#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:26:15 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223509 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234437.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_7234437 loop_ _publ_author_name 'Wang, Juan' 'Yang, Mingfang' 'Sun, Juan' 'Li, Hui' 'Liu, Jinjin' 'Wang, Qinglun' 'Li, Licun' 'Ma, Yue' 'Zhao, Bin' 'Cheng, Peng' _publ_section_title ; Enhancing the energy barrier of dysprosium(iii) single-molecule magnets by tuning the magnetic interactions through different N-oxide bridging ligands ; _journal_issue 41 _journal_name_full CrystEngComm _journal_page_first 6219 _journal_paper_doi 10.1039/C9CE01378D _journal_volume 21 _journal_year 2019 _chemical_formula_moiety 'C25 H11 F18 N2 O8 Tb' _chemical_formula_sum 'C25 H11 F18 N2 O8 Tb' _chemical_formula_weight 968.28 _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' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2014/7 _audit_update_record ; 2019-04-03 deposited with the CCDC. 2019-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 123.945(5) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 24.768(8) _cell_length_b 15.634(4) _cell_length_c 19.349(6) _cell_measurement_reflns_used 12101 _cell_measurement_temperature 113 _cell_measurement_theta_max 27.9 _cell_measurement_theta_min 1.6 _cell_volume 6215(3) _computing_cell_refinement ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_collection ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_data_reduction ; CrystalClear-SM Expert 2.1 b42 (Rigaku, 2015) ; _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _diffrn_ambient_temperature 113 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Rigaku Pilatus 200K' _diffrn_measurement_method 'profile data from \w-scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_unetI/netI 0.0289 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_number 31818 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 1.637 _exptl_absorpt_coefficient_mu 2.435 _exptl_absorpt_correction_T_max 0.784 _exptl_absorpt_correction_T_min 0.652 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.069 _exptl_crystal_description block _exptl_crystal_F_000 3728 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 2.115 _refine_diff_density_min -0.884 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.971 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 487 _refine_ls_number_reflns 5489 _refine_ls_number_restraints 24 _refine_ls_restrained_S_all 0.983 _refine_ls_R_factor_all 0.0769 _refine_ls_R_factor_gt 0.0758 _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^)+(0.1000P)^2^+450.