data_[Ti8Zr2O12(MeCOO)16] _audit_creation_date 2017-08-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C32 H48 O44 Ti8 Zr2, 4(C4 H6 N2)' _chemical_formula_sum 'C48 H72 N8 O44 Ti8 Zr2' _chemical_formula_weight 2030.77 _chemical_melting_point ? 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' 'N' 'N' 0.0061 0.0033 '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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'cubic' _space_group_IT_number 229 _space_group_name_H-M_alt 'I m -3 m' _space_group_name_Hall '-I 4 2 3' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'z+1/2, x+1/2, y+1/2' 'z+1/2, -x+1/2, -y+1/2' '-z+1/2, -x+1/2, y+1/2' '-z+1/2, x+1/2, -y+1/2' 'y+1/2, z+1/2, x+1/2' '-y+1/2, z+1/2, -x+1/2' 'y+1/2, -z+1/2, -x+1/2' '-y+1/2, -z+1/2, x+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' 'y+1/2, -x+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'x+1/2, z+1/2, -y+1/2' '-x+1/2, z+1/2, y+1/2' '-x+1/2, -z+1/2, -y+1/2' 'x+1/2, -z+1/2, y+1/2' 'z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, x+1/2' '-z+1/2, -y+1/2, -x+1/2' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-z+1/2, -x+1/2, -y+1/2' '-z+1/2, x+1/2, y+1/2' 'z+1/2, x+1/2, -y+1/2' 'z+1/2, -x+1/2, y+1/2' '-y+1/2, -z+1/2, -x+1/2' 'y+1/2, -z+1/2, x+1/2' '-y+1/2, z+1/2, x+1/2' 'y+1/2, z+1/2, -x+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -z+1/2, y+1/2' 'x+1/2, -z+1/2, -y+1/2' 'x+1/2, z+1/2, y+1/2' '-x+1/2, z+1/2, -y+1/2' '-z+1/2, -y+1/2, x+1/2' '-z+1/2, y+1/2, -x+1/2' 'z+1/2, -y+1/2, -x+1/2' 'z+1/2, y+1/2, x+1/2' _cell_length_a 24.260(4) _cell_length_b 24.260(4) _cell_length_c 24.260(4) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 14279(7) _cell_formula_units_Z 6 _cell_measurement_reflns_used 9561 _cell_measurement_temperature 100 _cell_measurement_theta_max 29.38 _cell_measurement_theta_min 2.37 _shelx_estimated_absorpt_T_max 0.913 _shelx_estimated_absorpt_T_min 0.913 _exptl_absorpt_coefficient_mu 0.925 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.417 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 6144 _exptl_crystal_preparation ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_unetI/netI 0.0122 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.994 _diffrn_reflns_limit_h_max 33 _diffrn_reflns_limit_h_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_number 92448 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.994 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.727 _diffrn_reflns_theta_min 1.679 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1787 _reflns_number_total 1969 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.321 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.049 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.141 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 86 _refine_ls_number_reflns 1969 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0187 _refine_ls_restrained_S_all 1.141 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+12.8980P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0519 _refine_ls_wR_factor_ref 0.0535 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.5 times of: All C(H,H,H) groups 2. Others Fixed Sof: H00A(0.5) H00B(0.5) H00C(0.5) H00G(0.5) H00H(0.5) H00I(0.5) H00D(0.5) H00E(0.5) H00F(0.5) 3.a Idealised Me refined as rotating group: C009(H00A,H00B,H00C), C00C(H00G,H00H,H00I), C00D(H00D,H00E,H00F) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr01 Zr 0.5000 0.15183(2) 0.5000 0.00922(7) Uani 1 8 d S T P . . Ti02 Ti 0.5000 0.06934(2) 0.60239(2) 0.01106(7) Uani 1 2 d S T P . . O003 O 0.5000 0.0000 0.57718(6) 0.0121(3) Uani 1 4 d S T P . . O004 O 0.44748(3) 0.09957(4) 0.55252(3) 0.01113(18) Uani 1 2 d S T P . . O005 O 0.5000 0.20053(4) 0.57571(4) 0.0160(2) Uani 1 2 d S T P . . O006 O 0.55815(3) 0.04623(3) 0.65898(3) 0.01797(16) Uani 1 1 d . . . . . O007 O 0.5000 0.14165(4) 0.64614(4) 0.0181(2) Uani 1 2 d S T P . . C008 C 0.57445(6) 0.0000 0.67669(6) 0.0144(3) Uani 1 2 d S T P . . C009 C 0.61506(7) 0.0000 0.72311(6) 0.0217(3) Uani 1 2 d S T P . . H00A H 0.6467 0.0232 0.7133 0.033 Uiso 0.5 1 calc GR . . A -1 H00B H 0.6276 -0.0378 0.7300 0.033 Uiso 0.5 1 calc GR . . A -1 H00C H 0.5975 0.0146 0.7564 0.033 Uiso 0.5 1 calc GR . . A -1 C00A C 0.5000 0.18976(6) 0.62639(6) 0.0170(3) Uani 1 2 d S T P . . N00B N 0.71992(8) 0.11451(11) 0.71992(8) 0.0640(6) Uani 1 2 d S T P . . C00C C 0.65071(7) 0.15741(12) 0.65071(7) 0.0541(6) Uani 1 2 d S T P . . H00G H 0.6686 0.1619 0.6148 0.081 Uiso 0.5 1 calc GR . . B -1 H00H H 0.6382 0.1934 0.6641 0.081 Uiso 0.5 1 calc GR . . B -1 H00I H 0.6190 0.1327 0.6469 0.081 Uiso 0.5 1 calc GR . . B -1 C00D C 0.5000 0.23679(7) 0.66649(7) 0.0330(4) Uani 1 2 d S T P . . H00D H 0.4844 0.2696 0.6488 0.050 Uiso 0.5 1 calc GR . . C -1 H00E H 0.5379 0.2445 0.6782 0.050 Uiso 0.5 1 calc GR . . C -1 H00F H 0.4777 0.2270 0.6987 0.050 Uiso 0.5 1 calc GR . . C -1 C00E C 0.68930(8) 0.13418(10) 0.68930(8) 0.0470(5) Uani 1 2 d S T P . . 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 Zr01 0.01019(9) 0.00728(12) 0.01019(9) 0.000 0.000 0.000 Ti02 0.01492(12) 0.00964(12) 0.00862(12) -0.00018(8) 0.000 0.000 O003 0.0159(7) 0.0112(6) 0.0092(6) 0.000 0.000 0.000 O004 0.0115(3) 0.0105(4) 0.0115(3) -0.0003(2) 0.0005(4) 0.0003(2) O005 0.0208(5) 0.0116(5) 0.0156(5) -0.0022(4) 0.000 0.000 O006 0.0236(4) 0.0153(4) 0.0150(3) -0.0004(3) -0.0063(3) -0.0001(3) O007 0.0272(6) 0.0146(5) 0.0124(5) -0.0032(4) 0.000 0.000 C008 0.0149(6) 0.0183(7) 0.0100(6) 0.000 0.0004(5) 0.000 C009 0.0227(8) 0.0245(8) 0.0178(7) 0.000 -0.0086(6) 0.000 C00A 0.0209(7) 0.0142(6) 0.0160(7) -0.0047(5) 0.000 0.000 N00B 0.0661(10) 0.0598(15) 0.0661(10) -0.0009(9) 0.0029(13) -0.0009(9) C00C 0.0535(9) 0.0554(15) 0.0535(9) -0.0099(8) -0.0085(12) -0.0099(8) C00D 0.0598(13) 0.0176(8) 0.0217(8) -0.0095(6) 0.000 0.000 C00E 0.0499(8) 0.0412(12) 0.0499(8) -0.0113(8) 0.0088(11) -0.0113(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_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zr01 Ti02 3.1897(6) . ? Zr01 Ti02 3.1896(6) 70_656 ? Zr01 Ti02 3.1896(6) 50_556 ? Zr01 Ti02 3.1896(6) 21_556 ? Zr01 O004 2.2032(10) 52_655 ? Zr01 O004 2.2032(10) 50_556 ? Zr01 O004 2.2032(10) 3_656 ? Zr01 O004 2.2032(10) . ? Zr01 O005 2.1839(11) 50_556 ? Zr01 O005 2.1839(11) 70_656 ? Zr01 O005 2.1839(11) . ? Zr01 O005 2.1839(11) 21_556 ? Ti02 Ti02 3.3647(7) 2_655 ? Ti02 O003 1.7900(6) . ? Ti02 O004 1.9039(5) 52_655 ? Ti02 O004 1.9039(5) . ? Ti02 O006 2.0469(8) 52_655 ? Ti02 O006 2.0469(8) . ? Ti02 O007 2.0504(11) . ? O003 Ti02 1.7900(6) 2_655 ? O004 Ti02 1.9039(5) 70_656 ? O005 C00A 1.2571(18) . ? O006 C008 1.2645(10) . ? O007 C00A 1.2616(18) . ? C008 O006 1.2644(10) 51 ? C008 C009 1.496(2) . ? C009 H00A 0.9800 . ? C009 H00B 0.9800 . ? C009 H00C 0.9800 . ? C00A C00D 1.499(2) . ? N00B C00E 1.154(4) . ? C00C H00G 0.9800 . ? C00C H00H 0.9800 . ? C00C H00I 0.9800 . ? C00C C00E 1.439(4) . ? C00D H00D 0.9800 . ? C00D H00E 0.9800 . ? C00D H00F 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 Ti02 Zr01 Ti02 66.823(6) 21_556 . ? Ti02 Zr01 Ti02 66.823(6) 70_656 . ? Ti02 Zr01 Ti02 66.823(6) 50_556 70_656 ? Ti02 Zr01 Ti02 102.290(11) 70_656 21_556 ? Ti02 Zr01 Ti02 66.823(6) 50_556 21_556 ? Ti02 Zr01 Ti02 102.290(11) 50_556 . ? O004 Zr01 Ti02 35.774(8) 3_656 50_556 ? O004 Zr01 Ti02 95.13(2) 50_556 21_556 ? O004 Zr01 Ti02 35.774(8) 3_656 21_556 ? O004 Zr01 Ti02 35.774(8) . . ? O004 Zr01 Ti02 35.774(8) 50_556 50_556 ? O004 Zr01 Ti02 35.774(8) 52_655 . ? O004 Zr01 Ti02 95.13(2) 3_656 . ? O004 Zr01 Ti02 95.13(2) 52_655 70_656 ? O004 Zr01 Ti02 95.13(2) 52_655 50_556 ? O004 Zr01 Ti02 35.774(8) . 70_656 ? O004 Zr01 Ti02 35.774(8) 52_655 21_556 ? O004 Zr01 Ti02 35.774(8) 50_556 70_656 ? O004 Zr01 Ti02 95.13(2) . 21_556 ? O004 Zr01 Ti02 95.13(2) 3_656 70_656 ? O004 Zr01 Ti02 95.13(2) 50_556 . ? O004 Zr01 Ti02 95.13(2) . 50_556 ? O004 Zr01 O004 109.75(5) . 3_656 ? O004 Zr01 O004 70.67(2) 52_655 3_656 ? O004 Zr01 O004 70.67(2) 50_556 3_656 ? O004 Zr01 O004 109.75(5) 50_556 52_655 ? O004 Zr01 O004 70.67(2) . 52_655 ? O004 Zr01 O004 70.67(2) . 50_556 ? O005 Zr01 Ti02 173.90(3) 50_556 . ? O005 Zr01 Ti02 173.90(3) 70_656 21_556 ? O005 Zr01 Ti02 109.842(15) 50_556 70_656 ? O005 Zr01 Ti02 173.90(3) 21_556 70_656 ? O005 Zr01 Ti02 109.842(15) 50_556 21_556 ? O005 Zr01 Ti02 71.61(3) 70_656 70_656 ? O005 Zr01 Ti02 109.842(15) 21_556 50_556 ? O005 Zr01 Ti02 173.90(3) . 50_556 ? O005 Zr01 Ti02 109.841(15) 70_656 . ? O005 Zr01 Ti02 71.61(3) 50_556 50_556 ? O005 Zr01 Ti02 71.61(3) . . ? O005 Zr01 Ti02 109.842(15) 70_656 50_556 ? O005 Zr01 Ti02 109.841(15) . 70_656 ? O005 Zr01 Ti02 109.841(15) . 21_556 ? O005 Zr01 Ti02 109.841(15) 21_556 . ? O005 Zr01 Ti02 71.61(3) 21_556 21_556 ? O005 Zr01 O004 142.909(9) 21_556 50_556 ? O005 Zr01 O004 79.92(3) 21_556 52_655 ? O005 Zr01 O004 142.908(9) . 3_656 ? O005 Zr01 O004 79.92(3) 50_556 3_656 ? O005 Zr01 O004 142.909(9) 50_556 . ? O005 Zr01 O004 79.91(3) . 52_655 ? O005 Zr01 O004 79.92(3) 70_656 . ? O005 Zr01 O004 79.92(3) 70_656 50_556 ? O005 Zr01 O004 79.92(3) 21_556 3_656 ? O005 Zr01 O004 142.909(9) 70_656 52_655 ? O005 Zr01 O004 142.909(9) 21_556 . ? O005 Zr01 O004 79.92(3) 50_556 50_556 ? O005 Zr01 O004 142.909(9) 70_656 3_656 ? O005 Zr01 O004 79.91(3) . . ? O005 Zr01 O004 142.908(9) . 50_556 ? O005 Zr01 O004 142.909(9) 50_556 52_655 ? O005 Zr01 O005 114.49(5) 21_556 70_656 ? O005 Zr01 O005 72.98(3) 70_656 50_556 ? O005 Zr01 O005 114.49(5) 50_556 . ? O005 Zr01 O005 72.98(3) 70_656 . ? O005 Zr01 O005 72.98(3) 21_556 50_556 ? O005 Zr01 O005 72.98(3) 21_556 . ? Zr01 Ti02 Ti02 128.853(6) . 2_655 ? O003 Ti02 Zr01 108.88(4) . . ? O003 Ti02 Ti02 19.97(4) . 2_655 ? O003 Ti02 O004 98.34(4) . 52_655 ? O003 Ti02 O004 98.34(4) . . ? O003 Ti02 O006 88.37(4) . . ? O003 Ti02 O006 88.37(4) . 52_655 ? O003 Ti02 O007 168.79(5) . . ? O004 Ti02 Zr01 42.57(3) 52_655 . ? O004 Ti02 Zr01 42.57(3) . . ? O004 Ti02 Ti02 112.65(3) . 2_655 ? O004 Ti02 Ti02 112.66(3) 52_655 2_655 ? O004 Ti02 O004 84.02(6) . 52_655 ? O004 Ti02 O006 173.21(4) 52_655 52_655 ? O004 Ti02 O006 173.21(4) . . ? O004 Ti02 O006 94.04(4) 52_655 . ? O004 Ti02 O006 94.04(4) . 52_655 ? O004 Ti02 O007 89.97(4) 52_655 . ? O004 Ti02 O007 89.97(4) . . ? O006 Ti02 Zr01 133.96(2) 52_655 . ? O006 Ti02 Zr01 133.96(2) . . ? O006 Ti02 Ti02 74.10(2) . 2_655 ? O006 Ti02 Ti02 74.10(2) 52_655 2_655 ? O006 Ti02 O006 87.14(4) . 52_655 ? O006 Ti02 O007 83.52(3) 52_655 . ? O006 Ti02 O007 83.52(3) . . ? O007 Ti02 Zr01 82.33(3) . . ? O007 Ti02 Ti02 148.82(3) . 2_655 ? Ti02 O003 Ti02 140.06(8) 2_655 . ? Ti02 O004 Zr01 101.65(3) 70_656 . ? Ti02 O004 Zr01 101.66(3) . . ? Ti02 O004 Ti02 134.60(5) 70_656 . ? C00A O005 Zr01 135.25(9) . . ? C008 O006 Ti02 133.35(8) . . ? C00A O007 Ti02 126.50(9) . . ? O006 C008 O006 124.99(13) 51 . ? O006 C008 C009 117.50(7) 51 . ? O006 C008 C009 117.50(7) . . ? C008 C009 H00A 109.5 . . ? C008 C009 H00B 109.5 . . ? C008 C009 H00C 109.5 . . ? H00A C009 H00B 109.5 . . ? H00A C009 H00C 109.5 . . ? H00B C009 H00C 109.5 . . ? O005 C00A O007 124.32(13) . . ? O005 C00A C00D 118.45(14) . . ? O007 C00A C00D 117.24(14) . . ? H00G C00C H00H 109.5 . . ? H00G C00C H00I 109.5 . . ? H00H C00C H00I 109.5 . . ? C00E C00C H00G 109.5 . . ? C00E C00C H00H 109.5 . . ? C00E C00C H00I 109.5 . . ? C00A C00D H00D 109.5 . . ? C00A C00D H00E 109.5 . . ? C00A C00D H00F 109.5 . . ? H00D C00D H00E 109.5 . . ? H00D C00D H00F 109.5 . . ? H00E C00D H00F 109.5 . . ? N00B C00E C00C 178.6(3) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.549 -0.758 -0.423 3394.9 682.6 '3 isopropanoland 1/2 acetonitrile' _olex2_submission_special_instructions 'No special instructions were received' data_[Ti8Zr2O12(EtCOO)16] _audit_creation_date 2017-08-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C48 H80 O44 Ti8 Zr2' _chemical_formula_sum 'C48 H80 O44 Ti8 Zr2' _chemical_formula_weight 1926.76 _chemical_melting_point ? 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _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 12.064(3) _cell_length_b 13.543(3) _cell_length_c 13.806(3) _cell_angle_alpha 104.331(3) _cell_angle_beta 109.519(3) _cell_angle_gamma 110.620(3) _cell_volume 1811.3(8) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4052 _cell_measurement_temperature 100 _cell_measurement_theta_max 27.5466 _cell_measurement_theta_min 2.4609 _shelx_estimated_absorpt_T_max 0.889 _shelx_estimated_absorpt_T_min 0.889 _exptl_absorpt_coefficient_mu 1.206 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 976 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0488 _diffrn_reflns_av_unetI/netI 0.0701 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.917 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 23285 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.917 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.661 _diffrn_reflns_theta_min 1.886 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.917 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6896 _reflns_number_total 9407 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.893 _refine_diff_density_min -0.577 _refine_diff_density_rms 0.115 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 468 _refine_ls_number_reflns 9407 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0667 _refine_ls_R_factor_gt 0.0425 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0362P)^2^+0.7151P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0888 _refine_ls_wR_factor_ref 0.0998 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Secondary CH2 refined with riding coordinates: C51(H51A,H51B), C57(H57A,H57B), C62(H62A,H62B), C69(H69A,H69B), C74(H74A, H74B), C79(H79A,H79B), C84(H84A,H84B), C85(H85A,H85B) 2.b Idealised Me refined as rotating group: C47(H47A,H47B,H47C), C72(H72A,H72B,H72C), C75(H75A,H75B,H75C), C78(H78A,H78B, H78C), C81(H81A,H81B,H81C), C88(H88A,H88B,H88C), C89(H89A,H89B,H89C), C93(H93A, H93B,H93C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.35628(3) 1.08766(3) 0.27622(2) 0.01273(8) Uani 1 1 d . . . . . Ti2 Ti 0.66415(5) 1.17100(5) 0.43428(5) 0.01436(12) Uani 1 1 d . . . . . Ti4 Ti 0.42666(5) 0.87972(5) 0.25453(4) 0.01445(12) Uani 1 1 d . . . . . Ti6 Ti 0.20464(5) 0.90745(5) 0.35929(5) 0.01455(12) Uani 1 1 d . . . . . Ti8 Ti 0.44247(6) 1.19870(5) 0.53939(4) 0.01417(12) Uani 1 1 d . . . . . O2 O 0.2912(2) 1.07108(18) 0.40669(16) 0.0147(4) Uani 1 1 d . . . . . O4 O 0.5261(2) 1.20369(17) 0.44404(17) 0.0140(4) Uani 1 1 d . . . . . O6 O 0.4941(2) 0.87958(18) 0.39217(17) 0.0152(4) Uani 1 1 d . . . . . O7 O 0.5206(2) 1.04241(18) 0.29890(17) 0.0147(4) Uani 1 1 d . . . . . O9 O 0.32582(19) 0.90116(17) 0.47217(17) 0.0151(4) Uani 1 1 d . . . . . O12 O 0.2862(2) 0.90895(17) 0.26187(16) 0.0139(4) Uani 1 1 d . . . . . O14 O 0.3174(2) 1.23582(18) 0.31184(17) 0.0180(5) Uani 1 1 d . . . . . O15 O 0.3054(2) 0.99675(19) 0.09969(17) 0.0187(5) Uani 1 1 d . . . . . O17 O 0.6939(2) 1.27066(19) 0.34490(19) 0.0213(5) Uani 1 1 d . . . . . O20 O 0.0375(2) 0.8867(2) 0.23032(18) 0.0204(5) Uani 1 1 d . . . . . O22 O 0.4794(2) 1.21243(19) 0.23307(18) 0.0188(5) Uani 1 1 d . . . . . O24 O 0.3813(2) 1.31237(19) 0.49629(18) 0.0211(5) Uani 1 1 d . . . . . O25 O 0.3164(2) 0.70277(19) 0.18981(18) 0.0252(5) Uani 1 1 d . . . . . O28 O 0.1869(2) 0.8581(2) 0.58596(19) 0.0229(5) Uani 1 1 d . . . . . O30 O 0.3514(2) 0.84981(19) 0.08708(17) 0.0215(5) Uani 1 1 d . . . . . O32 O 0.1414(2) 1.01683(19) 0.17536(17) 0.0179(5) Uani 1 1 d . . . . . O34 O 0.1017(2) 0.72800(19) 0.29078(18) 0.0239(5) Uani 1 1 d . . . . . O35 O 0.5743(2) 0.8509(2) 0.23320(19) 0.0252(5) Uani 1 1 d . . . . . O38 O 0.4009(2) 0.65067(19) 0.32742(18) 0.0251(5) Uani 1 1 d . . . . . O40 O 0.0965(2) 0.9044(2) 0.44540(19) 0.0223(5) Uani 1 1 d . . . . . O42 O 0.1871(2) 0.67896(19) 0.43107(19) 0.0242(5) Uani 1 1 d . . . . . O44 O 0.6604(2) 0.7977(2) 0.36995(19) 0.0245(5) Uani 1 1 d . . . . . C46 C 0.6022(3) 1.2728(3) 0.2677(3) 0.0209(7) Uani 1 1 d . . . . . C47 C 0.5466(5) 1.3196(4) 0.0960(4) 0.0535(13) Uani 1 1 d . . . . . H47A H 0.5375 1.2477 0.0476 0.080 Uiso 1 1 calc GR . . . . H47B H 0.5791 1.3805 0.0708 0.080 Uiso 1 1 calc GR . . . . H47C H 0.4594 1.3066 0.0913 0.080 Uiso 1 1 calc GR . . . . C50 C 0.6527(3) 0.8181(3) 0.2837(3) 0.0221(7) Uani 1 1 d . . . . . C51 C 0.2515(4) 0.8716(3) -0.0812(3) 0.0369(10) Uani 1 1 d . . . . . H51A H 0.2435 0.7944 -0.1155 0.044 Uiso 1 1 calc R . . . . H51B H 0.1607 0.8639 -0.1126 0.044 Uiso 1 1 calc R . . . . C54 C 0.0386(3) 0.9346(3) 0.1623(3) 0.0198(7) Uani 1 1 d . . . . . C56 C 0.3069(3) 0.9092(3) 0.0445(3) 0.0208(7) Uani 1 1 d . . . . . C57 C 0.6448(4) 1.3565(3) 0.2165(3) 0.0313(9) Uani 1 1 d . . . . . H57A H 0.6591 1.4326 0.2632 0.038 Uiso 1 1 calc R . . . . H57B H 0.7315 1.3668 0.2196 0.038 Uiso 1 1 calc R . . . . C59 C 0.3285(3) 0.6288(3) 0.2267(3) 0.0194(7) Uani 1 1 d . . . . . C62 C 0.2560(4) 0.5048(3) 0.1423(3) 0.0320(9) Uani 1 1 d . . . . . H62A H 0.2283 0.4522 0.1781 0.038 Uiso 1 1 calc R . . . . H62B H 0.1750 0.4904 0.0782 0.038 Uiso 1 1 calc R . . . . C63 C 0.3349(3) 1.3105(3) 0.3984(3) 0.0182(7) Uani 1 1 d . . . . . C65 C 0.1096(3) 0.6553(3) 0.3305(3) 0.0213(7) Uani 1 1 d . . . . . C68 C 0.1003(3) 0.8799(3) 0.5289(3) 0.0190(7) Uani 1 1 d . . . . . C69 C 0.0196(4) 0.5284(3) 0.2552(3) 0.0395(10) Uani 1 1 d . . . . . H69A H -0.0402 0.4956 0.2864 0.047 Uiso 1 1 calc R . . . . H69B H 0.0756 0.4895 0.2578 0.047 Uiso 1 1 calc R . . . . C72 C -0.0657(5) 0.4996(4) 0.1332(4) 0.0672(15) Uani 1 1 d . . . . . H72A H -0.1102 0.4156 0.0890 0.101 Uiso 1 1 calc GR . . . . H72B H -0.0091 0.5392 0.1035 0.101 Uiso 1 1 calc GR . . . . H72C H -0.1332 0.5252 0.1279 0.101 Uiso 1 1 calc GR . . . . C74 C 0.3010(4) 1.4042(3) 0.3852(3) 0.0285(8) Uani 1 1 d . . . . . H74A H 0.2120 1.3682 0.3191 0.034 Uiso 1 1 calc R . . . . H74B H 0.3669 1.4561 0.3690 0.034 Uiso 1 1 calc R . . . . C75 C 0.3344(5) 0.9525(6) -0.1128(4) 0.083(2) Uani 1 1 d . . . . . H75A H 0.2886 0.9286 -0.1945 0.124 Uiso 1 1 calc GR . . . . H75B H 0.4204 0.9523 -0.0914 0.124 Uiso 1 1 calc GR . . . . H75C H 0.3498 1.0307 -0.0735 0.124 Uiso 1 1 calc GR . . . . C78 C 0.2989(5) 1.4770(4) 0.4874(4) 0.0477(12) Uani 1 1 d . . . . . H78A H 0.2807 1.5386 0.4735 0.072 Uiso 1 1 calc GR . . . . H78B H 0.3858 1.5116 0.5540 0.072 Uiso 1 1 calc GR . . . . H78C H 0.2287 1.4277 0.5006 0.072 Uiso 1 1 calc GR . . . . C79 C -0.0895(3) 0.8859(3) 0.0556(3) 0.0326(9) Uani 1 1 d . . . . . H79A H -0.1011 0.9499 0.0395 0.039 Uiso 1 1 calc R . . . . H79B H -0.1666 0.8401 0.0649 0.039 Uiso 1 1 calc R . . . . C81 C 0.0021(4) 0.8571(4) 0.6635(3) 0.0367(10) Uani 1 1 d . . . . . H81A H 0.0001 0.7824 0.6554 0.055 Uiso 1 1 calc GR . . . . H81B H -0.0723 0.8583 0.6769 0.055 Uiso 1 1 calc GR . . . . H81C H 0.0869 0.9197 0.7274 0.055 Uiso 1 1 calc GR . . . . C84 C 0.7464(4) 0.8034(4) 0.2400(3) 0.0382(10) Uani 1 1 d . . . . . H84A H 0.8382 0.8666 0.2940 0.046 Uiso 1 1 calc R . . . . H84B H 0.7221 0.8114 0.1674 0.046 Uiso 1 1 calc R . . . . C85 C -0.0107(3) 0.8735(3) 0.5578(3) 0.0276(8) Uani 1 1 d . . . . . H85A H -0.0167 0.9458 0.5648 0.033 Uiso 1 1 calc R . . . . H85B H -0.0959 0.8086 0.4940 0.033 Uiso 1 1 calc R . . . . C88 C -0.0839(5) 0.8096(4) -0.0413(3) 0.0564(14) Uani 1 1 d . . . . . H88A H -0.1700 0.7722 -0.1094 0.085 Uiso 1 1 calc GR . . . . H88B H -0.0652 0.7501 -0.0224 0.085 Uiso 1 1 calc GR . . . . H88C H -0.0130 0.8569 -0.0550 0.085 Uiso 1 1 calc GR . . . . C89 C 0.7459(5) 0.6888(4) 0.2219(4) 0.0580(14) Uani 1 1 d . . . . . H89A H 0.6584 0.6260 0.1616 0.087 Uiso 1 1 calc GR . . . . H89B H 0.7636 0.6775 0.2918 0.087 Uiso 1 1 calc GR . . . . H89C H 0.8155 0.6884 0.2004 0.087 Uiso 1 1 calc GR . . . . C93 C 0.3481(6) 0.4831(5) 0.1017(6) 0.102(2) Uani 1 1 d . . . . . H93A H 0.3010 0.4041 0.0428 0.153 Uiso 1 1 calc GR . . . . H93B H 0.4250 0.4922 0.1647 0.153 Uiso 1 1 calc GR . . . . H93C H 0.3793 0.5387 0.0706 0.153 Uiso 1 1 calc GR . . . . 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 0.01448(15) 0.01596(15) 0.01162(14) 0.00765(12) 0.00664(12) 0.00925(12) Ti2 0.0138(3) 0.0172(3) 0.0152(3) 0.0094(2) 0.0071(2) 0.0084(2) Ti4 0.0191(3) 0.0168(3) 0.0123(3) 0.0077(2) 0.0080(2) 0.0116(2) Ti6 0.0134(3) 0.0181(3) 0.0147(3) 0.0095(2) 0.0067(2) 0.0082(2) Ti8 0.0184(3) 0.0166(3) 0.0122(3) 0.0076(2) 0.0077(2) 0.0114(2) O2 0.0167(11) 0.0200(11) 0.0115(10) 0.0079(9) 0.0073(9) 0.0113(9) O4 0.0157(11) 0.0153(11) 0.0142(10) 0.0079(9) 0.0070(9) 0.0095(9) O6 0.0201(11) 0.0178(11) 0.0136(11) 0.0082(9) 0.0092(9) 0.0124(10) O7 0.0168(11) 0.0186(11) 0.0143(11) 0.0088(9) 0.0085(9) 0.0114(9) O9 0.0129(10) 0.0175(11) 0.0163(11) 0.0090(9) 0.0073(9) 0.0068(9) O12 0.0151(11) 0.0165(11) 0.0121(10) 0.0068(9) 0.0067(9) 0.0086(9) O14 0.0226(12) 0.0199(12) 0.0173(11) 0.0089(10) 0.0100(10) 0.0145(10) O15 0.0238(12) 0.0246(12) 0.0127(11) 0.0086(10) 0.0092(10) 0.0154(10) O17 0.0223(12) 0.0250(13) 0.0246(13) 0.0172(11) 0.0127(10) 0.0128(10) O20 0.0151(11) 0.0290(13) 0.0186(12) 0.0147(10) 0.0065(10) 0.0099(10) O22 0.0199(12) 0.0230(12) 0.0194(12) 0.0135(10) 0.0113(10) 0.0110(10) O24 0.0310(13) 0.0242(13) 0.0163(11) 0.0107(10) 0.0108(10) 0.0201(11) O25 0.0316(14) 0.0191(12) 0.0172(12) 0.0072(10) 0.0042(11) 0.0111(11) O28 0.0225(12) 0.0374(14) 0.0243(12) 0.0211(11) 0.0148(11) 0.0204(11) O30 0.0322(13) 0.0245(13) 0.0144(11) 0.0096(10) 0.0113(10) 0.0187(11) O32 0.0162(11) 0.0218(12) 0.0172(11) 0.0099(10) 0.0065(9) 0.0105(10) O34 0.0218(12) 0.0198(12) 0.0187(12) 0.0077(10) 0.0021(10) 0.0057(10) O35 0.0351(14) 0.0392(15) 0.0232(13) 0.0207(12) 0.0197(11) 0.0286(12) O38 0.0332(14) 0.0203(12) 0.0168(12) 0.0083(10) 0.0051(11) 0.0137(11) O40 0.0224(12) 0.0367(14) 0.0230(12) 0.0207(11) 0.0149(10) 0.0197(11) O42 0.0251(13) 0.0198(12) 0.0212(12) 0.0100(10) 0.0058(10) 0.0078(10) O44 0.0323(14) 0.0393(15) 0.0231(12) 0.0199(11) 0.0189(11) 0.0279(12) C46 0.0304(19) 0.0197(17) 0.0212(17) 0.0107(14) 0.0169(16) 0.0145(15) C47 0.063(3) 0.062(3) 0.048(3) 0.042(3) 0.028(3) 0.028(3) C50 0.0269(18) 0.0300(19) 0.0204(17) 0.0138(15) 0.0159(15) 0.0177(16) C51 0.065(3) 0.040(2) 0.0164(18) 0.0129(17) 0.0168(19) 0.037(2) C54 0.0196(17) 0.0259(18) 0.0169(16) 0.0095(14) 0.0084(14) 0.0136(15) C56 0.0274(18) 0.0243(18) 0.0161(16) 0.0112(14) 0.0123(15) 0.0138(15) C57 0.033(2) 0.034(2) 0.033(2) 0.0235(18) 0.0175(18) 0.0136(18) C59 0.0189(16) 0.0156(16) 0.0199(17) 0.0062(14) 0.0074(14) 0.0066(14) C62 0.041(2) 0.0187(18) 0.0225(19) 0.0061(15) 0.0064(17) 0.0106(17) C63 0.0195(16) 0.0184(16) 0.0241(17) 0.0123(14) 0.0118(14) 0.0125(14) C65 0.0215(17) 0.0198(17) 0.0233(18) 0.0085(14) 0.0114(15) 0.0097(14) C68 0.0168(16) 0.0223(17) 0.0198(16) 0.0100(14) 0.0083(14) 0.0106(14) C69 0.037(2) 0.024(2) 0.030(2) 0.0067(17) 0.0007(18) 0.0052(18) C72 0.067(3) 0.048(3) 0.043(3) 0.006(2) 0.000(3) 0.016(3) C74 0.043(2) 0.028(2) 0.0274(19) 0.0151(16) 0.0160(18) 0.0276(18) C75 0.044(3) 0.143(6) 0.029(3) 0.042(3) 0.016(2) 0.008(3) C78 0.077(3) 0.047(3) 0.043(3) 0.024(2) 0.029(2) 0.049(3) C79 0.0161(17) 0.045(2) 0.027(2) 0.0212(18) 0.0027(15) 0.0064(17) C81 0.036(2) 0.057(3) 0.041(2) 0.033(2) 0.029(2) 0.027(2) C84 0.048(2) 0.066(3) 0.044(2) 0.039(2) 0.037(2) 0.045(2) C85 0.0257(19) 0.044(2) 0.033(2) 0.0230(18) 0.0215(17) 0.0240(18) C88 0.068(3) 0.035(3) 0.025(2) 0.0039(19) -0.004(2) 0.013(2) C89 0.054(3) 0.052(3) 0.076(4) 0.010(3) 0.043(3) 0.032(3) C93 0.104(5) 0.059(4) 0.116(6) -0.013(4) 0.068(5) 0.028(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 Ti2 3.2005(10) . ? Zr1 Ti4 3.1904(9) . ? Zr1 Ti6 3.2034(8) . ? Zr1 Ti8 3.1957(10) . ? Zr1 O2 2.221(2) . ? Zr1 O4 2.189(2) . ? Zr1 O7 2.223(2) . ? Zr1 O12 2.196(2) . ? Zr1 O14 2.194(2) . ? Zr1 O15 2.194(2) . ? Zr1 O22 2.177(2) . ? Zr1 O32 2.181(2) . ? Ti2 Ti6 3.3801(9) 2_676 ? Ti2 O4 1.905(2) . ? Ti2 O7 1.904(2) . ? Ti2 O9 1.800(2) 2_676 ? Ti2 O17 2.062(2) . ? Ti2 O28 2.060(2) 2_676 ? Ti2 O42 2.034(2) 2_676 ? Ti4 Ti8 3.3749(9) 2_676 ? Ti4 O6 1.801(2) . ? Ti4 O7 1.904(2) . ? Ti4 O12 1.898(2) . ? Ti4 O25 2.052(2) . ? Ti4 O30 2.051(2) . ? Ti4 O35 2.049(2) . ? Ti6 Ti2 3.3801(9) 2_676 ? Ti6 O2 1.904(2) . ? Ti6 O9 1.790(2) . ? Ti6 O12 1.914(2) . ? Ti6 O20 2.067(2) . ? Ti6 O34 2.072(2) . ? Ti6 O40 2.035(2) . ? Ti8 Ti4 3.3749(9) 2_676 ? Ti8 O2 1.911(2) . ? Ti8 O4 1.908(2) . ? Ti8 O6 1.785(2) 2_676 ? Ti8 O24 2.057(2) . ? Ti8 O38 2.054(2) 2_676 ? Ti8 O44 2.040(2) 2_676 ? O6 Ti8 1.785(2) 2_676 ? O9 Ti2 1.800(2) 2_676 ? O14 C63 1.256(4) . ? O15 C56 1.250(4) . ? O17 C46 1.269(4) . ? O20 C54 1.267(4) . ? O22 C46 1.254(4) . ? O24 C63 1.268(4) . ? O25 C59 1.260(4) . ? O28 Ti2 2.060(2) 2_676 ? O28 C68 1.258(4) . ? O30 C56 1.268(4) . ? O32 C54 1.260(4) . ? O34 C65 1.256(4) . ? O35 C50 1.260(4) . ? O38 Ti8 2.054(2) 2_676 ? O38 C59 1.260(4) . ? O40 C68 1.267(4) . ? O42 Ti2 2.034(2) 2_676 ? O42 C65 1.267(4) . ? O44 Ti8 2.040(2) 2_676 ? O44 C50 1.268(4) . ? C46 C57 1.509(5) . ? C47 C57 1.509(5) . ? C50 C84 1.495(5) . ? C51 C56 1.506(4) . ? C51 C75 1.465(6) . ? C54 C79 1.508(4) . ? C59 C62 1.503(4) . ? C62 C93 1.483(6) . ? C63 C74 1.497(4) . ? C65 C69 1.503(5) . ? C68 C85 1.501(4) . ? C69 C72 1.511(6) . ? C74 C78 1.522(5) . ? C79 C88 1.512(6) . ? C81 C85 1.496(5) . ? C84 C89 1.508(6) . ? 