#------------------------------------------------------------------------------ #$Date: 2024-12-03 01:33:35 +0200 (Tue, 03 Dec 2024) $ #$Revision: 296182 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/96/7249653.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_7249653 loop_ _publ_author_name 'Xu, Shixian' 'Lu, Na' 'Wang, Li' 'Liu, Sui-Jun' _publ_section_title ; Chain-based fluorescent TbIII metal-organic framework with good stability as a blue-shift and turn-on sensor toward H2PO4− ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D4CE01073F _journal_year 2024 _chemical_formula_moiety 'C60 H32 N6 O16 S3 Tb3' _chemical_formula_sum 'C60 H32 N6 O16 S3 Tb3' _chemical_formula_weight 1665.85 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2024-08-29 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-08-29 deposited with the CCDC. 2024-12-02 downloaded from the CCDC. ; _cell_angle_alpha 113.758(2) _cell_angle_beta 95.709(2) _cell_angle_gamma 102.086(2) _cell_formula_units_Z 2 _cell_length_a 8.7857(5) _cell_length_b 18.8668(11) _cell_length_c 20.7919(13) _cell_measurement_reflns_used 9961 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.52 _cell_measurement_theta_min 2.86 _cell_volume 3018.7(3) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/2 (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 293.15 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.986 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0625 _diffrn_reflns_av_unetI/netI 0.0723 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.986 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_number 44107 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.986 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.551 _diffrn_reflns_theta_min 2.818 _diffrn_source_current 30.0 _diffrn_source_power 1.35 _diffrn_source_voltage 45.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.654 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.5728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0965 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.7682. The \l/2 correction factor is Not present. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.833 _exptl_crystal_description block _exptl_crystal_F_000 1610 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.11 _exptl_transmission_factor_max 0.7456 _exptl_transmission_factor_min 0.5728 _refine_diff_density_max 4.589 _refine_diff_density_min -2.938 _refine_diff_density_rms 0.259 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 788 _refine_ls_number_reflns 13756 _refine_ls_number_restraints 12 _refine_ls_restrained_S_all 1.036 _refine_ls_R_factor_all 0.0786 _refine_ls_R_factor_gt 0.0562 _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^)+(0.0824P)^2^+14.5809P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1401 _refine_ls_wR_factor_ref 0.1535 