#------------------------------------------------------------------------------ #$Date: 2019-11-26 03:04:06 +0200 (Tue, 26 Nov 2019) $ #$Revision: 242463 $ #$URL: file:///home/coder/svn-repositories/cod/cif/4/13/24/4132490.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_4132490 loop_ _publ_author_name 'Zhang, Xin' 'Frey, Brandon L.' 'Chen, Yu-Sheng' 'Zhang, Jian' _publ_section_title ; Topology-Guided Stepwise Insertion of Three Secondary Linkers in Zirconium Metal-Organic Frameworks. ; _journal_issue 24 _journal_name_full 'Journal of the American Chemical Society' _journal_page_first 7710 _journal_page_last 7715 _journal_paper_doi 10.1021/jacs.8b04277 _journal_volume 140 _journal_year 2018 _chemical_formula_moiety 'C54 H26 O18 Zr3' _chemical_formula_sum 'C54 H26 O18 Zr3' _chemical_formula_weight 1236.41 _space_group_crystal_system orthorhombic _space_group_IT_number 65 _space_group_name_Hall '-C 2 2' _space_group_name_H-M_alt 'C m m m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _audit_creation_date 2016-03-18 _audit_creation_method ; Olex2 1.2 (compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 23.361(3) _cell_length_b 33.409(4) _cell_length_c 20.691(2) _cell_measurement_reflns_used 9987 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 14.91 _cell_measurement_theta_min 2.18 _cell_volume 16149(3) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.945 _diffrn_measured_fraction_theta_max 0.945 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_wavelength 0.41325 _diffrn_reflns_av_R_equivalents 0.1027 _diffrn_reflns_av_unetI/netI 0.0450 _diffrn_reflns_Laue_measured_fraction_full 0.945 _diffrn_reflns_Laue_measured_fraction_max 0.945 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 31483 _diffrn_reflns_point_group_measured_fraction_full 0.945 _diffrn_reflns_point_group_measured_fraction_max 0.945 _diffrn_reflns_theta_full 11.572 _diffrn_reflns_theta_max 11.572 _diffrn_reflns_theta_min 1.178 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.292 _exptl_absorpt_correction_type multi-scan _exptl_crystal_colour 'light yellow' _exptl_crystal_density_diffrn 0.509 _exptl_crystal_description block _exptl_crystal_F_000 13420 _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_diff_density_max 1.569 _refine_diff_density_min -0.811 _refine_diff_density_rms 0.115 _refine_ls_extinction_coef 0.031(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2014/7 (Sheldrick 2014' _refine_ls_goodness_of_fit_ref 1.109 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 201 _refine_ls_number_reflns 4011 _refine_ls_number_restraints 73 _refine_ls_restrained_S_all 1.117 _refine_ls_R_factor_all 0.1032 _refine_ls_R_factor_gt 0.0886 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1739P)^2^+109.5548P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2616 _refine_ls_wR_factor_ref 0.2858 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3408 _reflns_number_total 4011 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ja8b04277_si_010.cif _cod_data_source_block NPF-300-6 _cod_database_code 4132490 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups 2. Restrained distances C16-C15 = C16-C17 = C18-C17 = C19-C20 1.38 with sigma of 0.02 C14-C15 = C18-C19 1.46 with sigma of 0.02 O7-C20 1.35 with sigma of 0.02 C17-C15 = C16-C18 2.42 with sigma of 0.04 C18-C20 2.48 with sigma of 0.04 3. Rigid bond restraints O6, C14, C15, C16, C17, C18, C19, C20, O7 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints O6 \\sim C14 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19 \\sim C20 \\sim O7: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08 5. Others Fixed Sof: C20(0.5) O7(0.5) 6.a Aromatic/amide H refined with riding coordinates: C7(H7), C6(H6), C3(H3), C4(H4), C9(H9), C10(H10), C16(H16), C17(H17) ; _shelx_res_file ; z.res created by SHELXL-2014/7 TITL z in Cmmm #65 REM reset to Cmmm #65 CELL 0.41325 23.3613 33.409 20.6915 90 90 90 ZERR 244 0.0028 0.0035 0.0023 0 0 0 LATT 7 SYMM -X,-Y,+Z SYMM +X,-Y,-Z SYMM -X,+Y,-Z SFAC C H O Zr UNIT 244 244 244 244 DFIX 1.38 C16 C15 C16 C17 C18 C17 C19 C20 DFIX 1.46 C14 C15 C18 C19 DFIX 1.35 O7 C20 DANG 2.42 C17 C15 C16 C18 DANG 2.48 C18 C20 DELU O6 C14 C15 C16 C17 C18 C19 C20 O7 SIMU 0.04 0.08 1.7 O6 C14 C15 C16 C17 C18 C19 C20 O7 L.S. 10 PLAN 400 TEMP 23 BOND fmap 2 MORE -1 BOND $H CONF ACTA REM REM REM WGHT 0.173900 109.554802 EXTI 0.030580 FVAR 0.15115 ZR1 4 0.000000 0.073905 0.500000 10.25000 0.03784 0.02360 = 0.06065 0.00000 0.00000 0.00000 ZR2 4 0.075388 0.000000 0.414659 10.50000 0.04049 0.02963 = 0.06911 0.00000 0.00869 0.00000 O5 3 0.106333 0.060931 0.380721 11.00000 0.08266 0.04288 = 0.11059 -0.00766 0.03618 -0.01676 O1 3 0.000000 0.036161 0.415025 10.50000 0.04130 0.03642 = 0.15312 -0.03541 0.00000 