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 Ti2 Zr1 Ti6 102.50(2) . . ? Ti4 Zr1 Ti2 66.781(19) . . ? Ti4 Zr1 Ti6 66.95(2) . . ? Ti4 Zr1 Ti8 102.122(17) . . ? Ti8 Zr1 Ti2 66.897(17) . . ? Ti8 Zr1 Ti6 66.71(2) . . ? O2 Zr1 Ti2 95.48(6) . . ? O2 Zr1 Ti4 95.15(5) . . ? O2 Zr1 Ti6 35.60(5) . . ? O2 Zr1 Ti8 35.93(6) . . ? O2 Zr1 O7 110.00(7) . . ? O4 Zr1 Ti2 35.50(5) . . ? O4 Zr1 Ti4 94.42(5) . . ? O4 Zr1 Ti6 94.64(6) . . ? O4 Zr1 Ti8 35.68(5) . . ? O4 Zr1 O2 70.65(8) . . ? O4 Zr1 O7 70.17(8) . . ? O4 Zr1 O12 108.49(7) . . ? O4 Zr1 O14 80.08(8) . . ? O4 Zr1 O15 142.54(8) . . ? O7 Zr1 Ti2 35.68(5) . . ? O7 Zr1 Ti4 35.86(5) . . ? O7 Zr1 Ti6 95.39(6) . . ? O7 Zr1 Ti8 95.08(5) . . ? O12 Zr1 Ti2 94.70(5) . . ? O12 Zr1 Ti4 35.57(5) . . ? O12 Zr1 Ti6 35.73(5) . . ? O12 Zr1 Ti8 94.57(5) . . ? O12 Zr1 O2 70.37(7) . . ? O12 Zr1 O7 70.48(8) . . ? O14 Zr1 Ti2 109.38(6) . . ? O14 Zr1 Ti4 173.48(6) . . ? O14 Zr1 Ti6 109.77(6) . . ? O14 Zr1 Ti8 71.37(6) . . ? O14 Zr1 O2 79.78(8) . . ? O14 Zr1 O7 142.40(8) . . ? O14 Zr1 O12 143.22(8) . . ? O15 Zr1 Ti2 109.25(6) . . ? O15 Zr1 Ti4 71.03(6) . . ? O15 Zr1 Ti6 109.66(6) . . ? O15 Zr1 Ti8 173.15(6) . . ? O15 Zr1 O2 142.70(8) . . ? O15 Zr1 O7 79.30(8) . . ? O15 Zr1 O12 79.93(8) . . ? O15 Zr1 O14 115.48(8) . . ? O22 Zr1 Ti2 71.30(6) . . ? O22 Zr1 Ti4 109.55(6) . . ? O22 Zr1 Ti6 173.80(6) . . ? O22 Zr1 Ti8 109.99(6) . . ? O22 Zr1 O2 143.19(8) . . ? O22 Zr1 O4 80.37(8) . . ? O22 Zr1 O7 79.50(8) . . ? O22 Zr1 O12 142.70(8) . . ? O22 Zr1 O14 73.16(8) . . ? O22 Zr1 O15 73.03(8) . . ? O22 Zr1 O32 114.67(8) . . ? O32 Zr1 Ti2 173.92(6) . . ? O32 Zr1 Ti4 109.07(6) . . ? O32 Zr1 Ti6 71.52(6) . . ? O32 Zr1 Ti8 110.68(6) . . ? O32 Zr1 O2 80.28(8) . . ? O32 Zr1 O4 144.09(8) . . ? O32 Zr1 O7 142.04(8) . . ? O32 Zr1 O12 79.81(8) . . ? O32 Zr1 O14 74.30(8) . . ? O32 Zr1 O15 72.55(8) . . ? Zr1 Ti2 Ti6 128.58(2) . 2_676 ? O4 Ti2 Zr1 41.87(6) . . ? O4 Ti2 Ti6 111.45(6) . 2_676 ? O4 Ti2 O17 90.64(9) . . ? O4 Ti2 O28 175.14(9) . 2_676 ? O4 Ti2 O42 93.62(9) . 2_676 ? O7 Ti2 Zr1 42.91(6) . . ? O7 Ti2 Ti6 113.05(7) . 2_676 ? O7 Ti2 O4 83.51(9) . . ? O7 Ti2 O17 90.29(9) . . ? O7 Ti2 O28 95.61(9) . 2_676 ? O7 Ti2 O42 172.83(9) . 2_676 ? O9 Ti2 Zr1 108.94(7) 2_676 . ? O9 Ti2 Ti6 19.65(6) 2_676 2_676 ? O9 Ti2 O4 97.50(9) 2_676 . ? O9 Ti2 O7 98.65(9) 2_676 . ? O9 Ti2 O17 168.51(9) 2_676 . ? O9 Ti2 O28 87.35(9) 2_676 2_676 ? O9 Ti2 O42 88.22(10) 2_676 2_676 ? O17 Ti2 Zr1 82.53(6) . . ? O17 Ti2 Ti6 148.86(7) . 2_676 ? O28 Ti2 Zr1 136.09(7) 2_676 . ? O28 Ti2 Ti6 73.30(6) 2_676 2_676 ? O28 Ti2 O17 84.58(9) 2_676 . ? O42 Ti2 Zr1 132.66(7) 2_676 . ? O42 Ti2 Ti6 74.11(7) 2_676 2_676 ? O42 Ti2 O17 83.16(9) 2_676 . ? O42 Ti2 O28 86.70(10) 2_676 2_676 ? Zr1 Ti4 Ti8 127.93(2) . 2_676 ? O6 Ti4 Zr1 108.26(7) . . ? O6 Ti4 Ti8 19.66(6) . 2_676 ? O6 Ti4 O7 97.89(9) . . ? O6 Ti4 O12 97.36(9) . . ? O6 Ti4 O25 88.07(9) . . ? O6 Ti4 O30 168.63(9) . . ? O6 Ti4 O35 87.89(9) . . ? O7 Ti4 Zr1 43.16(6) . . ? O7 Ti4 Ti8 111.93(6) . 2_676 ? O7 Ti4 O25 174.04(9) . . ? O7 Ti4 O30 91.29(9) . . ? O7 Ti4 O35 94.14(9) . . ? O12 Ti4 Zr1 42.29(6) . . ? O12 Ti4 Ti8 111.57(6) . 2_676 ? O12 Ti4 O7 84.23(9) . . ? O12 Ti4 O25 95.06(9) . . ? O12 Ti4 O30 90.20(9) . . ? O12 Ti4 O35 174.66(9) . . ? O25 Ti4 Zr1 134.70(7) . . ? O25 Ti4 Ti8 73.85(6) . 2_676 ? O30 Ti4 Zr1 83.04(6) . . ? O30 Ti4 Ti8 149.01(6) . 2_676 ? O30 Ti4 O25 82.79(9) . . ? O35 Ti4 Zr1 134.89(7) . . ? O35 Ti4 Ti8 73.76(6) . 2_676 ? O35 Ti4 O25 86.03(10) . . ? O35 Ti4 O30 84.75(9) . . ? Zr1 Ti6 Ti2 128.91(2) . 2_676 ? O2 Ti6 Zr1 42.77(6) . . ? O2 Ti6 Ti2 112.02(6) . 2_676 ? O2 Ti6 O12 83.61(9) . . ? O2 Ti6 O20 91.91(9) . . ? O2 Ti6 O34 174.06(9) . . ? O2 Ti6 O40 96.18(9) . . ? O9 Ti6 Zr1 109.14(7) . . ? O9 Ti6 Ti2 19.77(6) . 2_676 ? O9 Ti6 O2 97.70(9) . . ? O9 Ti6 O12 98.91(9) . . ? O9 Ti6 O20 168.49(9) . . ? O9 Ti6 O34 87.56(9) . . ? O9 Ti6 O40 88.90(9) . . ? O12 Ti6 Zr1 42.07(6) . . ? O12 Ti6 Ti2 113.05(6) . 2_676 ? O12 Ti6 O20 88.40(9) . . ? O12 Ti6 O34 92.87(9) . . ? O12 Ti6 O40 172.15(9) . . ? O20 Ti6 Zr1 82.24(6) . . ? O20 Ti6 Ti2 148.80(6) . 2_676 ? O20 Ti6 O34 83.19(9) . . ? O34 Ti6 Zr1 132.69(7) . . ? O34 Ti6 Ti2 73.75(6) . 2_676 ? O40 Ti6 Zr1 135.63(7) . . ? O40 Ti6 Ti2 74.34(6) . 2_676 ? O40 Ti6 O20 83.76(9) . . ? O40 Ti6 O34 86.65(10) . . ? Zr1 Ti8 Ti4 129.95(2) . 2_676 ? O2 Ti8 Zr1 43.01(6) . . ? O2 Ti8 Ti4 113.23(7) . 2_676 ? O2 Ti8 O24 90.79(9) . . ? O2 Ti8 O38 172.60(9) . 2_676 ? O2 Ti8 O44 94.05(10) . 2_676 ? O4 Ti8 Zr1 42.02(6) . . ? O4 Ti8 Ti4 113.26(6) . 2_676 ? O4 Ti8 O2 83.81(9) . . ? O4 Ti8 O24 90.00(9) . . ? O4 Ti8 O38 94.41(10) . 2_676 ? O4 Ti8 O44 172.47(9) . 2_676 ? O6 Ti8 Zr1 110.11(7) 2_676 . ? O6 Ti8 Ti4 19.84(6) 2_676 2_676 ? O6 Ti8 O2 99.16(10) 2_676 . ? O6 Ti8 O4 98.91(9) 2_676 . ? O6 Ti8 O24 167.26(9) 2_676 . ? O6 Ti8 O38 88.20(10) 2_676 2_676 ? O6 Ti8 O44 88.55(9) 2_676 2_676 ? O24 Ti8 Zr1 82.59(6) . . ? O24 Ti8 Ti4 147.45(6) . 2_676 ? O38 Ti8 Zr1 133.45(7) 2_676 . ? O38 Ti8 Ti4 74.08(7) 2_676 2_676 ? O38 Ti8 O24 82.02(9) 2_676 . ? O44 Ti8 Zr1 134.05(7) 2_676 . ? O44 Ti8 Ti4 74.22(6) 2_676 2_676 ? O44 Ti8 O24 82.80(9) 2_676 . ? O44 Ti8 O38 86.80(10) 2_676 2_676 ? Ti6 O2 Zr1 101.62(9) . . ? Ti6 O2 Ti8 134.54(11) . . ? Ti8 O2 Zr1 101.07(9) . . ? Ti2 O4 Zr1 102.63(9) . . ? Ti2 O4 Ti8 135.28(11) . . ? Ti8 O4 Zr1 102.31(9) . . ? Ti8 O6 Ti4 140.49(12) 2_676 . ? Ti2 O7 Zr1 101.42(9) . . ? Ti4 O7 Zr1 100.99(9) . . ? Ti4 O7 Ti2 134.94(11) . . ? Ti6 O9 Ti2 140.59(12) . 2_676 ? Ti4 O12 Zr1 102.14(9) . . ? Ti4 O12 Ti6 135.35(11) . . ? Ti6 O12 Zr1 102.21(9) . . ? C63 O14 Zr1 135.7(2) . . ? C56 O15 Zr1 135.8(2) . . ? C46 O17 Ti2 125.4(2) . . ? C54 O20 Ti6 125.5(2) . . ? C46 O22 Zr1 136.1(2) . . ? C63 O24 Ti8 126.2(2) . . ? C59 O25 Ti4 132.8(2) . . ? C68 O28 Ti2 133.6(2) . 2_676 ? C56 O30 Ti4 125.4(2) . . ? C54 O32 Zr1 134.9(2) . . ? C65 O34 Ti6 132.7(2) . . ? C50 O35 Ti4 133.5(2) . . ? C59 O38 Ti8 132.1(2) . 2_676 ? C68 O40 Ti6 133.2(2) . . ? C65 O42 Ti2 133.7(2) . 2_676 ? C50 O44 Ti8 133.0(2) . 2_676 ? O17 C46 C57 117.3(3) . . ? O22 C46 O17 124.7(3) . . ? O22 C46 C57 118.0(3) . . ? O35 C50 O44 125.5(3) . . ? O35 C50 C84 117.6(3) . . ? O44 C50 C84 116.9(3) . . ? C75 C51 C56 113.1(4) . . ? O20 C54 C79 117.9(3) . . ? O32 C54 O20 124.3(3) . . ? O32 C54 C79 117.7(3) . . ? O15 C56 O30 124.6(3) . . ? O15 C56 C51 117.6(3) . . ? O30 C56 C51 117.8(3) . . ? C47 C57 C46 114.7(3) . . ? O25 C59 O38 125.5(3) . . ? O25 C59 C62 117.3(3) . . ? O38 C59 C62 117.1(3) . . ? C93 C62 C59 108.1(3) . . ? O14 C63 O24 124.1(3) . . ? O14 C63 C74 117.8(3) . . ? O24 C63 C74 118.0(3) . . ? O34 C65 O42 125.6(3) . . ? O34 C65 C69 118.9(3) . . ? O42 C65 C69 115.5(3) . . ? O28 C68 O40 125.1(3) . . ? O28 C68 C85 118.7(3) . . ? O40 C68 C85 116.2(3) . . ? C65 C69 C72 115.6(3) . . ? C63 C74 C78 114.7(3) . . ? C54 C79 C88 109.2(3) . . ? C50 C84 C89 114.1(3) . . ? C81 C85 C68 115.9(3) . . ? _olex2_submission_special_instructions 'No special instructions were received' data_[Ti8Zr2O12(PhCOO)16] _audit_creation_date 2017-08-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '2(C112 H80 O44 Ti8 Zr2)' _chemical_formula_sum 'C224 H160 O88 Ti16 Zr4' _chemical_formula_weight 5390.79 _chemical_melting_point ? 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/n 1' _space_group_name_Hall '-P 2yn' loop_ _space_group_symop_operation_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 14.896(4) _cell_length_b 24.070(6) _cell_length_c 15.304(4) _cell_angle_alpha 90 _cell_angle_beta 91.287(4) _cell_angle_gamma 90 _cell_volume 5486(2) _cell_formula_units_Z 1 _cell_measurement_reflns_used 4819 _cell_measurement_temperature 100 _cell_measurement_theta_max 23.4981 _cell_measurement_theta_min 2.6626 _shelx_estimated_absorpt_T_max 0.937 _shelx_estimated_absorpt_T_min 0.922 _exptl_absorpt_coefficient_mu 0.824 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.632 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 2720 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0793 _diffrn_reflns_av_unetI/netI 0.0798 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 48548 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.695 _diffrn_reflns_theta_min 1.887 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean 8 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8972 _reflns_number_total 12788 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 0.532 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.096 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 748 _refine_ls_number_reflns 12788 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0773 _refine_ls_R_factor_gt 0.0475 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0413P)^2^+0.6377P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0987 _refine_ls_wR_factor_ref 0.1108 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2.a Aromatic/amide H refined with riding coordinates: C2(H2), C61(H61), C79(H79), C97(H97), C105(H105), C110(H110), C124(H124), C126(H126), C130(H130), C138(H138), C139(H139), C146(H146), C152(H152), C155(H155), C168(H168), C170(H170), C171(H171), C183(H183), C193(H193), C196(H196), C198(H198), C200(H200), C204(H204), C205(H205), C209(H209), C214(H214), C222(H222), C229(H229), C240(H240), C254(H254), C255(H255), C261(H261), C266(H266), C273(H273), C277(H277), C293(H293), C298(H298), C304(H304), C308(H308), C312(H312) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr2 Zr 1.03185(2) 0.34943(2) 0.53667(2) 0.01538(8) Uani 1 1 d . . . . . Ti1 Ti 0.86037(4) 0.42571(2) 0.56814(4) 0.01744(13) Uani 1 1 d . . . . . Ti7 Ti 0.96016(4) 0.41118(2) 0.36367(4) 0.01743(13) Uani 1 1 d . . . . . Ti12 Ti 1.07264(4) 0.45105(2) 0.66701(4) 0.01677(13) Uani 1 1 d . . . . . Ti16 Ti 1.17149(4) 0.43671(2) 0.46064(4) 0.01737(13) Uani 1 1 d . . . . . C2 C 1.4376(3) 0.58839(17) 0.8789(3) 0.0408(10) Uani 1 1 d . . . . . H2 H 1.4909 0.5997 0.9091 0.049 Uiso 1 1 calc R . . . . O8 O 0.80609(14) 0.35277(9) 0.60773(14) 0.0234(5) Uani 1 1 d . . . . . O10 O 0.92646(14) 0.29752(9) 0.59480(13) 0.0199(5) Uani 1 1 d . . . . . O16 O 0.95160(15) 0.33106(9) 0.31733(14) 0.0220(5) Uani 1 1 d . . . . . O18 O 1.15549(15) 0.30514(9) 0.50501(14) 0.0213(5) Uani 1 1 d . . . . . O20 O 1.08639(14) 0.31683(8) 0.65927(13) 0.0201(5) Uani 1 1 d . . . . . O27 O 0.74055(14) 0.43401(9) 0.50139(15) 0.0250(5) Uani 1 1 d . . . . . O34 O 1.13046(14) 0.41463(8) 0.57251(13) 0.0174(5) Uani 1 1 d . . . . . O38 O 1.07301(14) 0.39364(8) 0.41732(13) 0.0165(5) Uani 1 1 d . . . . . O40 O 0.98364(16) 0.57026(9) 0.75204(14) 0.0254(5) Uani 1 1 d . . . . . O48 O 1.11716(15) 0.38830(9) 0.74890(13) 0.0216(5) Uani 1 1 d . . . . . O52 O 0.99662(14) 0.28637(8) 0.43860(13) 0.0198(5) Uani 1 1 d . . . . . O55 O 1.25359(14) 0.36767(9) 0.45671(14) 0.0224(5) Uani 1 1 d . . . . . O59 O 1.00530(15) 0.47858(9) 0.77341(13) 0.0218(5) Uani 1 1 d . . . . . C61 C 0.6775(2) 0.54797(18) 0.9166(2) 0.0374(10) Uani 1 1 d . . . . . H61 H 0.6719 0.5814 0.9492 0.045 Uiso 1 1 calc R . . . . O64 O 0.78235(15) 0.54594(9) 0.66372(14) 0.0223(5) Uani 1 1 d . . . . . O67 O 1.18649(14) 0.49055(9) 0.71992(14) 0.0224(5) Uani 1 1 d . . . . . O74 O 0.79767(15) 0.45310(9) 0.67597(15) 0.0259(5) Uani 1 1 d . . . . . O77 O 1.15920(15) 0.58199(9) 0.70184(15) 0.0264(6) Uani 1 1 d . . . . . C79 C 1.3653(3) 0.62336(17) 0.8752(2) 0.0402(10) Uani 1 1 d . . . . . H79 H 1.3674 0.6580 0.9048 0.048 Uiso 1 1 calc R . . . . O81 O 0.97135(14) 0.40896(8) 0.62716(13) 0.0170(5) Uani 1 1 d . . . . . O83 O 0.88328(14) 0.49684(8) 0.54157(13) 0.0182(5) Uani 1 1 d . . . . . O89 O 1.04580(14) 0.51543(8) 0.61389(13) 0.0169(5) Uani 1 1 d . . . . . O96 O 0.91416(14) 0.38794(8) 0.47254(13) 0.0178(5) Uani 1 1 d . . . . . C97 C 1.4342(3) 0.53678(18) 0.8395(2) 0.0395(10) Uani 1 1 d . . . . . H97 H 1.4848 0.5128 0.8426 0.047 Uiso 1 1 calc R . . . . O104 O 0.71694(14) 0.52610(9) 0.49121(14) 0.0231(5) Uani 1 1 d . . . . . C105 C 1.2891(3) 0.60793(15) 0.8281(2) 0.0307(9) Uani 1 1 d . . . . . H105 H 1.2397 0.6328 0.8231 0.037 Uiso 1 1 calc R . . . . C110 C 1.3874(3) 0.28458(16) 0.4587(2) 0.0365(9) Uani 1 1 d . . . . . H110 H 1.4083 0.3214 0.4688 0.044 Uiso 1 1 calc R . . . . C121 C 1.2845(2) 0.55597(14) 0.7878(2) 0.0236(8) Uani 1 1 d . . . . . C124 C 0.9730(3) 0.18417(15) 0.3554(3) 0.0440(11) Uani 1 1 d . . . . . H124 H 1.0046 0.1843 0.4100 0.053 Uiso 1 1 calc R . . . . C126 C 0.9513(4) 0.13405(17) 0.3145(3) 0.0653(15) Uani 1 1 d . . . . . H126 H 0.9674 0.0999 0.3417 0.078 Uiso 1 1 calc R . . . . C130 C 0.6525(3) 0.45063(18) 0.9023(2) 0.0410(10) Uani 1 1 d . . . . . H130 H 0.6290 0.4170 0.9249 0.049 Uiso 1 1 calc R . . . . C136 C 0.7965(2) 0.26197(13) 0.6626(2) 0.0216(7) Uani 1 1 d . . . . . C138 C 0.6945(2) 0.45049(16) 0.8227(2) 0.0308(9) Uani 1 1 d . . . . . H138 H 0.7007 0.4169 0.7908 0.037 Uiso 1 1 calc R . . . . C139 C 0.6446(3) 0.4989(2) 0.9491(3) 0.0469(12) Uani 1 1 d . . . . . H139 H 0.6163 0.4985 1.0042 0.056 Uiso 1 1 calc R . . . . C144 C 0.8470(2) 0.30694(14) 0.6184(2) 0.0208(7) Uani 1 1 d . . . . . C146 C 0.9068(4) 0.13396(18) 0.2354(3) 0.0684(16) Uani 1 1 d . . . . . H146 H 0.8939 0.0997 0.2071 0.082 Uiso 1 1 calc R . . . . C152 C 0.9286(2) 0.58293(15) 0.9221(2) 0.0273(8) Uani 1 1 d . . . . . H152 H 0.9474 0.6151 0.8916 0.033 Uiso 1 1 calc R . . . . C153 C 0.7275(2) 0.49991(14) 0.7898(2) 0.0230(7) Uani 1 1 d . . . . . C155 C 0.5828(2) 0.41184(15) 0.4125(2) 0.0316(9) Uani 1 1 d . . . . . H155 H 0.6198 0.3816 0.4304 0.038 Uiso 1 1 calc R . . . . C168 C 1.2537(3) 0.28083(18) 0.9216(2) 0.0416(10) Uani 1 1 d . . . . . H168 H 1.2867 0.2945 0.9709 0.050 Uiso 1 1 calc R . . . . C170 C 0.5027(3) 0.40211(17) 0.3671(3) 0.0399(10) Uani 1 1 d . . . . . H170 H 0.4860 0.3652 0.3516 0.048 Uiso 1 1 calc R . . . . C171 C 0.8930(2) 0.58779(17) 1.0043(2) 0.0351(9) Uani 1 1 d . . . . . H171 H 0.8885 0.6233 1.0309 0.042 Uiso 1 1 calc R . . . . C173 C 1.1633(2) 0.29828(14) 0.7927(2) 0.0213(7) Uani 1 1 d . . . . . C182 C 0.9485(2) 0.23345(14) 0.3161(2) 0.0253(8) Uani 1 1 d . . . . . C183 C 1.1573(2) 0.24150(14) 0.7789(2) 0.0296(8) Uani 1 1 d . . . . . H183 H 1.1241 0.2275 0.7299 0.036 Uiso 1 1 calc R . . . . C193 C 0.8405(2) 0.22006(14) 0.7069(2) 0.0296(8) Uani 1 1 d . . . . . H193 H 0.9042 0.2180 0.7071 0.036 Uiso 1 1 calc R . . . . C196 C 0.9027(3) 0.23253(15) 0.2365(2) 0.0324(9) Uani 1 1 d . . . . . H196 H 0.8860 0.2664 0.2089 0.039 Uiso 1 1 calc R . . . . C198 C 1.4484(3) 0.24215(18) 0.4421(3) 0.0525(12) Uani 1 1 d . . . . . H198 H 1.5111 0.2495 0.4437 0.063 Uiso 1 1 calc R . . . . C200 C 0.8810(3) 0.18218(17) 0.1968(3) 0.0501(12) Uani 1 1 d . . . . . H200 H 0.8483 0.1816 0.1428 0.060 Uiso 1 1 calc R . . . . C204 C 1.2133(2) 0.31773(15) 0.8626(2) 0.0296(8) Uani 1 1 d . . . . . H204 H 1.2204 0.3566 0.8708 0.035 Uiso 1 1 calc R . . . . C205 C 0.7906(3) 0.18062(16) 0.7517(2) 0.0378(10) Uani 1 1 d . . . . . H205 H 0.8205 0.1522 0.7841 0.045 Uiso 1 1 calc R . . . . C208 C 0.6082(2) 0.46529(14) 0.4314(2) 0.0205(7) Uani 1 1 d . . . . . C209 C 0.7030(2) 0.26416(15) 0.6619(2) 0.0337(9) Uani 1 1 d . . . . . H209 H 0.6725 0.2938 0.6328 0.040 Uiso 1 1 calc R . . . . C214 C 1.3284(3) 0.1782(2) 0.4283(5) 0.091(2) Uani 1 1 d . . . . . H214 H 1.3079 0.1412 0.4190 0.109 Uiso 1 1 calc R . . . . C220 C 1.1194(2) 0.33707(13) 0.7293(2) 0.0197(7) Uani 1 1 d . . . . . C222 C 1.3562(2) 0.52024(16) 0.7952(2) 0.0307(9) Uani 1 1 d . . . . . H222 H 1.3524 0.4842 0.7701 0.037 Uiso 1 1 calc R . . . . C229 C 0.7188(2) 0.54870(16) 0.8365(2) 0.0306(9) Uani 1 1 d . . . . . H229 H 0.7411 0.5826 0.8137 0.037 Uiso 1 1 calc R . . . . C232 C 1.2043(2) 0.54100(14) 0.7330(2) 0.0213(7) Uani 1 1 d . . . . . C238 C 0.6942(2) 0.47556(14) 0.4775(2) 0.0207(7) Uani 1 1 d . . . . . C240 C 0.8707(2) 0.48941(16) 1.0096(2) 0.0317(9) Uani 1 1 d . . . . . H240 H 0.8497 0.4575 1.0394 0.038 Uiso 1 1 calc R . . . . C245 C 1.2303(2) 0.31854(14) 0.4755(2) 0.0214(7) Uani 1 1 d . . . . . C250 C 1.2970(2) 0.27311(14) 0.4603(2) 0.0278(8) Uani 1 1 d . . . . . C254 C 1.1996(3) 0.20515(16) 0.8364(2) 0.0388(10) Uani 1 1 d . . . . . H254 H 1.1965 0.1663 0.8260 0.047 Uiso 1 1 calc R . . . . C255 C 0.5519(2) 0.50942(15) 0.4084(2) 0.0279(8) Uani 1 1 d . . . . . H255 H 0.5690 0.5464 0.4225 0.033 Uiso 1 1 calc R . . . . C261 C 0.8639(3) 0.54085(17) 1.0482(2) 0.0364(10) Uani 1 1 d . . . . . H261 H 0.8394 0.5442 1.1047 0.044 Uiso 1 1 calc R . . . . C266 C 1.2674(3) 0.21957(17) 0.4464(3) 0.0554(13) Uani 1 1 d . . . . . H266 H 1.2052 0.2111 0.4493 0.066 Uiso 1 1 calc R . . . . C270 C 0.7726(2) 0.50019(14) 0.7042(2) 0.0213(7) Uani 1 1 d . . . . . C273 C 0.4477(3) 0.44564(17) 0.3446(3) 0.0414(10) Uani 1 1 d . . . . . H273 H 0.3924 0.4387 0.3143 0.050 Uiso 1 1 calc R . . . . C277 C 0.4718(2) 0.49936(16) 0.3654(2) 0.0338(9) Uani 1 1 d . . . . . H277 H 0.4330 0.5293 0.3500 0.041 Uiso 1 1 calc R . . . . C285 C 0.9777(2) 0.52601(14) 0.7969(2) 0.0226(7) Uani 1 1 d . . . . . C290 C 0.9673(2) 0.28727(13) 0.3609(2) 0.0197(7) Uani 1 1 d . . . . . C292 C 0.9367(2) 0.53107(14) 0.8841(2) 0.0226(7) Uani 1 1 d . . . . . C293 C 0.9075(2) 0.48368(15) 0.9280(2) 0.0251(8) Uani 1 1 d . . . . . H293 H 0.9130 0.4480 0.9021 0.030 Uiso 1 1 calc R . . . . C298 C 1.2456(3) 0.22470(17) 0.9081(2) 0.0394(10) Uani 1 1 d . . . . . H298 H 1.2720 0.1994 0.9488 0.047 Uiso 1 1 calc R . . . . C304 C 1.4174(3) 0.18969(19) 0.4235(4) 0.0743(17) Uani 1 1 d . . . . . H304 H 1.4582 0.1614 0.4073 0.089 Uiso 1 1 calc R . . . . C308 C 0.6548(3) 0.22359(16) 0.7031(3) 0.0385(10) Uani 1 1 d . . . . . H308 H 0.5910 0.2240 0.6996 0.046 Uiso 1 1 calc R . . . . C312 C 0.6985(3) 0.18269(16) 0.7491(2) 0.0383(10) Uani 1 1 d . . . . . H312 H 0.6649 0.1555 0.7794 0.046 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 Zr2 0.01917(16) 0.00897(15) 0.01804(15) 0.00081(12) 0.00132(12) 0.00094(12) Ti1 0.0191(3) 0.0114(3) 0.0219(3) 0.0014(2) 0.0030(2) 0.0012(2) Ti7 0.0237(3) 0.0109(3) 0.0177(3) 0.0002(2) 0.0001(2) 0.0015(2) Ti12 0.0224(3) 0.0108(3) 0.0171(3) 0.0005(2) 0.0000(2) 0.0014(2) Ti16 0.0194(3) 0.0109(3) 0.0219(3) 0.0006(2) 0.0037(2) 0.0013(2) C2 0.034(2) 0.047(3) 0.041(2) -0.001(2) -0.0107(19) -0.010(2) O8 0.0232(12) 0.0158(12) 0.0314(13) 0.0030(10) 0.0065(10) 0.0012(10) O10 0.0226(12) 0.0131(12) 0.0240(12) 0.0038(9) 0.0016(10) -0.0006(10) O16 0.0305(13) 0.0117(12) 0.0239(12) -0.0013(9) 0.0004(10) 0.0005(10) O18 0.0220(13) 0.0172(12) 0.0251(12) 0.0004(10) 0.0053(10) 0.0044(10) O20 0.0255(13) 0.0128(12) 0.0221(12) 0.0023(9) 0.0016(10) 0.0014(10) O27 0.0201(12) 0.0140(12) 0.0408(14) 0.0021(10) -0.0022(11) 0.0020(10) O34 0.0197(12) 0.0119(11) 0.0208(11) 0.0010(9) 0.0001(9) 0.0021(9) O38 0.0210(12) 0.0090(11) 0.0196(11) -0.0003(9) 0.0034(9) 0.0031(9) O40 0.0395(15) 0.0149(12) 0.0222(12) 0.0005(10) 0.0076(11) 0.0050(11) O48 0.0301(13) 0.0146(12) 0.0202(11) 0.0009(9) 0.0000(10) 0.0020(10) O52 0.0261(13) 0.0132(12) 0.0202(12) -0.0009(9) 0.0001(10) 0.0009(10) O55 0.0203(12) 0.0150(12) 0.0320(13) 0.0004(10) 0.0037(10) 0.0004(10) O59 0.0311(13) 0.0140(12) 0.0204(12) 0.0003(9) 0.0037(10) 0.0009(10) C61 0.032(2) 0.053(3) 0.028(2) -0.0091(19) 0.0051(17) 0.007(2) O64 0.0271(13) 0.0149(12) 0.0251(12) 0.0024(10) 0.0059(10) -0.0003(10) O67 0.0261(13) 0.0130(12) 0.0279(13) 0.0003(10) -0.0031(10) 0.0004(10) O74 0.0319(14) 0.0169(13) 0.0292(13) 0.0025(10) 0.0105(11) 0.0011(11) O77 0.0310(14) 0.0139(12) 0.0339(14) 0.0004(10) -0.0079(11) 0.0006(10) C79 0.055(3) 0.032(2) 0.034(2) -0.0067(18) -0.0136(19) -0.009(2) O81 0.0199(12) 0.0122(11) 0.0189(11) 0.0019(9) 0.0004(9) 0.0017(9) O83 0.0201(12) 0.0136(12) 0.0212(11) 0.0002(9) 0.0033(9) 0.0014(9) O89 0.0215(12) 0.0109(11) 0.0183(11) 0.0001(9) -0.0007(9) 0.0021(9) O96 0.0215(12) 0.0110(11) 0.0209(11) 0.0005(9) 0.0009(9) -0.0010(9) C97 0.029(2) 0.049(3) 0.040(2) 0.008(2) -0.0050(18) 0.0055(19) O104 0.0221(13) 0.0157(12) 0.0316(13) -0.0004(10) -0.0002(10) 0.0008(10) C105 0.038(2) 0.025(2) 0.0293(19) -0.0014(16) -0.0037(17) -0.0027(17) C110 0.033(2) 0.026(2) 0.051(2) 0.0012(18) 0.0035(19) 0.0063(17) C121 0.0277(19) 0.0193(18) 0.0239(18) 0.0021(14) 0.0007(15) -0.0056(15) C124 0.066(3) 0.019(2) 0.047(2) -0.0047(18) -0.010(2) 0.002(2) C126 0.109(4) 0.012(2) 0.074(3) -0.004(2) -0.017(3) 0.007(2) C130 0.043(3) 0.050(3) 0.031(2) 0.006(2) 0.0060(18) -0.003(2) C136 0.0296(19) 0.0170(18) 0.0182(16) 0.0026(13) 0.0020(14) -0.0073(15) C138 0.027(2) 0.036(2) 0.029(2) 0.0066(17) 0.0052(16) -0.0037(17) C139 0.036(2) 0.075(4) 0.029(2) 0.004(2) 0.0085(19) 0.000(2) C144 0.0244(18) 0.0209(19) 0.0171(16) -0.0014(13) -0.0011(14) -0.0056(15) C146 0.127(5) 0.021(2) 0.056(3) -0.022(2) -0.008(3) -0.009(3) C152 0.031(2) 0.0227(19) 0.0279(19) -0.0028(15) 0.0042(16) 0.0001(16) C153 0.0209(18) 0.0239(19) 0.0243(18) 0.0004(15) 0.0027(14) 0.0013(15) C155 0.032(2) 0.0208(19) 0.042(2) 0.0009(16) -0.0058(17) 0.0027(16) C168 0.048(3) 0.051(3) 0.026(2) 0.0016(19) -0.0057(18) 0.016(2) C170 0.037(2) 0.031(2) 0.051(3) 0.0017(19) -0.012(2) -0.0073(18) C171 0.036(2) 0.037(2) 0.032(2) -0.0104(18) 0.0037(17) 0.0092(18) C173 0.0223(18) 0.0208(18) 0.0209(17) 0.0037(14) 0.0023(14) 0.0063(14) C182 0.030(2) 0.0172(18) 0.0287(19) -0.0034(15) 0.0064(15) -0.0019(15) C183 0.042(2) 0.0181(19) 0.0282(19) 0.0051(15) -0.0004(17) 0.0067(16) C193 0.029(2) 0.024(2) 0.036(2) 0.0055(16) -0.0007(16) -0.0057(16) C196 0.048(2) 0.020(2) 0.0286(19) -0.0011(15) -0.0001(17) -0.0085(17) C198 0.028(2) 0.042(3) 0.088(4) 0.001(3) 0.008(2) 0.013(2) C200 0.087(4) 0.032(2) 0.031(2) -0.0071(19) -0.004(2) -0.018(2) C204 0.037(2) 0.023(2) 0.0286(19) -0.0029(16) 0.0019(16) 0.0081(17) C205 0.048(3) 0.027(2) 0.038(2) 0.0152(17) -0.0024(19) -0.0018(19) C208 0.0190(17) 0.0199(18) 0.0227(17) -0.0017(14) -0.0010(14) -0.0047(14) C209 0.031(2) 0.026(2) 0.045(2) 0.0055(18) 0.0091(18) 0.0005(17) C214 0.046(3) 0.023(3) 0.205(7) -0.021(3) 0.018(4) 0.007(2) C220 0.0196(17) 0.0178(18) 0.0218(17) 0.0055(14) 0.0050(14) 0.0028(14) C222 0.033(2) 0.031(2) 0.0278(19) -0.0002(16) -0.0012(16) 0.0004(17) C229 0.026(2) 0.033(2) 0.033(2) -0.0010(17) 0.0015(16) 0.0035(17) C232 0.0237(18) 0.0184(18) 0.0220(17) -0.0017(14) 0.0054(14) 0.0003(15) C238 0.0202(17) 0.0203(18) 0.0217(17) 0.0017(14) 0.0053(14) -0.0007(14) C240 0.035(2) 0.038(2) 0.0230(19) 0.0057(17) 0.0041(16) -0.0019(18) C245 0.0231(18) 0.0175(18) 0.0237(17) -0.0033(14) 0.0002(14) 0.0027(15) C250 0.026(2) 0.0191(19) 0.038(2) 0.0041(16) 0.0052(16) 0.0059(15) C254 0.056(3) 0.024(2) 0.037(2) 0.0064(17) 