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2162 _refine_ls_wR_factor_ref 0.2169 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5359 _reflns_number_total 5489 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01378d2.cif _cod_data_source_block shelx _cod_depositor_comments 'Adding full bibliography for 7234434--7234439.cif.' _cod_original_cell_volume 6216(3) _cod_database_code 7234437 _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_res_file ; shelx.res created by SHELXL-2014/7 TITL shelx in C2/c CELL 0.71073 24.7682 15.6341 19.3492 90 123.945 90 ZERR 8 0.0081 0.0043 0.0063 0 0.005 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O Tb UNIT 200 88 144 16 64 8 ISOR 0.01 0.02 F5 ISOR 0.01 0.02 F6 ISOR 0.01 0.02 C15 ISOR 0.01 0.02 F16 L.S. 4 PLAN 50 TEMP 113.15 FREE F16 F17 BOND fmap 2 acta OMIT -3 50.02 REM REM REM WGHT 0.100000 450.000000 FVAR 1.52788 TB1 6 0.053912 0.787108 0.101140 11.00000 0.02645 0.03856 = 0.02157 -0.00271 0.01537 -0.00480 O2 5 0.068166 0.671101 0.189006 11.00000 0.03832 0.06692 = 0.02779 0.01127 0.01575 -0.00649 O1 5 -0.029920 0.685437 0.019725 11.00000 0.03498 0.03258 = 0.03175 0.00338 0.01841 -0.00714 O3 5 0.079727 0.719204 0.015092 11.00000 0.03530 0.03027 = 0.02666 -0.00532 0.01801 0.00166 O6 5 0.102749 0.886434 0.212003 11.00000 0.02992 0.04911 = 0.03742 -0.01856 0.01690 0.00102 O5 5 0.110907 0.887538 0.072532 11.00000 0.03662 0.02639 = 0.03758 0.00020 0.02224 -0.00823 O4 5 0.166875 0.749837 0.185919 11.00000 0.03265 0.04193 = 0.02346 -0.00054 0.01481 0.00161 C8 1 0.195142 0.708485 0.091928 11.00000 0.03575 0.03956 = 0.03833 0.00236 0.02181 0.01386 AFIX 43 H8 2 0.229915 0.696665 0.087534 11.00000 -1.20000 AFIX 0 C7 1 0.131683 0.700889 0.022086 11.00000 0.03556 0.03721 = 0.03768 -0.01244 0.02156 0.00501 F11 3 0.296603 0.673355 0.292166 11.00000 0.06222 0.07172 = 0.05066 0.02469 0.01263 0.02181 F3 3 -0.097884 0.483567 -0.043164 11.00000 0.10309 0.03323 = 0.10150 0.00790 -0.01816 -0.03271 C9 1 0.207094 0.733783 0.168794 11.00000 0.03445 0.02895 = 0.03726 0.01107 0.02041 0.00800 F9 3 0.168932 0.617833 -0.046369 11.00000 0.09586 0.18168 = 0.05579 -0.01266 0.03453 0.08613 C1 1 -0.097153 0.569501 -0.046886 11.00000 0.05263 0.05199 = 0.10043 0.03772 0.00264 -0.01163 F7 3 0.129338 0.739709 -0.098238 11.00000 0.09014 0.13550 = 0.04996 -0.00923 0.04409 -0.03243 F6 3 0.145397 0.535072 0.279701 11.00000 0.08434 0.15745 = 0.15803 0.08878 0.00002 -0.01263 C10 1 0.278017 0.739692 0.243363 11.00000 0.03836 0.02746 = 0.04475 -0.00234 0.01445 -0.00134 C6 1 0.125072 0.672711 -0.059687 11.00000 0.04758 0.06839 = 0.04036 -0.00637 0.02588 0.01730 F10 3 0.319193 0.749283 0.221739 11.00000 0.03351 0.20908 = 0.05073 0.02313 0.01644 -0.00212 C3 1 -0.001874 0.560768 0.100562 11.00000 0.06337 0.05740 = 0.08047 0.03161 -0.00169 -0.02988 AFIX 43 H3 2 -0.011041 0.502692 0.097670 11.00000 -1.20000 AFIX 0 C4 1 0.047626 0.594106 0.175096 11.00000 0.05296 0.06301 = 0.05224 0.02979 0.01424 -0.01372 C2 1 -0.037898 0.608815 0.031118 11.00000 0.04304 0.03653 = 0.04846 0.01350 0.00835 -0.01077 F2 3 -0.151923 