . 1.260(15) ? O7 C25 . 1.292(16) ? O8 C31 . 1.289(17) ? O9 C25 . 1.230(16) ? O10 C31 . 1.257(16) ? O11 C19 . 1.288(16) ? O12 C13 . 1.270(16) ? O13 C37 . 1.256(17) ? O14 C37 . 1.285(18) ? O15 C43 . 1.284(17) ? O16 C43 . 1.281(17) ? O17 C49 . 1.254(18) ? O18 C49 . 1.304(19) ? O19 C55 . 1.29(2) ? O20 C55 . 1.273(18) ? O21 C61 . 1.224(16) ? O22 C67 . 1.260(17) ? O23 C73 . 1.287(17) ? O24 C79 . 1.262(15) ? O25 C79 . 1.245(16) ? O26 C73 . 1.263(17) ? O27 C67 . 1.291(17) ? O28 C61 . 1.303(16) ? O29 C85 . 1.231(18) ? O30 C85 . 1.288(18) ? O31 C91 . 1.282(17) ? O32 C91 . 1.252(19) ? C1 C2 . 1.49(2) ? C2 C3 . 1.48(2) ? C2 H2A . 0.99 ? C2 H2B . 0.99 ? C3 C6 . 1.37(3) ? C3 C4 . 1.51(3) ? C3 C5 . 1.55(2) ? C4 H4A . 0.98 ? C4 H4B . 0.98 ? C4 H4C . 0.98 ? C5 H5A . 0.98 ? C5 H5B . 0.98 ? C5 H5C . 0.98 ? C6 H6A . 0.98 ? C6 H6B . 0.98 ? C6 H6C . 0.98 ? C7 C8 . 1.52(2) ? C8 C9 . 1.51(2) ? C8 H8A . 0.99 ? C8 H8B . 0.99 ? C9 C10 . 1.52(2) ? C9 C11 . 1.53(2) ? C9 C12 . 1.58(3) ? C10 H10A . 0.98 ? C10 H10B . 0.98 ? C10 H10C . 0.98 ? C11 H11A . 0.98 ? C11 H11B . 0.98 ? C11 H11C . 0.98 ? C12 H12A . 0.98 ? C12 H12B . 0.98 ? C12 H12C . 0.98 ? C13 C14 . 1.505(18) ? C14 C15 . 1.55(2) ? C14 H14A . 0.99 ? C14 H14B . 0.99 ? C15 C16 . 1.52(2) ? C15 C18 . 1.53(3) ? C15 C17 . 1.55(3) ? C16 H16A . 0.98 ? C16 H16B . 0.98 ? C16 H16C . 0.98 ? C17 H17A . 0.98 ? C17 H17B . 0.98 ? C17 H17C . 0.98 ? C18 H18A . 0.98 ? C18 H18B . 0.98 ? C18 H18C . 0.98 ? C19 C20 . 1.481(19) ? C20 C21 . 1.56(2) ? C20 H20A . 0.99 ? C20 H20B . 0.99 ? C21 C22 . 1.52(3) ? C21 C24 . 1.52(3) ? C21 C23 . 1.54(2) ? C22 H22A . 0.98 ? C22 H22B . 0.98 ? C22 H22C . 0.98 ? C23 H23A . 0.98 ? C23 H23B . 0.98 ? C23 H23C . 0.98 ? C24 H24A . 0.98 ? C24 H24B . 0.98 ? C24 H24C . 0.98 ? C25 C26 . 1.506(18) ? C26 C27 . 1.58(2) ? C26 H26A . 0.99 ? C26 H26B . 0.99 ? C27 C28 . 1.50(2) ? C27 C29 . 1.52(3) ? C27 C30 . 1.57(3) ? C28 H28A . 0.98 ? C28 H28B . 0.98 ? C28 H28C . 0.98 ? C29 H29A . 0.98 ? C29 H29B . 0.98 ? C29 H29C . 0.98 ? C30 H30A . 0.98 ? C30 H30B . 0.98 ? C30 H30C . 0.98 ? C31 C32 . 1.493(19) ? C32 C33 . 1.550(19) ? C32 H32A . 0.99 ? C32 H32B . 0.99 ? C33 C35 . 1.52(2) ? C33 C36 . 1.53(2) ? C33 C34 . 1.55(2) ? C34 H34A . 0.98 ? C34 H34B . 0.98 ? C34 H34C . 0.98 ? C35 H35A . 0.98 ? C35 H35B . 0.98 ? C35 H35C . 0.98 ? C36 H36A . 0.98 ? C36 H36B . 0.98 ? C36 H36C . 0.98 ? C37 C38 . 1.50(2) ? C38 C39 . 1.50(2) ? C38 H38A . 0.99 ? C38 H38B . 0.99 ? C39 C42 . 1.53(2) ? C39 C41 . 1.54(3) ? C39 C40 . 1.57(2) ? C40 H40A . 0.98 ? C40 H40B . 0.98 ? C40 H40C . 0.98 ? C41 H41A . 0.98 ? C41 H41B . 0.98 ? C41 H41C . 0.98 ? C42 H42A . 0.98 ? C42 H42B . 0.98 ? C42 H42C . 0.98 ? C43 C44 . 1.47(2) ? C44 C45 . 1.57(2) ? C44 H44A . 0.99 ? C44 H44B . 0.99 ? C45 C47 . 1.48(2) ? C45 C46 . 1.53(3) ? C45 C48 . 1.55(3) ? C46 H46A . 0.98 ? C46 H46B . 0.98 ? C46 H46C . 0.98 ? C47 H47A . 0.98 ? C47 H47B . 0.98 ? C47 H47C . 0.98 ? C48 H48A . 0.98 ? C48 H48B . 0.98 ? C48 H48C . 0.98 ? C49 C50 . 1.49(3) ? C50 C51 . 1.58(2) ? C50 H50A . 0.99 ? C50 H50B . 0.99 ? C51 C52 . 1.49(2) ? C51 C53 . 1.52(3) ? C51 C54 . 1.57(2) ? C52 H52A . 0.98 ? C52 H52B . 0.98 ? C52 H52C . 0.98 ? C53 H53A . 