0.004(2) 0.0104(19) C255 0.028(2) 0.026(2) 0.031(2) -0.0008(16) 0.0000(16) 0.0035(16) C261 0.036(2) 0.051(3) 0.0229(19) -0.0033(18) 0.0083(17) 0.003(2) C266 0.036(2) 0.020(2) 0.112(4) -0.002(2) 0.013(3) 0.0033(19) C270 0.0172(17) 0.0215(19) 0.0252(18) -0.0002(14) 0.0014(14) -0.0012(14) C273 0.030(2) 0.044(3) 0.049(3) -0.003(2) -0.0121(19) -0.0082(19) C277 0.029(2) 0.037(2) 0.035(2) -0.0012(18) -0.0062(17) 0.0080(18) C285 0.0225(18) 0.0222(19) 0.0230(17) -0.0015(15) 0.0000(14) -0.0019(15) C290 0.0182(17) 0.0133(17) 0.0277(18) -0.0038(14) 0.0049(14) 0.0011(14) C292 0.0236(18) 0.0219(19) 0.0226(17) 0.0015(14) 0.0027(14) 0.0007(15) C293 0.0241(19) 0.024(2) 0.0268(18) 0.0002(15) -0.0006(15) 0.0019(15) C298 0.053(3) 0.036(2) 0.028(2) 0.0124(18) -0.0001(19) 0.019(2) C304 0.038(3) 0.031(3) 0.155(6) -0.010(3) 0.009(3) 0.020(2) C308 0.032(2) 0.038(2) 0.046(2) 0.004(2) 0.0133(19) -0.0056(19) C312 0.047(3) 0.032(2) 0.037(2) 0.0080(18) 0.0114(19) -0.011(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 Zr2 Ti1 3.1911(8) . ? Zr2 Ti7 3.1987(8) . ? Zr2 Ti12 3.2057(8) . ? Zr2 Ti16 3.1940(8) . ? Zr2 O10 2.209(2) . ? Zr2 O18 2.192(2) . ? Zr2 O20 2.174(2) . ? Zr2 O34 2.210(2) . ? Zr2 O38 2.212(2) . ? Zr2 O52 2.190(2) . ? Zr2 O81 2.200(2) . ? Zr2 O96 2.195(2) . ? Ti1 Ti16 3.3731(11) 3_766 ? Ti1 O8 2.031(2) . ? Ti1 O27 2.046(2) . ? Ti1 O74 2.025(2) . ? Ti1 O81 1.909(2) . ? Ti1 O83 1.794(2) . ? Ti1 O96 1.913(2) . ? Ti7 Ti12 3.3832(11) 3_766 ? Ti7 O16 2.058(2) . ? Ti7 O38 1.902(2) . ? Ti7 O40 2.025(2) 3_766 ? Ti7 O77 2.028(2) 3_766 ? Ti7 O89 1.802(2) 3_766 ? Ti7 O96 1.900(2) . ? Ti12 Ti7 3.3833(11) 3_766 ? Ti12 O34 1.913(2) . ? Ti12 O48 2.062(2) . ? Ti12 O59 2.042(2) . ? Ti12 O67 2.091(2) . ? Ti12 O81 1.906(2) . ? Ti12 O89 1.791(2) . ? Ti16 Ti1 3.3730(11) 3_766 ? Ti16 O34 1.906(2) . ? Ti16 O38 1.903(2) . ? Ti16 O55 2.065(2) . ? Ti16 O64 2.080(2) 3_766 ? Ti16 O83 1.795(2) 3_766 ? Ti16 O104 2.013(2) 3_766 ? C2 C79 1.367(5) . ? C2 C97 1.381(5) . ? O8 C144 1.269(4) . ? O10 C144 1.265(4) . ? O16 C290 1.266(4) . ? O18 C245 1.254(4) . ? O20 C220 1.267(4) . ? O27 C238 1.265(4) . ? O40 Ti7 2.026(2) 3_766 ? O40 C285 1.272(4) . ? O48 C220 1.270(4) . ? O52 C290 1.257(4) . ? O55 C245 1.267(4) . ? O59 C285 1.268(4) . ? C61 C139 1.377(6) . ? C61 C229 1.384(5) . ? O64 Ti16 2.080(2) 3_766 ? O64 C270 1.273(4) . ? O67 C232 1.258(4) . ? O74 C270 1.272(4) . ? O77 Ti7 2.028(2) 3_766 ? O77 C232 1.279(4) . ? C79 C105 1.381(5) . ? O83 Ti16 1.796(2) 3_766 ? O89 Ti7 1.802(2) 3_766 ? C97 C222 1.391(5) . ? O104 Ti16 2.013(2) 3_766 ? O104 C238 1.279(4) . ? C105 C121 1.395(5) . ? C110 C198 1.394(5) . ? C110 C250 1.376(5) . ? C121 C222 1.374(5) . ? C121 C232 1.489(4) . ? C124 C126 1.394(5) . ? C124 C182 1.376(5) . ? C126 C146 1.367(6) . ? C130 C138 1.383(5) . ? C130 C139 1.371(6) . ? C136 C144 1.490(4) . ? C136 C193 1.375(5) . ? C136 C209 1.394(5) . ? C138 C153 1.386(5) . ? C146 C200 1.354(6) . ? C152 C171 1.381(5) . ? C152 C292 1.383(4) . ? C153 C229 1.383(5) . ? C153 C270 1.486(5) . ? C155 C170 1.387(5) . ? C155 C208 1.370(5) . ? C168 C204 1.394(5) . ? C168 C298 1.372(5) . ? C170 C273 1.369(5) . ? C171 C261 1.389(5) . ? C173 C183 1.385(4) . ? C173 C204 1.372(4) . ? C173 C220 1.487(4) . ? C182 C196 1.382(5) . ? C182 C290 1.490(4) . ? C183 C254 1.383(5) . ? C193 C205 1.395(5) . ? C196 C200 1.391(5) . ? C198 C304 1.372(6) . ? C205 C312 1.373(5) . ? C208 C238 1.470(4) . ? C208 C255 1.394(4) . ? C209 C308 1.374(5) . ? C214 C266 1.381(6) . ? C214 C304 1.358(6) . ? C240 C261 1.377(5) . ? C240 C293 1.382(5) . ? C245 C250 1.499(5) . ? C250 C266 1.377(5) . ? C254 C298 1.364(5) . ? C255 C277 1.372(4) . ? C273 C277 1.377(5) . ? C285 C292 1.485(4) . ? C292 C293 1.398(4) . ? C308 C312 1.367(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Ti1 Zr2 Ti7 66.678(19) . . ? Ti1 Zr2 Ti12 66.936(19) . . ? Ti1 Zr2 Ti16 101.92(2) . . ? Ti7 Zr2 Ti12 102.45(2) . . ? Ti16 Zr2 Ti7 66.478(19) . . ? Ti16 Zr2 Ti12 66.98(2) . . ? O10 Zr2 Ti1 71.71(6) . . ? O10 Zr2 Ti7 111.66(6) . . ? O10 Zr2 Ti12 107.91(6) . . ? O10 Zr2 Ti16 173.31(6) . . ? O10 Zr2 O34 140.90(8) . . ? O10 Zr2 O38 144.80(7) . . ? O18 Zr2 Ti1 173.09(6) . . ? O18 Zr2 Ti7 108.04(6) . . ? O18 Zr2 Ti12 111.11(6) . . ? O18 Zr2 Ti16 71.46(6) . . ? O18 Zr2 O10 114.98(8) . . ? O18 Zr2 O34 80.97(8) . . ? O18 Zr2 O38 78.56(8) . . ? O18 Zr2 O81 144.50(8) . . ? O18 Zr2 O96 140.65(8) . . ? O20 Zr2 Ti1 111.24(6) . . ? O20 Zr2 Ti7 173.33(6) . . ? O20 Zr2 Ti12 71.12(6) . . ? O20 Zr2 Ti16 108.54(6) . . ? O20 Zr2 O10 72.76(8) . . ? O20 Zr2 O18 73.48(8) . . ? O20 Zr2 O34 78.97(8) . . ? O20 Zr2 O38 141.34(8) . . ? O20 Zr2 O52 114.86(8) . . ? O20 Zr2 O81 80.92(8) . . ? O20 Zr2 O96 144.82(8) . . ? O34 Zr2 Ti1 94.81(6) . . ? O34 Zr2 Ti7 94.77(5) . . ? O34 Zr2 Ti12 35.73(6) . . ? O34 Zr2 Ti16 35.79(5) . . ? O34 Zr2 O38 70.64(7) . . ? O38 Zr2 Ti1 94.91(5) . . ? O38 Zr2 Ti7 35.59(5) . . ? O38 Zr2 Ti12 95.43(6) . . ? O38 Zr2 Ti16 35.72(5) . . ? O52 Zr2 Ti1 108.78(6) . . ? O52 Zr2 Ti7 71.61(6) . . ? O52 Zr2 Ti12 173.92(6) . . ? O52 Zr2 Ti16 110.74(6) . . ? O52 Zr2 O10 73.89(8) . . ? O52 Zr2 O18 72.60(8) . . ? O52 Zr2 O34 144.08(8) . . ? O52 Zr2 O38 80.45(8) . . ? O52 Zr2 O81 141.96(8) . . ? O52 Zr2 O96 79.03(8) . . ? O81 Zr2 Ti1 35.86(5) . . ? O81 Zr2 Ti7 94.85(5) . . ? O81 Zr2 Ti12 35.50(5) . . ? O81 Zr2 Ti16 94.60(6) . . ? O81 Zr2 O10 79.05(8) . . ? O81 Zr2 O34 70.16(8) . . ? O81 Zr2 O38 109.36(8) . . ? O96 Zr2 Ti1 35.96(6) . . ? O96 Zr2 Ti7 35.44(6) . . ? O96 Zr2 Ti12 95.41(6) . . ? O96 Zr2 Ti16 94.56(6) . . ? O96 Zr2 O10 81.44(8) . . ? O96 Zr2 O34 109.31(8) . . ? O96 Zr2 O38 70.19(8) . . ? O96 Zr2 O81 70.85(7) . . ? Zr2 Ti1 Ti16 130.99(2) . 3_766 ? O8 Ti1 Zr2 82.70(7) . . ? O8 Ti1 Ti16 146.29(7) . 3_766 ? O8 Ti1 O27 83.38(9) . . ? O27 Ti1 Zr2 132.30(7) . . ? O27 Ti1 Ti16 73.76(6) . 3_766 ? O74 Ti1 Zr2 134.09(7) . . ? O74 Ti1 Ti16 73.78(7) . 3_766 ? O74 Ti1 O8 81.05(9) . . ? O74 Ti1 O27 87.82(10) . . ? O81 Ti1 Zr2 42.46(6) . . ? O81 Ti1 Ti16 112.76(6) . 3_766 ? O81 Ti1 O8 91.30(9) . . ? O81 Ti1 O27 173.31(9) . . ? O81 Ti1 O74 95.37(9) . . ? O81 Ti1 O96 83.59(9) . . ? O83 Ti1 Zr2 110.97(7) . . ? O83 Ti1 Ti16 20.02(7) . 3_766 ? O83 Ti1 O8 166.28(10) . . ? O83 Ti1 O27 87.82(9) . . ? O83 Ti1 O74 88.14(9) . . ? O83 Ti1 O81 98.14(9) . . ? O83 Ti1 O96 101.24(9) . . ? O96 Ti1 Zr2 42.35(6) . . ? O96 Ti1 Ti16 115.25(7) . 3_766 ? O96 Ti1 O8 89.64(9) . . ? O96 Ti1 O27 92.30(9) . . ? O96 Ti1 O74 170.61(9) . . ? Zr2 Ti7 Ti12 127.94(2) . 3_766 ? O16 Ti7 Zr2 82.34(6) . . ? O16 Ti7 Ti12 149.67(6) . 3_766 ? O38 Ti7 Zr2 42.61(6) . . ? O38 Ti7 Ti12 113.65(6) . 3_766 ? O38 Ti7 O16 89.31(9) . . ? O38 Ti7 O40 92.74(9) . 3_766 ? O38 Ti7 O77 171.14(9) . 3_766 ? O40 Ti7 Zr2 133.57(7) 3_766 . ? O40 Ti7 Ti12 73.96(6) 3_766 3_766 ? O40 Ti7 O16 85.93(9) 3_766 . ? O40 Ti7 O77 85.69(10) 3_766 3_766 ? O77 Ti7 Zr2 136.01(7) 3_766 . ? O77 Ti7 Ti12 74.31(6) 3_766 3_766 ? O77 Ti7 O16 81.88(9) 3_766 . ? O89 Ti7 Zr2 108.35(7) 3_766 . ? O89 Ti7 Ti12 19.62(6) 3_766 3_766 ? O89 Ti7 O16 168.93(9) 3_766 . ? O89 Ti7 O38 100.50(9) 3_766 . ? O89 Ti7 O40 88.48(9) 3_766 3_766 ? O89 Ti7 O77 88.18(9) 3_766 3_766 ? O89 Ti7 O96 95.81(9) 3_766 . ? O96 Ti7 Zr2 42.07(6) . . ? O96 Ti7 Ti12 110.88(7) . 3_766 ? O96 Ti7 O16 90.32(9) . . ? O96 Ti7 O38 83.61(9) . . ? O96 Ti7 O40 174.81(9) . 3_766 ? O96 Ti7 O77 97.35(10) . 3_766 ? Zr2 Ti12 Ti7 129.55(2) . 3_766 ? O34 Ti12 Zr2 42.44(6) . . ? O34 Ti12 Ti7 114.23(7) . 3_766 ? O34 Ti12 O48 88.84(9) . . ? O34 Ti12 O59 171.62(9) . . ? O34 Ti12 O67 97.24(9) . . ? O48 Ti12 Zr2 82.71(6) . . ? O48 Ti12 Ti7 147.73(6) . 3_766 ? O48 Ti12 O67 81.42(9) . . ? O59 Ti12 Zr2 130.85(7) . . ? O59 Ti12 Ti7 73.77(6) . 3_766 ? O59 Ti12 O48 84.85(9) . . ? O59 Ti12 O67 87.27(9) . . ? O67 Ti12 Zr2 136.76(7) . . ? O67 Ti12 Ti7 73.83(6) . 3_766 ? O81 Ti12 Zr2 42.08(6) . . ? O81 Ti12 Ti7 111.45(6) . 3_766 ? O81 Ti12 O34 83.18(9) . . ? O81 Ti12 O48 92.67(9) . . ? O81 Ti12 O59 91.61(9) . . ? O81 Ti12 O67 174.06(9) . . ? O89 Ti12 Zr2 109.91(7) . . ? O89 Ti12 Ti7 19.74(6) . 3_766 ? O89 Ti12 O34 98.81(9) . . ? O89 Ti12 O48 167.12(9) . . ? O89 Ti12 O59 88.42(9) . . ? O89 Ti12 O67 87.32(9) . . ? O89 Ti12 O81 98.49(9) . . ? Zr2 Ti16 Ti1 127.05(2) . 3_766 ? O34 Ti16 Zr2 42.69(6) . . ? O34 Ti16 Ti1 110.12(7) . 3_766 ? O34 Ti16 O55 90.22(9) . . ? O34 Ti16 O64 175.39(9) . 3_766 ? O34 Ti16 O104 94.24(9) . 3_766 ? O38 Ti16 Zr2 42.73(6) . . ? O38 Ti16 Ti1 112.60(6) . 3_766 ? O38 Ti16 O34 84.31(9) . . ? O38 Ti16 O55 90.22(9) . . ? O38 Ti16 O64 93.37(9) . 3_766 ? O38 Ti16 O104 173.39(9) . 3_766 ? O55 Ti16 Zr2 82.66(7) . . ? O55 Ti16 Ti1 150.22(7) . 3_766 ? O55 Ti16 O64 85.80(9) . 3_766 ? O64 Ti16 Zr2 134.16(6) 3_766 . ? O64 Ti16 Ti1 74.44(6) 3_766 3_766 ? O83 Ti16 Zr2 107.07(7) 3_766 . ? O83 Ti16 Ti1 20.01(7) 3_766 3_766 ? O83 Ti16 O34 96.35(9) 3_766 . ? O83 Ti16 O38 97.61(9) 3_766 . ? O83 Ti16 O55 170.23(10) 3_766 . ? O83 Ti16 O64 87.90(9) 3_766 3_766 ? O83 Ti16 O104 88.96(9) 3_766 3_766 ? O104 Ti16 Zr2 134.29(7) 3_766 . ? O104 Ti16 Ti1 73.96(6) 3_766 3_766 ? O104 Ti16 O55 83.33(9) 3_766 . ? O104 Ti16 O64 87.61(9) 3_766 3_766 ? C79 C2 C97 121.0(4) . . ? C144 O8 Ti1 126.6(2) . . ? C144 O10 Zr2 133.7(2) . . ? C290 O16 Ti7 126.1(2) . . ? C245 O18 Zr2 135.4(2) . . ? C220 O20 Zr2 136.2(2) . . ? C238 O27 Ti1 133.3(2) . . ? Ti12 O34 Zr2 101.83(9) . . ? Ti16 O34 Zr2 101.52(9) . . ? Ti16 O34 Ti12 135.25(11) . . ? Ti7 O38 Zr2 101.80(9) . . ? Ti7 O38 Ti16 134.13(11) . . ? Ti16 O38 Zr2 101.55(9) . . ? C285 O40 Ti7 133.8(2) . 3_766 ? C220 O48 Ti12 125.29(19) . . ? C290 O52 Zr2 135.1(2) . . ? C245 O55 Ti16 125.4(2) . . ? C285 O59 Ti12 133.4(2) . . ? C139 C61 C229 120.0(4) . . ? C270 O64 Ti16 131.4(2) . 3_766 ? C232 O67 Ti12 131.8(2) . . ? C270 O74 Ti1 135.3(2) . . ? C232 O77 Ti7 133.9(2) . 3_766 ? C2 C79 C105 119.6(4) . . ? Ti1 O81 Zr2 101.67(9) . . ? Ti12 O81 Zr2 102.42(9) . . ? Ti12 O81 Ti1 135.23(11) . . ? Ti1 O83 Ti16 139.97(13) . 3_766 ? Ti12 O89 Ti7 140.64(12) . 3_766 ? Ti1 O96 Zr2 101.70(9) . . ? Ti7 O96 Zr2 102.48(9) . . ? Ti7 O96 Ti1 134.12(11) . . ? C2 C97 C222 119.5(4) . . ? C238 O104 Ti16 134.2(2) . 3_766 ? C79 C105 C121 120.2(4) . . ? C250 C110 C198 119.9(4) . . ? C105 C121 C232 119.8(3) . . ? C222 C121 C105 119.6(3) . . ? C222 C121 C232 120.5(3) . . ? C182 C124 C126 119.6(4) . . ? C146 C126 C124 120.1(4) . . ? C139 C130 C138 120.6(4) . . ? C193 C136 C144 121.1(3) . . ? C193 C136 C209 119.9(3) . . ? C209 C136 C144 119.0(3) . . ? C130 C138 C153 119.3(4) . . ? C130 C139 C61 120.2(4) . . ? O8 C144 C136 116.3(3) . . ? O10 C144 O8 124.7(3) . . ? O10 C144 C136 119.0(3) . . ? C200 C146 C126 120.8(4) . . ? C171 C152 C292 119.9(3) . . ? C138 C153 C270 119.7(3) . . ? C229 C153 C138 120.2(3) . . ? C229 C153 C270 120.1(3) . . ? C208 C155 C170 119.7(3) . . ? C298 C168 C204 119.7(4) . . ? C273 C170 C155 120.0(4) . . ? C152 C171 C261 120.1(4) . . ? C183 C173 C220 119.6(3) . . ? C204 C173 C183 119.2(3) . . ? C204 C173 C220 121.1(3) . . ? C124 C182 C196 119.5(3) . . ? C124 C182 C290 120.2(3) . . ? C196 C182 C290 120.2(3) . . ? C254 C183 C173 120.0(3) . . ? C136 C193 C205 119.2(3) . . ? C182 C196 C200 120.3(4) . . ? C304 C198 C110 119.6(4) . . ? C146 C200 C196 119.7(4) . . ? C173 C204 C168 120.5(4) . . ? C312 C205 C193 120.3(4) . . ? C155 C208 C238 119.5(3) . . ? C155 C208 C255 120.0(3) . . ? C255 C208 C238 120.4(3) . . ? C308 C209 C136 120.1(4) . . ? C304 C214 C266 120.8(5) . . ? O20 C220 O48 124.2(3) . . ? O20 C220 C173 117.8(3) . . ? O48 C220 C173 118.0(3) . . ? C121 C222 C97 120.0(4) . . ? C153 C229 C61 119.7(4) . . ? O67 C232 O77 125.4(3) . . ? O67 C232 C121 119.1(3) . . ? O77 C232 C121 115.5(3) . . ? O27 C238 O104 124.3(3) . . ? O27 C238 C208 118.0(3) . . ? O104 C238 C208 117.6(3) . . ? C261 C240 C293 120.8(4) . . ? O18 C245 O55 124.9(3) . . ? O18 C245 C250 117.8(3) . . ? O55 C245 C250 117.3(3) . . ? C110 C250 C245 120.6(3) . . ? C110 C250 C266 119.7(3) . . ? C266 C250 C245 119.7(3) . . ? C298 C254 C183 120.5(4) . . ? C277 C255 C208 119.9(3) . . ? C240 C261 C171 119.8(3) . . ? C250 C266 C214 119.8(4) . . ? O64 C270 C153 119.4(3) . . ? O74 C270 O64 124.7(3) . . ? O74 C270 C153 115.9(3) . . ? C170 C273 C277 120.6(4) . . ? C255 C277 C273 119.7(3) . . ? O40 C285 C292 116.9(3) . . ? O59 C285 O40 125.0(3) . . ? O59 C285 C292 118.1(3) . . ? O16 C290 C182 116.8(3) . . ? O52 C290 O16 124.7(3) . . ? O52 C290 C182 118.6(3) . . ? C152 C292 C285 119.5(3) . . ? C152 C292 C293 120.3(3) . . ? C293 C292 C285 120.2(3) . . ? C240 C293 C292 119.1(3) . . ? C254 C298 C168 120.1(3) . . ? C214 C304 C198 120.1(4) . . ? C312 C308 C209 120.0(4) . . ? C308 C312 C205 120.4(4) . . ? _olex2_submission_special_instructions 'No special instructions were received' data_[Ti8Zr2O12(p-TolCOO)16] _audit_creation_date 2017-08-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Kratzert, D., Holstein, J.J. & Krossing, I. (2015). J. Appl. Cryst. 48, 933-938. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C128 H112 O44 Ti8 Zr2, 2(C3 H7 N O)' _chemical_formula_sum 'C134 H126 N2 O46 Ti8 Zr2' _chemical_formula_weight 3066.00 _chemical_melting_point ? 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' 'N' 'N' 0.0061 0.0033 '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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'trigonal' _space_group_IT_number 167 _space_group_name_H-M_alt 'R -3 c' _space_group_name_Hall '-R 3 2"c' loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 32.890(7) _cell_length_b 32.890(7) _cell_length_c 73.485(15) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_volume 68844(31) _cell_formula_units_Z 18 _cell_measurement_reflns_used 9952 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 24.87 _cell_measurement_theta_min 2.48 _shelx_estimated_absorpt_T_max 0.942 _shelx_estimated_absorpt_T_min 0.942 _exptl_absorpt_coefficient_mu 0.601 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type 'none' _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 28224 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.1043 _diffrn_reflns_av_unetI/netI 0.0821 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 41 _diffrn_reflns_limit_h_min -42 _diffrn_reflns_limit_k_max 42 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 48 _diffrn_reflns_limit_l_min -95 _diffrn_reflns_number 118987 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 26.000 _diffrn_reflns_theta_max 27.487 _diffrn_reflns_theta_min 1.663 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9507 _reflns_number_total 17545 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 1.349 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.099 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.006 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 876 _refine_ls_number_reflns 17545 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1290 _refine_ls_R_factor_gt 0.0587 _refine_ls_restrained_S_all 1.006 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0754P)^2^+379.9355P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1409 _refine_ls_wR_factor_ref 0.1827 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Aromatic/amide H refined with riding coordinates: C44(H44), C45(H45), C46(H46), C47(H47), C48(H48), C49(H49), C2BA(H2BA), C3AA(H3AA), C5BA(H5BA), C5AA(H5AA), C4AA(H4AA), C0BA(H0BA), C2(H2), C4CA(H4CA), C1CA(H1CA), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C13(H13), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C20(H20), C23(H23), C24(H24), C32(H32), C33(H33), C34(H34) 2.b Idealised Me refined as rotating group: C1AA(H1AA,H1AB,H1AC), C0CA(H0CA,H0CB,H0CC), C22(H22A,H22B,H22C), C27(H27A, H27B,H27C), C28(H28A,H28B,H28C), C39(H39A,H39B,H39C), C1(H1A,H1B,H1C), C3(H3A, H3B,H3C), C4(H4A,H4B,H4C), C0AA(H0AA,H0AB,H0AC) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.11779(2) 0.44074(2) 0.05589(2) 0.02799(12) Uani 1 1 d . . . . . Ti2 Ti 0.16415(3) 0.38219(3) 0.07033(2) 0.02706(19) Uani 1 1 d . . . . . Ti3 Ti 0.01226(3) 0.38256(3) 0.07037(2) 0.0325(2) Uani 1 1 d . . . . . Ti4 Ti 0.06532(3) 0.33486(3) 0.04212(2) 0.03020(19) Uani 1 1 d . . . . . Ti5 Ti 0.11120(3) 0.42980(3) 0.09896(2) 0.0306(2) Uani 1 1 d . . . . . O1 O 0.04869(10) 0.37932(10) 0.05086(4) 0.0307(7) Uani 1 1 d . . . . . O2 O 0.15300(10) 0.51047(10) 0.06825(4) 0.0332(7) Uani 1 1 d . . . . . O3 O 0.07192(10) 0.42852(10) 0.07970(4) 0.0303(7) Uani 1 1 d . . . . . O4 O 0.12111(11) 0.3333 0.0833 0.0281(9) Uani 1 2 d S T P . . O5 O 0.14883(10) 0.42712(10) 0.07968(4) 0.0291(7) Uani 1 1 d . . . . . O6 O 0.04561(10) 0.29764(10) 0.06195(4) 0.0306(7) Uani 1 1 d . . . . . O7 O 0.12651(10) 0.37976(10) 0.05038(4) 0.0286(7) Uani 1 1 d . . . . . O0AA O 0.11748(11) 0.44049(11) 0.02603(4) 0.0360(7) Uani 1 1 d . . . . . O10 O 0.19070(10) 0.47564(10) 0.04690(4) 0.0312(7) Uani 1 1 d . . . . . O11 O 0.07992(10) 0.47497(10) 0.04687(4) 0.0365(8) Uani 1 1 d . . . . . O12 O 0.15924(11) 0.43998(11) 0.11813(4) 0.0383(8) Uani 1 1 d . . . . . O13 O 0.07030(11) 0.43851(11) 0.11826(4) 0.0381(8) Uani 1 1 d . . . . . O14 O 0.22262(10) 0.43346(10) 0.05667(4) 0.0323(7) Uani 1 1 d . . . . . O15 O -0.04998(11) 0.33778(11) 0.05848(5) 0.0419(8) Uani 1 1 d . . . . . O16 O 0.14725(11) 0.50275(10) 0.09846(4) 0.0364(8) Uani 1 1 d . . . . . O17 O 0.21158(10) 0.39319(11) 0.08974(4) 0.0394(8) Uani 1 1 d . . . . . O18 O 0.00576(12) 0.3333 0.0833 0.0324(10) Uani 1 2 d S T P . . O20 O 0.18309(10) 0.33642(11) 0.05866(4) 0.0356(7) Uani 1 1 d . . . . . O21 O -0.02696(11) 0.39231(11) 0.09002(5) 0.0428(8) Uani 1 1 d . . . . . O6BA O 0.00273(11) 0.29259(11) 0.03082(4) 0.0402(8) Uani 1 1 d . . . . . O23 O 0.00508(11) 0.43395(11) 0.05609(5) 0.0399(8) Uani 1 1 d . . . . . O25 O 0.08789(11) 0.29237(11) 0.03158(4) 0.0386(8) Uani 1 1 d . . . . . O2AA O 0.08067(12) 0.36590(12) 0.01671(5) 0.0415(8) Uani 1 1 d . . . . . C1BA C 0.21330(15) 0.36975(15) 0.10314(6) 0.0306(10) Uani 1 1 d . . . . . C7BA C 0.16167(16) 0.41549(16) 0.13083(7) 0.0350(11) Uani 1 1 d . . . . . C7AA C 0.04419(16) 0.41146(16) 0.13080(7) 0.0340(11) Uani 1 1 d . . . . . C3BA C 0.20462(16) 0.43673(17) 0.14218(7) 0.0386(12) Uani 1 1 d . . . . . C8BA C 0.25794(15) 0.39173(16) 0.11336(7) 0.0349(11) Uani 1 1 d . . . . . C4BA C 0.18800(16) 0.57896(15) 0.08579(7) 0.0353(11) Uani 1 1 d . . . . . C9BA C 0.26836(15) 0.49996(15) 0.03825(6) 0.0321(10) Uani 1 1 d . . . . . C8AA C 0.22454(15) 0.46748(15) 0.04785(6) 0.0298(10) Uani 1 1 d . . . . . C35 C -0.08598(16) 0.30012(17) 0.06396(7) 0.0399(12) Uani 1 1 d . . . . . C36 C -0.13078(17) 0.28794(17) 0.05443(8) 0.0450(13) Uani 1 1 d . . . . . C37 C 0.16096(15) 0.52707(15) 0.08417(7) 0.0343(11) Uani 1 1 d . . . . . C38 C 0.11012(19) 0.4270(2) -0.00534(7) 0.0461(13) Uani 1 1 d . . . . . C9AA C 0.10235(17) 0.40998(18) 0.01369(7) 0.0379(11) Uani 1 1 d . . . . . C40 C 0.01258(16) 0.42350(15) 0.14080(6) 0.0343(11) Uani 1 1 d . . . . . C41 C 0.03744(17) 0.46605(16) 0.04685(7) 0.0379(11) Uani 1 1 d . . . . . C42 C 0.23794(17) 0.67732(16) 0.08811(8) 0.0451(13) Uani 1 1 d . . . . . C43 C 0.02827(16) 0.49783(16) 0.03528(7) 0.0369(11) Uani 1 1 d . . . . . C44 C 0.30620(16) 0.49183(17) 0.03809(7) 0.0408(12) Uani 1 1 d . . . . . H44 H 0.3039 0.4652 0.0441 0.049 Uiso 1 1 calc R . . . . C45 C 0.26310(18) 0.37324(19) 0.12925(9) 0.0549(15) Uani 1 1 d . . . . . H45 H 0.2376 0.3452 0.1340 0.066 Uiso 1 1 calc R . . . . C46 C 0.21416(18) 0.64998(18) 0.10292(8) 0.0494(14) Uani 1 1 d . . . . . H46 H 0.2142 0.6648 0.1140 0.059 Uiso 1 1 calc R . . . . C47 C 0.27245(17) 0.53841(16) 0.02928(7) 0.0425(12) Uani 1 1 d . . . . . H47 H 0.2467 0.5439 0.0292 0.051 Uiso 1 1 calc R . . . . C48 C 0.13154(19) 0.4741(2) -0.00902(8) 0.0545(15) Uani 1 1 d . . . . . H48 H 0.1417 0.4963 0.0006 0.065 Uiso 1 1 calc R . . . . C49 C -0.01328(17) 0.39565(16) 0.15535(7) 0.0412(12) Uani 1 1 d . . . . . H49 H -0.0116 0.3685 0.1584 0.049 Uiso 1 1 calc R . . . . C2BA C 0.21165(17) 0.60624(17) 0.07073(7) 0.0430(12) Uani 1 1 d . . . . . H2BA H 0.2107 0.5915 0.0595 0.052 Uiso 1 1 calc R . . . . C3AA C 0.00903(17) 0.46212(17) 0.13623(7) 0.0422(12) Uani 1 1 d . . . . . H3AA H 0.0261 0.4811 0.1262 0.051 Uiso 1 1 calc R . . . . C5BA C -0.01936(18) 0.47338(18) 0.14632(8) 0.0505(14) Uani 1 1 d . . . . . H5BA H -0.0220 0.4999 0.1429 0.061 Uiso 1 1 calc R . . . . C5AA C 0.23652(18) 0.65464(17) 0.07197(8) 0.0467(13) Uani 1 1 d . . . . . H5AA H 0.2529 0.6727 0.0616 0.056 Uiso 1 1 calc R . . . . C4AA C -0.0413(2) 0.40732(18) 0.16533(8) 0.0541(15) Uani 1 1 d . . . . . H4AA H -0.0591 0.3879 0.1752 0.065 Uiso 1 1 calc R . . . . C6AA C -0.04406(19) 0.44693(18) 0.16123(8) 0.0547(16) Uani 1 1 d . . . . . C0BA C 0.19019(17) 0.60128(17) 0.10203(7) 0.0425(12) Uani 1 1 d . . . . . H0BA H 0.1753 0.5833 0.1126 0.051 Uiso 1 1 calc R . . . . C1AA C 0.2642(2) 0.73045(17) 0.08908(9) 0.0578(15) Uani 1 1 d . . . . . H1AA H 0.2417 0.7415 0.0905 0.087 Uiso 1 1 calc GR . . . . H1AB H 0.2823 0.7434 0.0779 0.087 Uiso 1 1 calc GR . . . . H1AC H 0.2856 0.7408 0.0995 0.087 Uiso 1 1 calc GR . . . . N1 N 0.04734(18) 0.56017(17) 0.07923(7) 0.0597(13) Uani 1 1 d . . . . . C2 C 0.06011(17) 0.52375(18) 0.02180(7) 0.0452(13) Uani 1 1 d . . . . . H2 H 0.0869 0.5204 0.0199 0.054 Uiso 1 1 calc R . . . . C3CA C 0.01572(19) 0.56061(18) 0.01377(8) 0.0485(14) Uani 1 1 d . . . . . C4CA C 0.24219(18) 0.48027(19) 0.13766(8) 0.0494(13) Uani 1 1 d . . . . . H4CA H 0.2415 0.4955 0.1268 0.059 Uiso 1 1 calc R . . . . C1CA C 0.05353(18) 0.55436(18) 0.01105(8) 0.0506(14) Uani 1 1 d . . . . . H1CA H 0.0754 0.5713 0.0017 0.061 Uiso 1 1 calc R . . . . C6 C 0.35140(18) 0.5617(2) 0.02024(8) 0.0542(15) Uani 1 1 d . . . . . C7 C 0.31371(19) 0.56948(19) 0.02030(8) 0.0530(15) Uani 1 1 d . . . . . H7 H 0.3160 0.5960 0.0142 0.064 Uiso 1 1 calc R . . . . C8 C 0.29656(17) 0.43217(18) 0.10661(8) 0.0487(14) Uani 1 1 d . . . . . H8 H 0.2934 0.4456 0.0956 0.058 Uiso 1 1 calc R . . . . C9 C 0.34687(18) 0.52275(19) 0.02914(8) 0.0520(15) Uani 1 1 d . . . . . H9 H 0.3725 0.5171 0.0291 0.062 Uiso 1 1 calc R . . . . C10 C -0.1308(2) 0.3162(2) 0.04060(8) 0.0534(15) Uani 1 1 d . . . . . H10 H -0.1024 0.3432 0.0370 0.064 Uiso 1 1 calc R . . . . C11 C 0.1382(2) 0.4891(3) -0.02685(10) 0.083(2) Uani 1 1 d . . . . . H11 H 0.1523 0.5217 -0.0294 0.100 Uiso 1 1 calc R . . . . C0CA C 0.3970(2) 0.5958(2) 0.01088(10) 0.080(2) Uani 1 1 d . . . . . H0CA H 0.4030 0.5798 0.0009 0.121 Uiso 1 1 calc GR . . . . H0CB H 0.4229 0.6073 0.0197 0.121 Uiso 1 1 calc GR . . . . H0CC H 0.3947 0.6223 0.0060 0.121 Uiso 1 1 calc GR . . . . C13 C -0.17242(18) 0.24856(19) 0.05948(9) 0.0609(17) Uani 1 1 d . . . . . H13 H -0.1728 0.2286 0.0689 0.073 Uiso 1 1 calc R . . . . C14 C -0.01058(18) 0.50256(19) 0.03758(8) 0.0516(14) Uani 1 1 d . . . . . H14 H -0.0335 0.4842 0.0464 0.062 Uiso 1 1 calc R . . . . C15 C 0.2454(2) 0.4372(2) 0.16934(10) 0.074(2) Uani 1 1 d . . . . . H15 H 0.2462 0.4224 0.1803 0.089 Uiso 1 1 calc R . . . . C16 C -0.0162(2) 0.5341(2) 0.02696(9) 0.0633(17) Uani 1 1 d . . . . . H16 H -0.0429 0.5376 0.0289 0.076 Uiso 1 1 calc R . . . . C17 C 0.3059(2) 0.3955(2) 0.13861(10) 0.0703(19) Uani 1 1 d . . . . . H17 H 0.3086 0.3832 0.1500 0.084 Uiso 1 1 calc R . . . . C18 C 0.2065(2) 0.41479(19) 0.15802(8) 0.0528(15) Uani 1 1 d . . . . . H18 H 0.1813 0.3846 0.1611 0.063 Uiso 1 1 calc R . . . . C19 C -0.1725(2) 0.3051(2) 0.03189(10) 0.0716(19) Uani 1 1 d . . . . . H19 H -0.1721 0.3244 0.0222 0.086 Uiso 1 1 calc R . . . . C20 C 0.3393(2) 0.4533(2) 0.11549(10) 0.0654(18) Uani 1 1 d . . . . . H20 H 0.3653 0.4804 0.1104 0.079 Uiso 1 1 calc R . . . . C21 C 0.3443(2) 0.4351(2) 0.13159(11) 0.070(2) Uani 1 1 d . . . . . C22 C 0.0881(2) 0.5888(2) 0.06781(9) 0.079(2) Uani 1 1 d . . . . . H22A H 0.1150 0.6092 0.0755 0.119 Uiso 1 1 calc GR . . . . H22B H 0.0812 0.6081 0.0596 0.119 Uiso 1 1 calc GR . . . . H22C H 0.0956 0.5683 0.0606 0.119 Uiso 1 1 calc GR . . . . C23 C 0.2808(2) 0.5014(2) 0.14914(9) 0.0675(18) Uani 1 1 d . . . . . H23 H 0.3065 0.5312 0.1460 0.081 Uiso 1 1 calc R . . . . C24 C 0.0966(3) 0.3952(3) -0.01941(9) 0.075(2) Uani 1 1 d . . . . . H24 H 0.0818 0.3625 -0.0169 0.090 Uiso 1 1 calc R . . . . C26 C 0.2829(2) 0.4806(2) 0.16484(11) 0.074(2) Uani 1 1 d . . . . . C27 C -0.0737(3) 0.4606(2) 0.17261(11) 0.095(3) Uani 1 1 d . . . . . H27A H -0.0570 0.4755 0.1839 0.143 Uiso 1 1 calc GR . . . . H27B H -0.1036 0.4325 0.1755 0.143 Uiso 1 1 calc GR . . . . H27C H -0.0797 0.4827 0.1658 0.143 Uiso 1 1 calc GR . . . . C28 C 0.0503(2) 0.5271(2) 0.09108(10) 0.078(2) Uani 1 1 d . . . . . H28A H 0.0589 0.5072 0.0840 0.117 Uiso 1 1 calc GR . . . . H28B H 0.0198 0.5074 0.0970 0.117 Uiso 1 1 calc GR . . . . H28C H 0.0742 0.5440 0.1004 0.117 Uiso 1 1 calc GR . . . . C29 C 0.1245(3) 0.4572(4) -0.04104(11) 0.094(3) Uani 1 1 d . . . . . C30 C -0.2142(2) 0.2670(2) 0.03697(11) 0.080(2) Uani 1 1 d . . . . . O31 O -0.0268(2) 0.5394(3) 0.08752(10) 0.129(2) Uani 1 1 d . . . . . C32 C -0.2136(2) 0.2386(2) 0.05063(11) 0.078(2) Uani 1 1 d . . . . . H32 H -0.2421 0.2114 0.0541 0.093 Uiso 1 1 calc R . . . . C33 C 0.0090(3) 0.5622(3) 0.07842(13) 0.099(3) Uani 1 1 d . . . . . H33 H 0.0085 0.5837 0.0699 0.118 Uiso 1 1 calc R . . . . C34 C 0.1046(4) 0.4109(4) -0.03718(11) 0.108(3) Uani 1 1 d . . . . . H34 H 0.0961 0.3889 -0.0468 0.130 Uiso 1 1 calc R . . . . C39 C 0.1321(3) 0.4742(4) -0.06076(10) 0.139(4) Uani 1 1 d . . . . . H39A H 0.1129 0.4887 -0.0633 0.209 Uiso 1 1 calc GR . . . . H39B H 0.1229 0.4474 -0.0689 0.209 Uiso 1 1 calc GR . . . . H39C H 0.1653 0.4973 -0.0627 0.209 Uiso 1 1 calc GR . . . . C1 C 0.0095(2) 0.5951(2) 0.00230(11) 0.079(2) Uani 1 1 d . . . . . H1A H 0.0103 0.6196 0.0101 0.118 Uiso 1 1 calc GR . . . . H1B H -0.0207 0.5787 -0.0040 0.118 Uiso 1 1 calc GR . . . . H1C H 0.0350 0.6095 -0.0066 0.118 Uiso 1 1 calc GR . . . . C3 C 0.3909(3) 0.4598(3) 0.14183(14) 0.130(4) Uani 1 1 d . . . . . H3A H 0.3865 0.4467 0.1541 0.195 Uiso 1 1 calc GR . . . . H3B H 0.4018 0.4935 0.1426 0.195 Uiso 1 1 calc GR . . . . H3C H 0.4142 0.4550 0.1353 0.195 Uiso 1 1 calc GR . . . . C4 C 0.3253(3) 0.5041(3) 0.17702(13) 0.130(4) Uani 1 1 d . . . . . H4A H 0.3155 0.5069 0.1893 0.196 Uiso 1 1 calc GR . . . . H4B H 0.3472 0.5354 0.1723 0.196 Uiso 1 1 calc GR . . . . H4C H 0.3408 0.4853 0.1774 0.196 Uiso 1 1 calc GR . . . . C0AA C -0.2594(3) 0.2563(3) 0.02749(14) 0.124(4) Uani 1 1 d . . . . . H0AA H -0.2545 0.2841 0.0208 0.186 Uiso 1 1 calc GR . . . . H0AB H -0.2842 0.2478 0.0366 0.186 Uiso 1 1 calc GR . . . . H0AC H -0.2686 0.2301 0.0190 0.186 Uiso 1 1 calc GR . . . . 