0.00000 C2 1 0.128734 0.128220 0.360873 11.00000 0.07613 0.03934 = 0.08385 -0.00334 0.00725 -0.02071 O4 3 0.057793 0.108055 0.435873 11.00000 0.05594 0.03748 = 0.07725 -0.00201 0.01388 -0.00359 O2 3 0.074012 0.035975 0.500000 10.50000 0.12625 0.08541 = 0.06703 0.00000 0.00000 0.07943 C7 1 0.127740 0.167449 0.381459 11.00000 0.10870 0.06218 = 0.08398 -0.01478 0.03353 -0.04070 AFIX 43 H7 2 0.106823 0.173918 0.418247 11.00000 -1.20000 AFIX 0 C6 1 0.156617 0.197361 0.349468 11.00000 0.12284 0.05112 = 0.08342 -0.01255 0.03325 -0.03485 AFIX 43 H6 2 0.154562 0.223632 0.364147 11.00000 -1.20000 AFIX 0 C3 1 0.159943 0.119648 0.307603 11.00000 0.11396 0.04036 = 0.10458 -0.01911 0.03643 -0.03102 AFIX 43 H3 2 0.160279 0.093409 0.292599 11.00000 -1.20000 AFIX 0 C5 1 0.188555 0.188171 0.295628 11.00000 0.11460 0.06050 = 0.07236 -0.00410 0.00178 -0.05140 C1 1 0.094782 0.097239 0.396016 11.00000 0.07245 0.02891 = 0.08145 0.00051 0.00166 -0.01533 C4 1 0.191821 0.148442 0.273918 11.00000 0.13822 0.06752 = 0.09285 -0.02208 0.04770 -0.05560 AFIX 43 H4 2 0.214270 0.141480 0.238543 11.00000 -1.20000 AFIX 0 O3 3 0.068157 0.000000 0.310310 10.50000 0.13408 0.05078 = 0.07117 0.00000 0.01290 0.00000 O6 3 0.168120 0.000000 0.425933 10.50000 0.03989 0.08137 = 0.22782 0.00000 0.01904 0.00000 C9 1 0.250000 0.250000 0.291722 10.50000 0.10284 0.07319 = 0.06661 0.00000 0.00000 -0.04822 AFIX 43 H9 2 0.250002 0.249999 0.336668 10.50000 -1.20000 AFIX 0 C8 1 0.220713 0.219795 0.259016 11.00000 0.11773 0.06931 = 0.06592 -0.00098 0.00669 -0.05161 C10 1 0.220374 0.220315 0.192461 11.00000 0.15771 0.09184 = 0.06809 -0.00175 0.01089 -0.08244 AFIX 43 H10 2 0.200351 0.200831 0.169669 11.00000 -1.20000 AFIX 0 C11 1 0.250000 0.250000 0.159457 10.50000 0.17287 0.13099 = 0.04746 0.00000 0.00000 -0.06572 C12 1 0.250000 0.250000 0.087877 10.50000 0.22082 0.12341 = 0.10739 0.00000 0.00000 -0.11449 C13 1 0.250000 0.250000 0.032445 10.50000 0.24489 0.13781 = 0.05522 0.00000 0.00000 -0.09784 C15 1 0.254884 0.000000 0.500000 10.25000 0.08444 0.51406 = 0.28201 0.00000 0.00000 0.00000 C16 1 0.285585 0.000000 0.441828 10.50000 0.11585 0.65617 = 0.39013 0.00000 0.09585 0.00000 AFIX 43 H16 2 0.266342 0.000000 0.402482 10.50000 -1.20000 AFIX 0 C14 1 0.192015 0.000000 0.500000 10.25000 0.08037 0.34092 = 0.24351 0.00000 0.00000 0.00000 C17 1 0.344290 0.000000 0.443444 10.50000 0.12076 0.74351 = 0.47197 0.00000 0.07223 0.00000 AFIX 43 H17 2 0.363861 0.000000 0.404305 10.50000 -1.20000 AFIX 0 C20 1 0.469909 0.024301 0.458645 10.50000 0.18368 0.82619 = 0.61791 0.01883 0.03135 0.00979 C19 1 0.438826 0.000000 0.500000 10.25000 0.17211 0.80190 = 0.58350 0.00000 0.00000 0.00000 C18 1 0.376205 0.000000 0.500000 10.25000 0.17400 0.78233 = 0.54274 0.00000 0.00000 0.00000 O7 3 0.461341 0.026399 0.393808 10.50000 0.24586 0.83168 = 0.62522 0.05131 0.02099 0.01687 HKLF 4 REM z in Cmmm #65 REM R1 = 0.0886 for 3408 Fo > 4sig(Fo) and 0.1032 for all 4011 data REM 201 parameters refined using 73 restraints END WGHT 0.1738 109.5113 REM Highest difference peak 1.569, deepest hole -0.811, 1-sigma level 0.115 Q1 1 0.0000 0.2115 0.5000 10.25000 0.05 1.10 Q2 1 0.0000 0.0742 0.3302 10.50000 0.05 0.91 Q3 1 0.1492 0.0729 0.5000 10.50000 0.05 0.89 Q4 1 0.0000 0.0000 0.5000 10.12500 0.05 0.59 Q5 1 0.1609 0.0000 0.2379 10.50000 0.05 0.54 Q6 1 0.2633 0.1822 0.5000 10.50000 0.05 0.54 Q7 1 0.0000 0.0903 0.2821 10.50000 0.05 0.53 Q8 1 0.1305 0.0162 0.2178 11.00000 0.05 0.49 Q9 1 0.0414 0.0182 0.4723 11.00000 0.05 0.46 Q10 1 0.1890 0.0658 0.4568 11.00000 0.05 0.46 Q11 1 0.0000 0.0252 0.5000 10.25000 0.05 0.45 Q12 1 0.0445 0.0635 0.2781 11.00000 0.05 0.44 Q13 1 0.1019 0.1063 0.5000 10.50000 0.05 0.43 Q14 1 0.0742 0.1504 0.4184 11.00000 0.05 0.41 Q15 1 0.0934 0.0417 0.5000 10.50000 0.05 0.39 Q16 1 0.3114 0.0476 0.5000 10.50000 0.05 0.39 Q17 1 0.0380 0.1376 0.4698 11.00000 0.05 0.37 Q18 1 0.0000 0.1601 0.2694 10.50000 0.05 0.37 Q19 1 0.2231 0.0000 0.2458 10.50000 0.05 0.37 Q20 1 0.0770 0.0000 0.0000 10.25000 0.05 0.36 Q21 1 0.2640 0.0301 0.4117 11.00000 0.05 0.36 Q22 1 0.1165 0.1381 0.4739 11.00000 0.05 0.35 Q23 1 0.2641 0.0000 0.3822 10.50000 0.05 0.35 Q24 1 0.0137 0.0469 0.3968 11.00000 0.05 0.34 Q25 1 0.0505 0.1089 0.4213 11.00000 0.05 0.33 Q26 1 0.5000 0.1385 0.5000 10.25000 0.05 0.33 Q27 1 0.0247 0.0551 0.3930 11.00000 0.05 0.33 Q28 1 0.3020 0.0603 0.4584 11.00000 0.05 0.33 Q29 1 0.0295 0.0191 0.2632 11.00000 0.05 0.33 Q30 1 0.2269 0.1286 0.5000 10.50000 0.05 0.32 Q31 1 0.1641 0.1603 0.0000 10.50000 0.05 0.32 Q32 1 0.0000 0.0430 0.1575 10.50000 0.05 0.32 Q33 1 0.2060 0.0000 0.4123 10.50000 0.05 0.31 Q34 1 0.0000 0.1297 0.2471 10.50000 0.05 0.31 Q35 1 0.1502 0.0703 0.3299 11.00000 0.05 0.31 Q36 1 0.4122 0.0000 0.1806 10.50000 0.05 0.31 Q37 1 0.1186 0.3085 0.2564 