####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_NU-1600 _database_code_depnum_ccdc_archive 'CCDC 1908939' loop_ _audit_author_name _audit_author_address 'Ken-ichi Otake' ;Kyoto Univ Japan ; _audit_update_record ; 2019-04-09 deposited with the CCDC. 2019-04-09 downloaded from the CCDC. ; # start Validation Reply Form _vrf_THETM01_NU-1600 ; PROBLEM: The value of sine(theta_max)/wavelength is less than 0.550 RESPONSE: The higher angle diffraction data was too weak for structural determination because of low quality crystal that weakly diffracted. ; _vrf_PLAT029_NU-1600 ; PROBLEM: _diffrn_measured_fraction_theta_full value Low . 0.922 Why? RESPONSE: The higher angle diffraction data was too weak for structural determination because of low quality crystal that weakly diffracted. ; # Added during the CSD deposition process: Tuesday 09 April 2019 11:14 AM # end Validation Reply Form _audit_creation_method SHELXL-2018/3 _shelx_SHELXL_version_number 2018/3 _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88.50 H45.20 O36 Zr6' _chemical_formula_sum 'C88.50 H45.20 O36 Zr6' _chemical_formula_weight 2231.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.1862 2.2449 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 10 _space_group_name_H-M_alt 'P 2/m' _space_group_name_Hall '-P 2y' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z' '-x, -y, -z' 'x, -y, z' _cell_length_a 21.6317(10) _cell_length_b 12.2815(5) _cell_length_c 21.6273(10) _cell_angle_alpha 90 _cell_angle_beta 119.975(2) _cell_angle_gamma 90 _cell_volume 4977.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 6089 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 55.71 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 0.745 _exptl_crystal_F_000 1104 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.10 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.06 _exptl_absorpt_coefficient_mu 2.827 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7636 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(SADABS-2014/5; Krause et al., 2015)' _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_source microsource _diffrn_measurement_device_type 'Bruker Kappa APEX-II CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'MX optics' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 16957 _diffrn_reflns_av_unetI/netI 0.0448 _diffrn_reflns_av_R_equivalents 0.0461 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.358 _diffrn_reflns_theta_max 54.224 _diffrn_reflns_theta_full 54.224 _diffrn_measured_fraction_theta_max 0.922 _diffrn_measured_fraction_theta_full 0.922 _diffrn_reflns_Laue_measured_fraction_max 0.922 _diffrn_reflns_Laue_measured_fraction_full 0.922 _diffrn_reflns_point_group_measured_fraction_max 0.922 _diffrn_reflns_point_group_measured_fraction_full 0.922 _reflns_number_total 5932 _reflns_number_gt 4046 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_max . _reflns_Friedel_fraction_full . _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. ; _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_publication_material 'Yadokari-XG (Wakita, Nemoto et al., 2009)' _refine_special_details SQUEEZE _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_number_reflns 5932 _refine_ls_number_parameters 559 _refine_ls_number_restraints 1613 _refine_ls_R_factor_all 0.1602 _refine_ls_R_factor_gt 0.1328 _refine_ls_wR_factor_ref 0.4298 _refine_ls_wR_factor_gt 0.3947 _refine_ls_goodness_of_fit_ref 1.748 _refine_ls_restrained_S_all 1.671 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 C1 C 0.8959(6) 0.6806(9) 0.1006(6) 0.103(3) Uani 0.706(8) 1 d D U P . . C2 C 0.8649(9) 0.7509(11) 0.1375(7) 0.143(5) Uani 0.706(8) 1 d D U P A . C3 C 0.8850(15) 0.738(2) 0.2070(10) 0.139(8) Uani 0.353(4) 1 d D U P A 4 H3 H 0.921048 0.686524 0.235403 0.167 Uiso 0.353(4) 1 calc R U P A 4 C4 C 0.8518(14) 0.801(2) 0.2374(12) 0.126(7) Uani 0.353(4) 1 d D U P A 4 H4 H 0.864757 0.790069 0.285961 0.151 Uiso 0.353(4) 1 calc R U P A 4 C5 C 0.8009(8) 0.8774(10) 0.1972(7) 0.121(4) Uani 0.706(8) 1 d D U P . . C6 C 0.7718(16) 0.877(3) 0.1237(10) 0.147(9) Uani 0.353(4) 1 d D U P A 4 H6 H 0.727495 0.911423 0.093328 0.176 Uiso 0.353(4) 1 calc R U P A 4 C7 C 0.8100(14) 0.823(2) 0.0949(12) 0.133(7) Uani 0.353(4) 1 d D U P A 4 H7 H 0.798166 0.835836 0.046927 0.159 Uiso 0.353(4) 1 calc R U P A 4 C3B C 0.9051(10) 0.8278(15) 0.1897(10) 0.141(8) Uani 0.353(4) 1 d D U P A 5 H3B H 0.954217 0.837457 0.204921 0.169 Uiso 0.353(4) 1 calc R U P A 5 C4B C 0.8722(11) 0.8915(15) 0.2197(10) 0.162(10) Uani 0.353(4) 1 d D U P A 5 H4B H 0.899302 0.943988 0.255440 0.194 Uiso 0.353(4) 1 calc R U P A 5 C6B C 0.7616(10) 0.8012(15) 0.1460(10) 0.128(7) Uani 0.353(4) 1 d D U P A 5 H6B H 0.712505 0.791396 0.130878 0.153 Uiso 0.353(4) 1 calc R U P A 5 C7B C 0.7947(11) 0.7366(14) 0.1156(10) 0.128(7) Uani 0.353(4) 1 d D U P A 5 H7B H 0.767577 0.683816 0.080194 0.153 Uiso 0.353(4) 1 calc R U P A 5 C8 C 0.7687(7) 0.9437(10) 0.2316(7) 0.106(4) Uani 0.706(8) 1 d . U P A . C9 C 0.7344(7) 0.8842(9) 0.2644(6) 0.100(4) Uani 0.706(8) 1 d . U P . . H9 H 0.734019 0.806870 0.263796 0.120 Uiso 0.706(8) 1 calc R U P A . C10 C 0.7025(5) 0.9398(8) 0.2962(5) 0.075(3) Uani 0.706(8) 1 d . U P A . C11 C 0.6680(6) 0.8954(8) 0.3338(6) 0.089(3) Uani 0.706(8) 1 d . U P . . H11 H 0.667950 0.814024 0.333797 0.107 Uiso 0.706(8) 1 calc R U P A . C12 C 0.5931(6) 0.9417(7) 0.2968(5) 0.077(3) Uani 0.706(8) 1 d . U P A . C13 C 0.5294(7) 0.8847(9) 0.2658(6) 0.101(4) Uani 0.706(8) 1 d . U P . . H13 H 0.529699 0.807356 0.266528 0.121 Uiso 0.706(8) 1 calc R U P A . C14 C 0.4631(7) 0.9423(9) 0.2328(7) 0.111(4) Uani 0.706(8) 1 d . U P A . C15 C 0.3989(8) 0.8782(10) 0.1983(8) 0.129(5) Uani 0.706(8) 1 d D U P . . C16 C 0.3849(15) 0.798(2) 0.2380(15) 0.124(7) Uani 0.353(4) 1 d D U P A 4 H16 H 0.416858 0.791401 0.287844 0.149 Uiso 0.353(4) 1 calc R U P A 4 C17 C 0.3265(12) 0.732(2) 0.2056(12) 0.144(9) Uani 0.353(4) 1 d D U P A 4 H17 H 0.321243 0.672386 0.230572 0.173 Uiso 0.353(4) 1 calc R U P A 4 C18 C 0.2762(10) 0.7529(12) 0.1368(8) 0.150(6) Uani 0.706(8) 1 d D U P . . C19 C 0.2847(15) 0.820(2) 0.0903(14) 0.137(8) Uani 0.353(4) 1 d D U P A 4 H19 H 0.248577 0.829986 0.041935 0.164 Uiso 0.353(4) 1 calc R U P A 4 C20 C 0.3534(18) 0.873(2) 0.1217(12) 0.145(9) Uani 0.353(4) 1 d D U P A 4 H20 H 0.368762 0.905052 0.091674 0.173 Uiso 0.353(4) 1 calc R U P A 4 C16B C 0.3470(14) 0.887(2) 0.2209(14) 0.160(10) Uani 0.353(4) 1 d D U P A 5 H16B H 0.354338 0.936927 0.257604 0.192 Uiso 0.353(4) 1 calc R U P A 5 C17B C 0.2888(17) 0.8257(18) 0.1904(11) 0.152(9) Uani 0.353(4) 1 d D U P A 5 H17B H 0.254875 0.832000 0.205876 0.182 Uiso 0.353(4) 1 calc R U P A 5 C19B C 0.3220(13) 0.7372(19) 0.1117(12) 0.125(8) Uani 0.353(4) 1 d D U P A 5 H19B H 0.313683 0.686359 0.075258 0.149 Uiso 0.353(4) 1 calc R U P A 5 C20B C 0.3795(16) 0.8003(16) 0.1433(11) 0.130(8) Uani 0.353(4) 1 d D U P A 5 H20B H 0.412308 0.791956 0.126570 0.156 Uiso 0.353(4) 1 calc R U P A 5 C21 C 0.2061(6) 0.6791(9) 0.1017(5) 0.118(4) Uani 0.706(8) 1 d D U P A . C22 C 0.7037(5) 0.9415(7) 0.4082(5) 0.078(3) Uani 0.706(8) 1 d . U P A . C23 C 0.7351(7) 0.8858(9) 0.4706(6) 0.105(4) Uani 0.706(8) 1 d . U P . . H23 H 0.735826 0.808440 0.470205 0.126 Uiso 0.706(8) 1 calc R U P A . C24 C 0.7669(7) 0.9428(9) 0.5364(6) 0.114(4) Uani 0.706(8) 1 d . U P A . C25 C 0.8013(7) 0.8743(9) 0.6042(7) 0.121(4) Uani 0.706(8) 1 d D U P . . C26 C 0.8741(11) 0.8860(18) 0.6519(10) 0.147(9) Uani 0.353(4) 1 d D U P A 4 H26 H 0.901417 0.937242 0.642719 0.176 Uiso 0.353(4) 1 calc R U P A 4 C27 C 0.9062(14) 0.8218(15) 0.7128(11) 0.141(8) Uani 0.353(4) 1 d D U P A 4 H27 H 0.955840 0.829688 0.745310 0.169 Uiso 0.353(4) 1 calc R U P A 4 C28 C 0.8672(7) 0.7461(12) 0.7274(9) 0.142(5) Uani 