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 0.0252(2) 0.0273(2) 0.0330(3) 0.00154(18) 0.00142(19) 0.01438(18) Ti2 0.0233(4) 0.0271(4) 0.0321(5) 0.0019(3) 0.0016(3) 0.0135(3) Ti3 0.0239(4) 0.0301(4) 0.0447(6) 0.0048(4) 0.0015(4) 0.0143(3) Ti4 0.0302(4) 0.0290(4) 0.0309(5) -0.0014(4) -0.0037(4) 0.0144(3) Ti5 0.0294(4) 0.0269(4) 0.0330(5) -0.0015(3) 0.0030(4) 0.0123(3) O1 0.0274(15) 0.0304(16) 0.0361(19) 0.0019(14) -0.0004(13) 0.0157(13) O2 0.0329(17) 0.0276(16) 0.039(2) 0.0000(15) 0.0019(15) 0.0150(14) O3 0.0285(15) 0.0256(15) 0.039(2) -0.0014(13) 0.0022(14) 0.0148(13) O4 0.0252(15) 0.031(2) 0.030(3) 0.0008(19) 0.0004(9) 0.0157(11) O5 0.0260(15) 0.0268(15) 0.0322(18) 0.0006(13) 0.0035(13) 0.0114(13) O6 0.0294(16) 0.0297(16) 0.0328(18) -0.0012(13) -0.0041(14) 0.0149(13) O7 0.0281(15) 0.0280(15) 0.0306(18) -0.0004(13) 0.0007(13) 0.0146(13) O0AA 0.0386(18) 0.0415(19) 0.0306(19) 0.0063(16) 0.0018(15) 0.0219(16) O10 0.0244(15) 0.0299(16) 0.039(2) 0.0030(14) 0.0018(13) 0.0132(13) O11 0.0323(17) 0.0368(18) 0.049(2) 0.0064(15) 0.0045(15) 0.0233(15) O12 0.0355(18) 0.0330(17) 0.037(2) -0.0028(15) -0.0034(15) 0.0102(15) O13 0.0403(18) 0.0334(17) 0.040(2) -0.0007(15) 0.0102(16) 0.0180(15) O14 0.0271(15) 0.0343(17) 0.0361(19) 0.0053(14) 0.0037(14) 0.0157(13) O15 0.0287(17) 0.0373(18) 0.058(2) 0.0071(16) -0.0054(16) 0.0149(15) O16 0.0355(17) 0.0299(16) 0.039(2) -0.0033(15) 0.0060(15) 0.0131(14) O17 0.0296(17) 0.0374(18) 0.042(2) 0.0068(16) -0.0049(15) 0.0103(14) O18 0.0252(15) 0.034(2) 0.041(3) 0.001(2) 0.0007(10) 0.0171(12) O20 0.0325(17) 0.0358(17) 0.045(2) 0.0048(15) 0.0064(15) 0.0218(15) O21 0.0359(18) 0.0406(19) 0.057(2) 0.0074(17) 0.0113(17) 0.0229(16) O6BA 0.0330(17) 0.0374(18) 0.041(2) 0.0018(16) -0.0075(15) 0.0105(15) O23 0.0306(17) 0.0345(18) 0.057(2) 0.0098(16) 0.0042(16) 0.0178(15) O25 0.0428(19) 0.0340(17) 0.040(2) -0.0010(15) 0.0016(15) 0.0195(15) O2AA 0.046(2) 0.042(2) 0.038(2) -0.0020(16) -0.0029(16) 0.0233(17) C1BA 0.028(2) 0.033(2) 0.035(3) 0.002(2) 0.005(2) 0.018(2) C7BA 0.035(2) 0.035(3) 0.037(3) -0.010(2) 0.001(2) 0.019(2) C7AA 0.031(2) 0.032(2) 0.033(3) -0.006(2) 0.002(2) 0.012(2) C3BA 0.034(3) 0.041(3) 0.046(3) -0.013(2) -0.004(2) 0.023(2) C8BA 0.027(2) 0.036(2) 0.049(3) -0.005(2) -0.006(2) 0.021(2) C4BA 0.032(2) 0.029(2) 0.044(3) -0.006(2) -0.003(2) 0.014(2) C9BA 0.026(2) 0.030(2) 0.036(3) -0.001(2) 0.002(2) 0.0114(19) C8AA 0.029(2) 0.027(2) 0.029(3) -0.0004(19) 0.0040(19) 0.0100(18) C35 0.032(2) 0.040(3) 0.050(3) 0.001(2) -0.001(2) 0.020(2) C36 0.036(3) 0.037(3) 0.063(4) -0.006(3) -0.008(3) 0.019(2) C37 0.026(2) 0.029(2) 0.048(3) -0.002(2) 0.005(2) 0.0144(19) C38 0.049(3) 0.073(4) 0.032(3) 0.003(3) 0.005(2) 0.042(3) C9AA 0.036(3) 0.048(3) 0.037(3) 0.005(3) 0.002(2) 0.028(2) C40 0.035(2) 0.030(2) 0.032(3) -0.006(2) 0.005(2) 0.012(2) C41 0.037(3) 0.034(2) 0.045(3) 0.000(2) 0.003(2) 0.019(2) C42 0.039(3) 0.027(2) 0.063(4) -0.007(3) -0.009(3) 0.012(2) C43 0.034(2) 0.031(2) 0.047(3) -0.004(2) -0.006(2) 0.018(2) C44 0.030(2) 0.043(3) 0.052(3) 0.010(2) 0.011(2) 0.020(2) C45 0.036(3) 0.048(3) 0.075(4) 0.014(3) -0.008(3) 0.017(2) C46 0.051(3) 0.039(3) 0.049(4) -0.007(3) 0.002(3) 0.016(3) C47 0.033(3) 0.038(3) 0.053(3) 0.003(2) 0.004(2) 0.015(2) C48 0.049(3) 0.074(4) 0.041(3) 0.022(3) 0.010(3) 0.031(3) C49 0.041(3) 0.032(2) 0.046(3) -0.002(2) 0.009(2) 0.014(2) C2BA 0.048(3) 0.033(3) 0.045(3) -0.001(2) 0.002(2) 0.017(2) C3AA 0.044(3) 0.037(3) 0.045(3) 0.001(2) 0.011(2) 0.019(2) C5BA 0.052(3) 0.037(3) 0.064(4) 0.000(3) 0.015(3) 0.023(3) C5AA 0.050(3) 0.036(3) 0.051(4) 0.004(3) 0.000(3) 0.018(2) C4AA 0.060(4) 0.040(3) 0.054(4) 0.005(3) 0.029(3) 0.019(3) C6AA 0.051(3) 0.040(3) 0.070(4) -0.005(3) 0.028(3) 0.020(3) C0BA 0.045(3) 0.033(3) 0.040(3) 0.001(2) 0.005(2) 0.012(2) C1AA 0.058(4) 0.033(3) 0.070(4) -0.005(3) -0.003(3) 0.013(3) N1 0.063(3) 0.054(3) 0.065(4) 0.005(3) 0.004(3) 0.032(3) C2 0.039(3) 0.046(3) 0.056(4) 0.007(3) -0.001(3) 0.025(2) C3CA 0.047(3) 0.040(3) 0.063(4) 0.007(3) -0.011(3) 0.025(3) C4CA 0.037(3) 0.050(3) 0.047(3) -0.002(3) -0.003(3) 0.012(2) C1CA 0.040(3) 0.044(3) 0.062(4) 0.012(3) 0.002(3) 0.016(2) C6 0.038(3) 0.051(3) 0.067(4) 0.008(3) 0.018(3) 0.017(3) C7 0.048(3) 0.041(3) 0.065(4) 0.014(3) 0.008(3) 0.019(3) C8 0.036(3) 0.041(3) 0.068(4) 0.006(3) -0.011(3) 0.019(2) C9 0.038(3) 0.053(3) 0.068(4) 0.009(3) 0.016(3) 0.026(3) C10 0.047(3) 0.054(3) 0.058(4) 0.001(3) -0.013(3) 0.025(3) C11 0.068(4) 0.127(7) 0.060(5) 0.053(5) 0.026(4) 0.053(5) C0CA 0.054(4) 0.067(4) 0.110(6) 0.033(4) 0.043(4) 0.023(3) C13 0.036(3) 0.045(3) 0.099(5) -0.002(3) -0.016(3) 0.018(3) C14 0.039(3) 0.050(3) 0.075(4) 0.015(3) 0.007(3) 0.028(3) C15 0.064(4) 0.067(4) 0.094(6) 0.015(4) -0.033(4) 0.036(4) C16 0.050(3) 0.068(4) 0.091(5) 0.017(4) 0.003(3) 0.044(3) C17 0.060(4) 0.067(4) 0.080(5) 0.011(4) -0.030(3) 0.029(3) C18 0.051(3) 0.043(3) 0.072(4) 0.001(3) -0.014(3) 0.030(3) C19 0.061(4) 0.069(4) 0.077(5) 0.001(4) -0.022(4) 0.026(4) C20 0.040(3) 0.049(3) 0.100(6) 0.009(3) -0.018(3) 0.016(3) C21 0.046(3) 0.048(3) 0.111(6) 0.002(4) -0.035(4) 0.020(3) C22 0.075(5) 0.068(4) 0.070(5) 0.004(4) 0.012(4) 0.017(4) C23 0.040(3) 0.064(4) 0.075(5) -0.005(3) -0.016(3) 0.008(3) C24 0.117(6) 0.096(5) 0.041(4) -0.007(4) 0.001(4) 0.075(5) C26 0.048(4) 0.077(5) 0.090(6) 0.002(4) -0.029(4) 0.025(3) C27 0.111(6) 0.069(4) 0.116(6) 0.020(4) 0.077(5) 0.053(4) C28 0.071(4) 0.066(4) 0.090(5) 0.016(4) 0.001(4) 0.029(4) C29 0.095(6) 0.184(10) 0.045(5) 0.040(6) 0.026(4) 0.100(7) C30 0.058(4) 0.064(4) 0.117(6) -0.020(4) -0.047(4) 0.030(4) O31 0.088(4) 0.152(6) 0.167(6) 0.024(5) 0.041(4) 0.076(4) C32 0.036(3) 0.049(4) 0.136(7) -0.001(4) -0.016(4) 0.012(3) C33 0.098(7) 0.096(6) 0.124(8) 0.007(5) 0.002(6) 0.065(6) C34 0.167(9) 0.168(10) 0.044(5) -0.006(6) 0.011(5) 0.125(9) C39 0.143(9) 0.259(14) 0.051(5) 0.053(7) 0.025(5) 0.127(9) C1 0.073(4) 0.056(4) 0.116(6) 0.028(4) 0.000(4) 0.039(4) C3 0.075(5) 0.075(5) 0.192(10) 0.028(6) -0.079(6) 0.001(4) C4 0.072(5) 0.122(7) 0.145(9) 0.022(6) -0.066(6) 0.009(5) C0AA 0.080(6) 0.096(6) 0.182(10) -0.010(6) -0.080(6) 0.033(5) _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 Ti2 3.1775(10) . ? Zr1 Ti3 3.1934(11) . ? Zr1 Ti4 3.1812(11) . ? Zr1 Ti5 3.1806(12) . ? Zr1 O1 2.189(3) . ? Zr1 O2 2.184(3) . ? Zr1 O3 2.211(3) . ? Zr1 O5 2.181(3) . ? Zr1 O7 2.201(3) . ? Zr1 O0AA 2.194(3) . ? Zr1 O10 2.180(3) . ? Zr1 O11 2.159(3) . ? Ti2 Ti2 3.3758(16) 17_554 ? Ti2 O4 1.7955(15) . ? Ti2 O5 1.912(3) . ? Ti2 O7 1.895(3) . ? Ti2 O14 2.076(3) . ? Ti2 O17 2.008(3) . ? Ti2 O20 2.080(3) . ? Ti3 Ti3 3.3902(17) 17_554 ? Ti3 O1 1.905(3) . ? Ti3 O3 1.907(3) . ? Ti3 O15 2.027(3) . ? Ti3 O18 1.7968(15) . ? Ti3 O21 2.066(3) . ? Ti3 O23 2.101(3) . ? Ti4 Ti5 3.3656(12) 17_554 ? Ti4 O1 1.911(3) . ? Ti4 O6 1.802(3) . ? Ti4 O7 1.905(3) . ? Ti4 O6BA 2.000(3) . ? Ti4 O25 2.035(3) . ? Ti4 O2AA 2.066(3) . ? Ti5 Ti4 3.3655(12) 17_554 ? Ti5 O3 1.903(3) . ? Ti5 O5 1.912(3) . ? Ti5 O6 1.782(3) 17_554 ? Ti5 O12 2.016(3) . ? Ti5 O13 2.071(3) . ? Ti5 O16 2.078(3) . ? O2 C37 1.262(6) . ? O4 Ti2 1.7955(15) 17_554 ? O6 Ti5 1.782(3) 17_554 ? O0AA C9AA 1.256(6) . ? O10 C8AA 1.271(5) . ? O11 C41 1.276(5) . ? O12 C7BA 1.261(6) . ? O13 C7AA 1.270(5) . ? O14 C8AA 1.267(5) . ? O15 C35 1.277(5) . ? O16 C37 1.259(6) . ? O17 C1BA 1.269(5) . ? O18 Ti3 1.7966(15) 17_554 ? O20 C1BA 1.262(5) 17_554 ? O21 C35 1.260(6) 17_554 ? O6BA C7AA 1.273(5) 17_554 ? O23 C41 1.259(5) . ? O25 C7BA 1.279(5) 17_554 ? O2AA C9AA 1.275(6) . ? C1BA O20 1.262(5) 17_554 ? C1BA C8BA 1.477(6) . ? C7BA O25 1.279(5) 17_554 ? C7BA C3BA 1.481(6) . ? C7AA O6BA 1.273(5) 17_554 ? C7AA C40 1.479(6) . ? C3BA C4CA 1.385(7) . ? C3BA C18 1.387(7) . ? C8BA C45 1.366(7) . ? C8BA C8 1.392(7) . ? C4BA C37 1.483(6) . ? C4BA C2BA 1.391(7) . ? C4BA C0BA 1.384(7) . ? C9BA C8AA 1.475(6) . ? C9BA C44 1.397(6) . ? C9BA C47 1.372(6) . ? C35 O21 1.260(6) 17_554 ? C35 C36 1.494(7) . ? C36 C10 1.377(7) . ? C36 C13 1.385(7) . ? C38 C9AA 1.480(7) . ? C38 C48 1.370(8) . ? C38 C24 1.379(8) . ? C40 C49 1.388(7) . ? C40 C3AA 1.374(7) . ? C41 C43 1.490(7) . ? C42 C46 1.379(7) . ? C42 C5AA 1.389(7) . ? C42 C1AA 1.515(7) . ? C43 C2 1.383(7) . ? C43 C14 1.373(6) . ? C44 H44 0.9500 . ? C44 C9 1.377(7) . ? C45 H45 0.9500 . ? C45 C17 1.400(7) . ? C46 H46 0.9500 . ? C46 C0BA 1.389(7) . ? C47 H47 0.9500 . ? C47 C7 1.391(7) . ? C48 H48 0.9500 . ? C48 C11 1.379(8) . ? C49 H49 0.9500 . ? C49 C4AA 1.374(7) . ? C2BA H2BA 0.9500 . ? C2BA C5AA 1.382(7) . ? C3AA H3AA 0.9500 . ? C3AA C5BA 1.380(7) . ? C5BA H5BA 0.9500 . ? C5BA C6AA 1.382(7) . ? C5AA H5AA 0.9500 . ? C4AA H4AA 0.9500 . ? C4AA C6AA 1.383(7) . ? C6AA C27 1.513(7) . ? C0BA H0BA 0.9500 . ? C1AA H1AA 0.9800 . ? C1AA H1AB 0.9800 . ? C1AA H1AC 0.9800 . ? N1 C22 1.459(8) . ? N1 C28 1.435(8) . ? N1 C33 1.299(9) . ? C2 H2 0.9500 . ? C2 C1CA 1.379(7) . ? C3CA C1CA 1.373(7) . ? C3CA C16 1.374(8) . ? C3CA C1 1.507(7) . ? C4CA H4CA 0.9500 . ? C4CA C23 1.387(7) . ? C1CA H1CA 0.9500 . ? C6 C7 1.384(7) . ? C6 C9 1.380(8) . ? C6 C0CA 1.516(7) . ? C7 H7 0.9500 . ? C8 H8 0.9500 . ? C8 C20 1.383(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C10 C19 1.387(8) . ? C11 H11 0.9500 . ? C11 C29 1.385(12) . ? C0CA H0CA 0.9800 . ? C0CA H0CB 0.9800 . ? C0CA H0CC 0.9800 . ? C13 H13 0.9500 . ? C13 C32 1.386(8) . ? C14 H14 0.9500 . ? C14 C16 1.384(7) . ? C15 H15 0.9500 . ? C15 C18 1.389(8) . ? C15 C26 1.381(9) . ? C16 H16 0.9500 . ? C17 H17 0.9500 . ? C17 C21 1.383(9) . ? C18 H18 0.9500 . ? C19 H19 0.9500 . ? C19 C30 1.369(9) . ? C20 H20 0.9500 . ? C20 C21 1.371(9) . ? C21 C3 1.526(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23 0.9500 . ? C23 C26 1.361(9) . ? C24 H24 0.9500 . ? C24 C34 1.380(10) . ? C26 C4 1.505(9) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C34 1.355(13) . ? C29 C39 1.527(10) . ? C30 C32 1.379(9) . ? C30 C0AA 1.514(8) . ? O31 C33 1.229(10) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 H4A 0.9800 . ? C4 H4B 0.9800 . ? C4 H4C 0.9800 . ? C0AA H0AA 0.9800 . ? C0AA H0AB 0.9800 . ? C0AA H0AC 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 Ti2 Zr1 Ti3 103.46(2) . . ? Ti2 Zr1 Ti4 66.72(2) . . ? Ti2 Zr1 Ti5 68.00(2) . . ? Ti4 Zr1 Ti3 67.54(2) . . ? Ti5 Zr1 Ti3 66.95(2) . . ? Ti5 Zr1 Ti4 102.93(2) . . ? O1 Zr1 Ti2 95.07(8) . . ? O1 Zr1 Ti3 35.65(8) . . ? O1 Zr1 Ti4 36.04(8) . . ? O1 Zr1 Ti5 94.76(8) . . ? O1 Zr1 O3 70.53(11) . . ? O1 Zr1 O7 71.10(10) . . ? O1 Zr1 O0AA 80.03(12) . . ? O2 Zr1 Ti2 109.54(8) . . ? O2 Zr1 Ti3 109.73(8) . . ? O2 Zr1 Ti4 173.97(9) . . ? O2 Zr1 Ti5 71.07(9) . . ? O2 Zr1 O1 143.15(11) . . ? O2 Zr1 O3 79.49(11) . . ? O2 Zr1 O7 142.30(11) . . ? O2 Zr1 O0AA 114.75(12) . . ? O3 Zr1 Ti2 96.67(8) . . ? O3 Zr1 Ti3 35.84(8) . . ? O3 Zr1 Ti4 96.04(7) . . ? O3 Zr1 Ti5 35.97(8) . . ? O5 Zr1 Ti2 36.10(8) . . ? O5 Zr1 Ti3 95.17(8) . . ? O5 Zr1 Ti4 94.79(8) . . ? O5 Zr1 Ti5 36.05(8) . . ? O5 Zr1 O1 108.81(11) . . ? O5 Zr1 O2 79.96(11) . . ? O5 Zr1 O3 71.07(11) . . ? O5 Zr1 O7 70.89(11) . . ? O5 Zr1 O0AA 143.37(11) . . ? O7 Zr1 Ti2 35.76(8) . . ? O7 Zr1 Ti3 96.49(7) . . ? O7 Zr1 Ti4 35.94(7) . . ? O7 Zr1 Ti5 96.47(8) . . ? O7 Zr1 O3 111.58(10) . . ? O0AA Zr1 Ti2 109.53(8) . . ? O0AA Zr1 Ti3 109.23(8) . . ? O0AA Zr1 Ti4 71.26(9) . . ? O0AA Zr1 Ti5 174.13(9) . . ? O0AA Zr1 O3 142.07(11) . . ? O0AA Zr1 O7 79.33(11) . . ? O10 Zr1 Ti2 71.67(8) . . ? O10 Zr1 Ti3 175.10(8) . . ? O10 Zr1 Ti4 109.37(8) . . ? O10 Zr1 Ti5 110.86(8) . . ? O10 Zr1 O1 142.74(11) . . ? O10 Zr1 O2 72.95(11) . . ? O10 Zr1 O3 143.74(11) . . ? O10 Zr1 O5 81.16(11) . . ? O10 Zr1 O7 79.27(11) . . ? O10 Zr1 O0AA 72.58(12) . . ? O11 Zr1 Ti2 174.54(8) . . ? O11 Zr1 Ti3 71.17(8) . . ? O11 Zr1 Ti4 109.54(9) . . ? O11 Zr1 Ti5 109.90(9) . . ? O11 Zr1 O1 79.98(11) . . ? O11 Zr1 O2 73.82(12) . . ? O11 Zr1 O3 79.56(11) . . ? O11 Zr1 O5 143.59(12) . . ? O11 Zr1 O7 142.24(12) . . ? O11 Zr1 O0AA 72.05(12) . . ? O11 Zr1 O10 113.69(11) . . ? Zr1 Ti2 Ti2 128.444(16) . 17_554 ? O4 Ti2 Zr1 108.51(12) . . ? O4 Ti2 Ti2 19.94(12) . 17_554 ? O4 Ti2 O5 96.08(12) . . ? O4 Ti2 O7 99.66(12) . . ? O4 Ti2 O14 168.58(15) . . ? O4 Ti2 O17 88.70(13) . . ? O4 Ti2 O20 87.66(12) . . ? O5 Ti2 Zr1 42.24(9) . . ? O5 Ti2 Ti2 110.40(9) . 17_554 ? O5 Ti2 O14 92.35(12) . . ? O5 Ti2 O17 94.98(13) . . ? O5 Ti2 O20 176.04(13) . . ? O7 Ti2 Zr1 42.75(9) . . ? O7 Ti2 Ti2 114.07(9) . 17_554 ? O7 Ti2 O5 83.77(13) . . ? O7 Ti2 O14 88.87(12) . . ? O7 Ti2 O17 171.63(13) . . ? O7 Ti2 O20 94.36(13) . . ? O14 Ti2 Zr1 82.90(8) . . ? O14 Ti2 Ti2 148.64(8) . 17_554 ? O14 Ti2 O20 84.11(12) . . ? O17 Ti2 Zr1 133.85(10) . . ? O17 Ti2 Ti2 74.14(9) . 17_554 ? O17 Ti2 O14 82.90(12) . . ? O17 Ti2 O20 86.36(13) . . ? O20 Ti2 Zr1 135.15(10) . . ? O20 Ti2 Ti2 73.55(9) . 17_554 ? Zr1 Ti3 Ti3 128.056(16) . 17_554 ? O1 Ti3 Zr1 42.05(9) . . ? O1 Ti3 Ti3 112.49(9) . 17_554 ? O1 Ti3 O3 83.58(13) . . ? O1 Ti3 O15 94.00(14) . . ? O1 Ti3 O21 173.65(13) . . ? O1 Ti3 O23 89.77(13) . . ? O3 Ti3 Zr1 42.75(9) . . ? O3 Ti3 Ti3 111.46(10) . 17_554 ? O3 Ti3 O15 174.68(14) . . ? O3 Ti3 O21 95.78(13) . . ? O3 Ti3 O23 91.54(12) . . ? O15 Ti3 Zr1 133.78(11) . . ? O15 Ti3 Ti3 73.84(10) . 17_554 ? O15 Ti3 O21 86.10(14) . . ? O15 Ti3 O23 83.69(13) . . ? O18 Ti3 Zr1 108.70(12) . . ? O18 Ti3 Ti3 19.36(12) . 17_554 ? O18 Ti3 O1 98.23(13) . . ? O18 Ti3 O3 97.79(13) . . ? O18 Ti3 O15 87.24(13) . . ? O18 Ti3 O21 88.11(13) . . ? O18 Ti3 O23 168.31(15) . . ? O21 Ti3 Zr1 135.73(10) . . ? O21 Ti3 Ti3 73.65(9) . 17_554 ? O21 Ti3 O23 83.93(13) . . ? O23 Ti3 Zr1 82.95(9) . . ? O23 Ti3 Ti3 148.99(9) . 17_554 ? Zr1 Ti4 Ti5 127.48(3) . 17_554 ? O1 Ti4 Zr1 42.38(9) . . ? O1 Ti4 Ti5 110.58(9) . 17_554 ? O1 Ti4 O6BA 94.74(13) . . ? O1 Ti4 O25 174.84(13) . . ? O1 Ti4 O2AA 91.06(13) . . ? O6 Ti4 Zr1 107.48(10) . . ? O6 Ti4 Ti5 20.00(9) . 17_554 ? O6 Ti4 O1 96.00(13) . . ? O6 Ti4 O7 98.67(13) . . ? O6 Ti4 O6BA 88.15(13) . . ? O6 Ti4 O25 88.40(13) . . ? O6 Ti4 O2AA 169.22(14) . . ? O7 Ti4 Zr1 42.72(8) . . ? O7 Ti4 Ti5 112.91(9) . 17_554 ? O7 Ti4 O1 83.99(12) . . ? O7 Ti4 O6BA 173.15(14) . . ? O7 Ti4 O25 92.69(13) . . ? O7 Ti4 O2AA 90.14(13) . . ? O6BA Ti4 Zr1 134.40(10) . . ? O6BA Ti4 Ti5 73.85(10) . 17_554 ? O6BA Ti4 O25 88.09(14) . . ? O6BA Ti4 O2AA 83.14(14) . . ? O25 Ti4 Zr1 133.50(9) . . ? O25 Ti4 Ti5 74.35(9) . 17_554 ? O25 Ti4 O2AA 84.98(13) . . ? O2AA Ti4 Zr1 83.22(9) . . ? O2AA Ti4 Ti5 149.28(10) . 17_554 ? Zr1 Ti5 Ti4 129.56(3) . 17_554 ? O3 Ti5 Zr1 43.05(9) . . ? O3 Ti5 Ti4 114.21(9) . 17_554 ? O3 Ti5 O5 84.00(13) . . ? O3 Ti5 O12 172.16(13) . . ? O3 Ti5 O13 91.82(13) . . ? O3 Ti5 O16 90.08(13) . . ? O5 Ti5 Zr1 42.16(9) . . ? O5 Ti5 Ti4 111.73(9) . 17_554 ? O5 Ti5 O12 93.08(13) . . ? O5 Ti5 O13 173.74(13) . . ? O5 Ti5 O16 91.78(12) . . ? O6 Ti5 Zr1 109.34(10) 17_554 . ? O6 Ti5 Ti4 20.24(10) 17_554 17_554 ? O6 Ti5 O3 99.43(13) 17_554 . ? O6 Ti5 O5 97.53(13) 17_554 . ? O6 Ti5 O12 88.15(13) 17_554 . ? O6 Ti5 O13 87.73(13) 17_554 . ? O6 Ti5 O16 167.30(14) 17_554 . ? O12 Ti5 Zr1 132.30(10) . . ? O12 Ti5 Ti4 73.63(9) . 17_554 ? O12 Ti5 O13 90.46(14) . . ? O12 Ti5 O16 82.72(13) . . ? O13 Ti5 Zr1 132.69(10) . . ? O13 Ti5 Ti4 74.23(9) . 17_554 ? O13 Ti5 O16 83.55(12) . . ? O16 Ti5 Zr1 83.36(9) . . ? O16 Ti5 Ti4 147.07(10) . 17_554 ? Ti3 O1 Zr1 102.30(13) . . ? Ti3 O1 Ti4 136.44(16) . . ? Ti4 O1 Zr1 101.58(12) . . ? C37 O2 Zr1 136.5(3) . . ? Ti3 O3 Zr1 101.41(13) . . ? Ti5 O3 Zr1 100.98(12) . . ? Ti5 O3 Ti3 134.65(16) . . ? Ti2 O4 Ti2 140.1(2) . 17_554 ? Ti2 O5 Zr1 101.66(13) . . ? Ti2 O5 Ti5 136.78(16) . . ? Ti5 O5 Zr1 101.78(13) . . ? Ti5 O6 Ti4 139.76(18) 17_554 . ? Ti2 O7 Zr1 101.49(13) . . ? Ti2 O7 Ti4 133.96(16) . . ? Ti4 O7 Zr1 101.34(12) . . ? C9AA O0AA Zr1 136.4(3) . . ? C8AA O10 Zr1 136.2(3) . . ? C41 O11 Zr1 137.0(3) . . ? C7BA O12 Ti5 134.9(3) . . ? C7AA O13 Ti5 131.2(3) . . ? C8AA O14 Ti2 125.6(3) . . ? C35 O15 Ti3 132.7(3) . . ? C37 O16 Ti5 124.4(3) . . ? C1BA O17 Ti2 135.1(3) . . ? Ti3 O18 Ti3 141.3(2) 17_554 . ? C1BA O20 Ti2 132.5(3) 17_554 . ? C35 O21 Ti3 132.5(3) 17_554 . ? C7AA O6BA Ti4 134.4(3) 17_554 . ? C41 O23 Ti3 123.8(3) . . ? C7BA O25 Ti4 132.5(3) 17_554 . ? C9AA O2AA Ti4 125.4(3) . . ? O17 C1BA C8BA 115.6(4) . . ? O20 C1BA O17 124.5(4) 17_554 . ? O20 C1BA C8BA 119.9(4) 17_554 . ? O12 C7BA O25 124.6(4) . 17_554 ? O12 C7BA C3BA 117.8(4) . . ? O25 C7BA C3BA 117.5(4) 17_554 . ? O13 C7AA O6BA 124.5(4) . 17_554 ? O13 C7AA C40 119.5(4) . . ? O6BA C7AA C40 115.9(4) 17_554 . ? C4CA C3BA C7BA 120.0(5) . . ? C4CA C3BA C18 119.3(5) . . ? C18 C3BA C7BA 120.5(5) . . ? C45 C8BA C1BA 122.1(4) . . ? C45 C8BA C8 118.2(4) . . ? C8 C8BA C1BA 119.7(4) . . ? C2BA C4BA C37 119.9(4) . . ? C0BA C4BA C37 121.4(5) . . ? C0BA C4BA C2BA 118.7(4) . . ? C44 C9BA C8AA 120.5(4) . . ? C47 C9BA C8AA 120.5(4) . . ? C47 C9BA C44 119.1(4) . . ? O10 C8AA C9BA 117.6(4) . . ? O14 C8AA O10 123.5(4) . . ? O14 C8AA C9BA 118.9(4) . . ? O15 C35 C36 115.1(4) . . ? O21 C35 O15 125.0(4) 17_554 . ? O21 C35 C36 119.9(4) 17_554 . ? C10 C36 C35 119.9(5) . . ? C10 C36 C13 119.6(5) . . ? C13 C36 C35 120.4(5) . . ? O2 C37 C4BA 116.6(4) . . ? O16 C37 O2 124.6(4) . . ? O16 C37 C4BA 118.9(5) . . ? C48 C38 C9AA 120.6(5) . . ? C48 C38 C24 120.0(6) . . ? C24 C38 C9AA 119.4(6) . . ? O0AA C9AA O2AA 123.8(5) . . ? O0AA C9AA C38 117.1(5) . . ? O2AA C9AA C38 119.2(5) . . ? C49 C40 C7AA 119.1(4) . . ? C3AA C40 C7AA 121.5(4) . . ? C3AA C40 C49 119.4(4) . . ? O11 C41 C43 114.9(4) . . ? O23 C41 O11 124.2(4) . . ? O23 C41 C43 120.9(4) . . ? C46 C42 C5AA 117.9(5) . . ? C46 C42 C1AA 121.7(5) . . ? C5AA C42 C1AA 120.4(5) . . ? C2 C43 C41 119.0(4) . . ? C14 C43 C41 122.4(5) . . ? C14 C43 C2 118.6(5) . . ? C9BA C44 H44 120.3 . . ? C9 C44 C9BA 119.5(5) . . ? C9 C44 H44 120.3 . . ? C8BA C45 H45 119.9 . . ? C8BA C45 C17 120.2(5) . . ? C17 C45 H45 119.9 . . ? C42 C46 H46 119.2 . . ? C42 C46 C0BA 121.7(5) . . ? C0BA C46 H46 119.2 . . ? C9BA C47 H47 119.5 . . ? C9BA C47 C7 121.0(5) . . ? C7 C47 H47 119.5 . . ? C38 C48 H48 120.3 . . ? C38 C48 C11 119.5(7) . . ? C11 C48 H48 120.3 . . ? C40 C49 H49 119.9 . . ? C4AA C49 C40 120.1(5) . . ? C4AA C49 H49 119.9 . . ? C4BA C2BA H2BA 119.7 . . ? C5AA C2BA C4BA 120.6(5) . . ? C5AA C2BA H2BA 119.7 . . ? C40 C3AA H3AA 120.0 . . ? C40 C3AA C5BA 119.9(5) . . ? C5BA C3AA H3AA 120.0 . . ? C3AA C5BA H5BA 119.3 . . ? C3AA C5BA C6AA 121.4(5) . . ? C6AA C5BA H5BA 119.3 . . ? C42 C5AA H5AA 119.5 . . ? C2BA C5AA C42 121.1(5) . . ? C2BA C5AA H5AA 119.5 . . ? C49 C4AA H4AA 119.5 . . ? C49 C4AA C6AA 121.0(5) . . ? C6AA C4AA H4AA 119.5 . . ? C5BA C6AA C4AA 118.1(5) . . ? C5BA C6AA C27 120.9(5) . . ? C4AA C6AA C27 121.0(5) . . ? C4BA C0BA C46 120.1(5) . . ? C4BA C0BA H0BA 120.0 . . ? C46 C0BA H0BA 120.0 . . ? C42 C1AA H1AA 109.5 . . ? C42 C1AA H1AB 109.5 . . ? C42 C1AA H1AC 109.5 . . ? H1AA C1AA H1AB 109.5 . . ? H1AA C1AA H1AC 109.5 . . ? H1AB C1AA H1AC 109.5 . . ? C28 N1 C22 116.7(6) . . ? C33 N1 C22 123.0(7) . . ? C33 N1 C28 120.3(6) . . ? C43 C2 H2 119.5 . . ? C1CA C2 C43 120.9(5) . . ? C1CA C2 H2 119.5 . . ? C1CA C3CA C16 118.1(5) . . ? C1CA C3CA C1 120.4(6) . . ? C16 C3CA C1 121.6(5) . . ? C3BA C4CA H4CA 120.2 . . ? C3BA C4CA C23 119.5(5) . . ? C23 C4CA H4CA 120.2 . . ? C2 C1CA H1CA 119.7 . . ? C3CA C1CA C2 120.7(5) . . ? C3CA C1CA H1CA 119.7 . . ? C7 C6 C0CA 120.8(5) . . ? C9 C6 C7 118.6(5) . . ? C9 C6 C0CA 120.6(5) . . ? C47 C7 H7 120.0 . . ? C6 C7 C47 120.1(5) . . ? C6 C7 H7 120.0 . . ? C8BA C8 H8 119.2 . . ? C20 C8 C8BA 121.7(5) . . ? C20 C8 H8 119.2 . . ? C44 C9 C6 121.8(5) . . ? C44 C9 H9 119.1 . . ? C6 C9 H9 119.1 . . ? C36 C10 H10 120.0 . . ? C36 C10 C19 119.9(6) . . ? C19 C10 H10 120.0 . . ? C48 C11 H11 119.6 . . ? C48 C11 C29 120.7(8) . . ? C29 C11 H11 119.6 . . ? C6 C0CA H0CA 109.5 . . ? C6 C0CA H0CB 109.5 . . ? C6 C0CA H0CC 109.5 . . ? H0CA C0CA H0CB 109.5 . . ? H0CA C0CA H0CC 109.5 . . ? H0CB C0CA H0CC 109.5 . . ? C36 C13 H13 120.4 . . ? C36 C13 C32 119.2(6) . . ? C32 C13 H13 120.4 . . ? C43 C14 H14 120.1 . . ? C43 C14 C16 119.8(5) . . ? C16 C14 H14 120.1 . . ? C18 C15 H15 119.5 . . ? C26 C15 H15 119.5 . . ? C26 C15 C18 121.0(6) . . ? C3CA C16 C14 121.8(5) . . ? C3CA C16 H16 119.1 . . ? C14 C16 H16 119.1 . . ? C45 C17 H17 119.5 . . ? C21 C17 C45 121.0(6) . . ? C21 C17 H17 119.5 . . ? C3BA C18 C15 119.7(5) . . ? C3BA C18 H18 120.1 . . ? C15 C18 H18 120.1 . . ? C10 C19 H19 119.3 . . ? C30 C19 C10 121.4(6) . . ? C30 C19 H19 119.3 . . ? C8 C20 H20 120.0 . . ? C21 C20 C8 120.1(6) . . ? C21 C20 H20 120.0 . . ? C17 C21 C3 121.2(6) . . ? C20 C21 C17 118.7(5) . . ? C20 C21 C3 120.0(6) . . ? N1 C22 H22A 109.5 . . ? N1 C22 H22B 109.5 . . ? N1 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C4CA C23 H23 119.1 . . ? C26 C23 C4CA 121.8(6) . . ? C26 C23 H23 119.1 . . ? C38 C24 H24 120.1 . . ? C38 C24 C34 119.7(8) . . ? C34 C24 H24 120.1 . . ? C15 C26 C4 120.5(7) . . ? C23 C26 C15 118.6(6) . . ? C23 C26 C4 120.9(7) . . ? C6AA C27 H27A 109.5 . . ? C6AA C27 H27B 109.5 . . ? C6AA C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N1 C28 H28A 109.5 . . ? N1 C28 H28B 109.5 . . ? N1 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C11 C29 C39 120.4(10) . . ? C34 C29 C11 119.1(7) . . ? C34 C29 C39 120.5(10) . . ? C19 C30 C32 118.2(6) . . ? C19 C30 C0AA 120.3(7) . . ? C32 C30 C0AA 121.6(7) . . ? C13 C32 H32 119.2 . . ? C30 C32 C13 121.7(6) . . ? C30 C32 H32 119.2 . . ? N1 C33 H33 116.6 . . ? O31 C33 N1 126.9(9) . . ? O31 C33 H33 116.6 . . ? C24 C34 H34 119.5 . . ? C29 C34 C24 121.0(8) . . ? C29 C34 H34 119.5 . . ? C29 C39 H39A 109.5 . . ? C29 C39 H39B 109.5 . . ? C29 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C3CA C1 H1A 109.5 . . ? C3CA C1 H1B 109.5 . . ? C3CA C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C21 C3 H3A 109.5 . . ? C21 C3 H3B 109.5 . . ? C21 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C26 C4 H4A 109.5 . . ? C26 C4 H4B 109.5 . . ? C26 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C30 C0AA H0AA 109.5 . . ? C30 C0AA H0AB 109.5 . . ? C30 C0AA H0AC 109.5 . . ? H0AA C0AA H0AB 109.5 . . ? H0AA C0AA H0AC 109.5 . . ? H0AB C0AA H0AC 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 Zr1 Ti2 O4 Ti2 -178.68(3) . . . 