11.00000 0.05 0.31 Q38 1 0.1635 0.0493 0.1696 11.00000 0.05 0.31 Q39 1 0.0678 0.0204 0.2669 11.00000 0.05 0.30 Q40 1 0.0000 0.0000 0.1314 10.25000 0.05 0.30 Q41 1 0.0819 0.1075 0.4387 11.00000 0.05 0.30 Q42 1 0.0937 0.0886 0.0000 10.50000 0.05 0.29 Q43 1 0.0000 0.2556 0.4112 10.50000 0.05 0.29 Q44 1 0.2069 0.0315 0.4333 11.00000 0.05 0.29 Q45 1 0.4328 0.1324 0.4687 11.00000 0.05 0.28 Q46 1 0.0366 0.0307 0.1576 11.00000 0.05 0.27 Q47 1 0.0517 0.0618 0.2389 11.00000 0.05 0.27 Q48 1 0.1141 0.2592 0.2107 11.00000 0.05 0.26 Q49 1 0.1818 0.0000 0.2972 10.50000 0.05 0.26 Q50 1 0.1076 0.2673 0.2196 11.00000 0.05 0.26 Q51 1 0.1867 0.0666 0.1519 11.00000 0.05 0.26 Q52 1 0.1686 0.3047 0.4126 11.00000 0.05 0.26 Q53 1 0.5000 0.0321 0.0000 10.25000 0.05 0.25 Q54 1 0.0526 0.1677 0.4824 11.00000 0.05 0.25 Q55 1 0.0932 0.0770 0.3815 11.00000 0.05 0.25 Q56 1 0.2134 0.0536 0.1657 11.00000 0.05 0.25 Q57 1 0.1728 0.1442 0.5000 10.50000 0.05 0.25 Q58 1 0.0807 0.2952 0.3209 11.00000 0.05 0.25 Q59 1 0.0134 0.0357 0.0000 10.50000 0.05 0.25 Q60 1 0.4276 0.0000 0.2948 10.50000 0.05 0.25 Q61 1 0.0874 0.1825 0.1522 11.00000 0.05 0.24 Q62 1 0.0601 0.1975 0.1985 11.00000 0.05 0.24 Q63 1 0.0390 0.0566 0.4400 11.00000 0.05 0.24 Q64 1 0.2192 0.1386 0.3744 11.00000 0.05 0.24 Q65 1 0.1569 0.1718 0.0597 11.00000 0.05 0.24 Q66 1 0.1080 0.2309 0.2409 11.00000 0.05 0.23 Q67 1 0.3062 0.1320 0.3968 11.00000 0.05 0.23 Q68 1 0.0504 0.0887 0.3009 11.00000 0.05 0.23 Q69 1 0.0967 0.0000 0.4778 10.50000 0.05 0.23 Q70 1 0.4104 0.0000 0.3230 10.50000 0.05 0.23 Q71 1 0.1215 0.0107 0.2695 11.00000 0.05 0.23 Q72 1 0.1226 0.0605 0.4253 11.00000 0.05 0.23 Q73 1 0.4769 0.1235 0.4420 11.00000 0.05 0.22 Q74 1 0.0628 0.1722 0.1998 11.00000 0.05 0.22 Q75 1 0.1519 0.1466 0.0969 11.00000 0.05 0.22 Q76 1 0.0916 0.2735 0.2469 11.00000 0.05 0.22 Q77 1 0.2409 0.1187 0.3343 11.00000 0.05 0.22 Q78 1 0.1052 0.2965 0.1954 11.00000 0.05 0.21 Q79 1 0.2760 0.0980 0.5000 10.50000 0.05 0.21 Q80 1 0.1689 0.2579 0.1950 11.00000 0.05 0.21 Q81 1 0.2615 0.1111 0.3644 11.00000 0.05 0.21 Q82 1 0.0287 0.1490 0.3683 11.00000 0.05 0.21 Q83 1 0.1079 0.2175 0.2990 11.00000 0.05 0.20 Q84 1 0.0682 0.2518 0.2304 11.00000 0.05 0.20 Q85 1 0.3533 0.1718 0.1841 11.00000 0.05 0.20 Q86 1 0.2530 0.2029 0.3505 11.00000 0.05 0.20 Q87 1 0.1187 0.1707 0.1025 11.00000 0.05 0.20 Q88 1 0.0722 0.2571 0.5000 10.50000 0.05 0.20 Q89 1 0.3442 0.1511 0.1980 11.00000 0.05 0.20 Q90 1 0.2523 0.0997 0.3094 11.00000 0.05 0.20 Q91 1 0.1784 0.2714 0.2135 11.00000 0.05 0.20 Q92 1 0.3530 0.0565 0.0000 10.50000 0.05 0.20 Q93 1 0.1603 0.1015 0.1054 11.00000 0.05 0.20 Q94 1 0.1223 0.1010 0.4579 11.00000 0.05 0.19 Q95 1 0.5000 0.0000 0.0992 10.25000 0.05 0.19 Q96 1 0.0000 0.1511 0.5000 10.25000 0.05 0.19 Q97 1 0.2711 0.0000 0.0000 10.25000 0.05 0.19 Q98 1 0.1357 0.1371 0.0000 10.50000 0.05 0.19 Q99 1 0.1320 0.2603 0.1612 11.00000 0.05 0.19 Q100 1 0.2876 0.0000 0.0766 10.50000 0.05 0.19 Q101 1 0.1276 0.2401 0.2706 11.00000 0.05 0.18 Q102 1 0.1063 0.2862 0.1530 11.00000 0.05 0.18 Q103 1 0.1941 0.1489 0.4304 11.00000 0.05 0.18 Q104 1 0.1472 0.0000 0.0973 10.50000 0.05 0.18 Q105 1 0.5000 0.0861 0.2852 10.50000 0.05 0.18 Q106 1 0.1859 0.2294 0.0510 11.00000 0.05 0.18 Q107 1 0.3554 0.0355 0.1497 11.00000 0.05 0.18 Q108 1 0.1594 0.2219 0.1720 11.00000 0.05 0.18 Q109 1 0.0220 0.1418 0.3225 11.00000 0.05 0.17 Q110 1 0.5000 0.0907 0.4343 10.50000 0.05 0.17 Q111 1 0.0928 0.2485 0.0773 11.00000 0.05 0.17 Q112 1 0.1851 0.2376 0.0000 10.50000 0.05 0.17 Q113 1 0.1430 0.1599 0.4394 11.00000 0.05 0.17 Q114 1 0.4045 0.1024 0.5000 10.50000 0.05 0.17 Q115 1 0.0888 0.0471 0.0831 11.00000 0.05 0.17 Q116 1 0.1211 0.3073 0.3468 11.00000 0.05 0.17 Q117 1 0.1449 0.0321 0.3379 11.00000 0.05 0.17 Q118 1 0.1411 0.0990 0.2818 11.00000 0.05 0.17 Q119 1 0.1877 0.0997 0.2330 11.00000 0.05 0.17 Q120 1 0.3695 0.0489 0.4236 11.00000 0.05 0.17 Q121 1 0.5000 0.0819 0.3728 10.50000 0.05 0.17 Q122 1 0.1030 0.1034 0.3447 11.00000 0.05 0.16 Q123 1 0.2091 0.1277 0.1079 11.00000 0.05 0.16 Q124 1 0.4649 0.0324 0.3407 11.00000 0.05 0.16 Q125 1 0.3814 0.0000 0.4034 10.50000 0.05 0.16 Q126 1 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29.66 5.45 10 12 12 17.64 4.54 -10 -12 -13 46.66 5.85 -10 -12 -13 45.15 5.14 -10 -12 13 44.62 5.34 -10 -12 13 44.55 4.90 -10 12 -13 40.97 5.16 -10 12 -13 62.33 7.43 10 -12 -13 68.77 6.84 10 -12 -13 58.44 5.28 10 -12 13 43.31 5.09 10 -12 13 79.77 6.68 10 12 -13 57.39 6.14 10 12 -13 34.88 4.93 10 12 13 57.52 6.03 -10 -12 -14 42.55 5.83 -10 -12 -14 30.52 4.86 -10 -12 14 44.87 5.41 -10 -12 14 37.54 4.73 -10 12 -14 37.16 6.30 -10 12 -14 47.21 5.08 10 -12 -14 40.96 4.74 10 -12 -14 53.26 5.51 10 -12 14 70.56 8.36 10 12 -14 42.99 5.97 10 12 -14 33.33 4.77 -10 -12 -15 17.20 5.58 -10 -12 -15 0.68 4.38 -10 -12 