#------------------------------------------------------------------------------ #$Date: 2020-06-05 13:21:14 +0300 (Fri, 05 Jun 2020) $ #$Revision: 252741 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/79/1557943.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_1557943 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_moiety 'C24 H14 F24 O10 Th' _chemical_formula_sum 'C24 H14 F24 O10 Th' _chemical_formula_weight 1150.39 _chemical_properties_physical Moisture-sensitive _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _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 97.371(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.8993(5) _cell_length_b 15.9751(7) _cell_length_c 17.3394(7) _cell_measurement_reflns_used 17900 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 30.266 _cell_measurement_theta_min 2.224 _cell_volume 3543.6(3) _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-2014/7 (Sheldrick, 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 0.996 _diffrn_measurement_device_type 'Bruker D8 with PHOTON 100 detector' _diffrn_measurement_method 'phi and omega shutterless scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7749 _diffrn_reflns_av_R_equivalents 0.0560 _diffrn_reflns_av_unetI/netI 0.0449 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17900 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 27.710 _diffrn_reflns_theta_max 30.266 _diffrn_reflns_theta_min 2.224 _diffrn_source 'Advanced Light Source, station 11.3.1' _exptl_absorpt_coefficient_mu 2.472 _exptl_absorpt_correction_T_max 0.7460 _exptl_absorpt_correction_T_min 0.5866 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.156 _exptl_crystal_description shard _exptl_crystal_F_000 2176 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: DME/hexane' _exptl_crystal_size_max 0.070 _exptl_crystal_size_mid 0.010 _exptl_crystal_size_min 0.010 _refine_diff_density_max 1.855 _refine_diff_density_min -1.216 _refine_diff_density_rms 0.128 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 522 _refine_ls_number_reflns 4079 _refine_ls_number_restraints 42 _refine_ls_restrained_S_all 1.073 _refine_ls_R_factor_all 0.0394 _refine_ls_R_factor_gt 0.0296 _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^)+(0.0109P)^2^+12.4450P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0536 _refine_ls_wR_factor_ref 0.0569 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3549 _reflns_number_total 4079 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06117g2.cif _cod_data_source_block shelx _cod_depositor_comments ; The following automatic conversions were performed: data name '__diffrn_radiation_type' was replaced with '_diffrn_radiation_type'. Automatic conversion script Id: cif_correct_tags 7550 2019-12-06 10:49:48Z antanas 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_sg_symbol_H-M 'C 2/c' _cod_database_code 1557943 _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 0.846 _shelx_estimated_absorpt_t_max 0.976 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL shelxt_a.res in C2/c CELL 0.77490 12.8993 15.9751 17.3394 90.000 97.371 90.000 ZERR 4.00 0.0005 0.0007 0.0007 0.000 0.003 0.000 LATT 7 SYMM - X, Y, 1/2 - Z SFAC C H O F TH DISP Th -9.69906 4.19381 19615.89 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 96 56 40 96 4 MERG 2 ISOR 0.01 C3' C11' C5' F1 F1' C6 C6' FMAP 2 PLAN 20 SIZE 0.010 0.010 0.070 ACTA 55.42 BOND $H LIST 6 L.S. 10 TEMP -173.00 WGHT 0.010900 12.445000 FVAR 0.06222 0.49505 TH1 5 0.500000 0.613656 0.250000 10.50000 0.01846 0.02242 = 0.01664 0.00000 0.00610 0.00000 PART 1 O4 3 0.367847 0.549601 0.159437 10.50000 0.02174 0.01669 = 0.02402 -0.00325 0.00444 0.00371 O1 3 0.625006 0.725728 0.268161 10.50000 0.02783 0.01874 = 0.02679 -0.00607 0.01234 -0.00015 O5 3 0.561504 0.476717 0.186327 10.50000 0.02065 0.02950 = 0.02080 0.00038 0.00953 0.00597 PART 2 O3' 3 0.333319 0.623175 0.304784 10.50000 0.01618 0.03138 = 0.03144 -0.01187 0.00677 -0.01079 PART 1 C6 1 0.267213 0.552374 0.146719 10.50000 0.02490 0.03086 = 0.02309 0.00224 0.00400 0.00030 C4 1 0.237361 0.591991 0.273892 10.50000 0.01857 0.04010 = 0.01853 0.00551 0.00908 0.00051 C5 1 0.200464 0.574973 0.197270 10.50000 0.01571 0.02561 = 0.03505 0.00991 0.00276 0.00530 AFIX 43 H5 2 0.127757 0.579136 0.179860 10.50000 -1.20000 AFIX 0 C1 1 0.645671 0.785661 0.315887 10.50000 0.02580 0.02644 = 0.03029 0.00389 0.00142 -0.00078 PART 2 C7' 1 0.462397 0.401320 0.200358 10.50000 0.02635 0.01652 = 0.02797 -0.00757 0.01620 -0.00372 AFIX 23 H7'1 2 0.473596 0.350442 0.169893 10.50000 -1.20000 H7'2 2 0.386830 0.412291 0.200176 10.50000 -1.20000 AFIX 0 C9' 1 0.170268 0.663230 0.337819 10.50000 0.04159 0.04410 = 0.06196 0.02297 0.03766 0.01779 F1' 4 0.191824 0.625821 0.404605 10.50000 0.06665 0.10782 = 0.03985 -0.00223 0.02618 0.03357 F2' 4 0.190295 0.739167 0.354529 10.50000 0.08447 0.06278 = 0.08956 -0.03289 0.05186 -0.00439 F3' 4 0.067911 0.656905 0.313181 10.50000 0.02366 0.15437 = 0.06774 -0.03528 0.00922 0.01652 PART 1 F4 4 0.124046 0.515315 0.051919 10.50000 0.04232 0.07590 = 0.06373 -0.02508 -0.01556 0.00639 F5 4 0.263900 0.443999 0.055670 10.50000 0.06405 0.05825 = 0.05779 -0.02779 -0.02845 0.02185 F6 4 0.257802 0.567818 0.014493 10.50000 0.07264 0.08026 = 0.02165 0.01436 -0.01247 -0.00167 C10 1 0.224144 0.520089 0.064867 10.50000 0.05143 0.01894 = 0.03027 -0.01562 -0.01102 0.00120 F10 4 0.695759 0.874335 0.218223 10.50000 0.10111 0.06448 = 0.03478 0.01384 -0.00500 -0.04915 F11 4 0.743144 0.912919 0.334465 10.50000 0.07733 0.03415 = 0.04804 -0.01260 0.01292 -0.02708 F12 4 0.817716 0.805752 0.290415 10.50000 0.03896 0.05775 = 0.10529 -0.01236 0.02502 -0.02176 C12 1 0.728717 0.845678 0.289541 10.50000 0.04004 0.04372 = 0.02224 -0.00765 0.00450 -0.00790 C2 1 0.605695 0.800654 0.384111 10.50000 0.03616 0.02841 = 0.02802 -0.00644 0.00429 -0.00433 AFIX 43 H2 2 0.624515 0.850231 0.412790 10.50000 -1.20000 AFIX 0 C8 1 0.567452 0.477169 0.104009 10.50000 0.05016 0.03716 = 0.01642 -0.00395 0.01098 -0.00441 AFIX 137 H8A 2 0.611411 0.430599 0.090839 10.50000 -1.50000 H8B 2 0.597892 0.530189 0.089482 10.50000 -1.50000 H8C 2 0.497101 0.471028 0.075652 10.50000 -1.50000 AFIX 0 C3 1 0.536894 0.742882 0.411810 10.50000 0.03726 0.03075 = 0.01471 -0.00633 0.00656 0.00350 PART 2 F10' 4 0.587621 0.912699 0.217068 10.50000 0.12393 0.06781 = 0.07023 0.03747 -0.03456 -0.05541 C1' 1 0.583162 0.810969 0.312815 10.50000 0.02725 0.02721 = 0.03158 0.00446 