0.596861 -0.056169 11.00000 0.04432 0.07533 = 0.13306 0.03301 -0.00165 -0.02365 F8 3 0.066514 0.638811 -0.113774 11.00000 0.07244 0.05440 = 0.04006 -0.02386 0.02884 -0.00279 F5 3 0.081072 0.571003 0.312465 11.00000 0.20063 0.13917 = 0.05540 0.03966 0.03217 -0.04244 C14 1 0.147495 0.938551 0.237244 11.00000 0.03163 0.06155 = 0.04373 -0.02515 0.01389 0.00280 C15 1 0.173190 0.975876 0.324358 11.00000 0.04992 0.05968 = 0.06299 -0.03529 0.02068 -0.00819 F1 3 -0.100039 0.588568 -0.115953 11.00000 0.09869 0.04742 = 0.05144 0.01151 -0.01306 -0.01556 C12 1 0.156032 0.939008 0.118658 11.00000 0.04195 0.03599 = 0.05843 0.00166 0.03046 -0.00664 C13 1 0.175802 0.968578 0.199491 11.00000 0.04022 0.03010 = 0.06176 -0.01256 0.01327 -0.01113 AFIX 43 H13 2 0.208721 1.009182 0.226459 11.00000 -1.20000 AFIX 0 F4 3 0.062813 0.455440 0.238043 11.00000 0.11591 0.09258 = 0.10605 0.07006 0.00746 -0.02827 F13 3 0.150057 0.994673 -0.000848 11.00000 0.12099 0.17229 = 0.07656 -0.04758 0.06760 -0.09446 C11 1 0.191691 0.971919 0.080626 11.00000 0.06547 0.06433 = 0.11964 -0.02288 0.06116 -0.03132 C5 1 0.083870 0.538445 0.251086 11.00000 0.07077 0.12700 = 0.07167 0.05026 -0.00222 -0.04523 F15 3 0.233729 0.909894 0.090087 11.00000 0.19594 0.05956 = 0.33813 -0.03042 0.23825 -0.02520 F12 3 0.287721 0.806256 0.289911 11.00000 0.04923 0.07106 = 0.10583 -0.03100 -0.00220 0.00314 F14 3 0.227365 1.040434 0.116739 11.00000 0.05676 0.05937 = 0.12347 0.00900 0.03699 -0.02442 F16 3 0.177140 1.058512 0.324767 11.00000 0.23755 0.12070 = 0.13749 -0.05286 0.12109 -0.05305 F17 3 0.220704 0.936093 0.382092 11.00000 0.09600 0.22804 = 0.04848 -0.04108 0.02152 0.04749 F18 3 0.129140 0.967620 0.346357 11.00000 0.07076 0.21359 = 0.07200 -0.07060 0.03645 -0.01636 O8 5 -0.023786 0.827039 0.127602 11.00000 0.02895 0.04883 = 0.03171 -0.00189 0.02233 -0.00523 N2 4 -0.085806 0.803676 0.090793 11.00000 0.03207 0.01914 = 0.03185 -0.00171 0.02451 -0.00192 C21 1 -0.129053 0.810381 0.009450 11.00000 0.03321 0.06855 = 0.03489 0.01879 0.02120 0.00094 AFIX 43 H21 2 -0.115611 0.830088 -0.023987 11.00000 -1.20000 AFIX 0 C23 1 -0.215098 0.760103 0.018877 11.00000 0.03196 0.03320 = 0.03629 0.00537 0.02366 0.00271 C22 1 -0.192803 0.789140 -0.026586 11.00000 0.03171 0.07291 = 0.03457 0.00639 0.01901 -0.01358 AFIX 43 H22 2 -0.221700 0.794781 -0.083953 11.00000 -1.20000 AFIX 0 C25 1 -0.104786 0.773500 0.139053 11.00000 0.04741 0.08512 = 0.03568 0.01023 0.02451 -0.01578 AFIX 43 H25 2 -0.074687 0.767036 0.196082 11.00000 -1.20000 AFIX 0 C24 1 -0.168137 0.752514 0.104082 11.00000 0.03781 0.14704 = 0.03643 0.00183 0.02737 -0.03089 AFIX 43 H24 2 -0.180707 0.732288 0.138281 11.00000 -1.20000 AFIX 0 O7 5 -0.022705 0.868290 -0.017789 11.00000 0.03156 0.03922 = 0.02586 0.00427 0.02250 -0.00361 N1 4 -0.018865 0.872012 -0.083659 11.00000 0.02504 0.04020 = 0.01537 -0.00253 0.01246 -0.00221 C16 1 -0.033118 