#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:21:14 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252741 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557944.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_1557944 loop_ _publ_author_name 'Moreau, Liane M.' 'Herve, Alexandre' 'Straub, Mark D.' 'Russo, Dominic R.' 'Abergel, Rebecca J.' 'Alayoglu, Selim' 'Arnold, John' 'Braun, Augustin' 'Deblonde, Gauthier J. P.' 'Liu, Yangdongling' 'Lohrey, Trevor D.' 'Olive, Daniel T.' 'Qiao, Yusen' 'Rees, Julian A.' 'Shuh, David K.' 'Teat, Simon J.' 'Booth, Corwin H.' 'Minasian, Stefan G.' _publ_section_title ; Structural properties of ultra-small thorium and uranium dioxide nanoparticles embedded in a covalent organic framework ; _journal_issue 18 _journal_name_full 'Chemical Science' _journal_page_first 4648 _journal_paper_doi 10.1039/C9SC06117G _journal_volume 11 _journal_year 2020 _chemical_formula_sum 'C20 H4 F24 O8 U' _chemical_formula_weight 1066.26 _chemical_properties_physical Air-sensitive,Moisture-sensitive _space_group_crystal_system tetragonal _space_group_IT_number 88 _space_group_name_Hall '-I 4ad' _space_group_name_H-M_alt 'I 41/a :2' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-09-09 deposited with the CCDC. 2020-04-13 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 12 _cell_length_a 17.4457(4) _cell_length_b 17.4457(4) _cell_length_c 29.8629(9) _cell_measurement_reflns_used 39526 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 27.827 _cell_measurement_theta_min 2.335 _cell_volume 9088.8(4) _computing_cell_refinement 'SAINT V8.37A Bruker, Madison WI' _computing_data_collection 'Bruker APEX3 Bruker, Madison WI' _computing_data_reduction 'SAINT V8.37A Bruker, Madison WI' _computing_molecular_graphics ORTEP-32 _computing_publication_material WinGX _computing_structure_refinement SHELXL-2014 _computing_structure_solution SHELXT _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.42 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker D8 with PHOTON 100 detector' _diffrn_measurement_method 'phi and omega shutterless scans' _diffrn_radiation_monochromator 'silicon 111' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_R_equivalents 0.0829 _diffrn_reflns_av_unetI/netI 0.0438 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_number 39526 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 27.710 _diffrn_reflns_theta_max 27.827 _diffrn_reflns_theta_min 2.335 _diffrn_source 'Advanced Light Source, station 11.3.1' _exptl_absorpt_coefficient_mu 3.108 