17_554 ? Zr1 Ti2 O7 Ti4 -118.3(3) . . . . ? Zr1 Ti3 O18 Ti3 179.06(4) . . . 17_554 ? Zr1 Ti4 O6 Ti5 179.9(2) . . . 17_554 ? Zr1 O2 C37 O16 -1.5(7) . . . . ? Zr1 O2 C37 C4BA 179.2(3) . . . . ? Zr1 O0AA C9AA O2AA -0.1(7) . . . . ? Zr1 O0AA C9AA C38 179.2(3) . . . . ? Zr1 O10 C8AA O14 -5.6(7) . . . . ? Zr1 O10 C8AA C9BA 175.1(3) . . . . ? Zr1 O11 C41 O23 14.0(8) . . . . ? Zr1 O11 C41 C43 -167.8(3) . . . . ? Ti2 Ti2 O7 Zr1 121.32(8) 17_554 . . . ? Ti2 Ti2 O7 Ti4 3.0(2) 17_554 . . . ? Ti2 O14 C8AA O10 3.1(6) . . . . ? Ti2 O14 C8AA C9BA -177.6(3) . . . . ? Ti2 O17 C1BA O20 -3.7(7) . . . 17_554 ? Ti2 O17 C1BA C8BA 176.6(3) . . . . ? Ti3 O15 C35 O21 -21.7(8) . . . 17_554 ? Ti3 O15 C35 C36 156.8(3) . . . . ? Ti3 O23 C41 O11 -9.3(7) . . . . ? Ti3 O23 C41 C43 172.6(3) . . . . ? Ti4 O2AA C9AA O0AA 0.3(6) . . . . ? Ti4 O2AA C9AA C38 -179.0(3) . . . . ? Ti5 O12 C7BA O25 -3.2(7) . . . 17_554 ? Ti5 O12 C7BA C3BA 179.8(3) . . . . ? Ti5 O13 C7AA O6BA 11.4(7) . . . 17_554 ? Ti5 O13 C7AA C40 -169.9(3) . . . . ? Ti5 O16 C37 O2 3.1(6) . . . . ? Ti5 O16 C37 C4BA -177.6(3) . . . . ? O1 Ti3 O18 Ti3 -138.95(10) . . . 17_554 ? O1 Ti4 O6 Ti5 138.1(3) . . . 17_554 ? O3 Ti3 O18 Ti3 136.46(10) . . . 17_554 ? O4 Ti2 O7 Zr1 106.87(12) . . . . ? O4 Ti2 O7 Ti4 -11.5(2) . . . . ? O5 Ti2 O4 Ti2 -137.23(9) . . . 17_554 ? O5 Ti2 O7 Zr1 11.74(12) . . . . ? O5 Ti2 O7 Ti4 -106.6(2) . . . . ? O7 Ti2 O4 Ti2 138.08(9) . . . 17_554 ? O7 Ti4 O6 Ti5 -137.1(3) . . . 17_554 ? O11 C41 C43 C2 19.0(7) . . . . ? O11 C41 C43 C14 -160.6(5) . . . . ? O12 C7BA C3BA C4CA -6.0(7) . . . . ? O12 C7BA C3BA C18 169.8(4) . . . . ? O13 C7AA C40 C49 -175.3(4) . . . . ? O13 C7AA C40 C3AA 3.3(7) . . . . ? O14 Ti2 O4 Ti2 0.2(5) . . . 17_554 ? O14 Ti2 O7 Zr1 -80.75(12) . . . . ? O14 Ti2 O7 Ti4 160.9(2) . . . . ? O15 Ti3 O18 Ti3 -45.30(10) . . . 17_554 ? O15 C35 C36 C10 1.2(7) . . . . ? O15 C35 C36 C13 -178.4(5) . . . . ? O17 Ti2 O4 Ti2 -42.36(10) . . . 17_554 ? O17 C1BA C8BA C45 172.4(5) . . . . ? O17 C1BA C8BA C8 -8.7(6) . . . . ? O20 Ti2 O4 Ti2 44.05(9) . . . 17_554 ? O20 Ti2 O7 Zr1 -164.76(12) . . . . ? O20 Ti2 O7 Ti4 76.9(2) . . . . ? O20 C1BA C8BA C45 -7.3(7) 17_554 . . . ? O20 C1BA C8BA C8 171.6(4) 17_554 . . . ? O21 Ti3 O18 Ti3 40.88(10) . . . 17_554 ? O21 C35 C36 C10 179.8(5) 17_554 . . . ? O21 C35 C36 C13 0.3(8) 17_554 . . . ? O6BA Ti4 O6 Ti5 43.6(3) . . . 17_554 ? O6BA C7AA C40 C49 3.5(7) 17_554 . . . ? O6BA C7AA C40 C3AA -177.8(5) 17_554 . . . ? O23 Ti3 O18 Ti3 -6.2(5) . . . 17_554 ? O23 C41 C43 C2 -162.7(5) . . . . ? O23 C41 C43 C14 17.7(8) . . . . ? O25 Ti4 O6 Ti5 -44.6(3) . . . 17_554 ? O25 C7BA C3BA C4CA 176.8(4) 17_554 . . . ? O25 C7BA C3BA C18 -7.4(7) 17_554 . . . ? O2AA Ti4 O6 Ti5 7.5(9) . . . 17_554 ? C1BA C8BA C45 C17 -179.3(5) . . . . ? C1BA C8BA C8 C20 -178.4(5) . . . . ? C7BA C3BA C4CA C23 175.1(5) . . . . ? C7BA C3BA C18 C15 -174.2(5) . . . . ? C7AA C40 C49 C4AA 177.2(5) . . . . ? C7AA C40 C3AA C5BA -177.4(5) . . . . ? C3BA C4CA C23 C26 -0.1(10) . . . . ? C8BA C45 C17 C21 -3.2(10) . . . . ? C8BA C8 C20 C21 -1.5(10) . . . . ? C4BA C2BA C5AA C42 -1.1(8) . . . . ? C9BA C44 C9 C6 -0.2(9) . . . . ? C9BA C47 C7 C6 0.3(9) . . . . ? C8AA C9BA C44 C9 -179.6(5) . . . . ? C8AA C9BA C47 C7 179.5(5) . . . . ? C35 C36 C10 C19 -179.3(5) . . . . ? C35 C36 C13 C32 178.8(6) . . . . ? C36 C10 C19 C30 1.3(10) . . . . ? C36 C13 C32 C30 -0.4(11) . . . . ? C37 C4BA C2BA C5AA 179.2(5) . . . . ? C37 C4BA C0BA C46 -177.3(5) . . . . ? C38 C48 C11 C29 -1.6(9) . . . . ? C38 C24 C34 C29 -1.9(12) . . . . ? C9AA C38 C48 C11 -179.7(5) . . . . ? C9AA C38 C24 C34 -178.6(6) . . . . ? C40 C49 C4AA C6AA -0.5(9) . . . . ? C40 C3AA C5BA C6AA 1.0(8) . . . . ? C41 C43 C2 C1CA -178.6(5) . . . . ? C41 C43 C14 C16 177.2(5) . . . . ? C42 C46 C0BA C4BA -2.8(8) . . . . ? C43 C2 C1CA C3CA 1.5(8) . . . . ? C43 C14 C16 C3CA 1.4(10) . . . . ? C44 C9BA C8AA O10 -177.2(4) . . . . ? C44 C9BA C8AA O14 3.5(7) . . . . ? C44 C9BA C47 C7 -0.9(8) . . . . ? C45 C8BA C8 C20 0.5(8) . . . . ? C45 C17 C21 C20 2.1(11) . . . . ? C45 C17 C21 C3 179.4(7) . . . . ? C46 C42 C5AA C2BA 0.7(8) . . . . ? C47 C9BA C8AA O10 2.4(7) . . . . ? C47 C9BA C8AA O14 -176.9(4) . . . . ? C47 C9BA C44 C9 0.8(8) . . . . ? C48 C38 C9AA O0AA -2.1(7) . . . . ? C48 C38 C9AA O2AA 177.2(5) . . . . ? C48 C38 C24 C34 -0.1(10) . . . . ? C48 C11 C29 C34 -0.3(11) . . . . ? C48 C11 C29 C39 -179.8(6) . . . . ? C49 C40 C3AA C5BA 1.3(8) . . . . ? C49 C4AA C6AA C5BA 2.7(9) . . . . ? C49 C4AA C6AA C27 -178.0(6) . . . . ? C2BA C4BA C37 O2 -13.8(6) . . . . ? C2BA C4BA C37 O16 166.9(4) . . . . ? C2BA C4BA C0BA C46 2.4(7) . . . . ? C3AA C40 C49 C4AA -1.5(8) . . . . ? C3AA C5BA C6AA C4AA -3.0(9) . . . . ? C3AA C5BA C6AA C27 177.7(6) . . . . ? C5AA C42 C46 C0BA 1.3(8) . . . . ? C0BA C4BA C37 O2 165.9(4) . . . . ? C0BA C4BA C37 O16 -13.5(7) . . . . ? C0BA C4BA C2BA C5AA -0.5(7) . . . . ? C1AA C42 C46 C0BA -179.9(5) . . . . ? C1AA C42 C5AA C2BA -178.2(5) . . . . ? C2 C43 C14 C16 -2.5(8) . . . . ? C4CA C3BA C18 C15 1.6(8) . . . . ? C4CA C23 C26 C15 0.0(11) . . . . ? C4CA C23 C26 C4 179.6(7) . . . . ? C1CA C3CA C16 C14 1.2(9) . . . . ? C7 C6 C9 C44 -0.4(9) . . . . ? C8 C8BA C45 C17 1.8(8) . . . . ? C8 C20 C21 C17 0.2(11) . . . . ? C8 C20 C21 C3 -177.1(7) . . . . ? C9 C6 C7 C47 0.3(9) . . . . ? C10 C36 C13 C32 -0.7(9) . . . . ? C10 C19 C30 C32 -2.4(11) . . . . ? C10 C19 C30 C0AA 178.7(7) . . . . ? C11 C29 C34 C24 2.0(13) . . . . ? C0CA C6 C7 C47 -178.6(6) . . . . ? C0CA C6 C9 C44 178.5(6) . . . . ? C13 C36 C10 C19 0.3(9) . . . . ? C14 C43 C2 C1CA 1.1(8) . . . . ? C16 C3CA C1CA C2 -2.6(9) . . . . ? C18 C3BA C4CA C23 -0.7(8) . . . . ? C18 C15 C26 C23 0.9(11) . . . . ? C18 C15 C26 C4 -178.7(8) . . . . ? C19 C30 C32 C13 1.9(12) . . . . ? C22 N1 C33 O31 179.9(8) . . . . ? C24 C38 C9AA O0AA 176.4(5) . . . . ? C24 C38 C9AA O2AA -4.2(7) . . . . ? C24 C38 C48 C11 1.8(8) . . . . ? C26 C15 C18 C3BA -1.7(10) . . . . ? C28 N1 C33 O31 3.2(14) . . . . ? C39 C29 C34 C24 -178.4(7) . . . . ? C1 C3CA C1CA C2 178.3(6) . . . . ? C1 C3CA C16 C14 -179.7(6) . . . . ? C0AA C30 C32 C13 -179.2(7) . . . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 -0.226 3227.6 398.0 '1DMF, 1/2 isopropanol' 2 0.022 0.333 0.583 202.0 18.1 ? 3 -0.022 0.311 0.917 202.0 18.1 ? 4 0.000 0.356 0.250 202.0 18.1 ? 5 0.000 0.644 0.750 202.0 16.1 ? 6 0.022 0.689 0.083 202.0 16.1 ? 7 -0.022 0.667 0.417 202.0 16.1 ? 8 0.333 0.667 -0.831 3227.6 398.0 '1DMF, 1/2 isopropanol' 9 0.311 0.333 0.083 202.0 16.1 ? 10 0.311 0.978 0.583 202.0 18.1 ? 11 0.333 0.311 0.417 202.0 16.1 ? 12 0.333 0.022 0.917 202.0 18.1 ? 13 0.356 0.356 0.750 202.0 16.1 ? 14 0.356 1.000 0.250 202.0 18.1 ? 15 0.667 0.333 -0.164 3227.6 398.0 '1DMF, 1/2 isopropanol' 16 0.644 0.644 0.250 202.0 18.1 ? 17 0.644 0.000 0.750 202.0 16.1 ? 18 0.667 0.689 0.583 202.0 18.1 ? 19 0.667 0.978 0.083 202.0 16.1 ? 20 0.689 0.667 0.917 202.0 18.1 ? 21 0.689 0.022 0.417 202.0 16.1 ? _olex2_submission_special_instructions 'No special instructions were received' data_[Ti8Zr2O12(PTBB)16] _audit_creation_date 2017-08-16 _audit_creation_method ; Olex2 1.2 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375) ; _shelx_SHELXL_version_number '2014/7' _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_id_orcid ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. A71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C176 H208 O44 Ti8 Zr2' _chemical_formula_sum 'C176 H208 O44 Ti8 Zr2' _chemical_formula_weight 3593.05 _chemical_absolute_configuration ? _chemical_melting_point ? 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' 'Zr' 'Zr' -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'monoclinic' _space_group_IT_number 4 _space_group_name_H-M_alt 'P 1 21 1' _space_group_name_Hall 'P 2yb' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 15.818(12) _cell_length_b 35.48(3) _cell_length_c 18.356(14) _cell_angle_alpha 90 _cell_angle_beta 108.901(12) _cell_angle_gamma 90 _cell_volume 9745(13) _cell_formula_units_Z 2 _cell_measurement_reflns_used 795 _cell_measurement_temperature 100 _cell_measurement_theta_max 15.0316 _cell_measurement_theta_min 2.2715 _shelx_estimated_absorpt_T_max 0.963 _shelx_estimated_absorpt_T_min 0.954 _exptl_absorpt_coefficient_mu 0.480 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type ? _exptl_absorpt_process_details ? _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 3744 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.3746 _diffrn_reflns_av_unetI/netI 0.4927 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 39 _diffrn_reflns_limit_k_min -39 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 82153 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 23.428 _diffrn_reflns_theta_max 23.428 _diffrn_reflns_theta_min 1.588 _diffrn_ambient_temperature 100 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.955 _reflns_Friedel_fraction_full 0.984 _reflns_Friedel_fraction_max 0.984 _reflns_number_gt 7874 _reflns_number_total 28257 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. Structure factors included contributions from the .fab file. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _refine_diff_density_max 2.627 _refine_diff_density_min -1.019 _refine_diff_density_rms 0.169 _refine_ls_abs_structure_details ; Flack x determined using 1921 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.48(7) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1297 _refine_ls_number_reflns 28257 _refine_ls_number_restraints 1523 _refine_ls_R_factor_all 0.3539 _refine_ls_R_factor_gt 0.1501 _refine_ls_restrained_S_all 0.948 _refine_ls_shift/su_max 0.012 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3350 _refine_ls_wR_factor_ref 0.4523 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C60-C59 = C18-C69 2.2 with sigma of 0.005 C1-C63 = C84-C65 = C4-C19 = C75-C57 1.5 with sigma of 0.005 C7-O1 1.25 with sigma of 0.005 C59-C75 = C107-C43 = C18-C19 1.4 with sigma of 0.005 C88-C40 = C49-C42 = C156-C78 = C156-C51 = C3-C95 1.4 with sigma of 0.005 C93-C81 = C89-C97 = C59-C178 = C63-C3 = C63-C32 1.4 with sigma of 0.005 C19-O22 \\sim C19-O31 with sigma of 0.02 C99-C100 \\sim C99-C101 \\sim C100-C101 with sigma of 0.04 C103-C104 \\sim C103-C105 \\sim C103-C106 \\sim C103-C102 with sigma of 0.02 C104-C105 \\sim C104-C106 \\sim C105-C106 with sigma of 0.04 C102-C104 \\sim C102-C105 \\sim C102-C106 with sigma of 0.04 C113-C114 \\sim C113-C115 \\sim C113-C116 \\sim C113-C112 with sigma of 0.02 C114-C115 \\sim C114-C116 \\sim C115-C116 with sigma of 0.04 C112-C114 \\sim C112-C115 \\sim C112-C116 with sigma of 0.04 C118-C119 \\sim C118-C120 \\sim C118-C121 \\sim C118-C117 with sigma of 0.02 C119-C120 \\sim C119-C121 \\sim C120-C121 with sigma of 0.04 C117-C119 \\sim C117-C120 \\sim C117-C121 with sigma of 0.04 C123-C124 \\sim C123-C125 \\sim C123-C126 \\sim C123-C122 with sigma of 0.02 C124-C125 \\sim C124-C126 \\sim C125-C126 with sigma of 0.04 C122-C124 \\sim C122-C125 \\sim C122-C126 with sigma of 0.04 C128-C129 \\sim C128-C130 \\sim C128-C131 \\sim C128-C127 with sigma of 0.02 C129-C130 \\sim C129-C131 \\sim C130-C131 with sigma of 0.04 C127-C129 \\sim C127-C130 \\sim C127-C131 with sigma of 0.04 C133-C134 \\sim C133-C135 \\sim C133-C136 \\sim C133-C132 with sigma of 0.02 C134-C135 \\sim C134-C136 \\sim C135-C136 with sigma of 0.04 C132-C134 \\sim C132-C135 \\sim C132-C136 with sigma of 0.04 C138-C139 \\sim C138-C140 \\sim C138-C141 \\sim C138-C137 with sigma of 0.02 C139-C140 \\sim C139-C141 \\sim C140-C141 with sigma of 0.04 C137-C139 \\sim C137-C140 \\sim C137-C141 with sigma of 0.04 C143-C144 \\sim C143-C145 \\sim C143-C146 \\sim C143-C142 with sigma of 0.02 C144-C145 \\sim C144-C146 \\sim C145-C146 with sigma of 0.04 C142-C144 \\sim C142-C145 \\sim C142-C146 with sigma of 0.04 C148-C149 \\sim C148-C150 \\sim C148-C151 \\sim C148-C147 with sigma of 0.02 C149-C150 \\sim C149-C151 \\sim C150-C151 with sigma of 0.04 C147-C149 \\sim C147-C150 \\sim C147-C151 with sigma of 0.04 C153-C154 \\sim C153-C155 \\sim C153-C156 \\sim C153-C152 with sigma of 0.02 C154-C155 \\sim C154-C156 \\sim C155-C156 with sigma of 0.04 C152-C154 \\sim C152-C155 \\sim C152-C156 with sigma of 0.04 C158-C159 \\sim C158-C160 \\sim C158-C161 \\sim C158-C157 with sigma of 0.02 C159-C160 \\sim C159-C161 \\sim C160-C161 with sigma of 0.04 C157-C159 \\sim C157-C160 \\sim C157-C161 with sigma of 0.04 C163-C164 \\sim C163-C165 \\sim C163-C166 \\sim C163-C162 with sigma of 0.02 C164-C165 \\sim C164-C166 \\sim C165-C166 with sigma of 0.04 C162-C164 \\sim C162-C165 \\sim C162-C166 with sigma of 0.04 C168-C169 \\sim C168-C170 \\sim C168-C171 \\sim C168-C167 with sigma of 0.02 C169-C170 \\sim C169-C171 \\sim C170-C171 with sigma of 0.04 C167-C169 \\sim C167-C170 \\sim C167-C171 with sigma of 0.04 C173-C174 \\sim C173-C175 \\sim C173-C176 \\sim C173-C172 with sigma of 0.02 C174-C175 \\sim C174-C176 \\sim C175-C176 with sigma of 0.04 C172-C174 \\sim C172-C175 \\sim C172-C176 with sigma of 0.04 C108-C109 \\sim C108-C110 \\sim C108-C111 \\sim C108-C107 with sigma of 0.02 C109-C110 \\sim C109-C111 \\sim C110-C111 with sigma of 0.04 C107-C109 \\sim C107-C110 \\sim C107-C111 with sigma of 0.04 C5-O14 \\sim C5-O42 with sigma of 0.02 C98-C99 \\sim C98-C100 \\sim C98-C101 \\sim C98-C97 with sigma of 0.02 C97-C99 \\sim C97-C100 \\sim C97-C101 with sigma of 0.04 C41-C151 \\sim C151-C12 \\sim C52-C12 \\sim C41-C39 \\sim C44-C39 \\sim C52-C44 with sigma of 0.02 3. Restrained planarity C102, C64, C29, C40, C88, C85 with sigma of 0.1 C145, C95, C3, C63, C32, C82, C143, C1 with sigma of 0.1 C9, C48, C68, C71, C56, C132, C20, C133 with sigma of 0.1 C7, C6, C46, C91, C174, C93, C81, C173 with sigma of 0.1 C47, C177, C89, C97, C21, C87 with sigma of 0.1 4. Uiso/Uaniso restraints and constraints C102 \\sim C103 \\sim C104 \\sim C105 \\sim C106: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C112 \\sim C113 \\sim C114 \\sim C115 \\sim C116: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C122 \\sim C123 \\sim C124 \\sim C125 \\sim C126: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C127 \\sim C128 \\sim C129 \\sim C130 \\sim C131: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C132 \\sim C133 \\sim C134 \\sim C135 \\sim C136: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C137 \\sim C138 \\sim C139 \\sim C140 \\sim C141: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C142 \\sim C143 \\sim C144 \\sim C145 \\sim C146: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C147 \\sim C148 \\sim C149 \\sim C150 \\sim C151: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C152 \\sim C153 \\sim C154 \\sim C155 \\sim C156: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C157 \\sim C158 \\sim C159 \\sim C160 \\sim C161: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C162 \\sim C163 \\sim C164 \\sim C165 \\sim C166: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C167 \\sim C168 \\sim C169 \\sim C170 \\sim C171: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C172 \\sim C173 \\sim C174 \\sim C175 \\sim C176: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C107 \\sim C108 \\sim C109 \\sim C110 \\sim C111: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 C97 \\sim C98 \\sim C99 \\sim C100 \\sim C101: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C84) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O1) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O10) \\sim Ueq, Uanis(O11) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(O13) \\sim Ueq, Uanis(O14) \\sim Ueq, Uanis(O15) \\sim Ueq, Uanis(O16) \\sim Ueq, Uanis(O17) \\sim Ueq, Uanis(O18) \\sim Ueq, Uanis(O19) \\sim Ueq, Uanis(O20) \\sim Ueq, Uanis(O21) \\sim Ueq, Uanis(O22) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O24) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O27) \\sim Ueq, Uanis(O28) \\sim Ueq, Uanis(O29) \\sim Ueq, Uanis(O30) \\sim Ueq, Uanis(O31) \\sim Ueq, Uanis(O32) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O35) \\sim Ueq, Uanis(O36) \\sim Ueq, Uanis(O37) \\sim Ueq, Uanis(O38) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(O41) \\sim Ueq, Uanis(O42) \\sim Ueq, Uanis(O43) \\sim Ueq, Uanis(O44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C4) \\sim Ueq, Uanis(C19) \\sim Ueq, Uanis(C69) \\sim Ueq, Uanis(C96) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C18) \\sim Ueq, Uanis(C159) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C57) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C178) \\sim Ueq, Uanis(C137) \\sim Ueq, Uanis(C79) \\sim Ueq, Uanis(C60) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C38) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C15) \\sim Ueq, Uanis(C10) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq, Uanis(C74) \\sim Ueq, Uanis(C151) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C130) = Uanis(C128) = Uanis(C127) = Uanis(C129) = Uanis(C131) = Uanis(C70) = Uanis(C62) = Uanis(C23) = Uanis(C77) = Uanis(C86) Uanis(C1) = Uanis(C63) = Uanis(C3) = Uanis(C95) = Uanis(C145) = Uanis(C82) = Uanis(C32) = Uanis(C143) = Uanis(C146) = Uanis(C144) = Uanis(C142) Uanis(C57) = Uanis(C75) = Uanis(C59) = Uanis(C178) = Uanis(C137) = Uanis(C79) = Uanis(C60) Uanis(C7) = Uanis(C6) = Uanis(C46) = Uanis(C91) = Uanis(C174) = Uanis(C93) = Uanis(C81) = Uanis(C172) = Uanis(C176) = Uanis(C173) = Uanis(C175) Uanis(C33) = Uanis(C61) = Uanis(C72) = Uanis(C27) = Uanis(C58) = Uanis(C92) Uanis(C5) = Uanis(C25) = Uanis(C11) = Uanis(C36) = Uanis(C43) = Uanis(C16) = Uanis(C107) = Uanis(C108) = Uanis(C109) = Uanis(C111) = Uanis(C110) Uanis(C34) = Uanis(C22) = Uanis(C162) = Uanis(C31) = Uanis(C67) = Uanis(C2) = Uanis(C37) Uanis(C66) = Uanis(C40) = Uanis(C88) = Uanis(C29) = Uanis(C64) = Uanis(C102) = Uanis(C85) = Uanis(C103) = Uanis(C106) = Uanis(C104) = Uanis(C105) Uanis(C15) = Uanis(C10) = Uanis(C76) = Uanis(C54) = Uanis(C53) = Uanis(C122) = Uanis(C45) = Uanis(C123) = Uanis(C125) = Uanis(C124) = Uanis(C126) Uanis(C30) = Uanis(C47) = Uanis(C177) = Uanis(C89) = Uanis(C97) = Uanis(C21) = Uanis(C87) Uanis(C65) = Uanis(C50) = Uanis(C55) = Uanis(C117) = Uanis(C80) = Uanis(C73) = Uanis(C118) = Uanis(C120) = Uanis(C121) = Uanis(C119) Uanis(C24) = Uanis(C18) = Uanis(C19) = Uanis(C69) = Uanis(C96) = Uanis(C4) Uanis(C49) = Uanis(C90) = Uanis(C78) = Uanis(C156) = Uanis(C51) = Uanis(C42) = Uanis(C13) Uanis(C17) = Uanis(C28) = Uanis(C26) = Uanis(C94) = Uanis(C169) = Uanis(C8) = Uanis(C14) Uanis(C9) = Uanis(C68) = Uanis(C48) = Uanis(C20) = Uanis(C132) = Uanis(C56) = Uanis(C71) = Uanis(C133) = Uanis(C135) = Uanis(C134) = Uanis(C136) Uanis(C74) = Uanis(C44) = Uanis(C39) = Uanis(C41) = Uanis(C151) = Uanis(C12) = Uanis(C52) Uanis(C30) = Uanis(C47) = Uanis(C87) = Uanis(C21) = Uanis(C97) = Uanis(C89) = Uanis(C177) = Uanis(C100) = Uanis(C98) = Uanis(C101) = Uanis(C99) Uanis(C84) = Uanis(C65) = Uanis(C50) = Uanis(C55) = Uanis(C73) = Uanis(C80) = Uanis(C117) = Uanis(C118) = Uanis(C120) = Uanis(C121) = Uanis(C119) 5. Rigid body (RIGU) restrains C102, C103, C104, C105, C106 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C112, C113, C114, C115, C116 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C117, C118, C119, C120, C121 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C122, C123, C124, C125, C126 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C127, C128, C129, C130, C131 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C132, C133, C134, C135, C136 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C137, C138, C139, C140, C141 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C142, C143, C144, C145, C146 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C147, C148, C149, C150, C151 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C152, C153, C154, C155, C156 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C157, C158, C159, C160, C161 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C162, C163, C164, C165, C166 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C167, C168, C169, C170, C171 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C172, C173, C174, C175, C176 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C107, C108, C109, C110, C111 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 C97, C98, C99, C100, C101 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6.a Me refined with riding coordinates: C99(H99A,H99B,H99C), C100(H10A,H10B,H10C), C101(H10D,H10E,H10F), C104(H10G, H10H,H10I), C105(H10J,H10K,H10L), C106(H10M,H10N,H10O), C109(H10P,H10Q,H10R), C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C114(H11G,H11H,H11I), C115(H11J, H11K,H11L), C116(H11M,H11N,H11O), C119(H11P,H11Q,H11R), C120(H12A,H12B,H12C), C121(H12D,H12E,H12F), C124(H12G,H12H,H12I), C125(H12J,H12K,H12L), C126(H12M, H12N,H12O), C127(H12P,H12Q,H12R), C129(H12S,H12T,H12U), C130(H13A,H13B,H13C), C134(H13D,H13E,H13F), C135(H13G,H13H,H13I), C136(H13J,H13K,H13L), C139(H13M, H13N,H13O), C140(H14A,H14B,H14C), C141(H14D,H14E,H14F), C142(H14G,H14H,H14I), C144(H14J,H14K,H14L), C146(H14M,H14N,H14O), C147(H14P,H14Q,H14R), C149(H14S, H14T,H14U), C150(H15A,H15B,H15C), C152(H15D,H15E,H15F), C154(H15G,H15H,H15I), C155(H15J,H15K,H15L), C157(H15M,H15N,H15O), C160(H16A,H16B,H16C), C161(H16D, H16E,H16F), C164(H16G,H16H,H16I), C165(H16J,H16K,H16L), C166(H16M,H16N,H16O), C167(H16P,H16Q,H16R), C170(H17A,H17B,H17C), C171(H17D,H17E,H17F), C172(H17G, H17H,H17I), C175(H17J,H17K,H17L), C176(H17M,H17N,H17O) 6.b Aromatic/amide H refined with riding coordinates: C3(H3), C8(H8), C11(H11), C12(H12), C14(H14), C16(H16), C18(H18), C20(H20), C21(H21), C22(H22), C24(H24), C26(H26), C27(H27), C29(H29), C31(H31), C32(H32), C34(H34), C36(H36), C39(H39), C41(H41), C42(H42), C43(H43), C45(H45), C46(H46), C48(H48), C50(H50), C51(H51), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C58(H58), C59(H59), C60(H60), C62(H62), C64(H64), C67(H67), C69(H69), C70(H70), C71(H71), C72(H72), C73(H73), C76(H76), C77(H77), C78(H78), C79(H79), C80(H80), C81(H81), C82(H82), C85(H85), C86(H86), C87(H87), C88(H88), C89(H89), C90(H90), C91(H91), C92(H92), C93(H93), C94(H94), C95(H95), C96(H96), C177(H177), C178(H178) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr01 Zr 0.3518(3) 0.59441(13) 0.3122(3) 0.0464(13) Uani 1 1 d . . . . . Zr02 Zr 0.5331(3) 0.40383(13) 0.3144(3) 0.0499(14) Uani 1 1 d . . . . . Ti9 Ti 0.3346(5) 0.4284(2) 0.3015(6) 0.052(3) Uani 1 1 d . . . . . Ti04 Ti 0.6347(5) 0.4822(2) 0.3273(5) 0.050(3) Uani 1 1 d . . . . . Ti05 Ti 0.4409(6) 0.5409(2) 0.4548(5) 0.054(3) Uani 1 1 d . . . . . Ti06 Ti 0.5252(5) 0.4532(2) 0.4585(5) 0.048(2) Uani 1 1 d . . . . . Ti07 Ti 0.3623(5) 0.5456(2) 0.1713(5) 0.047(2) Uani 1 1 d . . . . . Ti08 Ti 0.4465(5) 0.4582(2) 0.1736(5) 0.045(2) Uani 1 1 d . . . . . Ti0A Ti 0.5516(5) 0.5704(2) 0.3246(5) 0.046(2) Uani 1 1 d . . . . . O1 