0.804135 -0.131573 11.00000 0.02815 0.01449 = 0.02879 0.00575 0.01591 -0.00325 AFIX 43 H16 2 -0.047654 0.754333 -0.120688 11.00000 -1.20000 AFIX 0 C20 1 -0.001045 0.948973 -0.102202 11.00000 0.02853 0.01794 = 0.02678 0.00030 0.02135 -0.00241 AFIX 43 H20 2 0.006342 0.997688 -0.070478 11.00000 -1.20000 AFIX 0 C18 1 -0.004728 0.879440 -0.215638 11.00000 0.02574 0.03058 = 0.01655 -0.00392 0.01292 -0.00244 C19 1 0.005314 0.951275 -0.167795 11.00000 0.03182 0.01236 = 0.02642 -0.00500 0.02028 -0.00516 AFIX 43 H19 2 0.016720 1.002528 -0.180820 11.00000 -1.20000 AFIX 0 C17 1 -0.026452 0.807007 -0.197975 11.00000 0.03811 0.01551 = 0.02137 -0.00414 0.01649 -0.00318 AFIX 43 H17 2 -0.036896 0.758875 -0.231415 11.00000 -1.20000 AFIX 0 HKLF 4 REM shelx in C2/c REM R1 = 0.0758 for 5359 Fo > 4sig(Fo) and 0.0769 for all 5490 data REM 487 parameters refined using 24 restraints END WGHT 0.0000 238.8223 REM Highest difference peak 2.115, deepest hole -0.884, 1-sigma level 0.166 Q1 1 0.2406 1.0267 0.3464 11.00000 0.05 2.12 Q2 1 0.3352 0.8606 0.1947 11.00000 0.05 1.50 Q3 1 0.1445 0.5832 0.3238 11.00000 0.05 1.13 Q4 1 0.1532 0.5198 0.2539 11.00000 0.05 1.04 Q5 1 0.3095 0.6657 0.2490 11.00000 0.05 0.89 Q6 1 0.0585 0.6065 0.3211 11.00000 0.05 0.84 Q7 1 0.1503 1.0748 0.2877 11.00000 0.05 0.81 Q8 1 0.1776 0.9028 -0.0007 11.00000 0.05 0.79 Q9 1 0.0944 0.7954 0.1292 11.00000 0.05 0.77 Q10 1 0.1790 0.9411 0.3585 11.00000 0.05 0.75 Q11 1 0.1028 0.5537 0.3103 11.00000 0.05 0.70 Q12 1 0.2295 0.9629 0.0380 11.00000 0.05 0.69 Q13 1 0.2159 1.0774 0.2677 11.00000 0.05 0.69 Q14 1 0.3224 0.6766 0.1838 11.00000 0.05 0.68 Q15 1 0.2368 1.0006 0.0756 11.00000 0.05 0.63 Q16 1 0.0629 0.5978 0.1121 11.00000 0.05 0.61 Q17 1 0.0218 0.6178 -0.2130 11.00000 0.05 0.61 Q18 1 0.2957 0.7952 0.2273 11.00000 0.05 0.60 Q19 1 0.0511 0.6844 0.0975 11.00000 0.05 0.60 Q20 1 0.1185 0.7422 0.0682 11.00000 0.05 0.57 Q21 1 -0.0010 0.9166 -0.0874 11.00000 0.05 0.57 Q22 1 0.1212 0.6222 0.3188 11.00000 0.05 0.57 Q23 1 0.1695 0.4843 -0.0508 11.00000 0.05 0.54 Q24 1 0.2021 1.0393 0.3553 11.00000 0.05 0.53 Q25 1 0.2770 0.7520 0.3045 11.00000 0.05 0.53 Q26 1 0.2152 0.6343 0.0668 11.00000 0.05 0.52 Q27 1 0.0824 0.6669 0.0309 11.00000 0.05 0.50 Q28 1 0.0351 0.6843 0.2007 11.00000 0.05 0.49 Q29 1 -0.0289 0.6624 -0.1189 11.00000 0.05 0.48 Q30 1 0.0481 0.4998 0.2607 11.00000 0.05 0.48 Q31 1 -0.0006 0.5623 0.1414 11.00000 0.05 0.47 Q32 1 -0.0141 0.6650 -0.1907 11.00000 0.05 0.47 Q33 1 0.2841 0.9620 0.0889 11.00000 0.05 0.47 Q34 1 -0.1403 0.7655 0.1646 11.00000 0.05 0.46 Q35 1 0.2079 0.7600 0.1159 11.00000 0.05 0.46 Q36 1 0.0927 0.8837 0.0248 11.00000 0.05 0.46 Q37 1 0.2483 0.9147 0.1227 11.00000 0.05 0.45 Q38 1 -0.0922 0.7772 -0.0147 11.00000 0.05 0.45 Q39 1 0.0046 0.4751 0.1831 11.00000 0.05 0.45 Q40 1 0.0496 0.6340 -0.0368 11.00000 0.05 0.45 Q41 1 0.1076 0.7574 -0.0084 11.00000 0.05 0.45 