#------------------------------------------------------------------------------ #$Date: 2019-11-07 21:26:15 +0200 (Thu, 07 Nov 2019) $ #$Revision: 223509 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/44/7234435.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_7234435 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 'C38 H14 F36 N4 O14 Tb2' _chemical_formula_sum 'C38 H14 F36 N4 O14 Tb2' _chemical_formula_weight 1752.37 _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 ; 2019-03-05 deposited with the CCDC. 2019-09-30 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 104.26(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 21.080(4) _cell_length_b 12.930(3) _cell_length_c 22.428(5) _cell_measurement_reflns_used 6678 _cell_measurement_temperature 133.15 _cell_measurement_theta_max 25.0441 _cell_measurement_theta_min 1.8639 _cell_volume 5925(2) _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 133.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _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 0.0626 _diffrn_reflns_av_unetI/netI 0.0540 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 23123 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.009 _diffrn_reflns_theta_max 25.009 _diffrn_reflns_theta_min 1.864 _exptl_absorpt_coefficient_mu 2.541 _exptl_absorpt_correction_T_max 0.776 _exptl_absorpt_correction_T_min 0.639 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details SADABS _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.965 _exptl_crystal_description block _exptl_crystal_F_000 3344 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _refine_diff_density_max 1.249 _refine_diff_density_min -2.105 _refine_diff_density_rms 0.133 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.173 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 424 _refine_ls_number_reflns 5234 _refine_ls_number_restraints 195 _refine_ls_restrained_S_all 1.303 _refine_ls_R_factor_all 0.0827 _refine_ls_R_factor_gt 0.0671 _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^)+(0.0968P)^2^+4.4963P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1717 _refine_ls_wR_factor_ref 0.1879 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4148 _reflns_number_total 5234 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9ce01378d2.cif _cod_data_source_block shelxl_CCDC1 _cod_depositor_comments 'Adding full bibliography for 7234434--7234439.cif.' _cod_database_code 7234435 _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 ; shelxl.res created by SHELXL-2014/7 TITL shelxl in C2/c CELL 0.71073 21.0799 12.9303 22.4277 90 104.263 90 ZERR 4 0.0042 0.0026 0.0045 0 0.03 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H