0.706(8) 1 d D U P . . C29 C 0.7960(11) 0.7387(18) 0.6783(9) 0.140(9) Uani 0.353(4) 1 d D U P A 4 H29 H 0.768538 0.687196 0.687097 0.168 Uiso 0.353(4) 1 calc R U P A 4 C30 C 0.7611(13) 0.8009(15) 0.6166(11) 0.133(8) Uani 0.353(4) 1 d D U P A 4 H30 H 0.711390 0.792855 0.584317 0.159 Uiso 0.353(4) 1 calc R U P A 4 C26B C 0.8538(10) 0.7996(14) 0.6159(12) 0.126(8) Uani 0.353(4) 1 d D U P A 5 H26B H 0.867703 0.791988 0.580821 0.152 Uiso 0.353(4) 1 calc R U P A 5 C27B C 0.8869(12) 0.7354(17) 0.6765(11) 0.131(8) Uani 0.353(4) 1 d D U P A 5 H27B H 0.922710 0.684694 0.682688 0.157 Uiso 0.353(4) 1 calc R U P A 5 C29B C 0.8133(11) 0.8230(17) 0.7130(13) 0.153(9) Uani 0.353(4) 1 d D U P A 5 H29B H 0.799195 0.830794 0.747865 0.184 Uiso 0.353(4) 1 calc R U P A 5 C30B C 0.7792(13) 0.8880(18) 0.6533(11) 0.140(9) Uani 0.353(4) 1 d D U P A 5 H30B H 0.743033 0.938490 0.646594 0.168 Uiso 0.353(4) 1 calc R U P A 5 C31 C 0.9008(6) 0.6827(8) 0.7955(5) 0.106(4) Uani 0.706(8) 1 d D U P A . C32 C 1.000000 0.842200 0.000000 0.150(9) Uiso 0.5 2 d S U P . . Zr1X Zr 0.9053(2) 0.6432(2) -0.04704(14) 0.1003(11) Uani 0.3333 1 d D U P B 1 Zr2X Zr 1.0002(2) 0.500000 0.1155(2) 0.0774(13) Uani 0.3333 2 d DS TU P B 1 O1X O 0.9902(18) 0.6425(16) 0.0526(14) 0.106(8) Uiso 0.3333 1 d D U P B 1 O2X O 0.907(2) 0.500000 0.0076(16) 0.090(11) Uiso 0.3333 2 d DS U P B 1 O2AX O 0.9128(18) 0.500000 -0.0966(17) 0.062(11) Uiso 0.3333 2 d DS U P B 1 O3X O 0.9132(10) 0.5989(12) 0.1241(9) 0.098(5) Uiso 0.3333 1 d D U P B 1 O4X O 0.9020(16) 0.706(3) 0.0512(13) 0.181(8) Uiso 0.3333 1 d D U P B 1 O5X O 0.9254(10) 0.6037(13) 0.7947(9) 0.101(5) Uiso 0.3333 1 d D U P A 1 O6X O 0.8785(13) 0.701(2) 0.8350(12) 0.147(7) Uiso 0.3333 1 d D U P A 1 O7X O 0.1661(12) 0.690(2) 0.1439(12) 0.142(7) Uiso 0.3333 1 d D U P A 1 O8X O 0.1947(18) 0.617(2) 0.0373(12) 0.209(11) Uiso 0.3333 1 d D U P A 1 O9X O 0.9204(12) 0.8138(15) -0.0389(10) 0.126(6) Uani 0.3333 1 d . U P B 1 Zr1Y Zr 0.95263(19) 0.64329(19) 0.04716(15) 0.1002(11) Uani 0.3333 1 d D U P B 2 Zr2Y Zr 0.8844(3) 0.500000 -0.1154(3) 0.0797(15) Uani 0.3333 2 d DS TU P B 2 O1Y O 0.9034(17) 0.500000 -0.0085(10) 0.080(10) Uiso 0.3333 2 d DS U P B 2 O1AY O 1.0095(15) 0.500000 0.0958(17) 0.079(9) Uiso 0.3333 2 d DS U P B 2 O2Y O 0.9405(13) 0.6446(17) -0.0529(13) 0.096(7) Uiso 0.3333 1 d D U P B 2 O3Y O 0.8773(10) 0.5991(12) 0.7917(9) 0.097(4) Uiso 0.3333 1 d D U P A 2 O4Y O 0.9500(14) 0.724(2) 0.8492(13) 0.188(9) Uiso 0.3333 1 d D U P A 2 O5Y O 0.1594(11) 0.7102(18) 0.0399(10) 0.137(6) Uiso 0.3333 1 d D U P A 2 O6Y O 0.2041(8) 0.6058(12) 0.1337(8) 0.093(4) Uiso 0.3333 1 d D U P A 2 O7Y O 0.9634(12) 0.622(2) 0.1509(14) 0.174(9) Uiso 0.3333 1 d D U P B 2 O8Y O 0.8492(13) 0.687(2) 0.0195(10) 0.149(7) Uiso 0.3333 1 d D U P B 2 O9Y O 0.9593(12) 0.8114(16) 0.0384(11) 0.140(6) Uani 0.3333 1 d . U P B 2 Zr1Z Zr 1.04632(17) 0.64428(18) 0.09327(17) 0.1012(10) Uani 0.3333 1 d D U P B 3 Zr2Z Zr 0.8845(3) 0.500000 0.0004(2) 0.0774(12) Uani 0.3333 2 d DS TU P B 3 O1Z O 0.9436(15) 0.6393(16) -0.001(2) 0.120(6) Uiso 0.3333 1 d D U P B 3 O2Z O 0.9936(15) 0.500000 0.095(2) 0.082(12) Uiso 0.3333 2 d DS U P B 3 O2AZ O 1.1021(17) 0.500000 0.097(3) 0.09(2) Uiso 0.3333 2 d DS U P B 3 O3Z O 0.8688(9) 0.6081(11) 0.0743(8) 0.087(4) Uiso 0.3333 1 d D U P B 3 O4Z O 0.9545(11) 0.705(2) 0.1237(13) 0.147(7) Uiso 0.3333 1 d D U P B 3 O5Z O 0.2111(9) 0.6001(12) 0.0879(9) 0.099(5) Uiso 0.3333 1 d D U P A 3 O6Z O 0.1619(15) 0.729(2) 0.0991(16) 0.205(10) Uiso 0.3333 1 d D U P A 3 O7Z O 0.8511(14) 0.623(2) 0.8122(14) 0.181(10) Uiso 0.3333 1 d D U P A 3 O8Z O 0.9833(10) 0.691(2) 0.8373(11) 0.142(7) Uiso 0.3333 1 d D U P A 3 O9Z O 1.0414(12) 0.812(2) 0.0801(12) 0.140(7) Uiso 0.3333 1 d . U P B 3 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 C1 0.091(7) 0.131(8) 0.119(7) -0.003(7) 0.076(6) -0.015(7) C2 0.169(11) 0.122(9) 0.146(10) 0.018(8) 0.086(10) -0.013(8) C3 0.155(15) 0.126(14) 0.145(13) 0.005(12) 0.081(12) 0.009(12) C4 0.139(14) 0.121(13) 0.134(13) -0.009(11) 0.081(11) 0.007(12) C5 0.140(10) 0.108(8) 0.141(9) -0.005(7) 0.088(8) 0.006(7) C6 0.171(16) 0.143(16) 0.145(14) -0.002(13) 0.094(13) 0.025(13) C7 0.151(15) 0.153(15) 0.140(14) 0.004(12) 0.108(12) 0.022(13) C3B 0.159(15) 0.143(15) 0.153(14) -0.015(13) 0.103(12) 0.001(13) C4B 0.174(16) 0.153(16) 0.159(15) -0.010(14) 0.083(14) -0.014(14) C6B 0.153(14) 0.117(13) 0.132(13) -0.002(12) 0.086(11) 0.008(12) C7B 0.145(14) 0.113(13) 0.143(13) 0.000(12) 0.086(12) -0.003(12) C8 0.118(9) 0.104(7) 0.118(8) -0.004(6) 0.076(7) 0.001(6) C9 0.108(9) 0.091(7) 0.107(7) 0.005(6) 0.059(7) 0.000(6) C10 0.078(7) 0.078(5) 0.070(5) -0.004(4) 0.037(5) 0.001(5) C11 0.093(7) 0.073(5) 0.090(6) 0.005(5) 0.038(6) 0.004(5) C12 0.085(7) 0.074(5) 0.069(5) -0.006(4) 0.036(5) -0.010(5) C13 0.110(9) 0.073(6) 0.109(8) 0.000(5) 0.046(7) 0.004(6) C14 0.102(9) 0.090(6) 0.135(9) -0.004(6) 0.056(8) -0.007(6) C15 0.108(9) 0.106(8) 0.150(10) -0.004(7) 0.047(8) 0.004(7) C16 0.113(13) 0.126(13) 0.134(13) 0.001(12) 0.063(11) -0.016(11) C17 0.140(15) 0.119(13) 0.148(14) 0.004(12) 0.054(12) -0.025(12) C18 0.159(12) 0.122(10) 0.149(10) 0.005(8) 0.062(9) -0.004(9) C19 0.131(15) 0.111(13) 0.141(14) 0.020(12) 0.047(12) -0.020(12) C20 0.130(15) 0.125(15) 0.153(15) -0.003(13) 0.052(13) -0.024(13) C16B 0.134(15) 0.144(15) 0.164(16) -0.022(14) 0.047(13) -0.020(13) C17B 0.132(15) 0.134(14) 0.161(15) -0.033(14) 0.051(13) -0.024(13) C19B 0.120(14) 0.104(13) 0.147(14) -0.033(12) 0.065(11) -0.010(11) C20B 0.123(14) 0.104(13) 0.145(14) -0.018(12) 0.054(12) 0.011(11) C21 0.094(8) 0.129(9) 0.115(8) 0.004(7) 0.042(7) 0.023(7) C22 0.090(7) 0.073(5) 0.068(5) 0.006(4) 0.037(5) 0.001(5) C23 0.135(10) 0.094(7) 0.073(6) -0.002(5) 0.041(6) 0.003(6) C24 0.147(10) 0.098(7) 0.072(6) 0.006(5) 0.037(6) 0.001(7) C25 0.136(10) 0.105(8) 0.100(7) 0.003(6) 0.042(7) 0.013(7) C26 0.155(15) 0.131(14) 0.105(13) 0.004(12) 0.028(12) 0.013(13) C27 0.158(15) 0.143(15) 0.106(13) 0.019(12) 0.054(12) -0.008(13) C28 0.149(11) 0.130(10) 0.125(9) -0.013(8) 0.053(8) -0.017(8) C29 0.144(14) 0.114(13) 0.125(13) 0.020(11) 0.039(12) -0.017(12) C30 0.157(15) 0.118(13) 0.108(12) 0.025(11) 0.056(12) -0.028(12) C26B 0.132(14) 0.123(14) 0.108(13) 0.008(11) 0.048(11) 0.035(12) C27B 0.143(14) 0.107(13) 0.115(13) 0.006(11) 0.045(11) 0.014(12) C29B 0.171(16) 0.139(15) 0.103(13) 0.007(12) 0.034(13) 0.008(14) C30B 0.171(16) 0.119(14) 0.113(13) -0.002(12) 0.057(12) 0.009(13) C31 0.125(9) 0.122(8) 0.067(5) -0.018(6) 0.045(6) -0.002(7) Zr1X 0.138(3) 0.0991(16) 0.0774(17) 0.0177(10) 0.0636(18) 0.0353(15) Zr2X 0.110(3) 0.0686(19) 0.068(2) 0.000 0.0544(19) 0.000 O9X 0.172(14) 0.097(10) 0.126(11) 0.033(9) 0.086(11) 0.032(10) Zr1Y 0.086(2) 0.0979(16) 0.0785(17) -0.0139(10) 0.0128(15) 0.0207(12) Zr2Y 0.069(3) 0.069(2) 0.067(2) 0.000 0.008(2) 0.000 O9Y 0.173(13) 0.099(10) 0.133(11) 0.000(9) 0.066(11) 0.041(10) Zr1Z 0.087(2) 0.0978(16) 0.132(2) -0.0321(13) 0.0646(19) -0.0160(11) Zr2Z 0.078(3) 0.0683(18) 0.098(2) 0.000 0.053(2) 0.000 _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 C1 O3Z 1.061(14) . ? C1 O3X 1.102(15) . ? C1 O4Z 1.145(17) . ? C1 O4X 1.181(18) . ? C1 O7Y 1.498(18) . ? C1 O8Y 1.528(17) . ? C1 C2 1.538(19) . ? C1 Zr1Y 2.115(12) . ? C2 C3 1.350(16) . ? C2 C7B 1.357(16) . ? C2 C3B 1.394(16) . ? C2 C7 1.395(16) . ? C3 C4 1.42(2) . ? C3 H3 0.9500 . ? C4 C5 1.376(16) . ? C4 H4 0.9500 . ? C5 C6B 1.372(15) . ? C5 C4B 1.376(16) . ? C5 C6 1.387(17) . ? C5 C8 1.490(18) . ? C6 C7 1.42(2) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C3B C4B 1.42(2) . ? C3B H3B 0.9500 . ? C4B H4B 0.9500 . ? C6B C7B 1.43(2) . ? C6B H6B 0.9500 . ? C7B H7B 0.9500 . ? C8 C8 1.38(2) 4_575 ? C8 C9 1.453(16) . ? C9 C10 1.375(15) . ? C9 H9 0.9500 . ? C10 C11 1.456(15) . ? C10 C10 1.480(19) 4_575 ? C11 C22 