#------------------------------------------------------------------------------ #$Date: 2021-11-04 01:57:54 +0200 (Thu, 04 Nov 2021) $ #$Revision: 270275 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/86/7708689.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_7708689 loop_ _publ_author_name 'Wang, Xiangxiang' 'Zhang, Hao' 'Qi, Chao' 'Zhou, Fan' 'Ni, Linhan' 'Chen, Saisai' 'Qi, Junwen' 'Wang, Chaohai' 'Zheng, Tao' 'Li, Jiansheng' _publ_section_title ; Hydrangea-like architectures composed of Zr-based metal--organic framework nanosheets with enhanced iodine capture ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT02748D _journal_year 2021 _chemical_formula_moiety 'C83 H57 N2 O32 Zr6, 12[H2O]' _chemical_formula_sum 'C83 H81 N2 O44 Zr6' _chemical_formula_weight 2357.81 _space_group_crystal_system tetragonal _space_group_IT_number 121 _space_group_name_Hall 'I -4 2' _space_group_name_H-M_alt 'I -4 2 m' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-10-12 _audit_creation_method ; Olex2 1.5-dev (compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6225) ; _audit_update_record ; 2021-10-13 deposited with the CCDC. 2021-10-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 30.976(7) _cell_length_b 30.976(7) _cell_length_c 24.946(5) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 296(2) _cell_measurement_theta_max 17.57 _cell_measurement_theta_min 2.47 _cell_volume 23936(9) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _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 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/3 (Sheldrick, 2018)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.978 _diffrn_measured_fraction_theta_max 0.978 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0906 _diffrn_reflns_av_unetI/netI 0.0463 _diffrn_reflns_Laue_measured_fraction_full 0.978 _diffrn_reflns_Laue_measured_fraction_max 0.978 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 35923 _diffrn_reflns_point_group_measured_fraction_full 0.979 _diffrn_reflns_point_group_measured_fraction_max 0.979 _diffrn_reflns_theta_full 17.691 _diffrn_reflns_theta_max 17.691 _diffrn_reflns_theta_min 2.135 _exptl_absorpt_coefficient_mu 0.578 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_correction_T_min 0.980 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'Bruker, SADABS' _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.309 _exptl_crystal_description block _exptl_crystal_F_000 9480 _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.226 _refine_diff_density_min -0.248 _refine_diff_density_rms 0.040 _refine_ls_abs_structure_details ; Flack x determined using 1510 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.04(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 533 _refine_ls_number_reflns 4000 _refine_ls_number_restraints 1505 _refine_ls_restrained_S_all 0.997 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0318 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+35.7868P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.0749 _reflns_Friedel_coverage 0.834 _reflns_Friedel_fraction_full 0.980 _reflns_Friedel_fraction_max 0.980 _reflns_number_gt 3579 _reflns_number_total 4000 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt02748d2.cif _cod_data_source_block b _cod_original_cell_volume 23936(12) _cod_database_code 7708689 _shelx_shelxl_version_number 2018/3 _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 At 1.5 times of: All O(H,H) groups 2. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A All non-hydrogen atoms restrained to be isotropic: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O10) \\sim Ueq, Uanis(O8) \\sim Ueq, Uanis(O9) \\sim Ueq, Uanis(O15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 5.a Riding coordinates: C41(H41), C43(H43) 5.b Rotating group: O12(H12A,H12B) 5.c Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14), C15(H15), C17(H17), C18(H18), C20(H20), C21(H21), C23(H23), C24(H24), C26(H26), C27(H27), C29(H29), C30(H30), C32(H32), C33(H33), C35(H35), C36(H36), C40(H40), C42(H42) 5.d Fitted hexagon refined as free rotating group: C13(C14,C15,C16,C17,C18), C25(C26,C27,C28,C29,C30), C31(C32,C33,C34,C35,C36) ; _smtbx_masks_special_details ; A solvent mask was calculated and 1010 electrons were found in a volume of 9238\%A^3^ in 2 voids per unit cell. This is consistent with the presence of 12[H2O] per Formula Unit which account for 960 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL B I -4 R = 0.04 New:I-42m b.res created by SHELXL-2018/3 at 09:51:10 on 12-Oct-2021 REM RESI 0 REM ##### CELL 0.71073 30.976 30.976 24.946 90 90 90 ZERR 8 0.007 0.007 0.005 0 0 0 LATT -2 SYMM +Y,-X,-Z SYMM -X,-Y,+Z SYMM -Y,+X,-Z SYMM +X,-Y,-Z SYMM -Y,-X,+Z SYMM -X,+Y,-Z SYMM +Y,+X,+Z SFAC C H N O Zr UNIT 664 648 16 352 48 DELU SIMU ISOR 0.01 0.02 RIGU 0.001 0.001 ISOR 0.005 0.01 O10 O8 O9 O15 L.S. 20 0 143 PLAN 40 TEMP 23 CONF CONN 8 $Zr LIST 4 BOND $H MORE -1 ABIN fmap 2 acta REM REM REM > REM REM > REM > REM REM WGHT 0.036900 35.786804 FVAR 0.09326 ZR1 5 0.732477 0.186681 0.832558 11.00000 0.03908 0.03980 = 0.01867 0.00201 -0.00198 -0.02051 ZR2 5 0.836801 0.163199 0.786626 10.50000 0.04217 0.04217 = 0.01884 -0.00434 0.00434 -0.02121 ZR3 5 0.775286 0.224714 0.954557 10.50000 0.04120 0.04120 = 0.01661 -0.00356 0.00356 -0.01771 ZR4 5 0.799445 0.120373 0.910282 11.00000 0.04392 0.03455 = 0.01880 0.00430 -0.00173 -0.01721 O1 4 0.372379 -0.194717 0.344978 11.00000 0.03786 0.02474 = 0.05471 0.00338 -0.02088 -0.01498 O2 4 0.413031 -0.234277 0.401800 11.00000 0.04166 0.03976 = 0.03515 -0.00173 -0.01942 -0.01378 O3 4 0.771258 0.111886 -0.007127 11.00000 0.04034 0.05117 = 0.02529 0.00166 0.00210 -0.01393 O4 4 0.754739 0.179631 0.017068 11.00000 0.05343 0.05380 = 0.02357 -0.00396 0.01029 -0.01441 O5 4 0.791065 0.148001 0.719051 11.00000 0.06903 0.07021 = 0.01651 -0.00766 0.00104 -0.02668 O6 4 0.723645 0.159342 0.750982 11.00000 0.05287 0.04849 = 0.02611 0.00362 -0.01375 -0.02737 O7 4 0.849159 0.150841 0.868212 10.50000 0.03555 0.03555 = 0.03055 0.00410 -0.00410 -0.01103 O8 4 0.872170 0.218928 0.823884 11.00000 0.03240 0.04002 = 0.01278 0.00843 0.00183 -0.01021 O9 4 0.758965 0.173120 0.905356 11.00000 0.03515 0.03682 = 0.02140 0.00370 -0.00035 -0.02510 O10 4 0.790344 0.209656 0.803697 