F N O Tb UNIT 152 56 144 16 56 8 DELU 0.01 0.005 F11 C10 DELU 0.01 0.005 F12 C10 DELU 0.01 0.005 O3 C7 DELU 0.01 0.005 C8 C9 DELU 0.01 0.005 C9 C10 DELU 0.01 0.005 F1 C1 DELU 0.01 0.005 F2 C1 DELU 0.01 0.005 C12 C13 DELU 0.005 0.005 Tb1 Tb1 DELU 0.01 0.005 F8 C6 SIMU 0.005 0.005 3.8 Tb1 O5 O7 O4 O3 O1 O2 O6 ISOR 0.001 0.001 Tb1 ISOR 0.01 0.02 F2 F3 F18 F16 F14 F7 F13 F10 F17 L.S. 10 PLAN 20 FREE F9 F8 BOND fmap 2 acta OMIT -3 50.02 REM REM REM WGHT 0.096800 4.496300 FVAR 1.36359 TB1 6 0.304380 0.235599 0.090291 11.00000 0.06113 0.05131 = 0.07604 0.00692 0.02132 0.00474 O1 5 0.356211 0.219320 0.192904 11.00000 0.07866 0.06588 = 0.09262 0.00459 0.01973 0.00907 O2 5 0.364975 0.078759 0.102340 11.00000 0.07592 0.06216 = 0.08998 0.00324 0.01635 0.00921 O3 5 0.233037 0.106317 0.107043 11.00000 0.07968 0.06703 = 0.09936 0.00649 0.02165 0.00003 O4 5 0.228864 0.310056 0.138104 11.00000 0.07833 0.06868 = 0.09546 0.00391 0.02226 0.00934 O5 5 0.352746 0.398628 0.117821 11.00000 0.07528 0.06160 = 0.09637 0.00287 0.01962 0.00260 O6 5 0.387969 0.259100 0.038646 11.00000 0.07195 0.06410 = 0.09062 0.00287 0.02472 0.00136 O7 5 0.238551 0.344527 0.009570 11.00000 0.07405 0.05644 = 0.09170 0.00346 0.01728 0.00655 N1 4 0.226904 0.446371 0.019394 11.00000 0.10057 0.04410 = 0.09312 0.00072 0.00951 0.02421 N2 4 0.205493 0.648756 0.039122 11.00000 0.23004 0.06602 = 0.15667 -0.01840 -0.00302 0.04243 C1 1 0.410393 0.187794 0.294269 11.00000 0.11512 0.11721 = 0.08626 -0.02849 -0.00181 0.04016 C2 1 0.390461 0.151981 0.226205 11.00000 0.08925 0.08362 = 0.07548 0.01832 0.02005 0.01842 C3 1 0.409088 0.056488 0.207431 11.00000 0.09262 0.08150 = 0.07567 0.01857 0.02295 0.01625 AFIX 43 H3 2 0.431673 0.010298 0.236890 11.00000 -1.20000 AFIX 0 C4 1 0.395020 0.029039 0.146895 11.00000 0.06599 0.06151 = 0.08230 0.01472 0.01445 0.01523 C5 1 0.420538 -0.074213 0.131472 11.00000 0.13720 0.08357 = 0.08653 0.00043 0.01937 0.03901 C6 1 0.167988 -0.010025 0.143627 11.00000 0.11202 0.13098 = 0.23970 0.05828 0.07845 -0.02993 C7 1 0.195648 0.098363 0.144278 11.00000 0.08715 0.10515 = 0.11379 0.01821 0.04135 0.00361 C8 1 0.179219 0.174045 0.177608 11.00000 0.10248 0.13592 = 0.13569 0.01748 0.05961 -0.01021 AFIX 43 H8 2 0.155789 0.157074 0.206361 11.00000 -1.20000 AFIX 0 C9 1 0.194550 0.273302 0.172050 11.00000 0.08048 0.13173 = 0.09303 0.00839 0.04320 0.01144 C10 1 0.167141 0.358875 0.208409 11.00000 0.14953 0.16285 = 0.23910 -0.01412 0.13665 0.01120 C11 1 0.420371 0.540729 0.151231 11.00000 0.14844 0.09399 = 0.13525 -0.02405 0.03248 -0.03781 C12 1 0.405284 0.440908 0.114644 11.00000 0.08222 0.06761 = 0.11562 0.00732 0.01558 -0.01459 C13 1 0.447801 0.406318 0.082120 