1.506(14) . ? C11 C12 1.514(15) . ? C11 H11 1.0000 . ? C12 C13 1.384(15) . ? C12 C12 1.432(18) 4_575 ? C13 C14 1.429(16) . ? C13 H13 0.9500 . ? C14 C14 1.42(2) 4_575 ? C14 C15 1.439(18) . ? C15 C20B 1.418(19) . ? C15 C16 1.431(19) . ? C15 C16B 1.43(2) . ? C15 C20 1.45(2) . ? C16 C17 1.37(3) . ? C16 H16 0.9500 . ? C17 C18 1.358(18) . ? C17 H17 0.9500 . ? C18 C19B 1.360(19) . ? C18 C17B 1.379(19) . ? C18 C19 1.381(18) . ? C18 C21 1.60(2) . ? C19 C20 1.45(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C16B C17B 1.33(4) . ? C16B H16B 0.9500 . ? C17B H17B 0.9500 . ? C19B C20B 1.33(4) . ? C19B H19B 0.9500 . ? C20B H20B 0.9500 . ? C21 O5Z 1.037(15) . ? C21 O6Z 1.116(18) . ? C21 O6Y 1.150(15) . ? C21 O5Y 1.266(16) . ? C21 O8X 1.493(19) . ? C21 O7X 1.545(17) . ? C21 Zr1X 2.132(13) 2_655 ? C22 C23 1.354(13) . ? C22 C22 1.436(18) 4_575 ? C23 C24 1.419(15) . ? C23 H23 0.9500 . ? C24 C24 1.41(2) 4_575 ? C24 C25 1.524(17) . ? C25 C30 1.368(18) . ? C25 C30B 1.376(19) . ? C25 C26B 1.382(18) . ? C25 C26 1.393(19) . ? C26 C27 1.39(2) . ? C26 H26 0.9500 . ? C27 C28 1.394(18) . ? C27 H27 0.9500 . ? C28 C29 1.368(17) . ? C28 C27B 1.373(19) . ? C28 C29B 1.408(19) . ? C28 C31 1.494(19) . ? C29 C30 1.39(2) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C26B C27B 1.38(2) . ? C26B H26B 0.9500 . ? C27B H27B 0.9500 . ? C29B C30B 1.38(2) . ? C29B H29B 0.9500 . ? C30B H30B 0.9500 . ? C31 O5X 1.111(15) . ? C31 O3Y 1.131(15) . ? C31 O6X 1.195(17) . ? C31 O4Y 1.224(18) . ? C31 O7Z 1.491(18) . ? C31 O8Z 1.550(17) . ? C31 Zr1Z 2.138(11) 2_756 ? C32 O9Y 1.53(3) 2_755 ? C32 O9Y 1.53(3) . ? C32 O9X 1.53(2) . ? C32 O9X 1.53(2) 2_755 ? C32 O9Z 1.55(2) . ? C32 O9Z 1.55(2) 2_755 ? Zr1X O7X 1.97(2) 2_655 ? Zr1X O1X 2.02(3) . ? Zr1X O2X 2.106(15) . ? Zr1X O2AX 2.108(15) . ? Zr1X O9X 2.115(19) . ? Zr1X O4X 2.29(3) . ? Zr1X O8X 2.30(3) 2_655 ? Zr1X O1X 2.32(3) 2_755 ? Zr1X O6X 2.42(2) 1_554 ? Zr1X Zr1X 3.518(5) 4_565 ? Zr1X Zr2X 3.530(5) . ? Zr2X O2AX 2.12(3) 3_765 ? Zr2X O1X 2.160(17) . ? Zr2X O1X 2.160(17) 4_565 ? Zr2X O2X 2.19(4) . ? Zr2X O5X 2.205(16) 2_756 ? Zr2X O5X 2.205(16) 3_766 ? Zr2X O3X 2.324(18) . ? Zr2X O3X 2.324(18) 4_565 ? O6X O7X 1.26(3) 2_656 ? Zr1Y O2Y 2.05(3) . ? Zr1Y O8Y 2.08(3) . ? Zr1Y O9Y 2.08(2) . ? Zr1Y O1Y 2.098(13) . ? Zr1Y O1AY 2.103(15) . ? Zr1Y O7Y 2.15(3) . ? Zr1Y O2Y 2.25(3) 2_755 ? Zr1Y O5Y 2.35(2) 2_655 ? Zr1Y O4Y 2.39(3) 2_756 ? Zr1Y Zr1Y 3.520(5) 4_565 ? Zr1Y Zr2Y 3.528(5) . ? Zr2Y O1AY 2.12(3) 3_765 ? Zr2Y O1Y 2.136(18) . ? Zr2Y O6Y 2.180(16) 3_665 ? Zr2Y O6Y 2.180(16) 2_655 ? Zr2Y O2Y 2.19(2) 4_565 ? Zr2Y O2Y 2.19(2) . ? Zr2Y O3Y 2.289(17) 4_564 ? Zr2Y O3Y 2.289(17) 1_554 ? O5Y O8Y 1.23(3) 2_655 ? Zr1Z O8Z 1.99(2) 2_756 ? Zr1Z O9Z 2.08(2) . ? Zr1Z O1Z 2.11(3) 2_755 ? Zr1Z O2Z 2.120(12) . ? Zr1Z O2AZ 2.120(12) . ? Zr1Z O1Z 2.14(3) . ? Zr1Z O7Z 2.15(3) 2_756 ? Zr1Z O4Z 2.50(2) . ? Zr1Z O6Z 2.65(3) 1_655 ? Zr1Z Zr1Z 3.495(6) 2_755 ? Zr1Z Zr2Z 3.521(5) . ? Zr2Z O1Z 2.146(17) . ? Zr2Z O1Z 2.146(17) 4_565 ? Zr2Z O2Z 2.22(4) . ? Zr2Z O3Z 2.232(15) . ? Zr2Z O3Z 2.232(15) 4_565 ? Zr2Z O2AZ 2.27(5) 3_765 ? Zr2Z O5Z 2.343(17) 3_665 ? Zr2Z O5Z 2.343(17) 2_655 ? O4Z O8Z 1.19(2) 2_756 ? 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 O3Z C1 O4Z 130.3(19) . . ? O3X C1 O4X 119(2) . . ? O7Y C1 O8Y 134.9(18) . . ? O3Z C1 C2 118.7(13) . . ? O3X C1 C2 114.1(13) . . ? O4Z C1 C2 107.6(15) . . ? O4X C1 C2 127(2) . . ? O7Y C1 C2 114.4(14) . . ? O8Y C1 C2 110.8(12) . . ? O7Y C1 Zr1Y 70.8(12) . . ? O8Y C1 Zr1Y 67.4(11) . . ? C2 C1 Zr1Y 158.1(8) . . ? C7B C2 C3B 120.5(15) . . ? C3 C2 C7 120.4(19) . . ? C3 C2 C1 121.9(13) . . ? C7B C2 C1 116.7(12) . . ? C3B C2 C1 122.9(13) . . ? C7 C2 C1 117.5(12) . . ? C2 C3 C4 119.6(19) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? C5 C4 C3 120.5(18) . . ? C5 C4 H4 119.7 . . ? C3 C4 H4 119.7 . . ? C6B C5 C4B 120.3(15) . . ? C4 C5 C6 118.9(17) . . ? C6B C5 C8 121.2(14) . . ? C4B C5 C8 118.4(13) . . ? C4 C5 C8 118.8(14) . . ? C6 C5 C8 121.2(14) . . ? C5 C6 C7 118.3(19) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C2 C7 C6 119.7(18) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? C2 C3B C4B 119.6(11) . . ? C2 C3B H3B 120.2 . . ? C4B C3B H3B 120.2 . . ? C5 C4B C3B 119.9(12) . . ? C5 C4B H4B 120.0 . . ? C3B C4B H4B 120.0 . . ? C5 C6B C7B 119.9(11) . . ? C5 C6B H6B 120.1 . . ? C7B C6B H6B 120.1 . . ? C2 C7B C6B 119.8(12) . . ? C2 C7B H7B 120.1 . . ? C6B C7B H7B 120.1 . . ? C8 C8 C9 120.2(7) 4_575 . ? C8 C8 C5 123.1(7) 4_575 . ? C9 C8 C5 116.7(11) . . ? C10 C9 C8 120.1(11) . . ? C10 C9 H9 120.0 . . ? C8 C9 H9 120.0 . . ? C9 C10 C11 128.3(10) . . ? C9 C10 C10 119.7(7) . 4_575 ? C11 C10 C10 111.9(6) . 4_575 ? C10 C11 C22 108.9(9) . . ? C10 C11 C12 106.1(8) . . ? C22 C11 C12 105.4(9) . . ? C10 C11 H11 112.0 . . ? C22 C11 H11 112.0 . . ? C12 C11 H11 112.0 . . ? C13 C12 C12 120.4(6) . 4_575 ? C13 C12 C11 127.6(9) . . ? C12 C12 C11 112.0(5) 4_575 . ? C12 C13 C14 119.9(10) . . ? C12 C13 H13 120.0 . . ? C14 C13 H13 120.0 . . ? C14 C14 C13 119.7(7) 4_575 . ? C14 C14 C15 123.2(7) 4_575 . ? C13 C14 C15 117.1(11) . . ? C20B C15 C16B 113(2) . . ? C20B C15 C14 128(2) . . ? C16 C15 C14 120.2(16) . . ? C16B C15 C14 119.9(18) . . ? C16 C15 C20 115(2) . . ? C14 C15 C20 123.1(19) . . ? C17 C16 C15 121(2) . . ? C17 C16 H16 119.4 . . ? C15 C16 H16 119.4 . . ? C18 C17 C16 119(2) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C19B C18 C17B 123(2) . . ? C17 C18 C19 126(2) . . ? C17 C18 C21 117.7(14) . . ? C19B C18 C21 116.0(16) . . ? C17B C18 C21 121(2) . . ? C19 C18 C21 115.6(13) . . ? C18 C19 C20 114(2) . . ? C18 C19 H19 123.0 . . ? C20 C19 H19 123.0 . . ? C19 C20 C15 121(3) . . ? C19 C20 H20 119.7 . . ? C15 C20 H20 119.7 . . ? C17B C16B C15 120(3) . . ? C17B C16B H16B 120.1 . . ? C15 C16B H16B 120.1 . . ? C16B C17B C18 122(3) . . ? C16B C17B H17B 119.1 . . ? C18 C17B H17B 119.1 . . ? C20B C19B C18 113(2) . . ? C20B C19B H19B 123.4 . . ? C18 C19B H19B 123.4 . . ? C19B C20B C15 129(3) . . ? C19B C20B H20B 115.3 . . ? C15 C20B H20B 115.3 . . ? O5Z C21 O6Z 136(3) . . ? O6Y C21 O5Y 128.4(18) . . ? O8X C21 O7X 135.6(19) . . ? O5Z C21 C18 117.2(14) . . ? O6Z C21 C18 107(2) . . ? O6Y C21 C18 118.1(12) . . ? O5Y C21 C18 113.5(14) . . ? O8X C21 C18 114.0(17) . . ? O7X C21 C18 110.4(12) . . ? O8X C21 Zr1X 76.3(15) . 2_655 ? O7X C21 Zr1X 62.3(9) . 2_655 ? C18 C21 Zr1X 157.3(7) . 2_655 ? C23 C22 C22 120.4(6) . 4_575 ? C23 C22 C11 127.5(9) . . ? C22 C22 C11 112.1(5) 4_575 . ? C22 C23 C24 120.0(10) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C24 C24 C23 119.6(6) 4_575 . ? C24 C24 C25 123.5(6) 4_575 . ? C23 C24 C25 116.9(10) . . ? C30B C25 C26B 120.8(19) . . ? C30 C25 C26 121.1(19) . . ? C30 C25 C24 120.0(14) . . ? C30B C25 C24 119.0(15) . . ? C26B C25 C24 120.2(15) . . ? C26 C25 C24 118.9(14) . . ? C27 C26 C25 119(2) . . ? C27 C26 H26 120.4 . . ? C25 C26 H26 120.4 . . ? C26 C27 C28 121(2) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C29 C28 C27 116(2) . . ? C27B C28 C29B 116(2) . . ? C29 C28 C31 122.4(13) . . ? C27B C28 C31 123.2(14) . . ? C27 C28 C31 121.3(13) . . ? C29B C28 C31 120.7(15) . . ? C28 C29 C30 125(2) . . ? C28 C29 H29 117.6 . . ? C30 C29 H29 117.6 . . ? C25 C30 C29 117(2) . . ? C25 C30 H30 121.4 . . ? C29 C30 H30 121.4 . . ? C25 C26B C27B 123(2) . . ? C25 C26B H26B 118.6 . . ? C27B C26B H26B 118.6 . . ? C28 C27B C26B 119(2) . . ? C28 C27B H27B 120.5 . . ? C26B C27B H27B 120.5 . . ? C30B C29B C28 126(3) . . ? C30B C29B H29B 116.8 . . ? C28 C29B H29B 116.8 . . ? C25 C30B C29B 115(2) . . ? C25 C30B H30B 122.5 . . ? C29B C30B H30B 122.5 . . ? O5X C31 O6X 122.9(19) . . ? O3Y C31 O4Y 126(2) . . ? O5X C31 C28 116.2(12) . . ? O3Y C31 C28 114.9(12) . . ? O6X C31 C28 115.8(15) . . ? O4Y C31 C28 119.1(18) . . ? O7Z C31 C28 116.2(12) . . ? O7Z C31 O8Z 130.7(17) . . ? C28 C31 O8Z 113.0(10) . . ? O5X C31 Zr1Z 80.4(11) . 