0.00223 -0.00649 C12' 1 0.633781 0.889716 0.283925 10.50000 0.04495 0.03557 = 0.03248 -0.00726 0.00241 -0.01691 F11' 4 0.631607 0.953554 0.330800 10.50000 0.20174 0.04803 = 0.07998 -0.02081 0.06829 -0.05593 PART 1 C7 1 0.523726 0.398329 0.212331 10.50000 0.02259 0.03288 = 0.03463 -0.00302 0.00783 -0.00203 AFIX 23 H7A 2 0.582671 0.358175 0.217839 10.50000 -1.20000 H7B 2 0.470552 0.376690 0.170878 10.50000 -1.20000 AFIX 0 PART 2 O1' 3 0.590403 0.748482 0.269625 10.50000 0.02155 0.02068 = 0.01725 -0.00724 0.00737 -0.00314 C4' 1 0.236047 0.630139 0.278311 10.50000 0.02896 0.02887 = 0.03813 -0.00161 0.01035 0.00137 PART 1 F1 4 0.189281 0.585646 0.398791 10.50000 0.07374 0.12162 = 0.03069 0.02256 0.03598 0.03526 F2 4 0.115336 0.678716 0.323057 10.50000 0.09592 0.12569 = 0.06468 0.01451 0.05082 0.06665 F3 4 0.074454 0.554883 0.314161 10.50000 0.05332 0.17054 = 0.11489 0.01513 0.05797 -0.00680 C9 1 0.158896 0.607923 0.332765 10.50000 0.02138 0.10790 = 0.03448 0.02795 0.01057 0.02369 O3 3 0.327262 0.592098 0.303292 10.50000 0.02203 0.02845 = 0.01944 -0.00585 0.00705 -0.01134 PART 2 O5' 3 0.520406 0.473602 0.178537 10.50000 0.02318 0.02629 = 0.01980 -0.00017 0.00942 0.00153 C5' 1 0.189942 0.612304 0.201694 10.50000 0.01801 0.03413 = 0.03465 0.00642 0.00266 0.01457 AFIX 43 H5' 2 0.117452 0.621980 0.186906 10.50000 -1.20000 AFIX 0 C2' 1 0.538967 0.813900 0.380677 10.50000 0.04698 0.02281 = 0.02162 -0.00577 0.00664 -0.00508 AFIX 43 H2' 2 0.536136 0.865705 0.407228 10.50000 -1.20000 AFIX 0 C8' 1 0.525953 0.471360 0.095171 10.50000 0.03235 0.03789 = 0.01108 -0.00422 0.00780 0.00123 AFIX 137 H8'1 2 0.561451 0.420004 0.082134 10.50000 -1.50000 H8'2 2 0.565052 0.520113 0.080336 10.50000 -1.50000 H8'3 2 0.455088 0.472454 0.066965 10.50000 -1.50000 AFIX 0 C6' 1 0.249897 0.581154 0.149071 10.50000 0.02219 0.03580 = 0.02860 0.00402 -0.00517 -0.00840 O4' 3 0.348222 0.574233 0.157140 10.50000 0.02091 0.02369 = 0.01969 -0.00157 0.00620 0.00945 F12' 4 0.730382 0.876577 0.275780 10.50000 0.04715 0.07765 = 0.23633 0.03808 0.03406 -0.02265 PART 1 F7 4 0.422068 0.697689 0.510817 10.50000 0.09759 0.04922 = 0.02472 0.00228 0.03120 0.02509 F8 4 0.550714 0.746886 0.542008 10.50000 0.23580 0.24955 = 0.03833 -0.00448 0.03093 0.12889 F9 4 0.476623 0.838324 0.498658 10.50000 0.15633 0.05271 = 0.08108 -0.03135 0.07887 0.00059 C11 1 0.500055 0.758510 0.491690 10.50000 0.05084 0.04132 = 0.00989 -0.01232 0.00104 0.00227 PART 2 F4' 4 0.096736 0.555333 0.060564 10.50000 0.02660 0.12132 = 0.04660 -0.02134 -0.01488 0.00232 F6' 4 0.232592 0.599923 0.010696 10.50000 0.07385 0.16038 = 0.02577 0.03870 -0.00794 0.00070 F5' 4 0.225600 0.473087 0.056528 10.50000 0.06605 0.09227 = 0.07278 -0.05231 -0.03434 0.02152 C10' 1 0.201454 0.554343 0.069139 10.50000 0.05302 0.04684 = 0.04514 -0.02364 -0.00012 -0.00812 C3' 1 0.498536 0.742857 0.411044 10.50000 0.04418 0.02587 = 0.03370 0.00431 0.01123 0.00510 F9' 4 0.426165 0.820292 0.505318 10.50000 0.15337 0.04531 = 0.07665 0.00532 0.07331 0.03037 F7' 4 0.398815 0.706063 0.496211 10.50000 0.28475 0.27610 = 0.12419 -0.10665 0.14542 -0.10499 F8' 4 0.575434 0.739689 0.548214 10.50000 0.12717 0.07885 = 0.01948 0.01128 -0.01817 -0.01495 C11' 1 0.452742 0.743746 0.491022 10.50000 