#------------------------------------------------------------------------------ #$Date: 2024-09-20 04:21:42 +0300 (Fri, 20 Sep 2024) $ #$Revision: 294817 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249357.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7249357 loop_ _publ_author_name 'Garz\'on-Serrano, Andrea Y.' 'Lozano, Johan D.' 'Perez, Leon D.' 'Sierra, C\'esar A.' 'Mac\'ias, Mario A.' _publ_section_title ; Zr6O8 core cluster with formula unit [Zr6O4(OH)4(OH2)8(CH3COO)4(SO4)4]·nH2O obtained under mild conditions ; _journal_issue 41 _journal_name_full 'RSC Advances' _journal_page_first 29910 _journal_page_last 29918 _journal_paper_doi 10.1039/D4RA03940H _journal_volume 14 _journal_year 2024 _chemical_absolute_configuration unk _chemical_formula_moiety 'C8 H32 O40 S4 Zr6, 13[H2O]' _chemical_formula_sum 'C8 H58 O53 S4 Zr6' _chemical_formula_weight 1678.125 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_Hall 'C -2yc' _space_group_name_H-M_alt 'C 1 c 1' _symmetry_Int_Tables_number 9 _audit_creation_date 2024-08-12 _audit_creation_method ; Olex2 1.5-dev (compiled 2024.08.07 svn.r83e07e25 for OlexSys, GUI svn.r6697) ; _audit_update_record ; 2024-08-14 deposited with the CCDC. 2024-09-09 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 116.436(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.9608(13) _cell_length_b 27.9958(19) _cell_length_c 14.7493(11) _cell_measurement_reflns_used 3708 _cell_measurement_temperature 298(2) _cell_measurement_theta_max 75.3770 _cell_measurement_theta_min 4.6130 _cell_volume 5161.9(9) _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) (compiled Aug 13 2014,18:06:01) ; _computing_molecular_graphics 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5-dev (Dolomanov et al., 2009)' _computing_structure_refinement 'olex2.refine 1.5-dev (Bourhis et al., 2015)' _computing_structure_solution 'Superflip (Palatinus & Chapuis, 2007)' _diffrn_ambient_temperature 298.15 _diffrn_detector_area_resol_mean 10.6144 _diffrn_detector_type Atlas _diffrn_measured_fraction_theta_full 0.9979 _diffrn_measured_fraction_theta_max 0.9773 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0599 _diffrn_reflns_av_unetI/netI 0.0795 _diffrn_reflns_Laue_measured_fraction_full 0.9979 _diffrn_reflns_Laue_measured_fraction_max 0.9773 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 13189 _diffrn_reflns_point_group_measured_fraction_full 0.6621 _diffrn_reflns_point_group_measured_fraction_max 0.6453 _diffrn_reflns_theta_full 67.6840 _diffrn_reflns_theta_max 76.09 _diffrn_reflns_theta_min 3.87 _exptl_absorpt_coefficient_mu 12.285 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.63737 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.119a (Rigaku Oxford Diffraction, 2021) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.159 _exptl_crystal_description octahedral _exptl_crystal_F_000 3350.454 _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _platon_squeeze_details ) _refine_diff_density_max 1.0548 _refine_diff_density_min -0.9730 _refine_diff_density_rms 0.1436 _refine_ls_abs_structure_details 'Hooft, R.W.W., Straver, L.H., Spek, A.L. (2010). J. Appl. Cryst., 43, 665-668.' _refine_ls_abs_structure_Flack 0.05(3) _refine_ls_d_res_high 0.7942 _refine_ls_d_res_low 11.4147 _refine_ls_goodness_of_fit_ref 1.0233 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_constraints 47 _refine_ls_number_parameters 538 _refine_ls_number_reflns 6972 _refine_ls_number_restraints 103 _refine_ls_restrained_S_all 1.0154 _refine_ls_R_factor_all 0.0632 _refine_ls_R_factor_gt 0.0517 _refine_ls_shift/su_max -0.0001 _refine_ls_shift/su_mean 0.0000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0838P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1315 _refine_ls_wR_factor_ref 0.1437 _reflns_Friedel_coverage 0.312 _reflns_limit_h_max 17 _reflns_limit_h_min -11 _reflns_limit_k_max 35 _reflns_limit_k_min -35 _reflns_limit_l_max 17 _reflns_limit_l_min -18 _reflns_number_gt 5931 _reflns_number_total 6972 _reflns_threshold_expression I>=2u(I) _iucr_refine_instructions_details ; TITL 2023Uniandes_Cu_05_PCA_auto in C2/c CELL 1.54184 13.96081 27.99582 14.7493 90 116.43578 90 ZERR 4 0.0013 0.0019 0.0011 0 0.0105 0 LATT -7 SYMM +X,-Y,0.5+Z SFAC C H O S Zr UNIT 32 232 212 16 24 EQIV $1 -0.5+X,1.5-Y,-0.5+Z EQIV $2 +X,1-Y,-0.5+Z EQIV $3 +X,1-Y,0.5+Z EQIV $4 0.5+X,1.5-Y,0.5+Z CONF ACTA ISOR 0.01 0.02 O16D RIGU 0.01 0.02 O16D O15D O13D S4D O14D RIGU O12D O11D O10D O9D S3D RIGU O4D O1D S1D O2D O3D DFIX 0.85 O8C H8Ca O8C H8Cb DANG 1.34 H8Ca H8Cb SADI Zr3 H8Ca Zr3 H8Cb L.S. 20 0 156 PLAN 10 SIZE 0.21 0.18 0.19 TEMP 25 HTAB O8C O1C HTAB O7C O8E_$1 HTAB O7C O6C HTAB O7C O1D_$1 HTAB C6E O7D HTAB O5C O12D_$3 HTAB O5C O4C HTAB O4C O12D_$3 HTAB O4C O5E_$3 HTAB O4C O5C HTAB O1A O12D_$3 HTAB O2A O4D_$1 HTAB O1C O8D_$4 HTAB O1C O8C HTAB O4A O16D_$2 HTAB O3A O8D_$4 HTAB O2C O3C LIST 4 FMAP 2 ACTA ABIN BASF 0.20605 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 13 5 4 OMIT 15 7 0 OMIT 16 6 -3 WGHT 0.083837 0 FVAR 1.278396 REM REM REM > REM REM > REM > REM REM Zr1 5 0.066365 0.537115 0.436907 11.00000 0.04544 0.02483 = 0.01991 0.00058 0.01441 0.00072 O16D 3 0.233132 0.508348 0.771649 11.00000 0.17089 0.05918 = 0.04750 0.01601 0.05061 -0.00665 O15D 3 0.350286 0.533286 0.702326 11.00000 0.09973 0.11273 = 0.08656 0.01523 0.02701 0.02526 O14D 3 0.215982 0.586218 0.695351 11.00000 0.06395 0.03248 = 0.02572 0.01280 0.01979 0.01085 O13D 3 0.174209 0.513645 0.593341 11.00000 0.05706 0.03653 = 0.02141 0.00281 0.00747 0.00799 O12D 3 -0.090037 0.447340 0.151694 11.00000 0.10204 0.03970 = 0.03946 -0.01113 0.02311 -0.00682 O11D 3 -0.206537 0.490629 0.198760 11.00000 0.08583 0.06818 = 0.06519 -0.01342 0.03244 -0.01990 O10D 3 -0.021039 0.486604 0.310893 11.00000 0.10366 0.02900 = 0.01870 -0.00792 0.01903 -0.01853 O9D 3 -0.083345 0.534005 0.157757 11.00000 0.07155 0.03468 = 0.02140 -0.00953 0.01531 -0.00997 O8E 3 0.326489 0.650056 0.648457 11.00000 0.02874 0.05288 = 0.03396 0.00246 0.00920 -0.00529 C8E 1 0.507967 0.644275 0.682848 11.00000 0.05765 0.08290 = 0.04522 -0.01982 0.00609 -0.00442 AFIX 33 H8Ea 2 0.515556 0.649429 0.750072 11.00000 -1.50000 H8Eb 2 0.544752 0.615512 0.681503 11.00000 -1.50000 H8Ec 2 0.538067 0.670832 0.663211 11.00000 -1.50000 AFIX 0 O8D 3 -0.164772 0.739382 0.018061 11.00000 0.04943 0.04279 = 0.02916 0.00560 0.01284 0.00747 O8C 3 0.144016 0.764249 0.337586 11.00000 0.04922 0.05181 = 0.02684 0.00427 0.00788 -0.01632 H8Ca 2 0.204391 0.751091 0.351993 11.00000 -1.50000 H8Cb 2 0.163194 0.787139 0.380260 11.00000 -1.50000 O7E 3 0.370353 0.632810 0.519901 11.00000 0.02946 0.05059 = 0.02924 -0.00156 0.00884 -0.00871 C7E 1 0.401530 0.640062 0.616760 11.00000 0.05034 0.04020 = 0.01836 -0.00481 0.00799 -0.00517 O7D 3 0.011892 0.709513 0.065820 11.00000 0.05855 0.04119 = 0.05328 0.00785 0.03432 -0.00328 O7C 3 -0.098782 0.767580 0.326720 11.00000 0.04889 0.04997 = 0.03402 -0.01261 0.01548 0.00284 AFIX 7 H7Ca 2 -0.155443 0.753936 0.322499 11.00000 -1.50000 H7Cb 2 -0.117429 0.779380 0.267782 11.00000 -1.50000 AFIX 0 O6E 3 0.202657 0.614375 0.218342 11.00000 0.04782 0.06941 = 0.01932 0.00164 0.01204 -0.00263 C6E 1 0.140883 0.616526 0.041815 11.00000 0.08681 0.05364 = 0.03814 -0.00445 0.04610 0.00053 AFIX 33 H6Ea 2 0.214776 0.624311 0.063173 11.00000 -1.50000 H6Eb 2 0.123365 0.587928 0.001730 11.00000 -1.50000 H6Ec 2 0.096775 0.642308 0.002156 11.00000 -1.50000 AFIX 0 O6D 3 -0.117515 0.664011 0.097836 11.00000 0.03664 0.03203 = 0.02632 0.00652 0.01047 0.00065 O6C 3 -0.237482 0.684073 0.394553 11.00000 0.05689 0.04882 = 0.03039 -0.00946 0.01820 0.00734 AFIX 7 H6Ca 2 -0.229303 0.708974 0.430234 11.00000 -1.50000 H6Cb 2 -0.301521 0.685851 0.348494 11.00000 -1.50000 AFIX 0 O5E 3 0.029113 0.598210 0.119685 11.00000 0.05159 0.04162 = 0.02304 -0.00769 0.02131 -0.01069 C5E 1 0.121694 0.608753 0.133148 11.00000 0.06862 0.04315 = 0.03005 -0.00617 0.03377 -0.00250 O5D 3 -0.043643 0.735694 0.193222 11.00000 0.06548 0.03817 = 0.01698 0.00219 0.01007 -0.00302 O5C 3 -0.207376 0.575291 0.459545 11.00000 0.03898 0.04551 = 0.04120 0.01221 0.01399 -0.00470 AFIX 7 H5Ca 2 -0.253884 0.561806 0.406341 11.00000 -1.50000 H5Cb 2 -0.244078 0.589802 0.484232 11.00000 -1.50000 AFIX 0 O4E 3 -0.226345 0.599725 0.149473 11.00000 0.04228 0.04624 = 0.02693 -0.00261 0.00984 -0.00955 C4E 1 -0.406112 0.585841 0.123158 11.00000 0.04894 0.17165 = 0.04195 -0.03883 0.02281 -0.06398 AFIX 33 H4Ea 2 -0.415189 0.579762 0.055740 11.00000 -1.50000 H4Eb 2 -0.427358 0.558155 0.148125 11.00000 -1.50000 H4Ec 2 -0.449558 0.612580 0.122302 11.00000 -1.50000 AFIX 0 O4D 3 0.183254 0.802568 0.646163 11.00000 0.04293 0.03733 = 0.03429 -0.00609 0.00781 -0.00334 S4D 4 0.234827 0.535088 0.694412 11.00000 0.07849 0.03765 = 0.02596 0.00799 0.00622 0.01219 O4C 3 -0.033039 0.488958 0.480804 11.00000 0.05138 0.04261 = 0.02920 0.00563 0.01917 -0.00443 AFIX 7 H4Ca 2 0.005287 0.477293 0.539118 11.00000 -1.50000 H4Cb 2 -0.080894 0.504954 0.488133 11.00000 -1.50000 AFIX 0 O4B 3 0.012611 0.670747 0.466008 11.00000 0.04200 0.02776 = 0.02780 -0.00575 0.01838 -0.00976 O1A 3 0.019717 0.585578 0.532107 11.00000 0.05019 0.02786 = 0.01981 -0.00387 0.01285 0.00037 AFIX 13 0.82 H1A 2 0.010383 0.572920 0.577682 11.00000 -1.20000 AFIX 0 O2A 3 -0.113988 0.667700 0.286280 11.00000 0.03201 0.03656 = 0.02270 0.00383 0.00972 -0.00693 AFIX 13 0.82 H2A 2 -0.169355 0.681215 0.247762 11.00000 -1.20000 AFIX 0 O1D 3 0.188026 0.717261 0.636712 11.00000 0.04806 0.03151 = 0.02781 -0.00325 0.01544 -0.00392 S1D 4 0.120095 0.761499 0.597956 11.00000 0.03774 0.03219 = 0.02723 -0.00582 0.01081 -0.00060 O1C 3 0.311122 0.680544 0.349411 11.00000 0.06420 0.04635 = 0.02988 0.00306 0.02528 -0.01091 AFIX 7 H1Ca 2 0.342323 0.668728 0.316527 11.00000 -1.50000 H1Cb 2 0.361794 0.689787 0.404953 11.00000 -1.50000 AFIX 0 O1B 3 0.173730 0.594756 0.483218 11.00000 0.06615 0.03121 = 0.01491 -0.00039 0.01725 -0.01037 Zr2 5 -0.053583 0.607541 0.215103 11.00000 0.03923 0.02813 = 0.01763 0.00031 0.01097 -0.00189 O4A 3 0.101221 0.564322 0.310578 11.00000 0.04134 0.02884 = 0.02212 -0.00141 