11.00000 0.07435 0.11636 = 0.11362 -0.00219 0.02935 -0.02354 AFIX 43 H13 2 0.486403 0.442846 0.084776 11.00000 -1.20000 AFIX 0 C14 1 0.435843 0.318713 0.045152 11.00000 0.06379 0.08584 = 0.10440 0.00839 0.02627 -0.00154 C15 1 0.482435 0.286358 0.008216 11.00000 0.07091 0.19823 = 0.12850 0.01498 0.05657 0.00476 C16 1 0.271257 0.515062 0.008870 11.00000 0.13360 0.04329 = 0.13032 0.01603 0.00209 0.00242 AFIX 43 H16 2 0.307670 0.495578 -0.004903 11.00000 -1.20000 AFIX 0 C17 1 0.257588 0.618656 0.020553 11.00000 0.19439 0.05195 = 0.17497 0.00175 -0.02836 0.00977 AFIX 43 H17 2 0.286977 0.669136 0.014878 11.00000 -1.20000 AFIX 0 C18 1 0.162723 0.573393 0.046755 11.00000 0.18132 0.09819 = 0.12196 -0.02060 0.00074 0.06990 AFIX 43 H18 2 0.125029 0.592461 0.058512 11.00000 -1.20000 AFIX 0 C19 1 0.173496 0.470196 0.037645 11.00000 0.12000 0.08835 = 0.08558 -0.00330 0.00532 0.04638 AFIX 43 H19 2 0.144583 0.419476 0.044015 11.00000 -1.20000 AFIX 0 F4 3 0.460139 -0.121803 0.176225 11.00000 0.17202 0.11970 = 0.10946 0.00217 0.00213 0.08655 F6 3 0.453718 -0.063357 0.087442 11.00000 0.18265 0.14422 = 0.15043 0.00685 0.08313 0.07116 F5 3 0.371485 -0.136700 0.107823 11.00000 0.15323 0.06887 = 0.20080 -0.03228 -0.00487 0.00696 F3 3 0.443137 0.109641 0.329650 11.00000 0.21844 0.13943 = 0.09578 0.00074 0.00009 0.06490 F2 3 0.362083 0.207979 0.316215 11.00000 0.21847 0.23012 = 0.09806 -0.00563 0.06293 0.08967 F1 3 0.449655 0.263630 0.301103 11.00000 0.29685 0.17516 = 0.11870 -0.03720 0.01304 -0.08272 F18 3 0.456779 0.271131 -0.047386 11.00000 0.15363 0.32712 = 0.14337 -0.03938 0.07458 0.01547 F15 3 0.479891 0.570956 0.159371 11.00000 0.17230 0.20321 = 0.26891 -0.10488 0.04647 -0.10373 F9 3 0.209031 -0.082082 0.143858 11.00000 0.22476 0.11123 = 0.33164 0.04431 0.11446 -0.03807 F16 3 0.527289 0.353090 0.007542 11.00000 0.20014 0.26975 = 0.31237 -0.09023 0.17252 -0.08481 F12 3 0.195775 0.443276 0.214079 11.00000 0.30973 0.17186 = 0.32146 -0.10887 0.20142 -0.03566 F14 3 0.383038 0.610985 0.130091 11.00000 0.27872 0.11569 = 0.31163 -0.07873 -0.08505 0.03934 F7 3 0.144452 -0.027677 0.189822 11.00000 0.35895 0.22646 = 0.30250 0.00431 0.22159 -0.12150 F13 3 0.415274 0.529395 0.205643 11.00000 0.34263 0.22895 = 0.19397 -0.10730 0.13046 -0.12591 F10 3 0.111590 0.390158 0.168174 11.00000 0.18709 0.26798 = 0.31246 -0.08692 0.05483 0.09277 F11 3 0.147380 0.328511 0.250830 11.00000 0.53927 0.24608 = 0.33399 0.02390 0.36468 0.07308 F8 3 0.120869 -0.023457 0.097684 11.00000 0.18366 0.19285 = 0.41880 0.00033 -0.03440 -0.11782 F17 3 0.512950 0.208763 0.025351 11.00000 0.23024 0.30052 = 0.24876 0.08473 0.14819 0.15724 HKLF 4 REM shelxl in C2/c REM R1 = 0.0671 for 4148 Fo > 4sig(Fo) and 