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.4622 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour orange _exptl_crystal_density_diffrn 2.338 _exptl_crystal_description block _exptl_crystal_F_000 5952 _exptl_crystal_recrystallization_method Sublimation _exptl_crystal_size_max 0.050 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.020 _refine_diff_density_max 2.614 _refine_diff_density_min -1.265 _refine_diff_density_rms 0.157 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 359 _refine_ls_number_reflns 4162 _refine_ls_number_restraints 63 _refine_ls_restrained_S_all 1.021 _refine_ls_R_factor_all 0.0911 _refine_ls_R_factor_gt 0.0543 _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^)+(0.0753P)^2^+147.6267P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1361 _refine_ls_wR_factor_ref 0.1667 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2711 _reflns_number_total 4162 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06117g2.cif _cod_data_source_block shelx_CCDC1 _cod_depositor_comments ; The following automatic conversions were performed: data item '_atom_sites_solution_secondary' value 'diffmap' was changed to 'difmap'. Automatic conversion script Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas Adding full bibliography for 1557943--1557944.cif. ; _cod_original_cell_volume 9088.8(5) _cod_original_sg_symbol_H-M 'I 41/a' _cod_database_code 1557944 _shelx_shelxl_version_number 2014/7 _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. ; _shelx_estimated_absorpt_t_min 0.860 _shelx_estimated_absorpt_t_max 0.940 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in I4(1)/a CELL 0.77490 17.4457 17.4457 29.8629 90.000 90.000 90.000 ZERR 12.00 0.0004 0.0004 0.0009 0.000 0.000 0.000 LATT 2 SYMM 1/2 - X, - Y, 1/2 + Z SYMM 3/4 - Y, 1/4 + X, 1/4 + Z SYMM 3/4 + Y, 3/4 - X, 3/4 + Z SFAC C O F U H DISP U -7.31847 4.58716 21402.31 DISP F 0.02109 0.01246 64.36 DISP O 0.01323 0.00737 40.17 DISP C 0.00399 0.00197 13.60 DISP H 0.00000 0.00000 0.67 UNIT 240 96 288 12 48 MERG 2 ISOR 0.01 C12 C13 C14 C15 RIGU 0.004 0.004 O5 O6 C11 C12 C13 C14 C15 FMAP 2 PLAN 20 SIZE 0.020 0.030 0.050 ACTA 55.42 BOND $H LIST 4 WPDB -2 L.S. 10 TEMP -173.00 WGHT 0.075300 147.626694 FVAR 0.01863 C1 1 0.602917 0.476501 0.321474 11.00000 0.08889 0.03638 = 0.08698 0.00132 0.00273 -0.00166 C2 1 0.580370 0.424424 0.359137 11.00000 0.06102 0.06887 = 0.05702 -0.00099 0.00007 0.01788 C3 1 0.594789 0.444430 0.403525 11.00000 0.06526 0.05211 = 0.05957 -0.00492 -0.00072 0.00547 AFIX 43 H3 5 0.619732 0.491409 