15 19.48 5.12 -10 -12 15 12.75 4.36 10 -12 -15 17.26 4.43 10 -12 -15 14.84 3.50 10 12 -15 17.62 5.61 10 12 -15 9.78 4.70 -10 -12 -16 28.35 5.47 -10 -12 -16 30.80 5.11 -10 -12 16 27.53 5.45 -10 -12 16 35.15 4.86 10 -12 -16 23.95 4.95 10 -12 -16 23.66 3.92 10 12 -16 36.31 6.30 10 12 -16 31.24 5.03 -10 -14 0 571.50 8.30 -10 -14 0 415.72 7.62 10 14 0 525.84 8.41 -10 -14 -1 184.97 6.54 -10 -14 -1 147.61 6.48 -10 -14 1 184.44 6.27 -10 -14 1 139.36 6.33 10 14 -1 138.75 6.35 10 14 1 168.62 6.46 -10 -14 -2 207.02 6.85 -10 -14 -2 163.70 6.46 -10 -14 2 193.37 6.49 -10 -14 2 163.95 6.46 -10 14 -2 159.76 3.83 10 14 -2 160.46 6.70 10 14 2 180.71 6.64 -10 -14 -3 247.52 7.16 -10 -14 -3 194.50 6.69 -10 -14 3 233.11 6.73 -10 -14 3 177.82 6.57 -10 14 -3 170.14 4.20 -10 14 3 179.33 3.89 10 14 -3 186.28 7.27 10 14 3 233.21 7.01 -10 -14 -4 248.84 7.81 -10 -14 -4 264.71 7.25 -10 -14 4 172.91 6.53 -10 14 -4 189.01 4.59 -10 14 4 203.55 5.17 10 -14 4 242.99 5.00 10 14 -4 207.42 7.17 10 14 4 270.56 7.28 -10 -14 -5 212.06 7.74 -10 -14 -5 228.78 7.46 -10 -14 5 165.12 6.64 -10 14 -5 165.07 4.90 10 -14 5 212.73 5.34 10 14 -5 177.19 7.48 10 14 5 246.96 7.36 -10 -14 -6 120.97 7.48 -10 -14 -6 114.19 7.01 -10 -14 6 75.46 6.41 -10 14 -6 84.81 4.99 -10 14 -6 121.50 4.13 10 -14 -6 84.96 4.82 10 -14 6 98.71 5.21 10 14 -6 89.40 6.80 10 14 6 108.40 6.98 -10 -14 -7 59.58 7.15 -10 -14 -7 56.15 6.68 -10 -14 7 56.58 6.79 -10 -14 7 32.25 3.97 -10 14 -7 36.65 3.48 -10 14 -7 64.33 4.66 10 -14 -7 39.35 4.89 10 -14 7 48.15 5.14 10 14 -7 38.12 4.25 10 14 7 63.28 6.91 -10 -14 -8 64.44 7.32 -10 -14 -8 70.97 6.98 -10 -14 8 61.85 6.92 -10 -14 8 45.69 4.26 -10 14 -8 54.59 5.64 -10 14 -8 66.24 5.25 10 -14 -8 58.69 5.27 10 -14 8 61.22 5.78 10 14 -8 43.66 4.36 10 14 8 78.14 7.16 -10 -14 -9 65.41 7.52 -10 -14 -9 73.62 7.10 -10 -14 9 60.31 7.16 -10 -14 9 45.32 4.33 -10 14 -9 48.02 4.18 -10 14 -9 74.91 5.76 10 -14 -9 55.19 5.43 10 -14 9 52.14 6.07 10 14 -9 59.09 7.00 10 14 9 65.25 7.58 10 14 9 86.32 7.54 -10 -14 -10 11.80 4.60 -10 -14 -10 10.49 4.12 -10 -14 10 18.30 4.49 -10 -14 10 6.69 3.81 -10 14 -10 10.00 3.87 -10 14 -10 13.95 3.67 10 -14 -10 7.68 3.50 10 -14 10 5.62 3.72 10 14 -10 4.27 4.05 10 14 10 7.95 4.52 10 14 10 15.42 4.97 -10 -14 -11 4.64 4.61 -10 -14 -11 9.17 4.25 -10 -14 11 6.53 4.48 -10 -14 11 6.50 4.01 -10 14 -11 1.87 4.08 -10 14 -11 5.06 3.81 10 -14 -11 4.55 3.67 10 -14 11 1.15 3.99 10 -14 11 5.39 2.68 10 14 -11 6.49 4.21 10 14 11 5.68 4.61 -10 -14 -12 34.04 5.35 -10 -14 -12 36.97 4.74 -10 -14 12 33.51 5.20 -10 -14 12 31.70 4.53 -10 14 -12 28.19 4.86 -10 14 -12 35.48 4.53 10 -14 -12 37.05 4.27 10 -14 12 31.74 4.75 10 -14 12 44.65 3.55 10 14 -12 38.24 4.83 -10 -14 -13 64.63 6.11 -10 -14 -13 78.43 8.48 -10 -14 13 73.39 8.41 -10 -14 13 66.80 7.44 -10 14 -13 50.24 5.41 -10 14 -13 59.51 7.42 10 -14 -13 73.46 6.92 10 -14 -13 89.48 4.86 10 -14 13 77.53 6.18 10 14 -13 54.04 5.29 -10 -14 -14 87.46 9.06 -10 -14 -14 86.52 8.08 -10 -14 14 62.75 6.00 -10 -14 14 85.36 7.94 10 -14 -14 92.51 7.27 10 -14 -14 105.28 5.35 10 14 -14 108.70 9.80 10 14 -14 77.39 8.33 -10 -14 -15 91.07 9.09 -10 -14 -15 88.23 8.36 -10 -14 15 79.50 10.74 10 -14 -15 100.56 7.53 10 -14 -15 87.89 5.53 10 14 -15 77.71 7.13 10 14 -15 58.84 5.75 -10 -16 0 22.32 3.71 -10 -16 0 17.99 3.57 10 16 0 20.38 3.71 -10 -16 -1 27.08 3.70 -10 -16 -1 20.25 3.72 -10 -16 1 28.58 3.71 -10 -16 1 18.88 3.63 10 16 -1 19.41 3.70 10 16 1 30.30 3.88 -10 -16 -2 71.08 6.45 -10 -16 -2 55.49 6.25 -10 -16 2 73.81 5.89 -10 -16 2 44.16 3.97 10 16 -2 47.81 4.29 10 16 2 73.93 6.30 -10 -16 -3 56.40 6.47 -10 -16 -3 45.41 4.04 -10 -16 3 61.91 5.93 -10 -16 3 38.45 3.89 10 16 -3 36.33 4.08 10 16 3 64.33 6.27 -10 -16 -4 25.64 4.35 -10 -16 -4 26.94 3.92 -10 -16 -4 22.51 3.78 -10 -16 4 27.72 3.70 -10 -16 4 14.93 3.61 -10 16 -4 12.97 2.47 10 -16 4 20.32 2.63 10 16 -4 13.33 3.79 10 16 4 30.07 3.95 -10 -16 -5 16.88 4.34 -10 -16 -5 16.49 3.88 -10 -16 5 8.61 3.53 -10 16 -5 14.81 2.73 10 -16 5 16.92 2.86 10 16 -5 6.43 3.77 10 16 5 21.31 4.00 -10 -16 -6 46.21 4.87 -10 -16 -6 49.95 4.44 -10 -16 6 27.73 3.85 -10 16 -6 41.50 4.76 10 -16 -6 34.13 3.04 10 -16 6 42.40 4.85 10 16 -6 39.06 4.53 10 16 6 50.07 4.50 -10 -16 -7 76.68 7.55 -10 -16 -7 78.51 6.86 -10 -16 7 63.58 7.10 -10 -16 7 64.35 6.38 -10 16 -7 58.15 5.29 -10 16 -7 88.20 4.54 10 -16 -7 54.58 4.88 10 -16 7 65.73 5.39 10 16 -7 67.07 6.98 -10 -16 -8 47.45 5.03 -10 -16 -8 45.57 4.50 -10 -16 8 51.35 5.21 -10 -16 8 39.94 4.41 -10 16 -8 48.03 5.50 -10 16 -8 61.33 5.09 10 -16 -8 36.56 3.43 10 -16 8 48.24 5.65 10 16 -8 38.73 4.64 -10 -16 -9 4.04 4.42 -10 -16 -9 6.91 4.05 -10 -16 9 7.83 4.31 -10 -16 9 9.98 4.10 -10 16 -9 9.09 3.61 -10 16 -9 9.79 3.23 10 -16 -9 7.61 3.25 10 -16 9 10.58 3.57 10 16 -9 0.07 3.89 -10 -16 -10 -2.76 4.53 -10 -16 -10 -2.10 4.12 -10 -16 