0.0827 for all 5225 data REM 424 parameters refined using 195 restraints END WGHT 0.1044 6.7281 REM Highest difference peak 1.249, deepest hole -2.105, 1-sigma level 0.133 Q1 1 0.3032 0.3168 0.0898 11.00000 0.05 1.19 Q2 1 0.4108 0.2715 0.2682 11.00000 0.05 0.92 Q3 1 0.5472 0.2749 0.0510 11.00000 0.05 0.67 Q4 1 0.3652 0.5764 0.1698 11.00000 0.05 0.66 Q5 1 0.4184 0.6185 0.1136 11.00000 0.05 0.66 Q6 1 0.4754 0.3607 -0.0393 11.00000 0.05 0.57 Q7 1 0.0921 0.2730 0.2035 11.00000 0.05 0.56 Q8 1 0.5067 0.3737 -0.0162 11.00000 0.05 0.54 Q9 1 0.3861 0.2381 0.1967 11.00000 0.05 0.54 Q10 1 0.2537 0.3529 0.0038 11.00000 0.05 0.48 Q11 1 0.3387 0.1669 0.0532 11.00000 0.05 0.45 Q12 1 0.2264 0.3412 0.0186 11.00000 0.05 0.45 Q13 1 0.2768 0.1668 0.1292 11.00000 0.05 0.43 Q14 1 0.2087 0.2673 0.1204 11.00000 0.05 0.43 Q15 1 0.4779 0.1830 -0.0132 11.00000 0.05 0.42 Q16 1 0.3735 0.2545 0.1368 11.00000 0.05 0.41 Q17 1 0.2396 0.3630 0.1397 11.00000 0.05 0.41 Q18 1 0.3226 0.3275 0.0357 11.00000 0.05 0.41 Q19 1 0.3279 0.3180 0.1517 11.00000 0.05 0.40 Q20 1 0.4683 0.1928 -0.0294 11.00000 0.05 0.39 ; _shelx_res_checksum 87792 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 0.30438(2) 0.23560(3) 0.09029(2) 0.0621(2) Uani 1 1 d . U O1 O 0.3562(3) 0.2193(5) 0.1929(3) 0.0793(11) Uani 1 1 d . U O2 O 0.3650(3) 0.0788(5) 0.1023(3) 0.0767(12) Uani 1 1 d . U O3 O 0.2330(3) 0.1063(5) 0.1070(3) 0.0821(11) Uani 1 1 d . U O4 O 0.2289(3) 0.3101(5) 0.1381(3) 0.0807(11) Uani 1 1 d . U O5 O 0.3527(3) 0.3986(5) 0.1178(3) 0.0780(11) Uani 1 1 d . U O6 O 0.3880(3) 0.2591(4) 0.0386(3) 0.0747(11) Uani 1 1 d . U O7 O 0.2386(3) 0.3445(5) 0.0096(3) 0.0746(11) Uani 1 1 d . U N1 N 0.2269(4) 0.4464(6) 0.0194(4) 0.082(2) Uani 1 1 d . . N2 N 0.2055(9) 0.6488(10) 0.0391(7) 0.160(6) Uani 1 1 d . . C1 C 0.4104(7) 0.1878(12) 0.2943(6) 0.111(4) Uani 1 1 d . U C2 C 0.3905(4) 0.1520(8) 0.2262(4) 0.083(3) Uani 1 1 d . . C3 C 0.4091(5) 0.0565(8) 0.2074(4) 0.083(3) Uani 1 1 d . . H3 H 0.4317 0.0103 0.2369 0.099 Uiso 1 1 calc R U C4 C 0.3950(4) 0.0290(7) 0.1469(4) 0.071(2) Uani 1 1 d . . C5 C 0.4205(7) -0.0742(10) 0.1315(5) 0.104(4) Uani 1 1 d . . C6 C 0.1680(8) -0.0100(14) 0.1436(11) 0.155(6) Uani 1 1 d . U C7 C 0.1956(5) 0.0984(11) 0.1443(6) 0.099(3) Uani 1 1 d . U C8 C 0.1792(6) 0.1740(13) 0.1776(7) 0.119(4) Uani 1 1 d . U H8 H 0.1558 0.1571 0.2064 0.143 Uiso 1 1 calc R U C9 C 0.1945(6) 0.2733(11) 0.1720(6) 0.098(3) Uani 1 1 d . U C10 C 0.1671(11) 0.3589(18) 0.2084(12) 0.168(7) Uani 1 1 d . U C11 C 0.4204(9) 0.5407(12) 0.1512(8) 0.126(5) Uani 1 1 d . . C12 C 0.4053(5) 0.4409(8) 0.1146(5) 0.090(3) Uani 1 1 d . U C13 C 0.4478(5) 0.4063(10) 0.0821(5) 0.100(3) Uani 1 1 d . U H13 H 0.4864 0.4428 0.0848 