0.98 ? C53 H53B . 0.98 ? C53 H53C . 0.98 ? C54 H54A . 0.98 ? C54 H54B . 0.98 ? C54 H54C . 0.98 ? C55 C56 . 1.48(2) ? C56 C57 . 1.46(3) ? C56 H56A . 0.99 ? C56 H56B . 0.99 ? C57 C58 . 1.45(3) ? C57 C60 . 1.46(3) ? C57 C59 . 1.48(3) ? C58 H58A . 0.98 ? C58 H58B . 0.98 ? C58 H58C . 0.98 ? C59 H59A . 0.98 ? C59 H59B . 0.98 ? C59 H59C . 0.98 ? C60 H60A . 0.98 ? C60 H60B . 0.98 ? C60 H60C . 0.98 ? C61 C62 . 1.509(19) ? C62 C63 . 1.561(18) ? C62 H62A . 0.99 ? C62 H62B . 0.99 ? C63 C64 . 1.48(2) ? C63 C66 . 1.53(2) ? C63 C65 . 1.58(2) ? C64 H64A . 0.98 ? C64 H64B . 0.98 ? C64 H64C . 0.98 ? C65 H65A . 0.98 ? C65 H65B . 0.98 ? C65 H65C . 0.98 ? C66 H66A . 0.98 ? C66 H66B . 0.98 ? C66 H66C . 0.98 ? C67 C68 . 1.509(19) ? C68 C69 . 1.55(2) ? C68 H68A . 0.99 ? C68 H68B . 0.99 ? C69 C72 . 1.51(2) ? C69 C71 . 1.57(2) ? C69 C70 . 1.59(2) ? C70 H70A . 0.98 ? C70 H70B . 0.98 ? C70 H70C . 0.98 ? C71 H71A . 0.98 ? C71 H71B . 0.98 ? C71 H71C . 0.98 ? C72 H72A . 0.98 ? C72 H72B . 0.98 ? C72 H72C . 0.98 ? C73 C74 . 1.48(2) ? C74 C75 . 1.58(2) ? C74 H74A . 0.99 ? C74 H74B . 0.99 ? C75 C76 . 1.50(2) ? C75 C77 . 1.54(2) ? C75 C78 . 1.56(2) ? C76 H76A . 0.98 ? C76 H76B . 0.98 ? C76 H76C . 0.98 ? C77 H77A . 0.98 ? C77 H77B . 0.98 ? C77 H77C . 0.98 ? C78 H78A . 0.98 ? C78 H78B . 0.98 ? C78 H78C . 0.98 ? C79 C80 . 1.526(17) ? C80 C81 . 1.530(19) ? C80 H80A . 0.99 ? C80 H80B . 0.99 ? C81 C84 . 1.49(2) ? C81 C83 . 1.52(2) ? C81 C82 . 1.54(2) ? C82 H82A . 0.98 ? C82 H82B . 0.98 ? C82 H82C . 0.98 ? C83 H83A . 0.98 ? C83 H83B . 0.98 ? C83 H83C . 0.98 ? C84 H84A . 0.98 ? C84 H84B . 0.98 ? C84 H84C . 0.98 ? C85 C86 . 1.50(2) ? C86 C87 . 1.56(2) ? C86 H86A . 0.99 ? C86 H86B . 0.99 ? C87 C90 . 1.51(3) ? C87 C88 . 1.51(2) ? C87 C89 . 1.56(2) ? C88 H88A . 0.98 ? C88 H88B . 0.98 ? C88 H88C . 0.98 ? C89 H89A . 0.98 ? C89 H89B . 0.98 ? C89 H89C . 0.98 ? C90 H90A . 0.98 ? C90 H90B . 0.98 ? C90 H90C . 0.98 ? C91 C92 . 1.57(2) ? C92 C93 . 1.50(2) ? C92 H92A . 0.99 ? C92 H92B . 0.99 ? C93 C95 . 1.46(3) ? C93 C94 . 1.51(3) ? C93 C96 . 1.56(2) ? C94 H94A . 0.98 ? C94 H94B . 0.98 ? C94 H94C . 0.98 ? C95 H95A . 0.98 ? C95 H95B . 0.98 ? C95 H95C . 0.98 ? C96 H96A . 0.98 ? C96 H96B . 0.98 ? C96 H96C . 0.98 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O7 Hf1 O5 . . 105.8(4) ? O7 Hf1 O8 . . 79.0(4) ? O5 Hf1 O8 . . 76.8(4) ? O7 Hf1 O2 . . 87.2(4) ? O5 Hf1 O2 . . 150.1(4) ? O8 Hf1 O2 . . 132.8(4) ? O7 Hf1 O6 . . 76.6(4) ? O5 Hf1 O6 . . 78.9(3) ? O8 Hf1 O6 . . 139.1(4) ? O2 Hf1 O6 . . 78.2(4) ? O7 Hf1 O3 . . 150.1(4) ? O5 Hf1 O3 . . 88.4(4) ? O8 Hf1 O3 . . 78.9(4) ? O2 Hf1 O3 . . 93.3(4) ? O6 Hf1 O3 . . 132.8(4) ? O7 Hf1 O1 . . 77.1(4) ? O5 Hf1 O1 . . 149.9(4) ? O8 Hf1 O1 . . 74.4(4) ? O2 Hf1 O1 . . 58.5(4) ? O6 Hf1 O1 . . 129.8(4) ? O3 Hf1 O1 . . 77.7(4) ? O7 Hf1 O4 . . 149.6(4) ? O5 Hf1 O4 . . 76.2(4) ? O8 Hf1 O4 . . 129.6(4) ? O2 Hf1 O4 . . 79.3(4) ? O6 Hf1 O4 . . 74.0(4) ? O3 Hf1 O4 . . 58.7(4) ? O1 Hf1 O4 . . 116.7(4) ? O7 Hf1 C7 . . 172.8(4) ? O5 Hf1 C7 . . 81.2(4) ? O8 Hf1 C7 . . 104.8(4) ? O2 Hf1 C7 . . 85.8(4) ? O6 Hf1 C7 . . 103.4(4) ? O3 Hf1 C7 . . 29.4(4) ? O1 Hf1 C7 . . 97.8(4) ? O4 Hf1 C7 . . 29.4(4) ? O7 Hf1 C1 . . 