0.410341 11.00000 -1.20000 AFIX 0 C4 1 0.572421 0.395146 0.437880 11.00000 0.06122 0.06051 = 0.05456 -0.00667 -0.00870 0.01119 C5 1 0.593133 0.417024 0.485630 11.00000 0.08402 0.07406 = 0.05499 -0.01022 -0.00959 0.01115 C6 1 0.352957 0.312573 0.574349 11.00000 0.08736 0.11561 = 0.05586 0.01578 -0.02568 -0.00228 C7 1 0.384947 0.258939 0.610451 11.00000 0.07225 0.06733 = 0.05969 0.01624 0.00137 -0.00017 C8 1 0.364516 0.181464 0.608169 11.00000 0.08031 0.06431 = 0.05805 -0.00198 -0.00404 -0.00028 AFIX 43 H8 5 0.331821 0.164349 0.584777 11.00000 -1.20000 AFIX 0 C9 1 0.390993 0.129810 0.639215 11.00000 0.05260 0.06049 = 0.05650 0.00716 0.00449 -0.00582 C10 1 0.368627 0.046864 0.635163 11.00000 0.07252 0.05890 = 0.06865 -0.00661 -0.00771 -0.00925 C11 1 0.709375 0.134251 0.768760 11.00000 0.09931 0.10347 = 0.12292 0.00783 -0.03278 0.02256 C12 1 0.630408 0.160163 0.762068 11.00000 0.11192 0.13777 = 0.09737 0.01981 -0.01481 0.02892 C13 1 0.573498 0.124976 0.794308 11.00000 0.12436 0.13384 = 0.11455 0.01060 -0.01206 0.00684 AFIX 43 H13 5 0.592110 0.092901 0.817603 11.00000 -1.20000 AFIX 0 C14 1 0.489850 0.138612 0.790952 11.00000 0.12067 0.09793 = 0.08477 0.01427 -0.00903 -0.00030 C15 1 0.424448 0.108344 0.825524 11.00000 0.14029 0.10428 = 0.08453 0.01792 0.00365 -0.01643 O1 2 0.550263 0.361389 0.346384 11.00000 0.07575 0.05524 = 0.05096 -0.00006 -0.00096 -0.01229 O2 2 0.538763 0.331360 0.434202 11.00000 0.06275 0.05579 = 0.04905 0.00082 -0.00680 -0.00209 O3 2 0.425922 0.288856 0.638361 11.00000 0.07441 0.04945 = 0.05459 0.00081 -0.01575 -0.00401 O4 2 0.435261 0.145644 0.671970 11.00000 0.06125 0.04782 = 0.05393 0.00660 0.00014 -0.00437 O5 2 0.607376 0.189698 0.729202 11.00000 0.06151 0.05762 = 0.06570 -0.00797 -0.00894 0.00704 O6 2 0.459183 0.176154 0.761812 11.00000 0.08742 0.06596 = 0.05086 0.00945 -0.00279 -0.00750 F1 3 0.638653 0.539559 0.335754 11.00000 0.18436 0.07646 = 0.07505 0.00449 -0.00129 -0.02859 F2 3 0.647279 0.444709 0.291983 11.00000 0.09278 0.08699 = 0.07404 -0.00018 0.02791 0.00021 F3 3 0.540753 0.500429 0.299516 11.00000 0.10722 0.11000 = 0.07244 0.02016 -0.00006 0.02916 F4 3 0.618672 0.485725 0.489173 11.00000 0.27171 0.10240 = 0.08319 0.00150 -0.05880 -0.05524 F5 3 0.648706 0.373592 0.499907 11.00000 0.13208 0.15169 = 0.06187 0.00496 -0.03057 0.03901 F6 3 0.538658 0.408067 0.513305 11.00000 0.09486 0.21257 = 0.08346 -0.05950 0.02353 -0.03353 F7 3 0.403691 0.357932 0.558268 11.00000 0.14622 0.15999 = 0.14633 0.09471 -0.02023 -0.03841 F8 3 0.303825 0.361380 0.593311 11.00000 0.15655 0.09798 = 0.13206 -0.02661 -0.07119 0.04343 F9 3 0.314034 0.278967 0.542958 11.00000 0.21130 0.08862 = 0.07935 0.00949 -0.05490 -0.00131 F10 3 0.358401 0.016558 0.675458 11.00000 0.12726 0.07191 = 0.09529 0.01918 0.01234 -0.02347 F11 3 0.423884 0.006255 0.617036 11.00000 0.09319 0.06589 = 0.12589 -0.01528 0.01843 0.00936 F12 3 0.307669 0.036026 0.613155 11.00000 0.09718 0.07674 = 0.16109 0.00356 -0.04676 -0.00580 F13 3 0.743999 0.122328 0.734677 11.00000 0.10000 0.41681 = 0.15479 -0.11970 -0.01812 0.11760 F14 3 0.746132 0.172612 0.795358 11.00000 0.12361 0.27446 = 0.17598 -0.11930 -0.01066 -0.06329 F17 3 0.389685 0.054152 0.804031 11.00000 0.12682 0.11495 = 0.10034 0.03835 -0.00280 -0.01210 F16 3 0.381246 0.149138 0.843759 11.00000 0.40729 0.21759 = 0.15239 -0.03515 0.03377 0.17356 F15 3 0.705309 0.071905 0.786766 11.00000 0.22675 0.17555 = 0.51629 0.14724 -0.02113 -0.00858 F18 3 0.470829 0.076304 0.854012 11.00000 0.16607 0.25296 = 0.11878 -0.04453 -0.01900 -0.02594 U1 4 0.500000 0.250000 0.375000 10.25000 0.05344 0.05344 = 0.05103 0.00000 0.00000 0.00000 U2 4 0.500000 0.250000 0.700222 10.50000 0.05465 0.05248 = 0.04945 0.00000 0.00000 -0.00134 HKLF 4 REM shelxt_a.res in I4(1)/a REM R1 = 0.0543 for 2711 Fo > 4sig(Fo) and 0.0911 for all 4162 data REM 359 parameters refined using 63 restraints END WGHT 0.0749 148.0950 REM Highest difference peak 2.614, deepest hole -1.265, 1-sigma level 0.157 Q1 1 0.5000 0.2500 0.7259 10.50000 0.05 2.61 Q2 1 0.4034 0.1872 0.7918 11.00000 0.05 1.66 Q3 1 0.5000 0.2500 0.8750 10.25000 0.05 1.57 Q4 1 0.6474 0.2606 0.7947 11.00000 0.05 1.52 Q5 1 0.6527 0.2140 0.7662 11.00000 0.05 1.14 Q6 1 0.5000 0.2500 0.5512 10.50000 0.05 1.10 Q7 1 0.3439 0.1183 0.8573 11.00000 0.05 0.74 Q8 1 0.7142 0.1026 0.8146 11.00000 0.05 0.70 Q9 1 0.7600 0.1885 0.7355 11.00000 0.05 0.68 Q10 1 0.4512 0.2805 0.6744 11.00000 0.05 0.66 Q11 1 0.4239 0.2819 0.5365 11.00000 0.05 0.65 Q12 1 0.4976 0.3707 0.6075 11.00000 0.05 0.64 Q13 1 0.4698 0.1743 0.8638 11.00000 0.05 0.60 Q14 1 0.7308 0.0675 0.7601 11.00000 0.05 0.60 Q15 1 0.6675 0.0703 0.7751 11.00000 0.05 0.60 Q16 1 0.4505 0.1586 0.8565 11.00000 0.05 0.59 Q17 1 0.5952 0.3169 0.4642 11.00000 0.05 0.57 Q18 1 0.4732 0.1014 0.8284 11.00000 0.05 0.52 Q19 1 0.7824 0.1531 0.7758 11.00000 0.05 0.51 Q20 1 0.5958 0.3465 0.5147 11.00000 0.05 0.50 ; _shelx_res_checksum 20633 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.6029(8) 0.4765(7) 0.3215(5) 0.071(3) Uani 1 1 d . . . . . C2 C 0.5804(7) 0.4244(7) 0.3591(4) 0.062(3) Uani 1 1 d . . . . . C3 C 0.5948(7) 0.4444(6) 