0.120 Uiso 1 1 calc R U C14 C 0.4358(4) 0.3187(9) 0.0452(5) 0.084(3) Uani 1 1 d . . C15 C 0.4824(7) 0.2864(17) 0.0082(8) 0.127(5) Uani 1 1 d . . C16 C 0.2713(6) 0.5151(8) 0.0089(5) 0.108(4) Uani 1 1 d . . H16 H 0.3077 0.4956 -0.0049 0.129 Uiso 1 1 calc R U C17 C 0.2576(8) 0.6187(11) 0.0206(8) 0.153(7) Uani 1 1 d . . H17 H 0.2870 0.6691 0.0149 0.184 Uiso 1 1 calc R U C18 C 0.1627(9) 0.5734(13) 0.0468(7) 0.140(6) Uani 1 1 d . . H18 H 0.1250 0.5925 0.0585 0.168 Uiso 1 1 calc R U C19 C 0.1735(6) 0.4702(9) 0.0376(5) 0.101(4) Uani 1 1 d . . H19 H 0.1446 0.4195 0.0440 0.122 Uiso 1 1 calc R U F4 F 0.4601(4) -0.1218(6) 0.1762(3) 0.139(3) Uani 1 1 d . . F6 F 0.4537(4) -0.0634(7) 0.0874(4) 0.152(3) Uani 1 1 d . . F5 F 0.3715(4) -0.1367(6) 0.1078(4) 0.149(3) Uani 1 1 d . . F3 F 0.4431(4) 0.1096(7) 0.3297(3) 0.158(3) Uani 1 1 d . U F2 F 0.3621(5) 0.2080(10) 0.3162(4) 0.178(4) Uani 1 1 d . U F1 F 0.4497(8) 0.2636(9) 0.3011(5) 0.204(6) Uani 1 1 d . U F18 F 0.4568(6) 0.2711(10) -0.0474(6) 0.201(5) Uani 1 1 d . U F15 F 0.4799(5) 0.5710(10) 0.1594(6) 0.216(6) Uani 1 1 d . . F9 F 0.2090(6) -0.0821(9) 0.1439(7) 0.215(5) Uani 1 1 d . . F16 F 0.5273(6) 0.3531(12) 0.0075(6) 0.242(6) Uani 1 1 d . U F12 F 0.1958(7) 0.4433(11) 0.2141(7) 0.246(7) Uani 1 1 d . U F14 F 0.3830(7) 0.6110(10) 0.1301(7) 0.263(7) Uani 1 1 d . U F7 F 0.1445(8) -0.0277(11) 0.1898(7) 0.271(7) Uani 1 1 d . U F13 F 0.4153(7) 0.5294(11) 0.2056(6) 0.244(6) Uani 1 1 d . U F10 F 0.1116(6) 0.3902(13) 0.1682(7) 0.257(7) Uani 1 1 d . U F11 F 0.1474(10) 0.3285(13) 0.2508(8) 0.328(11) Uani 1 1 d . U F8 F 0.1209(6) -0.0235(10) 0.0977(9) 0.284(9) Uani 1 1 d . U F17 F 0.5130(8) 0.2088(12) 0.0254(7) 0.244(7) Uani 1 1 d . U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0611(3) 0.0513(3) 0.0760(3) 0.00692(17) 0.0213(2) 0.00474(16) O1 0.079(2) 0.066(2) 0.093(2) 0.0046(19) 0.0197(19) 0.0091(18) O2 0.076(2) 0.062(2) 0.090(2) 0.003(2) 0.016(2) 0.009(2) O3 0.080(2) 0.067(2) 0.099(2) 0.006(2) 0.0217(19) 0.0000(19) O4 0.078(2) 0.069(2) 0.095(2) 0.004(2) 0.022(2) 0.009(2) O5 0.075(2) 0.062(2) 0.096(2) 0.003(2) 0.0196(19) 0.0026(19) O6 0.072(2) 0.064(2) 0.091(2) 0.0029(19) 0.025(2) 0.0014(19) O7 0.074(2) 0.056(2) 0.092(2) 0.0035(19) 0.0173(18) 0.0066(19) N1 0.101(5) 0.044(4) 0.093(5) 0.001(4) 0.010(4) 0.024(4) N2 0.230(17) 0.066(8) 0.157(12) -0.018(8) -0.003(11) 0.042(10) C1 0.115(8) 0.117(10) 0.086(7) -0.028(7) -0.002(6) 0.040(6) C2 0.089(6) 0.084(7) 0.075(6) 0.018(5) 0.020(5) 0.018(5) C3 0.093(6) 0.082(7) 0.076(6) 0.019(5) 0.023(5) 0.016(5) C4 0.066(5) 0.062(6) 0.082(6) 0.015(4) 0.014(4) 0.015(4) C5 0.137(10) 0.084(8) 0.087(7) 0.000(6) 0.019(7) 0.039(8) C6 0.112(11) 0.131(15) 0.240(17) 0.058(14) 0.078(10) -0.030(10) C7 