80.7(5) ? O5 Hf1 C1 . . 173.4(5) ? O8 Hf1 C1 . . 103.2(4) ? O2 Hf1 C1 . . 29.6(4) ? O6 Hf1 C1 . . 104.6(4) ? O3 Hf1 C1 . . 85.1(5) ? O1 Hf1 C1 . . 28.9(4) ? O4 Hf1 C1 . . 99.2(5) ? C7 Hf1 C1 . . 92.5(5) ? O11 Hf2 O10 . . 106.5(4) ? O11 Hf2 O12 . . 75.7(4) ? O10 Hf2 O12 . . 79.9(4) ? O11 Hf2 O9 . . 80.6(4) ? O10 Hf2 O9 . . 76.5(4) ? O12 Hf2 O9 . . 140.0(3) ? O11 Hf2 O16 . . 150.9(4) ? O10 Hf2 O16 . . 88.4(4) ? O12 Hf2 O16 . . 132.5(4) ? O9 Hf2 O16 . . 78.8(4) ? O11 Hf2 O13 . . 89.2(4) ? O10 Hf2 O13 . . 150.0(4) ? O12 Hf2 O13 . . 79.5(4) ? O9 Hf2 O13 . . 132.2(3) ? O16 Hf2 O13 . . 89.6(4) ? O11 Hf2 O15 . . 148.8(4) ? O10 Hf2 O15 . . 76.6(4) ? O12 Hf2 O15 . . 74.4(4) ? O9 Hf2 O15 . . 129.2(4) ? O16 Hf2 O15 . . 58.2(4) ? O13 Hf2 O15 . . 77.0(4) ? O11 Hf2 O14 . . 77.6(4) ? O10 Hf2 O14 . . 149.4(4) ? O12 Hf2 O14 . . 129.5(4) ? O9 Hf2 O14 . . 74.3(4) ? O16 Hf2 O14 . . 77.2(4) ? O13 Hf2 O14 . . 57.9(4) ? O15 Hf2 O14 . . 115.9(4) ? O11 Hf2 C37 . . 82.1(4) ? O10 Hf2 C37 . . 171.3(4) ? O12 Hf2 C37 . . 104.4(4) ? O9 Hf2 C37 . . 103.6(4) ? O16 Hf2 C37 . . 83.1(4) ? O13 Hf2 C37 . . 28.6(4) ? O15 Hf2 C37 . . 97.0(4) ? O14 Hf2 C37 . . 29.4(4) ? O11 Hf2 C43 . . 170.0(4) ? O10 Hf2 C43 . . 83.1(4) ? O12 Hf2 C43 . . 103.6(4) ? O9 Hf2 C43 . . 105.2(4) ? O16 Hf2 C43 . . 29.0(4) ? O13 Hf2 C43 . . 80.8(4) ? O15 Hf2 C43 . . 29.2(4) ? O14 Hf2 C43 . . 95.8(4) ? C37 Hf2 C43 . . 88.5(4) ? O21 Hf3 O24 . . 105.6(3) ? O21 Hf3 O23 . . 77.0(4) ? O24 Hf3 O23 . . 79.0(4) ? O21 Hf3 O22 . . 78.8(3) ? O24 Hf3 O22 . . 76.3(3) ? O23 Hf3 O22 . . 139.0(4) ? O21 Hf3 O19 . . 89.2(4) ? O24 Hf3 O19 . . 148.8(4) ? O23 Hf3 O19 . . 77.9(4) ? O22 Hf3 O19 . . 134.3(4) ? O21 Hf3 O18 . . 149.6(4) ? O24 Hf3 O18 . . 88.9(4) ? O23 Hf3 O18 . . 132.8(4) ? O22 Hf3 O18 . . 78.9(4) ? O19 Hf3 O18 . . 91.7(4) ? O21 Hf3 O20 . . 77.1(4) ? O24 Hf3 O20 . . 150.3(4) ? O23 Hf3 O20 . . 129.4(4) ? O22 Hf3 O20 . . 75.3(4) ? O19 Hf3 O20 . . 59.0(4) ? O18 Hf3 O20 . . 77.3(4) ? O21 Hf3 O17 . . 150.3(3) ? O24 Hf3 O17 . . 75.3(4) ? O23 Hf3 O17 . . 74.1(4) ? O22 Hf3 O17 . . 128.6(4) ? O19 Hf3 O17 . . 78.5(4) ? O18 Hf3 O17 . . 58.8(4) ? O20 Hf3 O17 . . 117.2(4) ? O21 Hf3 C55 . . 82.9(5) ? O24 Hf3 C55 . . 171.4(5) ? O23 Hf3 C55 . . 104.7(5) ? O22 Hf3 C55 . . 104.6(5) ? O19 Hf3 C55 . . 29.7(4) ? O18 Hf3 C55 . . 82.9(5) ? O20 Hf3 C55 . . 29.3(4) ? O17 Hf3 C55 . . 98.1(5) ? O21 Hf3 C49 . . 173.6(4) ? O24 Hf3 C49 . . 80.5(4) ? O23 Hf3 C49 . . 102.8(4) ? O22 Hf3 C49 . . 104.7(4) ? O19 Hf3 C49 . . 84.6(5) ? O18 Hf3 C49 . . 30.0(4) ? O20 Hf3 C49 . . 98.5(5) ? O17 Hf3 C49 . . 28.8(4) ? C55 Hf3 C49 . . 91.1(5) ? O27 Hf4 O26 . . 107.3(4) ? O27 Hf4 O25 . . 78.5(3) ? O26 Hf4 O25 . . 76.1(3) ? O27 Hf4 O28 . . 76.6(3) ? O26 Hf4 O28 . . 80.2(4) ? O25 Hf4 O28 . . 138.5(4) ? O27 Hf4 O30 . . 85.8(4) ? O26 Hf4 O30 . . 152.5(3) ? O25 Hf4 O30 . . 131.0(3) ? O28 Hf4 O30 . . 79.5(4) ? O27 Hf4 O31 . . 150.1(3) ? O26 Hf4 O31 . . 85.3(4) ? O25 Hf4 O31 . . 78.5(4) ? O28 Hf4 O31 . . 132.9(4) ? O30 Hf4 O31 . . 95.1(4) ? O27 Hf4 O29 . . 77.7(4) ? O26 Hf4 O29 . . 147.7(4) ? O25 Hf4 O29 . . 73.7(3) ? O28 Hf4 O29 . . 131.0(4) ? O30 Hf4 O29 . . 57.6(3) ? O31 Hf4 O29 . . 77.8(4) ? O27 Hf4 O32 . . 