10.50000 0.03857 0.03857 = 0.01195 0.00470 -0.00470 -0.01611 O11 4 0.674943 0.205579 0.880376 11.00000 0.04089 0.06092 = 0.07527 -0.00783 0.01220 -0.01551 O12 4 0.812434 0.055242 0.877163 11.00000 0.09618 0.04004 = 0.06440 -0.01411 -0.00611 -0.01786 AFIX 7 H12A 2 0.799456 0.051886 0.846685 11.00000 -1.50000 H12B 2 0.800885 0.035728 0.897421 11.00000 -1.50000 AFIX 0 O13 4 0.853779 0.090170 0.955345 11.00000 0.07066 0.04878 = 0.05216 0.01309 -0.01746 -0.00301 O14 4 0.903394 0.146313 0.766439 11.00000 0.06647 0.08593 = 0.06745 -0.02013 0.02208 0.00765 O15 4 0.827440 0.172560 0.963414 10.50000 0.03737 0.03737 = 0.02723 0.00310 -0.00310 -0.02099 O16 4 0.750047 0.249953 0.872962 10.50000 0.03768 0.03768 = 0.02995 0.00062 -0.00062 -0.00951 O17 4 0.698680 0.237123 0.784832 11.00000 0.07299 0.07479 = 0.04615 -0.00580 -0.02411 0.01083 N1 3 0.632190 0.030741 0.371900 11.00000 0.04268 0.03594 = 0.02667 0.00284 -0.00054 -0.01344 C1 1 0.434708 -0.163744 0.375764 11.00000 0.02293 0.03110 = 0.04012 -0.00553 -0.00605 -0.00396 C2 1 0.435080 -0.132329 0.337200 11.00000 0.03039 0.03144 = 0.04203 -0.00309 -0.00178 0.00062 AFIX 43 H2 2 0.415026 -0.133371 0.309486 11.00000 -1.20000 AFIX 0 C3 1 0.465113 -0.098728 0.338824 11.00000 0.03360 0.02797 = 0.03657 -0.00491 0.00413 0.00084 AFIX 43 H3 2 0.464290 -0.077844 0.312059 11.00000 -1.20000 AFIX 0 C4 1 0.496123 -0.095213 0.378714 11.00000 0.03400 0.03478 = 0.03119 -0.00429 0.00853 -0.00688 C5 1 0.497097 -0.127505 0.418303 11.00000 0.03445 0.04456 = 0.04255 0.00565 -0.00668 -0.02227 AFIX 43 H5 2 0.517758 -0.126377 0.445315 11.00000 -1.20000 AFIX 0 C6 1 0.467790 -0.160622 0.417327 11.00000 0.02661 0.03381 = 0.03769 -0.00268 -0.00496 -0.01263 AFIX 43 H6 2 0.468987 -0.181690 0.443846 11.00000 -1.20000 AFIX 0 C7 1 0.531386 -0.063130 0.379365 11.00000 0.04935 0.04472 = 0.02789 0.00750 -0.00440 -0.01945 C8 1 0.543886 -0.043389 0.329794 11.00000 0.04700 0.05417 = 0.02348 0.00607 -0.00667 -0.02134 AFIX 43 H8 2 0.530153 -0.051586 0.298243 11.00000 -1.20000 AFIX 0 C9 1 0.575722 -0.012629 0.327964 11.00000 0.04678 0.04833 = 0.01591 -0.00387 0.00339 -0.01861 AFIX 43 H9 2 0.582700 0.000105 0.295334 11.00000 -1.20000 AFIX 0 C10 1 0.597138 -0.000485 0.372718 11.00000 0.04357 0.03876 = 0.01576 -0.00086 0.00254 -0.01495 C11 1 0.585993 -0.018988 0.420361 11.00000 0.03843 0.04092 = 0.01766 0.00142 0.00403 -0.01096 AFIX 43 H11 2 0.600176 -0.011354 0.451823 11.00000 -1.20000 AFIX 0 C12 1 0.553605 -0.048953 0.421040 11.00000 0.05245 0.05233 = 0.02364 0.01208 -0.00463 -0.02416 AFIX 43 H12 2 0.546463 -0.060568 0.454254 11.00000 -1.20000 AFIX 66 C13 1 0.738299 0.120645 0.075782 11.00000 0.06134 0.05945 = 0.04416 0.01078 0.02375 0.00351 C14 1 0.731105 0.149288 0.117734 11.00000 0.09264 0.05931 = 0.04808 0.01117 0.03828 -0.00067 AFIX 43 H14 2 0.736964 0.178514 0.113273 11.00000 -1.20000 AFIX 65 C15 1 0.715154 0.134250 0.166352 11.00000 0.10846 0.05516 = 0.05072 0.00773 0.04216 -0.01232 AFIX 43 H15 2 0.710341 0.153414 0.194421 11.00000 -1.20000 AFIX 65 C16 1 0.706397 0.090568 0.173019 11.00000 0.07587 0.05497 = 0.04457 0.00785 0.01622 -0.01356 C17 1 0.713591 0.061924 0.131068 11.00000 0.12968 0.05861 = 0.05724 0.00241 0.04110 -0.02075 AFIX 43 H17 2 0.707732 0.032698 0.135529 11.00000 -1.20000 AFIX 65 C18 1 0.729541 0.076962 0.082450 11.00000 0.10814 0.06134 = 0.05836 0.00753 0.03944 -0.00761 AFIX 43 H18 2 0.734354 0.057798 0.054382 11.00000 -1.20000 AFIX 0 O18 4 0.702801 0.232905 0.964725 11.00000 0.05661 0.07664 = 0.05744 0.00286 0.02025 -0.00377 C19 1 0.687874 0.074470 0.225917 11.00000 0.04494 0.04415 = 0.04114 0.00555 0.00485 -0.01352 C20 1 0.679650 0.101795 0.269354 11.00000 0.08483 0.04274 = 0.04778 0.00261 0.02005 -0.02411 AFIX 43 H20 2 0.687409 0.130723 0.266757 11.00000 -1.20000 AFIX 0 C21 1 0.661083 0.087856 0.314360 11.00000 0.05331 0.03363 = 0.04152 0.00430 0.00737 -0.01364 AFIX 43 H21 2 0.654463 0.107787 0.341001 11.00000 -1.20000 AFIX 0 C22 1 0.651282 0.044708 0.322886 11.00000 0.03568 0.03301 = 0.03121 0.00360 0.00219 -0.01030 C23 1 0.662315 0.015868 0.283765 11.00000 0.04780 0.03715 = 0.03388 0.00153 0.00433 -0.00777 AFIX 43 H23 2 0.657774 -0.013475 0.289285 11.00000 -1.20000 AFIX 0 C24 1 0.680227 0.029957 0.235888 11.00000 0.05538 0.04506 = 0.03621 -0.00174 0.00727 -0.01956 AFIX 43 H24 2 0.687393 0.009808 0.209722 11.00000 -1.20000 AFIX 66 C25 1 0.731991 0.131407 0.662230 11.00000 0.06074 0.05827 = 0.03206 -0.00251 -0.00418 -0.02238 C26 1 0.689059 0.118452 0.660212 11.00000 0.06280 0.07803 = 0.03930 -0.01642 -0.00057 -0.02818 AFIX 43 H26 2 0.671897 0.120247 0.690720 11.00000 -1.20000 AFIX 65 C27 1 0.671778 0.102814 0.612596 11.00000 0.05629 0.08981 = 0.04072 -0.01792 -0.00276 -0.02468 AFIX 43 H27 2 0.643054 0.094147 0.611246 11.00000 -1.20000 AFIX 65 C28 1 0.697429 0.100131 0.566999 11.00000 0.05495 0.04967 = 0.03758 -0.00630 -0.00517 -0.01116 C29 1 0.740361 0.113086 0.569016 11.00000 0.05895 0.09455 = 0.03866 -0.01572 -0.00104 -0.02406 AFIX 43 H29 2 0.757523 0.111291 0.538508 11.00000 -1.20000 AFIX 65 C30 1 0.757642 0.128724 0.616631 11.00000 0.06483 0.09330 = 0.03831 -0.01459 0.00110 -0.03519 AFIX 43 H30 2 0.786366 0.137392 0.617981 11.00000 -1.20000 AFIX 66 C31 1 0.679497 0.084121 0.514875 11.00000 0.05479 0.03837 = 0.03368 0.00163 -0.00626 -0.00732 C32 1 0.705283 0.057431 0.483551 11.00000 0.05428 0.06240 = 0.04203 -0.01073 -0.01550 0.00523 AFIX 43 H32 2 0.733274 0.050982 0.494395 11.00000 -1.20000 AFIX 65 C33 1 0.689232 0.040381 0.436020 11.00000 0.05236 0.05388 = 0.03771 -0.00517 -0.01024 -0.00036 AFIX 43 H33 2 0.706484 0.022523 0.415062 11.00000 -1.20000 AFIX 65 C34 1 0.647395 0.050020 0.419811 11.00000 0.04540 0.02120 = 0.02820 0.00713 -0.00401 -0.01453 C35 1 0.621609 0.076710 0.451135 11.00000 0.04997 0.04086 = 0.04046 -0.00734 -0.00538 -0.00932 AFIX 43 H35 2 0.593617 0.083159 0.440290 11.00000 -1.20000 AFIX 65 C36 1 0.637659 0.093761 0.498666 11.00000 0.05477 0.03955 = 0.04371 -0.01013 -0.00879 -0.00436 AFIX 43 H36 2 0.620406 0.111618 0.519623 11.00000 -1.20000 AFIX 0 C37 1 0.403810 -0.199888 0.374031 11.00000 0.02794 0.03646 = 0.02861 -0.00513 -0.00542 -0.00897 C38 1 0.754722 0.139466 0.022694 11.00000 0.04948 0.05431 = 0.03658 -0.00030 0.01192 -0.01401 C39 1 0.750700 0.150252 0.713725 11.00000 0.06819 0.05292 = 0.03273 -0.00197 -0.00351 -0.02782 C40 1 0.891226 0.108774 0.969478 10.50000 0.07776 0.07776 = 0.07017 0.01956 -0.01956 -0.01803 AFIX 43 H40 2 0.907369 0.092632 0.993692 10.50000 -1.20000 AFIX 0 C41 1 0.895916 0.104084 0.756641 10.50000 0.08424 0.08424 = 0.08022 -0.01388 0.01388 0.00690 AFIX 3 H41 2 0.913306 0.086690 0.744522 10.50000 -1.20000 AFIX 0 C42 1 0.670131 0.219728 0.930142 11.00000 0.06668 0.08411 = 0.07528 -0.01059 0.00972 -0.00011 AFIX 43 H42 2 0.642063 0.220977 0.943285 11.00000 -1.20000 AFIX 0 C43 1 0.722558 0.277442 0.768273 10.50000 0.09795 0.09795 = 0.12271 0.02376 -0.02376 -0.00490 AFIX 3 H43 2 0.707538 0.292470 0.741923 10.50000 -1.20000 AFIX 0 HKLF 4 1 0 1 0 -1 0 0 0 0 1 REM B I -4 R = 0.04 New:I-42m REM wR2 = 0.0749, GooF = S = 1.065, Restrained GooF = 0.997 for all data REM R1 = 0.0318 for 3579 Fo > 4sig(Fo) and 0.0388 for all 4000 data REM 533 parameters refined using 1505 restraints END WGHT 0.0370 35.7487 REM Highest difference peak 0.226, deepest hole -0.248, 1-sigma level 0.040 Q1 1 0.7359 0.2641 0.7047 10.50000 0.05 0.23 Q2 1 0.7691 0.2089 0.1628 11.00000 0.05 0.22 Q3 1 0.6711 0.2685 0.7998 11.00000 0.05 0.20 Q4 1 0.8067 0.1933 0.7165 10.50000 0.05 0.20 Q5 1 0.7667 0.0917 0.6427 11.00000 0.05 0.20 Q6 1 0.8039 0.2040 0.7992 11.00000 0.05 0.19 Q7 1 0.5000 -0.0571 0.5000 10.50000 0.05 0.19 Q8 1 0.7817 0.0344 0.8341 11.00000 0.05 0.18 Q9 1 0.7480 0.2520 0.9737 10.50000 0.05 0.18 Q10 1 0.8711 0.1289 0.7811 10.50000 0.05 0.18 Q11 1 0.7691 0.0413 0.8218 11.00000 0.05 0.17 Q12 1 0.7063 0.0921 0.0596 11.00000 0.05 0.17 Q13 1 0.6351 0.0818 0.1787 11.00000 0.05 0.16 Q14 1 0.9262 0.0738 0.7615 10.50000 0.05 0.16 Q15 1 0.7816 0.1824 0.8641 11.00000 0.05 0.16 Q16 1 0.7248 0.2584 1.0013 11.00000 0.05 0.16 Q17 1 0.3868 -0.1601 0.2593 11.00000 0.05 0.15 Q18 1 0.8417 0.1582 0.9986 10.50000 0.05 0.15 Q19 1 0.5985 -0.0645 0.3053 11.00000 0.05 0.15 Q20 1 0.7000 0.1366 0.0830 11.00000 0.05 0.15 Q21 1 0.8162 0.1838 0.9611 10.50000 0.05 0.15 Q22 1 0.8485 0.2430 0.8359 11.00000 0.05 0.15 Q23 1 0.6560 0.2400 0.8743 11.00000 0.05 0.14 Q24 1 0.7612 0.2241 0.8352 11.00000 0.05 0.14 Q25 1 0.7370 0.0626 0.1478 11.00000 0.05 0.14 Q26 1 0.5989 0.0287 0.2994 11.00000 0.05 0.14 Q27 1 0.4090 -0.1121 0.2692 11.00000 0.05 0.14 Q28 1 0.7547 0.0808 0.0840 11.00000 0.05 0.14 Q29 1 0.8581 0.1419 0.9801 10.50000 0.05 0.13 Q30 1 0.4123 -0.1171 0.2571 11.00000 0.05 0.13 Q31 1 0.6900 0.2200 0.8366 11.00000 0.05 0.13 Q32 1 0.6273 0.0757 0.2538 11.00000 0.05 0.13 Q33 1 0.5510 0.0143 0.4202 11.00000 0.05 0.13 Q34 1 0.6379 0.2373 0.9953 11.00000 0.05 0.13 Q35 1 0.6361 0.0590 0.2806 11.00000 0.05 0.13 Q36 1 0.9224 0.1344 0.8222 11.00000 0.05 0.13 Q37 1 0.7643 0.0348 0.9018 11.00000 0.05 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6 1.6425 2.1568 19 9 8 -0.4355 -14.6816 19 9 10 -20.1689 11.3402 19 9 12 -5.4911 -11.4266 19 10 1 -27.3729 -2.5513 19 10 3 -9.5704 14.0403 19 10 5 15.1259 3.1076 19 10 7 27.8226 15.8239 19 10 9 6.8250 -15.2054 19 10 11 14.9120 -6.6327 19 11 0 -14.5111 0.3628 19 11 2 3.8731 4.7217 19 11 4 -14.6057 -11.9110 19 11 6 -9.5474 8.7367 19 11 8 -16.8364 0.0090 19 11 10 -12.3294 8.1486 19 12 1 21.4089 1.2527 19 12 3 13.7986 24.0209 19 12 5 22.4447 -23.3381 19 12 7 -21.7413 -10.7070 19 12 9 6.7676 -13.3605 19 12 11 18.9895 -19.1945 19 13 0 -20.0936 -0.5850 19 13 2 -8.8178 5.1204 19 13 4 56.3846 -6.5989 19 13 6 5.6956 1.9880 19 13 8 -8.9468 2.2202 19 13 10 -4.2663 6.0723 19 14 1 25.5757 -4.4747 19 14 3 -10.4366 8.1535 19 14 5 -24.5618 -0.7068 19 14 7 2.3605 -1.2926 19 14 9 -23.6008 -8.1378 19 15 0 5.4291 0.6940 19 15 2 -5.9071 -29.8807 19 15 4 30.4008 -10.5352 19 15 6 -0.1613 3.3394 19 15 8 4.4124 -5.0755 19 16 1 -17.6941 3.4867 19 16 3 -3.8962 7.2588 19 16 5 3.1774 -7.9536 19 16 7 6.1507 -5.3389 19 17 0 15.1616 -0.3450 19 17 2 1.5188 2.7943 19 17 4 -8.9986 -16.3195 19 18 1 -13.8902 -17.7897 20 0 0 7.3576 0.7046 20 0 2 11.1404 0.3945 20 0 4 1.4115 -0.6225 20 0 6 -13.3130 0.4757 20 0 8 -3.5453 -0.9211 20 0 10 0.5394 -0.6343 20 0 12 -19.2385 0.1473 20 1 1 20.9681 20.5947 20 1 3 17.2718 -16.1353 20 1 5 -0.9876 4.5264 20 1 7 -0.7540 12.8458 20 1 9 -25.8919 17.2855 20 1 11 24.6682 11.6273 20 1 13 6.1312 -1.9749 20 2 0 -13.6883 -2.4049 20 2 2 4.6734 -1.9309 20 2 4 -5.9342 4.5337 20 2 6 6.7974 0.9830 20 2 8 8.7681 -6.4014 20 2 10 -7.9436 3.2596 20 2 12 1.7398 -12.2251 20 3 1 -26.9606 14.3553 20 3 3 -9.9708 -30.6559 20 3 5 6.4491 -0.1726 20 3 7 -7.5659 10.0956 20 3 9 0.3372 14.5768 20 3 11 14.3009 5.0899 20 3 13 -7.4410 -0.4750 20 4 0 -0.5504 3.1788 20 4 2 -10.3204 8.5389 20 4 4 20.3254 17.0424 20 4 6 -4.0840 25.1767 20 4 8 2.7923 -14.8717 20 4 10 7.8369 16.5766 20 4 12 -7.0830 0.9978 20 5 1 -3.3351 11.9941 20 5 3 -12.4196 -10.6044 20 5 5 16.3426 16.8900 20 5 7 7.5591 11.7387 20 5 9 10.2566 10.8171 20 5 11 25.1855 -25.8071 20 5 13 -0.1257 0.3547 20 6 0 0.9403 0.4378 20 6 2 9.0630 5.8086 20 6 4 -31.8599 1.5022 20 6 6 -10.6701 10.9010 20 6 8 6.1721 -14.0724 20 6 10 -0.6404 10.3418 20 6 12 -3.7869 5.1996 20 7 1 16.5977 4.3684 20 7 3 30.0627 -21.5616 20 7 5 -6.0374 -6.0177 20 7 7 -6.5324 -14.4341 20 7 9 1.5710 -8.7332 20 7 11 -8.4233 8.4473 20 8 0 3.2585 -2.9564 20 8 2 3.1272 -12.1553 20 8 4 2.6818 32.4214 20 8 6 4.2859 8.7874 20 8 8 12.1898 -8.2972 20 8 10 -1.3658 4.6664 20 8 12 -13.5045 -4.7287 20 9 1 -30.3572 -21.0374 20 9 3 -10.1559 -8.6043 20 9 5 9.8979 -7.1152 20 9 7 16.8101 5.3217 20 9 9 -5.3946 -12.9558 20 9 11 -7.2336 -1.2905 20 10 0 -18.7568 1.2493 20 10 2 12.3048 7.1919 20 10 4 -21.2980 1.6425 20 10 6 -8.8817 9.0966 20 10 8 -1.0733 -2.7582 20 10 10 -12.9689 6.8819 20 11 1 -7.9413 0.1012 20 11 3 11.3119 10.7046 20 11 5 31.8878 -15.4751 20 11 7 -7.1588 -5.5176 20 11 9 8.3425 -0.4773 20 12 0 -14.7253 0.3917 20 12 2 -16.2717 8.2848 20 12 4 19.6664 -15.0765 20 12 6 -1.3155 2.0318 20 12 8 -15.6950 6.2391 20 13 1 39.3602 -21.7900 20 13 3 7.9137 31.2011 20 13 5 -9.7227 -8.0661 20 13 7 -19.4209 -6.4281 20 13 9 -9.9829 -7.2291 20 14 0 7.6847 0.9654 20 14 2 -6.1529 -4.9084 20 14 4 31.4841 -19.7726 20 14 6 0.9307 9.8758 20 14 8 1.5737 2.6180 20 15 1 -6.3923 2.7972 20 15 3 2.1958 11.3549 20 15 5 -8.5068 1.2034 20 16 0 29.5210 -1.1317 20 16 2 -14.7153 2.9511 20 16 4 4.3389 -9.9251 20 17 1 -14.3774 -19.3972 21 0 1 21.9683 -0.0597 21 0 3 -4.4633 -1.0361 21 0 5 16.4186 0.3288 21 0 7 0.2331 -1.0452 21 