0.01129 -0.00586 AFIX 13 0.82 H4A 2 0.117743 0.544075 0.279887 11.00000 -1.20000 AFIX 0 O3A 3 0.190958 0.684894 0.464494 11.00000 0.04368 0.02814 = 0.01485 -0.00343 0.01220 -0.00436 AFIX 13 0.82 H3A 2 0.239332 0.704591 0.488372 11.00000 -1.20000 AFIX 0 Zr3 5 0.030105 0.713396 0.357836 11.00000 0.03691 0.02539 = 0.01963 0.00086 0.01012 0.00055 Zr4 5 0.152533 0.643131 0.580191 11.00000 0.03811 0.02664 = 0.01743 -0.00043 0.01035 0.00047 Zr5 5 0.218315 0.623858 0.379917 11.00000 0.03599 0.02958 = 0.01962 -0.00121 0.01142 0.00059 Zr6 5 -0.119626 0.627809 0.416179 11.00000 0.03654 0.03069 = 0.01880 0.00132 0.01086 -0.00084 O1E 3 0.070964 0.651527 0.675722 11.00000 0.02402 0.04785 = 0.02519 -0.00254 0.00971 -0.00073 C1E 1 -0.028751 0.657670 0.657455 11.00000 0.06855 0.04212 = 0.02312 0.00010 0.01857 0.00218 O2C 3 0.327993 0.564638 0.388238 11.00000 0.03808 0.04495 = 0.03841 -0.00480 0.00979 0.01161 AFIX 7 H2Ca 2 0.392991 0.573629 0.419312 11.00000 -1.50000 H2Cb 2 0.319282 0.558114 0.328622 11.00000 -1.50000 AFIX 0 O2B 3 0.071207 0.655199 0.294433 11.00000 0.03572 0.02415 = 0.01690 -0.00423 0.00595 -0.00576 O2D 3 0.088545 0.764870 0.488305 11.00000 0.05974 0.03098 = 0.02527 -0.00808 0.01209 -0.00681 S2D 4 -0.078418 0.712169 0.092057 11.00000 0.04237 0.03576 = 0.02472 0.00657 0.01421 0.00130 O2E 3 -0.103759 0.650628 0.569427 11.00000 0.03422 0.06805 = 0.02191 -0.00108 0.01544 0.00207 C2E 1 -0.048968 0.668769 0.744518 11.00000 0.04229 0.14618 = 0.04758 -0.04319 0.02872 -0.00756 AFIX 137 H2Ea 2 -0.081097 0.699817 0.735664 11.00000 -1.50000 H2Eb 2 -0.096435 0.645297 0.749678 11.00000 -1.50000 H2Ec 2 0.017383 0.668463 0.805243 11.00000 -1.50000 AFIX 0 O3E 3 -0.266089 0.605727 0.283340 11.00000 0.04481 0.05731 = 0.01712 0.00069 0.00917 -0.00518 C3E 1 -0.288615 0.597033 0.192139 11.00000 0.04736 0.05021 = 0.02748 -0.00374 0.01284 -0.01576 O3D 3 0.024121 0.758795 0.615354 11.00000 0.05031 0.03659 = 0.04090 -0.01451 0.02086 -0.00543 S3D 4 -0.096568 0.488453 0.203190 11.00000 0.07663 0.03347 = 0.02985 -0.00618 0.01646 -0.01183 O3C 3 0.179834 0.482738 0.431588 11.00000 0.06823 0.05292 = 0.05174 0.01253 0.03835 0.02461 AFIX 7 H3Ca 2 0.224287 0.475354 0.491703 11.00000 -1.50000 H3Cb 2 0.217936 0.495360 0.406273 11.00000 -1.50000 AFIX 0 O3B 3 -0.058437 0.581796 0.345347 11.00000 0.03675 0.04428 = 0.01405 0.00505 0.00869 0.00496 HKLF 4 END Q1 1 0.125 0.520833 0.74 11 0.05 1.05 Q2 1 0.145833 0.614583 0.58 11 0.05 0.99 Q3 1 0.3125 0.510417 0.76 11 0.05 0.87 Q4 1 0.3125 0.625 0.42 11 0.05 0.78 Q5 1 0.229167 0.59375 0.38 11 0.05 0.77 Q14 1 0.208333 0.65625 0.38 11 0.05 0.72 Q6 1 -0.208333 0.520833 0.26 11 0.05 0.75 Q7 1 0.208333 0.645833 0.52 11 0.05 0.75 Q9 1 0.020833 0.479167 0.18 11 0.05 0.74 Q10 1 0.0625 0.541667 0.44 11 0.05 0.74 Q12 1 0.25 0.645833 0.62 11 0.05 0.73 Q11 1 -0.041667 0.604167 0.22 11 0.05 0.74 Q13 1 -0.145833 0.604167 0.18 11 0.05 0.73 Q15 1 -0.0625 0.71875 0.32 11 0.05 0.7 Q16 1 0.0625 0.645833 0.54 11 0.05 0.68 Q18 1 -0.083333 0.65625 0.42 11 0.05 0.68 Q19 1 0.104167 0.697917 0.16 11 0.05 0.68 Q22 1 0.083333 0.5 0.42 11 0.05 0.65 Q20 1 0 0.604167 0.16 11 0.05 0.66 Q17 1 -0.1875 0.770833 0.04 11 0.05 0.68 Q21 1 0.145833 0.677083 0.6 11 0.05 0.66 Q24 1 0.25 0.802083 0.68 11 0.05 0.64 Q23 1 0.333333 0.552083 0.6 11 0.05 0.65 Q25 1 0.041667 0.708333 0.36 11 0.05 0.62 Q26 1 0.125 0.625 0.34 11 0.05 0.62 Q31 1 -0.208333 0.625 0.38 11 0.05 0.59 Q28 1 0.041667 0.677083 0.32 11 0.05 0.61 Q33 1 0.125 0.677083 0.52 11 0.05 0.58 Q32 1 -0.166667 0.458333 0.14 11 0.05 0.59 Q30 1 -0.020833 0.625 0.38 11 0.05 0.6 Q34 1 -0.083333 0.572917 0.22 11 0.05 0.57 Q29 1 0 0.552083 0.64 11 0.05 0.61 Q35 1 0.0625 0.677083 0.42 11 0.05 0.56 Q8 1 -0.125 0.59375 0.42 11 0.05 0.75 Q27 1 -0.083333 0.645833 0.16 11 0.05 0.62 Q36 1 0.041667 0.572917 0.36 11 0.05 0.55 REM The information below was added by Olex2. REM REM R1 = 0.0517 for 5931 Fo > 4sig(Fo) and 0.0632 for all 6972 data REM 538 parameters refined using 103 restraints REM Highest difference peak 1.0548, deepest hole -0.9730 REM Mean Shift 0.0000, Max Shift -0.0001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0632 REM R1_gt = 0.0517 REM wR_ref = 0.1437 REM GOOF = 1.0233 REM Shift_max = -0.0001 REM Shift_mean = 0.0000 REM Reflections_all = 6972 REM Reflections_gt = 5931 REM Parameters = 538 REM Hole = -0.9730 REM Peak = 1.0548 REM Flack = 0.05(3) ; _cod_data_source_file d4ra03940h2.cif _cod_data_source_block 2023uniandes_cu_05_pca-9_sq _cod_original_sg_symbol_Hall ' C -2yc' _cod_database_code 7249357 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.79(3) 0.21(3) 2. Fixed Uiso At 1.2 times of: All O(H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 3. Restrained distances O8C-H8Ca = O8C-H8Cb 0.85 with sigma of 0.02 H8Ca-H8Cb 1.34 with sigma of 0.04 Zr3-H8Ca \\sim Zr3-H8Cb with sigma of 0.02 4. Uiso/Uaniso restraints and constraints Uanis(O16D) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Rigid body (RIGU) restrains O16D, O15D, O13D, S4D, O14D with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 O12D, O11D, O10D, O9D, S3D with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O4D, O1D, S1D, O2D, O3D with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6.a Rotating group: O7C(H7Ca,H7Cb), O6C(H6Ca,H6Cb), O5C(H5Ca,H5Cb), O4C(H4Ca,H4Cb), O2C(H2Ca, H2Cb), O3C(H3Ca,H3Cb), O1C(H1Ca,H1Cb) 6.b Ternary CH refined with riding coordinates: O1A(H1A), O2A(H2A), O4A(H4A), O3A(H3A) 6.c Me refined with riding coordinates: C8E(H8Ea,H8Eb,H8Ec), C6E(H6Ea,H6Eb,H6Ec), C4E(H4Ea,H4Eb,H4Ec) 6.d Idealised Me refined as rotating group: C2E(H2Ea,H2Eb,H2Ec) ; _smtbx_masks_special_details ; A solvent mask was calculated and 534 electrons were found in a volume of 1917\%A^3^ in 1 void per unit cell. This is consistent with the presence of 13[H2O] per Formula Unit which account for 520 electrons per unit cell. ; _shelx_fab_file ; -6 0 18 3.75 -1.56 -8 0 18 -0.74 -2.91 -10 0 18 4.66 -0.36 -5 1 18 1.50 1.97 -7 1 18 -1.27 -1.65 -9 1 18 1.76 -1.55 -11 1 18 3.00 -2.91 -6 2 18 -1.66 1.68 -8 2 18 -0.50 1.52 -10 2 18 1.57 -2.53 -5 3 18 -4.09 1.82 -7 3 18 -0.55 0.47 -9 3 18 -0.35 0.65 -11 3 18 0.88 -1.61 -6 4 18 0.08 0.05 -8 4 18 0.26 -2.05 -10 4 18 -0.22 -2.96 -5 5 18 -2.51 2.05 -7 5 18 2.91 -1.54 -9 5 18 0.94 -3.93 -6 6 18 -0.34 2.31 -8 6 18 -1.67 -2.06 -10 6 18 -0.25 -1.28 -7 7 18 -2.21 -0.43 -9 7 18 -2.63 1.92 -8 8 18 -2.19 -1.33 -3 1 17 1.97 -1.49 -5 1 17 -1.46 -5.14 -7 1 17 -1.44 -3.14 -9 1 17 -0.65 -1.77 -11 1 17 -1.89 -0.45 -13 1 17 -1.66 -1.99 -4 2 17 -2.07 -1.66 -6 2 17 -1.03 0.42 -8 2 17 -2.16 -3.43 -10 2 17 -2.76 -2.18 -12 2 17 -0.60 -1.60 -3 3 17 -1.12 -2.84 -5 3 17 -2.02 5.39 -7 3 17 1.65 1.58 -9 3 17 -0.36 -1.50 -11 3 17 -0.04 2.20 -13 3 17 2.96 0.00 -2 4 17 -1.51 3.25 -4 4 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0.31 -3.34 -4 8 16 3.88 -1.62 -6 8 16 -2.58 -4.94 -8 8 16 -1.59 2.67 -10 8 16 0.03 0.95 -12 8 16 -3.80 -2.72 -1 9 16 0.26 -2.20 -3 9 16 0.26 -1.44 -5 9 16 4.49 -2.14 -7 9 16 2.33 -0.09 -9 9 16 3.33 3.57 -11 9 16 -0.95 -2.04 -13 9 16 0.27 0.66 -2 10 16 -1.75 3.12 -4 10 16 0.82 -0.82 -6 10 16 2.14 3.74 -8 10 16 5.15 2.49 -10 10 16 2.16 1.34 -12 10 16 -1.21 0.53 -1 11 16 -5.05 1.41 -3 11 16 -1.15 1.19 -5 11 16 -0.57 -0.69 -7 11 16 0.43 5.27 -9 11 16 3.12 1.02 -11 11 16 -0.73 1.05 -13 11 16 -0.89 -1.81 -2 12 16 -2.53 -2.28 -4 12 16 3.03 -2.29 -6 12 16 -1.67 -0.21 -8 12 16 -0.86 2.57 -10 12 16 0.77 -2.06 -12 12 16 0.47 0.76 -3 13 16 6.06 -0.90 -5 13 16 -0.55 -2.39 -7 13 16 -0.18 -1.41 -9 13 16 0.56 -0.74 -11 13 16 -1.12 -0.82 -2 14 16 2.79 0.79 -4 14 16 3.84 -1.08 -6 14 16 0.09 0.27 -8 14 16 1.94 -0.05 -10 14 16 0.45 -1.12 -3 15 16 -0.36 2.64 -5 15 16 1.13 -0.75 -7 15 16 -0.63 4.83 -9 15 16 3.09 -0.48 -4 16 16 -2.38 -1.38 -6 16 16 0.35 0.51 -8 16 16 -0.53 3.09 -7 17 16 0.65 -3.24 -3 1 15 5.03 0.24 -5 1 15 -2.21 -2.56 -7 1 15 6.22 2.57 -9 1 15 3.45 1.08 -11 1 15 0.70 -3.15 -13 1 15 1.71 -0.34 -15 1 15 2.53 1.35 -2 2 15 6.04 1.31 -4 2 15 0.06 -0.22 -6 2 15 -1.77 0.21 -8 2 15 4.89 3.40 -10 2 15 1.41 -0.21 -12 2 15 -0.78 -1.12 -14 2 15 2.28 -0.54 -5 3 15 4.26 -1.39 -7 3 15 -4.78 7.34 -9 3 15 -0.61 3.56 -11 3 15 -6.10 3.40 -13 3 15 -4.23 2.74 -15 3 15 0.11 -0.80 -4 4 15 1.12 -1.47 -6 4 15 -3.58 3.34 -8 4 15 -4.76 -1.61 -10 4 15 -6.07 7.11 -12 4 15 -7.90 -0.13 -14 4 15 -0.65 3.14 -3 5 15 4.16 -4.35 -5 5 15 -4.27 1.89 -7 5 15 3.89 -4.41 -9 5 15 -8.45 0.32 -11 5 15 0.20 -0.97 -13 5 15 -2.57 0.62 -15 5 15 -0.32 2.35 -4 6 15 4.24 3.27 -6 6 15 1.36 -2.97 -8 6 15 -0.05 -1.33 -10 6 15 2.12 -1.13 -12 6 15 1.98 -1.23 -14 6 15 -0.50 0.48 -3 7 15 -4.55 8.63 -5 7 15 4.82 -1.30 -7 7 15 -4.58 -0.54 -9 7 15 4.96 3.21 -11 7 15 2.91 -1.93 -13 7 15 2.83 0.92 2 8 15 1.80 -1.67 -4 8 15 -2.43 -2.26 -6 8 15 -1.67 3.76 -8 8 15 -2.54 4.42 -10 8 15 3.47 -0.12 -12 8 15 0.05 2.85 -14 8 15 0.79 4.05 -3 9 15 2.71 -6.36 -5 9 15 -7.73 -4.18 -7 9 15 0.17 4.61 -9 9 15 0.37 -1.24 -11 9 15 -2.00 1.67 -13 9 15 0.39 0.54 0 10 15 3.77 -1.87 -2 10 15 1.98 -3.25 -4 10 15 -0.59 -8.48 -6 10 15 -0.89 -2.40 -8 10 15 4.81 2.37 -10 10 15 -3.92 -2.88 -12 10 15 3.62 1.09 -14 10 15 -3.41 -1.02 1 11 15 1.56 0.35 -1 11 15 0.82 -0.39 -3 11 15 0.38 -3.21 -5 11 15 2.51 1.63 -7 11 15 5.51 2.39 -9 11 15 0.94 1.34 -11 11 15 0.32 2.05 -13 11 15 -2.20 -1.48 0 12 15 0.61 3.65 -2 12 15 -1.78 -0.80 -4 12 15 -1.18 4.38 -6 12 15 6.41 7.42 -8 12 15 1.18 2.71 -10 12 15 0.37 4.91 -12 12 15 -2.06 -2.04 -3 13 15 -0.53 0.77 -5 13 15 0.90 4.85 -7 13 15 0.41 3.85 -9 13 15 -2.90 2.48 -11 13 15 -0.92 0.33 -13 13 15 -1.79 -0.38 0 14 15 -0.23 -5.53 -2 14 15 2.19 -1.47 -4 14 15 -0.25 0.51 -6 14 15 -2.17 -5.76 -8 14 15 -3.71 1.03 -10 14 15 -3.92 -0.75 -12 14 15 -0.13 1.37 -1 15 15 2.27 -3.40 -3 15 15 -0.73 -2.01 -5 15 15 1.46 -5.55 -7 15 15 -3.23 -6.03 -9 15 15 -1.55 -0.22 -11 15 15 -0.10 -0.83 -2 16 15 0.62 -0.08 -4 16 15 0.33 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-1.87 -3.39 -6 20 15 -0.18 -1.16 1 1 16 -0.54 -0.40 1 3 16 2.03 -1.65 -1 1 17 -0.04 -1.35 -2 2 17 3.11 -1.03 -1 3 17 0.42 2.20 -2 8 17 -0.30 1.89 0 2 0 11.05 0.09 14 4 0 -9.68 -7.50 15 9 0 -43.77 16.66 15 11 0 -15.73 20.20 14 12 