149.8(4) ? O26 Hf4 O32 . . 78.8(4) ? O25 Hf4 O32 . . 131.0(4) ? O28 Hf4 O32 . . 75.3(4) ? O30 Hf4 O32 . . 78.2(4) ? O31 Hf4 O32 . . 58.0(4) ? O29 Hf4 O32 . . 113.4(4) ? O27 Hf4 C85 . . 79.5(4) ? O26 Hf4 C85 . . 172.0(4) ? O25 Hf4 C85 . . 101.6(4) ? O28 Hf4 C85 . . 105.9(4) ? O30 Hf4 C85 . . 29.5(4) ? O31 Hf4 C85 . . 86.8(5) ? O29 Hf4 C85 . . 28.1(4) ? O32 Hf4 C85 . . 97.6(4) ? O27 Hf4 C91 . . 171.8(4) ? O26 Hf4 C91 . . 80.8(4) ? O25 Hf4 C91 . . 105.4(5) ? O28 Hf4 C91 . . 103.8(4) ? O30 Hf4 C91 . . 86.2(5) ? O31 Hf4 C91 . . 29.3(4) ? O29 Hf4 C91 . . 96.4(4) ? O32 Hf4 C91 . . 28.6(4) ? C85 Hf4 C91 . . 92.6(5) ? C1 O1 Hf1 . . 91.0(9) ? C1 O2 Hf1 . . 94.4(9) ? C7 O3 Hf1 . . 93.0(9) ? C7 O4 Hf1 . . 89.6(9) ? C13 O5 Hf1 . . 163.5(9) ? C19 O6 Hf1 . . 130.5(9) ? C25 O7 Hf1 . . 161.9(9) ? C31 O8 Hf1 . . 130.1(9) ? C25 O9 Hf2 . . 128.6(9) ? C31 O10 Hf2 . . 162.9(9) ? C19 O11 Hf2 . . 165.2(9) ? C13 O12 Hf2 . . 130.3(9) ? C37 O13 Hf2 . . 94.9(9) ? C37 O14 Hf2 . . 90.0(8) ? C43 O15 Hf2 . . 91.0(8) ? C43 O16 Hf2 . . 95.7(9) ? C49 O17 Hf3 . . 90.6(10) ? C49 O18 Hf3 . . 93.1(9) ? C55 O19 Hf3 . . 93.3(9) ? C55 O20 Hf3 . . 90.6(10) ? C61 O21 Hf3 . . 167.4(9) ? C67 O22 Hf3 . . 131.5(9) ? C73 O23 Hf3 . . 130.9(9) ? C79 O24 Hf3 . . 160.1(9) ? C79 O25 Hf4 . . 130.9(8) ? C73 O26 Hf4 . . 161.9(9) ? C67 O27 Hf4 . . 162.5(9) ? C61 O28 Hf4 . . 128.1(9) ? C85 O29 Hf4 . . 92.0(9) ? C85 O30 Hf4 . . 93.7(9) ? C91 O31 Hf4 . . 93.2(9) ? C91 O32 Hf4 . . 90.7(9) ? O1 C1 O2 . . 116.1(14) ? O1 C1 C2 . . 124.7(15) ? O2 C1 C2 . . 118.9(15) ? O1 C1 Hf1 . . 60.1(8) ? O2 C1 Hf1 . . 56.0(7) ? C2 C1 Hf1 . . 172.0(13) ? C3 C2 C1 . . 120.1(15) ? C3 C2 H2A . . 107.3 ? C1 C2 H2A . . 107.3 ? C3 C2 H2B . . 107.3 ? C1 C2 H2B . . 107.3 ? H2A C2 H2B . . 106.9 ? C6 C3 C2 . . 111.2(19) ? C6 C3 C4 . . 113.(2) ? C2 C3 C4 . . 105.2(16) ? C6 C3 C5 . . 111.5(16) ? C2 C3 C5 . . 110.4(14) ? C4 C3 C5 . . 105.6(17) ? C3 C4 H4A . . 109.5 ? C3 C4 H4B . . 109.5 ? H4A C4 H4B . . 109.5 ? C3 C4 H4C . . 109.5 ? H4A C4 H4C . . 109.5 ? H4B C4 H4C . . 109.5 ? C3 C5 H5A . . 109.5 ? C3 C5 H5B . . 109.5 ? H5A C5 H5B . . 109.5 ? C3 C5 H5C . . 109.5 ? H5A C5 H5C . . 109.5 ? H5B C5 H5C . . 109.5 ? C3 C6 H6A . . 109.5 ? C3 C6 H6B . . 109.5 ? H6A C6 H6B . . 109.5 ? C3 C6 H6C . . 109.5 ? H6A C6 H6C . . 109.5 ? H6B C6 H6C . . 109.5 ? O4 C7 O3 . . 118.7(13) ? O4 C7 C8 . . 120.4(14) ? O3 C7 C8 . . 120.9(14) ? O4 C7 Hf1 . . 61.1(7) ? O3 C7 Hf1 . . 57.6(7) ? C8 C7 Hf1 . . 177.6(11) ? C9 C8 C7 . . 114.1(14) ? C9 C8 H8A . . 108.7 ? C7 C8 H8A . . 108.7 ? C9 C8 H8B . . 108.7 ? C7 C8 H8B . . 108.7 ? H8A C8 H8B . . 107.6 ? C8 C9 C10 . . 110.7(14) ? C8 C9 C11 . . 108.6(14) ? C10 C9 C11 . . 108.4(16) ? C8 C9 C12 . . 110.2(15) ? C10 C9 C12 . . 108.2(18) ? C11 C9 C12 . . 110.7(18) ? 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 ? C9 C11 H11A . . 109.5 ? C9 C11 H11B . . 109.5 ? H11A C11 H11B . . 109.5 ? C9 C11 H11C . . 109.5 ? H11A C11 H11C . . 109.5 ? H11B C11 H11C . . 109.5 ? C9 C12 H12A . . 109.5 ? C9 C12 H12B . . 109.5 ? H12A C12 H12B . . 109.5 ? C9 C12 H12C . . 109.5 ? H12A C12 H12C . . 109.5 ? H12B C12 H12C . . 109.5 ? O12 C13 O5 . . 122.6(12) ? O12 C13 C14 . . 