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10392 _reflns_number_total 13756 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce01073f2.cif _cod_data_source_block JXUST-52 _cod_database_code 7249653 _shelx_shelxl_version_number 2019/2 _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_max 0.689 _shelx_estimated_absorpt_t_min 0.629 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2. Uiso/Uaniso restraints and constraints O13 \\sim O14: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(O13) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O13) = Uanis(O14) 3. Rigid body (RIGU) restrains O13 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02 4.a Rotating group: O1W(H1WA,H1WB) 4.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C12(H12), C15(H15), C16(H16), C17(H17), C18(H18), C25(H25), C24(H24), C23(H23), C26(H26), C30(H30), C32(H32), C35(H35), C36(H36), C37(H37), C38(H38), C43(H43), C44(H44), C45(H45), C46(H46), C50(H50), C51(H51), C56(H56), C57(H57), C58(H58), C59(H59) ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 1_a.res in P-1 New: P-1 1_a.res created by SHELXL-2019/2 at 19:42:59 on 29-Aug-2024 CELL 0.71073 8.7857 18.8668 20.7919 113.758 95.709 102.086 ZERR 2 0.0005 0.0011 0.0013 0.002 0.002 0.002 LATT 1 SFAC C H N O S Tb UNIT 120 64 12 32 6 6 EQIV $1 1-X,-Y,-Z EQIV $2 2-X,-Y,-Z RIGU 0.01 0.02 O13 SIMU 0.01 0.02 2 O13 O14 ISOR 0.001 0.002 O13 ISOR 0.01 0.02 C1 EADP O13 O14 L.S. 5 PLAN 10 SIZE 0.11 0.13 0.14 TEMP 20 CONF FREE Tb2 Tb1 FREE Tb2 Tb1_$1 FREE Tb2 Tb2_$2 FREE Tb1 Tb1_$1 FREE Tb3 Tb2 FREE Tb3 C20 LIST 6 MORE -1 BOND $H ABIN fmap 2 acta REM REM REM WGHT 0.082400 14.580900 FVAR 0.20038 TB1 6 0.600652 0.118230 0.052216 11.00000 0.01092 0.01753 = 0.01172 0.00369 -0.00066 0.00394 S1 5 0.983126 -0.190382 -0.565692 11.00000 0.05867 0.06150 = 0.02641 0.02206 0.00623 0.03990 N1 3 0.883285 -0.175306 -0.625796 11.00000 0.04866 0.03742 = 0.02247 0.01568 0.00414 0.02405 O1 4 0.514143 -0.132788 -0.952091 11.00000 0.02595 0.04851 = 0.02194 0.02003 0.00813 0.01949 C1 1 0.623578 -0.151712 -0.925957 11.00000 0.01234 0.02974 = 0.00900 0.00894 -0.00558 0.00149 TB2 6 0.823180 -0.021223 -0.073932 11.00000 0.01140 0.01853 = 0.01059 0.00402 -0.00123 0.00471 S2 5 1.408401 0.770496 0.357376 11.00000 0.03986 0.03283 = 0.02869 0.01392 0.00317 0.00167 N2 3 0.945499 -0.127411 -0.494129 11.00000 0.03645 0.05253 = 0.02403 0.02000 0.00193 0.02152 O2 4 0.726104 -0.179215 -0.958299 11.00000 0.02365 0.05342 = 0.02196 0.01750 0.00561 0.01383 C2 1 0.638370 -0.140385 -0.849280 11.00000 0.02617 0.03201 = 0.01715 0.01680 0.00636 0.00981 TB3 6 1.037859 0.188803 -0.005764 11.00000 0.01533 0.01925 = 0.01358 0.00553 -0.00083 0.00499 S3 5 0.641460 -0.320895 -0.572595 11.00000 0.07159 0.03172 = 0.02875 0.01189 -0.00300 0.01918 N3 3 1.278722 0.683832 0.318798 11.00000 0.03453 0.03100 = 0.02356 0.01076 0.00490 