0 21.74 -6.31 14 14 0 -16.95 -3.36 14 16 0 -4.08 -7.85 13 19 0 0.10 -2.38 9 29 0 -1.53 -0.49 8 30 0 -1.23 1.68 7 31 0 1.31 0.45 13 1 1 -8.44 -11.05 -16 4 1 15.63 -13.67 -16 6 1 14.01 34.49 15 7 1 8.37 9.35 -15 11 1 8.65 17.32 14 12 1 -3.30 9.60 -15 13 1 -6.31 -7.05 14 14 1 2.41 -0.77 -14 16 1 0.62 0.60 -14 18 1 1.27 1.62 -13 21 1 1.01 2.91 12 22 1 -2.30 -1.50 -12 24 1 -1.96 5.15 -10 28 1 0.36 0.59 -8 30 1 -2.86 4.19 8 30 1 2.34 0.06 7 31 1 0.03 -1.04 5 33 1 2.63 -3.34 4 34 1 -0.72 -3.27 -3 35 1 -0.41 0.53 1 35 1 0.95 -4.38 13 1 2 1.44 4.21 -16 8 2 26.79 9.27 14 10 2 14.76 8.29 -15 13 2 7.12 -2.38 -15 15 2 5.16 2.83 13 15 2 4.05 1.70 12 20 2 1.61 -1.58 11 23 2 3.06 -2.31 -11 27 2 -0.48 -1.54 9 27 2 -4.58 -0.22 -9 29 2 1.40 0.85 1 35 2 0.06 -0.26 14 6 3 -4.82 0.12 -16 8 3 -1.13 -4.09 -16 10 3 4.39 5.34 13 13 3 8.00 -1.37 -15 15 3 3.93 -0.73 3 17 3 -8.35 7.98 12 18 3 -2.35 -1.08 -14 20 3 -2.22 2.47 -13 23 3 -1.81 -1.77 10 24 3 -3.28 0.94 -11 27 3 0.35 1.69 8 28 3 -1.59 -2.82 2 34 3 -0.57 1.53 -1 35 3 -3.66 3.07 -10 0 4 -7.83 -15.25 -17 1 4 3.64 -12.38 -10 2 4 5.00 10.12 -17 3 4 -31.52 27.34 -17 5 4 -2.36 10.21 13 7 4 0.91 -13.57 13 9 4 -8.30 -4.81 13 11 4 -1.53 2.05 -16 12 4 0.37 8.98 12 16 4 3.31 7.23 9 25 4 2.03 1.34 -11 27 4 -2.39 1.16 6 30 4 -0.84 0.23 5 31 4 -3.68 0.83 4 32 4 0.79 1.94 3 33 4 2.25 -1.83 -4 34 4 -0.91 1.15 -17 1 5 -9.02 20.96 13 1 5 -6.56 1.84 -17 3 5 12.70 -4.90 13 3 5 -4.28 4.65 -17 5 5 2.03 -0.76 13 5 5 0.75 -5.31 -17 7 5 -6.65 1.14 12 12 5 -0.20 0.47 -16 14 5 -2.17 1.62 6 14 5 -8.25 0.32 11 17 5 0.61 -5.05 9 23 5 0.67 -0.03 -12 26 5 -3.34 -1.62 -2 34 5 0.27 1.12 12 0 6 -6.64 -2.34 -17 1 6 8.20 -6.35 -17 3 6 2.60 9.86 -17 5 6 1.25 12.36 12 6 6 3.04 5.90 12 8 6 -4.82 -5.58 -17 9 6 -7.28 -0.65 -16 14 6 -0.33 3.17 10 18 6 -0.65 0.16 9 21 6 2.83 0.32 8 24 6 0.63 -2.87 -12 26 6 0.63 -0.40 5 29 6 1.72 3.83 4 30 6 2.23 3.37 3 31 6 0.08 2.53 2 32 6 -1.89 0.32 -5 33 6 -1.09 1.22 -17 1 7 6.50 -10.16 -17 3 7 2.54 -1.75 -17 9 7 5.32 4.24 11 9 7 1.78 0.43 9 19 7 0.58 -0.46 8 22 7 -2.87 0.48 7 23 7 -0.82 -0.05 6 26 7 0.61 0.07 5 27 7 3.17 2.54 -6 32 7 -1.04 3.20 0 32 7 0.53 -1.34 -17 1 8 -2.01 -4.30 -17 9 8 1.74 1.39 6 24 8 6.13 -3.23 -11 27 8 1.07 -3.67 -7 31 8 2.48 -0.95 -4 32 8 -0.84 1.23 -17 1 9 3.63 -4.71 10 2 9 1.62 2.58 -17 3 9 1.70 -3.34 10 4 9 -0.33 -3.24 -17 7 9 0.99 1.53 -17 9 9 1.02 3.05 8 16 9 2.03 0.07 7 19 9 -6.24 3.42 6 22 9 -0.83 2.97 -13 23 9 -0.41 0.99 3 27 9 -2.06 -5.42 2 28 9 -0.94 -1.82 1 29 9 0.10 1.93 -5 31 9 -0.11 -0.10 -3 31 9 -2.00 -0.90 -17 1 10 4.25 5.14 -17 3 10 -0.03 -5.25 9 3 10 0.57 -4.08 -17 5 10 2.91 0.28 9 5 10 -2.68 4.22 -17 7 10 2.27 -2.53 -17 9 10 2.23 0.82 8 12 10 -2.63 -0.64 -16 14 10 1.03 1.23 7 15 10 -4.42 0.31 -12 24 10 -0.92 -2.26 3 25 10 0.15 -1.88 0 28 10 -5.38 3.01 -7 29 10 2.83 0.55 -1 29 10 -3.15 1.74 -4 30 10 -0.81 -0.04 -17 1 11 1.23 -2.88 8 4 11 0.97 3.36 -17 5 11 -2.59 2.14 -17 7 11 -2.72 -0.13 7 11 11 0.82 -4.85 -16 12 11 -4.32 -1.02 6 14 11 -3.55 1.56 6 16 11 2.60 0.69 3 23 11 2.03 -1.45 2 24 11 1.85 -0.74 1 25 11 1.20 -1.55 -10 26 11 -0.96 1.27 -9 27 11 1.48 0.65 -6 28 11 -0.18 4.01 -2 28 11 -0.07 -1.28 -17 1 12 0.48 -0.34 7 1 12 -3.85 -0.34 -17 3 12 -3.36 -3.68 7 3 12 3.92 3.61 -17 5 12 -1.03 -2.36 6 10 12 -0.14 -1.76 5 13 12 -2.87 4.02 -15 15 12 0.34 -2.65 5 15 12 2.39 2.79 -14 18 12 1.72 2.16 4 18 12 0.21 -0.62 -12 22 12 0.36 -1.30 2 22 12 -1.62 1.23 1 23 12 -1.60 2.47 -5 27 12 -0.29 -0.25 5 9 13 -0.58 1.34 4 14 13 2.23 -0.77 3 17 13 0.54 -0.09 -13 19 13 -0.95 -5.53 -12 20 13 -1.25 -2.04 1 21 13 0.18 1.79 0 22 13 -1.09 1.73 -2 24 13 -1.25 2.14 -7 25 13 0.18 -0.21 -5 25 13 0.09 0.92 -4 0 14 4.90 -1.41 -16 6 14 -2.31 0.02 4 6 14 -0.28 -0.12 4 8 14 0.99 -0.19 3 11 14 -2.09 2.00 -13 17 14 -2.28 2.69 -12 18 14 1.22 -1.22 -11 19 14 3.15 -0.12 -5 23 14 1.32 -0.10 3 1 15 -0.20 0.14 3 3 15 -0.83 -2.97 -15 7 15 1.51 2.84 2 10 15 -0.93 -0.19 -14 12 15 -1.16 -1.90 1 13 15 1.29 0.25 -13 15 15 0.98 1.95 -12 16 15 -1.69 -0.87 -1 17 15 -2.84 2.07 -10 18 15 -1.48 -4.42 -2 18 15 -2.62 0.05 -3 19 15 -0.19 -1.23 -4 20 15 0.44 -5.67 -7 21 15 0.20 1.27 -5 21 15 1.33 -3.55 -14 0 16 -1.14 0.18 -14 2 16 -3.79 -0.05 -14 4 16 0.58 1.51 1 5 16 -0.96 2.12 -14 6 16 0.18 1.53 -14 8 16 -0.34 1.67 0 10 16 -2.87 -1.36 -1 13 16 0.09 -1.77 -12 14 16 -0.27 1.89 -11 15 16 0.81 1.02 -10 16 16 1.36 -0.86 -9 17 16 -1.49 1.59 -5 17 16 -1.08 -1.52 -8 18 16 -0.15 -2.57 -6 18 16 -0.45 -2.65 -13 5 17 0.52 1.56 -1 5 17 -0.60 -0.25 -13 7 17 -2.24 -1.48 -12 10 17 -0.42 -2.90 -3 11 17 0.32 -3.79 -8 14 17 -2.19 1.22 -6 14 17 1.62 -0.70 -4 0 18 1.85 2.58 -4 2 18 -3.31 1.44 -4 4 18 -3.46 0.40 -11 5 18 -2.85 -1.19 -5 7 18 -0.14 1.72 -10 8 18 0.76 -0.08 -6 8 18 0.55 2.55 -9 9 18 0.39 -1.11 -7 9 18 2.37 -1.06 0 0 0 0.00 0.00 # SQUEEZE RESULTS (Version = 50315) # 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 ; _platon_squeeze_void_probe_radius 1.20 _iucr_refine_fcf_details ; data_2023uniandes_cu_05_pca-9_sq_CCDC1 _computing_structure_refinement 'olex2.refine 1.5-dev (Bourhis et al., 2015)' _shelx_refln_list_code 4 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x,-y,z+1/2 3 x+1/2,y+1/2,z 4 x+1/2,-y+1/2,z+1/2 _space_group_crystal_system monoclinic _space_group_IT_number 9 _space_group_name_H-M_alt 'C 1 c 1' _space_group_name_Hall ' C -2yc' _symmetry_space_group_name_H-M 'C 1 c 1' _symmetry_space_group_name_Hall ' C -2yc' _symmetry_Int_Tables_number 9 _cell_length_a 13.9608(13) _cell_length_b 27.9958(19) _cell_length_c 14.7493(11) _cell_angle_alpha 90 _cell_angle_beta 116.436(11) _cell_angle_gamma 90 _cell_volume 5161.9(9) loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_calc _refln_F_squared_meas _refln_F_squared_sigma _refln_F_squared_weight _refln_observed_status -11 15 13 6023.470 5058.670 624.306 37.680 o -11 17 13 8246.700 6442.410 654.410 27.764 o -11 17 14 5533.730 4318.200 451.543 59.925 o -11 19 13 5624.370 4539.050 497.414 52.698 o -11 21 12 3425.160 2975.020 419.002 92.832 o -11 25 4 2354.520 2376.710 402.190 115.922 o -11 25 5 3807.700 3602.300 454.215 76.486 o -10 12 13 4472.860 3769.010 667.046 40.785 o -10 12 14 567.953 795.144 363.970 172.075 o -10 12 15 8283.480 7222.990 668.820 26.196 o -10 14 13 7825.860 6528.990 790.622 23.082 o -10 14 14 8250.200 7916.680 778.286 21.745 o -10 14 15 1897.900 1491.540 323.979 183.735 o -10 16 13 1877.200 1907.690 448.545 102.978 o -10 16 14 16027.400 14905.100 991.558 8.611 o -10 16 15 7574.010 5081.390 487.766 41.787 o -10 18 13 10086.100 9083.670 842.155 16.910 o -10 18 14 358.327 580.175 278.951 294.421 o -10 20 7 12636.700 11545.600 1083.380 10.435 o -10 20 13 8835.010 8586.270 732.046 21.686 o -10 20 14 8559.310 7421.790 561.556 29.652 o -10 22 7 8505.010 7386.420 831.538 20.148 o -10 22 8 1092.600 756.528 333.621 197.326 o -10 22 12 1377.890 1176.680 340.567 181.915 o -10 22 13 6901.730 5750.300 513.320 41.446 o -10 24 6 27.547 -308.046 308.046 245.500 o -10 24 7 373.422 62.387 268.929 319.857 o -10 24 8 9824.940 8897.900 790.353 18.473 o -10 24 12 57.746 -48.563 161.805 889.481 o -10 26 5 1308.720 1522.630 390.158 140.672 o -10 26 6 376.546 256.380 230.592 431.669 o -10 26 7 27.323 -6.598 220.311 479.952 o -10 28 2 364.754 255.344 198.917 577.712 o -10 28 3 40.298 -243.945 243.945 391.445 o -10 28 4 1821.960 1149.430 277.841 244.869 o -10 28 5 896.160 995.768 274.910 285.335 o -9 -19 -5 1105.900 189.455 230.414 404.499 o -9 -17 -6 174.226 -102.842 210.305 525.612 o -9 7 15 13262.300 13242.600 1054.220 9.929 o -9 9 13 4143.520 4147.410 761.208 33.272 o -9 9 14 497.051 328.721 311.273 237.097 o -9 9 15 2518.800 2037.790 471.501 89.119 o -9 9 16 1985.520 2075.770 388.882 129.580 o -9 11 13 2623.200 2364.740 539.128 69.356 o -9 11 14 8491.130 8756.000 934.892 16.744 o -9 11 15 1665.260 1502.710 383.302 141.051 o -9 11 16 29.402 -166.596 238.166 410.690 o -9 13 13 4339.400 4824.880 749.656 33.073 o -9 13 14 9316.590 8425.280 901.458 16.828 o -9 13 15 6216.000 5668.480 661.575 33.590 o -9 13 16 105.124 -37.236 191.222 636.510 o -9 15 13 773.104 824.643 426.004 125.339 o -9 15 14 9261.800 8558.550 879.357 17.307 o -9 15 15 6935.940 6511.060 671.366 30.052 o -9 15 16 2035.970 1449.890 278.669 229.594 o -9 17 13 3766.560 3249.090 630.993 47.647 o -9 17 14 3715.750 3257.570 528.872 63.145 o -9 17 15 6726.890 5462.200 555.341 39.630 o -9 19 8 3966.980 3556.080 705.576 38.767 o -9 19 9 157.991 58.356 319.549 227.905 o -9 19 13 1926.610 1976.120 471.659 93.561 o -9 19 14 1919.390 1806.260 394.110 129.275 o -9 19 15 1070.010 1069.260 247.708 335.671 o -9 21 7 3635.190 3289.630 659.752 44.599 o -9 21 8 4570.680 3551.850 683.065 39.325 o -9 21 9 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-9 -4 657.972 768.881 285.792 273.847 o 15 -9 -3 1037.470 1939.910 509.097 85.722 o 15 -9 -2 3535.290 3341.440 4553.650 1.119 o 15 -9 -1 933.396 -191.982 191.982 588.613 o 15 -7 -14 2146.370 2012.040 335.744 162.043 o 15 -7 -13 19.299 31.535 167.799 827.286 o 15 -7 -12 1413.480 1683.540 282.239 243.823 o 15 -7 -11 1637.720 1621.770 328.112 184.328 o 15 -7 -10 5083.510 4704.210 423.554 66.162 o 15 -7 -9 1598.090 1671.320 414.812 122.246 o 15 -7 -8 535.962 481.845 209.244 510.126 o 15 -7 -7 4626.250 5082.170 413.821 70.229 o 15 -7 -6 9351.460 11105.700 1699.780 6.502 o 15 -7 -5 7163.030 7311.360 643.749 29.866 o 15 -7 -4 3691.940 2026.200 381.845 108.376 o 15 -7 -3 3591.450 870.861 1748.470 7.496 o 15 -7 -2 12793.700 26931.500 13920.200 0.119 o 15 -7 -1 11564.000 24864.000 16490.000 0.085 o 15 -5 -15 2638.900 2676.290 313.522 157.723 o 15 -5 -14 3989.790 3540.770 557.387 56.227 o 15 -5 -13 1185.800 1101.240 204.511 454.622 o 15 -5 -12 1895.010 1971.820 277.763 226.006 o 15 -5 -11 4698.010 5149.850 421.986 67.859 o 15 -5 -10 2348.530 2462.230 280.522 196.229 o 15 -5 -9 299.786 257.858 198.958 580.115 o 15 -5 -8 727.485 565.911 214.485 473.573 o 15 -5 -7 4641.910 5717.530 502.885 54.350 o 15 -5 -6 10453.500 14049.900 773.391 15.006 o 15 -5 -5 5943.340 9225.460 1067.340 15.664 o 15 -5 -4 3615.570 863.269 1849.710 6.709 o 15 -5 -3 605.468 118.298 1179.200 16.737 o 15 -5 -2 1107.100 2341.530 327.593 188.596 o 15 -5 -1 2592.380 3061.830 1499.990 10.115 o 15 -3 -15 2034.410 2048.550 288.244 207.431 o 15 -3 -14 4492.810 4637.820 418.437 72.794 o 15 -3 -13 4059.460 4359.720 398.520 83.075 o 15 -3 -12 3168.370 3582.700 467.802 78.789 o 15 -3 -11 3697.640 3761.770 390.680 93.244 o 15 -3 -10 906.078 760.940 210.455 471.001 o 15 -3 -9 252.342 158.457 195.601 603.492 o 15 -3 -8 489.200 552.324 216.952 476.433 o 15 -3 -7 1666.900 1408.540 263.278 268.150 o 15 -3 -6 4956.360 5501.080 473.259 56.888 o 15 -3 -5 5425.100 7502.500 723.892 29.599 o 15 -3 -4 1147.180 1818.660 575.866 67.559 o 15 -3 -3 634.563 461.755 253.984 348.502 o 15 -3 -2 3079.930 1577.270 1543.050 9.596 o 15 -3 -1 3575.810 2366.430 642.882 48.129 o 15 -1 -15 1141.500 1037.160 209.536 443.623 o 15 -1 -14 1656.140 1552.430 232.806 320.535 o 15 -1 -13 969.893 1035.400 231.042 386.386 o 15 -1 -12 1582.350 1447.010 294.219 225.799 o 15 -1 -11 1889.550 2040.630 361.742 148.095 o 15 -1 -10 458.307 191.185 197.849 580.926 o 15 -1 -9 2149.260 2412.730 394.694 121.998 o 15 -1 -8 1993.000 1893.070 262.371 243.100 o 15 -1 -7 126.982 -180.477 180.477 714.132 o 15 -1 -6 1682.650 1370.780 297.566 219.649 o 15 -1 -5 795.640 526.780 252.680 345.900 o 15 -1 -4 244.160 -195.441 195.441 606.942 o 15 -1 -3 552.761 -200.426 200.426 566.483 o 15 -1 -2 604.492 -252.061 252.061 360.203 o 15 -1 -1 3212.490 2569.320 414.955 98.980 o 15 1 0 3725.620 2238.720 249.989 171.521 o 15 1 1 2684.210 1405.260 199.647 307.783 o 15 3 0 5181.750 4304.690 332.696 83.585 o 15 3 1 2399.230 1756.410 1252.820 14.532 o 15 5 0 4884.820 6147.830 3263.570 2.147 o 15 5 1 5866.410 21748.800 14082.800 0.117 o 16 -14 -9 521.659 307.826 172.705 745.426 o 16 -14 -8 5727.850 5599.930 498.188 49.007 o 16 -14 -7 1621.940 1784.890 320.883 189.842 o 16 -12 -10 8224.580 7297.640 560.902 30.856 o 16 -12 -9 68.216 88.088 198.843 588.628 o 16 -12 -8 5802.370 6463.520 612.300 36.986 o 16 -12 -7 3371.450 3759.910 505.560 68.171 o 16 -12 -6 939.182 866.171 297.283 247.154 o 16 -12 -5 2851.440 3156.400 442.978 90.463 o 16 -10 -12 346.081 264.561 150.678 994.790 o 16 -10 -11 2308.900 2046.290 477.398 88.718 o 16 -10 -10 2141.210 2434.460 672.311 47.814 o 16 -10 -9 11637.400 11183.800 518.014 19.484 o 16 -10 -8 1440.060 1660.510 432.358 114.742 o 16 -10 -7 2876.670 3672.650 542.238 64.106 o 16 -10 -6 372.061 327.365 261.808 335.494 o 16 -10 -5 572.999 700.785 325.989 213.863 o 16 -10 -4 41.557 -178.792 248.558 377.049 o 16 -8 -13 326.150 470.884 173.275 751.278 o 16 -8 -12 201.871 231.735 174.470 757.484 o 16 -8 -11 5145.790 5177.980 648.255 38.372 o 16 -8 -10 3319.820 3340.090 399.505 98.138 o 16 -8 -9 8.363 -114.082 143.707 1128.060 o 16 -8 -8 1906.070 1842.280 264.215 245.800 o 16 -8 -7 2111.190 1531.730 391.542 130.031 o 16 -8 -6 96.725 -300.927 314.912 234.848 o 16 -8 -5 529.786 139.818 325.461 217.627 o 16 -8 -4 373.912 267.309 254.928 354.090 o 16 -6 -13 389.246 302.509 162.936 848.364 o 16 -6 -12 225.497 351.490 215.132 497.954 o 16 -6 -11 4.692 -64.963 150.405 1029.830 o 16 -6 -10 2495.540 1864.560 270.566 211.958 o 16 -6 -9 2459.710 2400.850 308.134 170.302 o 16 -6 -8 1498.120 1209.430 247.909 309.498 o 16 -6 -7 3005.690 2717.710 315.267 146.611 o 16 -6 -6 165.380 -377.489 377.489 163.389 o 16 -6 -5 864.223 194.338 187.458 612.619 o 16 -6 -4 370.280 288.736 269.435 317.295 o 16 -6 -2 987.684 341.650 195.033 551.652 o 16 -4 -14 9372.780 9642.010 560.668 24.687 o 16 -4 -13 3073.930 3346.470 413.413 96.543 o 16 -4 -12 55.329 239.380 230.165 438.965 o 16 -4 -11 314.122 236.928 162.015 868.196 o 16 -4 -10 1005.180 1043.700 234.591 373.839 o 16 -4 -9 74.556 98.933 182.172 700.969 o 16 -4 -8 908.993 840.191 235.488 382.081 o 16 -4 -7 1184.290 1089.210 240.192 347.555 o 16 -4 -6 5525.690 6895.450 818.254 25.293 o 16 -4 -5 993.546 2188.150 523.048 81.118 o 16 -4 -4 7002.470 18506.600 10206.200 0.222 o 16 -4 -3 886.054 3674.040 2590.570 3.459 o 16 -4 -2 1457.590 2819.610 272.886 232.614 o 16 -2 -14 3405.250 3511.640 362.386 108.592 o 16 -2 -13 2594.720 2503.380 264.954 200.112 o 16 -2 -12 1762.870 1793.060 256.554 264.994 o 16 -2 -11 367.208 531.424 199.855 565.544 o 16 -2 -10 859.277 711.676 180.262 627.826 o 16 -2 -9 15961.100 17347.400 803.840 9.165 o 16 -2 -8 620.868 442.537 336.817 201.421 o 16 -2 -7 153.753 -127.307 155.644 958.748 o 16 -2 -6 2161.860 1537.120 495.422 85.565 o 16 -2 -5 652.920 303.373 319.959 223.156 o 16 -2 -4 3552.340 15737.700 9419.990 0.261 o 16 -2 -3 4754.350 18147.800 11560.900 0.174 o 16 -2 -2 5225.270 14164.300 10257.400 0.220 o 16 -2 -1 8875.760 19856.000 13196.900 0.133 o 16 0 -14 4987.350 5238.460 426.895 64.180 o 16 0 -12 721.157 736.494 286.298 271.921 o 16 0 -10 15435.400 18163.400 1154.410 7.257 o 16 0 -8 9639.690 11865.200 2465.770 3.407 o 16 0 -6 2287.630 1349.690 448.697 101.845 o 16 0 -4 14098.900 29290.000 921.259 6.793 o 16 0 -2 2440.600 6058.930 410.064 89.046 o 17 -7 -8 247.374 -165.617 237.322 412.234 o 17 -7 -7 197.940 99.523 183.451 688.314 o 17 -7 -6 324.923 80.160 211.071 518.082 o 17 -5 -9 1703.220 1825.640 328.008 180.639 o 17 -5 -8 351.024 89.469 195.162 603.889 o 17 -5 -7 271.698 426.838 221.156 469.261 o 17 -3 -11 770.193 607.632 189.609 588.966 o 17 -3 -8 1375.530 787.868 267.502 286.417 o ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 x,y,z 2 x,-y,z+1/2 3 x+1/2,y+1/2,z 4 x+1/2,-y+1/2,z+1/2 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_refinement_flags_posn _atom_site_refinement_flags_adp Zr1 Zr 0.06637(9) 0.53712(3) 0.43691(7) 0.0301(2) Uani 1.000000 . . O16D O 0.2331(17) 0.5083(5) 0.7716(11) 0.092(5) Uani 1.000000 . U O15D O 0.3503(16) 0.5333(7) 0.7023(16) 0.105(6) Uani 1.000000 . U O14D O 0.2160(9) 0.5862(3) 0.6954(7) 0.041(2) Uani 1.000000 . U O13D O 0.1742(8) 0.5136(3) 0.5933(6) 0.042(2) Uani 1.000000 . U O12D O -0.0900(12) 0.4473(4) 0.1517(9) 0.064(3) Uani 1.000000 . U O11D O -0.2065(12) 0.4906(5) 0.1988(12) 0.074(3) Uani 1.000000 . U O10D O -0.0210(11) 0.4866(3) 0.3109(7) 0.053(3) Uani 1.000000 . U O9D O -0.0833(10) 0.5340(3) 0.1578(7) 0.045(2) Uani 1.000000 . U O8E O 0.3265(8) 0.6501(4) 0.6485(8) 0.040(2) Uani 1.000000 . . C8E C 0.5080(16) 0.6443(8) 0.6828(15) 0.068(6) Uani 1.000000 . . H8Ea H 0.5156(16) 0.6494(8) 0.7501(15) 0.102(8) Uiso 1.000000 R . H8Eb H 0.5448(16) 0.6155(8) 0.6815(15) 0.102(8) Uiso 1.000000 R . H8Ec H 0.5381(16) 0.6708(8) 0.6632(15) 0.102(8) Uiso 1.000000 R . O8D O -0.1648(8) 0.7394(4) 0.0181(7) 0.042(2) Uani 1.000000 . . O8C O 0.1440(9) 0.7642(4) 0.3376(7) 0.046(2) Uani 1.000000 D . H8Ca H 0.204(5) 0.751(2) 0.352(13) 0.069(4) Uiso 1.000000 DR . H8Cb H 0.163(11) 0.787(3) 0.380(9) 0.069(4) Uiso 1.000000 DR . O7E O 0.3704(7) 0.6328(4) 0.5199(7) 0.038(2) Uani 1.000000 . . C7E C 0.4015(12) 0.6401(5) 0.6168(10) 0.039(3) Uani 1.000000 . . O7D O 0.0119(9) 0.7095(4) 0.0658(9) 0.048(2) Uani 1.000000 . . O7C O -0.0988(8) 0.7676(4) 0.3267(7) 0.045(2) Uani 1.000000 . . H7Ca H -0.155(5) 0.7539(9) 0.322(13) 0.068(3) Uiso 1.000000 GR . H7Cb H -0.117(9) 0.779(4) 0.268(5) 0.068(3) Uiso 1.000000 GR . O6E O 0.2027(9) 0.6144(5) 0.2183(7) 0.047(3) Uani 1.000000 . . C6E C 0.1409(15) 0.6165(6) 0.0418(12) 0.053(4) Uani 1.000000 . . H6Ea H 0.2148(15) 0.6243(6) 0.0632(12) 0.079(6) Uiso 1.000000 R . H6Eb H 0.1234(15) 0.5879(6) 0.0017(12) 0.079(6) Uiso 1.000000 R . H6Ec H 0.0968(15) 0.6423(6) 0.0022(12) 0.079(6) Uiso 1.000000 R . O6D O -0.1175(7) 0.6640(3) 0.0978(7) 0.0330(18) Uani 1.000000 . . O6C O -0.2375(9) 0.6841(4) 0.3946(8) 0.046(2) Uani 1.000000 . . H6Ca H -0.229(4) 0.709(3) 0.430(7) 0.069(4) Uiso 1.000000 GR . H6Cb H -0.302(4) 0.686(3) 0.348(7) 0.069(4) Uiso 1.000000 GR . O5E O 0.0291(8) 0.5982(3) 0.1197(7) 0.037(2) Uani 1.000000 . . C5E C 0.1217(14) 0.6088(5) 0.1331(11) 0.043(3) Uani 1.000000 . . O5D O -0.0436(9) 0.7357(4) 0.1932(6) 0.043(2) Uani 1.000000 . . O5C O -0.2074(8) 0.5753(4) 0.4595(8) 0.043(2) Uani 1.000000 . . H5Ca H -0.254(9) 0.562(4) 0.4063(13) 0.065(3) Uiso 1.000000 GR . H5Cb H -0.244(10) 0.5898(6) 0.484(11) 0.065(3) Uiso 1.000000 GR . O4E O -0.2263(8) 0.5997(4) 0.1495(7) 0.041(2) Uani 1.000000 . . C4E C -0.4061(15) 0.5858(11) 0.1232(14) 0.087(9) Uani 1.000000 . . H4Ea H -0.4152(15) 0.5798(11) 0.0557(14) 0.130(13) Uiso 1.000000 R . H4Eb H -0.4274(15) 0.5582(11) 0.1481(14) 0.130(13) Uiso 1.000000 R . H4Ec H -0.4496(15) 0.6126(11) 0.1223(14) 0.130(13) Uiso 1.000000 R . O4D O 0.1833(8) 0.8026(4) 0.6462(8) 0.042(2) Uani 1.000000 . U S4D S 0.2348(4) 0.53509(13) 0.6944(3) 0.0537(10) Uani 1.000000 . U O4C O -0.0330(8) 0.4890(4) 0.4808(7) 0.041(2) Uani 1.000000 . . H4Ca H 0.005(3) 0.477(4) 0.539(5) 0.061(3) Uiso 1.000000 GR . H4Cb H -0.081(7) 0.5050(9) 0.488(11) 0.061(3) Uiso 1.000000 GR . O4B O 0.0126(7) 0.6707(3) 0.4660(6) 0.0315(17) Uani 1.000000 . . O1A O 0.0197(7) 0.5856(3) 0.5321(6) 0.0336(18) Uani 1.000000 . . H1A H 0.0104(7) 0.5729(3) 0.5777(6) 0.040(2) Uiso 1.000000 R . O2A O -0.1140(7) 0.6677(3) 0.2863(6) 0.0313(17) Uani 1.000000 . . H2A H -0.1694(7) 0.6812(3) 0.2478(6) 0.038(2) Uiso 1.000000 R . O1D O 0.1880(8) 0.7173(3) 0.6367(7) 0.0363(18) Uani 1.000000 . U S1D S 0.1201(2) 0.76150(10) 0.5980(2) 0.0337(6) Uani 1.000000 . U O1C O 0.3111(9) 0.6805(4) 0.3494(8) 0.045(2) Uani 1.000000 . . O1B O 0.1737(9) 0.5948(3) 0.4832(6) 0.038(2) Uani 1.000000 . . Zr2 Zr -0.05358(8) 0.60754(3) 0.21510(7) 0.0290(2) Uani 1.000000 . . O4A O 0.1012(7) 0.5643(3) 0.3106(6) 0.0318(17) Uani 1.000000 . . H4A H 0.1177(7) 0.5441(3) 0.2799(6) 0.038(2) Uiso 1.000000 R . O3A O 0.1910(7) 0.6849(3) 0.4645(6) 0.0292(16) Uani 1.000000 . . H3A H 0.2393(7) 0.7046(3) 0.4884(6) 0.035(2) Uiso 1.000000 R . Zr3 Zr 0.03010(8) 0.71340(3) 0.35784(7) 0.0282(2) Uani 1.000000 D . Zr4 Zr 0.15253(9) 0.64313(3) 0.58019(7) 0.0281(2) Uani 1.000000 . . Zr5 Zr 0.21832(8) 0.62386(3) 0.37992(7) 0.0288(2) Uani 1.000000 . . Zr6 Zr -0.11963(9) 0.62781(3) 0.41618(7) 0.0292(2) Uani 1.000000 . . O1E O 0.0710(7) 0.6515(3) 0.6757(7) 0.0328(18) Uani 1.000000 . . C1E C -0.0288(14) 0.6577(6) 0.6575(11) 0.045(3) Uani 1.000000 . . O2C O 0.3280(8) 0.5646(4) 0.3882(8) 0.043(2) Uani 1.000000 . . H2Ca H 0.3930(8) 0.5736(18) 0.419(11) 0.065(3) Uiso 1.000000 GR . H2Cb