117.6(13) ? O5 C13 C14 . . 119.9(12) ? C13 C14 C15 . . 111.2(12) ? C13 C14 H14A . . 109.4 ? C15 C14 H14A . . 109.4 ? C13 C14 H14B . . 109.4 ? C15 C14 H14B . . 109.4 ? H14A C14 H14B . . 108.0 ? C16 C15 C18 . . 109.1(15) ? C16 C15 C17 . . 109.9(16) ? C18 C15 C17 . . 112.9(17) ? C16 C15 C14 . . 106.6(15) ? C18 C15 C14 . . 110.4(13) ? C17 C15 C14 . . 107.8(13) ? C15 C16 H16A . . 109.5 ? C15 C16 H16B . . 109.5 ? H16A C16 H16B . . 109.5 ? C15 C16 H16C . . 109.5 ? H16A C16 H16C . . 109.5 ? H16B C16 H16C . . 109.5 ? C15 C17 H17A . . 109.5 ? C15 C17 H17B . . 109.5 ? H17A C17 H17B . . 109.5 ? C15 C17 H17C . . 109.5 ? H17A C17 H17C . . 109.5 ? H17B C17 H17C . . 109.5 ? C15 C18 H18A . . 109.5 ? C15 C18 H18B . . 109.5 ? H18A C18 H18B . . 109.5 ? C15 C18 H18C . . 109.5 ? H18A C18 H18C . . 109.5 ? H18B C18 H18C . . 109.5 ? O6 C19 O11 . . 121.7(12) ? O6 C19 C20 . . 118.0(12) ? O11 C19 C20 . . 120.3(11) ? C19 C20 C21 . . 114.1(11) ? C19 C20 H20A . . 108.7 ? C21 C20 H20A . . 108.7 ? C19 C20 H20B . . 108.7 ? C21 C20 H20B . . 108.7 ? H20A C20 H20B . . 107.6 ? C22 C21 C24 . . 110.5(15) ? C22 C21 C23 . . 107.8(16) ? C24 C21 C23 . . 113.1(15) ? C22 C21 C20 . . 107.5(13) ? C24 C21 C20 . . 110.4(14) ? C23 C21 C20 . . 107.3(13) ? C21 C22 H22A . . 109.5 ? C21 C22 H22B . . 109.5 ? H22A C22 H22B . . 109.5 ? C21 C22 H22C . . 109.5 ? H22A C22 H22C . . 109.5 ? H22B C22 H22C . . 109.5 ? C21 C23 H23A . . 109.5 ? C21 C23 H23B . . 109.5 ? H23A C23 H23B . . 109.5 ? C21 C23 H23C . . 109.5 ? H23A C23 H23C . . 109.5 ? H23B C23 H23C . . 109.5 ? C21 C24 H24A . . 109.5 ? C21 C24 H24B . . 109.5 ? H24A C24 H24B . . 109.5 ? C21 C24 H24C . . 109.5 ? H24A C24 H24C . . 109.5 ? H24B C24 H24C . . 109.5 ? O9 C25 O7 . . 125.5(12) ? O9 C25 C26 . . 119.3(12) ? O7 C25 C26 . . 115.0(12) ? C25 C26 C27 . . 112.4(11) ? C25 C26 H26A . . 109.1 ? C27 C26 H26A . . 109.1 ? C25 C26 H26B . . 109.1 ? C27 C26 H26B . . 109.1 ? H26A C26 H26B . . 107.8 ? C28 C27 C29 . . 109.0(17) ? C28 C27 C30 . . 108.5(17) ? C29 C27 C30 . . 112.(2) ? C28 C27 C26 . . 106.7(14) ? C29 C27 C26 . . 111.0(15) ? C30 C27 C26 . . 109.2(14) ? C27 C28 H28A . . 109.5 ? C27 C28 H28B . . 109.5 ? H28A C28 H28B . . 109.5 ? C27 C28 H28C . . 109.5 ? H28A C28 H28C . . 109.5 ? H28B C28 H28C . . 109.5 ? C27 C29 H29A . . 109.5 ? C27 C29 H29B . . 109.5 ? H29A C29 H29B . . 109.5 ? C27 C29 H29C . . 109.5 ? H29A C29 H29C . . 109.5 ? H29B C29 H29C . . 109.5 ? C27 C30 H30A . . 109.5 ? C27 C30 H30B . . 109.5 ? H30A C30 H30B . . 109.5 ? C27 C30 H30C . . 109.5 ? H30A C30 H30C . . 109.5 ? H30B C30 H30C . . 109.5 ? O10 C31 O8 . . 123.7(13) ? O10 C31 C32 . . 118.4(12) ? O8 C31 C32 . . 117.7(12) ? C31 C32 C33 . . 116.4(11) ? C31 C32 H32A . . 108.2 ? C33 C32 H32A . . 108.2 ? C31 C32 H32B . . 108.2 ? C33 C32 H32B . . 108.2 ? H32A C32 H32B . . 107.3 ? C35 C33 C36 . . 109.5(14) ? C35 C33 C34 . . 111.7(15) ? C36 C33 C34 . . 109.0(14) ? C35 C33 C32 . . 108.2(12) ? C36 C33 C32 . . 107.0(12) ? C34 C33 C32 . . 111.3(13) ? C33 C34 H34A . . 109.5 ? C33 C34 H34B . . 109.5 ? H34A C34 H34B . . 109.5 ? C33 C34 H34C . . 109.5 ? H34A C34 H34C . . 109.5 ? H34B C34 H34C . . 109.5 ? C33 C35 H35A . . 