0 9 -3.2868 0.7779 21 0 11 22.5544 0.3037 21 1 0 1.0469 0.6526 21 1 2 13.7155 12.6640 21 1 4 -12.0278 5.9631 21 1 6 1.7795 0.7337 21 1 8 -10.4905 6.3613 21 1 10 3.6251 5.7227 21 1 12 -3.4789 -4.3218 21 2 1 -13.2204 16.9048 21 2 3 10.7253 -11.5013 21 2 5 9.0358 -2.7859 21 2 7 -11.0900 -3.6559 21 2 9 -7.4116 9.0780 21 2 11 4.0843 6.3103 21 3 0 -7.0517 -2.6270 21 3 2 4.0237 -6.2332 21 3 4 -11.0969 20.8337 21 3 6 5.6236 21.2912 21 3 8 9.7427 10.9564 21 3 10 -0.3435 1.0997 21 3 12 0.1185 -15.4815 21 4 1 -18.5702 -1.9979 21 4 3 -23.3428 -2.1928 21 4 5 23.3982 5.0002 21 4 7 5.0848 10.8070 21 4 9 11.3552 10.2384 21 4 11 29.4265 -14.7837 21 5 0 9.9156 3.6411 21 5 2 -1.9407 -0.9938 21 5 4 8.0358 -10.2819 21 5 6 -3.2767 13.5179 21 5 8 -7.2752 -25.5210 21 5 10 -11.1448 20.6075 21 5 12 -13.5935 4.3049 21 6 1 11.2742 12.3155 21 6 3 7.6536 -10.3169 21 6 5 -11.1911 19.1591 21 6 7 -0.1280 -7.7570 21 6 9 8.9112 -0.8911 21 6 11 22.0729 -13.2017 21 7 0 -11.1872 -1.1246 21 7 2 16.7145 -11.9408 21 7 4 -8.4483 9.2398 21 7 6 23.2416 1.4021 21 7 8 -0.1734 -9.2229 21 7 10 -8.9981 3.6436 21 8 1 0.3402 0.5531 21 8 3 -3.4617 -16.4246 21 8 5 -3.5280 -8.6703 21 8 7 2.9148 -22.9865 21 8 9 -7.1133 -13.8759 21 8 11 -9.6967 5.3866 21 9 0 6.2698 -1.3593 21 9 2 -0.3852 -1.9709 21 9 4 5.2678 40.4280 21 9 6 -5.0740 13.1373 21 9 8 0.9248 -7.9335 21 9 10 4.8024 0.4352 21 10 1 -28.2109 -3.2089 21 10 3 3.4123 -20.5548 21 10 5 21.7772 -13.1142 21 10 7 6.7674 -3.0688 21 10 9 -4.7704 2.0930 21 11 0 -18.4507 0.9576 21 11 2 -1.5292 1.1735 21 11 4 -2.2663 3.3815 21 11 6 -3.3311 -3.4850 21 11 8 -8.0195 4.1146 21 12 1 18.1040 -9.4183 21 12 3 14.0971 5.7214 21 12 5 9.4326 -9.2013 21 12 7 -12.8635 -10.6388 21 13 0 21.2233 0.0593 21 13 2 -10.2615 -1.6128 21 13 4 14.2476 -25.1986 21 13 6 -0.8367 8.1300 21 14 1 4.0728 0.3946 21 14 3 15.1695 19.7398 21 14 5 -0.8486 4.5651 21 15 0 20.1974 -0.0632 21 15 2 -0.5964 5.6487 21 15 4 3.4622 -2.8130 22 0 0 5.8085 2.4719 22 0 2 7.8059 -0.1723 22 0 4 -9.0900 0.5275 22 0 6 6.5486 -2.2393 22 0 8 -23.7492 0.8987 22 0 10 12.3541 2.9733 22 1 1 -8.0781 2.3641 22 1 3 1.1505 -9.8585 22 1 5 9.9954 -7.4165 22 1 7 -7.3401 1.0762 22 1 9 10.2313 -4.0355 22 1 11 -3.1826 -6.1402 22 2 0 -18.1068 -0.2936 22 2 2 18.2062 17.2390 22 2 4 -45.6486 11.7768 22 2 6 11.3897 14.6207 22 2 8 5.9140 20.7032 22 2 10 -1.0621 1.8422 22 3 1 -12.6619 -10.1140 22 3 3 -1.6023 13.9252 22 3 5 14.4285 -13.2781 22 3 7 -3.5449 -6.4969 22 3 9 -3.7067 5.2215 22 3 11 -2.1511 4.9794 22 4 0 21.5686 -2.5652 22 4 2 -16.6279 -9.5928 22 4 4 1.5092 6.8556 22 4 6 -3.4250 14.9543 22 4 8 -7.6645 -3.7058 22 4 10 -3.0247 6.1428 22 5 1 -1.4646 -6.8680 22 5 3 -5.2659 7.1648 22 5 5 6.2841 12.7151 22 5 7 11.4196 13.2910 22 5 9 9.6293 8.5907 22 5 11 24.2079 -19.1939 22 6 0 -4.7169 2.2147 22 6 2 14.7696 -0.9506 22 6 4 -1.1906 -19.6316 22 6 6 20.6191 -12.5982 22 6 8 -20.6842 -10.3486 22 6 10 -18.0482 6.8408 22 7 1 12.0720 7.0691 22 7 3 -8.6247 3.6327 22 7 5 -7.0754 9.9539 22 7 7 -0.5757 -23.5846 22 7 9 6.8189 -7.4385 22 8 0 13.4707 -0.5635 22 8 2 -6.5247 -5.7778 22 8 4 13.5835 21.7239 22 8 6 12.0140 -4.7959 22 8 8 -13.4371 -1.4818 22 9 1 -8.9673 -7.8931 22 9 3 -8.3158 -13.9704 22 9 5 13.6062 -17.1598 22 9 7 4.5441 -3.1690 22 9 9 -4.0582 -2.6739 22 10 0 -6.0701 0.1622 22 10 2 0.1579 5.3956 22 10 4 5.8983 30.3210 22 10 6 -6.6651 0.1990 22 10 8 -6.2608 -3.5673 22 11 1 -2.4461 -0.7251 22 11 3 7.7651 -21.2187 22 11 5 7.0861 -10.4338 22 11 7 -0.0810 -5.8972 22 12 0 19.1740 -0.2815 22 12 2 -7.7510 -13.0257 22 12 4 4.5743 -11.9701 22 12 6 2.1360 -0.4174 22 13 1 0.7118 -1.1152 22 13 3 17.9581 8.9807 22 13 5 13.3864 1.4307 22 14 0 12.3249 -0.7710 22 14 2 6.0637 0.9532 23 0 1 -11.3112 0.0368 23 0 3 -0.1148 0.2575 23 0 5 -3.2402 -0.7321 23 0 7 6.7634 -0.3886 23 0 9 11.4946 0.7548 23 1 0 -3.6291 0.8167 23 1 2 1.1832 15.3311 23 1 4 -16.4405 0.4698 23 1 6 1.1974 -2.9694 23 1 8 -5.2288 1.7970 23 1 10 3.1153 6.4282 23 2 1 -9.3273 -6.6642 23 2 3 -7.2451 -3.7030 23 2 5 2.1540 -11.7377 23 2 7 -4.5874 -0.6878 23 2 9 -4.3204 -2.3104 23 3 0 -11.5740 -0.4946 23 3 2 -6.1756 9.6606 23 3 4 -22.6026 6.6912 23 3 6 1.2581 20.7776 23 3 8 5.1810 4.4247 23 3 10 -3.8349 3.8551 23 4 1 8.8840 -4.5023 23 4 3 -8.4415 11.2575 23 4 5 6.4631 -8.6442 23 4 7 7.1504 9.8827 23 4 9 -3.4749 8.2307 23 5 0 12.8994 -2.0438 23 5 2 -12.5918 1.4226 23 5 4 11.5082 5.5169 23 5 6 1.2080 -13.7631 23 5 8 -16.8611 -4.4774 23 6 1 4.9150 14.9076 23 6 3 -2.8483 6.4296 23 6 5 7.3981 16.3205 23 6 7 1.0524 2.5139 23 6 9 8.9514 5.9472 23 7 0 -8.5835 1.4746 23 7 2 10.9943 2.9265 23 7 4 -0.6336 -8.1474 23 7 6 13.7199 -18.4750 23 7 8 -18.9962 9.1517 23 8 1 8.5291 2.0059 23 8 3 -17.8238 6.6850 23 8 5 8.3711 -5.1836 23 8 7 -1.2602 -2.5818 23 9 0 4.0617 0.3837 23 9 2 -8.3084 14.3401 23 9 4 15.3454 20.6522 23 9 6 -3.8916 -11.7262 23 10 1 -1.3474 -9.9158 23 10 3 -5.1884 -10.0425 23 10 5 6.6366 -9.5686 23 11 0 0.2076 -0.1386 23 11 2 3.3163 -6.3649 23 11 4 -2.6566 4.7392 23 12 1 -2.6329 2.5755 23 12 3 8.1343 -4.1739 24 0 0 34.5444 -1.8204 24 0 2 -20.9005 0.0632 24 0 4 25.0028 -0.8921 24 0 6 -15.9854 2.4226 24 0 8 -6.4512 -1.3000 24 1 1 -8.1509 8.2030 24 1 3 -5.5854 -8.0678 24 1 5 -8.3170 3.5631 24 1 7 9.1176 5.7123 24 2 0 -20.0121 0.8004 24 2 2 -4.9520 12.6663 24 2 4 -12.1849 -8.4215 24 2 6 -3.2456 1.0291 24 2 8 5.0513 -8.2494 24 3 1 9.6532 -10.9785 24 3 3 -21.8932 3.0982 24 3 5 1.2305 -10.3337 24 3 7 0.9013 -0.3354 24 4 0 1.5992 1.0667 24 4 2 -21.4652 10.3421 24 4 4 21.3407 14.6428 24 4 6 -7.4710 4.6732 24 4 8 -1.5383 -4.0928 24 5 1 9.8297 24.0203 24 5 3 -1.8841 1.2390 24 5 5 4.3630 3.3901 24 5 7 -0.0729 9.2230 24 6 0 -16.9376 -2.0375 24 6 2 8.2657 5.6017 24 6 4 -3.0216 3.5527 24 6 6 4.6982 -12.8641 24 7 1 6.6185 20.9377 24 7 3 0.3542 3.3723 24 7 5 4.6850 2.4077 24 8 0 -3.8593 1.2967 24 8 2 -0.2927 15.3631 24 8 4 9.0287 1.9774 24 9 1 4.1267 -4.1347 24 9 3 -13.2646 5.0387 24 10 0 -7.6591 0.0250 24 10 2 4.0835 5.2106 25 0 1 -13.5294 -0.3165 25 0 3 1.9191 0.2480 25 0 5 -7.9348 1.2668 25 1 0 26.2782 -1.9482 25 1 2 -11.4549 -2.9068 25 1 4 19.0159 -0.8053 25 1 6 -10.1698 -10.0605 25 2 1 2.1732 -0.4083 25 2 3 -13.0091 1.0613 25 2 5 -0.6312 3.9975 25 3 0 -12.3715 3.2471 25 3 2 -11.5613 13.8612 25 3 4 5.6857 -9.4980 25 3 6 -4.7039 3.5095 25 4 1 2.8509 -2.3715 25 4 3 -15.0221 9.1326 25 4 5 4.3681 -5.8200 25 5 0 -3.7305 -0.1014 25 5 2 -3.3552 2.9821 25 5 4 19.1273 13.6588 25 6 1 7.5998 24.0446 25 6 3 12.1347 -2.4335 25 7 0 -11.2993 -1.5931 25 7 2 5.1638 11.7036 25 8 1 2.0074 3.3529 26 0 0 35.2082 -3.8229 26 0 2 0.5341 -0.2254 26 1 1 -11.0125 8.9395 26 1 3 2.0274 -5.7696 26 2 0 1.2409 1.9646 26 2 2 -2.9094 2.2339 26 3 1 -5.4205 -9.9839 0 0 0 0.0 0.0 ; _shelx_fab_checksum 46783 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' 'y, -x, -z' '-x, -y, z' '-y, x, -z' 'x, -y, -z' '-y, -x, z' '-x, y, -z' 'y, x, z' 'x+1/2, y+1/2, z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'y+1/2, x+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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zr1 Zr 0.73248(4) 0.18668(4) 0.83256(5) 0.0325(4) Uani 1 1 d . U . . . Zr2 Zr 0.83680(4) 0.16320(4) 0.78663(7) 0.0344(6) Uani 1 2 d S TU P . . Zr3 Zr 0.77529(4) 0.22471(4) 0.95456(7) 0.0330(6) Uani 1 2 d S TU P . . Zr4 Zr 0.79945(4) 0.12037(4) 0.91028(5) 0.0324(4) Uani 1 1 d . U . . . O1 O 0.3724(2) -0.1947(2) 0.3450(3) 0.039(2) Uani 1 1 d . U . . . O2 O 0.4130(2) -0.2343(3) 0.4018(3) 0.039(2) Uani 1 1 d . U . . . O3 O 0.7713(2) 0.1119(3) -0.0071(3) 0.039(2) Uani 1 1 d . U . . . O4 O 0.7547(3) 0.1796(3) 0.0171(3) 0.044(2) Uani 1 1 d . U . . . O5 O 0.7911(3) 0.1480(3) 0.7191(3) 0.052(2) Uani 1 1 d . U . . . O6 O 0.7236(3) 0.1593(3) 0.7510(3) 0.042(2) Uani 1 1 d . U . . . O7 O 0.8492(2) 0.1508(2) 0.8682(4) 0.034(2) Uani 1 2 d S TU P . . O8 O 0.8722(2) 0.2189(2) 0.8239(3) 0.0284(18) Uani 1 1 d . U . . . O9 O 0.7590(2) 0.1731(2) 0.9054(3) 0.0311(16) Uani 1 1 d . U . . . O10 O 0.7903(2) 0.2097(2) 0.8037(4) 0.0297(19) Uani 1 2 d S TU P . . O11 O 0.6749(3) 0.2056(3) 0.8804(4) 0.059(2) Uani 1 1 d . U . . . O12 O 0.8124(3) 0.0552(3) 0.8772(4) 0.067(3) Uani 1 1 d . U . . . H12A H 0.799456 0.051886 0.846685 0.100 Uiso 1 1 d R U . . . H12B H 0.800885 0.035728 0.897421 0.100 Uiso 1 1 d R U . . . O13 O 0.8538(3) 0.0902(3) 0.9553(3) 0.057(2) Uani 1 1 d . U . . . O14 O 0.9034(3) 0.1463(3) 0.7664(4) 0.073(3) Uani 1 1 d . U . . . O15 O 0.8274(2) 0.1726(2) 0.9634(4) 0.034(2) Uani 1 2 d S TU P . . O16 O 0.7500(2) 0.2500(2) 0.8730(4) 0.035(2) Uani 1 2 d S TU P . . O17 O 0.6987(3) 0.2371(3) 0.7848(3) 0.065(2) Uani 1 1 d . U . . . N1 N 0.6322(3) 0.0307(3) 0.3719(4) 0.035(2) Uani 1 1 d . U . . . C1 C 0.4347(4) -0.1637(4) 0.3758(5) 0.031(3) Uani 1 1 d . U . . . C2 C 0.4351(4) -0.1323(4) 0.3372(5) 0.035(3) Uani 1 1 d . U . . . H2 H 0.415026 -0.133371 0.309486 0.042 Uiso 1 1 calc R U . . . C3 C 0.4651(3) -0.0987(4) 0.3388(5) 0.033(3) Uani 1 1 d . U . . . H3 H 0.464290 -0.077844 0.312059 0.039 Uiso 1 1 calc R U . . . C4 C 0.4961(4) -0.0952(4) 0.3787(5) 0.033(3) Uani 1 1 d . U . . . C5 C 0.4971(4) -0.1275(4) 0.4183(5) 0.041(3) Uani 1 1 d . U . . . H5 H 0.517758 -0.126377 0.445315 0.049 Uiso 1 1 calc R U . . . C6 C 0.4678(3) -0.1606(4) 0.4173(5) 0.033(3) Uani 1 1 d . U . . . H6 H 0.468987 -0.181690 0.443846 0.039 Uiso 1 1 calc R U . . . C7 C 0.5314(4) -0.0631(4) 0.3794(5) 0.041(3) Uani 1 1 d . U . . . C8 C 0.5439(4) -0.0434(4) 0.3298(5) 0.042(3) Uani 1 1 d . U . . . H8 H 0.530153 -0.051586 0.298243 0.050 Uiso 1 1 calc R U . . . C9 C 0.5757(4) -0.0126(4) 0.3280(5) 0.037(3) Uani 1 1 d . U . . . H9 H 0.582700 0.000105 0.295334 0.044 Uiso 1 1 calc R U . . . C10 C 0.5971(4) -0.0005(4) 0.3727(5) 0.033(3) Uani 1 1 d . U . . . C11 C 0.5860(4) -0.0190(4) 0.4204(5) 0.032(3) Uani 1 1 d . U . . . H11 H 0.600176 -0.011354 0.451823 0.039 Uiso 1 1 calc R U . . . C12 C 0.5536(4) -0.0490(4) 0.4210(5) 0.043(3) Uani 1 1 d . U . . . H12 H 0.546463 -0.060568 0.454254 0.051 Uiso 1 1 calc R U . . . C13 C 0.7383(3) 0.1206(3) 0.0758(3) 0.055(3) Uani 1 1 d G U . . . C14 C 0.7311(3) 0.1493(2) 0.1177(4) 0.067(4) Uani 1 1 d G U . . . H14 H 0.736964 0.178514 0.113273 0.080 Uiso 1 1 calc R U . . . C15 C 0.7152(3) 0.1342(3) 0.1664(3) 0.071(4) Uani 1 1 d G U . . . H15 H 0.710341 0.153414 0.194421 0.086 Uiso 1 1 calc R U . . . C16 C 0.7064(3) 0.0906(3) 0.1730(3) 0.058(4) Uani 1 1 d G U . . . C17 C 0.7136(3) 0.0619(2) 0.1311(4) 0.082(5) Uani 1 1 d G U . . . H17 H 0.707732 0.032698 0.135529 0.098 Uiso 1 1 calc R U . . . C18 C 0.7295(3) 0.0770(3) 0.0824(3) 0.076(4) Uani 1 1 d G U . . . H18 H 0.734354 0.057798 0.054382 0.091 Uiso 1 1 calc R U . . . O18 O 0.7028(3) 0.2329(3) 0.9647(3) 0.064(2) Uani 1 1 d . U . . . C19 C 0.6879(4) 0.0745(4) 0.2259(5) 0.043(3) Uani 1 1 d . U . . . C20 C 0.6797(4) 0.1018(4) 0.2694(5) 0.058(4) Uani 1 1 d . U . . . H20 H 0.687409 0.130723 0.266757 0.070 Uiso 1 1 calc R U . . . C21 C 0.6611(4) 0.0879(4) 0.3144(5) 0.043(3) Uani 1 1 d . U . . . H21 H 0.654463 0.107787 0.341001 0.051 Uiso 1 1 calc R U . . . C22 C 0.6513(4) 0.0447(4) 0.3229(5) 0.033(3) Uani 1 1 d . U . . . C23 C 0.6623(4) 0.0159(4) 0.2838(5) 0.040(3) Uani 1 1 d . U . . . H23 H 0.657774 -0.013475 0.289285 0.048 Uiso 1 1 calc R U . . . C24 C 0.6802(4) 0.0300(4) 0.2359(5) 0.046(3) Uani 1 1 d . U . . . H24 H 0.687393 0.009808 0.209722 0.055 Uiso 1 1 calc R U . . . C25 C 0.7320(3) 0.1314(3) 0.6622(3) 0.050(3) Uani 1 1 d G U . . . C26 C 0.6891(3) 0.1185(3) 0.6602(3) 0.060(4) Uani 1 1 d G U . . . H26 H 0.671897 0.120247 0.690720 0.072 Uiso 1 1 calc R U . . . C27 C 0.6718(2) 0.1028(3) 0.6126(3) 0.062(4) Uani 1 1 d G U . . . H27 H 0.643054 0.094147 0.611246 0.075 Uiso 1 1 calc R U . . . C28 C 0.6974(3) 0.1001(3) 0.5670(3) 0.047(3) Uani 1 1 d G U . . . C29 C 0.7404(3) 0.1131(3) 0.5690(3) 0.064(4) Uani 1 1 d G U . . . H29 H 0.757523 0.111291 0.538508 0.077 Uiso 1 1 calc R U . . . C30 C 0.7576(2) 0.1287(3) 0.6166(3) 0.065(4) Uani 1 1 d G U . . . H30 H 0.786366 0.137392 0.617981 0.079 Uiso 1 1 calc R U . . . C31 C 0.6795(3) 0.0841(3) 0.5149(3) 0.042(3) Uani 1 1 d G U . . . C32 C 0.7053(2) 0.0574(3) 0.4836(3) 0.053(4) Uani 1 1 d G U . . . H32 H 0.733274 0.050982 0.494395 0.063 Uiso 1 1 calc R U . . . C33 C 0.6892(2) 0.0404(2) 0.4360(3) 0.048(3) Uani 1 1 d G U . . . H33 H 0.706484 0.022523 0.415062 0.058 Uiso 1 1 calc R U . . . C34 C 0.6474(3) 0.0500(2) 0.4198(2) 0.032(3) Uani 1 1 d G U . . . C35 C 0.6216(2) 0.0767(3) 0.4511(3) 0.044(3) Uani 1 1 d G U . . . H35 H 0.593617 0.083159 0.440290 0.053 Uiso 1 1 calc R U . . . C36 C 0.6377(2) 0.0938(2) 0.4987(3) 0.046(3) Uani 1 1 d G U . . . H36 H 0.620406 0.111618 0.519623 0.055 Uiso 1 1 calc R U . . . C37 C 0.4038(4) -0.1999(4) 0.3740(5) 