0.4035(4) 0.059(3) Uani 1 1 d . . . . . H3 H 0.6197 0.4914 0.4103 0.071 Uiso 1 1 calc R U . . . C4 C 0.5724(7) 0.3951(7) 0.4379(4) 0.059(3) Uani 1 1 d . . . . . C5 C 0.5931(8) 0.4170(8) 0.4856(4) 0.071(3) Uani 1 1 d . . . . . C6 C 0.3530(9) 0.3126(10) 0.5743(5) 0.086(4) Uani 1 1 d . . . . . C7 C 0.3849(7) 0.2589(7) 0.6105(4) 0.066(3) Uani 1 1 d . . . . . C8 C 0.3645(7) 0.1815(7) 0.6082(4) 0.068(3) Uani 1 1 d . . . . . H8 H 0.3318 0.1643 0.5848 0.081 Uiso 1 1 calc R U . . . C9 C 0.3910(6) 0.1298(7) 0.6392(4) 0.057(3) Uani 1 1 d . . . . . C10 C 0.3686(8) 0.0469(7) 0.6352(4) 0.067(3) Uani 1 1 d . . . . . C11 C 0.7094(11) 0.1343(12) 0.7688(7) 0.109(5) Uani 1 1 d . U . . . C12 C 0.6304(11) 0.1602(11) 0.7621(6) 0.116(5) Uani 1 1 d . U . . . C13 C 0.5735(12) 0.1250(12) 0.7943(6) 0.124(5) Uani 1 1 d . U . . . H13 H 0.5921 0.0929 0.8176 0.149 Uiso 1 1 calc R U . . . C14 C 0.4899(11) 0.1386(10) 0.7910(5) 0.101(4) Uani 1 1 d . U . . . C15 C 0.4244(14) 0.1083(12) 0.8255(6) 0.110(5) Uani 1 1 d . U . . . O1 O 0.5503(5) 0.3614(4) 0.3464(2) 0.0607(19) Uani 1 1 d . . . . . O2 O 0.5388(4) 0.3314(4) 0.4342(2) 0.0559(18) Uani 1 1 d . . . . . O3 O 0.4259(5) 0.2889(4) 0.6384(2) 0.0595(19) Uani 1 1 d . . . . . O4 O 0.4353(4) 0.1456(4) 0.6720(2) 0.0543(17) Uani 1 1 d . . . . . O5 O 0.6074(4) 0.1897(4) 0.7292(3) 0.0616(19) Uani 1 1 d . U . . . O6 O 0.4592(5) 0.1762(5) 0.7618(2) 0.068(2) Uani 1 1 d . U . . . F1 F 0.6387(6) 0.5396(5) 0.3358(3) 0.112(3) Uani 1 1 d . . . . . F2 F 0.6473(5) 0.4447(5) 0.2920(2) 0.085(2) Uani 1 1 d . . . . . F3 F 0.5408(5) 0.5004(5) 0.2995(3) 0.097(3) Uani 1 1 d . . . . . F4 F 0.6187(8) 0.4857(6) 0.4892(3) 0.152(5) Uani 1 1 d . . . . . F5 F 0.6487(6) 0.3736(6) 0.4999(3) 0.115(3) Uani 1 1 d . . . . . F6 F 0.5387(5) 0.4081(7) 0.5133(3) 0.130(4) Uani 1 1 d . . . . . F7 F 0.4037(7) 0.3579(7) 0.5583(4) 0.151(5) Uani 1 1 d . . . . . F8 F 0.3038(7) 0.3614(6) 0.5933(4) 0.129(4) Uani 1 1 d . . . . . F9 F 0.3140(7) 0.2790(5) 0.5430(3) 0.126(4) Uani 1 1 d . . . . . F10 F 0.3584(5) 0.0166(4) 0.6755(3) 0.098(3) Uani 1 1 d . . . . . F11 F 0.4239(5) 0.0063(5) 0.6170(3) 0.095(3) Uani 1 1 d . . . . . F12 F 0.3077(5) 0.0360(5) 0.6132(3) 0.112(3) Uani 1 1 d . . . . . F13 F 0.7440(7) 0.1223(12) 0.7347(5) 0.224(10) Uani 1 1 d . . . . . F14 F 0.7461(7) 0.1726(10) 0.7954(5) 0.191(7) Uani 1 1 d . . . . . F17 F 0.3897(6) 0.0542(6) 0.8040(3) 0.114(3) Uani 1 1 d . . . . . F16 F 0.3812(13) 0.1491(10) 0.8438(5) 0.259(11) Uani 1 1 d . . . . . F15 F 0.7053(12) 0.0719(12) 0.7868(10) 0.306(15) Uani 1 1 d . . . . . F18 F 0.4708(8) 0.0763(10) 