H 0.319(9) 0.558(4) 0.3286(14) 0.065(3) Uiso 1.000000 GR . O2B O 0.0712(7) 0.6552(3) 0.2944(6) 0.0277(16) Uani 1.000000 . . O2D O 0.0885(8) 0.7649(3) 0.4883(7) 0.041(2) Uani 1.000000 . U S2D S -0.0784(3) 0.71217(11) 0.0921(2) 0.0346(6) Uani 1.000000 . . O2E O -0.1038(8) 0.6506(4) 0.5694(7) 0.040(2) Uani 1.000000 . . C2E C -0.0490(13) 0.6688(10) 0.7445(14) 0.075(7) Uani 1.000000 . . H2Ea H -0.081(14) 0.700(3) 0.736(7) 0.113(10) Uiso 1.000000 GR . H2Eb H -0.096(12) 0.645(4) 0.750(9) 0.113(10) Uiso 1.000000 GR . H2Ec H 0.017(2) 0.668(7) 0.805(2) 0.113(10) Uiso 1.000000 GR . O3E O -0.2661(8) 0.6057(4) 0.2833(7) 0.041(2) Uani 1.000000 . . C3E C -0.2886(13) 0.5970(6) 0.1921(11) 0.043(3) Uani 1.000000 . . O3D O 0.0241(8) 0.7588(3) 0.6154(8) 0.0424(19) Uani 1.000000 . U S3D S -0.0966(3) 0.48845(12) 0.2032(2) 0.0493(8) Uani 1.000000 . U O3C O 0.1798(10) 0.4827(4) 0.4316(9) 0.053(3) Uani 1.000000 . . H3Ca H 0.224(9) 0.475(5) 0.4917(9) 0.080(4) Uiso 1.000000 GR . H3Cb H 0.218(10) 0.4954(19) 0.406(13) 0.080(4) Uiso 1.000000 GR . O3B O -0.0584(7) 0.5818(3) 0.3453(6) 0.0327(17) Uani 1.000000 . . H1Ca H 0.342(11) 0.6687(14) 0.317(11) 0.068(3) Uiso 1.000000 GR . H1Cb H 0.362(8) 0.690(4) 0.4050(13) 0.068(3) Uiso 1.000000 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_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Zr1 0.0454(6) 0.0248(4) 0.0199(4) 0.0007(4) 0.0144(4) 0.0006(3) O16D 0.171(14) 0.059(7) 0.048(6) -0.007(6) 0.051(6) 0.016(5) O15D 0.100(11) 0.113(14) 0.087(12) 0.025(7) 0.027(6) 0.015(10) O14D 0.064(6) 0.032(4) 0.026(4) 0.011(4) 0.020(4) 0.013(3) O13D 0.057(6) 0.037(4) 0.021(4) 0.008(4) 0.007(4) 0.003(3) O12D 0.102(8) 0.040(4) 0.039(5) -0.007(3) 0.023(4) -0.011(3) O11D 0.086(5) 0.068(7) 0.065(7) -0.020(3) 0.032(3) -0.013(5) O10D 0.104(6) 0.029(4) 0.019(3) -0.019(3) 0.019(3) -0.008(2) O9D 0.072(6) 0.035(4) 0.021(4) -0.010(3) 0.015(3) -0.010(2) O8E 0.029(5) 0.053(6) 0.034(5) -0.005(4) 0.009(4) 0.002(4) C8E 0.058(11) 0.083(14) 0.045(9) -0.004(9) 0.006(8) -0.020(9) O8D 0.049(5) 0.043(5) 0.029(4) 0.007(4) 0.013(4) 0.006(4) O8C 0.049(6) 0.052(6) 0.027(4) -0.016(5) 0.008(4) 0.004(4) O7E 0.029(5) 0.051(5) 0.029(4) -0.009(4) 0.009(4) -0.002(4) C7E 0.050(8) 0.040(7) 0.018(5) -0.005(6) 0.008(5) -0.005(5) O7D 0.059(6) 0.041(5) 0.053(6) -0.003(4) 0.034(5) 0.008(4) O7C 0.049(6) 0.050(6) 0.034(5) 0.003(4) 0.015(4) -0.013(4) O6E 0.048(6) 0.069(7) 0.019(4) -0.003(5) 0.012(4) 0.002(4) C6E 0.087(12) 0.054(8) 0.038(7) 0.001(8) 0.046(8) -0.004(6) O6D 0.037(5) 0.032(4) 0.026(4) 0.001(3) 0.010(4) 0.007(3) O6C 0.057(6) 0.049(6) 0.030(4) 0.007(5) 0.018(4) -0.009(4) O5E 0.052(6) 0.042(5) 0.023(4) -0.011(4) 0.021(4) -0.008(4) C5E 0.069(10) 0.043(7) 0.030(6) -0.002(7) 0.034(7) -0.006(5) O5D 0.065(6) 0.038(5) 0.017(4) -0.003(4) 0.010(4) 0.002(3) O5C 0.039(5) 0.046(5) 0.041(5) -0.005(4) 0.014(4) 0.012(4) O4E 0.042(5) 0.046(5) 0.027(4) -0.010(4) 0.010(4) -0.003(4) C4E 0.049(11) 0.17(2) 0.042(9) -0.064(13) 0.023(8) -0.039(12) O4D 0.043(4) 0.037(4) 0.034(4) -0.003(2) 0.008(3) -0.006(2) S4D 0.078(3) 0.0377(16) 0.0260(14) 0.0122(16) 0.0062(15) 0.0080(12) O4C 0.051(6) 0.043(5) 0.029(4) -0.004(4) 0.019(4) 0.006(4) O4B 0.042(5) 0.028(4) 0.028(4) -0.010(3) 0.018(4) -0.006(3) O1A 0.050(5) 0.028(4) 0.020(4) 0.000(3) 0.013(3) -0.004(3) O2A 0.032(4) 0.037(4) 0.023(4) -0.007(3) 0.010(3) 0.004(3) O1D 0.048(5) 0.032(4) 0.028(4) -0.004(2) 0.015(3) -0.003(2) S1D 0.0377(14) 0.0322(13) 0.0272(12) -0.0006(11) 0.0108(10) -0.0058(10) O1C 0.064(6) 0.046(5) 0.030(4) -0.011(5) 0.025(5) 0.003(4) O1B 0.066(6) 0.031(4) 0.015(3) -0.010(4) 0.017(4) -0.000(3) Zr2 0.0392(5) 0.0281(4) 0.0176(4) -0.0019(4) 0.0110(4) 0.0003(3) O4A 0.041(5) 0.029(4) 0.022(4) -0.006(3) 0.011(3) -0.001(3) O3A 0.044(5) 0.028(4) 0.015(3) -0.004(3) 0.012(3) -0.003(3) Zr3 0.0369(5) 0.0254(4) 0.0196(4) 0.0005(4) 0.0101(4) 0.0009(3) Zr4 0.0381(5) 0.0266(4) 0.0174(4) 0.0005(4) 0.0104(4) -0.0004(3) Zr5 0.0360(5) 0.0296(5) 0.0196(4) 0.0006(4) 0.0114(4) -0.0012(3) Zr6 0.0365(5) 0.0307(5) 0.0188(4) -0.0008(4) 0.0109(4) 0.0013(3) O1E 0.024(4) 0.048(5) 0.025(4) -0.001(4) 0.010(3) -0.003(4) C1E 0.069(10) 0.042(7) 0.023(6) 0.002(7) 0.019(6) 0.000(5) O2C 0.038(5) 0.045(5) 0.038(5) 0.012(4) 0.010(4) -0.005(4) O2B 0.036(4) 0.024(4) 0.017(3) -0.006(3) 0.006(3) -0.004(3) O2D 0.060(5) 0.031(4) 0.025(3) -0.007(3) 0.012(2) -0.008(2) S2D 0.0424(16) 0.0358(14) 0.0247(12) 0.0013(12) 0.0142(12) 0.0066(10) O2E 0.034(5) 0.068(7) 0.022(4) 0.002(4) 0.015(4) -0.001(4) C2E 0.042(8) 0.15(2) 0.048(9) -0.008(10) 0.029(7) -0.043(11) O3E 0.045(5) 0.057(6) 0.017(4) -0.005(4) 0.009(4) 0.001(4) C3E 0.047(8) 0.050(8) 0.027(6) -0.016(6) 0.013(6) -0.004(5) O3D 0.050(4) 0.037(4) 0.041(4) -0.005(3) 0.021(2) -0.015(3) S3D 0.077(2) 0.0335(14) 0.0299(14) -0.0118(14) 0.0165(14) -0.0062(11) O3C 0.068(7) 0.053(6) 0.052(6) 0.025(5) 0.038(6) 0.013(5) O3B 0.037(4) 0.044(5) 0.014(3) 0.005(4) 0.009(3) 0.005(3) loop_ _atom_type_symbol _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_Cromer_Mann_a1 _atom_type_scat_Cromer_Mann_a2 _atom_type_scat_Cromer_Mann_a3 _atom_type_scat_Cromer_Mann_a4 _atom_type_scat_Cromer_Mann_b1 _atom_type_scat_Cromer_Mann_b2 _atom_type_scat_Cromer_Mann_b3 _atom_type_scat_Cromer_Mann_b4 _atom_type_scat_Cromer_Mann_c _atom_type_scat_source _atom_type_scat_dispersion_source C 0.01788 0.00908 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870 51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236 57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' O 0.04960 0.03234 3.04850 2.28680 1.54630 0.86700 13.27710 5.70110 0.32390 32.90890 0.25080 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' S 0.33376 0.55840 6.90530 5.20340 1.43790 1.58630 1.46790 22.21510 0.25360 56.17200 0.86690 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' Zr -0.17084 2.25071 17.87650 10.94800 5.41732 3.65721 1.27618 11.91600 0.11762 87.66270 2.06929 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)' 'Brennan, Cowan, Rev. Sci. Instrum., 1992, 63, 850' loop_ _diffrn_refln_index_h _diffrn_refln_index_k _diffrn_refln_index_l _diffrn_refln_intensity_net _diffrn_refln_intensity_u _diffrn_refln_scale_group_code 0 0 2 2623.19 798.095 1 0 0 3 249.421 784.656 1 0 0 4 478793 11245.8 1 0 0 5 31.1866 751.543 1 0 0 6 130193 7410.63 1 0 0 7 7.85612 967.163 1 0 0 8 108987 8108.53 1 0 0 9 -428.852 1154.27 1 0 0 10 27662 2430.67 4 0 0 10 29874.3 2570.47 13 0 0 10 29302.1 4366 2 0 0 11 -260.572 860.012 4 0 0 11 2369.94 1634.65 2 0 0 12 22134.9 2265.68 4 0 0 12 22793.7 2431.72 14 0 0 13 -543.117 691.024 4 0 0 13 311.173 704.998 14 0 0 14 56472 3167.37 4 0 0 14 61795.4 3511.12 14 0 0 15 52.0604 439.708 14 0 0 16 3471.47 645.009 14 0 0 -16 2859.92 497.168 17 0 -2 1 883400 8609.19 1 0 -2 2 22736.7 1873.14 1 0 2 2 21996.7 1753.21 1 0 2 3 14467.1 1786.18 1 0 -2 3 14268.8 1758.78 1 0 2 4 324065 9408.48 1 0 -2 4 314481 9140.26 1 0 -2 5 89441.2 5496.47 1 0 2 5 88756.3 5570.46 1 0 -2 6 6722.67 1870.59 1 0 2 6 4885.51 1551.93 1 0 2 7 33832.1 4295.17 1 0 -2 7 37169.5 4322.82 1 0 -2 8 85062.8 7181.34 1 0 -2 9 20570.8 3853.51 1 0 2 9 20888.1 3285.47 2 0 2 10 28801.3 2528.6 4 0 -2 10 26448.6 2382.89 4 0 2 10 27803.6 2515.08 13 0 -2 10 29120.1 5008 1 0 2 10 26213.5 3905.21 2 0 -2 10 26234.8 4078.19 2 0 2 11 38167.7 2958.61 4 0 -2 11 39002.1 2956.66 4 0 -2 11 44434.5 3274.66 14 0 2 11 42719.8 3138.02 13 0 -2 11 43420.4 5738.52 2 0 2 12 6650.42 1359.06 4 0 -2 12 7107.17 1385.63 4 0 -2 12 7422.77 1439.23 14 0 2 13 30278.1 2558.71 4 0 -2 13 29220.1 2531.09 4 0 -2 13 31376.8 2740.3 14 0 2 13 30575.5 2659.29 14 0 2 14 793.285 604.615 4 0 -2 14 446.517 693.254 14 0 2 14 26.1856 526.626 14 0 2 15 6123.89 953.046 4 0 -2 15 6639.58 1105.66 14 0 2 15 6793.34 1090.38 14 0 2 16 10154 1033.46 14 0 -2 16 10666.9 1084.13 14 0 2 -16 9214.56 878.82 17 0 4 0 92917.5 1945.32 3 0 -4 1 3161.78 687.338 1 0 -4 2 38.5466 608.051 1 0 -4 3 43082.7 3059.86 1 0 -4 4 22679.1 2561.15 1 0 -4 5 18730 2584.82 1 0 -4 6 202967 9329.43 1 0 -4 7 13311.1 2736.51 1 0 -4 8 29477.9 4278.3 1 0 4 8 30302.9 3515.76 2 0 -4 9 10817.5 2897.98 1 0 -4 10 22405.2 2264.56 4 0 4 10 22640.8 2189.66 4 0 -4 10 23624.4 4542.47 1 0 -4 10 26441.4 2501.76 14 0 4 10 23652 2323.21 13 0 4 11 27941.3 2591.98 4 0 -4 11 30610.8 2701.41 4 0 -4 11 31411.8 2791.51 14 0 4 11 26811.3 2564.64 13 0 -4 11 32385.2 5052.72 2 0 -4 11 29159.4 4971.24 1 0 -4 12 61591.6 3724.29 4 0 4 12 65319.4 3804.29 4 0 -4 12 67430.9 4089.68 14 0 4 12 64752.6 3869.6 13 0 4 13 8805.26 1415.49 4 0 -4 13 9257.71 1473.11 4 0 -4 13 10107.4 1658.68 14 0 4 13 11683.3 1705.62 14 0 4 14 5184.97 1034.78 4 0 -4 14 3135.13 898.143 14 0 4 14 3480.06 1000.47 14 0 4 15 927.489 525.221 4 0 -4 15 1314.16 651.262 14 0 4 15 1719.28 683.818 14 0 -4 16 6918.44 672.874 6 0 4 16 7479.86 861.069 14 0 4 -16 6937.15 800.948 17 0 6 0 877.285 363.683 3 0 -6 1 25995.6 1955.86 1 0 -6 2 3750.92 1416.51 1 0 -6 3 277142 8397.38 1 0 6 3 246708 4035.84 2 0 6 4 4877.59 848.789 2 0 -6 4 5597.06 1469.92 1 0 -6 5 140535 7254.7 1 0 6 5 129580 4816.03 2 0 6 6 66592.1 3958.44 2 0 -6 6 72107.6 5639.73 1 0 -6 7 18079 3177.06 1 0 -6 8 36777.8 4803.5 1 0 -6 9 17947.5 3617.76 1 0 -6 10 31798.4 2768.43 4 0 6 10 36094.8 2853.4 4 0 -6 10 32386.3 5192.85 1 0 -6 10 38809.2 3027.1 14 0 6 10 33713.7 2736.11 13 0 -6 11 198433 6707.77 4 0 6 11 205037 6751.53 4 0 -6 11 189511 13050.9 1 0 6 11 207481 6919.2 13 0 -6 11 208980 7149.81 14 0 6 12 9438.28 1557.52 4 0 -6 12 10569.1 1730.75 14 0 6 12 8548.84 1527.83 13 0 6 13 370.232 761.946 4 0 -6 13 -419.146 853.925 14 0 6 14 1174.25 690.596 4 0 -6 14 1614.17 866.265 14 0 6 14 2221.63 837.415 14 0 6 15 11958 1226.91 4 0 6 15 11270.6 1285.99 14 0 -6 15 13239.6 1450.39 14 0 6 -16 3461.35 637.026 17 0 6 16 2937.27 539.45 14 0 8 0 434753 5912.99 3 0 -8 0 443567 8781.29 1 0 8 -1 683968 8760.97 3 0 -8 1 711035 11708.2 1 0 -8 2 13497.8 1906.57 1 0 -8 3 34691.4 3302.69 1 0 -8 4 19548.1 2671.77 1 0 -8 5 14373.5 2480.2 1 0 -8 6 124471 7633.77 1 0 -8 7 278420 12417.7 1 0 -8 8 625.682 942.866 1 0 -8 9 -570.347 1109.04 1 0 8 10 79354.9 4206.3 4 0 -8 10 82638 8364.27 1 0 -8 10 79819.4 4417.81 14 0 8 10 80505.7 4272.11 13 0 8 11 