0.031(3) Uani 1 1 d . U . . . C38 C 0.7547(4) 0.1395(5) 0.0227(6) 0.047(4) Uani 1 1 d . U . . . C39 C 0.7507(5) 0.1503(4) 0.7137(6) 0.051(3) Uani 1 1 d . U . . . C40 C 0.8912(5) 0.1088(5) 0.9695(8) 0.075(6) Uani 1 2 d S TU P . . H40 H 0.907369 0.092632 0.993692 0.090 Uiso 1 2 calc R U P . . C41 C 0.8959(6) 0.1041(6) 0.7566(9) 0.083(6) Uani 1 2 d S TU P . . H41 H 0.913306 0.086690 0.744522 0.099 Uiso 1 2 d R U P . . C42 C 0.6701(5) 0.2197(5) 0.9301(6) 0.075(4) Uani 1 1 d . U . . . H42 H 0.642063 0.220977 0.943285 0.090 Uiso 1 1 calc R U . . . C43 C 0.7226(6) 0.2774(6) 0.7683(10) 0.106(7) Uani 1 2 d S TU P . . H43 H 0.707538 0.292470 0.741923 0.127 Uiso 1 2 d R U P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Zr1 0.0391(9) 0.0398(9) 0.0187(8) 0.0020(7) -0.0020(7) -0.0205(7) Zr2 0.0422(8) 0.0422(8) 0.0188(11) -0.0043(7) 0.0043(7) -0.0212(11) Zr3 0.0412(8) 0.0412(8) 0.0166(11) -0.0036(7) 0.0036(7) -0.0177(10) Zr4 0.0439(10) 0.0345(9) 0.0188(8) 0.0043(7) -0.0017(7) -0.0172(7) O1 0.038(5) 0.025(5) 0.055(6) 0.003(4) -0.021(4) -0.015(4) O2 0.042(5) 0.040(5) 0.035(5) -0.002(4) -0.019(4) -0.014(4) O3 0.040(5) 0.051(5) 0.025(5) 0.002(4) 0.002(4) -0.014(4) O4 0.053(6) 0.054(5) 0.024(5) -0.004(4) 0.010(4) -0.014(4) O5 0.069(4) 0.070(6) 0.017(4) -0.008(4) 0.001(4) -0.027(5) O6 0.053(5) 0.048(5) 0.026(4) 0.004(3) -0.014(3) -0.027(4) O7 0.036(3) 0.036(3) 0.031(4) 0.004(2) -0.004(2) -0.011(4) O8 0.032(4) 0.040(4) 0.013(4) 0.008(3) 0.002(3) -0.010(3) O9 0.035(3) 0.037(3) 0.021(3) 0.004(3) 0.000(3) -0.025(3) O10 0.039(3) 0.039(3) 0.012(4) 0.005(2) -0.005(2) -0.016(3) O11 0.041(4) 0.061(6) 0.075(5) -0.008(4) 0.012(4) -0.016(4) O12 0.096(7) 0.040(4) 0.064(6) -0.014(4) -0.006(6) -0.018(4) O13 0.071(5) 0.049(5) 0.052(5) 0.013(4) -0.017(4) -0.003(4) O14 0.066(5) 0.086(6) 0.067(6) -0.020(5) 0.022(4) 0.008(5) O15 0.037(3) 0.037(3) 0.027(4) 0.003(2) -0.003(2) -0.021(4) O16 0.038(3) 0.038(3) 0.030(5) 0.001(2) -0.001(2) -0.010(4) O17 0.073(5) 0.075(5) 0.046(4) -0.006(4) -0.024(4) 0.011(4) N1 0.043(5) 0.036(5) 0.027(4) 0.003(3) -0.001(3) -0.013(4) C1 0.023(6) 0.031(5) 0.040(6) -0.006(4) -0.006(4) -0.004(4) C2 0.030(6) 0.031(6) 0.042(6) -0.003(5) -0.002(5) 0.001(4) C3 0.034(6) 0.028(6) 0.037(6) -0.005(5) 0.004(4) 0.001(4) C4 0.034(6) 0.035(6) 0.031(6) -0.004(4) 0.009(4) -0.007(4) C5 0.034(6) 0.045(6) 0.043(6) 0.006(5) -0.007(5) -0.022(5) C6 0.027(6) 0.034(6) 0.038(6) -0.003(5) -0.005(4) -0.013(4) C7 0.049(6) 0.045(6) 0.028(5) 0.008(5) -0.004(4) -0.019(5) C8 0.047(7) 0.054(7) 0.023(5) 0.006(5) -0.007(5) -0.021(5) C9 0.047(6) 0.048(7) 0.016(5) -0.004(5) 0.003(4) -0.019(5) C10 0.044(6) 0.039(6) 0.016(5) -0.001(4) 0.003(4) -0.015(5) C11 0.038(6) 0.041(7) 0.018(5) 0.001(5) 0.004(4) -0.011(5) C12 0.052(7) 0.052(7) 0.024(5) 0.012(5) -0.005(5) -0.024(5) C13 0.061(8) 0.059(5) 0.044(5) 0.011(4) 0.024(5) 0.004(6) C14 0.093(9) 0.059(6) 0.048(6) 0.011(4) 0.038(6) -0.001(7) C15 0.108(10) 0.055(5) 0.051(6) 0.008(5) 0.042(6) -0.012(6) C16 0.076(9) 0.055(5) 0.045(5) 0.008(4) 0.016(6) -0.014(6) C17 0.130(11) 0.059(6) 0.057(6) 0.002(4) 0.041(7) -0.021(7) C18 0.108(10) 0.061(5) 0.058(6) 0.008(5) 0.039(7) -0.008(6) O18 0.057(5) 0.077(6) 0.057(5) 0.003(5) 0.020(4) -0.004(4) C19 0.045(8) 0.044(5) 0.041(5) 0.006(4) 0.005(5) -0.014(5) C20 0.085(9) 0.043(6) 0.048(5) 0.003(4) 0.020(6) -0.024(6) C21 0.053(8) 0.034(5) 0.042(5) 0.004(4) 0.007(5) -0.014(5) C22 0.036(7) 0.033(5) 0.031(4) 0.004(4) 0.002(4) -0.010(5) C23 0.048(8) 0.037(5) 0.034(5) 0.002(4) 0.004(5) -0.008(5) C24 0.055(8) 0.045(5) 0.036(5) -0.002(4) 0.007(5) -0.020(6) C25 0.061(5) 0.058(8) 0.032(4) -0.003(5) -0.004(4) -0.022(6) C26 0.063(5) 0.078(9) 0.039(5) -0.016(6) -0.001(4) -0.028(6) C27 0.056(6) 0.090(9) 0.041(5) -0.018(6) -0.003(4) -0.025(6) C28 0.055(5) 0.050(8) 0.038(5) -0.006(5) -0.005(4) -0.011(5) C29 0.059(5) 0.095(9) 0.039(5) -0.016(6) -0.001(4) -0.024(6) C30 0.065(6) 0.093(9) 0.038(5) -0.015(6) 0.001(4) -0.035(7) C31 0.055(5) 0.038(7) 0.034(5) 0.002(5) -0.006(4) -0.007(5) C32 0.054(6) 0.062(8) 0.042(6) -0.011(5) -0.015(4) 0.005(5) C33 0.052(5) 0.054(8) 0.038(6) -0.005(5) -0.010(4) 0.000(5) C34 0.045(5) 0.021(6) 0.028(4) 0.007(4) -0.004(4) -0.015(4) C35 0.050(6) 0.041(7) 0.040(5) -0.007(5) -0.005(4) -0.009(5) C36 0.055(5) 0.040(7) 0.044(6) -0.010(5) -0.009(4) -0.004(5) C37 0.028(5) 0.036(5) 0.029(6) -0.005(4) -0.005(4) -0.009(4) C38 0.049(8) 0.054(5) 0.037(5) 0.000(4) 0.012(5) -0.014(5) C39 0.068(5) 0.053(8) 0.033(5) -0.002(5) -0.004(3) -0.028(5) C40 0.078(7) 0.078(7) 0.070(12) 0.020(7) -0.020(7) -0.018(7) C41 0.084(6) 0.084(6) 0.080(13) -0.014(6) 0.014(6) 0.007(7) C42 0.067(7) 0.084(10) 0.075(6) -0.011(6) 0.010(5) 0.000(7) C43 0.098(8) 0.098(8) 0.123(14) 0.024(8) -0.024(8) -0.005(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Zr Zr -2.9673 0.5597 '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 _geom_angle_publ_flag O1 Zr1 O6 75.3(3) 14 . y O1 Zr1 O8 73.2(3) 14 6_665 y O1 Zr1 O11 73.5(3) 14 . y O1 Zr1 O16 141.7(3) 14 . y O1 Zr1 O17 114.2(3) 14 . y O6 Zr1 O8 72.7(3) . 6_665 y O6 Zr1 O11 119.6(3) . . y O6 Zr1 O16 140.0(3) . . y O6 Zr1 O17 73.7(3) . . y O9 Zr1 O1 85.2(3) . 14 y O9 Zr1 O6 142.0(3) . . y O9 Zr1 O8 70.6(3) . 6_665 y O9 Zr1 O10 91.9(3) . . y O9 Zr1 O11 84.2(3) . . y O9 Zr1 O16 71.7(3) . . y O9 Zr1 O17 144.2(3) . . y O10 Zr1 O1 143.3(3) . 14 y O10 Zr1 O6 85.3(3) . . y O10 Zr1 O8 71.4(3) . 6_665 y O10 Zr1 O11 142.6(3) . . y O10 Zr1 O16 69.4(3) . . y O10 Zr1 O17 88.8(4) . . y O11 Zr1 O8 139.4(3) . 6_665 y O11 Zr1 O16 74.1(3) . . y O11 Zr1 O17 74.0(3) . . y O16 Zr1 O8 123.5(3) . 6_665 y O17 Zr1 O8 142.0(3) . 6_665 y O17 Zr1 O16 75.2(3) . . y O5 Zr2 O5 72.7(4) . 6_665 y O7 Zr2 O5 143.1(2) . 6_665 y O7 Zr2 O5 143.1(2) . . y O7 Zr2 O8 69.6(2) . . y O7 Zr2 O8 69.6(2) . 6_665 y O7 Zr2 O14 90.4(4) . . y O7 Zr2 O14 90.4(4) . 6_665 y O8 Zr2 O5 74.0(3) . 6_665 y O8 Zr2 O5 141.0(3) . . y O8 Zr2 O5 141.0(3) 6_665 6_665 y O8 Zr2 O5 74.0(3) 6_665 . y O8 Zr2 O8 125.4(4) 6_665 . y O10 Zr2 O5 82.1(3) . . y O10 Zr2 O5 82.1(3) . 6_665 y O10 Zr2 O7 93.1(4) . . y O10 Zr2 O8 73.8(2) . 6_665 y O10 Zr2 O8 73.8(2) . . y O10 Zr2 O14 149.9(3) . . y O10 Zr2 O14 150.0(3) . 6_665 y O14 Zr2 O5 77.3(4) . 6_665 y O14 Zr2 O5 77.3(4) 6_665 . y O14 Zr2 O5 111.8(4) 6_665 6_665 y O14 Zr2 O5 111.8(4) . . y O14 Zr2 O8 79.6(3) . . y O14 Zr2 O8 134.7(3) . 