0.06683 0.05784 = 0.04398 -0.02627 -0.00538 0.01650 PART 0 O2 3 0.498967 0.674520 0.380019 11.00000 0.03764 0.02545 = 0.01959 -0.00276 0.00672 0.00295 HKLF 4 REM shelxt_a.res in C2/c REM R1 = 0.0296 for 3549 Fo > 4sig(Fo) and 0.0394 for all 4079 data REM 522 parameters refined using 42 restraints END WGHT 0.0110 12.4230 REM Highest difference peak 1.855, deepest hole -1.216, 1-sigma level 0.128 Q1 1 0.0000 0.6593 0.2500 10.50000 0.05 1.86 Q2 1 0.2185 0.6872 0.3891 11.00000 0.05 0.91 Q3 1 0.5000 0.5854 0.2500 10.50000 0.05 0.69 Q4 1 0.5000 0.5252 0.2500 10.50000 0.05 0.62 Q5 1 -0.0001 0.5976 0.2783 11.00000 0.05 0.56 Q6 1 0.5041 0.6540 0.3229 11.00000 0.05 0.52 Q7 1 0.5702 0.3437 0.1800 11.00000 0.05 0.52 Q8 1 0.5474 0.9435 0.2630 11.00000 0.05 0.52 Q9 1 0.1203 0.5771 0.3671 11.00000 0.05 0.50 Q10 1 0.5277 0.6407 0.2633 11.00000 0.05 0.50 Q11 1 0.5401 0.6374 0.3812 11.00000 0.05 0.48 Q12 1 0.0521 0.6146 0.2756 11.00000 0.05 0.47 Q13 1 0.5404 0.5412 0.2245 11.00000 0.05 0.46 Q14 1 0.4260 0.6263 0.1807 11.00000 0.05 0.44 Q15 1 0.4021 0.7765 0.5604 11.00000 0.05 0.43 Q16 1 0.0589 0.6797 0.2157 11.00000 0.05 0.42 Q17 1 0.4368 0.8880 0.5477 11.00000 0.05 0.42 Q18 1 0.1388 0.6502 0.2135 11.00000 0.05 0.42 Q19 1 0.2170 0.5026 -0.0302 11.00000 0.05 0.41 Q20 1 0.1311 0.5949 0.3106 11.00000 0.05 0.40 ; _shelx_res_checksum 52358 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_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 Th1 Th 0.5000 0.61366(2) 0.2500 0.01884(6) Uani 1 2 d S T P A . O4 O 0.3678(12) 0.5496(7) 0.1594(10) 0.021(2) Uani 0.5 1 d . . P A 1 O1 O 0.6250(6) 0.7257(5) 0.2682(6) 0.0237(18) Uani 0.5 1 d . . P A 1 O5 O 0.5615(5) 0.4767(8) 0.1863(7) 0.0231(19) Uani 0.5 1 d . . P A 1 O3' O 0.3333(12) 0.6232(6) 0.3048(10) 0.026(2) Uani 0.5 1 d . . P A 2 C6 C 0.2672(13) 0.5524(8) 0.1467(10) 0.026(3) Uani 0.5 1 d . U P A 1 C4 C 0.2374(11) 0.5920(7) 0.2739(7) 0.025(2) Uani 0.5 1 d . . P A 1 C5 C 0.2005(8) 0.5750(6) 0.1973(7) 0.025(2) Uani 0.5 1 d . . P A 1 H5 H 0.1278 0.5791 0.1799 0.031 Uiso 0.5 1 calc R U P A 1 C1 C 0.6457(7) 0.7857(5) 0.3159(5) 0.0277(17) Uani 0.5 1 d . . P A 1 C7' C 0.4624(7) 0.4013(5) 0.2004(4) 0.0225(17) Uani 0.5 1 d . . P A 2 H7'1 H 0.4736 0.3504 0.1699 0.027 Uiso 0.5 1 calc R U P A 2 H7'2 H 0.3868 0.4123 0.2002 0.027 Uiso 0.5 1 calc R U P A 2 C9' C 0.1703(11) 0.6632(10) 0.3378(9) 0.047(4) Uani 0.5 1 d . . P A 2 F1' F 0.1918(14) 0.6258(7) 0.4046(10) 0.070(4) Uani 0.5 1 d . U P A 2 F2' F 0.1903(6) 0.7392(4) 0.3545(4) 0.075(2) Uani 0.5 1 d . . P A 2 F3' F 0.0679(7) 0.6569(12) 0.3132(9) 0.082(4) Uani 0.5 1 d . . P A 2 F4 F 0.1240(7) 0.5153(6) 0.0519(6) 0.063(2) Uani 0.5 1 d . . P A 1 F5 F 0.2639(7) 0.4440(7) 0.0557(6) 0.063(3) Uani 0.5 1 d . . P A 1 F6 F 0.2578(13) 0.5678(9) 0.0145(9) 0.060(3) Uani 0.5 1 d . . P A 1 C10 C 0.2241(13) 0.5201(8) 0.0649(9) 0.035(3) Uani 0.5 1 d . . P A 1 F10 F 0.6958(7) 0.8743(5) 0.2182(4) 0.068(3) Uani 0.5 1 d . . P A 1 F11 F 0.7431(6) 0.9129(4) 0.3345(4) 0.0528(18) Uani 0.5 1 d . . P A 1 F12 F 0.8177(4) 0.8058(4) 0.2904(4) 0.0660(18) Uani 0.5 1 d . . P A 1 C12 C 0.7287(12) 0.8457(9) 0.2895(7) 0.035(3) Uani 0.5 1 d . . P A 1 C2 C 0.6057(7) 0.8007(6) 0.3841(5) 0.0309(19) Uani 0.5 1 d . . P A 1 H2 H 0.6245 0.8502 