Q42 1 0.1688 0.7398 -0.1100 11.00000 0.05 0.45 Q43 1 -0.1055 0.9173 -0.1179 11.00000 0.05 0.45 Q44 1 0.1974 0.9832 0.3086 11.00000 0.05 0.45 Q45 1 -0.1376 0.5629 -0.0618 11.00000 0.05 0.43 Q46 1 -0.1872 0.6419 0.0338 11.00000 0.05 0.43 Q47 1 0.0135 0.7600 -0.2106 11.00000 0.05 0.43 Q48 1 -0.0226 0.9528 -0.1499 11.00000 0.05 0.43 Q49 1 0.3471 0.6156 0.3253 11.00000 0.05 0.43 Q50 1 0.2988 0.7225 0.3019 11.00000 0.05 0.43 ; _shelx_res_checksum 34223 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 Tb1 Tb 0.05391(3) 0.78711(4) 0.10114(3) 0.0278(2) Uani 1 1 d . . O2 O 0.0682(4) 0.6711(7) 0.1890(5) 0.046(2) Uani 1 1 d . . O1 O -0.0299(4) 0.6854(5) 0.0197(5) 0.0332(19) Uani 1 1 d . . O3 O 0.0797(4) 0.7192(5) 0.0151(5) 0.0304(18) Uani 1 1 d . . O6 O 0.1027(4) 0.8864(6) 0.2120(5) 0.040(2) Uani 1 1 d . . O5 O 0.1109(4) 0.8875(5) 0.0725(5) 0.0327(19) Uani 1 1 d . . O4 O 0.1669(4) 0.7498(6) 0.1859(5) 0.0331(19) Uani 1 1 d . . C8 C 0.1951(6) 0.7085(9) 0.0919(8) 0.037(3) Uani 1 1 d . . H8 H 0.2299 0.6967 0.0875 0.045 Uiso 1 1 calc R U C7 C 0.1317(6) 0.7009(8) 0.0221(8) 0.036(3) Uani 1 1 d . . F11 F 0.2966(5) 0.6734(7) 0.2922(6) 0.072(3) Uani 1 1 d . . F3 F -0.0979(6) 0.4836(6) -0.0432(8) 0.120(6) Uani 1 1 d . . C9 C 0.2071(6) 0.7338(8) 0.1688(8) 0.033(3) Uani 1 1 d . . F9 F 0.1689(6) 0.6178(10) -0.0464(7) 0.115(6) Uani 1 1 d . . C1 C -0.0972(9) 0.5695(12) -0.0469(15) 0.090(8) Uani 1 1 d . . F7 F 0.1293(6) 0.7397(9) -0.0982(6) 0.089(4) Uani 1 1 d . . F6 F 0.1454(8) 0.5351(13) 0.2797(12) 0.170(8) Uani 1 1 d . U C10 C 0.2780(7) 0.7397(8) 0.2434(9) 0.042(3) Uani 1 1 d . . C6 C 0.1251(7) 0.6727(11) -0.0597(9) 0.051(4) Uani 1 1 d . . F10 F 0.3192(5) 0.7493(11) 0.2217(6) 0.102(5) Uani 1 1 d . . C3 C -0.0019(9) 0.5608(12) 0.1006(12) 0.090(8) Uani 1 1 d . . H3 H -0.0110 0.5027 0.0977 0.108 Uiso 1 1 calc R U C4 C 0.0476(8) 0.5941(12) 0.1751(10) 0.064(5) Uani 1 1 d . . C2 C -0.0379(7) 0.6088(9) 0.0311(9) 0.052(4) Uani 1 1 d . . F2 F -0.1519(5) 0.5969(8) -0.0562(9) 0.112(5) Uani 1 1 d . . F8 F 0.0665(5) 0.6388(6) -0.1138(5) 0.057(2) Uani 1 1 d . . F5 F 0.0811(10) 0.5710(12) 0.3125(9) 0.153(7) Uani 1 1 d . U C14 C 0.1475(7) 0.9386(11) 0.2372(9) 0.050(4) Uani 1 1 d . . C15 C 0.1732(8) 0.9759(12) 0.3244(11) 0.063(4) Uani 1 1 d . U F1 F -0.1000(6) 0.5886(7) -0.1160(6) 0.096(5) Uani 1 1 d . . C12 C 0.1560(7) 0.9390(9) 0.1187(9) 0.044(3) Uani 1 1 d . . C13 C 0.1758(7) 0.9686(9) 0.1995(10) 0.052(4) Uani 1 1 d . . H13 H 0.2087 1.0092 0.2265 0.063 Uiso 1 1 calc R U F4 F 0.0628(7) 0.4554(9) 0.2380(9) 0.134(7) Uani 1 1 d . . F13 F 0.1501(7) 0.9947(11) -0.0008(8) 0.117(6) Uani 1 1 d . . C11 C 0.1917(10) 0.9719(13) 0.0806(16) 0.078(6) Uani 1 1 d . . C5 C 0.0839(11) 0.5384(18) 0.2511(15) 0.113(11) Uani 1 1 d . . F15 F 0.2337(9) 0.9099(8) 0.0901(14) 0.150(8) Uani 1 1 d . . F12 F 0.2877(5) 0.8063(7) 0.2899(8) 0.100(5) Uani 1 1 d . . F14 F 0.2274(5) 