6_665 y O14 Zr2 O8 79.6(3) 6_665 6_665 y O14 Zr2 O8 134.7(3) 6_665 . y O14 Zr2 O14 59.7(5) . 6_665 y O4 Zr3 O4 82.2(4) 6_666 1_556 y O4 Zr3 O15 71.8(3) 6_666 . y O4 Zr3 O15 71.8(3) 1_556 . y O4 Zr3 O16 138.0(2) 6_666 . y O4 Zr3 O16 138.0(2) 1_556 . y O4 Zr3 O18 72.8(3) 6_666 6_665 y O4 Zr3 O18 72.8(3) 1_556 . y O4 Zr3 O18 121.2(3) 6_666 . y O4 Zr3 O18 121.2(3) 1_556 6_665 y O9 Zr3 O4 81.9(3) 6_665 6_666 y O9 Zr3 O4 143.1(3) 6_665 1_556 y O9 Zr3 O4 81.9(3) . 1_556 y O9 Zr3 O4 143.1(3) . 6_666 y O9 Zr3 O9 91.5(4) . 6_665 y O9 Zr3 O15 71.7(3) . . y O9 Zr3 O15 71.7(3) 6_665 . y O9 Zr3 O16 70.0(3) 6_665 . y O9 Zr3 O16 70.0(3) . . y O9 Zr3 O18 143.0(3) . 6_665 y O9 Zr3 O18 84.9(3) 6_665 6_665 y O9 Zr3 O18 143.0(3) 6_665 . y O9 Zr3 O18 84.9(3) . . y O15 Zr3 O16 124.0(4) . . y O18 Zr3 O15 139.7(2) . . y O18 Zr3 O15 139.7(2) 6_665 . y O18 Zr3 O16 74.2(3) . . y O18 Zr3 O16 74.2(3) 6_665 . y O18 Zr3 O18 76.5(5) . 6_665 y O3 Zr4 O2 71.9(3) 1_556 14 y O3 Zr4 O15 72.3(3) 1_556 . y O7 Zr4 O2 144.3(3) . 14 y O7 Zr4 O3 142.9(3) . 1_556 y O7 Zr4 O8 70.0(3) . 6_665 y O7 Zr4 O12 95.2(3) . . y O7 Zr4 O13 83.5(4) . . y O7 Zr4 O15 71.9(3) . . y O8 Zr4 O2 74.5(3) 6_665 14 y O8 Zr4 O3 142.5(3) 6_665 1_556 y O8 Zr4 O15 125.9(3) 6_665 . y O9 Zr4 O2 79.4(3) . 14 y O9 Zr4 O3 84.9(3) . 1_556 y O9 Zr4 O7 93.5(3) . . y O9 Zr4 O8 72.9(3) . 6_665 y O9 Zr4 O12 144.0(3) . . y O9 Zr4 O13 145.2(3) . . y O9 Zr4 O15 72.7(3) . . y O12 Zr4 O2 73.3(3) . 14 y O12 Zr4 O3 107.8(3) . 1_556 y O12 Zr4 O8 77.4(3) . 6_665 y O12 Zr4 O13 70.7(3) . . y O12 Zr4 O15 143.0(4) . . y O13 Zr4 O2 121.7(3) . 14 y O13 Zr4 O3 77.4(3) . 1_556 y O13 Zr4 O8 136.0(3) . 6_665 y O13 Zr4 O15 73.5(3) . . y O15 Zr4 O2 135.9(3) . 14 y C37 O1 Zr1 132.6(8) . 14_554 ? C37 O2 Zr4 132.4(7) . 14_554 ? C38 O3 Zr4 128.8(9) . 1_554 ? C38 O4 Zr3 135.6(9) . 1_554 ? C39 O5 Zr2 133.8(9) . . ? C39 O6 Zr1 131.8(9) . . ? Zr4 O7 Zr2 115.7(3) 6_665 . ? Zr4 O7 Zr2 115.7(3) . . ? Zr4 O7 Zr4 114.4(5) . 6_665 ? Zr2 O8 Zr1 98.7(3) . 6_665 ? Zr4 O8 Zr1 98.8(3) 6_665 6_665 ? Zr4 O8 Zr2 104.7(3) 6_665 . ? Zr1 O9 Zr3 117.8(3) . . ? Zr1 O9 Zr4 117.5(3) . . ? Zr4 O9 Zr3 115.2(3) . . ? Zr1 O10 Zr1 118.7(5) 6_665 . ? Zr1 O10 Zr2 115.8(3) . . ? Zr1 O10 Zr2 115.8(3) 6_665 . ? C42 O11 Zr1 132.9(9) . . ? Zr4 O12 H12A 110.6 . . ? Zr4 O12 H12B 110.1 . . ? H12A O12 H12B 103.7 . . ? C40 O13 Zr4 127.2(11) . . ? C41 O14 Zr2 96.4(11) . . ? Zr4 O15 Zr3 100.2(3) . . ? Zr4 O15 Zr3 100.2(3) 6_665 . ? Zr4 O15 Zr4 101.8(4) . 6_665 ? Zr1 O16 Zr1 102.5(4) . 6_665 ? Zr1 O16 Zr3 100.4(3) . . ? Zr1 O16 Zr3 100.3(3) 6_665 . ? C43 O17 Zr1 119.8(11) . . ? C22 N1 C10 121.6(10) . . ? C34 N1 C10 121.1(9) . . ? C34 N1 C22 117.2(8) . . ? C2 C1 C6 116.5(10) . . ? C2 C1 C37 121.7(11) . . ? C6 C1 C37 121.8(12) . . ? C1 C2 H2 119.5 . . ? C1 C2 C3 121.0(12) . . ? C3 C2 H2 119.5 . . ? C2 C3 H3 118.6 . . ? C4 C3 C2 122.7(12) . . ? C4 C3 H3 118.6 . . ? C3 C4 C5 117.6(11) . . ? C3 C4 C7 124.9(11) . . ? C5 C4 C7 117.1(11) . . ? C4 C5 H5 119.8 . . ? C6 C5 C4 120.4(12) . . ? C6 C5 H5 119.8 . . ? C1 C6 H6 119.1 . . ? C5 C6 C1 121.8(12) . . ? C5 C6 H6 119.1 . . ? C8 C7 C4 118.5(11) . . ? C12 C7 C4 128.1(12) . . ? C12 C7 C8 113.3(11) . . ? C7 C8 H8 119.4 . . ? C9 C8 C7 121.3(11) . . ? C9 C8 H8 119.4 . . ? C8 C9 H9 119.4 . . ? C10 C9 C8 121.2(12) . . ? C10 C9 H9 119.4 . . ? C9 C10 N1 122.7(11) . . ? C9 C10 C11 118.6(11) . . ? C11 C10 N1 118.7(11) . . ? C10 C11 H11 120.6 . . ? C10 C11 C12 118.8(12) . . ? C12 C11 H11 120.6 . . ? C7 C12 C11 126.7(12) . . ? C7 C12 H12 116.6 . . ? C11 C12 H12 116.6 . . ? C14 C13 C18 120.0 . . ? C14 C13 C38 117.4(8) . . ? C18 C13 C38 122.6(8) . . ? C13 C14 H14 120.0 . . ? C15 C14 C13 120.0 . . ? C15 C14 H14 120.0 . . ? C14 C15 H15 120.0 . . ? C14 C15 C16 120.0 . . ? C16 C15 H15 120.0 . . ? C15 C16 C17 120.0 . . ? C15 C16 C19 119.7(8) . . ? C17 C16 C19 120.2(8) . . ? C16 C17 H17 120.0 . . ? C16 C17 C18 120.0 . . ? C18 C17 H17 120.0 . . ? C13 C18 H18 120.0 . . ? C17 C18 C13 120.0 . . ? C17 C18 H18 120.0 . . ? C42 O18 Zr3 128.1(9) . . ? C20 C19 C16 122.8(11) . . ? C20 C19 C24 114.9(12) . . ? C24 C19 C16 122.2(11) . . ? C19 C20 H20 118.8 . . ? C21 C20 C19 122.3(13) . . ? C21 C20 H20 118.8 . . ? C20 C21 H21 118.8 . . ? C20 C21 C22 122.4(13) . . ? C22 C21 H21 118.8 . . ? C21 C22 N1 121.0(11) . . ? C23 C22 N1 121.2(11) . . ? C23 C22 C21 117.8(12) . . ? C22 C23 H23 119.7 . . ? C22 C23 C24 120.6(12) . . ? C24 C23 H23 119.7 . . ? C19 C24 H24 119.2 . . ? C23 C24 C19 121.5(12) . . ? C23 C24 H24 119.2 . . ? C26 C25 C30 120.0 . . ? C26 C25 C39 120.3(8) . . ? C30 C25 C39 119.7(8) . . ? C25 C26 H26 120.0 . . ? C25 C26 C27 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 H27 120.0 . . ? C28 C27 C26 120.0 . . ? C28 C27 H27 120.0 . . ? C27 C28 C29 120.0 . . ? C27 C28 C31 121.2(6) . . ? C29 C28 C31 118.8(6) . . ? C28 C29 H29 120.0 . . ? C30 C29 C28 120.0 . . ? C30 C29 H29 120.0 . . ? C25 C30 H30 120.0 . . ? C29 C30 C25 120.0 . . ? C29 C30 H30 120.0 . . ? C32 C31 C28 118.1(6) . . ? C32 C31 C36 120.0 . . ? C36 C31 C28 121.8(6) . . ? C31 C32 H32 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 H33 120.0 . . ? C34 C33 C32 120.0 . . ? C34 C33 H33 120.0 . . ? C33 C34 N1 117.7(7) . . ? C33 C34 C35 120.0 . . ? C35 C34 N1 122.3(7) . . ? C34 C35 H35 120.0 . . ? C36 C35 C34 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 H36 120.0 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? O1 C37 O2 126.6(11) . . ? O1 C37 C1 115.8(12) . . ? O2 C37 C1 117.6(12) . . ? O3 C38 O4 128.0(14) . . ? O3 C38 C13 113.1(12) . . ? O4 C38 C13 118.3(12) . . ? O5 C39 O6 125.8(13) . . ? O5 C39 C25 116.4(13) . . ? O6 C39 C25 116.5(12) . . ? O13 C40 O13 132.3(19) . 6_665 ? O13 C40 H40 113.9 . . ? O13 C40 H40 113.9 6_665 . ? Zr2 C41 H41 174.5 . . ? O14 C41 Zr2 53.7(10) . . ? O14 C41 Zr2 53.7(10) 6_665 . ? O14 C41 O14 107(2) 6_665 . ? O14 C41 H41 126.2 . . ? O14 C41 H41 126.2 6_665 . ? O11 C42 O18 126.6(14) . . ? O11 C42 H42 116.7 . . ? O18 C42 H42 116.7 . . ? O17 C43 O17 137.4(19) . 6_665 ? O17 C43 H43 111.2 6_665 . ? O17 C43 H43 111.3 . . ? 