0.8540(4) 0.179(6) Uani 1 1 d . . . . . U1 U 0.5000 0.2500 0.3750 0.0526(2) Uani 1 4 d S T P . . U2 U 0.5000 0.2500 0.70022(2) 0.0522(2) Uani 1 2 d S T P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.089(10) 0.036(6) 0.087(9) 0.001(6) 0.003(8) -0.002(6) C2 0.061(7) 0.069(8) 0.057(6) -0.001(6) 0.000(5) 0.018(6) C3 0.065(7) 0.052(7) 0.060(7) -0.005(5) -0.001(5) 0.005(5) C4 0.061(7) 0.061(7) 0.055(6) -0.007(5) -0.009(5) 0.011(6) C5 0.084(9) 0.074(9) 0.055(7) -0.010(6) -0.010(7) 0.011(7) C6 0.087(10) 0.116(13) 0.056(8) 0.016(8) -0.026(7) -0.002(10) C7 0.072(8) 0.067(8) 0.060(7) 0.016(6) 0.001(6) 0.000(7) C8 0.080(9) 0.064(8) 0.058(7) -0.002(6) -0.004(6) 0.000(7) C9 0.053(7) 0.060(7) 0.056(6) 0.007(5) 0.004(5) -0.006(5) C10 0.073(9) 0.059(8) 0.069(8) -0.007(6) -0.008(6) -0.009(7) C11 0.099(8) 0.103(13) 0.123(13) 0.008(11) -0.033(7) 0.023(8) C12 0.112(6) 0.138(9) 0.097(6) 0.020(6) -0.015(5) 0.029(6) C13 0.124(6) 0.134(9) 0.115(8) 0.011(7) -0.012(5) 0.007(5) C14 0.121(6) 0.098(8) 0.085(6) 0.014(6) -0.009(5) 0.000(5) C15 0.140(8) 0.104(9) 0.085(7) 0.018(7) 0.004(6) -0.016(7) O1 0.076(5) 0.055(5) 0.051(4) 0.000(3) -0.001(4) -0.012(4) O2 0.063(5) 0.056(5) 0.049(4) 0.001(3) -0.007(3) -0.002(4) O3 0.074(5) 0.049(4) 0.055(4) 0.001(3) -0.016(4) -0.004(4) O4 0.061(5) 0.048(4) 0.054(4) 0.007(3) 0.000(3) -0.004(3) O5 0.062(5) 0.058(5) 0.066(4) -0.008(3) -0.009(3) 0.007(4) O6 0.087(5) 0.066(5) 0.051(4) 0.009(3) -0.003(4) -0.008(4) F1 0.184(9) 0.076(6) 0.075(5) 0.004(4) -0.001(5) -0.029(6) F2 0.093(6) 0.087(6) 0.074(5) 0.000(4) 0.028(4) 0.000(5) F3 0.107(7) 0.110(7) 0.072(5) 0.020(4) 0.000(4) 0.029(5) F4 0.272(15) 0.102(7) 0.083(6) 0.002(5) -0.059(8) -0.055(8) F5 0.132(8) 0.152(8) 0.062(5) 0.005(5) -0.031(5) 0.039(6) F6 0.095(7) 0.213(11) 0.083(6) -0.060(7) 0.024(5) -0.034(7) F7 0.146(10) 0.160(10) 0.146(9) 0.095(8) -0.020(7) -0.038(8) F8 0.157(10) 0.098(7) 0.132(8) -0.027(6) -0.071(7) 0.043(7) F9 0.211(12) 0.089(6) 0.079(6) 0.009(4) -0.055(6) -0.001(7) F10 0.127(7) 0.072(5) 0.095(6) 0.019(4) 0.012(5) -0.023(5) F11 0.093(6) 0.066(5) 0.126(7) -0.015(4) 0.018(5) 0.009(4) F12 0.097(7) 0.077(6) 0.161(9) 0.004(5) -0.047(6) -0.006(5) F13 0.100(9) 0.42(3) 0.155(11) -0.120(15) -0.018(8) 0.118(13) F14 0.124(10) 0.274(18) 0.176(12) -0.119(12) -0.011(8) -0.063(11) F17 0.127(8) 0.115(8) 0.100(7) 0.038(6) -0.003(6) -0.012(6) F16 0.41(3) 0.218(16) 0.152(13) -0.035(11) 0.034(15) 0.174(18) F15 0.23(2) 0.176(17) 0.52(4) 0.15(2) -0.02(2) -0.009(15) F18 0.166(12) 0.253(17) 0.119(9) -0.045(10) -0.019(9) -0.026(11) U1 0.0534(3) 