2_756 ? O6X C31 Zr1Z 54.3(13) . 2_756 ? C28 C31 Zr1Z 161.3(7) . 2_756 ? O9Y C32 O9Y 151.3(14) 2_755 . ? O9X C32 O9X 153.7(13) . 2_755 ? O9Y C32 O9Z 60.0(11) 2_755 2_755 ? O9Y C32 O9Z 112.5(11) . 2_755 ? O9X C32 O9Z 57.8(10) . 2_755 ? O9X C32 O9Z 115.1(10) 2_755 2_755 ? O9Z C32 O9Z 152.6(18) . 2_755 ? O7X Zr1X O1X 161.9(9) 2_655 . ? O7X Zr1X O2X 128.9(12) 2_655 . ? O1X Zr1X O2X 69.1(9) . . ? O7X Zr1X O2AX 85.6(11) 2_655 . ? O1X Zr1X O2AX 106.2(11) . . ? O2X Zr1X O2AX 66.6(10) . . ? O7X Zr1X O9X 78.7(9) 2_655 . ? O1X Zr1X O9X 84.0(8) . . ? O2X Zr1X O9X 145.3(8) . . ? O2AX Zr1X O9X 145.2(8) . . ? O7X Zr1X C21 44.0(5) 2_655 2_655 ? O1X Zr1X C21 140.1(9) . 2_655 ? O2X Zr1X C21 100.8(12) . 2_655 ? O2AX Zr1X C21 104.1(10) . 2_655 ? O9X Zr1X C21 85.8(7) . 2_655 ? O7X Zr1X O4X 121.2(10) 2_655 . ? O1X Zr1X O4X 56.3(10) . . ? O2X Zr1X O4X 76.2(10) . . ? O2AX Zr1X O4X 142.7(10) . . ? O9X Zr1X O4X 70.6(9) . . ? C21 Zr1X O4X 84.0(8) 2_655 . ? O7X Zr1X O8X 82.2(9) 2_655 2_655 ? O1X Zr1X O8X 107.4(10) . 2_655 ? O2X Zr1X O8X 65.9(13) . 2_655 ? O2AX Zr1X O8X 104.3(11) . 2_655 ? O9X Zr1X O8X 104.1(9) . 2_655 ? C21 Zr1X O8X 39.2(6) 2_655 2_655 ? O4X Zr1X O8X 59.7(9) . 2_655 ? O7X Zr1X O1X 102.3(9) 2_655 2_755 ? O1X Zr1X O1X 70.4(10) . 2_755 ? O2X Zr1X O1X 106.0(10) . 2_755 ? O2AX Zr1X O1X 69.3(9) . 2_755 ? O9X Zr1X O1X 83.9(8) . 2_755 ? C21 Zr1X O1X 146.2(8) 2_655 2_755 ? O4X Zr1X O1X 122.0(9) . 2_755 ? O8X Zr1X O1X 171.6(9) 2_655 2_755 ? O7X Zr1X O6X 31.3(7) 2_655 1_554 ? O1X Zr1X O6X 137.5(10) . 1_554 ? O2X Zr1X O6X 139.6(9) . 1_554 ? O2AX Zr1X O6X 75.4(9) . 1_554 ? O9X Zr1X O6X 75.1(8) . 1_554 ? C21 Zr1X O6X 75.3(6) 2_655 1_554 ? O4X Zr1X O6X 140.9(10) . 1_554 ? O8X Zr1X O6X 113.3(8) 2_655 1_554 ? O1X Zr1X O6X 70.9(9) 2_755 1_554 ? O7X Zr1X Zr1X 107.1(7) 2_655 4_565 ? O1X Zr1X Zr1X 89.7(6) . 4_565 ? O2X Zr1X Zr1X 33.4(6) . 4_565 ? O2AX Zr1X Zr1X 33.4(6) . 4_565 ? O9X Zr1X Zr1X 172.3(6) . 4_565 ? C21 Zr1X Zr1X 101.9(3) 2_655 4_565 ? O4X Zr1X Zr1X 109.5(7) . 4_565 ? O8X Zr1X Zr1X 82.1(7) 2_655 4_565 ? O1X Zr1X Zr1X 89.8(5) 2_755 4_565 ? O6X Zr1X Zr1X 107.0(6) 1_554 4_565 ? O7X Zr1X Zr2X 164.4(7) 2_655 . ? O1X Zr1X Zr2X 33.6(6) . . ? O2X Zr1X Zr2X 35.5(10) . . ? O2AX Zr1X Zr2X 86.3(8) . . ? O9X Zr1X Zr2X 115.0(5) . . ? C21 Zr1X Zr2X 126.1(3) 2_655 . ? O4X Zr1X Zr2X 61.0(8) . . ? O8X Zr1X Zr2X 86.9(6) 2_655 . ? O1X Zr1X Zr2X 87.3(7) 2_755 . ? O6X Zr1X Zr2X 155.3(6) 1_554 . ? Zr1X Zr1X Zr2X 60.11(6) 4_565 . ? O2AX Zr2X O1X 72.4(10) 3_765 . ? O2AX Zr2X O1X 72.4(10) 3_765 4_565 ? O1X Zr2X O1X 108.2(13) . 4_565 ? O2AX Zr2X O2X 102.9(14) 3_765 . ? O1X Zr2X O2X 65.1(7) . . ? O1X Zr2X O2X 65.1(7) 4_565 . ? O2AX Zr2X O5X 80.9(9) 3_765 2_756 ? O1X Zr2X O5X 83.5(9) . 2_756 ? O1X Zr2X O5X 145.3(11) 4_565 2_756 ? O2X Zr2X O5X 144.7(4) . 2_756 ? O2AX Zr2X O5X 80.9(9) 3_765 3_766 ? O1X Zr2X O5X 145.3(11) . 3_766 ? O1X Zr2X O5X 83.5(9) 4_565 3_766 ? O2X Zr2X O5X 144.7(4) . 3_766 ? O5X Zr2X O5X 70.6(9) 2_756 3_766 ? O2AX Zr2X O3X 148.1(4) 3_765 . ? O1X Zr2X O3X 78.3(9) . . ? O1X Zr2X O3X 130.1(10) 4_565 . ? O2X Zr2X O3X 74.8(9) . . ? O5X Zr2X O3X 83.8(7) 2_756 . ? O5X Zr2X O3X 119.7(7) 3_766 . ? O2AX Zr2X O3X 148.1(4) 3_765 4_565 ? O1X Zr2X O3X 130.1(10) . 4_565 ? O1X Zr2X O3X 78.3(9) 4_565 4_565 ? O2X Zr2X O3X 74.8(9) . 4_565 ? O5X Zr2X O3X 119.7(7) 2_756 4_565 ? O5X Zr2X O3X 83.8(7) 3_766 4_565 ? O3X Zr2X O3X 63.0(8) . 4_565 ? O2AX Zr2X Zr1X 86.5(8) 3_765 . ? O1X Zr2X Zr1X 31.1(8) . . ? O1X Zr2X Zr1X 87.2(7) 4_565 . ? O2X Zr2X Zr1X 34.0(4) . . ? O5X Zr2X Zr1X 113.3(4) 2_756 . ? O5X Zr2X Zr1X 166.1(5) 3_766 . ? O3X Zr2X Zr1X 74.2(4) . . ? O3X Zr2X Zr1X 104.4(5) 4_565 . ? O2AX Zr2X Zr1X 86.5(8) 3_765 4_565 ? O1X Zr2X Zr1X 87.2(7) . 4_565 ? O1X Zr2X Zr1X 31.1(8) 4_565 4_565 ? O2X Zr2X Zr1X 34.0(4) . 4_565 ? O5X Zr2X Zr1X 166.1(5) 2_756 4_565 ? O5X Zr2X Zr1X 113.3(4) 3_766 4_565 ? O3X Zr2X Zr1X 104.4(5) . 4_565 ? O3X Zr2X Zr1X 74.2(4) 4_565 4_565 ? Zr1X Zr2X Zr1X 59.78(11) . 4_565 ? O2AX Zr2X Zr1X 33.1(4) 3_765 2_755 ? O1X Zr2X Zr1X 39.6(8) . 2_755 ? O1X Zr2X Zr1X 92.1(7) 4_565 2_755 ? O2X Zr2X Zr1X 88.1(8) . 2_755 ? O5X Zr2X Zr1X 76.2(5) 2_756 2_755 ? O5X Zr2X Zr1X 109.7(6) 3_766 2_755 ? O3X Zr2X Zr1X 115.7(4) . 2_755 ? O3X Zr2X Zr1X 162.7(5) 4_565 2_755 ? Zr1X Zr2X Zr1X 60.35(13) . 2_755 ? Zr1X Zr2X Zr1X 90.07(12) 4_565 2_755 ? O2AX Zr2X Zr1X 33.1(4) 3_765 3_765 ? O1X Zr2X Zr1X 92.1(7) . 3_765 ? O1X Zr2X Zr1X 39.6(8) 4_565 3_765 ? O2X Zr2X Zr1X 88.1(8) . 3_765 ? O5X Zr2X Zr1X 109.7(6) 2_756 3_765 ? O5X Zr2X Zr1X 76.2(5) 3_766 3_765 ? O3X Zr2X Zr1X 162.7(5) . 3_765 ? O3X Zr2X Zr1X 115.7(4) 4_565 3_765 ? Zr1X Zr2X Zr1X 90.07(12) . 3_765 ? Zr1X Zr2X Zr1X 60.35(13) 4_565 3_765 ? Zr1X Zr2X Zr1X 59.69(13) 2_755 3_765 ? Zr1X O1X Zr2X 115.3(13) . . ? Zr1X O1X Zr1X 109.6(10) . 2_755 ? Zr2X O1X Zr1X 104.0(12) . 2_755 ? Zr1X O2X Zr1X 113.3(13) . 4_565 ? Zr1X O2X Zr2X 110.5(13) . . ? Zr1X O2X Zr2X 110.5(13) 4_565 . ? Zr1X O2AX Zr1X 113.1(12) 4_565 . ? Zr1X O2AX Zr2X 113.6(10) 4_565 3_765 ? Zr1X O2AX Zr2X 113.6(10) . 3_765 ? C1 O3X Zr2X 122.8(13) . . ? C1 O4X Zr1X 145(2) . . ? C31 O5X Zr2X 129.4(13) . 3_766 ? C31 O6X O7X 153(3) . 2_656 ? C31 O6X Zr1X 136.8(17) . 1_556 ? O7X O6X Zr1X 54.1(14) 2_656 1_556 ? O6X O7X C21 167(2) 2_656 . ? O6X O7X Zr1X 94.6(18) 2_656 2_655 ? C21 O7X Zr1X 73.6(10) . 2_655 ? C21 O8X Zr1X 64.5(12) . 2_655 ? C32 O9X Zr1X 110.9(10) . . ? O2Y Zr1Y O8Y 98.2(9) . . ? O2Y Zr1Y O9Y 82.8(9) . . ? O8Y Zr1Y O9Y 80.1(10) . . ? O2Y Zr1Y O1Y 68.8(7) . . ? O8Y Zr1Y O1Y 83.6(11) . . ? O9Y Zr1Y O1Y 144.8(7) . . ? O2Y Zr1Y O1AY 105.6(12) . . ? O8Y Zr1Y O1AY 129.7(11) . . ? O9Y Zr1Y O1AY 145.5(9) . . ? O1Y Zr1Y O1AY 65.6(10) . . ? O2Y Zr1Y C1 140.7(8) . . ? O8Y Zr1Y C1 42.7(5) . . ? O9Y Zr1Y C1 85.4(8) . . ? O1Y Zr1Y C1 103.2(8) . . ? O1AY Zr1Y C1 105.2(10) . . ? O2Y Zr1Y O7Y 173.5(9) . . ? O8Y Zr1Y O7Y 82.6(8) . . ? O9Y Zr1Y O7Y 103.7(9) . . ? O1Y Zr1Y O7Y 104.9(9) . . ? O1AY Zr1Y O7Y 69.3(12) . . ? C1 Zr1Y O7Y 41.1(5) . . ? C1 Zr1Y O2Y 145.9(7) . 2_755 ? C1 Zr1Y O5Y 73.4(6) . 2_655 ? C1 Zr1Y O4Y 83.0(8) . 2_756 ? C1 Zr1Y Zr1Y 102.5(3) . 4_565 ? O2Y Zr1Y Zr2Y 35.0(6) . . ? O8Y Zr1Y Zr2Y 89.4(6) . . ? O9Y Zr1Y Zr2Y 114.6(6) . . ? O1Y Zr1Y Zr2Y 33.9(5) . . ? O1AY Zr1Y Zr2Y 86.0(8) . . ? C1 Zr1Y Zr2Y 125.8(3) . . ? O7Y Zr1Y Zr2Y 138.8(7) . . ? O2Y Zr1Y Zr2Y 88.0(6) 2_755 . ? O5Y Zr1Y Zr2Y 68.0(5) 2_655 . ? O4Y Zr1Y Zr2Y 150.9(8) 2_756 . ? Zr1Y Zr1Y Zr2Y 60.08(6) 4_565 . ? O1AY Zr2Y O1Y 100.4(13) 3_765 . ? O1AY Zr2Y O2Y 70.5(9) 3_765 . ? O1Y Zr2Y O2Y 65.5(7) . . ? O6Y Zr2Y O2Y 139.4(9) 3_665 . ? O6Y Zr2Y O2Y 78.2(8) 2_655 . ? O2Y Zr2Y O2Y 108.1(11) 4_565 . ? O1AY Zr2Y Zr1Y 85.9(8) 3_765 . ? O1Y Zr2Y Zr1Y 33.2(4) . . ? O6Y Zr2Y Zr1Y 111.7(5) 3_665 . ? O6Y Zr2Y Zr1Y 77.0(4) 2_655 . ? O2Y Zr2Y Zr1Y 87.9(6) 4_565 . ? O2Y Zr2Y Zr1Y 32.4(7) . . ? O3Y Zr2Y Zr1Y 162.1(5) 4_564 . ? O3Y Zr2Y Zr1Y 114.9(4) 1_554 . ? Zr1Y O1Y Zr2Y 112.9(7) . . ? Zr1Y O1Y Zr2Y 112.9(7) 4_565 . ? Zr1Y O1AY Zr1Y 113.6(13) 4_565 . ? Zr1Y O2Y Zr2Y 112.6(10) . . ? C31 O3Y Zr2Y 126.0(12) . 1_556 ? C31 O4Y Zr1Y 131(2) . 2_756 ? O8Y O5Y C21 131(2) 2_655 . ? C21 O5Y Zr1Y 134.3(16) . 2_655 ? C21 O6Y Zr2Y 130.6(13) . 