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 O1 2.194(7) 14 y Zr1 O6 2.221(8) . y Zr1 O8 2.374(7) 6_665 y Zr1 O9 2.037(7) . y Zr1 O10 2.059(5) . y Zr1 O11 2.223(8) . y Zr1 O16 2.270(7) . y Zr1 O17 2.226(9) . y Zr2 O5 2.252(8) . y Zr2 O5 2.252(8) 6_665 y Zr2 O7 2.106(10) . y Zr2 O8 2.246(7) 6_665 y Zr2 O8 2.246(7) . y Zr2 O10 2.079(10) . y Zr2 O14 2.187(9) . y Zr2 O14 2.187(9) 6_665 y Zr3 O4 2.188(8) 6_666 y Zr3 O4 2.188(8) 1_556 y Zr3 O9 2.078(7) . y Zr3 O9 2.078(7) 6_665 y Zr3 O15 2.295(11) . y Zr3 O16 2.316(10) . y Zr3 O18 2.274(9) 6_665 y Zr3 O18 2.274(9) . y Zr4 O2 2.278(8) 14 y Zr4 O3 2.253(8) 1_556 y Zr4 O7 2.089(6) . y Zr4 O8 2.241(7) 6_665 y Zr4 O9 2.063(7) . y Zr4 O12 2.217(8) . y Zr4 O13 2.230(8) . y Zr4 O15 2.263(6) . y O1 C37 1.224(13) . ? O2 C37 1.302(13) . ? O3 C38 1.243(14) . ? O4 C38 1.252(14) . ? O5 C39 1.259(15) . ? O6 C39 1.283(15) . ? O11 C42 1.325(15) . ? O12 H12A 0.8663 . ? O12 H12B 0.8653 . ? O13 C40 1.342(11) . ? O14 C41 1.351(14) . ? O17 C43 1.509(12) . ? N1 C10 1.454(13) . ? N1 C22 1.425(14) . ? N1 C34 1.417(10) . ? C1 C2 1.368(15) . ? C1 C6 1.461(15) . ? C1 C37 1.474(15) . ? C2 H2 0.9300 . ? C2 C3 1.397(14) . ? C3 H3 0.9300 . ? C3 C4 1.387(15) . ? C4 C5 1.406(15) . ? C4 C7 1.477(15) . ? C5 H5 0.9300 . ? C5 C6 1.370(14) . ? C6 H6 0.9300 . ? C7 C8 1.433(15) . ? C7 C12 1.322(15) . ? C8 H8 0.9300 . ? C8 C9 1.372(15) . ? C9 H9 0.9300 . ? C9 C10 1.352(14) . ? C10 C11 1.364(14) . ? C11 H11 0.9300 . ? C11 C12 1.367(15) . ? C12 H12 0.9300 . ? C13 C14 1.3900 . ? C13 C18 1.3900 . ? C13 C38 1.534(15) . ? C14 H14 0.9300 . ? C14 C15 1.3900 . ? C15 H15 0.9300 . ? C15 C16 1.3900 . ? C16 C17 1.3900 . ? C16 C19 1.523(13) . ? C17 H17 0.9300 . ? C17 C18 1.3900 . ? C18 H18 0.9300 . ? O18 C42 1.391(16) . ? C19 C20 1.398(16) . ? C19 C24 1.421(15) . ? C20 H20 0.9300 . ? C20 C21 1.333(15) . ? C21 H21 0.9300 . ? C21 C22 1.387(15) . ? C22 C23 1.366(15) . ? C23 H23 0.9300 . ? C23 C24 1.387(15) . ? C24 H24 0.9300 . ? C25 C26 1.3900 . ? C25 C30 1.3900 . ? C25 C39 1.525(15) . ? C26 H26 0.9300 . ? C26 C27 1.3900 . ? C27 H27 0.9300 . ? C27 C28 1.3900 . ? C28 C29 1.3900 . ? C28 C31 1.498(8) . ? C29 H29 0.9300 . ? C29 C30 1.3900 . ? C30 H30 0.9300 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C32 H32 0.9300 . ? C32 C33 1.3900 . ? C33 H33 0.9300 . ? C33 C34 1.3900 . ? C34 C35 1.3900 . ? C35 H35 0.9300 . ? C35 C36 1.3900 . ? C36 H36 0.9300 . ? C40 H40 0.9300 . ? C41 H41 0.8197 . ? C42 H42 0.9300 . ? C43 H43 0.9302 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Zr1 O1 C37 O2 10(2) 14_554 . . . ? Zr1 O1 C37 C1 -172.3(7) 14_554 . . . ? Zr1 O6 C39 O5 14(2) . . . . ? Zr1 O6 C39 C25 179.8(6) . . . . ? Zr1 O11 C42 O18 10(2) . . . . ? Zr1 O17 C43 O17 -18(3) . . . 6_665 ? Zr2 O5 C39 O6 -7(2) . . . . ? Zr2 O5 C39 C25 -173.0(6) . . . . ? Zr2 O14 C41 O14 -2.1(18) . . . 6_665 ? Zr3 O4 C38 O3 7(2) 1_554 . . . ? Zr3 O4 C38 C13 177.6(7) 1_554 . . . ? Zr3 O18 C42 O11 -11(2) . . . . ? Zr4 O2 C37 O1 1(2) 14_554 . . . ? Zr4 O2 C37 C1 -176.4(7) 14_554 . . . ? Zr4 O3 C38 O4 -10(2) 1_554 . . . ? Zr4 O3 C38 C13 178.8(6) 1_554 . . . ? Zr4 O13 C40 O13 -11(3) . . . 6_665 ? N1 C10 C11 C12 -178.8(10) . . . . ? N1 C22 C23 C24 178.9(11) . . . . ? N1 C34 C35 C36 178.0(8) . . . . ? C1 C2 C3 C4 0.4(18) . . . . ? C2 C1 C6 C5 1.3(17) . . . . ? C2 C1 C37 O1 -17.6(18) . . . . ? C2 C1 C37 O2 160.4(11) . . . . ? C2 C3 C4 C5 0.9(17) . . . . ? C2 C3 C4 C7 173.3(11) . . . . ? C3 C4 C5 C6 -1.0(17) . . . . ? C3 C4 C7 C8 -21.1(19) . . . . ? C3 C4 C7 C12 157.8(13) . . . . ? C4 C5 C6 C1 -0.1(18) . . . . ? C4 C7 C8 C9 178.5(11) . . . . ? C4 C7 C12 C11 -179.6(12) . . . . ? C5 C4 C7 C8 151.4(11) . . . . ? C5 C4 C7 C12 -30(2) . . . . ? C6 C1 C2 C3 -1.4(17) . . . . ? C6 C1 C37 O1 165.3(11) . . . . ? C6 C1 C37 O2 -16.8(18) . . . . ? C7 C4 C5 C6 -174.0(11) . . . . ? C7 C8 C9 C10 1.5(19) . . . . ? C8 C7 C12 C11 -1(2) . . . . ? C8 C9 C10 N1 177.5(11) . . . . ? C8 C9 C10 C11 -1.1(18) . . . . ? C9 C10 C11 C12 -0.2(18) . . . . ? C10 N1 C22 C21 137.3(12) . . . . ? C10 N1 C22 C23 -45.7(17) . . . . ? C10 N1 C34 C33 114.1(9) . . . . ? C10 N1 C34 C35 -64.0(11) . . . . ? C10 C11 C12 C7 1(2) . . . . ? C12 C7 C8 C9 -0.6(18) . . . . ? C13 C14 C15 C16 0.0 . . . . ? C14 C13 C18 C17 0.0 . . . . ? C14 C13 C38 O3 161.6(9) . . . . ? C14 C13 C38 O4 -10.4(15) . . . . ? C14 C15 C16 C17 0.0 . . . . ? C14 C15 C16 C19 -178.5(9) . . . . ? C15 C16 C17 C18 0.0 . . . . ? C15 C16 C19 C20 -1.0(16) . . . . ? C15 C16 C19 C24 -176.9(10) . . . . ? C16 C17 C18 C13 0.0 . . . . ? C16 C19 C20 C21 176.0(12) . . . . ? C16 C19 C24 C23 -178.3(11) . . . . ? C17 C16 C19 C20 -179.5(10) . . . . ? C17 C16 C19 C24 4.6(15) . . . . ? C18 C13 C14 C15 0.0 . . . . ? C18 C13 C38 O3 -20.2(15) . . . . ? C18 C13 C38 O4 167.9(9) . . . . ? C19 C16 C17 C18 178.5(10) . . . . ? C19 C20 C21 C22 5(2) . . . . ? C20 C19 C24 C23 5.5(19) . . . . ? C20 C21 C22 N1 178.8(12) . . . . ? C20 C21 C22 C23 1.6(19) . . . . ? C21 C22 C23 C24 -3.9(18) . . . . ? C22 N1 C10 C9 -11.4(18) . . . . ? C22 N1 C10 C11 167.1(11) . . . . ? C22 N1 C34 C33 -68.8(10) . . . . ? C22 N1 C34 C35 113.2(9) . . . . ? C22 C23 C24 C19 0.3(19) . . . . ? C24 C19 C20 C21 -8(2) . . . . ? C25 C26 C27 C28 0.0 . . . . ? C26 C25 C30 C29 0.0 . . . . ? C26 C25 C39 O5 157.3(9) . . . . ? C26 C25 C39 O6 -10.3(15) . . . . ? C26 C27 C28 C29 0.0 . . . . ? C26 C27 C28 C31 -178.9(8) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C27 C28 C31 C32 -140.2(5) . . . . ? C27 C28 C31 C36 37.0(9) . . . . ? C28 C29 C30 C25 0.0 . . . . ? C28 C31 C32 C33 177.3(7) . . . . ? C28 C31 C36 C35 -177.2(8) . . . . ? C29 C28 C31 C32 40.8(8) . . . . ? C29 C28 C31 C36 -142.0(5) . . . . ? C30 C25 C26 C27 0.0 . . . . ? C30 C25 C39 O5 -25.1(15) . . . . ? C30 C25 C39 O6 167.3(9) . . . . ? C31 C28 C29 C30 179.0(8) . . . . ? C31 C32 C33 C34 0.0 . . . . ? C32 C31 C36 C35 0.0 . . . . ? C32 C33 C34 N1 -178.1(7) . . . . ? C32 C33 C34 C35 0.0 . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 N1 C10 C9 165.6(11) . . . . ? C34 N1 C10 C11 -15.8(16) . . . . ? C34 N1 C22 C21 -39.8(15) . . . . ? C34 N1 C22 C23 137.2(11) . . . . ? C34 C35 C36 C31 0.0 . . . . ? C36 C31 C32 C33 0.0 . . . . ? C37 C1 C2 C3 -178.7(10) . . . . ? C37 C1 C6 C5 178.6(11) . . . . ? C38 C13 C14 C15 178.3(10) . . . . ? C38 C13 C18 C17 -178.2(10) . . . . ? C39 C25 C26 C27 177.6(9) . . . . ? C39 C25 C30 C29 -177.6(9) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 0.000 0.000 -0.361 4605.4 505.0 '48 H2O' 2 0.000 0.500 0.000 7.3 0.0 ? 3 0.000 0.500 0.500 7.3 0.0 ? 4 0.500 0.500 -0.723 4605.4 505.0 '48 H2O' 5 0.500 0.000 0.000 7.3 0.0 ? 6 0.500 0.000 0.500 7.3 0.0 ?