0.4128 0.037 Uiso 0.5 1 calc R U P A 1 C8 C 0.5675(10) 0.4772(12) 0.1040(10) 0.034(3) Uani 0.5 1 d . . P A 1 H8A H 0.6114 0.4306 0.0908 0.051 Uiso 0.5 1 calc R U P A 1 H8B H 0.5979 0.5302 0.0895 0.051 Uiso 0.5 1 calc R U P A 1 H8C H 0.4971 0.4710 0.0757 0.051 Uiso 0.5 1 calc R U P A 1 C3 C 0.5369(10) 0.7429(13) 0.4118(10) 0.027(3) Uani 0.5 1 d . . P A 1 F10' F 0.5876(7) 0.9127(4) 0.2171(4) 0.091(3) Uani 0.5 1 d . . P A 2 C1' C 0.5832(7) 0.8110(5) 0.3128(5) 0.0288(18) Uani 0.5 1 d . . P A 2 C12' C 0.6338(7) 0.8897(6) 0.2839(5) 0.0379(19) Uani 0.5 1 d . . P A 2 F11' F 0.6316(8) 0.9536(4) 0.3308(4) 0.106(3) Uani 0.5 1 d . . P A 2 C7 C 0.5237(7) 0.3983(6) 0.2123(5) 0.0297(19) Uani 0.5 1 d . . P A 1 H7A H 0.5827 0.3582 0.2178 0.036 Uiso 0.5 1 calc R U P A 1 H7B H 0.4706 0.3767 0.1709 0.036 Uiso 0.5 1 calc R U P A 1 O1' O 0.5904(6) 0.7485(5) 0.2696(5) 0.0194(16) Uani 0.5 1 d . . P A 2 C4' C 0.2360(13) 0.6301(6) 0.2783(9) 0.031(3) Uani 0.5 1 d . . P A 2 F1 F 0.1893(14) 0.5856(8) 0.3988(8) 0.073(4) Uani 0.5 1 d . U P A 1 F2 F 0.1153(10) 0.6787(10) 0.3231(7) 0.092(6) Uani 0.5 1 d . . P A 1 F3 F 0.0745(6) 0.5549(7) 0.3142(5) 0.109(3) Uani 0.5 1 d . . P A 1 C9 C 0.1589(7) 0.6079(11) 0.3328(6) 0.054(3) Uani 0.5 1 d . . P A 1 O3 O 0.3273(13) 0.5921(6) 0.3033(9) 0.023(2) Uani 0.5 1 d . . P A 1 O5' O 0.5204(5) 0.4736(8) 0.1785(7) 0.0225(18) Uani 0.5 1 d . . P A 2 C5' C 0.1899(9) 0.6123(7) 0.2017(7) 0.029(2) Uani 0.5 1 d . U P A 2 H5' H 0.1175 0.6220 0.1869 0.035 Uiso 0.5 1 calc R U P A 2 C2' C 0.5390(8) 0.8139(5) 0.3807(5) 0.0303(18) Uani 0.5 1 d . . P A 2 H2' H 0.5361 0.8657 0.4072 0.036 Uiso 0.5 1 calc R U P A 2 C8' C 0.5260(9) 0.4714(13) 0.0952(10) 0.027(3) Uani 0.5 1 d . . P A 2 H8'1 H 0.5615 0.4200 0.0821 0.040 Uiso 0.5 1 calc R U P A 2 H8'2 H 0.5651 0.5201 0.0803 0.040 Uiso 0.5 1 calc R U P A 2 H8'3 H 0.4551 0.4725 0.0670 0.040 Uiso 0.5 1 calc R U P A 2 C6' C 0.2499(12) 0.5812(8) 0.1491(10) 0.030(3) Uani 0.5 1 d . U P A 2 O4' O 0.3482(12) 0.5742(8) 0.1571(9) 0.021(2) Uani 0.5 1 d . . P A 2 F12' F 0.7304(11) 0.8766(8) 0.2758(13) 0.119(6) Uani 0.5 1 d . . P A 2 F7 F 0.4221(12) 0.6977(8) 0.5108(6) 0.055(3) Uani 0.5 1 d . . P A 1 F8 F 0.551(2) 0.7469(16) 0.5420(11) 0.173(11) Uani 0.5 1 d . . P A 1 F9 F 0.4766(11) 0.8383(7) 0.4987(8) 0.091(4) Uani 0.5 1 d . . P A 1 C11 C 0.5001(11) 0.7585(9) 0.4917(7) 0.034(3) Uani 0.5 1 d . . P A 1 F4' F 0.0967(6) 0.5553(6) 0.0606(5) 0.067(3) Uani 0.5 1 d . . P A 2 F6' F 0.2326(14) 0.5999(12) 0.0107(10) 0.088(5) Uani 0.5 1 d . . P A 2 F5' F 0.2256(10) 0.4731(9) 0.0565(7) 0.081(4) Uani 0.5 1 d . . P A 2 C10' C 0.2015(13) 0.5543(10) 0.0691(10) 0.049(4) Uani 0.5 1 d . . P A 2 C3' C 0.4985(10) 0.7429(14) 0.4110(12) 0.034(4) Uani 0.5 1 d . U P A 2 F9' F 0.4262(10) 0.8203(7) 0.5053(7) 0.087(4) Uani 0.5 1 d . . P A 2 F7' F 0.399(2) 0.7061(18) 0.4962(12) 0.218(14) Uani 0.5 1 d . . P A 2 F8' F 0.5754(14) 0.7397(9) 0.5482(8) 0.078(4) Uani 0.5 1 d . . P A 2 C11' C 0.4527(15) 0.7437(15) 0.4910(12) 0.057(5) Uani 0.5 1 d . U P A 2 O2 O 0.4990(2) 0.67452(16) 0.38002(14) 0.0273(6) Uani 1 1 d . . . . . 