10 3.99 4.58 -10 -16 10 -0.02 3.85 -10 16 -10 3.99 3.73 -10 16 -10 2.36 3.56 10 -16 -10 -4.79 3.34 10 -16 10 0.83 3.69 10 16 -10 3.33 4.46 -10 -16 -11 -6.93 4.47 -10 -16 -11 -3.62 4.04 -10 -16 11 4.08 4.65 -10 -16 11 3.86 3.98 -10 16 -11 -4.39 3.99 -10 16 -11 -5.52 3.66 10 -16 -11 -6.89 3.55 10 -16 11 0.26 4.02 10 16 -11 4.38 4.40 -10 -16 -12 -7.00 4.72 -10 -16 -12 -4.41 4.21 -10 -16 12 0.62 4.73 -10 -16 12 -2.74 3.82 -10 16 -12 -7.08 4.22 -10 16 -12 -10.12 3.88 10 -16 -12 -9.82 3.66 10 -16 12 -6.40 4.21 10 16 -12 3.28 4.47 -10 -16 -13 6.69 5.05 -10 -16 -13 2.06 4.17 -10 -16 13 2.40 4.89 -10 -16 13 3.86 4.28 10 -16 -13 2.07 3.84 10 -16 13 -7.23 2.98 10 16 -13 0.50 4.55 -10 -16 -14 10.70 5.31 -10 -16 -14 11.27 4.42 10 -16 -14 9.65 3.99 10 -16 14 5.52 5.81 10 16 -14 -7.21 4.64 -10 -16 -15 10.28 5.18 -10 -16 -15 14.36 4.46 10 -16 -15 6.52 4.13 10 -16 -15 9.99 3.01 10 16 -15 -7.09 4.86 -10 -18 0 29.14 4.01 -10 -18 0 25.61 3.83 10 18 0 28.49 4.04 -10 -18 -1 118.83 6.86 -10 -18 -1 83.11 6.40 -10 -18 1 116.38 6.72 -10 -18 1 83.53 6.13 10 18 -1 86.68 6.47 -10 -18 -2 54.92 6.49 -10 -18 -2 43.53 4.29 -10 -18 2 61.92 6.47 -10 -18 2 41.10 3.97 10 18 -2 41.13 4.42 -10 -18 -3 45.49 4.34 -10 -18 -3 31.66 4.05 -10 -18 3 51.26 6.00 -10 -18 3 34.85 3.97 10 18 -3 31.59 4.24 -10 -18 -4 53.00 4.92 -10 -18 -4 69.30 6.76 -10 -18 -4 56.10 6.41 -10 -18 4 66.68 6.44 -10 -18 4 42.21 4.15 10 18 -4 49.92 4.61 -10 -18 -5 24.82 4.51 -10 -18 -5 27.95 4.05 -10 -18 -5 17.64 3.94 -10 -18 5 32.33 3.95 -10 -18 5 16.07 3.79 -10 18 -5 16.00 2.69 10 -18 5 20.75 2.86 10 18 -5 22.70 4.25 -10 -18 -6 -1.98 4.24 -10 -18 -6 -1.87 3.74 -10 -18 6 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5.13 -19 -15 1 28.47 5.43 -19 -15 1 20.12 5.24 -19 15 -1 27.95 4.10 -19 -15 -2 -6.28 4.74 -19 -15 -2 -12.83 4.71 -19 -15 2 -4.51 4.78 -19 -15 2 -11.94 4.89 -19 15 -2 1.28 3.91 -19 -15 -3 9.56 5.04 -19 -15 3 6.58 4.84 -19 -15 3 1.71 4.95 -19 15 -3 12.03 6.62 -19 -15 -4 128.96 10.26 -19 -15 4 115.53 8.97 -19 -15 4 89.35 8.94 -19 -15 -5 244.18 11.46 -19 -15 -5 316.17 11.13 -19 -15 5 224.54 10.64 19 15 5 256.28 10.70 -19 -17 0 108.79 9.11 -19 -17 0 73.13 8.84 -19 17 0 70.24 6.46 -19 -17 -1 140.51 9.55 -19 -17 -1 118.33 9.45 -19 -17 1 139.30 9.12 -19 -17 1 121.77 9.62 -19 17 -1 108.60 6.59 -19 -17 -2 84.98 9.78 -19 -17 -2 36.36 5.52 -19 -17 2 75.55 8.66 -19 -17 2 43.91 5.61 -19 17 -2 65.94 7.55 -19 -17 -3 -4.54 5.12 -19 -17 -3 -3.65 5.08 -19 -17 3 -8.73 4.72 -19 -17 3 -2.55 5.03 -20 0 -2 -4.48 4.90 -20 0 -3 29.31 5.28 -20 0 -4 128.01 9.68 -20 0 -4 190.18 8.95 -20 0 -5 352.93 14.34 -20 0 -5 367.57 10.35 -20 0 -6 376.59 10.79 -20 0 -7 237.18 9.74 -20 -2 -1 36.52 5.35 -20 -2 -2 -5.56 4.78 -20 2 -2 3.56 4.28 -20 -2 -3 14.96 4.92 -20 2 -3 12.88 4.76 -20 -2 -4 88.96 9.50 -20 -2 -4 108.74 8.66 -20 2 -4 101.49 9.70 -20 2 -4 100.74 8.26 -20 -2 -5 159.00 9.91 -20 -2 -5 195.81 9.42 -20 2 -5 192.71 8.98 -20 -2 -6 282.27 10.30 -20 2 -6 295.52 12.36 -20 -2 -7 274.48 10.36 -20 -2 -8 144.39 9.76 -20 -2 -9 12.34 6.72 -20 -4 0 367.36 10.01 -20 -4 -1 283.84 9.91 -20 -4 -2 77.41 8.88 -20 -4 -3 -12.67 4.80 -20 4 -3 7.02 5.10 -20 4 -3 9.60 4.63 -20 -4 -4 5.26 5.57 -20 -4 -4 0.71 5.03 -20 4 -4 6.04 5.43 -20 -4 -5 93.96 9.56 -20 -4 -5 105.10 9.27 -20 -4 -6 213.99 11.25 -20 -4 -6 204.61 10.00 -20 -4 -7 170.90 10.20 -20 -4 -8 30.56 5.84 -20 -4 -9 9.13 5.40 -20 -6 0 733.55 12.89 -20 -6 -1 510.44 12.16 -20 -6 -2 156.42 10.02 -20 -6 -3 -12.52 5.15 -20 -6 -4 -8.35 5.12 -20 -6 -5 55.52 6.36 -20 -6 -5 58.05 6.04 -20 -6 -6 92.88 9.72 -20 -6 -6 49.00 6.33 -20 -6 -7 14.07 5.51 -20 -6 -8 -1.91 5.22 -20 -8 0 488.99 11.87 -20 -8 -1 410.85 11.47 -20 -8 1 399.51 11.48 -20 -8 -2 129.35 9.87 -20 -8 -3 -13.19 5.19 -20 -8 -4 -9.10 5.40 -20 -8 -5 39.00 6.21 -20 -8 -5 44.05 5.81 -20 -8 -6 24.81 5.93 -20 -8 -6 19.48 5.73 -20 -8 -7 11.90 6.10 -20 -8 -7 -3.48 5.23 -20 -8 -8 2.90 5.41 -20 -10 0 287.26 10.42 -20 -10 -1 144.74 9.57 -20 -10 1 146.89 9.50 -20 -10 -2 17.03 5.32 -20 -10 2 16.58 5.31 -20 -10 -3 -5.74 5.12 -20 -10 -4 31.82 5.63 -20 -10 -5 113.99 10.46 -20 -10 -5 118.19 9.80 -20 -10 -6 161.96 10.78 -20 -10 -6 198.46 11.02 -20 -10 -7 124.18 10.76 -20 -10 -7 148.00 10.36 -20 -12 0 71.52 8.68 -20 -12 -1 74.50 8.74 -20 -12 1 57.20 5.79 -20 -12 -2 3.61 5.19 -20 -12 2 -2.01 4.85 -20 -12 -3 23.91 5.48 -20 -12 3 19.26 5.35 -20 -12 -4 216.57 10.57 -20 -12 -5 314.22 12.19 -20 -12 -5 414.96 11.89 -20 -14 0 95.49 9.14 -20 -14 -1 21.36 5.40 -20 -14 1 22.03 5.48 -20 -14 -2 -13.43 5.07 -20 -14 2 -10.93 4.79 -20 -14 -3 29.77 5.78 -20 -14 3 25.13 5.52 -21 -1 -1 -2.86 4.80 -21 -1 -2 -7.24 4.75 -21 1 -2 -5.33 5.35 -21 -1 -3 43.33 5.54 -21 -1 -4 185.30 9.48 -21 -1 -5 310.42 12.16 -21 -3 -1 86.70 8.74 -21 -3 -2 3.00 5.12 -21 -3 -3 -4.39 4.99 -21 -3 -4 30.38 5.21 -21 -3 -5 129.48 9.76 -21 -3 -6 205.71 10.07 -21 -3 -7 186.85 12.15 -21 -5 0 404.21 11.09 -21 -5 -1 303.13 10.88 -21 -5 -2 103.71 9.48 -21 -5 -3 -5.99 5.35 -21 -5 -4 0.77 5.35 -21 -5 -5 54.70 5.98 -21 -5 -6 45.81 6.08 -21 -7 0 406.76 11.86 -21 -7 -1 329.88 11.31 -21 -7 1 305.24 10.88 -21 -7 -2 103.04 10.07 -21 -7 -3 0.23 5.43 -21 -7 -4 -14.45 5.19 -21 -7 -5 0.89 5.38 -21 -7 -6 -7.11 5.44 -21 -9 0 277.90 10.91 -21 -9 -1 139.27 9.90 -21 -9 1 139.84 9.99 -21 -9 -2 17.07 5.72 -21 -9 2 18.57 5.78 -21 -9 -3 -6.01 5.12 -21 -9 -4 -12.22 5.26 -21 -9 -5 17.79 5.67 -21 -11 0 29.73 5.60 -21 -11 -1 47.26 5.82 -21 -11 1 37.26 5.75 -21 -11 -2 8.43 5.41 -21 -11 2 7.69 5.19 -21 -11 -3 11.01 5.48 -22 -4 0 143.21 9.68 -22 -4 -1 104.76 9.28 -22 -4 -2 19.72 5.59 -22 -4 -3 -9.24 5.28 -22 -6 0 200.26 10.26 -22 -6 -1 177.59 10.25 -22 -6 1 170.94 9.78 -22 -6 -2 70.41 6.58 -22 -6 -3 6.96 5.40 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 66727 _shelx_shelxl_version_number 2014/7 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x, -y, -z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x, y, -z' '-x, y, z' 'x, -y, z' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z' 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 Zr1 Zr 0.0000 0.07391(3) 0.5000 0.0407(7) Uani 1 4 d S T P Zr2 Zr 0.07539(4) 0.0000 0.41466(4) 0.0464(7) Uani 1 2 d S T P O5 O 0.1063(3) 0.06093(18) 0.3807(3) 0.079(2) Uani 1 1 d . . . O1 O 0.0000 0.0362(2) 0.4150(5) 0.077(3) Uani 1 2 d S T P C2 C 0.1287(4) 0.1282(2) 0.3609(4) 0.066(3) Uani 1 1 d . . . O4 O 0.0578(3) 0.10806(15) 0.4359(3) 0.0569(15) Uani 1 1 d . . . O2 O 0.0740(5) 0.0360(3) 0.5000 0.093(4) Uani 1 2 d S T P C7 C 0.1277(5) 0.1674(3) 0.3815(5) 0.085(3) Uani 1 1 d . . . H7 H 0.1068 0.1739 0.4182 0.102 Uiso 1 1 calc R . . C6 C 0.1566(5) 0.1974(3) 0.3495(5) 0.086(3) Uani 1 1 d . . . H6 H 0.1546 0.2236 0.3641 0.103 Uiso 1 1 calc R . . C3 C 0.1599(5) 0.1196(3) 0.3076(5) 0.086(3) Uani 1 1 d . . . H3 H 0.1603 0.0934 0.2926 0.104 Uiso 1 1 calc R . . C5 C 0.1886(5) 0.1882(3) 0.2956(5) 0.082(3) Uani 1 1 d . . . C1 C 0.0948(4) 0.0972(3) 0.3960(5) 0.061(2) Uani 1 1 d . . . C4 C 0.1918(6) 0.1484(3) 0.2739(5) 0.100(4) Uani 1 1 d . . . H4 H 0.2143 0.1415 0.2385 0.119 Uiso 1 1 calc R . . O3 O 0.0682(5) 0.0000 0.3103(4) 0.085(3) Uani 1 2 d S T P O6 O 0.1681(4) 0.0000 0.4259(7) 0.116(4) Uani 1 2 d S TU P C9 C 0.2500 0.2500 0.2917(6) 0.081(4) Uani 1 2 d S T P H9 H 0.2500 0.2500 0.3367 0.097 Uiso 1 2 calc RS T P C8 C 0.2207(5) 0.2198(3) 0.2590(4) 0.084(3) Uani 1 1 d . . . C10 C 0.2204(6) 0.2203(3) 0.1925(5) 0.106(4) Uani 1 1 d . . . H10 H 0.2004 0.2008 0.1697 0.127 Uiso 1 1 calc R . . C11 C 0.2500 0.2500 0.1595(6) 0.117(7) Uani 1 2 d S T P C12 C 0.2500 0.2500 0.0879(11) 0.151(10) Uani 1 2 d S T P C13 C 0.2500 0.2500 0.0324(9) 0.146(10) Uani 1 2 d S T P C15 C 0.2549(12) 0.0000 0.5000 0.294(15) Uani 1 4 d DS TU P C16 C 0.2856(12) 0.0000 0.4418(14) 0.387(17) Uani 1 2 d DS TU P H16 H 0.2663 0.0000 0.4025 0.465 Uiso 1 2 calc RS T P C14 C 0.1920(12) 0.0000 0.5000 0.222(12) Uani 1 4 d DS TU P C17 C 0.3443(12) 0.0000 0.4434(16) 0.445(19) Uani 1 2 d DS TU P H17 H 0.3639 0.0000 0.4043 0.534 Uiso 1 2 calc RS T P C20 C 0.470(2) 0.024(3) 0.459(3) 0.54(3) Uani 0.5 1 d D U . C19 C 0.439(2) 0.0000 0.5000 0.52(3) Uani 1 4 d DS TU P C18 C 0.376(2) 0.0000 0.5000 0.50(2) Uani 1 4 d DS TU P O7 O 0.461(3) 0.026(3) 0.394(3) 0.57(3) Uani 0.5 1 d D U . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0378(10) 0.0236(9) 0.0606(10) 0.000 0.000 0.000 Zr2 0.0405(9) 0.0296(8) 0.0691(9) 0.000 0.0087(4) 0.000 O5 0.083(5) 0.043(4) 0.111(5) -0.008(3) 0.036(4) -0.017(3) O1 0.041(5) 0.036(5) 0.153(9) -0.035(5) 0.000 0.000 C2 0.076(6) 0.039(6) 0.084(6) -0.003(5) 0.007(5) -0.021(5) O4 0.056(4) 0.037(3) 0.077(4) -0.002(3) 0.014(3) -0.004(3) O2 0.126(9) 0.085(7) 0.067(5) 0.000 0.000 0.079(6) C7 0.109(8) 0.062(7) 0.084(6) -0.015(5) 0.034(6) -0.041(6) C6 0.123(9) 0.051(6) 0.083(7) -0.013(5) 0.033(6) -0.035(6) C3 0.114(9) 0.040(5) 0.105(7) -0.019(5) 0.036(7) -0.031(6) C5 0.115(9) 0.060(7) 0.072(6) -0.004(5) 0.002(6) -0.051(6) C1 0.072(7) 0.029(6) 0.081(6) 0.001(5) 0.002(5) -0.015(5) C4 0.138(10) 0.068(7) 0.093(7) -0.022(6) 0.048(7) -0.056(7) O3 0.134(9) 0.051(5) 0.071(6) 0.000 0.013(5) 0.000 O6 0.040(6) 0.081(7) 0.228(13) 0.000 0.019(6) 0.000 C9 0.103(11) 0.073(9) 0.067(8) 0.000 0.000 -0.048(9) C8 0.118(9) 0.069(7) 0.066(6) -0.001(5) 0.007(5) -0.052(6) C10 0.158(11) 0.092(8) 0.068(7) -0.002(6) 0.011(6) -0.082(8) C11 0.173(18) 0.131(14) 0.047(8) 0.000 0.000 -0.066(14) C12 0.22(3) 0.123(17) 0.107(18) 0.000 0.000 -0.114(18) C13 0.24(3) 0.138(17) 0.055(9) 0.000 0.000 -0.098(17) C15 0.084(12) 0.51(4) 0.28(3) 0.000 0.000 0.000 C16 0.116(16) 0.66(4) 0.39(3) 0.000 0.096(14) 0.000 C14 0.080(12) 0.34(3) 0.244(17) 0.000 0.000 0.000 C17 0.121(16) 0.74(5) 0.47(4) 0.000 0.072(15) 0.000 C20 0.18(3) 0.83(7) 0.62(6) 0.02(3) 0.03(3) 0.01(3) C19 0.17(3) 0.80(6) 0.58(6) 0.000 0.000 0.000 C18 0.17(3) 0.78(6) 0.54(4) 0.000 0.000 0.000 O7 0.25(4) 0.83(8) 0.63(6) 0.05(4) 0.02(4) 0.02(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0015 0.0009 '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 0.0056 0.0036 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -0.5364 2.6141 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Zr2 Zr1 Zr2 60.42(3) . 