1.0404(7) 0.1167(8) 0.087(4) Uani 1 1 d . . F16 F 0.1771(11) 1.0585(12) 0.3248(12) 0.156(7) Uani 1 1 d . U F17 F 0.2207(7) 0.9361(13) 0.3821(7) 0.134(7) Uani 1 1 d . . F18 F 0.1291(6) 0.9676(12) 0.3464(8) 0.121(6) Uani 1 1 d . . O8 O -0.0238(4) 0.8270(6) 0.1276(5) 0.0336(19) Uani 1 1 d . . N2 N -0.0858(5) 0.8037(6) 0.0908(6) 0.024(2) Uani 1 1 d . . C21 C -0.1291(6) 0.8104(10) 0.0095(8) 0.044(3) Uani 1 1 d . . H21 H -0.1156 0.8301 -0.0240 0.053 Uiso 1 1 calc R U C23 C -0.2151(6) 0.7601(8) 0.0189(8) 0.031(3) Uani 1 1 d . . C22 C -0.1928(6) 0.7891(10) -0.0266(9) 0.046(4) Uani 1 1 d . . H22 H -0.2217 0.7948 -0.0840 0.055 Uiso 1 1 calc R U C25 C -0.1048(8) 0.7735(12) 0.1391(9) 0.055(4) Uani 1 1 d . . H25 H -0.0747 0.7670 0.1961 0.066 Uiso 1 1 calc R U C24 C -0.1681(7) 0.7525(15) 0.1041(9) 0.070(6) Uani 1 1 d . . H24 H -0.1807 0.7323 0.1383 0.084 Uiso 1 1 calc R U O7 O -0.0227(4) 0.8683(5) -0.0178(5) 0.0287(17) Uani 1 1 d . . N1 N -0.0189(4) 0.8720(7) -0.0837(5) 0.026(2) Uani 1 1 d . . C16 C -0.0331(5) 0.8041(6) -0.1316(7) 0.024(2) Uani 1 1 d . . H16 H -0.0477 0.7543 -0.1207 0.029 Uiso 1 1 calc R U C20 C -0.0010(5) 0.9490(7) -0.1022(6) 0.021(2) Uani 1 1 d . . H20 H 0.0063 0.9977 -0.0705 0.025 Uiso 1 1 calc R U C18 C -0.0047(5) 0.8794(7) -0.2156(6) 0.024(2) Uani 1 1 d . . C19 C 0.0053(5) 0.9513(6) -0.1678(7) 0.021(2) Uani 1 1 d . . H19 H 0.0167 1.0025 -0.1808 0.026 Uiso 1 1 calc R U C17 C -0.0265(6) 0.8070(7) -0.1980(7) 0.025(2) Uani 1 1 d . . H17 H -0.0369 0.7589 -0.2314 0.030 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0264(3) 0.0386(4) 0.0216(3) -0.0027(2) 0.0154(2) -0.0048(2) O2 0.038(5) 0.067(7) 0.028(4) 0.011(4) 0.016(4) -0.006(5) O1 0.035(4) 0.033(5) 0.032(4) 0.003(4) 0.018(4) -0.007(4) O3 0.035(4) 0.030(4) 0.027(4) -0.005(3) 0.018(4) 0.002(4) O6 0.030(4) 0.049(6) 0.037(5) -0.019(4) 0.017(4) 0.001(4) O5 0.037(4) 0.026(4) 0.038(5) 0.000(4) 0.022(4) -0.008(4) O4 0.033(4) 0.042(5) 0.023(4) -0.001(4) 0.015(4) 0.002(4) C8 0.036(7) 0.040(7) 0.038(7) 0.002(6) 0.022(6) 0.014(6) C7 0.036(7) 0.037(7) 0.038(7) -0.012(6) 0.022(6) 0.005(5) F11 0.062(6) 0.072(7) 0.051(5) 0.025(5) 0.013(5) 0.022(5) F3 0.103(9) 0.033(5) 0.101(9) 0.008(6) -0.018(7) -0.033(6) C9 0.034(6) 0.029(7) 0.037(7) 0.011(5) 0.020(6) 0.008(5) F9 0.096(8) 0.182(14) 0.056(6) -0.013(7) 0.035(6) 0.086(9) C1 0.053(11) 0.052(11) 0.100(16) 0.038(11) 0.003(10) -0.012(9) F7 0.090(8) 0.135(11) 0.050(6) -0.009(7) 0.044(6) -0.032(8) F6 0.084(9) 0.157(13) 0.158(13) 0.089(11) 0.000(8) -0.013(9) C10 0.038(7) 0.027(7) 0.045(8) -0.002(6) 0.014(6) -0.001(6) C6 0.048(8) 0.068(10) 0.040(8) -0.006(8) 0.026(7) 0.017(8) F10 0.034(5) 0.209(15) 0.051(6) 0.023(8) 0.016(4) -0.002(7) C3 0.063(11) 0.057(11) 0.080(13) 0.032(10) -0.002(10) -0.030(9) C4 0.053(9) 0.063(11) 0.052(9) 0.030(8) 0.014(8) -0.014(8) C2 0.043(8) 0.037(8) 0.048(8) 0.014(7) 0.008(7) -0.011(6) F2 0.044(6) 