3_665 ? C1 O7Y Zr1Y 68.1(11) . . ? O5Y O8Y C1 151(2) 2_655 . ? O5Y O8Y Zr1Y 86.5(19) 2_655 . ? C1 O8Y Zr1Y 69.9(10) . . ? C32 O9Y Zr1Y 112.3(11) . . ? O8Z Zr1Z O9Z 78.5(10) 2_756 . ? O8Z Zr1Z O2Z 81.1(11) 2_756 . ? O9Z Zr1Z O2Z 147.3(8) . . ? O1Z Zr1Z O2Z 107.9(12) 2_755 . ? O8Z Zr1Z O2AZ 126.9(15) 2_756 . ? O9Z Zr1Z O2AZ 145.6(9) . . ? O1Z Zr1Z O2AZ 72.0(15) 2_755 . ? O2Z Zr1Z O2AZ 66.5(6) . . ? O8Z Zr1Z O1Z 98.9(10) 2_756 . ? O9Z Zr1Z O1Z 86.5(8) . . ? O1Z Zr1Z O1Z 69.3(10) 2_755 . ? O2Z Zr1Z O1Z 71.5(12) . . ? O2AZ Zr1Z O1Z 108.4(14) . . ? C31 Zr1Z O7Z 40.6(5) 2_756 2_756 ? O8Z Zr1Z O4Z 27.9(7) 2_756 . ? O9Z Zr1Z O4Z 75.3(9) . . ? O1Z Zr1Z O4Z 136.7(9) 2_755 . ? O2Z Zr1Z O4Z 74.7(8) . . ? O2AZ Zr1Z O4Z 138.4(10) . . ? O1Z Zr1Z O4Z 71.1(10) . . ? C31 Zr1Z O4Z 71.7(6) 2_756 . ? O7Z Zr1Z O4Z 111.4(8) 2_756 . ? C31 Zr1Z O6Z 84.1(7) 2_756 1_655 ? C31 Zr1Z Zr1Z 167.2(3) 2_756 2_755 ? O8Z Zr1Z Zr2Z 88.4(6) 2_756 . ? O9Z Zr1Z Zr2Z 116.9(6) . . ? O1Z Zr1Z Zr2Z 89.3(8) 2_755 . ? O2Z Zr1Z Zr2Z 36.8(10) . . ? O2AZ Zr1Z Zr2Z 89.2(8) . . ? O1Z Zr1Z Zr2Z 34.8(6) . . ? C31 Zr1Z Zr2Z 125.0(3) 2_756 . ? O7Z Zr1Z Zr2Z 137.6(7) 2_756 . ? O4Z Zr1Z Zr2Z 66.8(5) . . ? O6Z Zr1Z Zr2Z 150.4(7) 1_655 . ? Zr1Z Zr1Z Zr2Z 60.55(10) 2_755 . ? O1Z Zr2Z O2Z 69.4(11) . . ? O1Z Zr2Z O2Z 69.4(11) 4_565 . ? O1Z Zr2Z O3Z 80.9(9) . . ? O1Z Zr2Z O3Z 142.2(11) 4_565 . ? O2Z Zr2Z O3Z 79.0(8) . . ? O1Z Zr2Z Zr1Z 34.6(10) . . ? O1Z Zr2Z Zr1Z 88.8(8) 4_565 . ? O2Z Zr2Z Zr1Z 34.9(4) . . ? O3Z Zr2Z Zr1Z 75.9(4) . . ? O3Z Zr2Z Zr1Z 110.8(4) 4_565 . ? O2AZ Zr2Z Zr1Z 88.8(8) 3_765 . ? O5Z Zr2Z Zr1Z 161.8(5) 3_665 . ? O5Z Zr2Z Zr1Z 115.0(4) 2_655 . ? Zr1Z Zr2Z Zr1Z 60.43(12) 4_565 . ? Zr1Z O1Z Zr1Z 110.6(10) 2_755 . ? Zr1Z O1Z Zr2Z 112.3(14) 2_755 . ? Zr1Z O1Z Zr2Z 110.6(14) . . ? Zr1Z O2Z Zr2Z 108.3(13) . . ? Zr1Z O2Z Zr2Z 108.3(13) 4_565 . ? C1 O3Z Zr2Z 129.9(14) . . ? C1 O4Z O8Z 152(3) . 2_756 ? C1 O4Z Zr1Z 131.3(18) . . ? O8Z O4Z Zr1Z 51.6(15) 2_756 . ? C21 O5Z Zr2Z 123.3(14) . 3_665 ? C21 O6Z Zr1Z 123(2) . 1_455 ? C31 O7Z Zr1Z 69.1(10) . 2_756 ? O4Z O8Z C31 171(3) 2_756 . ? C31 O8Z Zr1Z 73.1(10) . 2_756 ? C32 O9Z Zr1Z 110.5(13) . . ? 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 C7 C2 C3 C4 -2(4) . . . . ? C1 C2 C3 C4 -177(2) . . . . ? C2 C3 C4 C5 -2(5) . . . . ? C3 C4 C5 C6 13(4) . . . . ? C3 C4 C5 C8 -179(2) . . . . ? C4 C5 C6 C7 -20(4) . . . . ? C8 C5 C6 C7 172(2) . . . . ? C3 C2 C7 C6 -4(4) . . . . ? C1 C2 C7 C6 170(2) . . . . ? C5 C6 C7 C2 16(5) . . . . ? C7B C2 C3B C4B -0.2(3) . . . . ? C1 C2 C3B C4B 178.3(10) . . . . ? C6B C5 C4B C3B 0.5(6) . . . . ? C8 C5 C4B C3B 178.2(11) . . . . ? C2 C3B C4B C5 -0.2(3) . . . . ? C4B C5 C6B C7B -0.4(9) . . . . ? C8 C5 C6B C7B -178.1(12) . . . . ? C3B C2 C7B C6B 0.3(6) . . . . ? C1 C2 C7B C6B -178.3(10) . . . . ? C5 C6B C7B C2 0.0(9) . . . . ? C6B C5 C8 C8 -123.8(10) . . . 4_575 ? C4B C5 C8 C8 58.5(12) . . . 4_575 ? C4 C5 C8 C8 124.9(17) . . . 4_575 ? C6 C5 C8 C8 -67(2) . . . 4_575 ? C6B C5 C8 C9 54.4(15) . . . . ? C4B C5 C8 C9 -123.3(12) . . . . ? C4 C5 C8 C9 -57(2) . . . . ? C6 C5 C8 C9 111(2) . . . . ? C8 C8 C9 C10 -0.7(13) 4_575 . . . ? C5 C8 C9 C10 -179.0(11) . . . . ? C8 C9 C10 C11 -177.7(10) . . . . ? C8 C9 C10 C10 0.7(13) . . . 4_575 ? C9 C10 C11 C22 122.9(11) . . . . ? C10 C10 C11 C22 -55.5(8) 4_575 . . . ? C9 C10 C11 C12 -124.0(11) . . . . ? C10 C10 C11 C12 57.5(8) 4_575 . . . ? C10 C11 C12 C13 123.0(11) . . . . ? C22 C11 C12 C13 -121.6(11) . . . . ? C10 C11 C12 C12 -57.6(8) . . . 4_575 ? C22 C11 C12 C12 57.8(8) . . . 4_575 ? C12 C12 C13 C14 0.8(14) 4_575 . . . ? C11 C12 C13 C14 -179.8(11) . . . . ? C12 C13 C14 C14 -0.8(14) . . . 4_575 ? C12 C13 C14 C15 176.8(12) . . . . ? C14 C14 C15 C20B 121.0(11) 4_575 . . . ? C13 C14 C15 C20B -56.5(17) . . . . ? C14 C14 C15 C16 -124.5(17) 4_575 . . . ? C13 C14 C15 C16 58(2) . . . . ? C14 C14 C15 C16B -61.2(13) 4_575 . . . ? C13 C14 C15 C16B 121.3(13) . . . . ? C14 C14 C15 C20 69(2) 4_575 . . . ? C13 C14 C15 C20 -109(2) . . . . ? C14 C15 C16 C17 -176(3) . . . . ? C20 C15 C16 C17 -8(4) . . . . ? C15 C16 C17 C18 -9(5) . . . . ? C16 C17 C18 C19 15(5) . . . . ? C16 C17 C18 C21 -176(2) . . . . ? C17 C18 C19 C20 -3(4) . . . . ? C21 C18 C19 C20 -171(2) . . . . ? C18 C19 C20 C15 -16(4) . . . . ? C16 C15 C20 C19 21(4) . . . . ? C14 C15 C20 C19 -171(2) . . . . ? C20B C15 C16B C17B 0.0(3) . . . . ? C14 C15 C16B C17B -178.1(12) . . . . ? C15 C16B C17B C18 -0.3(3) . . . . ? C19B C18 C17B C16B 0.8(7) . . . . ? C21 C18 C17B C16B 179.4(9) . . . . ? C17B C18 C19B C20B -0.9(9) . . . . ? C21 C18 C19B C20B -179.6(10) . . . . ? C18 C19B C20B C15 0.7(10) . . . . ? C16B C15 C20B C19B -0.3(7) . . . . ? C14 C15 C20B C19B 177.7(14) . . . . ? C10 C11 C22 C23 -122.7(13) . . . . ? C12 C11 C22 C23 123.8(12) . . . . ? C10 C11 C22 C22 55.6(9) . . . 4_575 ? C12 C11 C22 C22 -57.8(8) . . . 4_575 ? C22 C22 C23 C24 1.4(16) 4_575 . . . ? C11 C22 C23 C24 179.6(12) . . . . ? C22 C23 C24 C24 -1.4(16) . . . 4_575 ? C22 C23 C24 C25 -179.9(12) . . . . ? C24 C24 C25 C30 122.0(10) 4_575 . . . ? C23 C24 C25 C30 -59.5(17) . . . . ? C24 C24 C25 C30B 57.6(12) 4_575 . . . ? C23 C24 C25 C30B -123.9(13) . . . . ? C24 C24 C25 C26B -122.4(9) 4_575 . . . ? C23 C24 C25 C26B 56.1(16) . . . . ? C24 C24 C25 C26 -59.6(12) 4_575 . . . ? C23 C24 C25 C26 118.9(14) . . . . ? C30 C25 C26 C27 0.1(3) . . . . ? C24 C25 C26 C27 -178.3(11) . . . . ? C25 C26 C27 C28 -0.1(3) . . . . ? C26 C27 C28 C29 0.3(6) . . . . ? C26 C27 C28 C31 -175.7(11) . . . . ? C27 C28 C29 C30 -0.4(9) . . . . ? C31 C28 C29 C30 175.5(12) . . . . ? C26 C25 C30 C29 -0.2(6) . . . . ? C24 C25 C30 C29 178.1(12) . . . . ? C28 C29 C30 C25 0.4(9) . . . . ? C30B C25 C26B C27B -0.2(3) . . . . ? C24 C25 C26B C27B 179.9(11) . . . . ? C29B C28 C27B C26B 0.4(6) . . . . ? C31 C28 C27B C26B -178.5(9) . . . . ? C25 C26B C27B C28 -0.2(3) . . . . ? C27B C28 C29B C30B -0.3(10) . . . . ? C31 C28 C29B C30B 178.6(10) . . . . ? C26B C25 C30B C29B 0.3(7) . . . . ? C24 C25 C30B C29B -179.8(11) . . . . ? C28 C29B C30B C25 -0.1(10) . . . . ? O4X C1 O3X Zr2X 25.6(13) . . . . ? C2 C1 O3X Zr2X -154.8(11) . . . . ? O3X C1 O4X Zr1X 29(3) . . . . ? C2 C1 O4X Zr1X -151(3) . . . . ? O6X C31 O5X Zr2X -41(3) . . . 3_766 ? C28 C31 O5X Zr2X 165.4(12) . . . 3_766 ? O5X C31 O6X O7X -73(6) . . . 2_656 ? C28 C31 O6X O7X 81(6) . . . 2_656 ? O5X C31 O6X Zr1X 30(3) . . . 1_556 ? C28 C31 O6X Zr1X -176.8(18) . . . 1_556 ? O8X C21 O7X O6X -44(10) . . . 2_656 ? C18 C21 O7X O6X 135(10) . . . 2_656 ? Zr1X C21 O7X O6X -21(10) 2_655 . . 2_656 ? O8X C21 O7X Zr1X -23.3(9) . . . 2_655 ? C18 C21 O7X Zr1X 156.5(7) . . . 2_655 ? O7X C21 O8X Zr1X 21.2(8) . . . 2_655 ? C18 C21 O8X Zr1X -158.6(7) . . . 2_655 ? O9X C32 O9X Zr1X -0.4(7) 2_755 . . . ? O4Y C31 O3Y Zr2Y 21.9(15) . . . 1_556 ? C28 C31 O3Y Zr2Y -158.1(12) . . . 1_556 ? O3Y C31 O4Y Zr1Y 27(2) . . . 2_756 ? C28 C31 O4Y Zr1Y -153.0(19) . . . 2_756 ? O6Y C21 O5Y O8Y -91(3) . . . 2_655 ? C18 C21 O5Y O8Y 88(3) . . . 2_655 ? O6Y C21 O5Y Zr1Y -2.3(19) . . . 2_655 ? C18 C21 O5Y Zr1Y 176.6(17) . . . 2_655 ? O5Y C21 O6Y Zr2Y -11.9(14) . . . 3_665 ? C18 C21 O6Y Zr2Y 169.2(12) . . . 3_665 ? O8Y C1 O7Y Zr1Y 22.9(9) . . . . ? C2 C1 O7Y Zr1Y -157.0(8) . . . . ? O7Y C1 O8Y O5Y -60(5) . . . 2_655 ? C2 C1 O8Y O5Y 120(5) . . . 2_655 ? Zr1Y C1 O8Y O5Y -37(5) . . . 2_655 ? O7Y C1 O8Y Zr1Y -23.4(9) . . . . ? C2 C1 O8Y Zr1Y 156.5(8) . . . . ? O9Y C32 O9Y Zr1Y 0.8(7) 2_755 . . . ? O4Z C1 O3Z Zr2Z -35(3) . . . . ? C2 C1 O3Z Zr2Z 168.5(10) . . . . ? O3Z C1 O4Z O8Z -59(7) . . . 2_756 ? C2 C1 O4Z O8Z 100(6) . . . 2_756 ? O3Z C1 O4Z Zr1Z 25(3) . . . . ? C2 C1 O4Z Zr1Z -176.3(16) . . . . ? O6Z C21 O5Z Zr2Z 25.5(15) . . . 3_665 ? C18 C21 O5Z Zr2Z -155.6(11) . . . 3_665 ? O5Z C21 O6Z Zr1Z 22(2) . . . 1_455 ? C18 C21 O6Z Zr1Z -156.5(16) . . . 1_455 ? C28 C31 O7Z Zr1Z -161.0(8) . . . 2_756 ? O8Z C31 O7Z Zr1Z 19.0(8) . . . 2_756 ? O7Z C31 O8Z Zr1Z -20.1(9) . . . 2_756 ? C28 C31 O8Z Zr1Z 159.8(8) . . . 