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 Th1 0.01846(10) 0.02242(11) 0.01664(10) 0.000 0.00610(7) 0.000 O4 0.022(6) 0.017(6) 0.024(3) -0.003(4) 0.004(4) 0.004(4) O1 0.028(5) 0.019(4) 0.027(3) -0.006(3) 0.012(4) 0.000(3) O5 0.021(4) 0.029(4) 0.021(4) 0.000(3) 0.010(4) 0.006(5) O3' 0.016(4) 0.031(6) 0.031(4) -0.012(5) 0.007(3) -0.011(5) C6 0.025(6) 0.031(7) 0.023(5) 0.002(5) 0.004(4) 0.000(5) C4 0.019(5) 0.040(7) 0.019(5) 0.006(6) 0.009(4) 0.001(6) C5 0.016(4) 0.026(6) 0.035(5) 0.010(5) 0.003(4) 0.005(5) C1 0.026(4) 0.026(5) 0.030(4) 0.004(4) 0.001(4) -0.001(4) C7' 0.026(4) 0.017(4) 0.028(4) -0.008(3) 0.016(4) -0.004(4) C9' 0.042(8) 0.044(8) 0.062(8) 0.023(7) 0.038(7) 0.018(7) F1' 0.067(5) 0.108(10) 0.040(4) -0.002(6) 0.026(4) 0.034(7) F2' 0.084(5) 0.063(5) 0.090(5) -0.033(4) 0.052(4) -0.004(4) F3' 0.024(4) 0.154(11) 0.068(5) -0.035(6) 0.009(4) 0.017(5) F4 0.042(5) 0.076(6) 0.064(5) -0.025(4) -0.016(4) 0.006(4) F5 0.064(6) 0.058(6) 0.058(4) -0.028(4) -0.028(4) 0.022(4) F6 0.073(8) 0.080(8) 0.022(4) 0.014(5) -0.012(4) -0.002(5) C10 0.051(8) 0.019(8) 0.030(6) -0.016(7) -0.011(5) 0.001(7) F10 0.101(7) 0.064(5) 0.035(3) 0.014(3) -0.005(4) -0.049(5) F11 0.077(5) 0.034(4) 0.048(4) -0.013(3) 0.013(3) -0.027(3) F12 0.039(3) 0.058(4) 0.105(5) -0.012(4) 0.025(3) -0.022(3) C12 0.040(6) 0.044(8) 0.022(4) -0.008(5) 0.005(4) -0.008(6) C2 0.036(5) 0.028(5) 0.028(5) -0.006(3) 0.004(4) -0.004(4) C8 0.050(9) 0.037(6) 0.016(6) -0.004(4) 0.011(7) -0.004(8) C3 0.037(8) 0.031(6) 0.015(4) -0.006(4) 0.007(6) 0.003(7) F10' 0.124(7) 0.068(5) 0.070(5) 0.037(4) -0.035(4) -0.055(5) C1' 0.027(4) 0.027(5) 0.032(5) 0.004(4) 0.002(4) -0.006(4) C12' 0.045(5) 0.036(5) 0.032(4) -0.007(4) 0.002(4) -0.017(4) F11' 0.202(10) 0.048(4) 0.080(5) -0.021(4) 0.068(6) -0.056(6) C7 0.023(4) 0.033(5) 0.035(5) -0.003(4) 0.008(4) -0.002(4) O1' 0.022(4) 0.021(5) 0.017(3) -0.007(3) 0.007(3) -0.003(3) C4' 0.029(6) 0.029(6) 0.038(6) -0.002(6) 0.010(4) 0.001(6) F1 0.074(6) 0.122(10) 0.031(5) 0.023(7) 0.036(4) 0.035(8) F2 0.096(13) 0.126(14) 0.065(9) 0.015(8) 0.051(10) 0.067(11) F3 0.053(5) 0.171(10) 0.115(7) 0.015(6) 0.058(5) -0.007(5) C9 0.021(5) 0.108(11) 0.034(5) 0.028(7) 0.011(4) 0.024(7) O3 0.022(4) 0.028(6) 0.019(3) -0.006(5) 0.007(3) -0.011(5) O5' 0.023(4) 0.026(4) 0.020(4) 0.000(3) 0.009(4) 0.002(5) C5' 0.018(4) 0.034(6) 0.035(4) 0.006(5) 0.003(3) 0.015(5) C2' 0.047(5) 0.023(5) 0.022(4) -0.006(3) 0.007(4) -0.005(4) C8' 0.032(7) 0.038(6) 0.011(5) -0.004(4) 0.008(6) 0.001(7) C6' 0.022(6) 0.036(7) 0.029(5) 0.004(6) -0.005(4) -0.008(5) O4' 0.021(5) 0.024(7) 0.020(3) -0.002(5) 0.006(3) 0.009(4) F12' 0.047(6) 0.078(10) 0.236(19) 0.038(12) 0.034(9) -0.023(6) F7 0.098(7) 0.049(5) 0.025(4) 0.002(3) 0.031(4) 0.025(6) F8 0.24(2) 0.25(2) 0.038(10) -0.004(10) 0.031(11) 0.129(16) F9 0.156(11) 0.053(6) 0.081(6) -0.031(5) 0.079(7) 0.001(6) C11 0.051(8) 0.041(7) 0.010(5) -0.012(4) 0.001(5) 0.002(6) F4' 0.027(4) 0.121(9) 0.047(4) -0.021(5) -0.015(3) 0.002(4) F6' 0.074(8) 0.160(16) 0.026(4) 0.039(8) -0.008(4) 0.001(8) F5' 0.066(7) 0.092(12) 0.073(6) -0.052(8) -0.034(5) 0.022(7) C10' 0.053(9) 0.047(10) 0.045(7) -0.024(8) 0.000(6) -0.008(8) C3' 0.044(8) 0.026(5) 0.034(6) 0.004(4) 0.011(7) 0.005(7) F9' 0.153(11) 0.045(6) 0.077(5) 0.005(4) 0.073(7) 0.030(6) F7' 0.28(3) 0.28(3) 0.124(16) -0.107(14) 0.145(18) -0.10(2) F8' 0.127(9) 0.079(7) 0.019(5) 0.011(4) -0.018(5) -0.015(7) C11' 0.067(9) 0.058(9) 0.044(7) -0.026(6) -0.005(7) 0.016(8) O2 0.0376(15) 0.0254(15) 0.0196(13) -0.0028(11) 0.0067(11) 0.0029(12) 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)' H H 0.0000 0.0000 '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)' Th Th -9.6991 4.1938 '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 O4 Th1 O4 129.4(5) . 