O 0.296(2) 0.6268(9) 0.2098(19) 0.065(9) Uani 1 1 d D U . . . O2 O 0.271(2) 0.4255(8) 0.3913(17) 0.062(9) Uani 1 1 d . U . . . O3 O 0.4831(17) 0.5743(7) 0.3907(15) 0.042(7) Uani 1 1 d . U . . . O4 O 0.5606(17) 0.5410(8) 0.5389(14) 0.043(7) Uani 1 1 d . U . . . O5 O 0.4181(13) 0.5019(5) 0.2113(12) 0.015(5) Uani 1 1 d . U . . . O6 O 0.5561(16) 0.5211(7) 0.3242(14) 0.036(7) Uani 1 1 d . U . . . O7 O 0.3317(16) 0.5468(7) 0.3805(14) 0.036(7) Uani 1 1 d . U . . . O8 O 0.731(2) 0.5110(9) 0.4186(17) 0.065(9) Uani 1 1 d . U . . . O9 O 0.4278(16) 0.6444(6) 0.3218(13) 0.026(6) Uani 1 1 d . U . . . O10 O 0.6021(18) 0.4470(8) 0.3996(15) 0.049(8) Uani 1 1 d . U . . . O11 O 0.3563(16) 0.6248(7) 0.4249(15) 0.031(6) Uani 1 1 d . U . . . O12 O 0.6788(17) 0.5137(8) 0.2562(15) 0.049(8) Uani 1 1 d . U . . . O13 O 0.671(2) 0.3972(8) 0.3245(17) 0.062(9) Uani 1 1 d . U . . . O14 O 0.2114(17) 0.4270(7) 0.2176(15) 0.044(7) Uani 1 1 d D U . . . O15 O 0.4441(19) 0.5762(8) 0.2511(16) 0.054(8) Uani 1 1 d . U . . . O16 O 0.4469(15) 0.4214(6) 0.3850(14) 0.030(6) Uani 1 1 d . U . . . C1 C 0.663(3) 0.5448(15) 0.221(3) 0.088(6) Uani 1 1 d D . . . . O17 O 0.2913(19) 0.5899(8) 0.1066(16) 0.057(8) Uani 1 1 d . U . . . O18 O 0.4103(18) 0.5848(8) 0.5130(16) 0.051(8) Uani 1 1 d . U . . . O19 O 0.6183(14) 0.5700(6) 0.2457(13) 0.021(6) Uani 1 1 d . U . . . O20 O 0.1403(16) 0.5510(7) 0.2968(14) 0.039(7) Uani 1 1 d . U . . . O21 O 0.5284(16) 0.3755(7) 0.2071(15) 0.032(7) Uani 1 1 d . U . . . O22 O 0.4527(18) 0.4507(8) 0.5304(14) 0.050(8) Uani 1 1 d D U . . . O23 O 0.574(2) 0.6312(8) 0.3385(17) 0.056(9) Uani 1 1 d . U . . . O24 O 0.3251(17) 0.4583(7) 0.0928(15) 0.044(7) Uani 1 1 d . U . . . O25 O 0.4663(16) 0.4138(7) 0.1103(14) 0.033(7) Uani 1 1 d . U . . . O26 O 0.4964(15) 0.4894(6) 0.1063(13) 0.026(6) Uani 1 1 d . U . . . O27 O 0.3158(18) 0.3702(8) 0.2968(15) 0.047(8) Uani 1 1 d . U . . . O28 O 0.7410(16) 0.4473(7) 0.3302(14) 0.035(7) Uani 1 1 d . U . . . O29 O 0.6146(19) 0.4807(8) 0.5343(16) 0.059(8) Uani 1 1 d . U . . . O30 O 0.2823(14) 0.5480(6) 0.2334(12) 0.021(6) Uani 1 1 d . U . . . O31 O 0.3958(18) 0.5099(8) 0.5290(15) 0.050(8) Uani 1 1 d D U . . . O32 O 0.589(2) 0.4049(9) 0.5211(17) 0.068(9) Uani 1 1 d . U . . . O33 O 0.6721(18) 0.5698(8) 0.4029(15) 0.045(7) Uani 1 1 d . U . . . O34 O 0.454(2) 0.3518(8) 0.3091(17) 0.062(9) Uani 1 1 d . U . . . O35 O 0.5587(15) 0.4512(7) 0.2476(13) 0.031(6) Uani 1 1 d . U . . . C2 C 0.172(3) 0.4416(12) 0.456(3) 0.065(6) Uani 1 1 d . . . . . O36 O 0.2053(17) 0.4852(8) 0.3772(15) 0.050(8) Uani 1 1 d . U . . . C3 C 0.687(3) 0.5863(10) 0.123(2) 0.088(6) Uani 1 1 d D . . . . H3 H 0.6339 0.5991 0.1220 0.106 Uiso 1 1 calc R . . . . O37 O 0.4080(15) 0.4233(6) 0.2352(13) 0.029(6) Uani 1 1 d . U . . . O38 O 0.4317(18) 0.5470(8) 0.0935(16) 0.056(8) Uani 1 1 d . U . . . O39 O 0.5938(18) 0.3721(8) 0.4230(17) 0.048(8) Uani 1 1 d . U . . . O40 O 0.3312(14) 0.4782(6) 0.3021(13) 0.022(6) Uani 1 1 d . U . . . C4 C 0.408(3) 0.4784(12) 0.549(2) 0.050(5) Uani 1 1 d D U . . . C5 C 0.146(3) 0.4508(7) 0.199(3) 0.068(5) Uani 1 1 d D . . . . O41 O 0.2679(16) 0.5144(7) 0.0874(14) 0.042(7) Uani 1 1 d . U . . . O42 O 0.1600(16) 0.4864(7) 0.2148(14) 0.045(7) Uani 1 1 d D U . . . C6 C 0.206(3) 0.6459(16) 0.078(4) 0.109(7) Uani 1 1 d . . . . . C7 C 0.274(3) 0.6190(15) 0.140(2) 0.109(7) Uani 1 1 d D . . . . C8 C 0.579(3) 0.2952(11) 0.049(3) 0.060(5) Uani 1 1 d . . . . . H8 H 0.6126 0.2732 0.0687 0.072 Uiso 1 1 calc R . . . . O43 O 0.2193(17) 0.6060(7) 0.3029(14) 0.037(7) Uani 1 1 d . U . . . C9 C 0.747(3) 0.4102(12) 0.335(3) 0.082(5) Uani 1 1 d . . . . . C10 C 0.374(3) 0.6451(15) 0.546(3) 0.074(5) Uani 1 1 d . U . . . C11 C 0.032(3) 0.4018(11) 0.146(3) 0.068(5) Uani 1 1 d . . . . . H11 H 0.0783 0.3835 0.1559 0.081 Uiso 1 1 calc R . . . . C12 C 0.874(3) 0.5173(13) 0.684(3) 0.079(6) Uani 1 1 d D . . . . H12 H 0.9179 0.4988 0.7068 0.095 Uiso 1 1 calc R . . . . C13 C 0.618(4) 0.3771(13) 0.493(4) 0.102(8) Uani 1 1 d . . . . . C14 C 0.556(3) 0.3191(10) 0.100(3) 0.060(5) Uani 1 1 d . . . . . H14 H 0.5621 0.3106 0.1507 0.072 Uiso 1 1 calc R . . . . C15 C 0.385(3) 0.6170(15) 0.487(3) 0.074(5) Uani 1 1 d . U . . . C16 C -0.059(3) 0.3872(11) 0.115(3) 0.068(5) Uani 1 1 d . . . . . H16 H -0.0736 0.3612 0.1055 0.081 Uiso 1 1 calc R . . . . C17 C 0.501(3) 0.3823(11) 0.140(3) 0.060(5) Uani 1 1 d . . . . . C18 C 0.403(3) 0.4376(8) 0.668(2) 0.050(5) Uani 1 1 d D U . . . H18 H 0.4503 0.4226 0.6620 0.060 Uiso 1 1 calc R . . . . C19 C 0.374(3) 0.4657(8) 0.6127(19) 0.050(5) Uani 1 1 d D U . . . C20 C 0.987(3) 0.3835(11) 0.338(3) 0.082(5) Uani 1 1 d . . . . . H20 H 1.0407 0.3949 0.3372 0.098 Uiso 1 1 calc R . . . . O44 O 0.4753(18) 0.4952(8) 0.4231(15) 0.050(8) Uani 1 1 d . U . . . C21 C 0.496(4) 0.7587(17) 0.362(3) 0.094(6) Uani 1 1 d . . . . . H21 H 0.4509 0.7777 0.3512 0.113 Uiso 1 1 calc R . . . . C22 C 0.045(3) 0.4462(11) 0.497(3) 0.065(6) Uani 1 1 d . . . . . H22 H -0.0064 0.4596 0.4979 0.078 Uiso 1 1 calc R . . . . C23 C 0.826(3) 0.5604(14) 0.464(4) 0.097(6) Uani 1 1 d . . . . . C24 C 0.380(3) 0.4283(12) 0.725(3) 0.050(5) Uani 1 1 d . U . . . H24 H 0.4060 0.4076 0.7574 0.060 Uiso 1 1 calc R . . . . C25 C 0.060(3) 0.4400(11) 0.163(3) 0.068(5) Uani 1 1 d . . . . . C26 C 0.498(3) 0.3666(11) 0.004(3) 0.060(5) Uani 1 1 d . . . . . H26 H 0.4742 0.3904 -0.0159 0.072 Uiso 1 1 calc R . . . . C27 C 0.162(3) 0.4314(12) -0.008(3) 0.056(6) Uani 1 1 d . . . . . H27 H 0.2140 0.4172 -0.0047 0.068 Uiso 1 1 calc R . . . . C28 C 0.520(3) 0.3586(11) 0.075(3) 0.060(5) Uani 1 1 d . . . . . C29 C -0.018(4) 0.5888(17) 0.295(4) 0.166(9) Uani 1 1 d . . . . . H29 H -0.0276 0.5624 0.2930 0.199 Uiso 1 1 calc R . . . . C30 C 0.503(4) 0.6506(17) 0.323(3) 0.094(6) Uani 1 1 d . U . . . C31 C 0.090(3) 0.4606(11) 0.451(3) 0.065(6) Uani 1 1 d . . . . . H31 H 0.0681 0.4815 0.4176 0.078 Uiso 1 1 calc R . . . . C32 C 0.798(3) 0.5390(13) 0.172(3) 0.088(6) Uani 1 1 d D . . . . H32 H 0.8225 0.5183 0.2044 0.106 Uiso 1 1 calc R . . . . C33 C 0.253(3) 0.4776(12) 0.067(3) 0.056(6) Uani 1 1 d . . . . . C34 C 0.143(3) 0.3946(11) 0.548(3) 0.065(6) Uani 1 1 d . . . . . H34 H 0.1638 0.3730 0.5793 0.078 Uiso 1 1 calc R . . . . C36 C -0.012(3) 0.4632(11) 0.155(3) 0.068(5) Uani 1 1 d . . . . . H36 H -0.0006 0.4871 0.1791 0.081 Uiso 1 1 calc R . . . . C37 C 0.216(3) 0.4536(12) 0.413(3) 0.065(6) Uani 1 1 d . . . . . C38 C 0.740(3) 0.5471(11) 0.435(2) 0.038(10) Uani 1 1 d . U . . . C39 C 0.731(3) 0.5670(13) 0.625(3) 0.079(6) Uani 1 1 d D . . . . H39 H 0.6887 0.5857 0.6005 0.095 Uiso 1 1 calc R . . . . C40 C 0.063(4) 0.6059(11) 0.295(5) 0.166(9) Uani 1 1 d D . . . . C41 C 0.812(3) 0.5748(14) 0.679(3) 0.079(6) Uani 1 1 d D . . . . H41 H 0.8139 0.5983 0.7047 0.095 Uiso 1 1 calc R . . . . C42 C 0.702(4) 0.3616(13) 0.620(3) 0.102(8) Uani 1 1 d D . . . . H42 H 0.6917 0.3867 0.6338 0.122 Uiso 1 1 calc R . . . . C43 C -0.097(3) 0.4550(8) 0.115(3) 0.068(5) Uani 1 1 d D . . . . H43 H -0.1383 0.4750 0.0971 0.081 Uiso 1 1 calc R . . . . C44 C 0.719(3) 0.5288(12) 0.610(3) 0.079(6) Uani 1 1 d D U . . . C45 C 0.384(3) 0.6548(14) 0.686(3) 0.074(5) Uani 1 1 d . . . . . H45 H 0.3985 0.6460 0.7376 0.088 Uiso 1 1 calc R . . . . C46 C 0.185(3) 0.6778(16) 0.118(4) 0.109(7) Uani 1 1 d . . . . . H46 H 0.2080 0.6820 0.1722 0.131 Uiso 1 1 calc R . . . . C47 C 0.541(4) 0.6949(17) 0.351(3) 0.094(6) Uani 1 1 d . . . . . C48 C 0.903(3) 0.4045(12) 0.337(3) 0.082(5) Uani 1 1 d . . . . . H48 H 0.9079 0.4312 0.3373 0.098 Uiso 1 1 calc R . . . . C49 C 0.669(4) 0.3473(13) 0.545(3) 0.102(8) Uani 1 1 d D . . . . C50 C 0.433(3) 0.2838(13) 0.361(3) 0.067(4) Uani 1 1 d . . . . . H50 H 0.4896 0.2952 0.3837 0.081 Uiso 1 1 calc R . . . . C51 C 0.754(4) 0.3322(11) 0.678(4) 0.102(8) Uani 1 1 d D . . . . H51 H 0.7605 0.3349 0.7310 0.122 Uiso 1 1 calc R . . . . C52 C 0.794(3) 0.5067(15) 0.634(3) 0.079(6) Uani 1 1 d D . . . . H52 H 0.7900 0.4821 0.6124 0.095 Uiso 1 1 calc R . . . . C53 C 0.340(3) 0.7030(15) 0.585(3) 0.074(5) Uani 1 1 d . . . . . H53 H 0.3303 0.7292 0.5761 0.088 Uiso 1 1 calc R . . . . C54 C 0.385(3) 0.6373(15) 0.622(3) 0.074(5) Uani 1 1 d . . . . . H54 H 0.3989 0.6114 0.6326 0.088 Uiso 1 1 calc R . . . . C55 C 0.416(3) 0.2431(13) 0.371(3) 0.067(4) Uani 1 1 d . . . . . H55 H 0.4647 0.2260 0.3884 0.081 Uiso 1 1 calc R . . . . C56 C 0.888(3) 0.3320(12) 0.332(3) 0.082(5) Uani 1 1 d . . . . . H56 H 0.8807 0.3059 0.3201 0.098 Uiso 1 1 calc R . . . . C57 C 0.475(3) 0.5207(13) 0.059(3) 0.059(5) Uani 1 1 d D U . . . C58 C 0.085(3) 0.4148(12) -0.048(3) 0.056(6) Uani 1 1 d . . . . . H58 H 0.0802 0.3886 -0.0602 0.068 Uiso 1 1 calc R . . . . C59 C 0.489(3) 0.5634(9) -0.033(2) 0.059(5) Uani 1 1 d D U . . . H59 H 0.4427 0.5774 -0.0225 0.071 Uiso 1 1 calc R . . . . C60 C 0.569(3) 0.5113(10) -0.006(3) 0.059(5) Uani 1 1 d D U . . . H60 H 0.5818 0.4893 0.0249 0.071 Uiso 1 1 calc R . . . . C61 C 0.178(3) 0.4650(12) 0.027(3) 0.056(6) Uani 1 1 d . . . . . C62 C 0.907(3) 0.5390(14) 0.480(4) 0.097(6) Uani 1 1 d . . . . . H62 H 0.9017 0.5123 0.4782 0.116 Uiso 1 1 calc R . . . . C63 C 0.720(3) 0.5565(11) 0.175(3) 0.088(6) Uani 1 1 d D . . . . C64 C -0.073(4) 0.6123(16) 0.296(3) 0.166(9) Uani 1 1 d . . . . . H64 H -0.1276 0.6013 0.2973 0.199 Uiso 1 1 calc R . . . . C65 C 0.357(3) 0.3041(11) 0.317(3) 0.067(4) Uani 1 1 d D . . . . C66 C 0.148(5) 0.5880(17) 0.292(6) 0.166(9) Uani 1 1 d . . . . . C67 C 0.195(3) 0.4122(11) 0.495(3) 0.065(6) Uani 1 1 d . . . . . H67 H 0.2465 0.3994 0.4933 0.078 Uiso 1 1 calc R . . . . C68 C 0.819(3) 0.3901(11) 0.3367(18) 0.082(5) Uani 1 1 d . . . . . C69 C 0.320(2) 0.4886(9) 0.636(2) 0.050(5) Uani 1 1 d D U . . . H69 H 0.3082 0.5129 0.6139 0.060 Uiso 1 1 calc R . . . . C70 C 0.991(3) 0.5534(13) 0.498(4) 0.097(6) Uani 1 1 d . . . . . H70 H 1.0380 0.5361 0.5005 0.116 Uiso 1 1 calc R . . . . C71 C 0.813(3) 0.3482(11) 0.335(3) 0.082(5) Uani 1 1 d . . . . . H71 H 0.7618 0.3346 0.3363 0.098 Uiso 1 1 calc R . . . . C72 C 0.103(3) 0.4915(12) -0.003(3) 0.056(6) Uani 1 1 d . . . . . H72 H 0.1123 0.5176 0.0075 0.068 Uiso 1 1 calc R . . . . C73 C 0.275(3) 0.2916(14) 0.284(3) 0.067(4) Uani 1 1 d . . . . . H73 H 0.2278 0.3067 0.2514 0.081 Uiso 1 1 calc R . . . . C74 C 0.627(4) 0.5164(16) 0.559(3) 0.079(6) Uani 1 1 d . U . . . C75 C 0.533(3) 0.5337(11) 0.014(2) 0.059(5) Uani 1 1 d D U . . . C76 C 0.337(3) 0.6832(14) 0.519(3) 0.074(5) Uani 1 1 d . . . . . H76 H 0.3172 0.6921 0.4671 0.088 Uiso 1 1 calc R . . . . C77 C 0.838(3) 0.5994(14) 0.483(4) 0.097(6) Uani 1 1 d . . . . . H77 H 0.7899 0.6162 0.4772 0.116 Uiso 1 1 calc R . . . . C78 C 0.756(4) 0.2934(13) 0.575(3) 0.102(8) Uani 1 1 d D . . . . H78 H 0.7727 0.2701 0.5579 0.122 Uiso 1 1 calc R . . . . C79 C 0.596(3) 0.5109(13) -0.065(3) 0.059(5) Uani 1 1 d . U . . . H79 H 0.6226 0.4894 -0.0793 0.071 Uiso 1 1 calc R . . . . C80 C 0.263(3) 0.2524(13) 0.302(3) 0.067(4) Uani 1 1 d . . . . . H80 H 0.2069 0.2411 0.2768 0.081 Uiso 1 1 calc R . . . . C81 C 0.175(3) 0.6441(15) 0.001(4) 0.109(7) Uani 1 1 d D . . . . H81 H 0.1978 0.6255 -0.0248 0.131 Uiso 1 1 calc R . . . . C82 C 0.835(4) 0.5507(13) 0.125(3) 0.088(6) Uani 1 1 d . . . . . H82 H 0.8891 0.5390 0.1244 0.106 Uiso 1 1 calc R . . . . C84 C 0.381(4) 0.3441(11) 0.306(3) 0.067(4) Uani 1 1 d D U . . . C85 C -0.007(4) 0.6718(16) 0.288(5) 0.166(9) Uani 1 1 d . . . . . H85 H -0.0096 0.6982 0.2786 0.199 Uiso 1 1 calc R . . . . C86 C 0.933(3) 0.6120(13) 0.511(4) 0.097(6) Uani 1 1 d . . . . . H86 H 0.9443 0.6369 0.5309 0.116 Uiso 1 1 calc R . . . . C87 C 0.473(4) 0.7183(16) 0.346(3) 0.094(6) Uani 1 1 d . . . . . H87 H 0.4130 0.7095 0.3324 0.113 Uiso 1 1 calc R . . . . C88 C 0.071(4) 0.6452(11) 0.297(5) 0.166(9) Uani 1 1 d D . . . . H88 H 0.1285 0.6559 0.3046 0.199 Uiso 1 1 calc R . . . . C89 C 0.657(3) 0.7471(14) 0.399(3) 0.094(6) Uani 1 1 d D . . . . H89 H 0.7175 0.7552 0.4152 0.113 Uiso 1 1 calc R . . . . C90 C 0.696(4) 0.3167(13) 0.518(4) 0.102(8) Uani 1 1 d . . . . . H90 H 0.6764 0.3106 0.4650 0.122 Uiso 1 1 calc R . . . . C91 C 0.126(3) 0.7009(16) 0.066(4) 0.109(7) Uani 1 1 d . . . . . H91 H 0.1109 0.7227 0.0896 0.131 Uiso 1 1 calc R . . . . C92 C 0.022(3) 0.4795(12) -0.044(3) 0.056(6) Uani 1 1 d . . . . . H92 H -0.0277 0.4960 -0.0550 0.068 Uiso 1 1 calc R . . . . C93 C 0.109(3) 0.6689(15) -0.043(4) 0.109(7) Uani 1 1 d D . . . . H93 H 0.0800 0.6650 -0.0963 0.131 Uiso 1 1 calc R . . . . Ti1 Ti 0.2488(5) 0.5163(2) 0.2989(5) 0.045(2) Uani 1 1 d . . . . . C94 C 0.514(3) 0.3356(10) -0.046(3) 0.060(5) Uani 1 1 d . . . . . H94 H 0.4908 0.3396 -0.1003 0.072 Uiso 1 1 calc R . . . . C95 C 0.735(3) 0.5967(13) 0.075(2) 0.088(6) Uani 1 1 d D . . . . H95 H 0.7159 0.6171 0.0395 0.106 Uiso 1 1 calc R . . . . C96 C 0.276(3) 0.4784(12) 0.697(2) 0.050(5) Uani 1 1 d . U . . . H96 H 0.2270 0.4916 0.7034 0.060 Uiso 1 1 calc R . . . . C97 C 0.577(3) 0.7666(14) 0.389(3) 0.094(6) Uani 1 1 d D U . . . C98 C 0.611(2) 0.8061(12) 0.419(2) 0.094(6) Uani 1 1 d D U . . . C99 C 0.653(3) 0.8290(13) 0.369(3) 0.094(6) Uani 1 1 d D U . . . H99A H 0.7000 0.8142 0.3590 0.141 Uiso 1 1 calc R . . . . H99B H 0.6069 0.8353 0.3203 0.141 Uiso 1 1 calc R . . . . H99C H 0.6784 0.8523 0.3961 0.141 Uiso 1 1 calc R . . . . C100 C 0.680(3) 0.8068(14) 0.500(2) 0.094(6) Uani 1 1 d D U . . . H10A H 0.6575 0.7926 0.5358 0.141 Uiso 1 1 calc R . . . . H10B H 0.7361 0.7954 0.4988 0.141 Uiso 1 1 calc R . . . . H10C H 0.6914 0.8330 0.5181 0.141 Uiso 1 1 calc R . . . . C101 C 0.539(3) 0.8327(12) 0.430(3) 0.094(6) Uani 1 1 d D U . . . H10D H 0.5083 0.8202 0.4619 0.141 Uiso 1 1 calc R . . . . H10E H 0.5677 0.8558 0.4555 0.141 Uiso 1 1 calc R . . . . H10F H 0.4961 0.8389 0.3797 0.141 Uiso 1 1 calc R . . . . C102 C -0.075(3) 0.6489(13) 0.297(3) 0.166(9) Uani 1 1 d D U . . . C103 C -0.155(3) 0.6798(10) 0.302(3) 0.166(9) Uani 1 1 d D U . . . C104 C -0.130(4) 0.6971(13) 0.392(3) 0.166(9) Uani 1 1 d D U . . . H10G H -0.0729 0.7105 0.4055 0.249 Uiso 1 1 calc R . . . . H10H H -0.1772 0.7145 0.3939 0.249 Uiso 1 1 calc R . . . . H10I H -0.1259 0.6763 0.4278 0.249 Uiso 1 1 calc R . . . . C105 C -0.252(3) 0.6568(14) 0.276(4) 0.166(9) Uani 1 1 d D U . . . H10J H -0.2653 0.6470 0.2234 0.249 Uiso 1 1 calc R . . . . H10K H -0.2486 0.6358 0.3114 0.249 Uiso 1 1 calc R . . . . H10L H -0.2999 0.6741 0.2776 0.249 Uiso 1 1 calc R . . . . C106 C -0.157(4) 0.7153(13) 0.240(4) 0.166(9) Uani 1 1 d D U . . . H10M H -0.0989 0.7283 0.2567 0.249 Uiso 1 1 calc R . . . . H10N H -0.1681 0.7051 0.1883 0.249 Uiso 1 1 calc R . . . . H10O H -0.2042 0.7332 0.2399 0.249 Uiso 1 1 calc R . . . . C107 C -0.126(2) 0.4177(8) 0.099(3) 0.068(5) Uani 1 1 d D U . . . C108 C -0.234(2) 0.4043(7) 0.0663(18) 0.068(5) Uani 1 1 d D U . . . C109 C -0.277(2) 0.4255(10) -0.018(2) 0.068(5) Uani 1 1 d D U . . . H10P H -0.2754 0.4528 -0.0104 0.101 Uiso 1 1 calc R . . . . H10Q H -0.2408 0.4190 -0.0510 0.101 Uiso 1 1 calc R . . . . H10R H -0.3384 0.4172 -0.0426 0.101 Uiso 1 1 calc R . . . . C110 C -0.277(3) 0.4210(10) 0.132(2) 0.068(5) Uani 1 1 d D U . . . H11A H -0.2503 0.4076 0.1812 0.101 Uiso 1 1 calc R . . . . H11B H -0.2641 0.4480 0.1400 0.101 Uiso 1 1 calc R . . . . H11C H -0.3420 0.4171 0.1147 0.101 Uiso 1 1 calc R . . . . C111 C -0.233(3) 0.3576(8) 0.061(3) 0.068(5) Uani 1 1 d D U . . . H11D H -0.2070 0.3471 0.1132 0.101 Uiso 1 1 calc R . . . . H11E H -0.2937 0.3481 0.0380 0.101 Uiso 1 1 calc R . . . . H11F H -0.1962 0.3499 0.0296 0.101 Uiso 1 1 calc R . . . . C112 C 0.011(4) 0.4408(14) -0.071(3) 0.109(15) Uani 1 1 d D U . . . C113 C -0.083(3) 0.4243(11) -0.130(2) 0.114(13) Uani 1 1 d D U . . . C114 C -0.166(3) 0.4545(14) -0.142(3) 0.111(15) Uani 1 1 d D U . . . H11G H -0.2209 0.4438 -0.1766 0.166 Uiso 1 1 calc R . . . . H11H H -0.1732 0.4599 -0.0918 0.166 Uiso 1 1 calc R . . . . H11I H -0.1515 0.4779 -0.1637 0.166 Uiso 1 1 calc R . . . . C115 C -0.111(4) 0.3847(13) -0.096(3) 0.121(16) Uani 1 1 d D U . . . H11J H -0.1679 0.3754 -0.1315 0.181 Uiso 1 1 calc R . . . . H11K H -0.0645 0.3658 -0.0905 0.181 Uiso 1 1 calc R . . . . H11L H -0.1181 0.3894 -0.0454 0.181 Uiso 1 1 calc R . . . . C116 C -0.071(4) 0.4153(15) -0.214(3) 0.135(17) Uani 1 1 d D U . . . H11M H -0.1276 0.4053 -0.2491 0.202 Uiso 1 1 calc R . . . . H11N H -0.0555 0.4385 -0.2352 0.202 Uiso 1 1 calc R . . . . H11O H -0.0239 0.3966 -0.2073 0.202 Uiso 1 1 calc R . . . . C117 C 0.328(3) 0.2302(12) 0.354(2) 0.067(4) Uani 1 1 d D U . . . C118 C 0.3162(19) 0.1891(10) 0.3641(17) 0.067(4) Uani 1 1 d D U . . . C119 C 0.235(2) 0.1819(12) 0.385(2) 0.067(4) Uani 1 1 d D U . . . H11P H 0.2397 0.1948 0.4330 0.101 Uiso 1 1 calc R . . . . H11Q H 0.1827 0.1914 0.3437 0.101 Uiso 1 1 calc R . . . . H11R H 0.2285 0.1547 0.3908 0.101 Uiso 1 1 calc R . . . . C120 C 0.393(3) 0.1752(12) 0.427(2) 0.067(4) Uani 1 1 d D U . . . H12A H 0.3960 0.1882 0.4752 0.101 Uiso 1 1 calc R . . . . H12B H 0.3867 0.1480 0.4337 0.101 Uiso 1 1 calc R . . . . H12C H 0.4483 0.1800 0.4154 0.101 Uiso 1 1 calc R . . . . C121 C 0.310(3) 0.1703(11) 0.293(2) 0.067(4) Uani 1 1 d D U . . . H12D H 0.2588 0.1800 0.2511 0.101 Uiso 1 1 calc R . . . . H12E H 0.3651 0.1751 0.2799 0.101 Uiso 1 1 calc R . . . . H12F H 0.3035 0.1431 0.2982 0.101 Uiso 1 1 calc R . . . . C122 C 0.350(3) 0.6946(13) 0.650(3) 0.074(5) Uani 1 1 d D U . . . C123 C 0.353(2) 0.7250(10) 0.713(2) 0.074(5) Uani 1 1 d D U . . . C124 C 0.334(3) 0.7652(10) 0.676(3) 0.074(5) Uani 1 1 d D U . . . H12G H 0.3760 0.7706 0.6483 0.111 Uiso 1 1 calc R . . . . H12H H 0.2725 0.7661 0.6396 0.111 Uiso 1 1 calc R . . . . H12I H 0.3403 0.7841 0.7162 0.111 Uiso 1 1 calc R . . . . C125 C 0.444(3) 0.7278(12) 0.780(2) 0.074(5) Uani 1 1 d D U . . . H12J H 0.4924 0.7325 0.7586 0.111 Uiso 1 1 calc R . . . . H12K H 0.4417 0.7486 0.8147 0.111 Uiso 1 1 calc R . . . . H12L H 0.4557 0.7041 0.8092 0.111 Uiso 1 1 calc R . . . . C126 C 0.285(3) 0.7177(12) 0.756(2) 0.074(5) Uani 1 1 d D U . . . H12M H 0.2952 0.6927 0.7796 0.111 Uiso 1 1 calc R . . . . H12N H 0.2916 0.7369 0.7956 0.111 Uiso 1 1 calc R . . . . H12O H 0.2238 0.7189 0.7190 0.111 Uiso 1 1 calc R . . . . C127 C 1.151(3) 0.5821(11) 0.491(3) 0.097(6) Uani 1 1 d D U . . . H12P H 1.1213 0.5902 0.4378 0.145 Uiso 1 1 calc R . . . . H12Q H 1.2136 0.5904 0.5076 0.145 Uiso 1 1 calc R . . . . H12R H 1.1488 0.5546 0.4943 0.145 Uiso 1 1 calc R . . . . C128 C 1.107(2) 0.5985(9) 0.540(2) 0.097(6) Uani 1 1 d D U . . . C129 C 1.112(3) 0.6381(10) 0.533(3) 0.097(6) Uani 1 1 d D U . . . H12S H 1.0798 0.6459 0.4804 0.145 Uiso 1 1 calc R . . . . H12T H 1.0861 0.6503 0.5687 0.145 Uiso 1 1 calc R . . . . H12U H 1.1753 0.6457 0.5463 0.145 Uiso 1 1 calc R . . . . C130 C 1.153(3) 0.5859(12) 0.614(3) 0.097(6) Uani 1 1 d D U . . . H13A H 1.1477 0.5584 0.6165 0.145 Uiso 1 1 calc R . . . . H13B H 1.2161 0.5929 0.6281 0.145 Uiso 1 1 calc R . . . . H13C H 1.1269 0.5976 0.6505 0.145 Uiso 1 1 calc R . . . . C131 C 1.014(2) 0.5889(12) 0.512(3) 0.097(6) Uani 1 1 d D U . . . C132 C 0.973(3) 0.3439(10) 0.341(3) 0.082(5) Uani 1 1 d D U . . . C133 C 1.054(2) 0.3197(8) 0.3499(19) 0.082(5) Uani 1 1 d D U . . . C134 C 1.079(3) 0.3026(10) 0.429(2) 0.082(5) Uani 1 1 d D U . . . H13D H 1.0309 0.2857 0.4318 0.123 Uiso 1 1 calc R . . . . H13E H 1.1344 0.2884 0.4395 0.123 Uiso 1 1 calc R . . . . H13F H 1.0868 0.3227 0.4674 0.123 Uiso 1 1 calc R . . . . C135 C 1.127(2) 0.3456(10) 0.346(3) 0.082(5) Uani 1 1 d D U . . . H13G H 1.1421 0.3631 0.3897 0.123 Uiso 1 1 calc R . . . . H13H H 1.1802 0.3307 0.3481 0.123 Uiso 1 1 calc R . . . . H13I H 1.1073 0.3599 0.2978 0.123 Uiso 1 1 calc R . . . . C136 C 1.026(3) 0.2917(10) 0.285(3) 0.082(5) Uani 1 1 d D U . . . H13J H 0.9783 0.2757 0.2912 0.123 Uiso 1 1 calc R . . . . H13K H 1.0046 0.3051 0.2361 0.123 Uiso 1 1 calc R . . . . H13L H 1.0775 0.2760 0.2863 0.123 Uiso 1 1 calc R . . . . C137 C 0.582(3) 0.5455(12) -0.108(2) 0.059(5) Uani 1 1 d D U . . . C138 C 0.592(2) 0.5487(9) -0.189(2) 0.087(9) Uani 1 1 d D U . . . C139 C 0.590(3) 0.5891(11) -0.223(2) 0.084(12) Uani 1 1 d D U . . . H13M H 0.6319 0.6053 -0.1847 0.126 Uiso 1 1 calc R . . . . H13N H 0.6071 0.5880 -0.2696 0.126 Uiso 1 1 calc R . . . . H13O H 0.5295 0.5994 -0.2356 0.126 Uiso 1 1 calc R . . . . C140 C 0.523(3) 0.5285(13) -0.258(2) 0.110(13) Uani 1 1 d D U . . . H14A H 0.4624 0.5356 -0.2591 0.165 Uiso 1 1 calc R . . . . H14B H 0.5319 0.5361 -0.3060 0.165 Uiso 1 1 calc R . . . . H14C H 0.5303 0.5012 -0.2512 0.165 Uiso 1 1 calc R . . . . C141 C 0.680(3) 0.5333(11) -0.199(3) 0.076(11) Uani 1 1 d D U . . . H14D H 0.7315 0.5438 -0.1591 0.114 Uiso 1 1 calc R . . . . H14E H 0.6809 0.5058 -0.1953 0.114 Uiso 1 1 calc R . . . . H14F H 0.6825 0.5407 -0.2500 0.114 Uiso 1 1 calc R . . . . C142 C 0.960(3) 0.5895(12) 0.066(3) 0.088(6) Uani 1 1 d D U . . . H14G H 0.9810 0.5661 0.0945 0.132 Uiso 1 1 calc R . . . . H14H H 0.9889 0.5928 0.0268 0.132 Uiso 1 1 calc R . . . . H14I H 0.9742 0.6109 0.1017 0.132 Uiso 1 1 calc R . . . . C143 C 0.860(3) 0.5873(8) 0.028(2) 0.088(6) Uani 1 1 d D U . . . C144 C 0.818(3) 0.6216(11) -0.018(3) 0.088(6) Uani 1 1 d D U . . . H14J H 0.7538 0.6178 -0.0412 0.132 Uiso 1 1 calc R . . . . H14K H 0.8297 0.6437 0.0154 0.132 Uiso 1 1 calc R . . . . H14L H 0.8444 0.6257 -0.0595 0.132 Uiso 1 1 calc R . . . . C145 C 0.803(3) 0.5787(11) 0.078(2) 0.088(6) Uani 1 1 d D U . . . C146 C 0.835(3) 0.5554(11) -0.031(2) 0.088(6) Uani 1 1 d D U . . . H14M H 0.8601 0.5317 -0.0056 0.132 Uiso 1 1 calc R . . . . H14N H 0.7702 0.5534 -0.0523 0.132 Uiso 1 1 calc R . . . . H14O H 0.8599 0.5606 -0.0725 0.132 Uiso 1 1 calc R . . . . C147 C 1.047(3) 0.5465(15) 0.753(3) 0.124(14) Uani 1 1 d D U . . . H14P H 1.1028 0.5560 0.7899 0.186 Uiso 1 1 calc R . . . . H14Q H 1.0383 0.5202 0.7651 0.186 Uiso 1 1 calc R . . . . H14R H 1.0509 0.5480 0.7008 0.186 Uiso 1 1 calc R . . . . C148 C 0.973(3) 0.5688(12) 0.758(2) 0.107(10) Uani 1 1 d D U . . . C149 C 0.995(4) 0.6068(12) 0.741(3) 0.114(14) Uani 1 1 d D U . . . H14S H 1.0512 0.6146 0.7787 0.171 Uiso 1 1 calc R . . . . H14T H 1.0003 0.6076 0.6891 0.171 Uiso 1 1 calc R . . . . H14U H 0.9469 0.6239 0.7429 0.171 Uiso 1 1 calc R . . . . C150 C 0.971(3) 0.5689(15) 0.835(3) 0.115(14) Uani 1 1 d D U . . . H15A H 1.0284 0.5781 0.8695 0.173 Uiso 1 1 calc R . . . . H15B H 0.9228 0.5853 0.8380 0.173 Uiso 1 1 calc R . . . . H15C H 0.9609 0.5432 0.8494 0.173 Uiso 1 1 calc R . . . . C151 C 0.892(3) 0.5555(11) 0.704(3) 0.079(6) Uani 1 1 d D U . . . C152 C 0.951(4) 0.2782(13) 0.702(4) 0.143(16) Uani 1 1 d D U . . . H15D H 0.9898 0.2606 0.7391 0.215 Uiso 1 1 calc R . . . . H15E H 0.9498 0.2711 0.6497 0.215 Uiso 1 1 calc R . . . . H15F H 0.9747 0.3038 0.7131 0.215 Uiso 1 1 calc R . . . . C153 C 0.860(4) 0.2766(9) 0.706(2) 0.137(12) Uani 1 1 d D U . . . C154 C 0.854(4) 0.2861(16) 0.782(3) 0.158(17) Uani 1 1 d D U . . . H15G H 0.8964 0.2708 0.8220 0.237 Uiso 1 1 calc R . . . . H15H H 0.8675 0.3129 0.7931 0.237 Uiso 1 1 calc R . . . . H15I H 0.7930 0.2810 0.7828 0.237 Uiso 1 1 calc R . . . . C155 C 0.816(4) 0.2394(13) 0.692(3) 0.154(17) Uani 1 1 d D U . . . H15J H 0.8558 0.2204 0.7246 0.231 Uiso 1 1 calc R . . . . H15K H 0.7601 0.2404 0.7036 0.231 Uiso 1 1 calc R . . . . H15L H 0.8038 0.2325 0.6376 0.231 Uiso 1 1 calc R . . . . C156 C 0.793(3) 0.3013(11) 0.654(3) 0.102(8) Uani 1 1 d D U . . . C157 C 0.383(4) 0.4579(14) 0.887(3) 0.110(14) Uani 1 1 d D U . . . H15M H 0.3973 0.4842 0.8790 0.166 Uiso 1 1 calc R . . . . H15N H 0.3726 0.4555 0.9363 0.166 Uiso 1 1 calc R . . . . H15O H 0.4327 0.4416 0.8861 0.166 Uiso 1 1 calc R . . . . C158 C 0.294(3) 0.4455(10) 0.818(2) 0.096(11) Uani 1 1 d D U . . . C159 C 0.314(3) 0.4499(12) 0.737(2) 0.058(10) Uani 1 1 d D U . . . C160 C 0.214(3) 0.4744(14) 0.816(3) 0.114(15) Uani 1 1 d D U . . . H16A H 0.2331 0.5002 0.8105 0.172 Uiso 1 1 calc R . . . . H16B H 0.1609 0.4683 0.7722 0.172 Uiso 1 1 calc R . . . . H16C H 0.1997 