2_756 ? O9Z C32 O9Z Zr1Z -1.2(8) 2_755 . . . ? _refine_diff_density_max 0.617 _refine_diff_density_min -0.889 _refine_diff_density_rms 0.111 _shelx_res_file ; TITL P2m_a.res in P2/m p2m_a_sq.res created by SHELXL-2018/3 at 16:35:33 on 09-Apr-2019 REM Yadorkari-X generated CELL 1.54178 21.6317 12.2815 21.6273 90.0000 119.9750 90.0000 ZERR 1.0 0.0010 0.0005 0.0010 0.0000 0.0020 0.0000 LATT 1 SYMM -X, +Y, -Z REM SPGR P2/m monoclinic SFAC C H O Zr UNIT 88.5 45.2 36 6 TEMP -173.1 L.S. 50 FMAP 2 PLAN -15 ACTA CONF LIST 4 BOND $H MERG 2 OMIT -4 1 1 OMIT 1 3 2 OMIT -1 1 3 OMIT 0 1 6 OMIT -3 1 4 OMIT -8 5 5 OMIT -8 5 3 OMIT 0 0 3 OMIT -2 3 3 OMIT -1 1 4 OMIT -2 2 2 OMIT 1 1 3 fmap 2 ISOR 0.03 0.06 RIGU 0.03 0.06 SIMU 0.04 0.08 SADI 0.02 C1 C3 C1 C7 C21 C17 C21 C19 C31 C29 C31 C27 SADI 0.02 C5 C4 C5 C4B C5 C6 C5 C6B SADI 0.02 C2 C3 C2 C3B C2 C7 C2 C7B SADI 0.02 C3 C4 C3B C4B C6 C7 C6B C7B SADI 0.02 C3 C3B C4 C4B C6 C6B C7 C7B SADI 0.02 C2 C4B C2 C6B C5 C3B C5 C7B SADI 0.02 C3B C7B C4B C6B C3 C7 C4 C6 SADI 0.02 C18 C17 C18 C17B C18 C19 C18 C19B SADI 0.02 C15 C16 C15 C16B C15 C20 C15 C20B SADI 0.02 C25 C26 C25 C26B C25 C30 C25 C30B SADI 0.02 C28 C27 C28 C27B C28 C29 C28 C29B SADI 0.02 C26 C27 C26B C27B C29 C30 C29B C30B SADI 0.02 C26 C30B C29 C29B C26 C26B C27 C27B SADI 0.02 C26B C30 C26 C30B C27B C29 C27 C29B SADI 0.02 C28 O7Z C28 O8Z SADI 0.02 C21 O7X C21 O8X C1 O7Y C1 O8Y C31 O7Z C31 O8Z SADI 0.02 C1 O3X C1 O4X C31 O5X C31 O6X SADI 0.02 C21 O5Y C21 O6Y C31 O3Y C31 O4Y SADI 0.02 C1 O3Z C1 O4Z C21 O5Z C21 O6Z SADI 0.02 Zr2X O1X Zr2Y O1Y Zr2Z O1Z SADI 0.02 Zr1X O2X Zr1X O2AX Zr1Y O1Y Zr1Y O1AY Zr1Z O2Z Zr1Z O2AZ SADI 0.02 O1X O2X O1Y O2Y O2Z O2AZ FLAT 0.01 C2 C3B C4B C5 C6B C7B FLAT 0.01 C15 C16B C17B C18 C19B C20B FLAT 0.01 C25 C26 C27 C28 C29 C30 FLAT 0.01 C25 C26B C27B C28 C29B C30B FLAT 0.02 O7X O8X C21 C18 FLAT 0.02 C18 C21 O5Z O6Z FLAT 0.02 C28 C31 O3Y O4Y FLAT 0.02 C18 C21 O5Y O6Y FLAT 0.02 C28 C31 O7Z O8Z FLAT 0.02 C1 C2 O7Y O8Y FLAT 0.02 C1 C2 O3X O4X ABIN WGHT 0.200000 FVAR 0.28845 0.70625 C1 1 0.895877 0.680606 0.100629 21.00000 0.09066 0.13118 = 0.11933 -0.00336 0.07562 -0.01539 C2 1 0.864851 0.750891 0.137483 21.00000 0.16927 0.12151 = 0.14614 0.01766 0.08570 -0.01272 PART 4 C3 1 0.884953 0.737680 0.206995 20.50000 0.15537 0.12627 = 0.14492 0.00525 0.08141 0.00909 AFIX 43 H3 2 0.921048 0.686524 0.235403 20.50000 -1.20000 AFIX 0 C4 1 0.851751 0.800836 0.237449 20.50000 0.13902 0.12073 = 0.13437 -0.00875 0.08078 0.00702 AFIX 43 H4 2 0.864757 0.790069 0.285961 20.50000 -1.20000 PART 0 AFIX 0 C5 1 0.800935 0.877417 0.197189 21.00000 0.13972 0.10752 = 0.14077 -0.00539 0.08838 0.00591 PART 4 C6 1 0.771817 0.876750 0.123671 20.50000 0.17091 0.14275 = 0.14536 -0.00238 0.09362 0.02456 AFIX 43 H6 2 0.727495 0.911423 0.093328 20.50000 -1.20000 AFIX 0 C7 1 0.809965 0.822893 0.094906 20.50000 0.15137 0.15299 = 0.14039 0.00442 0.10823 0.02227 AFIX 43 H7 2 0.798166 0.835836 0.046927 20.50000 -1.20000 PART 5 AFIX 0 C3B 1 0.905069 0.827832 0.189651 20.50000 0.15881 0.14260 = 0.15331 -0.01479 0.10267 0.00102 AFIX 43 H3B 2 0.954217 0.837457 0.204921 20.50000 -1.20000 AFIX 0 C4B 1 0.872199 0.891545 0.219734 20.50000 0.17357 0.15342 = 0.15902 -0.01029 0.08327 -0.01380 AFIX 43 H4B 2 0.899302 0.943988 0.255440 20.50000 -1.20000 AFIX 0 C6B 1 0.761616 0.801214 0.146047 20.50000 0.15347 0.11656 = 0.13217 -0.00236 0.08556 0.00817 AFIX 43 H6B 2 0.712505 0.791396 0.130878 20.50000 -1.20000 AFIX 0 C7B 1 0.794674 0.736616 0.115627 20.50000 0.14512 0.11328 = 0.14274 -0.00037 0.08563 -0.00290 AFIX 43 H7B 2 0.767577 0.683816 0.080194 20.50000 -1.20000 PART 0 AFIX 0 C8 1 0.768685 0.943689 0.231594 21.00000 0.11814 0.10363 = 0.11848 -0.00370 0.07602 0.00058 C9 1 0.734406 0.884217 0.264377 21.00000 0.10832 0.09099 = 0.10688 0.00482 0.05895 0.00001 AFIX 43 H9 2 0.734019 0.806870 0.263796 21.00000 -1.20000 AFIX 0 C10 1 0.702530 0.939756 0.296234 21.00000 0.07770 0.07814 = 0.06950 -0.00444 0.03664 0.00083 C11 1 0.667970 0.895447 0.333751 21.00000 0.09293 0.07326 = 0.09050 0.00474 0.03845 0.00398 AFIX 13 H11 2 0.667950 0.814024 0.333797 21.00000 -1.20000 AFIX 0 C12 1 0.593084 0.941712 0.296759 21.00000 0.08532 0.07368 = 0.06940 -0.00610 0.03587 -0.01042 C13 1 0.529377 0.884700 0.265824 21.00000 0.11029 0.07338 = 0.10888 -0.00050 0.04649 0.00435 AFIX 43 H13 2 0.529699 0.807356 0.266528 21.00000 -1.20000 AFIX 0 C14 1 0.463100 0.942321 0.232815 21.00000 0.10233 0.08984 = 0.13509 -0.00370 0.05567 -0.00746 C15 1 0.398909 0.878218 0.198338 21.00000 0.10812 0.10601 = 0.15033 -0.00354 0.04707 0.00388 PART 4 C16 1 0.384926 0.798368 0.237998 20.50000 0.11344 0.12602 = 0.13420 0.00115 0.06303 -0.01607 AFIX 43 H16 2 0.416858 0.791401 0.287844 20.50000 -1.20000 AFIX 0 C17 1 0.326531 0.731942 0.205561 20.50000 0.13995 0.11930 = 0.14826 0.00354 0.05377 -0.02461 AFIX 43 H17 2 0.321243 0.672386 0.230572 20.50000 -1.20000 PART 0 AFIX 0 C18 1 0.276235 0.752881 0.136826 21.00000 0.15946 0.12219 = 0.14940 0.00469 0.06208 -0.00362 PART 4 C19 1 0.284680 0.819840 0.090272 20.50000 0.13078 0.11060 = 0.14124 0.02001 0.04729 -0.02029 AFIX 43 H19 2 0.248577 0.829986 0.041935 20.50000 -1.20000 AFIX 0 C20 1 0.353368 0.873086 0.121692 20.50000 0.13004 0.12536 = 0.15330 -0.00287 0.05198 -0.02395 AFIX 43 H20 2 0.368762 0.905052 0.091674 20.50000 -1.20000 PART 5 AFIX 0 C16B 1 0.347042 0.887169 0.220925 20.50000 0.13383 0.14441 = 0.16418 -0.02192 0.04669 -0.02008 AFIX 43 H16B 2 0.354338 0.936927 0.257604 20.50000 -1.20000 AFIX 0 C17B 1 0.288807 0.825676 0.190394 20.50000 0.13154 0.13377 = 0.16066 -0.03290 0.05142 -0.02446 AFIX 43 H17B 2 0.254875 0.832000 0.205876 20.50000 -1.20000 AFIX 0 C19B 1 0.321993 0.737236 0.111705 20.50000 0.12048 0.10430 = 0.14667 -0.03289 0.06517 -0.01020 AFIX 43 H19B 2 0.313683 0.686359 0.075258 20.50000 -1.20000 AFIX 0 C20B 1 0.379463 0.800276 0.143282 20.50000 0.12334 0.10432 = 0.14462 -0.01814 0.05407 0.01064 AFIX 43 H20B 2 0.412308 0.791956 0.126570 20.50000 -1.20000 PART 0 AFIX 0 C21 1 0.206072 0.679108 0.101684 21.00000 0.09446 0.12916 = 0.11517 0.00447 0.04188 0.02317 C22 1 0.703723 0.941531 0.408233 21.00000 0.08980 0.07349 = 0.06806 0.00613 0.03729 0.00077 C23 1 0.735099 0.885774 0.470561 21.00000 0.13530 0.09382 = 0.07268 -0.00232 0.04113 0.00275 AFIX 43 H23 2 0.735826 0.808440 0.470205 21.00000 -1.20000 AFIX 0 C24 1 0.766899 0.942779 0.536420 21.00000 0.14686 0.09832 = 0.07193 0.00577 0.03664 0.00080 C25 1 0.801260 0.874272 0.604213 21.00000 0.13582 0.10481 = 0.09955 0.00307 0.04239 0.01326 PART 4 C26 1 0.874070 0.885962 0.651858 20.50000 0.15465 0.13102 = 0.10531 0.00376 0.02751 0.01278 AFIX 43 H26 2 0.901417 0.937242 0.642719 20.50000 -1.20000 AFIX 0 C27 1 0.906187 0.821821 0.712829 20.50000 0.15769 0.14292 = 0.10580 0.01921 0.05358 -0.00819 AFIX 43 H27 2 0.955840 0.829688 0.745310 20.50000 -1.20000 PART 0 AFIX 0 C28 1 0.867182 0.746133 0.727434 21.00000 0.14904 0.13027 = 0.12528 -0.01306 0.05295 -0.01662 PART 4 C29 1 0.796046 0.738681 0.678334 20.50000 0.14409 0.11406 = 0.12486 0.01977 0.03880 -0.01666 AFIX 43 H29 2 0.768538 0.687196 0.687097 20.50000 -1.20000 AFIX 0 C30 1 0.761079 0.800914 0.616575 20.50000 0.15720 0.11825 = 0.10825 0.02492 0.05563 -0.02769 AFIX 43 H30 2 0.711390 0.792855 0.584317 20.50000 -1.20000 PART 5 AFIX 0 C26B 1 0.853766 0.799585 0.615869 20.50000 0.13210 0.12287 = 0.10778 0.00816 0.04781 0.03521 AFIX 43 H26B 2 0.867703 0.791988 0.580821 20.50000 -1.20000 AFIX 0 C27B 1 0.886881 0.735412 0.676457 20.50000 0.14348 0.10727 = 0.11477 0.00639 0.04473 0.01392 AFIX 43 H27B 2 0.922710 0.684694 0.682688 20.50000 -1.20000 AFIX 0 C29B 1 0.813341 0.822999 0.712986 20.50000 0.17074 0.13881 = 0.10342 0.00728 0.03351 0.00793 AFIX 43 H29B 2 0.799195 0.830794 0.747865 20.50000 -1.20000 AFIX 0 C30B 1 0.779152 0.887993 0.653334 20.50000 0.17090 0.11851 = 0.11279 -0.00231 0.05745 0.00929 AFIX 43 H30B 2 0.743033 0.938490 0.646594 20.50000 -1.20000 PART 0 AFIX 0 C31 1 0.900818 0.682745 0.795496 21.00000 0.12489 0.12155 = 0.06748 -0.01836 0.04457 -0.00204 C32 1 11.000000 10.842200 10.000000 10.25000 0.14980 PART 1 ZR1X 4 0.905253 0.643224 -0.047039 10.33333 0.13757 0.09915 = 0.07738 0.01766 0.06357 0.03532 ZR2X 4 1.000230 0.500000 0.115527 10.16667 0.10965 0.06856 = 0.06752 0.00000 