2_655 ? O4 Th1 O1 79.8(3) . 2_655 ? O4 Th1 O1 144.5(4) 2_655 2_655 ? O4 Th1 O1 144.5(4) . . ? O4 Th1 O1 79.8(3) 2_655 . ? O1 Th1 O1 83.7(3) 2_655 . ? O1' Th1 O1' 57.1(3) . 2_655 ? O1' Th1 O4' 129.9(4) . . ? O1' Th1 O4' 79.0(3) 2_655 . ? O1' Th1 O4' 79.0(3) . 2_655 ? O1' Th1 O4' 129.9(4) 2_655 2_655 ? O4' Th1 O4' 150.2(5) . 2_655 ? O4 Th1 O2 133.1(4) . . ? O4 Th1 O2 69.8(4) 2_655 . ? O1 Th1 O2 75.1(2) 2_655 . ? O1 Th1 O2 70.6(2) . . ? O1' Th1 O2 65.4(2) . . ? O1' Th1 O2 73.8(2) 2_655 . ? O4' Th1 O2 127.3(3) . . ? O4' Th1 O2 66.2(4) 2_655 . ? O4 Th1 O2 69.8(4) . 2_655 ? O4 Th1 O2 133.1(4) 2_655 2_655 ? O1 Th1 O2 70.6(2) 2_655 2_655 ? O1 Th1 O2 75.1(2) . 2_655 ? O1' Th1 O2 73.8(2) . 2_655 ? O1' Th1 O2 65.4(2) 2_655 2_655 ? O4' Th1 O2 66.2(4) . 2_655 ? O4' Th1 O2 127.3(3) 2_655 2_655 ? O2 Th1 O2 133.37(12) . 2_655 ? O1' Th1 O3' 108.4(2) . . ? O1' Th1 O3' 64.9(3) 2_655 . ? O4' Th1 O3' 66.8(5) . . ? O4' Th1 O3' 115.2(5) 2_655 . ? O2 Th1 O3' 60.9(3) . . ? O2 Th1 O3' 115.9(4) 2_655 . ? O1' Th1 O3' 64.9(3) . 2_655 ? O1' Th1 O3' 108.4(2) 2_655 2_655 ? O4' Th1 O3' 115.2(5) . 2_655 ? O4' Th1 O3' 66.8(5) 2_655 2_655 ? O2 Th1 O3' 115.9(4) . 2_655 ? O2 Th1 O3' 60.9(3) 2_655 2_655 ? O3' Th1 O3' 172.9(4) . 2_655 ? C6 O4 Th1 135.6(11) . . ? C1 O1 Th1 136.7(7) . . ? C7 O5 C8 112.3(11) . . ? C7 O5 Th1 117.5(6) . . ? C8 O5 Th1 118.1(10) . . ? C4' O3' Th1 136.7(13) . . ? O4 C6 C5 127.5(16) . . ? O4 C6 C10 112.4(14) . . ? C5 C6 C10 120.0(14) . . ? O3 C4 C5 127.0(13) . . ? O3 C4 C9 113.3(12) . . ? C5 C4 C9 119.6(11) . . ? C6 C5 C4 120.4(12) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? O1 C1 C2 128.5(8) . . ? O1 C1 C12 111.7(8) . . ? C2 C1 C12 119.8(8) . . ? O5' C7' C7' 90.9(6) . 2_655 ? O5' C7' H7'1 113.5 . . ? C7' C7' H7'1 113.5 2_655 . ? O5' C7' H7'2 113.5 . . ? C7' C7' H7'2 113.5 2_655 . ? H7'1 C7' H7'2 110.8 . . ? F2' C9' F1' 102.8(15) . . ? F2' C9' F3' 108.0(12) . . ? F1' C9' F3' 109.8(15) . . ? F2' C9' C4' 112.0(10) . . ? F1' C9' C4' 111.8(12) . . ? F3' C9' C4' 111.9(16) . . ? F6 C10 F4 109.8(13) . . ? F6 C10 F5 107.0(15) . . ? F4 C10 F5 108.5(12) . . ? F6 C10 C6 108.4(13) . . ? F4 C10 C6 114.5(13) . . ? F5 C10 C6 108.4(11) . . ? F12 C12 F11 109.3(11) . . ? F12 C12 F10 110.6(10) . . ? F11 C12 F10 105.7(11) . . ? F12 C12 C1 109.4(10) . . ? F11 C12 C1 112.2(9) . . ? F10 C12 C1 109.6(10) . . ? C1 C2 C3 120.2(10) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? O5 C8 H8A 109.5 . . ? O5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O2 C3 C2 129.1(13) . . ? O2 C3 C11 112.2(13) . . ? C2 C3 C11 118.8(14) . . ? O1' C1' C2' 127.4(8) . . ? O1' C1' C12' 112.9(8) . . ? C2' C1' C12' 119.6(8) . . ? F10' C12' F12' 106.8(12) . . ? F10' C12' F11' 107.1(9) . . ? F12' C12' F11' 107.1(11) . . ? F10' C12' C1' 111.2(7) . . ? F12' C12' C1' 111.2(9) . . ? F11' C12' C1' 113.2(7) . . ? O5 C7 C7 117.5(6) . 