0.075(8) 0.133(11) 0.033(8) -0.002(6) -0.024(6) F8 0.072(6) 0.054(5) 0.040(4) -0.024(4) 0.029(4) -0.003(5) F5 0.201(15) 0.139(12) 0.055(7) 0.040(8) 0.032(8) -0.042(11) C14 0.032(7) 0.062(10) 0.044(8) -0.025(7) 0.014(6) 0.003(7) C15 0.050(7) 0.060(8) 0.063(8) -0.035(6) 0.021(6) -0.008(6) F1 0.099(9) 0.047(6) 0.051(6) 0.012(5) -0.013(6) -0.016(6) C12 0.042(7) 0.036(7) 0.058(9) 0.002(7) 0.030(7) -0.007(6) C13 0.040(8) 0.030(7) 0.062(10) -0.013(7) 0.013(7) -0.011(6) F4 0.116(11) 0.093(10) 0.106(10) 0.070(8) 0.007(8) -0.028(8) F13 0.121(11) 0.172(15) 0.077(8) -0.048(9) 0.068(8) -0.094(11) C11 0.065(11) 0.064(12) 0.120(18) -0.023(12) 0.061(13) -0.031(10) C5 0.071(14) 0.13(2) 0.072(14) 0.050(15) -0.002(11) -0.045(14) F15 0.196(16) 0.060(7) 0.34(3) -0.030(11) 0.238(19) -0.025(9) F12 0.049(6) 0.071(7) 0.106(9) -0.031(7) -0.002(6) 0.003(5) F14 0.057(6) 0.059(7) 0.123(10) 0.009(6) 0.037(6) -0.024(5) F16 0.238(16) 0.121(12) 0.137(12) -0.053(10) 0.121(11) -0.053(11) F17 0.096(9) 0.228(19) 0.048(6) -0.041(9) 0.022(7) 0.047(11) F18 0.071(7) 0.214(17) 0.072(8) -0.071(10) 0.036(6) -0.016(9) O8 0.029(4) 0.049(5) 0.032(4) -0.002(4) 0.022(4) -0.005(4) N2 0.032(5) 0.019(5) 0.032(5) -0.002(4) 0.025(4) -0.002(4) C21 0.033(7) 0.069(10) 0.035(7) 0.019(7) 0.021(6) 0.001(6) C23 0.032(6) 0.033(7) 0.036(6) 0.005(5) 0.024(6) 0.003(5) C22 0.032(7) 0.073(10) 0.035(7) 0.006(7) 0.019(6) -0.014(7) C25 0.047(8) 0.085(12) 0.036(7) 0.010(8) 0.025(7) -0.016(8) C24 0.038(8) 0.147(18) 0.036(8) 0.002(10) 0.027(7) -0.031(10) O7 0.032(4) 0.039(5) 0.026(4) 0.004(3) 0.022(3) -0.004(4) N1 0.025(5) 0.040(6) 0.015(4) -0.003(4) 0.012(4) -0.002(4) C16 0.028(5) 0.014(5) 0.029(6) 0.006(4) 0.016(5) -0.003(4) C20 0.029(5) 0.018(5) 0.027(5) 0.000(4) 0.021(5) -0.002(4) C18 0.026(5) 0.031(6) 0.017(5) -0.004(4) 0.013(4) -0.002(5) C19 0.032(6) 0.012(5) 0.026(5) -0.005(4) 0.020(5) -0.005(4) C17 0.038(6) 0.016(5) 0.021(5) -0.004(4) 0.016(5) -0.003(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' F F 0.0171 0.0103 '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' Tb Tb -0.1723 4.1537 '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_3 O8 Tb1 O3 149.5(3) . O8 Tb1 O6 72.1(3) . O3 Tb1 O6 137.6(3) . O8 Tb1 O7 76.1(3) . O3 Tb1 O7 86.6(3) . O6 Tb1 O7 104.8(3) . O8 Tb1 O2 81.9(3) . O3 Tb1 O2 99.9(3) . O6 Tb1 O2 93.2(3) . O7 Tb1 O2 145.3(3) . O8 Tb1 O5 123.0(3) . O3 Tb1 O5 72.6(3) . O6 Tb1 O5 73.0(3) . O7 Tb1 O5 71.2(3) . O2 Tb1 O5 143.3(3) . O8 Tb1 O1 78.6(3) . O3 Tb1 O1 73.2(3) . O6 Tb1 O1 148.8(3) . O7 Tb1 O1 77.6(3) . O2 Tb1 O1 71.9(3) . O5 Tb1 O1 134.4(3) . O8 Tb1 O4 134.9(3) . O3 Tb1 O4 72.5(3) . O6 Tb1 O4 74.2(3) . O7 Tb1 O4 142.2(3) . O2 Tb1 O4 71.0(3) . O5 Tb1 O4 72.6(3) . O1 Tb1 O4 123.0(3) . C4 O2 Tb1 133.4(9) . C2 O1 Tb1 133.4(9) . C7 O3 Tb1 134.4(8) . C14 O6 Tb1 133.2(9) . C12 O5 Tb1 131.8(9) . C9 O4 Tb1 132.3(8) . C7 C8 C9 120.6(12) . O3 C7 C8 128.4(11) . O3 