0.087(7) 0.105(9) 0.114(9) 0.018(7) 0.041(6) 0.004(6) C8 0.102(9) 0.136(11) 0.136(11) 0.017(10) 0.060(8) -0.010(9) C9 0.080(7) 0.132(9) 0.093(8) 0.008(7) 0.043(6) 0.011(6) C10 0.150(14) 0.163(15) 0.24(2) -0.014(14) 0.137(16) 0.011(12) C11 0.148(13) 0.094(11) 0.135(12) -0.024(9) 0.032(10) -0.038(10) C12 0.082(6) 0.068(6) 0.116(8) 0.007(5) 0.016(5) -0.015(5) C13 0.074(6) 0.116(10) 0.114(8) -0.002(7) 0.029(5) -0.024(6) C14 0.064(5) 0.086(8) 0.104(7) 0.008(6) 0.026(5) -0.002(5) C15 0.071(7) 0.198(18) 0.128(12) 0.015(12) 0.057(8) 0.005(9) C16 0.134(8) 0.043(6) 0.130(9) 0.016(6) 0.002(7) 0.002(6) C17 0.194(17) 0.052(8) 0.175(14) 0.002(8) -0.028(13) 0.010(9) C18 0.181(15) 0.098(11) 0.122(10) -0.021(9) 0.001(10) 0.070(11) C19 0.120(8) 0.088(8) 0.086(7) -0.003(6) 0.005(6) 0.046(7) F4 0.172(6) 0.120(6) 0.109(5) 0.002(4) 0.002(4) 0.087(5) F6 0.183(7) 0.144(8) 0.150(7) 0.007(5) 0.083(6) 0.071(6) F5 0.153(6) 0.069(5) 0.201(8) -0.032(5) -0.005(6) 0.007(4) F3 0.218(8) 0.139(7) 0.096(5) 0.001(5) 0.000(5) 0.065(6) F2 0.218(9) 0.230(10) 0.098(5) -0.006(6) 0.063(6) 0.090(8) F1 0.297(16) 0.175(11) 0.119(8) -0.037(6) 0.013(9) -0.083(9) F18 0.154(8) 0.327(15) 0.143(8) -0.039(8) 0.075(7) 0.015(7) F15 0.172(9) 0.203(12) 0.269(13) -0.105(10) 0.046(8) -0.104(9) F9 0.225(12) 0.111(8) 0.332(17) 0.044(10) 0.114(12) -0.038(8) F16 0.200(9) 0.270(14) 0.312(13) -0.090(11) 0.173(9) -0.085(9) F12 0.310(17) 0.172(12) 0.321(17) -0.109(13) 0.201(14) -0.036(11) F14 0.279(12) 0.116(8) 0.312(14) -0.079(9) -0.085(10) 0.039(8) F7 0.359(13) 0.226(12) 0.303(13) 0.004(10) 0.222(12) -0.121(10) F13 0.343(13) 0.229(12) 0.194(9) -0.107(9) 0.130(10) -0.126(11) F10 0.187(9) 0.268(14) 0.312(14) -0.087(11) 0.055(9) 0.093(10) F11 0.54(3) 0.246(17) 0.334(19) 0.024(14) 0.36(2) 0.073(18) F8 0.184(10) 0.193(12) 0.42(2) 0.000(13) -0.034(12) -0.118(10) F17 0.230(11) 0.301(14) 0.249(12) 0.085(11) 0.148(10) 0.157(11) 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_1 _geom_angle_site_symmetry_3 O1 Tb1 O4 77.8(2) . . O1 Tb1 O3 86.5(2) . . O4 Tb1 O3 71.5(2) . . O1 Tb1 O6 106.0(2) . . O4 Tb1 O6 148.2(2) . . O3 Tb1 O6 139.4(2) . . O1 Tb1 O5 75.6(2) . . O4 Tb1 O5 79.1(2) . . O3 Tb1 O5 148.3(2) . . O6 Tb1 O5 71.7(2) . . O1 Tb1 O2 72.5(2) . . O4 Tb1 O2 135.1(2) . . O3 Tb1 O2 73.8(2) . . O6 Tb1 O2 73.7(2) . . O5 Tb1 O2 123.2(2) . . O1 Tb1 O7 149.3(2) . 7 O4 Tb1 O7 117.2(2) . 7 O3 Tb1 O7 74.7(2) . 7 O6 Tb1 O7 75.9(2) . 7 O5 Tb1 O7 131.4(2) . 7 O2 Tb1 O7 79.0(2) . 7 O1 Tb1 O7 147.0(2) . . O4 Tb1 O7 77.0(2) . . O3 Tb1 O7 105.1(2) . . O6 Tb1 O7 85.3(2) . . O5 Tb1 O7 78.9(2) . . O2 Tb1 O7 140.2(2) . . O7 Tb1 O7 63.1(2) 7 . C2 O1 Tb1 136.2(7) . . C4 O2 Tb1 134.1(6) . . C7 O3 Tb1 133.0(8) . . C9 O4 Tb1 132.6(8) . . C12 O5 Tb1 135.0(7) . . C14 O6 Tb1 134.7(7) . . N1 O7 Tb1 121.2(5) . 