109.5 ? C33 C35 H35B . . 109.5 ? H35A C35 H35B . . 109.5 ? C33 C35 H35C . . 109.5 ? H35A C35 H35C . . 109.5 ? H35B C35 H35C . . 109.5 ? C33 C36 H36A . . 109.5 ? C33 C36 H36B . . 109.5 ? H36A C36 H36B . . 109.5 ? C33 C36 H36C . . 109.5 ? H36A C36 H36C . . 109.5 ? H36B C36 H36C . . 109.5 ? O13 C37 O14 . . 117.1(13) ? O13 C37 C38 . . 119.5(14) ? O14 C37 C38 . . 123.1(14) ? O13 C37 Hf2 . . 56.5(7) ? O14 C37 Hf2 . . 60.6(7) ? C38 C37 Hf2 . . 174.9(11) ? C37 C38 C39 . . 118.7(14) ? C37 C38 H38A . . 107.6 ? C39 C38 H38A . . 107.6 ? C37 C38 H38B . . 107.6 ? C39 C38 H38B . . 107.6 ? H38A C38 H38B . . 107.1 ? C38 C39 C42 . . 110.8(15) ? C38 C39 C41 . . 110.3(15) ? C42 C39 C41 . . 111.8(19) ? C38 C39 C40 . . 106.6(14) ? C42 C39 C40 . . 107.7(14) ? C41 C39 C40 . . 109.5(15) ? C39 C40 H40A . . 109.5 ? C39 C40 H40B . . 109.5 ? H40A C40 H40B . . 109.5 ? C39 C40 H40C . . 109.5 ? H40A C40 H40C . . 109.5 ? H40B C40 H40C . . 109.5 ? C39 C41 H41A . . 109.5 ? C39 C41 H41B . . 109.5 ? H41A C41 H41B . . 109.5 ? C39 C41 H41C . . 109.5 ? H41A C41 H41C . . 109.5 ? H41B C41 H41C . . 109.5 ? C39 C42 H42A . . 109.5 ? C39 C42 H42B . . 109.5 ? H42A C42 H42B . . 109.5 ? C39 C42 H42C . . 109.5 ? H42A C42 H42C . . 109.5 ? H42B C42 H42C . . 109.5 ? O16 C43 O15 . . 114.7(13) ? O16 C43 C44 . . 124.8(13) ? O15 C43 C44 . . 120.2(13) ? O16 C43 Hf2 . . 55.2(7) ? O15 C43 Hf2 . . 59.7(7) ? C44 C43 Hf2 . . 179.3(11) ? C43 C44 C45 . . 114.5(12) ? C43 C44 H44A . . 108.6 ? C45 C44 H44A . . 108.6 ? C43 C44 H44B . . 108.6 ? C45 C44 H44B . . 108.6 ? H44A C44 H44B . . 107.6 ? C47 C45 C46 . . 112.1(14) ? C47 C45 C48 . . 107.0(19) ? C46 C45 C48 . . 108.7(16) ? C47 C45 C44 . . 108.2(13) ? C46 C45 C44 . . 111.3(14) ? C48 C45 C44 . . 109.4(14) ? C45 C46 H46A . . 109.5 ? C45 C46 H46B . . 109.5 ? H46A C46 H46B . . 109.5 ? C45 C46 H46C . . 109.5 ? H46A C46 H46C . . 109.5 ? H46B C46 H46C . . 109.5 ? C45 C47 H47A . . 109.5 ? C45 C47 H47B . . 109.5 ? H47A C47 H47B . . 109.5 ? C45 C47 H47C . . 109.5 ? H47A C47 H47C . . 109.5 ? H47B C47 H47C . . 109.5 ? C45 C48 H48A . . 109.5 ? C45 C48 H48B . . 109.5 ? H48A C48 H48B . . 109.5 ? C45 C48 H48C . . 109.5 ? H48A C48 H48C . . 109.5 ? H48B C48 H48C . . 109.5 ? O17 C49 O18 . . 117.5(15) ? O17 C49 C50 . . 124.2(16) ? O18 C49 C50 . . 118.2(15) ? O17 C49 Hf3 . . 60.6(9) ? O18 C49 Hf3 . . 56.9(8) ? C50 C49 Hf3 . . 175.1(13) ? C49 C50 C51 . . 113.4(15) ? C49 C50 H50A . . 108.9 ? C51 C50 H50A . . 108.9 ? C49 C50 H50B . . 108.9 ? C51 C50 H50B . . 108.9 ? H50A C50 H50B . . 107.7 ? C52 C51 C53 . . 109.8(18) ? C52 C51 C54 . . 111.9(16) ? C53 C51 C54 . . 107.8(17) ? C52 C51 C50 . . 113.2(14) ? C53 C51 C50 . . 107.9(17) ? C54 C51 C50 . . 106.1(13) ? C51 C52 H52A . . 109.5 ? C51 C52 H52B . . 109.5 ? H52A C52 H52B . . 109.5 ? C51 C52 H52C . . 109.5 ? H52A C52 H52C . . 109.5 ? H52B C52 H52C . . 109.5 ? C51 C53 H53A . . 109.5 ? C51 C53 H53B . . 109.5 ? H53A C53 H53B . . 109.5 ? C51 C53 H53C . . 109.5 ? H53A C53 H53C . . 109.5 ? H53B C53 H53C . . 109.5 ? C51 C54 H54A . . 109.5 ? C51 C54 H54B . . 109.5 ? H54A C54 H54B . . 109.5 ? C51 C54 H54C . . 109.5 ? H54A C54 H54C . . 109.5 ? H54B C54 H54C . . 109.5 ? O20 C55 O19 . . 