0.00562 O3 4 0.916455 0.175951 -0.121085 11.00000 0.04925 0.03244 = 0.01504 0.00993 0.00100 0.01379 C3 1 0.727191 -0.176650 -0.822590 11.00000 0.04463 0.05135 = 0.01955 0.01002 0.00392 0.03400 AFIX 43 H3 2 0.773008 -0.213476 -0.853399 11.00000 -1.20000 AFIX 0 N4 3 1.395428 0.796205 0.439988 11.00000 0.02550 0.02696 = 0.02711 0.00767 -0.00410 0.00338 O4 4 0.962802 0.064080 -0.126047 11.00000 0.02521 0.03525 = 0.01702 0.01797 0.00390 0.01099 C4 1 0.560529 -0.091228 -0.804196 11.00000 0.06462 0.06340 = 0.01761 0.02363 0.01181 0.04416 AFIX 43 H4 2 0.490327 -0.069589 -0.821948 11.00000 -1.20000 AFIX 0 N5 3 0.717338 -0.308804 -0.494409 11.00000 0.05017 0.02602 = 0.01739 0.00432 -0.00425 0.00993 O5 4 1.647137 0.950908 0.823554 11.00000 0.02480 0.03191 = 0.02055 0.00953 -0.01159 -0.00244 C5 1 0.588356 -0.074327 -0.731581 11.00000 0.06227 0.05597 = 0.01656 0.01063 0.01124 0.03882 AFIX 43 H5 2 0.538230 -0.039657 -0.701140 11.00000 -1.20000 AFIX 0 N6 3 0.593272 -0.416586 -0.616961 11.00000 0.04134 0.03187 = 0.02312 0.00999 -0.00501 0.01501 O6 4 1.408878 0.913321 0.846628 11.00000 0.03274 0.04727 = 0.01272 0.01400 0.00549 0.01837 C6 1 0.751592 -0.160604 -0.751277 11.00000 0.05298 0.05785 = 0.01940 0.02102 0.01144 0.03664 AFIX 43 H6 2 0.813556 -0.186888 -0.735177 11.00000 -1.20000 AFIX 0 O7 4 0.690001 0.261726 0.097235 11.00000 0.02534 0.02491 = 0.01700 0.00165 0.00101 0.00744 C7 1 0.687567 -0.107140 -0.703160 11.00000 0.02134 0.03259 = 0.01286 0.00765 -0.00122 0.00823 O8 4 0.913751 0.283099 0.057287 11.00000 0.03311 0.02675 = 0.03186 0.00290 0.01279 0.01359 C8 1 0.722808 -0.081887 -0.624422 11.00000 0.02207 0.03659 = 0.01861 0.01904 0.00019 0.00456 O9 4 0.370511 -0.842130 -0.893592 11.00000 0.02489 0.01725 = 0.01815 0.00185 0.00204 0.00328 C9 1 0.670460 -0.022664 -0.576424 11.00000 0.03816 0.04360 = 0.01401 0.01335 0.00327 0.01518 AFIX 43 H9 2 0.608620 0.002330 -0.594341 11.00000 -1.20000 AFIX 0 C10 1 0.818218 -0.116317 -0.590639 11.00000 0.02900 0.02770 = 0.01913 0.01288 0.00491 0.00973 O10 4 0.209849 -0.767214 -0.896943 11.00000 0.02087 0.02508 = 0.01437 0.00340 -0.00421 0.00648 C11 1 0.851627 -0.089572 -0.514291 11.00000 0.02559 0.03314 = 0.01843 0.01549 0.00143 0.00881 C13 1 0.792168 -0.027691 -0.467420 11.00000 0.02296 0.03693 = 0.01693 0.01227 -0.00113 0.00838 O13 4 1.057514 0.069926 0.001149 11.00000 0.00909 0.01135 = 0.01078 0.00483 0.00190 0.00301 C12 1 0.703743 0.003008 -0.501862 11.00000 0.03858 0.03651 = 0.02158 0.00922 0.00402 0.01721 AFIX 43 H12 2 0.662501 0.043980 -0.473824 11.00000 -1.20000 AFIX 0 O12 4 0.977879 -0.091505 -0.138865 11.00000 0.02856 0.02831 = 0.01805 0.00642 0.00599 0.01818 C14 1 0.825535 0.003775 -0.388191 11.00000 0.02772 0.03549 = 0.02234 0.01427 0.00233 0.00744 O14 4 0.644063 -0.011619 0.003129 11.00000 0.00909 0.01135 = 0.01078 0.00483 0.00190 0.00301 C15 1 0.894251 -0.033555 -0.351368 11.00000 