10_556 Zr2 Zr1 Zr2 90.58(3) 2 10_556 Zr2 Zr1 Zr2 60.24(3) 9_556 10_556 Zr2 Zr1 Zr2 60.42(3) 2 9_556 Zr2 Zr1 Zr2 90.58(3) . 9_556 Zr2 Zr1 Zr2 60.24(3) . 2 O1 Zr1 Zr2 89.9(2) 10_556 2 O1 Zr1 Zr2 89.9(2) . 9_556 O1 Zr1 Zr2 35.03(13) 10_556 9_556 O1 Zr1 Zr2 35.02(13) . 2 O1 Zr1 Zr2 89.9(2) . 10_556 O1 Zr1 Zr2 35.02(13) . . O1 Zr1 Zr2 35.03(13) 10_556 10_556 O1 Zr1 Zr2 89.9(2) 10_556 . O1 Zr1 O1 108.7(5) 10_556 . O1 Zr1 O4 142.06(16) . 10_556 O1 Zr1 O4 142.06(16) 10_556 11 O1 Zr1 O4 79.2(3) . 11 O1 Zr1 O4 142.06(16) 10_556 . O1 Zr1 O4 79.2(3) . . O1 Zr1 O4 79.2(3) 10_556 4_556 O1 Zr1 O4 79.2(3) 10_556 10_556 O1 Zr1 O4 142.06(16) . 4_556 O4 Zr1 Zr2 75.79(15) 11 2 O4 Zr1 Zr2 166.36(15) 11 10_556 O4 Zr1 Zr2 75.79(15) 4_556 9_556 O4 Zr1 Zr2 111.57(15) 11 . O4 Zr1 Zr2 111.57(15) 10_556 9_556 O4 Zr1 Zr2 75.79(15) . . O4 Zr1 Zr2 111.02(15) . 10_556 O4 Zr1 Zr2 75.79(15) 10_556 10_556 O4 Zr1 Zr2 166.36(15) . 9_556 O4 Zr1 Zr2 111.57(15) 4_556 10_556 O4 Zr1 Zr2 111.57(15) . 2 O4 Zr1 Zr2 111.02(15) 10_556 . O4 Zr1 Zr2 166.36(15) 10_556 2 O4 Zr1 Zr2 111.02(15) 11 9_556 O4 Zr1 Zr2 111.02(15) 4_556 2 O4 Zr1 Zr2 166.36(15) 4_556 . O4 Zr1 O4 75.3(3) . 11 O4 Zr1 O4 117.8(3) . 4_556 O4 Zr1 O4 117.8(3) 10_556 11 O4 Zr1 O4 73.8(3) . 10_556 O4 Zr1 O4 75.3(3) 10_556 4_556 O4 Zr1 O4 73.8(3) 11 4_556 O2 Zr1 Zr2 89.4(3) 11 . O2 Zr1 Zr2 34.85(16) . 10_556 O2 Zr1 Zr2 89.4(3) . 2 O2 Zr1 Zr2 89.4(3) . 9_556 O2 Zr1 Zr2 89.4(3) 11 10_556 O2 Zr1 Zr2 34.85(16) . . O2 Zr1 Zr2 34.85(16) 11 2 O2 Zr1 Zr2 34.85(16) 11 9_556 O2 Zr1 O1 69.8(2) 11 10_556 O2 Zr1 O1 69.8(2) . . O2 Zr1 O1 69.8(2) 11 . O2 Zr1 O1 69.8(2) . 10_556 O2 Zr1 O4 79.2(3) 11 11 O2 Zr1 O4 142.92(15) 11 . O2 Zr1 O4 79.2(3) 11 4_556 O2 Zr1 O4 79.2(3) . . O2 Zr1 O4 142.92(15) . 11 O2 Zr1 O4 142.92(15) . 4_556 O2 Zr1 O4 79.2(3) . 10_556 O2 Zr1 O4 142.92(15) 11 10_556 O2 Zr1 O2 107.5(7) . 11 Zr1 Zr2 Zr1 89.42(3) 9_556 . Zr1 Zr2 Zr2 59.879(16) . 2 Zr1 Zr2 Zr2 59.791(16) 9_556 10_556 Zr1 Zr2 Zr2 59.791(16) . 10_556 Zr1 Zr2 Zr2 59.879(16) 9_556 2 Zr2 Zr2 Zr2 90.0 2 10_556 O5 Zr2 Zr1 71.62(16) . . O5 Zr2 Zr1 161.04(16) . 9_556 O5 Zr2 Zr1 71.63(16) 12 9_556 O5 Zr2 Zr1 161.05(16) 12 . O5 Zr2 Zr2 108.01(18) 12 10_556 O5 Zr2 Zr2 108.01(18) . 10_556 O5 Zr2 Zr2 108.56(18) 12 2 O5 Zr2 Zr2 108.56(18) . 2 O5 Zr2 O5 127.3(3) 12 . O1 Zr2 Zr1 35.6(2) . . O1 Zr2 Zr1 89.0(2) 2 . O1 Zr2 Zr1 89.0(2) . 9_556 O1 Zr2 Zr1 35.5(2) 2 9_556 O1 Zr2 Zr2 34.45(18) . 2 O1 Zr2 Zr2 89.8(3) 2 10_556 O1 Zr2 Zr2 89.8(3) . 10_556 O1 Zr2 Zr2 34.45(18) 2 2 O1 Zr2 O5 75.9(3) 2 12 O1 Zr2 O5 140.4(3) . 12 O1 Zr2 O5 140.4(3) 2 . O1 Zr2 O5 75.9(3) . . O1 Zr2 O1 68.9(4) . 2 O1 Zr2 O2 107.6(4) . 3_556 O1 Zr2 O2 70.5(3) 2 3_556 O1 Zr2 O2 107.6(4) 2 . O1 Zr2 O2 70.5(3) . . O1 Zr2 O3 86.5(4) 2 . O1 Zr2 O3 86.5(4) . . O1 Zr2 O6 145.04(18) . . O1 Zr2 O6 145.03(18) 2 . O2 Zr2 Zr1 88.4(3) 3_556 . O2 Zr2 Zr1 88.4(3) . 9_556 O2 Zr2 Zr1 35.0(2) . . O2 Zr2 Zr1 35.0(2) 3_556 9_556 O2 Zr2 Zr2 89.1(3) 3_556 2 O2 Zr2 Zr2 89.1(3) . 2 O2 Zr2 Zr2 34.3(2) . 10_556 O2 Zr2 Zr2 34.3(2) 3_556 10_556 O2 Zr2 O5 75.9(3) . . O2 Zr2 O5 139.9(3) 3_556 . O2 Zr2 O5 75.9(3) 3_556 12 O2 Zr2 O5 139.9(3) . 12 O2 Zr2 O2 68.5(5) . 3_556 O2 Zr2 O3 145.4(2) . . O2 Zr2 O3 145.4(2) 3_556 . O2 Zr2 O6 85.8(4) . . O2 Zr2 O6 85.8(4) 3_556 . O3 Zr2 Zr1 117.55(18) . . O3 Zr2 Zr1 117.55(18) . 9_556 O3 Zr2 Zr2 175.5(3) . 10_556 O3 Zr2 Zr2 85.5(3) . 2 O3 Zr2 O5 73.5(2) . 12 O3 Zr2 O5 73.5(2) . . O3 Zr2 O6 100.6(5) . . O6 Zr2 Zr1 116.4(2) . 9_556 O6 Zr2 Zr1 116.4(2) . . O6 Zr2 Zr2 173.9(4) . 2 O6 Zr2 Zr2 83.9(4) . 10_556 O6 Zr2 O5 73.5(2) . . O6 Zr2 O5 73.5(2) . 12 C1 O5 Zr2 134.8(6) . . Zr2 O1 Zr1 109.4(3) 2 . Zr2 O1 Zr1 109.4(3) . . Zr2 O1 Zr2 111.1(4) . 2 C7 C2 C1 120.0(9) . . C3 C2 C7 117.5(8) . . C3 C2 C1 122.5(8) . . C1 O4 Zr1 132.1(5) . . Zr2 O2 Zr1 110.2(3) . . Zr2 O2 Zr1 110.2(3) 10_556 . Zr2 O2 Zr2 111.5(5) . 10_556 C2 C7 H7 118.9 . . C6 C7 C2 122.3(9) . . C6 C7 H7 118.9 . . C7 C6 H6 120.2 . . C7 C6 C5 119.6(9) . . C5 C6 H6 120.2 . . C2 C3 H3 118.4 . . C2 C3 C4 123.1(8) . . C4 C3 H3 118.4 . . C6 C5 C4 120.0(8) . . C6 C5 C8 121.5(9) . . C4 C5 C8 118.5(9) . . O5 C1 C2 115.1(9) . . O4 C1 O5 125.6(7) . . O4 C1 C2 119.3(8) . . C3 C4 C5 117.4(9) . . C3 C4 H4 121.3 . . C5 C4 H4 121.3 . . C14 O6 Zr2 116.2(12) . . C8 C9 H9 119.0 . . C8 C9 H9 119.0 6 . C8 C9 C8 121.9(12) . 