117.0(14) ? O20 C55 C56 . . 124.9(16) ? O19 C55 C56 . . 117.9(14) ? O20 C55 Hf3 . . 60.1(8) ? O19 C55 Hf3 . . 57.0(8) ? C56 C55 Hf3 . . 174.6(13) ? C57 C56 C55 . . 123.8(16) ? C57 C56 H56A . . 106.4 ? C55 C56 H56A . . 106.4 ? C57 C56 H56B . . 106.4 ? C55 C56 H56B . . 106.4 ? H56A C56 H56B . . 106.4 ? C58 C57 C60 . . 116.(3) ? C58 C57 C56 . . 109.(2) ? C60 C57 C56 . . 106.(2) ? C58 C57 C59 . . 108.(2) ? C60 C57 C59 . . 105.(2) ? C56 C57 C59 . . 114.(2) ? C57 C58 H58A . . 109.5 ? C57 C58 H58B . . 109.5 ? H58A C58 H58B . . 109.5 ? C57 C58 H58C . . 109.5 ? H58A C58 H58C . . 109.5 ? H58B C58 H58C . . 109.5 ? C57 C59 H59A . . 109.5 ? C57 C59 H59B . . 109.5 ? H59A C59 H59B . . 109.5 ? C57 C59 H59C . . 109.5 ? H59A C59 H59C . . 109.5 ? H59B C59 H59C . . 109.5 ? C57 C60 H60A . . 109.5 ? C57 C60 H60B . . 109.5 ? H60A C60 H60B . . 109.5 ? C57 C60 H60C . . 109.5 ? H60A C60 H60C . . 109.5 ? H60B C60 H60C . . 109.5 ? O21 C61 O28 . . 122.7(13) ? O21 C61 C62 . . 121.3(13) ? O28 C61 C62 . . 115.9(12) ? C61 C62 C63 . . 112.3(11) ? C61 C62 H62A . . 109.1 ? C63 C62 H62A . . 109.1 ? C61 C62 H62B . . 109.1 ? C63 C62 H62B . . 109.1 ? H62A C62 H62B . . 107.9 ? C64 C63 C66 . . 111.5(16) ? C64 C63 C62 . . 112.1(14) ? C66 C63 C62 . . 111.6(12) ? C64 C63 C65 . . 108.3(14) ? C66 C63 C65 . . 106.3(14) ? C62 C63 C65 . . 106.7(13) ? C63 C64 H64A . . 109.5 ? C63 C64 H64B . . 109.5 ? H64A C64 H64B . . 109.5 ? C63 C64 H64C . . 109.5 ? H64A C64 H64C . . 109.5 ? H64B C64 H64C . . 109.5 ? C63 C65 H65A . . 109.5 ? C63 C65 H65B . . 109.5 ? H65A C65 H65B . . 109.5 ? C63 C65 H65C . . 109.5 ? H65A C65 H65C . . 109.5 ? H65B C65 H65C . . 109.5 ? C63 C66 H66A . . 109.5 ? C63 C66 H66B . . 109.5 ? H66A C66 H66B . . 109.5 ? C63 C66 H66C . . 109.5 ? H66A C66 H66C . . 109.5 ? H66B C66 H66C . . 109.5 ? O22 C67 O27 . . 122.9(13) ? O22 C67 C68 . . 116.7(12) ? O27 C67 C68 . . 120.4(13) ? C67 C68 C69 . . 112.7(11) ? C67 C68 H68A . . 109.0 ? C69 C68 H68A . . 109.0 ? C67 C68 H68B . . 109.0 ? C69 C68 H68B . . 109.0 ? H68A C68 H68B . . 107.8 ? C72 C69 C68 . . 112.5(12) ? C72 C69 C71 . . 109.9(13) ? C68 C69 C71 . . 106.2(12) ? C72 C69 C70 . . 109.9(13) ? C68 C69 C70 . . 110.5(12) ? C71 C69 C70 . . 107.8(13) ? C69 C70 H70A . . 109.5 ? C69 C70 H70B . . 109.5 ? H70A C70 H70B . . 109.5 ? C69 C70 H70C . . 109.5 ? H70A C70 H70C . . 109.5 ? H70B C70 H70C . . 109.5 ? C69 C71 H71A . . 109.5 ? C69 C71 H71B . . 109.5 ? H71A C71 H71B . . 109.5 ? C69 C71 H71C . . 109.5 ? H71A C71 H71C . . 109.5 ? H71B C71 H71C . . 109.5 ? C69 C72 H72A . . 109.5 ? C69 C72 H72B . . 109.5 ? H72A C72 H72B . . 109.5 ? C69 C72 H72C . . 109.5 ? H72A C72 H72C . . 109.5 ? H72B C72 H72C . . 109.5 ? O26 C73 O23 . . 123.7(13) ? O26 C73 C74 . . 119.3(13) ? O23 C73 C74 . . 117.0(13) ? C73 C74 C75 . . 114.1(12) ? C73 C74 H74A . . 108.7 ? C75 C74 H74A . . 108.7 ? C73 C74 H74B . . 108.7 ? C75 C74 H74B . . 108.7 ? H74A C74 H74B . . 107.6 ? C76 C75 C77 . . 110.9(14) ? C76 C75 C78 . . 111.0(13) ? C77 C75 C78 . . 109.4(14) ? C76 C75 C74 . . 105.6(13) ? C77 C75 C74 . . 109.5(12) ? C78 C75 C74 . . 110.3(13) ? C75 C76 H76A . . 109.5 ? C75 C76 H76B . . 109.5 ? H76A C76 H76B . . 109.5 ? C75 C76 H76C . . 