0.05436 0.00000 O1X 3 0.990239 0.642454 0.052625 10.33333 0.10640 O2X 3 0.907499 0.500000 0.007622 10.16667 0.09035 O2AX 3 0.912779 0.500000 -0.096565 10.16667 0.06159 O3X 3 0.913247 0.598912 0.124108 10.33333 0.09831 O4X 3 0.902027 0.705659 0.051244 10.33333 0.18139 O5X 3 0.925381 0.603744 0.794680 10.33333 0.10139 O6X 3 0.878503 0.700975 0.835047 10.33333 0.14731 O7X 3 0.166148 0.690213 0.143900 10.33333 0.14249 O8X 3 0.194659 0.617433 0.037331 10.33333 0.20942 O9X 3 0.920428 0.813844 -0.038917 10.33333 0.17189 0.09660 = 0.12589 0.03315 0.08607 0.03186 PART 2 ZR1Y 4 0.952628 0.643287 0.047163 10.33333 0.08634 0.09789 = 0.07852 -0.01394 0.01284 0.02067 ZR2Y 4 0.884416 0.500000 -0.115381 10.16667 0.06893 0.06925 = 0.06688 0.00000 0.00835 0.00000 O1Y 3 0.903358 0.500000 -0.008541 10.16667 0.07996 O1AY 3 1.009454 0.500000 0.095800 10.16667 0.07872 O2Y 3 0.940507 0.644564 -0.052907 10.33333 0.09596 O3Y 3 0.877318 0.599103 0.791664 10.33333 0.09691 O4Y 3 0.949975 0.723652 0.849246 10.33333 0.18751 O5Y 3 0.159377 0.710195 0.039868 10.33333 0.13718 O6Y 3 0.204068 0.605771 0.133673 10.33333 0.09316 O7Y 3 0.963436 0.622254 0.150884 10.33333 0.17395 O8Y 3 0.849177 0.687496 0.019520 10.33333 0.14904 O9Y 3 0.959265 0.811355 0.038406 10.33333 0.17348 0.09897 = 0.13309 -0.00020 0.06586 0.04056 PART 3 ZR1Z 4 1.046320 0.644284 0.093270 10.33333 0.08742 0.09776 = 0.13171 -0.03210 0.06465 -0.01603 ZR2Z 4 0.884524 0.500000 0.000403 10.16667 0.07835 0.06834 = 0.09761 0.00000 0.05302 0.00000 O1Z 3 0.943647 0.639335 -0.000995 10.33333 0.11964 O2Z 3 0.993600 0.500000 0.095406 10.16667 0.08160 O2AZ 3 1.102128 0.500000 0.097459 10.16667 0.09477 O3Z 3 0.868752 0.608133 0.074348 10.33333 0.08695 O4Z 3 0.954456 0.704834 0.123725 10.33333 0.14705 O5Z 3 0.211102 0.600075 0.087860 10.33333 0.09918 O6Z 3 0.161883 0.729464 0.099109 10.33333 0.20532 O7Z 3 0.851059 0.622756 0.812248 10.33333 0.18139 O8Z 3 0.983348 0.691249 0.837280 10.33333 0.14233 O9Z 3 1.041361 0.812413 0.080123 10.33333 0.13961 PART 0 HKLF 4 1 1 0 0 0 1 0 0 0 1 REM P2m_a.res in P2/m REM wR2 = 0.4298, GooF = S = 1.748, Restrained GooF = 1.671 for all data REM R1 = 0.1328 for 4046 Fo > 4sig(Fo) and 0.1602 for all 5932 data REM 559 parameters refined using 1613 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 0.617, deepest hole -0.889, 1-sigma level 0.111 Q1 1 0.2190 0.6262 0.1131 11.00000 0.05 0.62 Q2 1 1.0009 0.7090 0.0751 11.00000 0.05 0.44 Q3 1 0.8883 0.6324 0.1061 11.00000 0.05 0.44 Q4 1 0.3570 0.7334 0.2733 11.00000 0.05 0.37 Q5 1 0.8993 0.5000 0.0390 10.50000 0.05 0.34 Q6 1 0.4848 1.0000 0.2657 10.50000 0.05 0.33 Q7 1 0.8222 0.7224 0.1118 11.00000 0.05 0.32 Q8 1 0.3083 0.7015 0.1248 11.00000 0.05 0.31 Q9 1 0.4701 1.0000 0.2265 10.50000 0.05 0.31 Q10 1 0.8190 0.7225 0.7085 11.00000 0.05 0.30 Q11 1 0.4822 0.9006 0.2999 11.00000 0.05 0.28 Q12 1 0.7991 0.6160 0.6630 11.00000 0.05 0.28 Q13 1 0.9159 0.8826 -0.0795 11.00000 0.05 0.28 Q14 1 0.3972 0.8172 0.1771 11.00000 0.05 0.27 Q15 1 0.3373 0.9113 0.1191 11.00000 0.05 0.27 ; _shelx_res_checksum 78099 _shelx_hkl_file ; -1 0 0 0.00 0.10 2 0 0 1374.26 75.09 2 0 0 1280.07 75.19 2 0 0 1395.06 58.39 -2 0 0 1308.37 74.99 -2 0 0 1341.47 74.99 3 0 0 113.99 7.00 -3 0 0 103.89 6.80 -3 0 0 97.39 6.10 3 0 0 102.99 5.10 3 0 0 101.59 6.10 4 0 0 392.06 17.60 4 0 0 406.26 22.00 4 0 0 410.66 22.90 -4 0 0 361.96 21.90 -4 0 0 388.66 17.70 -4 0 0 357.56 22.50 5 0 0 689.73 38.50 5 0 0 660.13 37.30 5 0 0 645.14 29.60 -5 0 0 671.63 37.30 -5 0 0 636.04 37.90 -5 0 0 656.33 29.80 -6 0 0 688.53 43.50 6 0 0 781.92 34.30 -6 0 0 757.52 43.00 -6 0 0 730.23 34.50 6 0 0 772.22 43.00 6 0 0 842.02 44.50 7 0 0 25.40 3.80 -7 0 0 24.20 2.90 -7 0 0 24.20 2.40 -7 0 0 21.20 2.70 7 0 0 24.90 2.30 8 0 0 9.50 2.90 -9 0 0 71.49 4.20 -10 0 0 48.90 3.10 11 0 0 24.40 2.20 12 0 0 111.09 6.60 13 0 0 57.59 4.00 14 0 0 26.60 2.70 0 -1 0 3526.55 163.68 1 -1 0 4408.16 206.68 1 -1 0 4658.93 194.28 -1 -1 0 4309.47 192.98 -1 1 0 4460.55 248.38 2 -1 0 1526.55 68.89 2 -1 0 1558.34 82.59 2 -1 0 1522.75 83.09 2 -1 0 1433.56 64.59 -2 -1 0 1486.95 64.29 -2 1 0 1470.15 64.59 2 1 0 1501.25 64.19 -2 1 0 1296.07 82.59 -2 1 0 1533.75 82.89 3 -1 0 305.57 13.90 3 -1 0 285.57 13.30 3 -1 0 294.37 16.40 -3 -1 0 280.57 13.10 -3 1 0 275.07 13.40 3 1 0 284.17 13.00 -3 1 0 297.17 17.30 -3 1 0 286.97 16.50 4 -1 0 994.10 53.49 -4 -1 0 933.11 41.60 4 -1 0 933.11 41.80 4 -1 0 993.10 52.89 4 1 0 791.12 53.29 -4 1 0 978.60 53.99 -4 1 0 931.01 42.00 4 1 0 958.20 52.79 4 1 0 974.80 41.50 5 -1 0 69.49 5.10 5 -1 0 67.69 4.10 -5 -1 0 63.69 4.00 5 -1 0 58.19 3.90 -5 1 0 55.69 4.10 -5 1 0 58.59 5.70 5 1 0 62.39 5.60 5 1 0 62.79 4.20 -5 1 0 59.29 4.30 6 -1 0 17.50 2.70 6 -1 0 15.50 2.20 6 -1 0 18.80 1.80 -6 -1 0 19.40 2.30 6 1 0 14.90 3.40 -6 1 0 14.70 3.70 -6 1 0 16.70 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1.40 1.80 -3 2 -3 2.80 0.80 3 2 3 1.90 1.20 3 2 3 1.90 0.50 4 -2 3 30.30 2.40 4 -2 3 32.60 3.30 4 -2 3 31.40 2.70 -4 -2 -3 37.20 2.80 4 2 3 32.70 2.40 -4 2 -3 33.60 2.70 -4 2 -3 34.10 5.00 4 2 3 32.10 4.20 5 -2 3 19.10 1.90 -5 -2 -3 22.00 1.90 5 -2 3 22.60 2.40 -5 -2 -3 26.80 2.50 5 -2 3 17.20 2.70 5 2 3 18.60 3.90 5 2 3 21.90 1.90 -5 2 -3 19.00 4.40 -5 2 -3 21.30 2.20 -6 -2 -3 3.80 1.30 -6 -2 -3 4.90 1.30 6 -2 3 4.00 1.20 6 2 3 2.30 2.20 -6 2 -3 2.60 2.00 -7 -2 -3 177.58 8.30 7 -2 3 171.28 10.30 7 2 3 142.39 13.10 -7 2 -3 159.38 13.20 -8 -2 -3 6.80 1.30 -8 -2 -3 8.70 0.90 8 2 3 10.20 2.00 -9 -2 -3 1.20 0.30 -9 -2 -3 1.60 0.70 9 2 3 1.40 1.20 -10 -2 -3 6.60 1.30 -10 -2 -3 4.50 0.80 10 2 3 4.50 1.40 -11 -2 -3 21.30 1.90 -11 -2 -3 20.10 1.40 11 2 3 15.20 2.60 -12 -2 -3 12.10 1.10 -12 -2 -3 13.80 1.50 12 2 3 9.70 2.20 -13 -2 -3 6.20 1.30 13 2 3 1.40 1.00 14 2 3 -0.20 0.80 15 2 3 0.30 0.90 16 2 3 -0.30 1.10 20 3 -3 0.60 0.80 19 3 -3 0.70 1.00 19 3 -3 0.10 0.90 -18 -3 3 3.80 1.20 18 3 -3 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4 80.89 5.80 5 -3 -4 16.40 1.80 -5 -3 4 18.60 1.50 -5 3 4 13.10 2.00 -5 3 4 16.60 2.10 -4 -3 4 2.20 0.60 4 -3 -4 3.90 0.90 -4 3 4 2.60 0.80 -4 3 4 2.00 0.80 -3 -3 4 4.40 1.00 3 -3 -4 2.90 0.80 -3 3 4 3.20 0.90 -2 -3 4 65.69 3.60 2 -3 -4 71.59 3.70 -2 3 4 62.49 4.20 -2 3 4 66.89 4.00 2 3 -4 66.59 4.00 1 -3 -4 2.80 0.80 -1 -3 4 3.80 0.90 1 3 -4 3.70 1.40 1 3 -4 5.00 0.80 -1 3 4 2.10 0.50 -1 3 4 2.60 0.80 0 -3 -4 3.50 0.80 0 -3 4 2.30 0.80 0 3 4 2.00 0.50 0 3 -4 2.30 1.60 0 3 -4 3.40 0.90 -1 -3 -4 16.00 1.60 1 -3 4 14.00 1.80 1 3 4 15.50 1.10 -1 3 -4 18.80 3.60 -1 3 -4 16.40 1.70 -2 -3 -4 80.19 4.30 -2 -3 -4 67.89 4.70 2 -3 4 76.59 4.50 -2 3 -4 77.89 5.00 -2 3 -4 87.49 7.40 2 3 4 74.99 5.00 2 3 4 76.59 4.60 3 -3 4 54.69 3.60 -3 -3 -4 46.40 3.40 -3 -3 -4 51.69 3.30 3 3 4 48.90 3.20 3 3 4 42.90 4.00 -3 3 -4 46.10 6.20 -3 3 -4 49.00 3.60 4 -3 4 5.50 1.30 4 -3 4 3.40 1.10 -4 -3 -4 7.10 1.50 -4 -3 -4 7.30 1.70 4 3 4 6.70 1.00 -5 -3 -4 11.10 2.00 -5 -3 -4 13.40 1.00 -5 -3 -4 11.30 1.80 5 -3 4 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0.00 -15 9 14 -1.43 0.00 1 9 14 -0.23 0.00 -11 10 14 -0.01 0.00 -10 10 14 -0.52 0.00 -4 10 14 -0.10 0.00 -3 10 14 -0.14 0.00 -21 0 15 0.57 0.00 -20 0 15 -0.40 0.00 -19 0 15 0.10 0.00 -18 0 15 -0.21 0.00 -17 0 15 0.32 0.00 -16 0 15 0.12 0.00 -15 0 15 0.51 0.00 -14 0 15 -0.96 0.00 -21 1 15 -0.10 0.00 -20 1 15 0.13 0.00 -19 1 15 0.17 0.00 -18 1 15 -0.39 0.00 -17 1 15 -0.67 0.00 -16 1 15 -0.14 0.00 -21 2 15 0.34 0.00 -20 2 15 0.89 0.00 -19 2 15 0.26 0.00 -18 2 15 0.55 0.00 -17 2 15 0.12 0.00 -21 3 15 0.40 0.00 -20 3 15 -0.28 0.00 7 3 15 -0.19 0.00 -21 4 15 0.64 0.00 -18 7 15 -0.06 0.00 3 7 15 0.82 0.00 -16 8 15 -0.50 0.00 1 8 15 -0.48 0.00 -14 9 15 -0.17 0.00 -1 9 15 -0.59 0.00 -8 10 15 0.47 0.00 -7 10 15 0.52 0.00 -21 0 16 -0.49 0.00 -20 0 16 -0.28 0.00 -19 0 16 0.65 0.00 -18 0 16 0.17 0.00 -17 0 16 -0.76 0.00 -16 0 16 0.56 0.00 -15 0 16 -0.70 0.00 -21 1 16 -0.38 0.00 -20 1 16 0.25 0.00 -19 1 16 0.26 0.00 -18 1 16 -0.43 0.00 -17 1 16 -0.24 0.00 -16 1 16 0.93 0.00 6 1 16 -0.12 0.00 -21 2 16 -0.05 0.00 -20 2 16 -0.14 0.00 -19 2 16 -1.02 0.00 -18 2 16 0.01 0.00 -17 2 16 1.05 0.00 6 2 16 -0.16 0.00 -21 3 16 0.48 0.00 -20 3 16 -0.91 0.00 -19 3 16 -0.53 0.00 -18 3 16 -0.27 0.00 -21 4 16 -0.07 0.00 -20 4 16 -0.31 0.00 5 4 16 0.72 0.00 -20 5 16 -0.29 0.00 4 5 16 0.45 0.00 -19 6 16 -0.05 0.00 3 6 16 0.26 0.00 -15 8 16 -0.34 0.00 -1 8 16 -0.56 0.00 -12 9 16 0.46 0.00 -11 9 16 -0.23 0.00 -5 9 16 -0.14 0.00 -4 9 16 0.40 0.00 -21 0 17 0.34 0.00 -20 0 17 -0.27 0.00 -19 0 17 -0.74 0.00 -18 0 17 1.25 0.00 -17 0 17 -0.39 0.00 -16 0 17 1.21 0.00 -15 0 17 2.39 0.00 5 0 17 -0.40 0.00 -21 1 17 -0.05 0.00 -20 1 17 0.33 0.00 -19 1 17 -0.13 0.00 -18 1 17 0.30 0.00 -17 1 17 -0.60 0.00 -16 1 17 0.37 0.00 5 1 17 0.01 0.00 -21 2 17 -0.31 0.00 -20 2 17 0.27 0.00 -19 2 17 0.66 0.00 -18 2 17 -0.99 0.00 -17 2 17 -0.15 0.00 -21 3 17 0.52 0.00 -20 3 17 0.58 0.00 -19 3 17 0.06 0.00 4 3 17 0.97 0.00 -20 4 17 -0.52 0.00 -19 4 17 0.72 0.00 -18 6 17 -0.62 0.00 1 6 17 -0.43 0.00 -17 7 17 -0.59 0.00 0 7 17 -0.01 0.00 -14 8 17 -0.99 0.00 -3 8 17 -1.48 0.00 -21 0 18 0.05 0.00 -20 0 18 -0.57 0.00 -19 0 18 -0.38 0.00 -18 0 18 -0.48 0.00 -17 0 18 -0.72 0.00 -16 0 18 -0.03 0.00 -15 0 18 -0.22 0.00 -21 1 18 -0.46 0.00 -20 1 18 -0.34 0.00 -19 1 18 0.39 0.00 -18 1 18 0.22 0.00 -17 1 18 -0.62 0.00 -16 1 18 0.23 0.00 3 1 18 0.23 0.00 -21 2 18 -0.07 0.00 -20 2 18 -0.13 0.00 -19 2 18 0.27 0.00 -18 2 18 -1.24 0.00 3 2 18 0.07 0.00 -20 3 18 -0.68 0.00 -19 3 18 -0.25 0.00 -20 4 18 -0.38 0.00 2 4 18 0.16 0.00 -19 5 18 -0.63 0.00 1 5 18 -0.51 0.00 -17 6 18 0.79 0.00 -1 6 18 -0.05 0.00 -15 7 18 0.41 0.00 -5 7 18 1.78 0.00 -4 7 18 0.66 0.00 -3 7 18 0.14 0.00 -12 8 18 0.28 0.00 -11 8 18 0.49 0.00 -10 8 18 0.32 0.00 -9 8 18 0.60 0.00 -8 8 18 -0.25 0.00 -7 8 18 0.45 0.00 -6 8 18 -0.41 0.00 -21 0 19 0.20 0.00 -20 0 19 -0.49 0.00 -19 0 19 0.58 0.00 -18 0 19 -0.19 0.00 -17 0 19 0.07 0.00 -16 0 19 0.74 0.00 -15 0 19 -1.97 0.00 2 0 19 -0.90 0.00 -20 1 19 -0.48 0.00 -19 1 19 -0.05 0.00 -18 1 19 0.32 0.00 -17 1 19 -0.04 0.00 -20 2 19 -0.12 0.00 -19 2 19 0.26 0.00 -18 2 19 0.41 0.00 1 2 19 -0.84 0.00 -20 3 19 0.21 0.00 -19 3 19 0.29 0.00 1 3 19 -0.03 0.00 -19 4 19 1.13 0.00 0 4 19 1.60 0.00 -18 5 19 -0.32 0.00 -1 5 19 -0.12 0.00 -16 6 19 0.12 0.00 -4 6 19 -0.08 0.00 -3 6 19 -0.20 0.00 -13 7 19 -0.17 0.00 -12 7 19 -0.86 0.00 -7 7 19 -0.36 0.00 -6 7 19 -0.67 0.00 -20 0 20 0.36 0.00 -19 0 20 0.40 0.00 -18 0 20 0.01 0.00 -17 0 20 -0.12 0.00 -16 0 20 1.31 0.00 0 0 20 -1.87 0.00 -20 1 20 -0.12 0.00 -19 1 20 0.35 0.00 -18 1 20 0.23 0.00 -17 1 20 -0.10 0.00 0 1 20 -0.05 0.00 -19 2 20 0.18 0.00 -18 2 20 -0.07 0.00 -1 2 20 0.31 0.00 -19 3 20 -0.36 0.00 -1 3 20 -0.35 0.00 -18 4 20 0.12 0.00 -2 4 20 0.32 0.00 -16 5 20 0.15 0.00 -4 5 20 0.37 0.00 -14 6 20 -0.44 0.00 -13 6 20 0.29 0.00 -7 6 20 -0.03 0.00 -6 6 20 -0.44 0.00 -19 0 21 0.54 0.00 -18 0 21 -0.63 0.00 -17 0 21 1.22 0.00 -16 0 21 1.15 0.00 -2 0 21 0.16 0.00 -18 1 21 -0.18 0.00 -17 1 21 -0.15 0.00 -3 1 21 0.06 0.00 -18 2 21 0.29 0.00 -3 2 21 -0.22 0.00 -17 3 21 0.36 0.00 -4 3 21 0.54 0.00 -16 4 21 0.30 0.00 -5 4 21 0.24 0.00 -14 5 21 0.73 0.00 -13 5 21 0.09 0.00 -12 5 21 -0.61 0.00 -11 5 21 -0.34 0.00 -10 5 21 -0.35 0.00 -9 5 21 -0.41 0.00 -8 5 21 0.21 0.00 -7 5 21 0.43 0.00 -17 0 22 0.03 0.00 -16 0 22 1.07 0.00 -15 0 22 1.71 0.00 -5 0 22 0.62 0.00 -17 1 22 0.80 0.00 -16 1 22 -0.39 0.00 -6 1 22 0.13 0.00 -5 1 22 0.19 0.00 -16 2 22 0.51 0.00 -6 2 22 0.07 0.00 -15 3 22 1.24 0.00 -14 3 22 0.31 0.00 -8 3 22 -0.25 0.00 -7 3 22 0.38 0.00 -12 4 22 0.09 0.00 -11 4 22 -1.04 0.00 -10 4 22 0.28 0.00 0 0 0 0.00 0.00 # SQUEEZE RESULTS # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 136 21 ' ' 2 -0.002 -0.101 0.477 2545 508 ' ' _platon_squeeze_void_probe_radius 1.20 _platon_squeeze_details (replace by semicolon in column 1 when used as .sqf) TITL P2m_a P 2/m R = 0.23 CELL 21.6317 12.2815 21.6273 90.00 119.97 90.00 SPGR P2/m # Solvent Accessible Volume = 2686.1 # Electrons Found in S.A.V. = 525.2 # Note: Atoms in Void as Cxxx and Qxxx all others Q101 0.134 0.501 0.102 ! 1.37 eA-3 Q102 0.062 0.369 0.126 ! 1.28 eA-3 Q103 0.901 0.500 0.867 ! 1.28 eA-3 C104 0.337 0.499 0.669 ! 1.21 eA-3 C105 0.529 0.897 0.450 ! 1.09 eA-3 C106 0.608 0.323 0.010 ! 1.07 eA-3 C107 0.477 0.773 0.929 ! 0.98 eA-3 C108 0.439 0.502 0.838 ! 0.98 eA-3 C109 0.446 0.834 0.921 ! 0.95 eA-3 C110 0.367 0.494 0.236 ! 0.93 eA-3 C111 0.643 0.415 0.294 ! 0.91 eA-3 C112 0.304 0.496 0.994 ! 0.91 eA-3 C113 0.444 0.904 0.958 ! 0.91 eA-3 Q114 0.969 0.331 0.941 ! 0.91 eA-3 C115 0.869 0.501 0.304 ! 0.90 eA-3 C116 0.650 0.590 0.347 ! 0.90 eA-3 C117 0.518 0.315 0.405 ! 0.90 eA-3 C118 0.687 0.501 0.122 ! 0.89 eA-3 C119 0.413 0.380 0.482 ! 0.89 eA-3 C120 0.484 0.901 0.939 ! 0.88 eA-3 C121 0.515 0.894 0.381 ! 0.88 eA-3 C122 0.466 1.004 0.892 ! 0.88 eA-3 C123 0.563 0.244 0.472 ! 0.88 eA-3 C124 0.396 0.507 0.352 ! 0.87 eA-3 C125 0.354 0.493 0.971 ! 0.87 eA-3 C126 0.169 0.994 0.076 ! 0.87 eA-3 C127 0.916 0.997 0.843 ! 0.86 eA-3 C128 0.656 0.493 0.978 ! 0.86 eA-3 C129 0.616 0.506 0.413 ! 0.84 eA-3 C130 0.368 0.440 0.360 ! 0.84 eA-3 C131 0.476 0.830 0.979 ! 0.84 eA-3 C132 0.482 0.811 0.425 ! 0.83 eA-3 C133 0.485 0.186 0.984 ! 0.83 eA-3 C134 0.560 0.996 0.489 ! 0.83 eA-3 C135 0.667 0.401 0.390 ! 0.83 eA-3 C136 0.150 0.029 0.002 ! 0.83 eA-3 C137 0.139 1.001 0.960 ! 0.83 eA-3 C138 0.483 0.829 0.403 ! 0.83 eA-3 C139 0.562 0.415 0.963 ! 0.82 eA-3 C140 0.478 1.003 0.571 ! 0.82 eA-3 C141 0.601 0.507 0.352 ! 0.80 eA-3 C142 0.515 0.378 0.896 ! 0.79 eA-3 C143 0.834 1.001 0.898 ! 0.79 eA-3 C144 0.436 0.715 0.584 ! 0.79 eA-3 C145 0.618 0.354 0.174 ! 0.79 eA-3 C146 0.275 0.419 0.629 ! 0.78 eA-3 Q147 0.047 0.346 0.994 ! 0.78 eA-3 C148 0.484 0.815 0.486 ! 0.78 eA-3 C149 0.619 0.457 0.955 ! 0.78 eA-3 C150 0.554 0.395 0.912 ! 0.78 eA-3 Q151 0.453 0.364 0.235 ! 0.77 eA-3 C152 0.366 0.539 0.304 ! 0.77 eA-3 C153 0.180 0.249 0.603 ! 0.77 eA-3 Q154 0.444 0.363 0.300 ! 0.77 eA-3 C155 0.511 0.761 0.999 ! 0.77 eA-3 C156 0.438 0.316 0.546 ! 0.76 eA-3 C157 0.549 0.374 0.174 ! 0.76 eA-3 C158 0.383 0.466 0.737 ! 0.76 eA-3 C159 0.376 0.437 0.455 ! 0.76 eA-3 C160 0.446 0.064 0.933 ! 0.75 eA-3 C161 0.319 0.575 0.673 ! 0.75 eA-3 C162 0.564 0.777 0.493 ! 0.75 eA-3 C163 0.487 0.228 0.580 ! 0.75 eA-3 Q164 0.814 0.361 0.859 ! 0.74 eA-3 C165 0.608 0.498-0.002 ! 0.74 eA-3 C166 0.492 0.777 0.540 ! 0.74 eA-3 C167 0.443 0.500 0.735 ! 0.74 eA-3 C168 0.763 0.406 0.514 ! 0.74 eA-3 C169 0.623 0.372 0.083 ! 0.74 eA-3 C170 0.571 0.747 0.530 ! 0.73 eA-3 C171 0.599 0.501 0.611 ! 0.73 eA-3 C172 0.072 0.891 0.531 ! 0.73 eA-3 C173 0.453 0.506 0.357 ! 0.73 eA-3 C174 0.576 0.803 0.446 ! 0.73 eA-3 C175 0.558 0.358 0.407 ! 0.73 eA-3 C176 0.782 0.505 0.631 ! 0.73 eA-3 C177 0.368 0.332 0.785 ! 0.72 eA-3 C178 0.485 0.392 0.231 ! 0.72 eA-3 C179 0.419 0.407 0.735 ! 0.72 eA-3 C180 0.258 0.421 0.581 ! 0.72 eA-3 Q181 0.741 0.406 0.576 ! 0.72 eA-3 C182 0.449 0.109 0.508 ! 0.72 eA-3 C183 0.348 0.497 0.392 ! 0.72 eA-3 Q184 0.933 0.393 0.060 ! 0.71 eA-3 C185 0.432 0.690 0.610 ! 0.71 eA-3 C186 0.483 0.159 0.380 ! 0.71 eA-3 C187 0.563 0.258 0.068 ! 0.71 eA-3 C188 0.546 0.488 0.348 ! 0.71 eA-3 C189 0.562 0.744 0.586 ! 0.70 eA-3 C190 0.531 0.375 0.363 ! 0.70 eA-3 C191 0.297 0.425 0.699 ! 0.70 eA-3 C192 0.564 0.784 0.075 ! 0.70 eA-3 C193 0.734 0.488 0.640 ! 0.70 eA-3 C194 0.415 0.379 0.420 ! 0.70 eA-3 C195 0.643 0.423 0.011 ! 0.70 eA-3 C196 0.436 0.766 0.858 ! 0.70 eA-3 C197 0.710 0.499 0.578 ! 0.70 eA-3 C198 0.438 0.428 0.781 ! 0.70 eA-3 C199 0.521 0.704 0.446 ! 0.70 eA-3 (replace by semicolon in column 1 when used as .sqf) ; _shelx_fab_checksum 34892