23417.5 2361.28 4 0 -8 11 24119 2500.12 14 0 8 11 24218.3 2427.14 13 0 8 12 2820.31 1017.09 4 0 -8 12 3055.36 1098.78 14 0 8 12 2658.42 956.096 13 0 8 13 4543.59 1052.32 4 0 -8 13 3551.92 1073.06 14 0 8 14 1957.29 713.349 4 0 -8 14 1153.47 605.699 14 0 8 14 2253.55 814.624 14 0 8 15 23058 1623.64 4 0 8 15 22321.7 1686.03 14 0 8 16 696.952 300.158 14 0 8 -16 1065.67 378.615 17 0 10 0 2291.71 582.045 3 0 -10 0 1602.82 778.7 1 0 -10 1 24067.4 2588.94 1 0 10 -1 29637.8 1940.98 3 0 -10 2 119841 5840.7 1 0 -10 3 86639.8 5383.49 1 0 -10 4 33106.5 3733.39 1 0 -10 5 201601 9493.03 1 0 -10 6 58403.4 5468.91 1 0 -10 7 50812.2 5645.46 1 0 -10 8 55900.3 6359.18 1 0 10 9 191.656 671.714 4 0 -10 9 -639.267 829.838 14 0 10 9 322.806 641.51 13 0 10 10 3819.78 1032.26 4 0 -10 10 955.786 1338.69 2 0 -10 10 3796.34 2136.36 1 0 -10 10 3478.49 1071.42 14 0 10 10 2278.95 990.647 13 0 10 11 1742.6 820.976 4 0 -10 11 1661.83 799.016 14 0 10 11 2904.47 1065.17 13 0 10 12 39647.5 2938.64 4 0 10 12 42365.8 3077.02 13 0 -10 12 41930.2 3332.66 14 0 10 13 10431.2 1455.43 4 0 -10 13 8334.58 1509.52 14 0 10 13 9211.8 1388.95 13 0 10 14 10357.7 1325.34 4 0 10 14 8725.84 1230.61 14 0 10 15 21142.3 1498.43 4 0 10 15 18611 1407.47 14 0 10 -15 22800.3 1711.81 17 0 -12 0 132674 6300.09 1 0 12 0 134688 4011.73 3 0 12 -1 70582.4 3140.24 3 0 -12 1 72922.4 4775 1 0 -12 -1 72531.6 4802.85 1 0 12 -2 144692 5157.65 3 0 -12 2 147043 7064.69 1 0 -12 3 35164.4 3805.29 1 0 -12 4 192101 9319.96 1 0 -12 5 9785.34 2278.96 1 0 -12 6 90982.8 7312.67 1 0 -12 7 7762.14 2400.65 1 0 -12 8 -487.3 1078.91 1 0 12 9 328.75 714.416 4 0 -12 9 -318.701 623.67 14 0 12 9 -162.795 795.865 13 0 12 10 7657.86 1471.16 4 0 -12 10 6309.21 1436.17 14 0 12 10 6681.03 1401.73 13 0 12 11 7624.08 1483.86 4 0 -12 11 6287.06 1415.61 14 0 12 11 6101.69 1232.67 13 0 12 12 4166.66 1123.57 4 0 12 12 4350.97 1094.51 13 0 12 13 21803.9 2049.42 4 0 12 13 23327.6 2009.01 13 0 12 14 29541.4 1994.64 4 0 12 14 26071.9 1877.42 14 0 12 15 9557.81 945.233 4 0 12 -15 10448.8 1058.87 17 0 -14 0 -427.187 961.453 1 0 -14 1 188280 8522.44 1 0 -14 -1 192024 8614.61 1 0 -14 2 26489.6 3409.67 1 0 -14 3 41104.9 4424.14 1 0 -14 4 256641 11532.2 1 0 -14 5 65607.8 6364.95 1 0 -14 6 625.624 1234.84 1 0 -14 7 7553.34 2458.8 1 0 -14 8 846.508 1200.02 1 0 14 8 3096.08 1150.41 4 0 14 8 2581.66 862.258 10 0 -14 9 16432.8 3120.5 1 0 -14 9 20855.7 4297.91 2 0 14 9 15699.8 2028.43 4 0 14 9 14601.8 1910.11 13 0 14 10 55623.9 3585.43 4 0 14 10 54504.7 3546.8 13 0 14 11 4933.7 1203.53 4 0 14 11 4838.37 1254.35 13 0 14 12 27869.9 2347.48 4 0 14 12 26511.2 2292.65 13 0 14 13 780.794 671.024 4 0 14 13 -79.0146 625.854 13 0 14 14 883.311 528.219 4 0 14 14 480.169 367.645 14 0 14 -14 921.022 529.861 17 0 14 15 59.0005 296.074 4 0 14 -15 629.68 345.319 17 0 -16 0 20986.7 3181.12 1 0 -16 -1 174035 8962.22 1 0 -16 1 161873 8738.16 1 0 -16 -2 60434.2 5510.68 1 0 -16 2 63240 5671.71 1 0 -16 3 40608.5 4792.59 1 0 -16 4 497.53 1181.32 1 0 -16 5 61150.1 6401.22 1 0 -16 6 12795.9 2818.4 1 0 -16 7 7155.36 2626.44 1 0 16 7 7452.21 1405.36 4 0 16 7 7236.92 1424.07 10 0 -16 8 33823.8 5484.98 1 0 -16 8 46941.4 6216.25 2 0 16 8 44909 3218.58 4 0 16 8 46696.7 3119.33 10 0 16 9 44007.3 3192.29 4 0 16 9 39731.6 3040.98 13 0 16 10 22416.3 2308.42 4 0 16 10 20523.6 2183.7 13 0 16 11 10146.5 1519.52 4 0 16 11 9013.72 1453.78 13 0 16 12 19245.4 1938.13 4 0 16 12 16971.7 1708.16 13 0 16 13 9183.83 1194.76 4 0 16 -13 8186.15 1240.61 17 0 16 -13 6789.09 876.412 10 0 16 14 13408.6 1185.05 4 0 16 14 9675.94 890.89 14 0 16 -14 11949.4 1103.7 17 0 -18 0 -58.4585 860.519 1 0 -18 -1 3310.62 1676.51 1 0 -18 1 4355.77 1753.53 1 0 -18 -2 63956.8 6113.36 1 0 -18 2 62418.6 6174.11 1 0 -18 -3 23679.4 3956.75 1 0 -18 3 25174.3 4216.91 1 0 -18 4 2479.86 1554.75 1 0 -18 5 16965.3 3663.7 1 0 -18 6 14072.2 3432.79 1 0 -18 6 17690.8 3426.85 2 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5148.1 924.06 6 6 6 11 5223.21 936.072 6 6 -6 12 4586.53 663.197 6 6 6 12 3470.94 559.445 6 -6 8 17 842.198 406.014 14 6 8 -17 694.388 434.111 17 6 -8 -17 0.82681 476.361 15 6 8 -16 1958.23 667.046 17 -6 8 16 2019.37 670.48 13 -6 8 15 19686.6 1869.18 13 6 8 -15 20764.8 2011.2 17 6 8 -14 18964.2 2097.05 17 6 8 -14 18506.9 1902.47 15 -6 8 14 16831.7 1885.69 13 6 8 -13 2741.85 1053.57 15 6 8 -13 2663.71 1040.46 17 -6 8 13 1592.38 837.552 13 6 8 -12 7926.4 1540.09 17 -6 8 12 7775.2 1484.66 13 -6 -8 11 72821.2 7577.51 1 6 8 -11 77012.3 4214.39 17 -6 -8 10 2015.28 1323.46 1 6 8 -10 2006.33 817.542 17 -6 -8 9 34386.6 4646.79 1 -6 -8 8 19196.5 3337.2 1 6 8 -8 20026.8 3571.98 3 6 8 -7 24679.9 3644.61 3 -6 -8 7 27679.3 3754.81 1 -6 -8 6 1247.67 1030.89 1 6 8 -6 1787.52 1238.55 3 6 8 -5 102494 6674.58 3 -6 -8 5 110785 6653.44 1 6 -8 -4 108107 5747.04 2 6 8 -4 115900 6851.67 3 -6 -8 4 112729 6218.86 1 -6 -8 3 4660.34 1424.96 1 6 -8 -3 4817.67 1367.33 2 6 8 -3 4973.5 1521.8 3 6 8 -2 44682.4 4138.45 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7 11 -17 35744.2 1828.21 17 7 -11 -17 31513.6 1636.79 15 -7 11 16 27635 1794.71 13 7 11 -16 28705 2010.23 17 7 -11 -16 28122 1959.52 15 7 11 -15 17828.2 1813.31 17 -7 11 15 15384.5 1553.29 13 7 11 -14 60609.2 3657.28 17 -7 11 14 65211.4 3472.52 13 7 11 -13 20454 2215.86 17 -7 11 13 19524.9 2101.01 13 7 11 -12 68265.5 4030.22 17 7 11 -11 23347.9 2405.86 17 -7 -11 10 530.777 1339.83 1 7 11 -10 3087.81 1504.58 3 -7 -11 9 31.774 1351.51 1 7 11 -9 962.973 1649.76 3 7 11 -9 128.368 618.501 17 7 11 -8 3855.4 1769.46 3 -7 -11 8 4606.77 1987.6 1 -7 -11 7 2123.78 1392.75 1 7 11 -7 5753.67 2093.5 3 7 11 -6 36085.3 4680.04 3 -7 -11 6 35212.3 4464.16 1 7 11 -5 35072.7 4417.66 3 -7 -11 5 33105.2 4165.77 1 7 -11 -4 31372.6 3518.52 2 7 11 -4 31193.7 4017.03 3 -7 -11 4 34585.5 4149.23 1 7 -11 -3 35139.6 3789.1 2 7 11 -3 33034.8 4133.85 3 -7 -11 3 34259.1 3951.96 1 7 -11 -2 8918.69 2074.57 2 7 11 -2 8575.94 2276.79 3 -7 -11 2 7816.38 2050.06 1 7 -11 -1 7837.39 2161.79 2 -7 -11 1 7704.5 1963.93 1 7 -11 0 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19 -12 18841.9 1494.32 16 9 19 -12 20906 1929.48 17 9 19 -11 4660.74 1109.13 17 9 19 -10 4243.44 1095.08 17 9 19 -9 382.531 607.424 17 -9 19 9 95.3704 522.237 4 9 -19 -8 5753.65 1165.53 7 -9 19 8 5811.69 1153.12 4 9 -19 -7 12820.4 1703.03 7 9 -19 -6 14201.3 1753.96 7 9 19 -6 13646.2 1820.32 16 9 -19 -5 26030.1 2338.68 7 9 19 -5 29008.7 2662.72 16 9 -19 -4 67090.6 3683.23 7 9 19 -4 66805.1 3966.4 16 9 -19 -3 22015.4 2198.76 7 9 19 -3 21434.6 2270.88 16 9 19 -3 19187.5 2006.55 9 9 19 -3 19211.6 1908.24 11 9 -19 -2 5392.59 1273.5 7 9 19 -2 4664.59 1268.81 16 9 19 -2 4467.91 1306.12 10 9 19 -2 3738.5 996.633 11 9 19 -2 3292.14 962.313 9 9 -19 -1 15422.7 1901.7 7 9 19 -1 16377.3 1932.28 16 9 19 -1 14177.1 1862.41 10 9 19 -1 15623.4 1790.62 11 9 -19 0 24585.2 2341.29 7 9 19 0 22383 2178.29 16 9 19 0 21323.2 2144.1 11 9 19 0 21667.5 2283.63 10 9 -19 1 31968.4 2574.89 7 9 19 1 31312.6 2368.36 16 9 19 1 33077.6 2577.85 11 9 -19 2 27825.5 2370.55 7 9 19 2 22253.9 1856.55 16 9 19 2 29047.8 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3163.03 631.984 5 15 11 -10 2187.32 676.234 9 15 -11 -9 1624.98 500.548 5 15 11 -9 2050.68 547.678 16 15 11 -9 2372.97 720.277 9 15 -11 -8 2617.34 596.125 5 15 11 -8 2589.6 658.933 16 15 11 -8 3254.88 862.603 9 15 11 -7 4862.99 874.501 16 15 11 -7 5885.26 1049.33 9 15 11 -6 -97.437 592.054 16 15 11 -6 359.511 485.845 9 15 11 -5 592.939 535.477 16 15 11 -5 2213.36 697.967 9 15 11 -4 550.845 530.151 16 15 11 -4 511.17 532.3 9 15 11 -3 1664.13 611.974 9 15 11 -2 2223.41 574.511 9 15 -13 -13 9163.32 714.368 5 15 -13 -12 8099.44 767.948 5 15 13 -12 7105.6 691.794 9 15 -13 -11 2899.52 537.836 5 15 13 -11 2706.4 567.44 9 15 -13 -10 380.668 313.658 5 15 13 -10 104.26 410.655 9 15 -13 -9 1731.7 433.06 5 15 13 -9 1773.23 642.23 9 15 13 -8 2506.13 625.146 16 15 13 -8 4156.51 871.498 9 15 13 -7 5042.49 817.407 16 15 13 -7 7739.95 1067.68 9 15 13 -6 -461.269 516.37 16 15 13 -6 -281.13 448.467 9 15 13 -5 3730.64 781.869 16 15 13 -5 4286.98 825.635 9 15 13 -4 3289.45 733.276 16 15 13 -4 3096.01 674.593 9 15 13 -3 476.338 425.445 9 15 -15 -11 1396.33 342.542 5 15 15 -11 1787.99 418.841 9 15 -15 -10 188.771 213.984 5 15 15 -10 -357.615 399.862 9 15 15 -9 3546.92 537.37 16 15 15 -9 4577.1 769.749 9 15 15 -8 4978.78 705.942 16 15 15 -8 7397.38 962.99 9 15 15 -7 5538.29 791.615 16 15 15 -7 6588.66 895.485 9 15 15 -6 872.535 479.713 16 15 15 -6 920.32 442.013 9 15 15 -5 6669.85 867.84 16 15 15 -5 6907.49 866.249 9 15 15 -4 4430.99 718.99 16 15 15 -4 4609.76 668.347 9 15 17 -10 3029.93 506.535 9 15 17 -9 5078.01 645.268 9 15 17 -8 6114.38 660.95 16 15 17 -8 6185.36 759.81 9 15 17 -7 5120.81 660.795 16 15 17 -7 6163.27 749.405 9 15 17 -6 3169.55 576.042 16 15 17 -6 3105.6 542.622 9 15 17 -5 3782.83 596.929 16 15 17 -4 4207.02 573.394 16 16 0 -14 8561.19 697.673 5 16 0 -13 -552.665 379.255 5 16 0 -12 1203.65 467.896 5 16 0 -11 -209.139 387.873 5 16 0 -10 29684.4 1886.65 5 16 0 -9 282.078 454.219 5 16 0 -9 1609.89 721.879 9 16 0 -8 23151.6 1672.57 5 16 0 -8 15092 1443.93 9 16 0 -7 42.5776 486.173 9 16 0 -6 2205.79 733.303 9 16 0 -5 -736.767 700.048 9 16 0 -4 47868.6 1505.61 8 16 0 -3 17519.4 938.98 8 16 0 -2 9902.09 670.166 8 16 0 -1 15722 725.242 8 16 -2 -14 5739.06 592.246 5 16 2 -13 3805.19 593.554 5 16 -2 -13 4374.38 633.102 5 16 2 -12 2621.47 584.124 5 16 -2 -12 3199.43 602.209 5 16 2 -11 864.791 457.705 5 16 -2 -11 872.285 466.239 5 16 2 -10 1613.61 600.943 5 16 -2 -10 1299.72 523.428 5 16 2 -10 715.67 442.675 9 16 2 -9 27120.4 1842.36 5 16 -2 -9 29520 1873.78 5 16 -2 -8 1180.48 547.017 5 16 -2 -8 -258.415 474.468 9 16 2 -8 1619.74 727.054 9 16 -2 -7 -76.7994 326.345 5 16 -2 -7 -745.165 595.67 9 16 2 -7 69.124 554.936 9 16 2 -6 2512.11 809.667 9 16 2 -5 495.802 522.907 9 16 2 -4 772.797 576.22 9 16 2 -4 31562.9 1191.58 8 16 -2 -3 47310.9 1462.69 8 16 2 -3 9523.04 700.884 8 16 2 -2 3945.33 467.486 8 16 -2 -2 37472.6 1244.3 8 16 -2 -1 51706.7 1244.23 8 16 2 -1 8571.3 564.126 8 16 -4 -14 15757.9 916.298 5 16 -4 -13 5469.13 675.64 5 16 -4 -12 391.217 376.158 5 16 4 -11 260.605 