109.5 ? H76A C76 H76C . . 109.5 ? H76B C76 H76C . . 109.5 ? C75 C77 H77A . . 109.5 ? C75 C77 H77B . . 109.5 ? H77A C77 H77B . . 109.5 ? C75 C77 H77C . . 109.5 ? H77A C77 H77C . . 109.5 ? H77B C77 H77C . . 109.5 ? C75 C78 H78A . . 109.5 ? C75 C78 H78B . . 109.5 ? H78A C78 H78B . . 109.5 ? C75 C78 H78C . . 109.5 ? H78A C78 H78C . . 109.5 ? H78B C78 H78C . . 109.5 ? O25 C79 O24 . . 125.7(12) ? O25 C79 C80 . . 118.2(11) ? O24 C79 C80 . . 116.1(12) ? C79 C80 C81 . . 115.2(11) ? C79 C80 H80A . . 108.5 ? C81 C80 H80A . . 108.5 ? C79 C80 H80B . . 108.5 ? C81 C80 H80B . . 108.5 ? H80A C80 H80B . . 107.5 ? C84 C81 C83 . . 110.1(15) ? C84 C81 C80 . . 109.7(12) ? C83 C81 C80 . . 107.2(13) ? C84 C81 C82 . . 109.2(14) ? C83 C81 C82 . . 111.2(13) ? C80 C81 C82 . . 109.5(12) ? C81 C82 H82A . . 109.5 ? C81 C82 H82B . . 109.5 ? H82A C82 H82B . . 109.5 ? C81 C82 H82C . . 109.5 ? H82A C82 H82C . . 109.5 ? H82B C82 H82C . . 109.5 ? C81 C83 H83A . . 109.5 ? C81 C83 H83B . . 109.5 ? H83A C83 H83B . . 109.5 ? C81 C83 H83C . . 109.5 ? H83A C83 H83C . . 109.5 ? H83B C83 H83C . . 109.5 ? C81 C84 H84A . . 109.5 ? C81 C84 H84B . . 109.5 ? H84A C84 H84B . . 109.5 ? C81 C84 H84C . . 109.5 ? H84A C84 H84C . . 109.5 ? H84B C84 H84C . . 109.5 ? O29 C85 O30 . . 116.6(14) ? O29 C85 C86 . . 127.2(14) ? O30 C85 C86 . . 116.1(14) ? O29 C85 Hf4 . . 59.9(8) ? O30 C85 Hf4 . . 56.8(7) ? C86 C85 Hf4 . . 170.3(12) ? C85 C86 C87 . . 115.7(13) ? C85 C86 H86A . . 108.4 ? C87 C86 H86A . . 108.4 ? C85 C86 H86B . . 108.4 ? C87 C86 H86B . . 108.4 ? H86A C86 H86B . . 107.4 ? C90 C87 C88 . . 110.8(16) ? C90 C87 C86 . . 111.5(15) ? C88 C87 C86 . . 111.7(14) ? C90 C87 C89 . . 107.7(15) ? C88 C87 C89 . . 108.1(15) ? C86 C87 C89 . . 106.9(14) ? C87 C88 H88A . . 109.5 ? C87 C88 H88B . . 109.5 ? H88A C88 H88B . . 109.5 ? C87 C88 H88C . . 109.5 ? H88A C88 H88C . . 109.5 ? H88B C88 H88C . . 109.5 ? C87 C89 H89A . . 109.5 ? C87 C89 H89B . . 109.5 ? H89A C89 H89B . . 109.5 ? C87 C89 H89C . . 109.5 ? H89A C89 H89C . . 109.5 ? H89B C89 H89C . . 109.5 ? C87 C90 H90A . . 109.5 ? C87 C90 H90B . . 109.5 ? H90A C90 H90B . . 109.5 ? C87 C90 H90C . . 109.5 ? H90A C90 H90C . . 109.5 ? H90B C90 H90C . . 109.5 ? O32 C91 O31 . . 118.1(14) ? O32 C91 C92 . . 123.3(14) ? O31 C91 C92 . . 118.5(15) ? O32 C91 Hf4 . . 60.6(8) ? O31 C91 Hf4 . . 57.5(8) ? C92 C91 Hf4 . . 175.9(12) ? C93 C92 C91 . . 116.5(16) ? C93 C92 H92A . . 108.2 ? C91 C92 H92A . . 108.2 ? C93 C92 H92B . . 108.2 ? C91 C92 H92B . . 108.2 ? H92A C92 H92B . . 107.3 ? C95 C93 C92 . . 117.1(17) ? C95 C93 C94 . . 106.8(19) ? C92 C93 C94 . . 112.6(17) ? C95 C93 C96 . . 107.7(18) ? C92 C93 C96 . . 106.7(15) ? C94 C93 C96 . . 105.3(16) ? C93 C94 H94A . . 109.5 ? C93 C94 H94B . . 109.5 ? H94A C94 H94B . . 109.5 ? C93 C94 H94C . . 109.5 ? H94A C94 H94C . . 109.5 ? H94B C94 H94C . . 109.5 ? C93 C95 H95A . . 109.5 ? C93 C95 H95B . . 109.5 ? H95A C95 H95B . . 109.5 ? C93 C95 H95C . . 109.5 ? H95A C95 H95C . . 109.5 ? H95B C95 H95C . . 109.5 ? C93 C96 H96A . . 109.5 ? C93 C96 H96B . . 109.5 ? H96A C96 H96B . . 109.5 ? C93 C96 H96C . . 109.5 ? H96A C96 H96C . . 109.5 ? H96B C96 H96C . . 109.5 ? #===END