0.0534(3) 0.0510(4) 0.000 0.000 0.000 U2 0.0547(4) 0.0525(4) 0.0495(3) 0.000 0.000 -0.0013(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0040 0.0020 'Calculated using XDISP in WinGX (Farrugia, 1999)' O O 0.0132 0.0074 'Calculated using XDISP in WinGX (Farrugia, 1999)' F F 0.0211 0.0125 'Calculated using XDISP in WinGX (Farrugia, 1999)' U U -7.3185 4.5872 'Calculated using XDISP in WinGX (Farrugia, 1999)' H H 0.0000 0.0000 'Calculated using XDISP in WinGX (Farrugia, 1999)' 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 F2 C1 F3 106.6(11) . . ? F2 C1 F1 106.9(11) . . ? F3 C1 F1 106.2(10) . . ? F2 C1 C2 114.0(10) . . ? F3 C1 C2 110.2(11) . . ? F1 C1 C2 112.5(11) . . ? O1 C2 C3 125.0(11) . . ? O1 C2 C1 114.0(10) . . ? C3 C2 C1 121.0(12) . . ? C2 C3 C4 119.7(11) . . ? C2 C3 H3 120.2 . . ? C4 C3 H3 120.2 . . ? O2 C4 C3 127.5(10) . . ? O2 C4 C5 114.4(11) . . ? C3 C4 C5 118.0(11) . . ? F6 C5 F4 108.7(12) . . ? F6 C5 F5 105.8(12) . . ? F4 C5 F5 105.0(13) . . ? F6 C5 C4 113.7(12) . . ? F4 C5 C4 113.2(12) . . ? F5 C5 C4 109.8(10) . . ? F7 C6 F9 111.7(13) . . ? F7 C6 F8 102.1(15) . . ? F9 C6 F8 105.0(13) . . ? F7 C6 C7 112.9(12) . . ? F9 C6 C7 115.0(14) . . ? F8 C6 C7 109.0(12) . . ? O3 C7 C8 126.7(11) . . ? O3 C7 C6 115.7(12) . . ? C8 C7 C6 117.6(12) . . ? C9 C8 C7 121.0(12) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? O4 C9 C8 125.4(11) . . ? O4 C9 C10 115.3(10) . . ? C8 C9 C10 119.3(11) . . ? F12 C10 F11 108.8(11) . . ? F12 C10 F10 107.4(12) . . ? F11 C10 F10 104.9(11) . . ? F12 C10 C9 113.8(11) . . ? F11 C10 C9 111.2(11) . . ? F10 C10 C9 110.2(10) . . ? F13 C11 F15 104(2) . . ? F13 C11 F14 112(2) . . ? F15 C11 F14 103(2) . . ? F13 C11 C12 114.3(17) . . ? F15 C11 C12 106(2) . . ? F14 C11 C12 114.5(19) . . ? O5 C12 C11 124.7(19) . . ? O5 C12 C13 118.9(17) . . ? C11 C12 C13 113.9(17) . . ? C14 C13 C12 122.5(17) . . ? C14 C13 H13 118.7 . . ? C12 C13 H13 118.7 . . ? O6 C14 C13 124.7(16) . . ? O6 C14 C15 108.7(16) . . ? C13 C14 C15 126.6(16) . . ? F16 C15 F17 112(2) . . ? F16 C15 F18 110.9(19) . . ? F17 C15 F18 107.6(18) . . ? F16 C15 C14 123(2) . . ? F17 C15 C14 104.5(16) . . ? F18 C15 C14 96.8(18) . . ? C2 O1 U1 140.8(7) . . ? C4 O2 U1 136.6(7) . . ? C7 O3 U2 137.5(7) . . ? C9 O4 U2 138.5(7) . . ? C12 O5 U2 141.7(11) . . ? C14 O6 U2 136.2(11) . . ? O1 U1 O1 136.3(4) 6_554 . ? O1 U1 O1 97.96(12) 6_554 11_666 ? O1 U1 O1 97.96(12) . 11_666 ? O1 U1 O1 97.96(12) 6_554 16_656 ? O1 U1 O1 97.96(12) . 16_656 ? O1 U1 O1 136.3(4) 11_666 16_656 ? O1 U1 O2 74.6(3) 6_554 16_656 ? O1 U1 O2 73.1(3) . 