C7 C6 115.9(11) . C8 C7 C6 115.5(11) . O4 C9 C8 128.0(12) . O4 C9 C10 114.0(11) . C8 C9 C10 117.9(11) . F1 C1 F2 108.2(15) . F1 C1 F3 106(2) . F2 C1 F3 106.5(17) . F1 C1 C2 112.6(15) . F2 C1 C2 110(2) . F3 C1 C2 112.5(14) . F11 C10 F12 106.3(13) . F11 C10 F10 107.5(13) . F12 C10 F10 104.6(14) . F11 C10 C9 113.0(11) . F12 C10 C9 111.7(11) . F10 C10 C9 113.2(12) . F9 C6 F7 108.4(15) . F9 C6 F8 108.5(14) . F7 C6 F8 105.4(12) . F9 C6 C7 112.6(12) . F7 C6 C7 110.6(13) . F8 C6 C7 111.1(12) . C2 C3 C4 122.7(16) . O2 C4 C3 126.7(14) . O2 C4 C5 113.0(16) . C3 C4 C5 120.3(17) . O1 C2 C3 128.6(14) . O1 C2 C1 111.7(12) . C3 C2 C1 119.7(14) . O6 C14 C13 129.7(13) . O6 C14 C15 114.4(14) . C13 C14 C15 115.9(14) . F17 C15 F16 117.5(18) . F17 C15 F18 101.0(18) . F16 C15 F18 99.3(17) . F17 C15 C14 113.4(14) . F16 C15 C14 111.5(18) . F18 C15 C14 112.7(13) . O5 C12 C13 127.5(13) . O5 C12 C11 113.6(14) . C13 C12 C11 118.9(14) . C14 C13 C12 121.1(13) . F14 C11 F15 105.8(16) . F14 C11 F13 104.6(17) . F15 C11 F13 112(2) . F14 C11 C12 114.7(18) . F15 C11 C12 107.6(17) . F13 C11 C12 112.3(15) . F6 C5 F5 106(2) . F6 C5 F4 106(3) . F5 C5 F4 109(2) . F6 C5 C4 111.0(19) . F5 C5 C4 111(3) . F4 C5 C4 114.3(18) . N2 O8 Tb1 130.8(6) . C21 N2 O8 122.6(9) . C21 N2 C25 119.3(11) . O8 N2 C25 118.1(10) . N2 C21 C22 121.7(12) . C22 C23 C24 115.1(12) . C22 C23 C23 122.5(14) 7_465 C24 C23 C23 122.4(13) 7_465 C23 C22 C21 121.7(13) . N2 C25 C24 119.6(13) . C25 C24 C23 122.5(13) . N1 O7 Tb1 120.4(6) . C16 N1 O7 120.2(9) . C16 N1 C20 120.7(9) . O7 N1 C20 119.1(9) . N1 C16 C17 120.1(9) . C19 C20 N1 118.6(9) . C17 C18 C19 116.7(9) . C17 C18 C18 120.4(7) 2_554 C19 C18 C18 122.9(7) 2_554 C20 C19 C18 121.9(10) . C18 C17 C16 121.5(10) . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Tb1 O8 2.336(8) . Tb1 O3 2.345(8) . Tb1 O6 2.362(8) . Tb1 O7 2.373(8) . Tb1 O2 2.374(9) . Tb1 O5 2.374(8) . Tb1 O1 2.380(8) . Tb1 O4 2.394(8) . O2 C4 1.28(2) . O1 C2 1.254(16) . O3 C7 1.250(15) . O6 C14 1.235(18) . O5 C12 1.257(16) . O4 C9 1.238(15) . C8 C7 1.392(18) . C8 C9 1.402(18) . C7 C6 1.560(18) . F11 C10 1.301(17) . F3 C1 1.35(2) . C9 C10 1.532(18) . F9 C6 1.292(17) . C1 F1 1.33(3) . C1 F2 1.34(3) . C1 C2 1.53(2) . F7 C6 1.32(2) . F6 C5 1.30(3) . C10 F12 1.308(17) . C10 F10 1.309(18) . C6 F8 1.336(18) . C3 C2 1.35(2) . C3 C4 1.37(2) . C4 C5 1.50(2) . F5 C5 1.33(4) . C14 C13 1.35(2) . C14 C15 1.55(2) . C15 F17 1.25(2) . C15 F16 1.30(2) . C15 F18 1.38(2) . C12 C13 1.43(2) . C12 C11 1.52(2) . F4 C5 1.37(3) . F13 C11 1.36(3) . C11 F14 1.31(2) . C11 F15 1.36(2) . O8 N2 1.334(12) . N2 C21 1.324(16) . N2 C25 1.344(16) . C21 C22 1.364(18) . C23 C22 1.352(18) . C23 C24 1.394(19) . C23 C23 1.49(2) 7_465 C25 C24 1.36(2) . O7 N1 1.331(11) . N1 C16 1.321(14) . N1 C20 1.396(14) . C16 C17 1.385(16) . C20 C19 1.364(14) . C18 C17 1.376(15) . C18 C19 1.387(15) . C18 C18 1.473(19) 2_554