2_655 ? O5 C7 H7A 107.9 . . ? C7 C7 H7A 107.9 2_655 . ? O5 C7 H7B 107.9 . . ? C7 C7 H7B 107.9 2_655 . ? H7A C7 H7B 107.2 . . ? C1' O1' Th1 135.2(6) . . ? O3' C4' C5' 126.3(14) . . ? O3' C4' C9' 113.2(15) . . ? C5' C4' C9' 120.4(14) . . ? F1 C9 F2 118.1(14) . . ? F1 C9 F3 100.9(14) . . ? F2 C9 F3 101.2(9) . . ? F1 C9 C4 114.5(11) . . ? F2 C9 C4 112.1(11) . . ? F3 C9 C4 107.9(11) . . ? C4 O3 Th1 133.4(11) . . ? C7' O5' C8' 109.4(10) . . ? C7' O5' Th1 118.4(6) . . ? C8' O5' Th1 121.2(10) . . ? C6' C5' C4' 119.8(12) . . ? C6' C5' H5' 120.1 . . ? C4' C5' H5' 120.1 . . ? C1' C2' C3' 121.2(11) . . ? C1' C2' H2' 119.4 . . ? C3' C2' H2' 119.4 . . ? O5' C8' H8'1 109.5 . . ? O5' C8' H8'2 109.5 . . ? H8'1 C8' H8'2 109.5 . . ? O5' C8' H8'3 109.5 . . ? H8'1 C8' H8'3 109.5 . . ? H8'2 C8' H8'3 109.5 . . ? O4' C6' C5' 127.3(16) . . ? O4' C6' C10' 111.6(15) . . ? C5' C6' C10' 121.0(13) . . ? C6' O4' Th1 139.1(12) . . ? F8 C11 F9 102.9(18) . . ? F8 C11 F7 93.9(18) . . ? F9 C11 F7 116.6(11) . . ? F8 C11 C3 119.6(18) . . ? F9 C11 C3 109.8(13) . . ? F7 C11 C3 113.3(11) . . ? F4' C10' F6' 107.6(14) . . ? F4' C10' F5' 104.0(14) . . ? F6' C10' F5' 107.3(16) . . ? F4' C10' C6' 113.1(13) . . ? F6' C10' C6' 114.1(16) . . ? F5' C10' C6' 110.0(14) . . ? O2 C3' C2' 123.0(15) . . ? O2 C3' C11' 114.9(17) . . ? C2' C3' C11' 122.1(17) . . ? F7' C11' F9' 112(2) . . ? F7' C11' C3' 117(2) . . ? F9' C11' C3' 108(2) . . ? F7' C11' F8' 123(3) . . ? F9' C11' F8' 99.6(14) . . ? C3' C11' F8' 94.8(13) . . ? C3' O2 Th1 139.6(10) . . ? C3 O2 Th1 132.9(8) . . ? 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 Th1 O4 2.394(17) . ? Th1 O4 2.394(17) 2_655 ? Th1 O1 2.403(10) 2_655 ? Th1 O1 2.403(10) . ? Th1 O1' 2.452(9) . ? Th1 O1' 2.452(9) 2_655 ? Th1 O4' 2.452(17) . ? Th1 O4' 2.452(17) 2_655 ? Th1 O2 2.457(2) . ? Th1 O2 2.457(2) 2_655 ? Th1 O3' 2.464(16) . ? Th1 O3' 2.464(16) 2_655 ? O4 C6 1.29(2) . ? O1 C1 1.271(13) . ? O5 C7 1.437(15) . ? O5 C8 1.44(2) . ? O3' C4' 1.28(2) . ? C6 C5 1.354(19) . ? C6 C10 1.54(2) . ? C4 O3 1.21(2) . ? C4 C5 1.380(17) . ? C4 C9 1.548(15) . ? C5 H5 0.9500 . ? C1 C2 1.371(12) . ? C1 C12 1.550(15) . ? C7' O5' 1.452(14) . ? C7' C7' 1.864(17) 2_655 ? C7' H7'1 0.9900 . ? C7' H7'2 0.9900 . ? C9' F2' 1.266(18) . ? C9' F1' 1.30(2) . ? C9' F3' 1.34(2) . ? C9' C4' 1.513(18) . ? F4 C10 1.284(19) . ? F5 C10 1.337(15) . ? F6 C10 1.28(2) . ? F10 C12 1.336(18) . ? F11 C12 1.326(16) . ? F12 C12 1.312(17) . ? C2 C3 1.41(2) . ? C2 H2 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C3 O2 1.291(19) . ? C3 C11 1.54(2) . ? F10' C12' 1.287(10) . ? C1' O1' 1.259(12) . ? C1' C2' 1.373(12) . ? C1' C12' 1.531(12) . ? C12' F12' 1.289(16) . ? C12' F11' 1.307(10) . ? C7 C7 1.512(16) 2_655 ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C4' C5' 1.41(2) . ? F1 C9 1.215(19) . ? F2 C9 1.26(2) . ? F3 C9 1.385(17) . ? O5' C8' 1.46(2) . ? C5' C6' 1.364(19) . ? C5' H5' 0.9500 . ? C2' C3' 1.38(2) . ? C2' H2' 0.9500 . ? C8' H8'1 0.9800 . ? C8' H8'2 0.9800 . ? C8' H8'3 0.9800 . ? C6' O4' 1.26(2) . ? C6' C10' 1.51(2) . ? F7 C11 1.47(2) . ? F8 C11 1.04(2) . ? F9 C11 1.319(18) . ? F4' C10' 1.34(2) . ? F6' C10' 1.35(3) . ? F5' C10' 1.359(15) . ? C3' O2 1.22(2) . ? C3' C11' 1.58(3) . ? F9' C11' 1.30(2) . ? F7' C11' 0.93(4) . ? F8' C11' 1.76(3) . ?