0.4723 0.8640 0.172 Uiso 1 1 calc R . . . . C161 C 0.266(3) 0.4026(12) 0.827(3) 0.095(13) Uani 1 1 d D U . . . H16D H 0.3155 0.3858 0.8282 0.143 Uiso 1 1 calc R . . . . H16E H 0.2520 0.3999 0.8751 0.143 Uiso 1 1 calc R . . . . H16F H 0.2132 0.3959 0.7834 0.143 Uiso 1 1 calc R . . . . C162 C 0.068(3) 0.4130(10) 0.545(3) 0.065(6) Uani 1 1 d D U . . . C163 C 0.000(2) 0.3966(8) 0.582(2) 0.087(10) Uani 1 1 d D U . . . C164 C -0.077(3) 0.4239(12) 0.579(3) 0.097(13) Uani 1 1 d D U . . . H16G H -0.0525 0.4476 0.6051 0.146 Uiso 1 1 calc R . . . . H16H H -0.1122 0.4289 0.5257 0.146 Uiso 1 1 calc R . . . . H16I H -0.1155 0.4124 0.6058 0.146 Uiso 1 1 calc R . . . . C165 C 0.046(3) 0.3861(14) 0.667(3) 0.116(14) Uani 1 1 d D U . . . H16J H 0.0755 0.4083 0.6960 0.174 Uiso 1 1 calc R . . . . H16K H 0.0007 0.3769 0.6892 0.174 Uiso 1 1 calc R . . . . H16L H 0.0901 0.3662 0.6710 0.174 Uiso 1 1 calc R . . . . C166 C -0.045(3) 0.3606(10) 0.541(3) 0.095(12) Uani 1 1 d D U . . . H16M H -0.0746 0.3661 0.4863 0.142 Uiso 1 1 calc R . . . . H16N H 0.0006 0.3410 0.5461 0.142 Uiso 1 1 calc R . . . . H16O H -0.0888 0.3517 0.5642 0.142 Uiso 1 1 calc R . . . . C167 C 0.637(3) 0.3037(12) -0.116(3) 0.101(13) Uani 1 1 d D U . . . H16P H 0.6023 0.3261 -0.1396 0.151 Uiso 1 1 calc R . . . . H16Q H 0.6915 0.3114 -0.0759 0.151 Uiso 1 1 calc R . . . . H16R H 0.6518 0.2892 -0.1557 0.151 Uiso 1 1 calc R . . . . C168 C 0.582(3) 0.2798(9) -0.0819(19) 0.085(9) Uani 1 1 d D U . . . C169 C 0.558(3) 0.3016(10) -0.022(2) 0.060(5) Uani 1 1 d D U . . . C170 C 0.626(3) 0.2449(10) -0.045(2) 0.097(13) Uani 1 1 d D U . . . H17A H 0.6824 0.2513 -0.0045 0.145 Uiso 1 1 calc R . . . . H17B H 0.5868 0.2317 -0.0212 0.145 Uiso 1 1 calc R . . . . H17C H 0.6382 0.2286 -0.0830 0.145 Uiso 1 1 calc R . . . . C171 C 0.498(3) 0.2678(12) -0.141(3) 0.102(12) Uani 1 1 d D U . . . H17D H 0.4656 0.2900 -0.1680 0.153 Uiso 1 1 calc R . . . . H17E H 0.5118 0.2512 -0.1784 0.153 Uiso 1 1 calc R . . . . H17F H 0.4604 0.2543 -0.1165 0.153 Uiso 1 1 calc R . . . . C172 C 0.081(3) 0.7695(13) -0.063(3) 0.109(7) Uani 1 1 d D U . . . H17G H 0.1201 0.7623 -0.0923 0.164 Uiso 1 1 calc R . . . . H17H H 0.0394 0.7892 -0.0906 0.164 Uiso 1 1 calc R . . . . H17I H 0.1169 0.7790 -0.0122 0.164 Uiso 1 1 calc R . . . . C173 C 0.025(2) 0.7332(11) -0.052(2) 0.109(7) Uani 1 1 d D U . . . C174 C 0.087(3) 0.7003(12) -0.004(3) 0.109(7) Uani 1 1 d D U . . . C175 C -0.033(3) 0.7148(13) -0.131(3) 0.109(7) Uani 1 1 d D U . . . H17J H 0.0044 0.7102 -0.1635 0.164 Uiso 1 1 calc R . . . . H17K H -0.0583 0.6908 -0.1212 0.164 Uiso 1 1 calc R . . . . H17L H -0.0821 0.7319 -0.1581 0.164 Uiso 1 1 calc R . . . . C176 C -0.043(3) 0.7392(14) -0.005(3) 0.109(7) Uani 1 1 d D U . . . H17M H -0.0113 0.7506 0.0448 0.164 Uiso 1 1 calc R . . . . H17N H -0.0914 0.7559 -0.0344 0.164 Uiso 1 1 calc R . . . . H17O H -0.0677 0.7148 0.0025 0.164 Uiso 1 1 calc R . . . . C177 C 0.611(4) 0.7055(16) 0.372(2) 0.094(6) Uani 1 1 d . . . . . H177 H 0.6534 0.6862 0.3758 0.113 Uiso 1 1 calc R . . . . C178 C 0.517(3) 0.5715(13) -0.096(2) 0.059(5) Uani 1 1 d D U . . . H178 H 0.4949 0.5924 -0.1292 0.071 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 Zr01 0.049(3) 0.0085(19) 0.094(4) -0.005(2) 0.040(3) 0.002(2) Zr02 0.055(3) 0.010(2) 0.099(4) -0.003(2) 0.044(3) -0.001(2) Ti9 0.062(6) 0.004(4) 0.113(8) -0.007(4) 0.059(6) -0.003(4) Ti04 0.046(5) 0.003(4) 0.110(8) -0.004(4) 0.038(5) 0.001(4) Ti05 0.065(6) 0.015(4) 0.097(7) 0.000(5) 0.047(6) 0.003(4) Ti06 0.057(6) 0.015(4) 0.087(7) 0.009(4) 0.043(5) 0.012(4) Ti07 0.048(5) 0.011(4) 0.090(7) -0.008(4) 0.033(5) -0.004(4) Ti08 0.048(5) 0.009(4) 0.091(7) -0.007(4) 0.042(5) -0.004(4) Ti0A 0.054(5) 0.006(4) 0.087(7) 0.001(4) 0.035(5) 0.007(4) O1 0.065(9) 0.065(9) 0.066(9) 0.0002(15) 0.021(3) -0.0002(15) O2 0.062(9) 0.062(9) 0.062(9) -0.0003(15) 0.021(3) 0.0002(15) O3 0.042(7) 0.042(7) 0.042(7) -0.0001(15) 0.014(3) -0.0003(15) O4 0.043(7) 0.043(7) 0.043(7) 0.0001(15) 0.014(3) 0.0000(15) O5 0.015(6) 0.015(6) 0.016(6) -0.0003(14) 0.005(2) 0.0002(14) O6 0.036(7) 0.036(7) 0.036(7) -0.0005(15) 0.012(3) 0.0004(15) O7 0.036(7) 0.036(7) 0.036(7) 0.0000(15) 0.012(3) 0.0002(15) O8 0.065(9) 0.065(9) 0.065(9) -0.0003(15) 0.021(3) 0.0001(15) O9 0.026(6) 0.026(6) 0.027(6) 0.0001(15) 0.009(2) -0.0001(15) O10 0.049(8) 0.048(8) 0.049(8) -0.0002(15) 0.016(3) 0.0000(15) O11 0.032(7) 0.031(7) 0.032(7) -0.0004(15) 0.010(3) 0.0001(15) O12 0.050(8) 0.049(8) 0.050(8) -0.0001(15) 0.016(3) -0.0001(15) O13 0.062(9) 0.062(9) 0.062(9) 0.0001(15) 0.020(3) 0.0000(15) O14 0.044(7) 0.043(7) 0.044(7) -0.0002(15) 0.014(3) 0.0002(15) O15 0.054(8) 0.054(8) 0.054(8) -0.0003(15) 0.018(3) 0.0002(15) O16 0.031(6) 0.030(6) 0.031(6) 0.0001(15) 0.010(2) -0.0001(15) C1 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) O17 0.057(8) 0.057(8) 0.057(8) -0.0001(15) 0.018(3) -0.0001(15) O18 0.051(8) 0.051(8) 0.051(8) -0.0001(15) 0.017(3) 0.0002(15) O19 0.021(6) 0.021(6) 0.021(6) 0.0000(15) 0.007(2) 0.0000(15) O20 0.039(7) 0.039(7) 0.039(7) 0.0002(15) 0.013(3) 0.0002(15) O21 0.032(7) 0.032(7) 0.032(7) -0.0002(15) 0.010(3) 0.0000(15) O22 0.050(8) 0.050(8) 0.051(8) 0.0000(15) 0.017(3) 0.0001(15) O23 0.056(9) 0.056(9) 0.057(9) 0.0002(15) 0.018(3) 0.0000(15) O24 0.044(7) 0.044(7) 0.044(7) 0.0000(15) 0.014(3) -0.0002(15) O25 0.033(7) 0.033(7) 0.033(7) -0.0004(15) 0.011(3) 0.0004(15) O26 0.026(6) 0.026(6) 0.026(6) 0.0004(15) 0.008(2) 0.0000(15) O27 0.047(8) 0.047(8) 0.047(8) 0.0001(15) 0.015(3) 0.0000(15) O28 0.035(7) 0.035(7) 0.035(7) 0.0001(15) 0.011(3) 0.0001(15) O29 0.059(8) 0.059(8) 0.059(8) -0.0001(15) 0.019(3) 0.0000(15) O30 0.021(6) 0.021(6) 0.021(6) 0.0000(15) 0.007(2) -0.0003(14) O31 0.050(8) 0.050(8) 0.050(8) 0.0002(15) 0.016(3) 0.0000(15) O32 0.068(9) 0.068(9) 0.068(9) 0.0001(15) 0.022(3) 0.0000(15) O33 0.045(8) 0.045(8) 0.046(8) -0.0001(15) 0.015(3) -0.0001(15) O34 0.062(9) 0.062(9) 0.063(9) -0.0001(15) 0.020(3) 0.0002(15) O35 0.031(6) 0.031(6) 0.031(6) -0.0001(15) 0.010(2) 0.0000(15) C2 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) O36 0.050(8) 0.049(8) 0.050(8) 0.0000(15) 0.016(3) 0.0001(15) C3 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) O37 0.029(6) 0.029(7) 0.029(7) -0.0004(15) 0.009(2) -0.0001(15) O38 0.056(8) 0.056(8) 0.056(8) 0.0001(15) 0.019(3) -0.0001(15) O39 0.048(8) 0.047(8) 0.048(8) 0.0001(15) 0.016(3) -0.0001(15) O40 0.022(6) 0.021(6) 0.022(6) -0.0003(15) 0.007(2) 0.0004(14) C4 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C5 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) O41 0.042(7) 0.041(7) 0.042(7) -0.0003(15) 0.014(3) 0.0001(15) O42 0.045(7) 0.045(7) 0.045(7) 0.0001(15) 0.015(3) -0.0001(15) C6 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C7 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C8 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) O43 0.037(7) 0.037(7) 0.037(7) 0.0002(15) 0.012(3) -0.0002(15) C9 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C10 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C11 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C12 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C13 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C14 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C15 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C16 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C17 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C18 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C19 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C20 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) O44 0.050(8) 0.049(8) 0.050(8) -0.0003(15) 0.016(3) 0.0002(15) C21 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C22 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C23 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C24 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C25 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C26 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C27 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C28 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C29 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C30 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C31 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C32 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C33 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C34 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C36 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C37 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C38 0.038(10) 0.038(10) 0.038(10) -0.0001(15) 0.012(4) 0.0001(15) C39 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C40 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C41 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C42 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C43 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C44 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C45 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C46 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C47 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C48 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C49 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C50 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C51 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C52 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C53 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C54 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C55 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C56 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C57 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C58 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C59 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C60 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C61 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C62 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C63 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C64 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C65 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C66 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C67 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C68 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C69 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C70 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C71 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C72 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C73 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C74 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C75 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C76 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C77 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C78 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C79 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C80 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C81 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C82 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C84 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C85 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C86 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C87 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C88 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C89 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C90 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C91 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C92 0.035(11) 0.046(12) 0.098(18) -0.018(11) 0.035(13) -0.005(9) C93 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) Ti1 0.038(5) 0.009(4) 0.100(7) -0.007(4) 0.040(5) 0.001(3) C94 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C95 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C96 0.050(5) 0.050(5) 0.050(5) 0.0000(6) 0.0163(17) 0.0001(6) C97 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C98 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C99 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C100 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C101 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C102 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C103 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C104 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C105 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C106 0.116(16) 0.050(11) 0.38(3) -0.029(16) 0.146(18) 0.016(11) C107 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C108 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C109 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C110 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C111 0.053(9) 0.022(7) 0.146(14) -0.015(9) 0.056(10) -0.014(7) C112 0.12(3) 0.09(3) 0.12(3) -0.02(2) 0.02(2) -0.02(2) C113 0.12(3) 0.09(3) 0.11(3) -0.02(2) 0.02(2) -0.02(2) C114 0.12(3) 0.10(3) 0.10(3) -0.03(3) 0.01(3) -0.02(2) C115 0.14(4) 0.10(3) 0.11(3) -0.02(2) 0.02(3) -0.02(2) C116 0.16(4) 0.12(3) 0.12(3) -0.03(2) 0.04(3) -0.03(3) C117 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C118 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C119 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C120 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C121 0.067(5) 0.066(5) 0.068(5) 0.0005(14) 0.022(2) -0.0004(14) C122 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C123 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C124 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C125 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C126 0.074(5) 0.073(5) 0.074(5) -0.0002(7) 0.0238(16) 0.0001(7) C127 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C128 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C129 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C130 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C131 0.064(11) 0.046(10) 0.200(19) -0.045(12) 0.069(13) -0.010(9) C132 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C133 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C134 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C135 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C136 0.061(10) 0.024(7) 0.183(16) -0.026(9) 0.071(11) 0.004(7) C137 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) C138 0.12(2) 0.077(18) 0.073(12) 0.000(11) 0.042(12) -0.005(16) C139 0.10(3) 0.074(18) 0.08(2) 0.004(13) 0.037(19) -0.002(17) C140 0.14(2) 0.11(3) 0.085(17) -0.008(16) 0.042(15) -0.02(2) C141 0.12(2) 0.04(2) 0.08(2) 0.008(17) 0.051(16) -0.011(17) C142 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C143 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C144 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C145 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C146 0.099(13) 0.061(10) 0.121(15) 0.050(10) 0.059(12) 0.020(10) C147 0.102(17) 0.11(3) 0.15(3) -0.02(2) 0.019(17) 0.001(16) C148 0.094(13) 0.096(19) 0.113(16) -0.012(15) 0.011(12) -0.004(12) C149 0.12(3) 0.091(19) 0.13(3) -0.019(17) 0.04(2) -0.002(15) C150 0.12(3) 0.10(3) 0.114(16) -0.016(16) 0.019(15) -0.02(2) C151 0.079(6) 0.079(6) 0.079(6) -0.0001(8) 0.026(2) 0.0001(8) C152 0.17(3) 0.04(2) 0.22(4) 0.00(3) 0.07(2) 0.035(18) C153 0.16(2) 0.058(18) 0.18(3) 0.013(18) 0.05(2) 0.035(17) C154 0.19(4) 0.09(3) 0.18(3) 0.008(19) 0.06(2) 0.03(3) C155 0.20(3) 0.059(17) 0.20(4) 0.020(19) 0.05(3) 0.024(18) C156 0.14(2) 0.026(10) 0.15(2) -0.003(12) 0.058(18) 0.022(11) C157 0.15(2) 0.11(3) 0.078(18) 0.009(17) 0.050(15) 0.03(2) C158 0.14(2) 0.09(2) 0.079(15) 0.017(13) 0.061(13) 0.028(16) C159 0.058(10) 0.058(10) 0.058(10) -0.0001(15) 0.019(3) 0.0003(15) C160 0.16(3) 0.11(3) 0.10(3) 0.02(2) 0.08(2) 0.05(2) C161 0.12(3) 0.088(19) 0.10(3) 0.020(15) 0.07(2) 0.037(18) C162 0.058(11) 0.028(9) 0.137(17) -0.014(10) 0.071(11) -0.002(8) C163 0.067(17) 0.052(16) 0.18(2) 0.011(16) 0.098(17) 0.005(13) C164 0.08(2) 0.07(2) 0.18(3) 0.01(2) 0.10(2) 0.020(17) C165 0.09(2) 0.11(3) 0.18(2) 0.021(18) 0.097(18) 0.02(2) C166 0.07(2) 0.051(17) 0.20(3) 0.016(18) 0.09(2) 0.007(15) C167 0.17(3) 0.04(2) 0.12(3) -0.001(18) 0.09(2) 0.025(19) C168 0.16(2) 0.036(15) 0.091(18) -0.012(13) 0.076(16) 0.017(14) C169 0.107(14) 0.013(8) 0.073(13) -0.006(9) 0.047(12) 0.018(8) C170 0.16(3) 0.040(15) 0.11(3) -0.008(15) 0.07(2) 0.022(17) C171 0.17(2) 0.05(2) 0.11(2) -0.024(16) 0.064(18) 0.024(17) C172 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C173 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C174 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C175 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C176 0.085(14) 0.087(13) 0.140(18) 0.054(13) 0.014(13) 0.024(11) C177 0.094(6) 0.093(6) 0.095(6) -0.0005(15) 0.030(2) -0.0001(15) C178 0.059(5) 0.059(5) 0.059(5) 0.0000(6) 0.0193(17) 0.0000(6) _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 Zr01 Ti05 3.170(10) . ? Zr01 Ti07 3.159(9) . ? Zr01 Ti0A 3.209(9) . ? Zr01 O1 2.13(3) . ? Zr01 O3 2.23(3) . ? Zr01 O7 2.19(2) . ? Zr01 O9 2.12(2) . ? Zr01 O11 2.31(3) . ? Zr01 O15 2.21(3) . ? Zr01 O30 2.23(2) . ? Zr01 O43 2.09(3) . ? Zr01 Ti1 3.183(8) . ? Zr02 Ti9 3.192(9) . ? Zr02 Ti04 3.183(8) . ? Zr02 Ti06 3.209(9) . ? Zr02 Ti08 3.159(10) . ? Zr02 O10 2.21(3) . ? Zr02 O13 2.14(3) . ? Zr02 O16 2.25(2) . ? Zr02 O21 2.19(3) . ? Zr02 O34 2.22(3) . ? Zr02 O35 2.19(2) . ? Zr02 O37 2.15(2) . ? Zr02 O39 2.22(3) . ? Ti9 O2 2.19(3) . ? Ti9 O14 2.06(3) . ? Ti9 O16 1.95(2) . ? Ti9 O27 2.08(3) . ? Ti9 O37 1.94(2) . ? Ti9 O40 1.77(2) . ? Ti9 Ti1 3.396(10) . ? Ti04 Ti0A 3.387(10) . ? Ti04 O6 1.85(3) . ? Ti04 O8 2.13(3) . ? Ti04 O10 2.01(3) . ? Ti04 O12 2.01(3) . ? Ti04 O28 2.07(3) . ? Ti04 O35 1.91(2) . ? Ti05 Ti06 3.377(10) . ? Ti05 O3 1.93(3) . ? Ti05 O4 2.02(3) . ? Ti05 O7 1.83(3) . ? Ti05 O18 2.03(3) . ? Ti05 O31 2.05(3) . ? Ti05 O44 1.86(3) . ? Ti06 O10 1.88(3) . ? Ti06 O16 1.88(2) . ? Ti06 O22 2.01(3) . ? Ti06 O29 1.90(3) . ? Ti06 O32 2.13(3) . ? Ti06 O44 1.71(3) . ? Ti07 Ti08 3.372(10) . ? Ti07 O5 1.82(2) . ? Ti07 O15 1.94(3) . ? Ti07 O17 2.07(3) . ? Ti07 O30 1.96(2) . ? Ti07 O38 2.07(3) . ? Ti07 O41 2.08(3) . ? Ti08 O5 1.81(2) . ? Ti08 O24 2.01(3) . ? Ti08 O25 2.04(2) . ? Ti08 O26 2.00(2) . ? Ti08 O35 1.87(2) . ? Ti08 O37 1.90(2) . ? Ti0A O3 1.87(3) . ? Ti0A O6 1.75(3) . ? Ti0A O15 1.81(3) . ? Ti0A O19 2.05(2) . ? Ti0A O23 2.19(3) . ? Ti0A O33 1.98(3) . ? O1 C7 1.249(7) . ? O2 C37 1.47(5) . ? O4 C74 1.32(5) . ? O7 Ti1 1.97(3) . ? O8 C38 1.31(4) . ? O9 C30 1.21(6) . ? O11 C15 1.12(5) . ? O12 C1 1.26(5) . ? O13 C9 1.25(5) . ? O14 C5 1.29(3) . ? C1 O19 1.30(5) . ? C1 C63 1.498(7) . ? O17 C7 1.28(5) . ? O18 C15 1.25(5) . ? O20 C66 1.33(6) . ? O20 Ti1 2.10(3) . ? O21 C17 1.20(5) . ? O22 C4 1.32(5) . ? O23 C30 1.26(6) . ? O24 C33 1.28(4) . ? O25 C17 1.28(4) . ? O26 C57 1.38(5) . ? O27 C84 1.36(5) . ? O28 C9 1.32(5) . ? O29 C74 1.34(6) . ? O30 Ti1 1.84(2) . ? O31 C4 1.18(4) . ? O32 C13 1.26(5) . ? O33 C38 1.32(4) . ? O34 C84 1.16(5) . ? C2 C31 1.45(5) . ? C2 C37 1.27(5) . ? C2 C67 1.25(6) . ? O36 C37 1.29(5) . ? O36 Ti1 2.10(3) . ? C3 C63 1.397(7) . ? C3 C95 1.400(7) . ? O38 C57 1.42(5) . ? O39 C13 1.24(6) . ? O40 Ti1 1.87(2) . ? C4 C19 1.496(7) . ? C5 O42 1.30(3) . ? C5 C25 1.36(6) . ? O41 C33 1.36(5) . ? O42 Ti1 2.02(3) . ? C6 C7 1.60(7) . ? C6 C46 1.45(8) . ? C6 C81 1.34(8) . ? C8 C14 1.40(5) . ? C8 C169 1.25(5) . ? O43 C66 1.25(6) . ? C9 C68 1.34(5) . ? C10 C15 1.52(7) . ? C10 C54 1.37(6) . ? C10 C76 1.49(6) . ? C11 C16 1.46(5) . ? C11 C25 1.43(5) . ? C12 C52 1.36(3) . ? C12 C151 1.41(3) . ? C13 C49 1.48(7) . ? C14 C28 1.53(5) . ? C16 C107 1.47(5) . ? C17 C28 1.56(6) . ? C18 C19 1.395(7) . ? C18 C24 1.26(5) . ? C19 C69 1.35(4) . ? C20 C48 1.51(5) . ? C20 C132 1.43(5) . ? C21 C87 1.49(7) . ? C21 C97 1.25(6) . ? C22 C31 1.37(5) . ? C22 C162 1.44(6) . ? C23 C38 1.38(6) . ? C23 C62 1.44(7) . ? C23 C77 1.42(6) . ? C24 C159 1.37(5) . ? C25 C36 1.37(5) . ? C26 C28 1.26(6) . ? C26 C94 1.51(5) . ? C27 C58 1.33(5) . ? C27 C61 1.34(5) . ? C29 C40 1.41(7) . ? C29 C64 1.22(6) . ? C30 C47 1.70(8) . ? C32 C63 1.397(7) . ? C32 C82 1.25(6) . ? C33 C61 1.26(5) . ? C34 C67 1.58(6) . ? C34 C162 1.34(5) . ? C36 C43 1.33(5) . ? C39 C41 1.37(3) . ? C39 C44 1.39(3) . ? C40 C66 1.50(7) . ? C40 C88 1.401(7) . ? C41 C151 1.37(3) . ? C42 C49 1.399(7) . ? C42 C51 1.53(7) . ? C43 C107 1.401(7) . ? C44 C52 1.37(3) . ? C44 C74 1.53(6) . ? C45 C54 1.33(6) . ? C45 C122 1.57(6) . ? C46 C91 1.37(7) . ? C47 C87 1.33(7) . ? C47 C177 1.11(7) . ? C48 C68 1.43(6) . ? C49 C90 1.32(6) . ? C50 C55 1.49(6) . ? C50 C65 1.41(6) . ? C51 C156 1.400(7) . ? C53 C76 1.40(6) . ? C53 C122 1.19(6) . ? C55 C117 1.40(5) . ? C56 C71 1.34(5) . ? C56 C132 1.36(5) . ? C57 C75 1.495(7) . ? C58 C112 1.45(6) . ? C59 C75 1.395(7) . ? C59 C178 1.402(7) . ? C60 C75 1.10(4) . ? C60 C79 1.29(5) . ? C61 C72 1.47(6) . ? C62 C70 1.36(6) . ? C64 C102 1.30(7) . ? C65 C73 1.32(6) . ? C65 C84 1.500(7) . ? C68 C71 1.49(5) . ? C69 C96 1.53(5) . ? C70 C131 1.31(6) . ? C72 C92 1.32(5) . ? C73 C80 1.45(6) . ? C77 C86 1.49(6) . ? C78 C90 1.43(6) . ? C78 C156 1.399(7) . ? C79 C137 1.43(6) . ? C80 C117 1.40(5) . ? C81 C93 1.400(7) . ? C82 C145 1.31(6) . ? C85 C88 1.53(7) . ? C85 C102 1.40(7) . ? C86 C131 1.51(6) . ? C89 C97 1.400(7) . ? C89 C177 1.65(7) . ? C91 C174 1.23(7) . ? C92 C112 1.45(6) . ? C93 C174 1.42(7) . ? C94 C169 1.39(5) . ? C95 C145 1.23(6) . ? C96 C159 1.28(5) . ? C97 C98 1.54(3) . ? C98 C99 1.53(3) . ? C98 C100 1.54(3) . ? C98 C101 1.53(3) . ? C102 C103 1.69(4) . ? C103 C104 1.68(4) . ? C103 C105 1.67(4) . ? C103 C106 1.68(4) . ? C107 C108 1.70(3) . ? C108 C109 1.65(3) . ? C108 C110 1.68(3) . ? C108 C111 1.66(3) . ? C112 C113 1.64(3) . ? C113 C114 1.64(3) . ? C113 C115 1.65(3) . ? C113 C116 1.65(3) . ? C117 C118 1.49(3) . ? C118 C119 1.47(3) . ? C118 C120 1.47(3) . ? C118 C121 1.45(3) . ? C122 C123 1.57(3) . ? C123 C124 1.57(3) . ? C123 C125 1.57(3) . ? C123 C126 1.54(3) . ? C127 C128 1.42(3) . ? C128 C129 1.42(3) . ? C128 C130 1.40(3) . ? C128 C131 1.44(3) . ? C132 C133 1.51(3) . ? C133 C134 1.50(3) . ? C133 C135 1.50(3) . ? C133 C136 1.50(3) . ? C137 C138 1.56(3) . ? C137 C178 1.45(6) . ? C138 C139 1.56(3) . ? C138 C140 1.55(3) . ? C138 C141 1.55(3) . ? C142 C143 1.51(3) . ? C143 C144 1.51(3) . ? C143 C145 1.52(3) . ? C143 C146 1.52(3) . ? C147 C148 1.43(3) . ? C148 C149 1.45(3) . ? C148 C150 1.43(3) . ? C148 C151 1.43(3) . ? C152 C153 1.47(3) . ? C153 C154 1.47(3) . ? C153 C155 1.47(3) . ? C153 C156 1.47(3) . ? C157 C158 1.62(3) . ? C158 C159 1.63(3) . ? C158 C160 1.62(3) . ? C158 C161 1.61(3) . ? C162 C163 1.56(3) . ? C163 C164 1.55(3) . ? C163 C165 1.54(3) . ? C163 C166 1.54(3) . ? C167 C168 1.49(3) . ? C168 C169 1.49(3) . ? C168 C170 1.48(3) . ? C168 C171 1.48(3) . ? C172 C173 1.61(3) . ? C173 C174 1.60(3) . ? C173 C175 1.59(3) . ? C173 C176 1.59(3) . ? 