355.015 5 16 -4 -11 528.962 397.485 5 16 -4 -10 2002.01 565.221 5 16 4 -10 1382.77 521.775 9 16 -4 -9 -41.4515 382.031 5 16 4 -9 414.321 475.12 9 16 -4 -8 1239.6 487.275 5 16 4 -8 1545.06 627.474 9 16 -4 -7 1808.76 478.427 5 16 4 -7 1728.22 686.679 9 16 4 -6 11269.2 1337.27 9 16 4 -5 3576.09 854.816 9 16 4 -4 1840.33 662.317 9 16 4 -4 35200.3 1164.32 8 16 4 -3 -246.851 363.777 12 16 4 -3 8220.65 594.467 8 16 4 -2 4608.07 445.977 8 16 -6 -13 494.39 266.285 5 16 -6 -12 574.439 351.589 5 16 -6 -11 -54.4895 348.241 5 16 6 -11 -157.667 347.009 9 16 -6 -10 3408.77 661.42 5 16 6 -10 2674.91 594.593 9 16 -6 -9 4055.04 695.782 5 16 6 -9 3768.23 729.781 9 16 -6 -8 1915.21 506.102 5 16 6 -8 2077.52 676.077 9 16 -6 -7 4241.39 620.775 5 16 6 -7 4830.66 923.743 9 16 6 -6 -715.909 616.929 9 16 6 -5 576.129 381.397 12 16 6 -5 -31.0406 514.355 9 16 6 -4 471.88 440.336 9 16 6 -3 31326.8 952.881 8 16 6 -2 558.358 318.742 12 16 -8 -13 769.564 283.182 5 16 -8 -12 378.724 285.136 5 16 -8 -11 9585.49 899.049 5 16 8 -11 7466.61 747.126 9 16 -8 -10 6088.2 764.082 5 16 8 -10 4782.38 701.936 9 16 -8 -9 -223.582 279.29 5 16 8 -9 -128.735 433.988 9 16 -8 -8 2676 522.923 5 16 8 -8 3539.61 755.775 9 16 8 -7 2503.3 639.895 9 16 8 -6 -491.804 514.659 9 16 8 -5 -166.648 298.154 12 16 8 -5 897.151 504.513 9 16 8 -4 436.862 416.627 9 16 -10 -12 432.371 246.252 5 16 -10 -11 4095.45 556.739 5 16 10 -11 2535.03 454.62 9 16 -10 -10 4822.07 602.675 5 16 10 -10 2624.56 563.362 9 16 -10 -9 18457.2 1088.82 5 16 10 -9 17996.2 1346.25 9 16 10 -8 2713.77 706.601 9 16 10 -7 6002.19 886.177 9 16 10 -6 535.011 427.871 9 16 10 -5 1145.29 532.762 9 16 10 -4 -292.199 406.218 9 16 12 -10 11926.5 916.68 9 16 12 -9 143.961 324.968 9 16 12 -8 10563.3 1000.68 9 16 12 -7 6144.8 826.235 9 16 12 -6 1415.58 485.848 9 16 12 -5 5158.49 723.957 9 16 14 -9 503.079 282.251 9 16 14 -8 9151.94 814.186 9 16 14 -7 2917.04 524.418 9 17 -3 -11 993.051 309.878 5 17 3 -8 1287.61 437.177 9 17 5 -9 2983.63 536.062 9 17 5 -8 146.219 318.953 9 17 5 -7 697.58 361.435 9 17 7 -8 -270.668 387.855 9 17 7 -7 162.65 299.813 9 17 7 -6 131.006 344.952 9 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 O10D Zr1 O13D 123.2(4) . . y O4C Zr1 O13D 75.0(4) . . y O4C Zr1 O10D 71.1(4) . . y O1A Zr1 O13D 77.3(3) . . y O1A Zr1 O10D 134.7(4) . . y O1A Zr1 O4C 78.0(4) . . y O1B Zr1 O13D 80.4(4) . . y O1B Zr1 O10D 144.0(4) . . y O1B Zr1 O4C 144.9(3) . . y O1B Zr1 O1A 72.3(4) . . y Zr2 Zr1 O13D 161.6(3) . . y Zr2 Zr1 O10D 73.9(3) . . y Zr2 Zr1 O4C 120.4(3) . . y Zr2 Zr1 O1A 95.3(2) . . y Zr2 Zr1 O1B 81.3(2) . . y O4A Zr1 O13D 131.5(4) . . y O4A Zr1 O10D 76.3(3) . . y O4A Zr1 O4C 146.6(3) . . y O4A Zr1 O1A 122.7(3) . . y O4A Zr1 O1B 67.9(3) . . y O4A Zr1 Zr2 40.2(2) . . y Zr4 Zr1 O13D 74.6(2) . . y Zr4 Zr1 O10D 162.0(3) . . y Zr4 Zr1 O4C 115.2(3) . . y Zr4 Zr1 O1A 40.1(2) . . y Zr4 Zr1 O1B 32.3(3) . . y Zr4 Zr1 Zr2 88.85(3) . . y Zr4 Zr1 O4A 94.0(2) . . y Zr5 Zr1 O13D 104.3(3) . . y Zr5 Zr1 O10D 113.6(3) . . y Zr5 Zr1 O4C 174.0(3) . . y Zr5 Zr1 O1A 96.0(2) . . y Zr5 Zr1 O1B 30.5(2) . . y Zr5 Zr1 Zr2 59.23(3) . . y Zr5 Zr1 O4A 37.4(2) . . y Zr5 Zr1 Zr4 59.21(3) . . y Zr6 Zr1 O13D 115.7(3) . . y Zr6 Zr1 O10D 106.0(3) . . y Zr6 Zr1 O4C 86.1(3) . . y Zr6 Zr1 O1A 38.5(2) . . y Zr6 Zr1 O1B 82.4(3) . . y Zr6 Zr1 Zr2 59.62(3) . . y Zr6 Zr1 O4A 96.1(2) . . y Zr6 Zr1 Zr4 59.39(3) . . y Zr6 Zr1 Zr5 88.95(3) . . y O3C Zr1 O13D 70.7(4) . . y O3C Zr1 O10D 70.7(5) . . y O3C Zr1 O4C 98.1(4) . . y O3C Zr1 O1A 147.6(4) . . y O3C Zr1 O1B 97.0(5) . . y O3C Zr1 Zr2 113.6(3) . . y O3C Zr1 O4A 77.5(4) . . y O3C Zr1 Zr4 122.6(3) . . y O3C Zr1 Zr5 87.1(3) . . y O3C Zr1 Zr6 173.2(3) . . y O3B Zr1 O13D 146.8(4) . . y O3B Zr1 O10D 81.4(4) . . y O3B Zr1 O4C 95.9(4) . . y O3B Zr1 O1A 69.6(3) . . y O3B Zr1 O1B 91.1(4) . . y O3B Zr1 Zr2 31.8(2) . . y O3B Zr1 O4A 71.8(3) . . y O3B Zr1 Zr4 81.2(2) . . y O3B Zr1 Zr5 81.5(3) . . y O3B Zr1 Zr6 31.1(2) . . y O3B Zr1 O3C 142.4(4) . . y Zr4 O14D S4D 135.6(6) . . ? S4D O13D Zr1 138.5(6) . . ? S3D O10D Zr1 138.4(6) . . ? S3D O9D Zr2 132.1(6) . . ? Zr4 O8E C7E 134.1(9) . . ? Zr5 O7E C7E 138.3(10) . . ? C8E C7E O8E 119.8(14) . . ? O7E C7E O8E 118.4(13) . . ? O7E C7E C8E 121.1(16) . . ? Zr5 O6E C5E 131.9(9) . . ? S2D O6D Zr2 131.9(5) . . ? Zr2 O5E C5E 132.1(8) . . ? C6E C5E O6E 115.7(14) . . ? O5E C5E O6E 125.9(12) . . ? O5E C5E C6E 118.4(14) . . ? S2D O5D Zr3 137.5(6) . . ? C3E O4E Zr2 130.4(9) . . ? O15D S4D O16D 108.6(12) . . ? O14D S4D O16D 117.3(9) . . ? O14D S4D O15D 102.4(9) . . ? O13D S4D O16D 113.8(9) . . ? O13D S4D O15D 99.8(10) . . ? O13D S4D O14D 112.6(6) . . ? Zr4 O4B Zr3 116.3(4) . . ? Zr6 O4B Zr3 117.0(4) . . ? Zr6 O4B Zr4 116.4(4) . . ? Zr4 O1A Zr1 101.3(4) . . ? Zr6 O1A Zr1 103.5(3) . . ? Zr6 O1A Zr4 99.7(3) . . ? Zr3 O2A Zr2 101.4(3) . . ? Zr6 O2A Zr2 100.5(3) . . ? Zr6 O2A Zr3 104.5(3) . . ? Zr4 O1D S1D 129.1(5) . . ? O1D S1D O4D 109.1(6) . . ? O2D S1D O4D 108.1(6) . . ? O2D S1D O1D 107.3(5) . . ? O3D S1D O4D 111.2(6) . . ? O3D S1D O1D 111.0(6) . . ? O3D S1D O2D 110.0(6) . . ? Zr4 O1B Zr1 115.1(5) . . ? Zr5 O1B Zr1 118.2(4) . . ? Zr5 O1B Zr4 115.7(4) . . ? O9D Zr2 Zr1 76.3(3) . . y O6D Zr2 Zr1 168.4(2) . . y O6D Zr2 O9D 115.3(4) . . y O5E Zr2 Zr1 111.0(3) . . y O5E Zr2 O9D 72.8(4) . . y O5E Zr2 O6D 74.3(4) . . y O4E Zr2 Zr1 109.3(3) . . y O4E Zr2 O9D 75.6(4) . . y O4E Zr2 O6D 75.1(4) . . y O4E Zr2 O5E 119.9(4) . . y O2A Zr2 Zr1 95.9(2) . . y O2A Zr2 O9D 143.8(4) . . y O2A Zr2 O6D 74.7(3) . . y O2A Zr2 O5E 140.6(3) . . y O2A Zr2 O4E 73.8(3) . . y O4A Zr2 Zr1 38.8(2) . . y O4A Zr2 O9D 73.2(4) . . y O4A Zr2 O6D 141.9(3) . . y O4A Zr2 O5E 73.4(3) . . y O4A Zr2 O4E 139.9(3) . . y O4A Zr2 O2A 121.9(3) . . y Zr3 Zr2 Zr1 91.24(3) . . y Zr3 Zr2 O9D 167.4(3) . . y Zr3 Zr2 O6D 77.1(2) . . y Zr3 Zr2 O5E 110.7(2) . . y Zr3 Zr2 O4E 111.0(3) . . y Zr3 Zr2 O2A 38.1(2) . . y Zr3 Zr2 O4A 96.0(2) . . y Zr5 Zr2 Zr1 60.74(3) . . y Zr5 Zr2 O9D 110.5(3) . . y Zr5 Zr2 O6D 112.5(2) . . y Zr5 Zr2 O5E 75.2(3) . . y Zr5 Zr2 O4E 164.9(3) . . y Zr5 Zr2 O2A 95.2(2) . . y Zr5 Zr2 O4A 38.8(2) . . y Zr5 Zr2 Zr3 60.49(3) . . y Zr6 Zr2 Zr1 60.31(3) . . y Zr6 Zr2 O9D 113.6(3) . . y Zr6 Zr2 O6D 112.1(2) . . y Zr6 Zr2 O5E 165.4(3) . . y Zr6 Zr2 O4E 74.7(3) . . y Zr6 Zr2 O2A 38.9(2) . . y Zr6 Zr2 O4A 95.5(2) . . y Zr6 Zr2 Zr3 60.15(3) . . y Zr6 Zr2 Zr5 90.21(3) . . y O2B Zr2 Zr1 84.5(2) . . y O2B Zr2 O9D 141.5(4) . . y O2B Zr2 O6D 85.8(3) . . y O2B Zr2 O5E 83.7(3) . . y O2B Zr2 O4E 142.8(4) . . y O2B Zr2 O2A 70.4(3) . . y O2B Zr2 O4A 71.0(3) . . y O2B Zr2 Zr3 32.4(2) . . y O2B Zr2 Zr5 32.2(2) . . y O2B Zr2 Zr6 83.8(2) . . y O3B Zr2 Zr1 31.8(2) . . y O3B Zr2 O9D 87.3(4) . . y O3B Zr2 O6D 143.1(3) . . y O3B Zr2 O5E 142.4(4) . . y O3B Zr2 O4E 83.7(4) . . y O3B Zr2 O2A 70.6(3) . . y O3B Zr2 O4A 70.4(3) . . y O3B Zr2 Zr3 83.0(3) . . y O3B Zr2 Zr5 82.8(2) . . y O3B Zr2 Zr6 31.8(2) . . y O3B Zr2 O2B 93.8(3) . . y Zr2 O4A Zr1 101.0(3) . . ? Zr5 O4A Zr1 104.8(3) . . ? Zr5 O4A Zr2 100.5(3) . . ? Zr4 O3A Zr3 102.0(3) . . ? Zr5 O3A Zr3 104.3(3) . . ? Zr5 O3A Zr4 100.2(3) . . ? O7C Zr3 O8C 95.5(4) . . y O5D Zr3 O8C 72.2(4) . . y O5D Zr3 O7C 69.7(4) . . y O4B Zr3 O8C 142.3(3) . . y O4B Zr3 O7C 100.8(4) . . y O4B Zr3 O5D 145.5(4) . . y O2A Zr3 O8C 147.9(3) . . y O2A Zr3 O7C 79.5(4) . . y O2A Zr3 O5D 76.4(3) . . y O2A Zr3 O4B 69.2(3) . . y Zr2 Zr3 O8C 121.3(3) . . y Zr2 Zr3 O7C 115.2(3) . . y Zr2 Zr3 O5D 73.7(2) . . y Zr2 Zr3 O4B 81.7(2) . . y Zr2 Zr3 O2A 40.5(2) . . y O3A Zr3 O8C 76.8(4) . . y O3A Zr3 O7C 148.1(3) . . y O3A Zr3 O5D 133.4(3) . . y O3A Zr3 O4B 71.4(3) . . y O3A Zr3 O2A 122.9(3) . . y O3A Zr3 Zr2 94.7(2) . . y Zr4 Zr3 O8C 113.3(3) . . y Zr4 Zr3 O7C 125.3(3) . . y Zr4 Zr3 O5D 161.4(3) . . y Zr4 Zr3 O4B 31.7(3) . . y Zr4 Zr3 O2A 94.7(2) . . y Zr4 Zr3 Zr2 88.91(3) . . y Zr4 Zr3 O3A 39.8(2) . . y Zr5 Zr3 O8C 85.5(3) . . y Zr5 Zr3 O7C 173.9(2) . . y Zr5 Zr3 O5D 105.0(3) . . y Zr5 Zr3 O4B 81.9(2) . . y Zr5 Zr3 O2A 96.6(2) . . y Zr5 Zr3 Zr2 59.60(3) . . y Zr5 Zr3 O3A 37.95(19) . . y Zr5 Zr3 Zr4 59.29(3) . . y Zr6 Zr3 O8C 172.7(3) . . y Zr6 Zr3 O7C 90.0(3) . . y Zr6 Zr3 O5D 114.4(3) . . y Zr6 Zr3 O4B 31.1(2) . . y Zr6 Zr3 O2A 38.1(2) . . y Zr6 Zr3 Zr2 59.95(3) . . y Zr6 Zr3 O3A 96.0(2) . . y Zr6 Zr3 Zr4 59.43(3) . . y Zr6 Zr3 Zr5 89.59(3) . . y O2B Zr3 O8C 94.8(4) . . y O2B Zr3 O7C 142.7(3) . . y O2B Zr3 O5D 79.6(3) . . y O2B Zr3 O4B 92.6(3) . . y O2B Zr3 O2A 73.0(3) . . y O2B Zr3 Zr2 32.6(2) . . y O2B Zr3 O3A 69.3(3) . . y O2B Zr3 Zr4 82.3(2) . . y O2B Zr3 Zr5 31.3(2) . . y O2B Zr3 Zr6 83.7(2) . . y O2D Zr3 O8C 72.5(4) . . y O2D Zr3 O7C 72.1(4) . . y O2D Zr3 O5D 124.1(3) . . y O2D Zr3 O4B 80.4(3) . . y O2D Zr3 O2A 133.2(4) . . y O2D Zr3 Zr2 161.7(2) . . y O2D Zr3 O3A 76.0(3) . . y O2D Zr3 Zr4 73.8(2) . . y O2D Zr3 Zr5 113.8(3) . . y O2D Zr3 Zr6 104.8(3) . . y O2D Zr3 O2B 145.0(4) . . y O14D Zr4 Zr1 76.5(3) . . y O8E Zr4 Zr1 111.3(3) . . y O8E Zr4 O14D 74.1(4) . . y O4B Zr4 Zr1 83.2(2) . . y O4B Zr4 O14D 143.4(4) . . y O4B Zr4 O8E 142.3(3) . . y O1A Zr4 Zr1 38.6(2) . . y O1A Zr4 O14D 74.1(4) . . y O1A Zr4 O8E 141.0(4) . . y O1A Zr4 O4B 71.0(3) . . y O1D Zr4 Zr1 167.2(2) . . y O1D Zr4 O14D 116.2(4) . . y O1D Zr4 O8E 74.1(4) . . y O1D Zr4 O4B 85.9(3) . . y O1D Zr4 O1A 141.6(3) . . y O1B Zr4 Zr1 32.6(3) . . y O1B Zr4 O14D 85.9(3) . . y O1B Zr4 O8E 84.6(4) . . y O1B Zr4 O4B 93.2(4) . . y O1B Zr4 O1A 71.1(3) . . y O1B Zr4 O1D 142.5(3) . . y O3A Zr4 Zr1 96.44(19) . . y O3A Zr4 O14D 141.7(4) . . y O3A Zr4 O8E 73.8(3) . . y O3A Zr4 O4B 70.0(3) . . y O3A Zr4 O1A 122.8(3) . . y O3A Zr4 O1D 73.6(3) . . y O3A Zr4 O1B 70.9(3) . . y Zr3 Zr4 Zr1 90.99(3) . . y Zr3 Zr4 O14D 167.5(3) . . y Zr3 Zr4 O8E 110.9(3) . . y Zr3 Zr4 O4B 32.0(2) . . y Zr3 Zr4 O1A 96.4(2) . . y Zr3 Zr4 O1D 76.3(2) . . y Zr3 Zr4 O1B 83.3(2) . . y Zr3 Zr4 O3A 38.2(2) . . y Zr5 Zr4 Zr1 60.86(3) . . y Zr5 Zr4 O14D 111.8(3) . . y Zr5 Zr4 O8E 75.4(3) . . y Zr5 Zr4 O4B 83.0(2) . . y Zr5 Zr4 O1A 96.3(2) . . y Zr5 Zr4 O1D 111.3(2) . . y Zr5 Zr4 O1B 31.9(2) . . y Zr5 Zr4 O3A 39.12(19) . . y Zr5 Zr4 Zr3 60.31(3) . . y Zr6 Zr4 Zr1 60.54(3) . . y Zr6 Zr4 O14D 112.5(3) . . y Zr6 Zr4 O8E 165.9(3) . . y Zr6 Zr4 O4B 31.5(2) . . y Zr6 Zr4 O1A 39.6(2) . . y