7 N1 O7 Tb1 121.9(5) . . Tb1 O7 Tb1 116.9(2) 7 . C19 N1 C16 125.3(10) . . C19 N1 O7 118.3(9) . . C16 N1 O7 116.4(9) . . C17 N2 C18 117.0(13) . . F2 C1 F1 111.0(13) . . F2 C1 F3 105.5(14) . . F1 C1 F3 106.3(12) . . F2 C1 C2 113.4(11) . . F1 C1 C2 111.1(13) . . F3 C1 C2 109.1(10) . . O1 C2 C3 126.9(9) . . O1 C2 C1 110.8(9) . . C3 C2 C1 122.3(9) . . C4 C3 C2 121.6(9) . . O2 C4 C3 128.1(9) . . O2 C4 C5 114.7(9) . . C3 C4 C5 117.1(8) . . F4 C5 F5 108.3(12) . . F4 C5 F6 105.4(11) . . F5 C5 F6 105.4(11) . . F4 C5 C4 116.2(10) . . F5 C5 C4 110.2(10) . . F6 C5 C4 110.7(11) . . F8 C6 F9 108(2) . . F8 C6 F7 104.8(14) . . F9 C6 F7 105.4(17) . . F8 C6 C7 111.1(15) . . F9 C6 C7 114.7(12) . . F7 C6 C7 112.5(19) . . O3 C7 C8 126.4(12) . . O3 C7 C6 111.3(13) . . C8 C7 C6 122.2(12) . . C7 C8 C9 123.5(12) . . O4 C9 C8 127.2(12) . . O4 C9 C10 112.8(13) . . C8 C9 C10 120.1(12) . . F11 C10 F12 118(3) . . F11 C10 F10 102.4(17) . . F12 C10 F10 97(2) . . F11 C10 C9 115.3(19) . . F12 C10 C9 116.3(13) . . F10 C10 C9 103.5(19) . . F14 C11 F13 105.2(18) . . F14 C11 F15 110.1(16) . . F13 C11 F15 102.2(16) . . F14 C11 C12 113.2(14) . . F13 C11 C12 111.6(14) . . F15 C11 C12 113.7(14) . . O5 C12 C13 126.5(11) . . O5 C12 C11 114.2(11) . . C13 C12 C11 119.3(11) . . C12 C13 C14 122.7(9) . . O6 C14 C13 126.5(9) . . O6 C14 C15 112.7(12) . . C13 C14 C15 120.8(11) . . F17 C15 F18 105(2) . . F17 C15 F16 103.1(14) . . F18 C15 F16 103.5(15) . . F17 C15 C14 115.5(14) . . F18 C15 C14 114.6(12) . . F16 C15 C14 113.9(17) . . N1 C16 C17 114.2(13) . . N2 C17 C16 124.1(16) . . N2 C18 C19 122.3(16) . . N1 C19 C18 117.0(14) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Tb1 O1 2.301(7) . Tb1 O4 2.335(6) . Tb1 O3 2.340(6) . Tb1 O6 2.355(7) . Tb1 O5 2.357(6) . Tb1 O2 2.376(6) . Tb1 O7 2.431(6) 7 Tb1 O7 2.439(6) . O1 C2 1.254(10) . O2 C4 1.225(10) . O3 C7 1.286(12) . O4 C9 1.265(12) . O5 C12 1.253(10) . O6 C14 1.250(11) . O7 N1 1.367(9) . O7 Tb1 2.431(6) 7 N1 C19 1.326(13) . N1 C16 1.352(14) . N2 C17 1.33(2) . N2 C18 1.37(2) . C1 F2 1.263(15) . C1 F1 1.268(18) . C1 F3 1.363(15) . C1 C2 1.551(14) . C2 C3 1.392(13) . C3 C4 1.363(13) . C4 C5 1.511(14) . C5 F4 1.292(13) . C5 F5 1.316(15) . C5 F6 1.351(14) . C6 F8 1.25(2) . C6 F9 1.271(18) . C6 F7 1.275(19) . C6 C7 1.517(19) . C7 C8 1.328(18) . C8 C9 1.337(18) . C9 C10 1.57(2) . C10 F11 1.20(2) . C10 F12 1.24(2) . C10 F10 1.35(3) . C11 F14 1.219(19) . C11 F13 1.260(18) . C11 F15 1.284(18) . C11 C12 1.520(17) . C12 C13 1.363(15) . C13 C14 1.390(15) . C14 C15 1.492(16) . C15 F17 1.20(2) . C15 F18 1.247(19) . C15 F16 1.283(19) . C16 C17 1.408(18) . C18 C19 1.377(17) .