6 C9 C8 C5 120.7(8) . . C10 C8 C5 120.7(8) . . C10 C8 C9 118.6(9) . . C8 C10 H10 120.1 . . C8 C10 C11 119.9(9) . . C11 C10 H10 120.1 . . C10 C11 C10 121.1(12) . 6 C10 C11 C12 119.4(6) 6 . C10 C11 C12 119.5(6) . . C13 C12 C11 180.0 . . C12 C13 C13 180.0 . 13 C16 C15 C16 118(3) 10_556 . C16 C15 C14 120.8(17) 10_556 . C16 C15 C14 120.8(17) . . C15 C16 H16 120.3 . . C17 C16 C15 119(3) . . C17 C16 H16 120.3 . . O6 C14 O6 140(2) 10_556 . C15 C14 O6 110.0(10) . . C15 C14 O6 110.0(10) . 10_556 C16 C17 H17 118.1 . . C16 C17 C18 124(3) . . C18 C17 H17 118.1 . . C20 C20 C20 90.000(15) 11_655 12 C20 C20 C20 90.000(17) 11_655 10_556 C20 C20 C20 89.999(6) 12 10_556 C19 C20 C20 122(3) . 11_655 C19 C20 C20 54(4) . 12 C19 C20 C20 52(4) . 10_556 O7 C20 C20 171(5) . 10_556 O7 C20 C20 98(4) . 11_655 O7 C20 C20 93(7) . 12 O7 C20 C19 124(7) . . C20 C19 C20 76(7) 12 3_556 C20 C19 C20 72(9) 10_556 3_556 C20 C19 C20 117(6) 10_556 12 C20 C19 C20 72(9) 12 . C20 C19 C20 76(7) 10_556 . C20 C19 C20 117(6) 3_556 . C20 C19 C18 122(3) . . C20 C19 C18 122(3) 3_556 . C20 C19 C18 122(3) 12 . C20 C19 C18 122(3) 10_556 . C17 C18 C17 115(4) 10_556 . C17 C18 C19 123(2) 10_556 . C17 C18 C19 123(2) . . C20 O7 O7 82(4) . 11_655 C20 O7 O7 87(7) . 12 O7 O7 O7 89.998(11) 12 11_655 loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Zr1 Zr2 3.5095(10) . Zr1 Zr2 3.5095(10) 9_556 Zr1 Zr2 3.5095(10) 10_556 Zr1 Zr2 3.5095(10) 2 Zr1 O1 2.164(8) . Zr1 O1 2.164(8) 10_556 Zr1 O4 2.210(6) . Zr1 O4 2.210(6) 4_556 Zr1 O4 2.210(6) 11 Zr1 O4 2.210(6) 10_556 Zr1 O2 2.144(8) 11 Zr1 O2 2.144(8) . Zr2 Zr1 3.5094(10) 9_556 Zr2 Zr2 3.5224(19) 2 Zr2 Zr2 3.5317(19) 10_556 Zr2 O5 2.271(6) . Zr2 O5 2.271(6) 12 Zr2 O1 2.136(5) 2 Zr2 O1 2.136(5) . Zr2 O2 2.136(6) 3_556 Zr2 O2 2.136(6) . Zr2 O3 2.166(9) . Zr2 O6 2.179(10) . O5 C1 1.282(10) . O1 Zr2 2.136(5) 2 C2 C7 1.378(13) . C2 C3 1.352(12) . C2 C1 1.493(12) . O4 C1 1.248(11) . O2 Zr2 2.136(6) 10_556 C7 H7 0.9300 . C7 C6 1.375(13) . C6 H6 0.9300 . C6 C5 1.375(13) . C3 H3 0.9300 . C3 C4 1.402(13) . C5 C4 1.403(14) . C5 C8 1.502(13) . C4 H4 0.9300 . O6 C14 1.631(16) . C9 H9 0.9300 . C9 C8 1.394(11) . C9 C8 1.394(11) 6 C8 C10 1.377(13) . C10 H10 0.9300 . C10 C11 1.389(11) . C11 C10 1.389(11) 6 C11 C12 1.48(3) . C12 C13 1.15(2) . C13 C13 1.34(4) 13 C15 C16 1.401(18) 10_556 C15 C16 1.401(18) . C15 C14 1.469(19) . C16 H16 0.9300 . C16 C17 1.372(18) . C14 O6 1.631(16) 10_556 C17 H17 0.9300 . C17 C18 1.388(19) . C20 C20 1.71(14) 10_556 C20 C20 1.62(18) 12 C20 C20 1.41(11) 11_655 C20 C19 1.385(19) . C20 O7 1.36(2) . C19 C20 1.385(19) 10_556 C19 C20 1.385(19) 12 C19 C20 1.385(19) 3_556 C19 C18 1.46(2) . C18 C17 1.387(19) 10_556 O7 O7 1.8(2) 12 O7 O7 1.81(14) 11_655 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_4 Zr1 O4 C1 O5 3.3(15) . . Zr1 O4 C1 C2 -178.1(6) . . Zr2 O5 C1 C2 177.8(6) . . Zr2 O5 C1 O4 -3.6(16) . . Zr2 O6 C14 O6 0.000(3) . 10_556 Zr2 O6 C14 C15 180.000(2) . . C2 C7 C6 C5 -1.1(18) . . C2 C3 C4 C5 -2.9(19) . . C7 C2 C3 C4 1.5(17) . . C7 C2 C1 O5 -168.0(9) . . C7 C2 C1 O4 13.2(15) . . C7 C6 C5 C4 -0.4(18) . . C7 C6 C5 C8 179.9(11) . . C6 C5 C4 C3 2.3(18) . . C6 C5 C8 C9 40.8(16) . . C6 C5 C8 C10 -137.1(13) . . C3 C2 C7 C6 0.6(17) . . C3 C2 C1 O5 13.8(14) . . C3 C2 C1 O4 -165.0(10) . . C5 C8 C10 C11 179.5(10) . . C1 C2 C7 C6 -177.7(11) . . C1 C2 C3 C4 179.7(11) . . C4 C5 C8 C9 -138.9(11) . . C4 C5 C8 C10 43.2(18) . . C9 C8 C10 C11 1.5(18) . . C8 C5 C4 C3 -178.0(11) . . C8 C9 C8 C5 -178.7(13) 6 . C8 C9 C8 C10 -0.8(9) 6 . C8 C10 C11 C10 -0.8(9) . 6 C8 C10 C11 C12 179.2(9) . . C15 C16 C17 C18 0.000(5) . . C16 C15 C16 C17 0.000(4) 10_556 . C16 C15 C14 O6 180.000(2) . 10_556 C16 C15 C14 O6 0.000(2) . . C16 C15 C14 O6 180.000(2) 10_556 . C16 C15 C14 O6 0.000(2) 10_556 10_556 C16 C17 C18 C17 0.000(4) . 10_556 C16 C17 C18 C19 180.000(2) . . C14 C15 C16 C17 180.000(4) . . C20 C20 C19 C20 -61(5) 10_556 3_556 C20 C20 C19 C20 125(4) 12 10_556 C20 C20 C19 C20 64(4) 12 3_556 C20 C20 C19 C20 -125(4) 10_556 12 C20 C20 C19 C20 61(5) 11_655 10_556 C20 C20 C19 C20 0.00(3) 11_655 3_556 C20 C20 C19 C20 -64(4) 11_655 12 C20 C20 C19 C18 -116(4) 12 . C20 C20 C19 C18 119(5) 10_556 . C20 C20 C19 C18 180.00(3) 11_655 . C20 C20 O7 O7 90.4(12) 11_655 12 C20 C20 O7 O7 -90.4(12) 12 11_655 C20 C20 O7 O7 0.002(9) 11_655 11_655 C20 C20 O7 O7 0.000(6) 12 12 C20 C19 C18 C17 -43(5) 10_556 10_556 C20 C19 C18 C17 -43(5) 12 . C20 C19 C18 C17 -137(5) 3_556 . C20 C19 C18 C17 137(5) 10_556 . C20 C19 C18 C17 43(5) 3_556 10_556 C20 C19 C18 C17 43(5) . . C20 C19 C18 C17 137(5) 12 10_556 C20 C19 C18 C17 -137(5) . 10_556 C19 C20 O7 O7 -48(9) . 12 C19 C20 O7 O7 -138(10) . 11_655 O7 C20 C19 C20 65(11) . 12 O7 C20 C19 C20 129(13) . 3_556 O7 C20 C19 C20 -170(8) . 10_556 O7 C20 C19 C18 -51(13) . .