Zr6 Zr4 O1D 111.6(3) . . y Zr6 Zr4 O1B 83.6(3) . . y Zr6 Zr4 O3A 95.1(2) . . y Zr6 Zr4 Zr3 60.08(3) . . y Zr6 Zr4 Zr5 90.56(3) . . y O1E Zr4 Zr1 109.9(2) . . y O1E Zr4 O14D 74.2(4) . . y O1E Zr4 O8E 119.0(4) . . y O1E Zr4 O4B 84.9(3) . . y O1E Zr4 O1A 72.3(3) . . y O1E Zr4 O1D 75.5(4) . . y O1E Zr4 O1B 141.9(4) . . y O1E Zr4 O3A 141.1(3) . . y O1E Zr4 Zr3 111.2(2) . . y O1E Zr4 Zr5 165.6(2) . . y O1E Zr4 Zr6 75.0(2) . . y O7E Zr5 Zr1 106.3(3) . . y O6E Zr5 Zr1 111.9(3) . . y O6E Zr5 O7E 125.8(4) . . y O1C Zr5 Zr1 177.0(3) . . y O1C Zr5 O7E 72.8(4) . . y O1C Zr5 O6E 70.6(4) . . y O1B Zr5 Zr1 31.3(2) . . y O1B Zr5 O7E 80.5(4) . . y O1B Zr5 O6E 143.1(4) . . y O1B Zr5 O1C 146.3(4) . . y Zr2 Zr5 Zr1 60.04(3) . . y Zr2 Zr5 O7E 161.9(3) . . y Zr2 Zr5 O6E 72.2(3) . . y Zr2 Zr5 O1C 120.1(3) . . y Zr2 Zr5 O1B 82.6(3) . . y O4A Zr5 Zr1 37.8(2) . . y O4A Zr5 O7E 135.3(3) . . y O4A Zr5 O6E 74.2(4) . . y O4A Zr5 O1C 144.5(3) . . y O4A Zr5 O1B 69.1(3) . . y O4A Zr5 Zr2 40.7(2) . . y O3A Zr5 Zr1 97.0(2) . . y O3A Zr5 O7E 74.1(4) . . y O3A Zr5 O6E 134.4(4) . . y O3A Zr5 O1C 80.1(4) . . y O3A Zr5 O1B 73.0(3) . . y O3A Zr5 Zr2 94.9(2) . . y O3A Zr5 O4A 123.4(3) . . y Zr3 Zr5 Zr1 90.51(3) . . y Zr3 Zr5 O7E 111.6(3) . . y Zr3 Zr5 O6E 105.1(3) . . y Zr3 Zr5 O1C 87.2(3) . . y Zr3 Zr5 O1B 83.8(3) . . y Zr3 Zr5 Zr2 59.91(3) . . y Zr3 Zr5 O4A 97.1(2) . . y Zr3 Zr5 O3A 37.8(2) . . y Zr4 Zr5 Zr1 59.93(3) . . y Zr4 Zr5 O7E 72.5(3) . . y Zr4 Zr5 O6E 161.4(3) . . y Zr4 Zr5 O1C 117.2(3) . . y Zr4 Zr5 O1B 32.4(2) . . y Zr4 Zr5 Zr2 89.73(3) . . y Zr4 Zr5 O4A 95.0(2) . . y Zr4 Zr5 O3A 40.7(2) . . y Zr4 Zr5 Zr3 60.40(3) . . y O2C Zr5 Zr1 86.9(3) . . y O2C Zr5 O7E 71.5(4) . . y O2C Zr5 O6E 73.6(4) . . y O2C Zr5 O1C 95.4(4) . . y O2C Zr5 O1B 95.3(4) . . y O2C Zr5 Zr2 116.6(3) . . y O2C Zr5 O4A 79.3(4) . . y O2C Zr5 O3A 145.1(3) . . y O2C Zr5 Zr3 176.4(3) . . y O2C Zr5 Zr4 120.1(3) . . y O2B Zr5 Zr1 84.2(2) . . y O2B Zr5 O7E 143.0(3) . . y O2B Zr5 O6E 78.9(4) . . y O2B Zr5 O1C 94.8(4) . . y O2B Zr5 O1B 94.2(4) . . y O2B Zr5 Zr2 32.6(2) . . y O2B Zr5 O4A 73.3(3) . . y O2B Zr5 O3A 69.4(3) . . y O2B Zr5 Zr3 31.6(2) . . y O2B Zr5 Zr4 83.5(2) . . y O2B Zr5 O2C 145.4(3) . . y O6C Zr6 Zr1 176.9(3) . . y O5C Zr6 Zr1 88.7(3) . . y O5C Zr6 O6C 92.5(4) . . y O4B Zr6 Zr1 83.1(2) . . y O4B Zr6 O6C 97.4(4) . . y O4B Zr6 O5C 145.5(4) . . y O1A Zr6 Zr1 38.0(2) . . y O1A Zr6 O6C 145.0(3) . . y O1A Zr6 O5C 80.4(4) . . y O1A Zr6 O4B 72.6(3) . . y O2A Zr6 Zr1 97.3(2) . . y O2A Zr6 O6C 80.1(4) . . y O2A Zr6 O5C 145.2(4) . . y O2A Zr6 O4B 69.3(3) . . y O2A Zr6 O1A 123.9(3) . . y Zr2 Zr6 Zr1 60.07(3) . . y Zr2 Zr6 O6C 117.0(3) . . y Zr2 Zr6 O5C 122.0(3) . . y Zr2 Zr6 O4B 82.2(2) . . y Zr2 Zr6 O1A 95.3(2) . . y Zr2 Zr6 O2A 40.6(2) . . y Zr3 Zr6 Zr1 90.96(3) . . y Zr3 Zr6 O6C 88.0(3) . . y Zr3 Zr6 O5C 177.4(3) . . y Zr3 Zr6 O4B 31.9(2) . . y Zr3 Zr6 O1A 97.8(2) . . y Zr3 Zr6 O2A 37.4(2) . . y Zr3 Zr6 Zr2 59.90(3) . . y Zr4 Zr6 Zr1 60.07(3) . . y Zr4 Zr6 O6C 121.6(3) . . y Zr4 Zr6 O5C 117.2(3) . . y Zr4 Zr6 O4B 32.1(2) . . y Zr4 Zr6 O1A 40.6(2) . . y Zr4 Zr6 O2A 95.1(2) . . y Zr4 Zr6 Zr2 89.49(3) . . y Zr4 Zr6 Zr3 60.49(3) . . y O2E Zr6 Zr1 111.9(3) . . y O2E Zr6 O6C 71.1(4) . . y O2E Zr6 O5C 73.5(4) . . y O2E Zr6 O4B 78.7(4) . . y O2E Zr6 O1A 74.0(3) . . y O2E Zr6 O2A 133.3(4) . . y O2E Zr6 Zr2 160.2(3) . . y O2E Zr6 Zr3 104.3(3) . . y O2E Zr6 Zr4 71.5(2) . . y O3E Zr6 Zr1 103.3(3) . . y O3E Zr6 O6C 74.5(4) . . y O3E Zr6 O5C 69.6(4) . . y O3E Zr6 O4B 144.9(3) . . y O3E Zr6 O1A 132.1(4) . . y O3E Zr6 O2A 75.6(3) . . y O3E Zr6 Zr2 72.1(3) . . y O3E Zr6 Zr3 113.0(3) . . y O3E Zr6 Zr4 160.3(3) . . y O3E Zr6 O2E 127.5(4) . . y O3B Zr6 Zr1 31.4(2) . . y O3B Zr6 O6C 145.6(3) . . y O3B Zr6 O5C 98.1(4) . . y O3B Zr6 O4B 92.2(4) . . y O3B Zr6 O1A 69.4(3) . . y O3B Zr6 O2A 72.5(3) . . y O3B Zr6 Zr2 32.0(2) . . y O3B Zr6 Zr3 82.9(3) . . y O3B Zr6 Zr4 82.0(2) . . y O3B Zr6 O2E 143.3(4) . . y O3B Zr6 O3E 78.7(4) . . y C1E O1E Zr4 134.1(8) . . ? O2E C1E O1E 120.6(13) . . ? C2E C1E O1E 116.8(14) . . ? C2E C1E O2E 122.4(16) . . ? Zr3 O2B Zr2 115.0(4) . . ? Zr5 O2B Zr2 115.1(4) . . ? Zr5 O2B Zr3 117.1(4) . . ? Zr3 O2D S1D 135.6(6) . . ? O7D S2D O8D 110.7(6) . . ? O6D S2D O8D 108.9(6) . . ? O6D S2D O7D 110.6(6) . . ? O5D S2D O8D 108.3(6) . . ? O5D S2D O7D 110.3(7) . . ? O5D S2D O6D 108.0(5) . . ? C1E O2E Zr6 137.3(10) . . ? C3E O3E Zr6 134.1(10) . . ? C4E C3E O4E 116.5(13) . . ? O3E C3E O4E 127.6(14) . . ? O3E C3E C4E 115.7(14) . . ? O11D S3D O12D 108.6(8) . . ? O10D S3D O12D 111.6(7) . . ? O10D S3D O11D 106.0(8) . . ? O9D S3D O12D 114.0(7) . . ? O9D S3D O11D 105.9(8) . . ? O9D S3D O10D 110.1(6) . . ? Zr2 O3B Zr1 116.4(4) . . ? Zr6 O3B Zr1 117.5(4) . . ? Zr6 O3B Zr2 116.2(4) . . ? 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 O13D 2.220(9) . y Zr1 O10D 2.219(9) . y Zr1 O4C 2.228(9) . y Zr1 O1A 2.247(8) . y Zr1 O1B 2.099(9) . y Zr1 Zr2 3.5378(13) . y Zr1 O4A 2.257(8) . y Zr1 Zr4 3.5297(13) . y Zr1 Zr5 3.5625(14) . y Zr1 Zr6 3.5462(15) . y Zr1 O3C 2.223(10) . y Zr1 O3B 2.081(9) . y O16D S4D 1.372(13) . ? O15D S4D 1.56(2) . ? O14D S4D 1.457(10) . ? O14D Zr4 2.207(9) . y O13D S4D 1.475(9) . ? O12D S3D 1.404(12) . ? O11D S3D 1.509(16) . ? O10D S3D 1.465(10) . ? O9D Zr2 2.194(9) . y O9D S3D 1.490(10) . ? O8E C7E 1.353(18) . ? O8E Zr4 2.185(9) . y C8E C7E 1.37(2) . ? O8D S2D 1.433(10) . ? O8C Zr3 2.251(10) . y O7E C7E 1.311(16) . ? O7E Zr5 2.220(9) . y O7D S2D 1.476(10) . ? O7C Zr3 2.239(10) . y O6E C5E 1.27(2) . ? O6E Zr5 2.309(10) . y C6E C5E 1.502(16) . ? O6D Zr2 2.217(8) . y O6D S2D 1.471(9) . ? O6C Zr6 2.196(11) . y O5E C5E 1.25(2) . ? O5E Zr2 2.197(9) . y O5D Zr3 2.262(8) . y O5D S2D 1.500(9) . ? O5C Zr6 2.184(9) . y O4E Zr2 2.173(10) . y O4E C3E 1.282(19) . ? C4E C3E 1.53(2) . ? O4D S1D 1.431(10) . ? O4B Zr3 2.092(8) . y O4B Zr4 2.079(9) . y O4B Zr6 2.046(8) . y O1A Zr4 2.317(9) . y O1A Zr6 2.268(9) . y O2A Zr2 2.332(9) . y O2A Zr3 2.215(8) . y O2A Zr6 2.249(8) . y O1D S1D 1.509(10) . ? O1D Zr4 2.209(9) . y S1D O2D 1.478(9) . ? S1D O3D 1.474(10) . ? O1C Zr5 2.218(10) . y O1B Zr4 2.084(9) . y O1B Zr5 2.054(8) . y Zr2 O4A 2.325(9) . y Zr2 Zr3 3.5198(13) . y Zr2 Zr5 3.5087(15) . y Zr2 Zr6 3.5217(13) . y Zr2 O2B 2.090(8) . y Zr2 O3B 2.081(8) . y O4A Zr5 2.238(8) . y O3A Zr3 2.238(9) . y O3A Zr4 2.320(8) . y O3A Zr5 2.246(8) . y Zr3 Zr4 3.5434(13) . y Zr3 Zr5 3.5400(14) . y Zr3 Zr6 3.5289(14) . y Zr3 O2B 2.082(8) . y Zr3 O2D 2.247(9) . y Zr4 Zr5 3.5036(13) . y Zr4 Zr6 3.5055(15) . y Zr4 O1E 2.183(9) . y Zr5 O2C 2.223(9) . y Zr5 O2B 2.067(8) . y Zr6 O2E 2.263(9) . y Zr6 O3E 2.199(10) . y Zr6 O3B 2.068(9) . y O1E C1E 1.31(2) . ? C1E O2E 1.269(19) . ? C1E C2E 1.466(19) . ? O3E C3E 1.261(17) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8C H8Ca O1C 0.86(2) 2.48(6) 3.256(17) 150(10) . O7C H7Ca O6C 0.8554 2.71(6) 3.456(16) 146(9) . O7C H7Cb O8E 0.8550 2.53(5) 3.298(15) 150(9) 4_464 O7C H7Cb O1D 0.8550 2.54(11) 3.077(14) 122(10) 4_464 C6E H6Ec O7D 0.9600 2.611(18) 3.273(19) 126.4(4) . O4C H4Ca O5E 0.8503 2.37(7) 3.053(13) 137(9) 2_565 O4C H4Cb O12D 0.8502 2.81(11) 3.457(16) 134(12) 2_565 O4C H4Cb O5C 0.8502 2.55(3) 3.344(15) 156(5) . O1A H1A O12D 0.8200 2.200(17) 2.952(17) 152.5(4) 2_565 O2A H2A O4D 0.8200 1.985(13) 2.787(13) 165.7(4) 4_464 O4A H4A O16D 0.8200 2.22(2) 2.967(19) 151.1(5) 2_564 O3A H3A O8D 0.8200 1.981(13) 2.785(13) 166.9(4) 4_565 O1C H1Cb O8D 0.8500 2.72(14) 3.253(14) 122(13) 4_565 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 -0.034 0.010 0.409 1836 555 ' ' loop_ _restr_distance_atom_site_label_1 _restr_distance_atom_site_label_2 _restr_distance_site_symmetry_2 _restr_distance_target _restr_distance_target_weight_param _restr_distance_diff O8C H8Ca 1 0.8500 0.0200 -0.0055 O8C H8Cb 1 0.8500 0.0200 -0.0035 H8Ca H8Cb 1 1.3400 0.0400 0.0222 loop_ _restr_equal_distance_atom_site_label_1 _restr_equal_distance_atom_site_label_2 _restr_equal_distance_site_symmetry_2 _restr_equal_distance_class_id Zr3 H8Ca 1 1 Zr3 H8Cb 1 1 loop_ _restr_equal_distance_class_class_id _restr_equal_distance_class_target_weight_param _restr_equal_distance_class_average _restr_equal_distance_class_esd _restr_equal_distance_class_diff_max 1 0.0200 2.6930 0.0045 0.0045 loop_ _restr_U_iso_atom_site_label _restr_U_iso_weight_param O16D 0.0200 loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.79(3) 2 0.21(3) 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 -0.578 -0.582 -0.960 1917.0 534.2 '52 H2O' loop_ _platon_missing_refln_index_h _platon_missing_refln_index_k _platon_missing_refln_index_l _platon_missing_refln_theta 0 2 0 3.157 loop_ _restr_rigu_atom_site_label_1 _restr_rigu_atom_site_label_2 _restr_rigu_target_weight_param _restr_rigu_u13_diff _restr_rigu_u23_diff _restr_rigu_u33_diff O16D O15D 0.020000 0.059706 -0.041447 -0.019137 O16D O14D 0.020000 -0.020254 0.002117 0.018080 O16D O13D 0.020000 -0.005546 0.028431 0.015477 O16D S4D 0.010000 -0.009059 0.007734 -0.010443 O15D O14D 0.020000 -0.017024 0.013105 0.046969 O15D O13D 0.020000 0.023659 0.005396 0.054408 O15D S4D 0.010000 0.009263 0.004891 0.016965 O14D O13D 0.020000 -0.008277 -0.003745 0.007343 O14D S4D 0.010000 -0.001637 -0.001923 -0.004688 O13D S4D 0.010000 0.001516 -0.002087 -0.007565 O12D O11D 0.004000 0.013342 -0.025132 -0.004741 O12D O10D 0.004000 0.006051 -0.003296 0.015827 O12D O9D 0.004000 0.004896 0.001334 0.005134 O12D S3D 0.004000 -0.000362 0.000120 0.000187 O11D O10D 0.004000 -0.014423 -0.030659 -0.005130 O11D O9D 0.004000 -0.007335 0.011364 0.011687 O11D S3D 0.004000 0.006889 -0.002110 0.003055 O10D O9D 0.004000 -0.004715 0.006828 -0.006096 O10D S3D 0.004000 -0.014037 0.009647 -0.004833 O9D S3D 0.004000 0.002002 -0.002358 0.002392 O4D O1D 0.004000 -0.001418 0.002236 0.005368 O4D S1D 0.004000 0.002111 0.000472 0.002059 O4D O2D 0.004000 0.007944 -0.005553 0.008048 O4D O3D 0.004000 -0.000157 0.006284 -0.000769 O1D S1D 0.004000 -0.006114 0.005009 0.005132 O1D O2D 0.004000 0.002839 0.001498 -0.002498 O1D O3D 0.004000 -0.001295 0.006528 0.000778 S1D O2D 0.004000 -0.000917 0.002592 0.001718 S1D O3D 0.004000 0.000253 0.002859 -0.006708 O2D O3D 0.004000 -0.016213 -0.009177 0.002426