16_656 ? O1 U1 O2 153.5(3) 11_666 16_656 ? O1 U1 O2 70.2(2) 16_656 16_656 ? O1 U1 O2 73.1(3) 6_554 11_666 ? O1 U1 O2 74.6(3) . 11_666 ? O1 U1 O2 70.2(2) 11_666 11_666 ? O1 U1 O2 153.5(3) 16_656 11_666 ? O2 U1 O2 83.3(3) 16_656 11_666 ? O1 U1 O2 70.2(2) 6_554 6_554 ? O1 U1 O2 153.5(3) . 6_554 ? O1 U1 O2 74.6(3) 11_666 6_554 ? O1 U1 O2 73.1(3) 16_656 6_554 ? O2 U1 O2 123.9(2) 16_656 6_554 ? O2 U1 O2 123.9(2) 11_666 6_554 ? O1 U1 O2 153.5(3) 6_554 . ? O1 U1 O2 70.2(2) . . ? O1 U1 O2 73.1(3) 11_666 . ? O1 U1 O2 74.6(3) 16_656 . ? O2 U1 O2 123.9(2) 16_656 . ? O2 U1 O2 123.9(2) 11_666 . ? O2 U1 O2 83.3(3) 6_554 . ? O4 U2 O4 137.0(3) . 6_554 ? O4 U2 O5 95.7(3) . 6_554 ? O4 U2 O5 100.0(2) 6_554 6_554 ? O4 U2 O5 100.0(2) . . ? O4 U2 O5 95.7(3) 6_554 . ? O5 U2 O5 136.1(4) 6_554 . ? O4 U2 O3 75.8(3) . 6_554 ? O4 U2 O3 70.8(2) 6_554 6_554 ? O5 U2 O3 150.2(3) 6_554 6_554 ? O5 U2 O3 73.6(3) . 6_554 ? O4 U2 O3 70.8(2) . . ? O4 U2 O3 75.8(3) 6_554 . ? O5 U2 O3 73.6(3) 6_554 . ? O5 U2 O3 150.2(3) . . ? O3 U2 O3 76.6(4) 6_554 . ? O4 U2 O6 150.1(3) . 6_554 ? O4 U2 O6 72.9(2) 6_554 6_554 ? O5 U2 O6 72.8(3) 6_554 6_554 ? O5 U2 O6 73.3(3) . 6_554 ? O3 U2 O6 127.2(3) 6_554 6_554 ? O3 U2 O6 128.4(3) . 6_554 ? O4 U2 O6 72.9(2) . . ? O4 U2 O6 150.1(3) 6_554 . ? O5 U2 O6 73.3(3) 6_554 . ? O5 U2 O6 72.8(3) . . ? O3 U2 O6 128.4(3) 6_554 . ? O3 U2 O6 127.2(3) . . ? O6 U2 O6 77.3(4) 6_554 . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 F2 1.297(15) . ? C1 F3 1.334(15) . ? C1 F1 1.334(14) . ? C1 C2 1.498(17) . ? C2 O1 1.277(14) . ? C2 C3 1.394(15) . ? C3 C4 1.394(15) . ? C3 H3 0.9500 . ? C4 O2 1.263(13) . ? C4 C5 1.520(16) . ? C5 F6 1.269(15) . ? C5 F4 1.283(16) . ? C5 F5 1.302(14) . ? C6 F7 1.281(17) . ? C6 F9 1.298(16) . ? C6 F8 1.334(18) . ? C6 C7 1.533(17) . ? C7 O3 1.216(14) . ? C7 C8 1.399(17) . ? C8 C9 1.373(16) . ? C8 H8 0.9500 . ? C9 O4 1.277(13) . ? C9 C10 1.504(16) . ? C10 F12 1.264(15) . ? C10 F11 1.313(15) . ? C10 F10 1.326(14) . ? C11 F13 1.20(2) . ? C11 F15 1.22(2) . ? C11 F14 1.22(2) . ? C11 C12 1.46(2) . ? C12 O5 1.179(17) . ? C12 C13 1.51(2) . ? C13 C14 1.48(2) . ? C13 H13 0.9500 . ? C14 O6 1.213(17) . ? C14 C15 1.63(3) . ? C15 F16 1.17(2) . ? C15 F17 1.29(2) . ? C15 F18 1.30(2) . ? O1 U1 2.297(7) . ? O2 U1 2.366(7) . ? O3 U2 2.354(7) . ? O4 U2 2.303(7) . ? O5 U2 2.316(7) . ? O6 U2 2.356(7) . ? U1 O1 2.297(7) 6_554 ? U1 O1 2.297(7) 11_666 ? U1 O1 2.297(7) 16_656 ? U1 O2 2.366(7) 16_656 ? U1 O2 2.366(7) 11_666 ? U1 O2 2.366(7) 6_554 ? U2 O4 2.303(7) 6_554 ? U2 O5 2.316(7) 6_554 ? U2 O3 2.354(7) 6_554 ? U2 O6 2.356(7) 6_554 ?