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 Ti05 Zr01 Ti0A 67.5(2) . . ? Ti05 Zr01 Ti1 67.8(2) . . ? Ti07 Zr01 Ti05 102.8(2) . . ? Ti07 Zr01 Ti0A 66.5(2) . . ? Ti07 Zr01 Ti1 67.8(2) . . ? O1 Zr01 Ti05 174.7(9) . . ? O1 Zr01 Ti07 72.0(9) . . ? O1 Zr01 Ti0A 108.9(9) . . ? O1 Zr01 O3 140.9(11) . . ? O1 Zr01 O7 145.6(11) . . ? O1 Zr01 O11 114.8(11) . . ? O1 Zr01 O15 82.2(11) . . ? O1 Zr01 O30 81.4(10) . . ? O1 Zr01 Ti1 110.2(9) . . ? O3 Zr01 Ti05 37.0(7) . . ? O3 Zr01 Ti07 93.9(7) . . ? O3 Zr01 Ti0A 34.8(7) . . ? O3 Zr01 O11 79.5(9) . . ? O3 Zr01 O30 110.0(9) . . ? O3 Zr01 Ti1 96.7(7) . . ? O7 Zr01 Ti05 34.2(6) . . ? O7 Zr01 Ti07 95.9(7) . . ? O7 Zr01 Ti0A 94.4(6) . . ? O7 Zr01 O3 70.1(9) . . ? O7 Zr01 O11 79.3(9) . . ? O7 Zr01 O15 108.0(10) . . ? O7 Zr01 O30 70.7(9) . . ? O7 Zr01 Ti1 37.5(7) . . ? O9 Zr01 Ti05 110.1(7) . . ? O9 Zr01 Ti07 110.4(7) . . ? O9 Zr01 Ti0A 72.3(6) . . ? O9 Zr01 O1 71.6(10) . . ? O9 Zr01 O3 80.2(9) . . ? O9 Zr01 O7 141.5(9) . . ? O9 Zr01 O11 71.5(9) . . ? O9 Zr01 O15 80.6(10) . . ? O9 Zr01 O30 145.0(9) . . ? O9 Zr01 Ti1 176.3(7) . . ? O11 Zr01 Ti05 70.4(6) . . ? O11 Zr01 Ti07 172.9(7) . . ? O11 Zr01 Ti0A 108.4(6) . . ? O11 Zr01 Ti1 109.9(6) . . ? O15 Zr01 Ti05 93.1(7) . . ? O15 Zr01 Ti07 37.3(7) . . ? O15 Zr01 Ti0A 32.8(7) . . ? O15 Zr01 O3 66.6(10) . . ? O15 Zr01 O11 139.2(10) . . ? O15 Zr01 O30 73.9(9) . . ? O15 Zr01 Ti1 96.5(7) . . ? O30 Zr01 Ti05 95.0(6) . . ? O30 Zr01 Ti07 37.9(6) . . ? O30 Zr01 Ti0A 96.7(6) . . ? O30 Zr01 O11 142.1(8) . . ? O30 Zr01 Ti1 34.5(6) . . ? O43 Zr01 Ti05 110.6(7) . . ? O43 Zr01 Ti07 111.0(7) . . ? O43 Zr01 Ti0A 176.0(7) . . ? O43 Zr01 O1 72.8(11) . . ? O43 Zr01 O3 144.7(10) . . ? O43 Zr01 O7 82.6(9) . . ? O43 Zr01 O9 111.7(9) . . ? O43 Zr01 O11 73.7(9) . . ? O43 Zr01 O15 146.0(10) . . ? O43 Zr01 O30 79.8(9) . . ? O43 Zr01 Ti1 72.0(7) . . ? Ti1 Zr01 Ti0A 104.0(2) . . ? Ti9 Zr02 Ti06 67.2(2) . . ? Ti04 Zr02 Ti9 103.2(2) . . ? Ti04 Zr02 Ti06 67.3(2) . . ? Ti08 Zr02 Ti9 67.5(2) . . ? Ti08 Zr02 Ti04 66.6(2) . . ? Ti08 Zr02 Ti06 102.6(2) . . ? O10 Zr02 Ti9 96.4(7) . . ? O10 Zr02 Ti04 38.7(7) . . ? O10 Zr02 Ti06 34.9(7) . . ? O10 Zr02 Ti08 98.0(7) . . ? O10 Zr02 O16 69.7(9) . . ? O10 Zr02 O34 138.7(11) . . ? O10 Zr02 O39 75.2(10) . . ? O13 Zr02 Ti9 170.5(8) . . ? O13 Zr02 Ti04 67.3(8) . . ? O13 Zr02 Ti06 107.4(8) . . ? O13 Zr02 Ti08 107.3(8) . . ? O13 Zr02 O10 76.1(11) . . ? O13 Zr02 O16 140.4(10) . . ? O13 Zr02 O21 76.4(10) . . ? O13 Zr02 O34 117.3(11) . . ? O13 Zr02 O35 76.5(10) . . ? O13 Zr02 O37 141.4(10) . . ? O13 Zr02 O39 74.6(11) . . ? O16 Zr02 Ti9 37.1(6) . . ? O16 Zr02 Ti04 95.7(6) . . ? O16 Zr02 Ti06 35.1(6) . . ? O16 Zr02 Ti08 96.8(6) . . ? O21 Zr02 Ti9 108.2(7) . . ? O21 Zr02 Ti04 109.7(7) . . ? O21 Zr02 Ti06 173.0(7) . . ? O21 Zr02 Ti08 70.5(7) . . ? O21 Zr02 O10 145.1(9) . . ? O21 Zr02 O16 142.6(9) . . ? O21 Zr02 O34 74.1(10) . . ? O21 Zr02 O35 78.9(9) . . ? O21 Zr02 O39 116.9(10) . . ? O34 Zr02 Ti9 72.2(8) . . ? O34 Zr02 Ti04 174.9(8) . . ? O34 Zr02 Ti06 108.5(8) . . ? O34 Zr02 Ti08 112.5(8) . . ? O34 Zr02 O16 79.4(10) . . ? O34 Zr02 O39 72.0(11) . . ? O35 Zr02 Ti9 96.0(6) . . ? O35 Zr02 Ti04 36.1(6) . . ? O35 Zr02 Ti06 96.0(6) . . ? O35 Zr02 Ti08 35.4(6) . . ? O35 Zr02 O10 74.1(9) . . ? O35 Zr02 O16 111.4(8) . . ? O35 Zr02 O34 144.9(10) . . ? O35 Zr02 O39 141.8(9) . . ? O37 Zr02 Ti9 36.5(6) . . ? O37 Zr02 Ti04 95.8(6) . . ? O37 Zr02 Ti06 96.3(6) . . ? O37 Zr02 Ti08 36.1(6) . . ? O37 Zr02 O10 113.0(9) . . ? O37 Zr02 O16 72.8(9) . . ? O37 Zr02 O21 77.5(9) . . ? O37 Zr02 O34 81.5(10) . . ? O37 Zr02 O35 70.9(8) . . ? O37 Zr02 O39 143.5(9) . . ? O39 Zr02 Ti9 109.5(7) . . ? O39 Zr02 Ti04 108.4(8) . . ? O39 Zr02 Ti06 70.0(8) . . ? O39 Zr02 Ti08 172.5(8) . . ? O39 Zr02 O16 77.9(9) . . ? Zr02 Ti9 Ti1 129.1(3) . . ? O2 Ti9 Zr02 127.6(9) . . ? O2 Ti9 Ti1 77.0(8) . . ? O14 Ti9 Zr02 136.1(8) . . ? O14 Ti9 O2 90.5(11) . . ? O14 Ti9 O27 81.8(11) . . ? O14 Ti9 Ti1 74.5(8) . . ? O16 Ti9 Zr02 44.2(7) . . ? O16 Ti9 O2 85.7(11) . . ? O16 Ti9 O14 170.8(11) . . ? O16 Ti9 O27 89.4(10) . . ? O16 Ti9 Ti1 112.7(7) . . ? O27 Ti9 Zr02 81.8(8) . . ? O27 Ti9 O2 83.7(11) . . ? O27 Ti9 Ti1 149.1(8) . . ? O37 Ti9 Zr02 41.3(7) . . ? O37 Ti9 O2 168.0(11) . . ? O37 Ti9 O14 98.1(11) . . ? O37 Ti9 O16 84.5(10) . . ? O37 Ti9 O27 89.3(10) . . ? O37 Ti9 Ti1 113.2(7) . . ? O40 Ti9 Zr02 107.7(8) . . ? O40 Ti9 O2 91.2(11) . . ? O40 Ti9 O14 90.2(11) . . ? O40 Ti9 O16 98.3(11) . . ? O40 Ti9 O27 170.5(11) . . ? O40 Ti9 O37 97.0(10) . . ? O40 Ti9 Ti1 21.4(7) . . ? Zr02 Ti04 Ti0A 128.4(3) . . ? O6 Ti04 Zr02 109.4(8) . . ? O6 Ti04 Ti0A 19.1(8) . . ? O6 Ti04 O8 88.3(12) . . ? O6 Ti04 O10 99.8(11) . . ? O6 Ti04 O12 86.4(11) . . ? O6 Ti04 O28 168.3(11) . . ? O6 Ti04 O35 99.0(11) . . ? O8 Ti04 Zr02 134.0(9) . . ? O8 Ti04 Ti0A 75.2(9) . . ? O10 Ti04 Zr02 43.4(8) . . ? O10 Ti04 Ti0A 113.7(8) . . ? O10 Ti04 O8 92.9(12) . . ? O10 Ti04 O28 89.5(10) . . ? O12 Ti04 Zr02 135.4(9) . . ? O12 Ti04 Ti0A 72.0(8) . . ? O12 Ti04 O8 86.2(12) . . ? O12 Ti04 O10 173.8(11) . . ? O12 Ti04 O28 84.3(11) . . ? O28 Ti04 Zr02 82.3(7) . . ? O28 Ti04 Ti0A 149.2(7) . . ? O28 Ti04 O8 84.1(11) . . ? O35 Ti04 Zr02 42.5(7) . . ? O35 Ti04 Ti0A 112.0(8) . . ? O35 Ti04 O8 172.7(12) . . ? O35 Ti04 O10 85.1(11) . . ? O35 Ti04 O12 95.0(11) . . ? O35 Ti04 O28 88.8(10) . . ? Zr01 Ti05 Ti06 129.4(3) . . ? O3 Ti05 Zr01 44.0(8) . . ? O3 Ti05 Ti06 111.4(8) . . ? O3 Ti05 O4 92.4(11) . . ? O3 Ti05 O18 92.3(11) . . ? O3 Ti05 O31 174.6(12) . . ? O4 Ti05 Zr01 133.4(8) . . ? O4 Ti05 Ti06 73.7(8) . . ? O4 Ti05 O18 85.5(11) . . ? O4 Ti05 O31 86.2(11) . . ? O7 Ti05 Zr01 42.1(8) . . ? O7 Ti05 Ti06 113.0(8) . . ? O7 Ti05 O3 84.6(11) . . ? O7 Ti05 O4 173.3(11) . . ? O7 Ti05 O18 88.6(11) . . ? O7 Ti05 O31 96.2(11) . . ? O7 Ti05 O44 99.6(12) . . ? O18 Ti05 Zr01 81.9(8) . . ? O18 Ti05 Ti06 148.7(9) . . ? O18 Ti05 O31 82.4(12) . . ? O31 Ti05 Zr01 135.4(8) . . ? O31 Ti05 Ti06 73.3(8) . . ? O44 Ti05 Zr01 111.1(9) . . ? O44 Ti05 Ti06 18.3(9) . . ? O44 Ti05 O3 98.6(12) . . ? O44 Ti05 O4 86.8(12) . . ? O44 Ti05 O18 166.9(13) . . ? O44 Ti05 O31 86.5(12) . . ? Zr02 Ti06 Ti05 127.4(3) . . ? O10 Ti06 Zr02 42.2(9) . . ? O10 Ti06 Ti05 114.9(9) . . ? O10 Ti06 O16 85.2(11) . . ? O10 Ti06 O22 169.3(12) . . ? O10 Ti06 O29 90.8(12) . . ? O10 Ti06 O32 86.1(12) . . ? O16 Ti06 Zr02 43.5(7) . . ? O16 Ti06 Ti05 112.0(8) . . ? O16 Ti06 O22 93.5(11) . . ? O16 Ti06 O29 173.1(12) . . ? O16 Ti06 O32 89.5(11) . . ? O22 Ti06 Zr02 134.3(8) . . ? O22 Ti06 Ti05 75.5(8) . . ? O22 Ti06 O32 83.3(12) . . ? O29 Ti06 Zr02 131.7(9) . . ? O29 Ti06 Ti05 74.8(9) . . ? O29 Ti06 O22 89.4(12) . . ? O29 Ti06 O32 84.6(13) . . ? O32 Ti06 Zr02 82.3(9) . . ? O32 Ti06 Ti05 150.3(9) . . ? O44 Ti06 Zr02 107.4(10) . . ? O44 Ti06 Ti05 20.0(9) . . ? O44 Ti06 O10 100.9(12) . . ? O44 Ti06 O16 97.7(12) . . ? O44 Ti06 O22 89.8(12) . . ? O44 Ti06 O29 88.5(13) . . ? O44 Ti06 O32 170.3(13) . . ? Zr01 Ti07 Ti08 128.3(3) . . ? O5 Ti07 Zr01 106.6(7) . . ? O5 Ti07 Ti08 21.8(7) . . ? O5 Ti07 O15 93.1(11) . . ? O5 Ti07 O17 169.2(11) . . ? O5 Ti07 O30 97.0(9) . . ? O5 Ti07 O38 90.0(11) . . ? O5 Ti07 O41 89.0(10) . . ? O15 Ti07 Zr01 43.6(8) . . ? O15 Ti07 Ti08 109.9(9) . . ? O15 Ti07 O17 96.6(12) . . ? O15 Ti07 O30 86.3(11) . . ? O15 Ti07 O38 97.7(12) . . ? O15 Ti07 O41 176.5(12) . . ? O17 Ti07 Zr01 83.8(8) . . ? O17 Ti07 Ti08 147.6(9) . . ? O17 Ti07 O41 81.6(11) . . ? O30 Ti07 Zr01 44.4(6) . . ? O30 Ti07 Ti08 111.0(7) . . ? O30 Ti07 O17 88.3(10) . . ? O30 Ti07 O38 171.7(11) . . ? O30 Ti07 O41 90.6(10) . . ? O38 Ti07 Zr01 137.2(8) . . ? O38 Ti07 Ti08 74.5(8) . . ? O38 Ti07 O17 84.1(12) . . ? O38 Ti07 O41 85.1(11) . . ? O41 Ti07 Zr01 133.0(8) . . ? O41 Ti07 Ti08 72.8(8) . . ? Zr02 Ti08 Ti07 129.5(3) . . ? O5 Ti08 Zr02 107.8(7) . . ? O5 Ti08 Ti07 21.8(7) . . ? O5 Ti08 O24 89.1(10) . . ? O5 Ti08 O25 168.6(11) . . ? O5 Ti08 O26 87.5(9) . . ? O5 Ti08 O35 97.4(10) . . ? O5 Ti08 O37 99.4(10) . . ? O24 Ti08 Zr02 131.4(8) . . ? O24 Ti08 Ti07 73.2(8) . . ? O24 Ti08 O25 82.4(10) . . ? O25 Ti08 Zr02 83.6(7) . . ? O25 Ti08 Ti07 146.7(8) . . ? O26 Ti08 Zr02 133.6(7) . . ? O26 Ti08 Ti07 73.5(7) . . ? O26 Ti08 O24 91.0(10) . . ? O26 Ti08 O25 85.0(10) . . ? O35 Ti08 Zr02 42.8(7) . . ? O35 Ti08 Ti07 114.1(8) . . ? O35 Ti08 O24 172.5(11) . . ? O35 Ti08 O25 91.6(10) . . ? O35 Ti08 O26 92.9(10) . . ? O35 Ti08 O37 83.9(10) . . ? O37 Ti08 Zr02 41.8(7) . . ? O37 Ti08 Ti07 113.8(7) . . ? O37 Ti08 O24 91.5(10) . . ? O37 Ti08 O25 88.5(10) . . ? O37 Ti08 O26 172.7(10) . . ? Zr01 Ti0A Ti04 128.0(3) . . ? O3 Ti0A Zr01 42.7(8) . . ? O3 Ti0A Ti04 111.2(8) . . ? O3 Ti0A O19 174.4(11) . . ? O3 Ti0A O23 87.5(11) . . ? O3 Ti0A O33 98.8(12) . . ? O6 Ti0A Zr01 107.8(9) . . ? O6 Ti0A Ti04 20.2(8) . . ? O6 Ti0A O3 96.3(12) . . ? O6 Ti0A O15 98.1(13) . . ? O6 Ti0A O19 87.7(11) . . ? O6 Ti0A O23 168.8(13) . . ? O6 Ti0A O33 87.8(12) . . ? O15 Ti0A Zr01 41.5(9) . . ? O15 Ti0A Ti04 112.5(9) . . ? O15 Ti0A O3 82.8(13) . . ? O15 Ti0A O19 92.7(11) . . ? O15 Ti0A O23 92.9(12) . . ? O15 Ti0A O33 173.7(13) . . ? O19 Ti0A Zr01 132.2(7) . . ? O19 Ti0A Ti04 73.6(7) . . ? O19 Ti0A O23 89.4(10) . . ? O23 Ti0A Zr01 82.1(8) . . ? O23 Ti0A Ti04 149.6(9) . . ? O33 Ti0A Zr01 138.5(9) . . ? O33 Ti0A Ti04 72.7(8) . . ? O33 Ti0A O19 85.3(10) . . ? O33 Ti0A O23 81.1(12) . . ? C7 O1 Zr01 133(3) . . ? C37 O2 Ti9 129(3) . . ? Ti05 O3 Zr01 99.0(11) . . ? Ti0A O3 Zr01 102.6(12) . . ? Ti0A O3 Ti05 137.3(15) . . ? C74 O4 Ti05 132(3) . . ? Ti08 O5 Ti07 136.4(12) . . ? Ti0A O6 Ti04 140.8(15) . . ? Ti05 O7 Zr01 103.7(11) . . ? Ti05 O7 Ti1 137.7(14) . . ? Ti1 O7 Zr01 99.9(10) . . ? C38 O8 Ti04 130(3) . . ? C30 O9 Zr01 133(3) . . ? Ti04 O10 Zr02 97.9(11) . . ? Ti06 O10 Zr02 103.0(12) . . ? Ti06 O10 Ti04 131.2(15) . . ? C15 O11 Zr01 133(3) . . ? C1 O12 Ti04 140(3) . . ? C9 O13 Zr02 152(3) . . ? C5 O14 Ti9 132(3) . . ? Ti07 O15 Zr01 99.0(12) . . ? Ti0A O15 Zr01 105.7(13) . . ? Ti0A O15 Ti07 137.4(16) . . ? Ti9 O16 Zr02 98.6(10) . . ? Ti06 O16 Zr02 101.4(10) . . ? Ti06 O16 Ti9 135.1(13) . . ? O12 C1 O19 118(4) . . ? O12 C1 C63 118(4) . . ? O19 C1 C63 120(4) . . ? C7 O17 Ti07 120(3) . . ? C15 O18 Ti05 127(3) . . ? C1 O19 Ti0A 135(2) . . ? C66 O20 Ti1 119(3) . . ? C17 O21 Zr02 137(3) . . ? C4 O22 Ti06 127(2) . . ? C30 O23 Ti0A 115(3) . . ? C33 O24 Ti08 143(3) . . ? C17 O25 Ti08 124(3) . . ? C57 O26 Ti08 140(2) . . ? C84 O27 Ti9 125(2) . . ? C9 O28 Ti04 130(3) . . ? C74 O29 Ti06 136(3) . . ? Ti07 O30 Zr01 97.6(9) . . ? Ti1 O30 Zr01 102.3(10) . . ? Ti1 O30 Ti07 136.8(12) . . ? C4 O31 Ti05 132(3) . . ? C13 O32 Ti06 126(4) . . ? C38 O33 Ti0A 142(3) . . ? C84 O34 Zr02 137(3) . . ? Ti04 O35 Zr02 101.4(10) . . ? Ti08 O35 Zr02 101.8(10) . . ? Ti08 O35 Ti04 133.9(13) . . ? C37 C2 C31 117(5) . . ? C67 C2 C31 120(4) . . ? C67 C2 C37 122(4) . . ? C37 O36 Ti1 143(3) . . ? C63 C3 C95 118(4) . . ? Ti9 O37 Zr02 102.2(11) . . ? Ti08 O37 Zr02 102.0(10) . . ? Ti08 O37 Ti9 133.0(13) . . ? C57 O38 Ti07 137(2) . . ? C13 O39 Zr02 140(3) . . ? Ti9 O40 Ti1 138.3(13) . . ? O22 C4 C19 110(3) . . ? O31 C4 O22 132(3) . . ? O31 C4 C19 118(3) . . ? O14 C5 O42 121(4) . . ? O14 C5 C25 122(3) . . ? O42 C5 C25 117(3) . . ? C33 O41 Ti07 137(3) . . ? C5 O42 Ti1 135(3) . . ? C46 C6 C7 108(6) . . ? C81 C6 C7 131(6) . . ? C81 C6 C46 121(6) . . ? O1 C7 O17 130(5) . . ? O1 C7 C6 120(5) . . ? O17 C7 C6 110(4) . . ? C169 C8 C14 123(4) . . ? C66 O43 Zr01 138(3) . . ? O13 C9 O28 108(4) . . ? O13 C9 C68 125(4) . . ? O28 C9 C68 125(4) . . ? C54 C10 C15 126(5) . . ? C54 C10 C76 116(5) . . ? C76 C10 C15 118(5) . . ? C25 C11 C16 128(4) . . ? C52 C12 C151 121(5) . . ? O32 C13 C49 120(6) . . ? O39 C13 O32 120(5) . . ? O39 C13 C49 119(5) . . ? C8 C14 C28 120(4) . . ? O11 C15 O18 126(5) . . ? O11 C15 C10 118(5) . . ? O18 C15 C10 115(5) . . ? C11 C16 C107 112(3) . . ? O21 C17 O25 125(4) . . ? O21 C17 C28 125(4) . . ? O25 C17 C28 108(4) . . ? C24 C18 C19 132(4) . . ? C18 C19 C4 132(3) . . ? C69 C19 C4 120(3) . . ? C69 C19 C18 107(2) . . ? C132 C20 C48 110(4) . . ? Ti06 O44 Ti05 141.7(17) . . ? C97 C21 C87 117(6) . . ? C31 C22 C162 127(4) . . ? C38 C23 C62 127(4) . . ? C38 C23 C77 118(4) . . ? C77 C23 C62 115(5) . . ? C18 C24 C159 116(4) . . ? C5 C25 C11 125(4) . . ? C5 C25 C36 123(4) . . ? C36 C25 C11 111(4) . . ? C28 C26 C94 115(4) . . ? C58 C27 C61 131(4) . . ? C14 C28 C17 114(4) . . ? C26 C28 C14 118(4) . . ? C26 C28 C17 127(4) . . ? C64 C29 C40 112(6) . . ? O9 C30 O23 135(6) . . ? O9 C30 C47 115(5) . . ? O23 C30 C47 104(5) . . ? C22 C31 C2 115(4) . . ? C82 C32 C63 120(5) . . ? O24 C33 O41 111(4) . . ? C61 C33 O24 126(4) . . ? C61 C33 O41 123(4) . . ? C162 C34 C67 114(4) . . ? C43 C36 C25 126(4) . . ? C2 C37 O2 116(4) . . ? C2 C37 O36 127(4) . . ? O36 C37 O2 116(4) . . ? O8 C38 O33 119(4) . . ? O8 C38 C23 116(4) . . ? O33 C38 C23 122(4) . . ? C41 C39 C44 112(5) . . ? C29 C40 C66 130(5) . . ? C88 C40 C29 120(5) . . ? C88 C40 C66 110(5) . . ? C151 C41 C39 133(5) . . ? C49 C42 C51 112(4) . . ? C36 C43 C107 122(4) . . ? C39 C44 C74 117(4) . . ? C52 C44 C39 116(5) . . ? C52 C44 C74 126(4) . . ? C54 C45 C122 99(4) . . ? C91 C46 C6 109(6) . . ? C87 C47 C30 111(6) . . ? C177 C47 C30 129(7) . . ? C177 C47 C87 120(7) . . ? C68 C48 C20 129(4) . . ? C42 C49 C13 109(4) . . ? C90 C49 C13 121(5) . . ? C90 C49 C42 128(5) . . ? C65 C50 C55 114(4) . . ? C156 C51 C42 121(5) . . ? C12 C52 C44 125(5) . . ? C122 C53 C76 135(6) . . ? C45 C54 C10 140(6) . . ? C117 C55 C50 119(4) . . ? C71 C56 C132 135(4) . . ? O26 C57 O38 108(3) . . ? O26 C57 C75 122(3) . . ? O38 C57 C75 121(4) . . ? C27 C58 C112 113(4) . . ? C75 C59 C178 116(4) . . ? C75 C60 C79 129(4) . . ? C27 C61 C72 113(4) . . ? C33 C61 C27 126(4) . . ? C33 C61 C72 119(4) . . ? C70 C62 C23 126(5) . . ? C3 C63 C1 116(4) . . ? C32 C63 C1 127(4) . . ? C32 C63 C3 117(4) . . ? C29 C64 C102 135(7) . . ? C50 C65 C84 111(4) . . ? C73 C65 C50 128(4) . . ? C73 C65 C84 121(5) . . ? O20 C66 C40 108(5) . . ? O43 C66 O20 126(5) . . ? O43 C66 C40 123(5) . . ? C2 C67 C34 125(4) . . ? C9 C68 C48 127(4) . . ? C9 C68 C71 119(4) . . ? C48 C68 C71 114(4) . . ? C19 C69 C96 125(3) . . ? C131 C70 C62 126(5) . . ? C56 C71 C68 112(4) . . ? C92 C72 C61 121(4) . . ? C65 C73 C80 113(4) . . ? O4 C74 O29 121(5) . . ? O4 C74 C44 120(4) . . ? O29 C74 C44 119(4) . . ? C59 C75 C57 107(3) . . ? C60 C75 C57 116(4) . . ? C60 C75 C59 123(3) . . ? C53 C76 C10 105(5) . . ? C23 C77 C86 115(4) . . ? C156 C78 C90 127(5) . . ? C60 C79 C137 115(4) . . ? C117 C80 C73 125(5) . . ? C6 C81 C93 122(7) . . ? C32 C82 C145 122(5) . . ? O27 C84 C65 116(4) . . ? O34 C84 O27 123(4) . . ? O34 C84 C65 121(5) . . ? C102 C85 C88 105(5) . . ? C77 C86 C131 126(4) . . ? C47 C87 C21 117(6) . . ? C40 C88 C85 123(5) . . ? C97 C89 C177 96(4) . . ? C49 C90 C78 115(6) . . ? C174 C91 C46 136(7) . . ? C72 C92 C112 119(4) . . ? C81 C93 C174 117(6) . . ? Zr01 Ti1 Ti9 127.3(3) . . ? O7 Ti1 Zr01 42.6(7) . . ? O7 Ti1 Ti9 109.3(8) . . ? O7 Ti1 O20 91.8(10) . . ? O7 Ti1 O36 93.0(11) . . ? O7 Ti1 O42 177.8(11) . . ? O20 Ti1 Zr01 83.5(7) . . ? O20 Ti1 Ti9 149.1(7) . . ? O30 Ti1 Zr01 43.2(7) . . ? O30 Ti1 Ti9 111.8(7) . . ? O30 Ti1 O7 84.2(10) . . ? O30 Ti1 O20 92.1(10) . . ? O30 Ti1 O36 174.1(11) . . ? O30 Ti1 O40 96.7(10) . . ? O30 Ti1 O42 95.6(11) . . ? O36 Ti1 Zr01 132.7(8) . . ? O36 Ti1 Ti9 74.1(8) . . ? O36 Ti1 O20 82.7(10) . . ? O40 Ti1 Zr01 107.1(7) . . ? O40 Ti1 Ti9 20.3(7) . . ? O40 Ti1 O7 95.1(10) . . ? O40 Ti1 O20 169.3(10) . . ? O40 Ti1 O36 88.8(10) . . ? O40 Ti1 O42 87.1(10) . . ? O42 Ti1 Zr01 136.7(8) . . ? O42 Ti1 Ti9 72.8(8) . . ? O42 Ti1 O20 86.1(10) . . ? O42 Ti1 O36 87.0(11) . . ? C169 C94 C26 127(4) . . ? C145 C95 C3 118(5) . . ? C159 C96 C69 112(4) . . ? C21 C97 C89 135(6) . . ? C21 C97 C98 123(4) . . ? C89 C97 C98 102(4) . . ? C97 C98 C100 115(3) . . ? C99 C98 C97 116(3) . . ? C99 C98 C100 105(3) . . ? C99 C98 C101 103(3) . . ? C101 C98 C97 115(3) . . ? C101 C98 C100 101(3) . . ? C64 C102 C85 124(5) . . ? C64 C102 C103 132(4) . . ? C85 C102 C103 104(4) . . ? C104 C103 C102 110(3) . . ? C104 C103 C106 109(3) . . ? C105 C103 C102 108(3) . . ? C105 C103 C104 111(3) . . ? C105 C103 C106 111(3) . . ? C106 C103 C102 108(3) . . ? C16 C107 C108 116(2) . . ? C43 C107 C16 119(3) . . ? C43 C107 C108 124(3) . . ? C109 C108 C107 105(2) . . ? C109 C108 C110 113(2) . . ? C109 C108 C111 114(2) . . ? C110 C108 C107 104(2) . . ? C111 C108 C107 105(2) . . ? C111 C108 C110 114(2) . . ? C58 C112 C92 120(5) . . ? C58 C112 C113 116(4) . . ? C92 C112 C113 123(4) . . ? C112 C113 C114 112(3) . . ? C112 C113 C115 111(3) . . ? C112 C113 C116 109(3) . . ? C114 C113 C115 108(3) . . ? C114 C113 C116 109(3) . . ? C116 C113 C115 108(3) . . ? C55 C117 C118 117(4) . . ? C80 C117 C55 115(4) . . ? C80 C117 C118 123(4) . . ? C119 C118 C117 111(3) . . ? C120 C118 C117 109(3) . . ? C120 C118 C119 108(3) . . ? C121 C118 C117 108(3) . . ? C121 C118 C119 110(3) . . ? C121 C118 C120 111(3) . . ? C53 C122 C45 124(5) . . ? C53 C122 C123 122(4) . . ? C123 C122 C45 113(4) . . ? C124 C123 C122 110(2) . . ? C124 C123 C125 106(3) . . ? C125 C123 C122 115(3) . . ? C126 C123 C122 114(3) . . ? C126 C123 C124 108(3) . . ? C126 C123 C125 103(3) . . ? C127 C128 C131 110(3) . . ? C129 C128 C127 107(3) . . ? C129 C128 C131 107(3) . . ? C130 C128 C127 106(3) . . ? C130 C128 C129 112(3) . . ? C130 C128 C131 115(3) . . ? C70 C131 C86 110(4) . . ? C70 C131 C128 119(4) . . ? C128 C131 C86 130(4) . . ? C20 C132 C133 115(3) . . ? C56 C132 C20 117(4) . . ? C56 C132 C133 127(3) . . ? C134 C133 C132 106(2) . . ? C135 C133 C132 107(2) . . ? C135 C133 C134 109(2) . . ? C135 C133 C136 114(2) . . ? C136 C133 C132 106(2) . . ? C136 C133 C134 115(3) . . ? C79 C137 C138 123(4) . . ? C79 C137 C178 117(4) . . ? C178 C137 C138 113(3) . . ? C139 C138 C137 117(3) . . ? C140 C138 C137 119(3) . . ? C140 C138 C139 101(3) . . ? C140 C138 C141 100(3) . . ? C141 C138 C137 117(3) . . ? C141 C138 C139 101(3) . . ? C142 C143 C145 118(3) . . ? C142 C143 C146 111(3) . . ? C144 C143 C142 115(3) . . ? C144 C143 C145 105(3) . . ? C144 C143 C146 104(3) . . ? C146 C143 C145 102(2) . . ? C82 C145 C143 112(4) . . ? C95 C145 C82 126(4) . . ? C95 C145 C143 123(4) . . ? C147 C148 C149 105(3) . . ? C150 C148 C147 110(3) . . ? C150 C148 C149 107(3) . . ? C151 C148 C147 111(3) . . ? C151 C148 C149 113(3) . . ? C151 C148 C150 112(3) . . ? C12 C151 C148 124(4) . . ? C41 C151 C12 108(4) . . ? C41 C151 C148 126(4) . . ? C152 C153 C155 116(3) . . ? C154 C153 C152 115(4) . . ? C154 C153 C155 102(4) . . ? C156 C153 C152 117(3) . . ? C156 C153 C154 103(4) . . ? C156 C153 C155 103(3) . . ? C51 C156 C153 124(4) . . ? C78 C156 C51 114(4) . . ? C78 C156 C153 122(3) . . ? C157 C158 C159 108(3) . . ? C160 C158 C157 109(3) . . ? C160 C158 C159 107(3) . . ? C161 C158 C157 112(3) . . ? C161 C158 C159 109(3) . . ? C161 C158 C160 112(3) . . ? C24 C159 C158 119(3) . . ? C96 C159 C24 126(4) . . ? C96 C159 C158 114(3) . . ? C22 C162 C163 120(3) . . ? C34 C162 C22 118(4) . . ? C34 C162 C163 122(3) . . ? C164 C163 C162 114(2) . . ? C165 C163 C162 112(3) . . ? C165 C163 C164 107(3) . . ? C166 C163 C162 111(2) . . ? C166 C163 C164 106(2) . . ? C166 C163 C165 107(3) . . ? C167 C168 C169 110(3) . . ? C170 C168 C167 115(3) . . ? C170 C168 C169 107(3) . . ? C170 C168 C171 106(3) . . ? C171 C168 C167 111(3) . . ? C171 C168 C169 108(3) . . ? C8 C169 C94 115(4) . . ? C8 C169 C168 129(3) . . ? C94 C169 C168 116(3) . . ? C174 C173 C172 113(2) . . ? C175 C173 C172 113(3) . . ? C175 C173 C174 106(3) . . ? C176 C173 C172 117(3) . . ? C176 C173 C174 102(3) . . ? C176 C173 C175 105(3) . . ? C91 C174 C93 115(5) . . ? C91 C174 C173 125(5) . . ? C93 C174 C173 120(4) . . ? C47 C177 C89 134(7) . . ? C59 C178 C137 115(4) . . ? _smtbx_masks_special_details ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.069 -0.006 0.367 9.9 0.0 ? 2 0.077 -0.003 0.679 17.6 0.0 ? 3 -0.537 0.224 0.047 793.5 43.9 '1 acetonitrile' 4 -0.077 0.497 0.321 17.6 0.0 ? 5 0.069 0.494 0.633 9.9 0.0 ? 6 -0.445 0.724 -0.030 793.5 43.1 '1 acetonitrile' 7 0.390 0.911 0.237 84.0 17.0 '1/2 isopropanol' 8 0.610 0.411 0.763 84.0 16.5 '1/2 isopropanol' # start Validation Reply Form _vrf_RINTA01_a ; PROBLEM: The value of Rint is greater than 0.25 RESPONSE: The crystal quality is not good because it is directly taken from hot acetonitrile. The acetonitrile molecules on the surface of crystal would be rapidly evaporated, leading to the formation of crack in the crystal. Furthermore, the excessive p-t-butyl benzoic acid in the hot acetonitrile would be remained on the surface of crystal with the leaving of acetonitrile. In addition, the Mo-K¦Á sealed-tube as X-ray source for the single diffraction make a relatively weaker diffraction data. However, the significant Fourier peaks were clear to construct the p-t-butyl benzoic acid ligands coordinated on the Ti8Zr2 clusters. Also the Ti8Zr2 clusters are isostructural to coordinate with different terminal carboxylic acids. We believe this proposed structure is well determined for this compound. ; _vrf_PLAT020_a ; PROBLEM: The value of Rint is greater than 0.12 ......... 0.375 Report RESPONSE: The crystal quality is not good because it is directly taken from hot acetonitrile. The acetonitrile molecules on the surface of crystal would be rapidly evaporated, leading to the formation of crack in the crystal. Furthermore, the excessive p-t-butyl benzoic acid in the hot acetonitrile would be remained on the surface of crystal with the leaving of acetonitrile. In addition, the Mo-K¦Á sealed-tube as X-ray source for the single diffraction make a relatively weaker diffraction data. However, the significant Fourier peaks were clear to construct the p-t-butyl benzoic acid ligands coordinated on the Ti8Zr2 clusters. Also the Ti8Zr2 clusters are isostructural to coordinate with different terminal carboxylic acids. We believe this proposed structure is well determined for this compound. ; _vrf_PLAT026_a ; PROBLEM: Ratio Observed / Unique Reflections (too) Low .. 28 % RESPONSE: The crystal quality is not good because it is directly taken from hot acetonitrile. The acetonitrile molecules on the surface of crystal would be rapidly evaporated, leading to the formation of crack in the crystal. Furthermore, the excessive p-t-butyl benzoic acid in the hot acetonitrile would be remained on the surface of crystal with the leaving of acetonitrile. In addition, the Mo-K¦Á sealed-tube as X-ray source for the single diffraction make a relatively weaker diffraction data. However, the significant Fourier peaks were clear to construct the p-t-butyl benzoic acid ligands coordinated on the Ti8Zr2 clusters. Also the Ti8Zr2 clusters are isostructural to coordinate with different terminal carboxylic acids. We believe this proposed structure is well determined for this compound. ; _vrf_PLAT213_a ; PROBLEM: Atom Ti04 has ADP max/min Ratio ..... 6.4 prolat RESPONSE: The crystal quality is not good because it is directly taken from hot acetonitrile. The acetonitrile molecules on the surface of crystal would be rapidly evaporated, leading to the formation of crack in the crystal. Furthermore, the excessive p-t-butyl benzoic acid in the hot acetonitrile would be remained on the surface of crystal with the leaving of acetonitrile. In addition, the Mo-K¦Á sealed-tube as X-ray source for the single diffraction make a relatively weaker diffraction data. However, the significant Fourier peaks were clear to construct the p-t-butyl benzoic acid ligands coordinated on the Ti8Zr2 clusters. Also the Ti8Zr2 clusters are isostructural to coordinate with different terminal carboxylic acids. We believe this proposed structure is well determined for this compound. ; _vrf_PLAT369_a ; PROBLEM: Long C(sp2)-C(sp2) Bond C30 - C47 .. 1.70 Ang. RESPONSE: The crystal quality is not good because it is directly taken from hot acetonitrile. The acetonitrile molecules on the surface of crystal would be rapidly evaporated, leading to the formation of crack in the crystal. Furthermore, the excessive p-t-butyl benzoic acid in the hot acetonitrile would be remained on the surface of crystal with the leaving of acetonitrile. In addition, the Mo-K¦Á sealed-tube as X-ray source for the single diffraction make a relatively weaker diffraction data. However, the significant Fourier peaks were clear to construct the p-t-butyl benzoic acid ligands coordinated on the Ti8Zr2 clusters. Also the Ti8Zr2 clusters are isostructural to coordinate with different terminal carboxylic acids. We believe this proposed structure is well determined for this compound. ; # end Validation Reply Form _olex2_submission_special_instructions 'No special instructions were received'