0.03707 0.03156 = 0.01759 0.00792 0.00042 0.00918 AFIX 43 H15 2 0.919900 -0.081044 -0.377439 11.00000 -1.20000 AFIX 0 O15 4 0.775244 0.107360 -0.028966 11.00000 0.00902 0.02242 = 0.01351 0.00905 0.00294 0.00447 C16 1 0.787890 0.073852 -0.346189 11.00000 0.05360 0.05793 = 0.02259 0.01957 0.01146 0.03337 AFIX 43 H16 2 0.742325 0.100299 -0.368779 11.00000 -1.20000 AFIX 0 C17 1 0.815426 0.105615 -0.272480 11.00000 0.04517 0.04777 = 0.02311 0.01204 0.00269 0.02376 AFIX 43 H17 2 0.787558 0.152372 -0.246256 11.00000 -1.20000 AFIX 0 C18 1 0.924744 -0.001483 -0.277318 11.00000 0.03650 0.03006 = 0.02249 0.00971 -0.00738 0.00556 AFIX 43 H18 2 0.972610 -0.026855 -0.254261 11.00000 -1.20000 AFIX 0 C19 1 0.884660 0.068007 -0.237252 11.00000 0.03485 0.03073 = 0.01502 0.01289 0.00235 0.00821 C20 1 0.921235 0.104523 -0.157804 11.00000 0.02044 0.03576 = 0.01011 0.00862 -0.00186 0.00684 O1W 4 1.171247 0.316288 -0.001672 11.00000 0.04046 0.04455 = 0.07647 0.03249 0.01389 0.00903 AFIX 7 H1WA 2 1.125366 0.357998 -0.001713 11.00000 -1.50000 H1WB 2 1.281787 0.336649 0.000458 11.00000 -1.50000 AFIX 0 C21 1 1.498777 0.919825 0.805486 11.00000 0.02112 0.02517 = 0.01825 0.00628 -0.00630 0.00604 C25 1 1.461950 0.826097 0.602799 11.00000 0.02596 0.04216 = 0.01547 0.01027 0.00580 0.00901 AFIX 43 H25 2 1.529383 0.817702 0.570317 11.00000 -1.20000 AFIX 0 C24 1 1.264639 0.858347 0.700523 11.00000 0.02040 0.04250 = 0.01662 0.01079 0.00467 0.00750 AFIX 43 H24 2 1.197200 0.870323 0.732778 11.00000 -1.20000 AFIX 0 C23 1 1.525629 0.870458 0.675878 11.00000 0.01215 0.03344 = 0.02240 0.00856 0.00089 0.00161 AFIX 43 H23 2 1.635276 0.891158 0.691787 11.00000 -1.20000 AFIX 0 C22 1 1.427333 0.884206 0.725390 11.00000 0.02025 0.02252 = 0.00746 0.00395 -0.00794 0.00116 C28 1 1.227770 0.733536 0.502344 11.00000 0.02044 0.02805 = 0.02027 0.00885 -0.00213 0.00883 C27 1 1.298478 0.794151 0.577774 11.00000 0.01820 0.02216 = 0.01708 0.00694 -0.00144 0.00808 C26 1 1.201416 0.814421 0.627328 11.00000 0.02135 0.03763 = 0.02305 0.00917 0.00251 0.00287 AFIX 43 H26 2 1.091692 0.798261 0.611205 11.00000 -1.20000 AFIX 0 C29 1 1.283702 0.735433 0.440547 11.00000 0.01860 0.02173 = 0.02208 0.00617 -0.00283 0.00417 C30 1 1.106402 0.667695 0.488833 11.00000 0.03017 0.03609 = 0.01746 0.01269 0.00110 0.00342 AFIX 43 H30 2 1.065346 0.663791 0.527187 11.00000 -1.20000 AFIX 0 C31 1 1.215876 0.671199 0.370665 11.00000 0.01868 0.02985 = 0.01687 0.00625 -0.00429 0.00956 C32 1 1.040439 0.605219 0.419117 11.00000 0.03053 0.02477 = 0.03029 0.00734 -0.00327 0.00175 AFIX 43 H32 2 0.957543 0.562459 0.414240 11.00000 -1.20000 AFIX 0 C33 1 1.089311 0.603375 0.359384 11.00000 0.02269 0.02226 = 0.01941 0.00444 0.00087 0.00388 C34 1 1.020575 0.532475 0.287632 11.00000 0.02307 0.01763 = 0.02569 0.00254 -0.00519 0.00140 C35 1 1.112208 0.501280 0.238627 11.00000 0.02313 0.02629 = 0.02538 0.00627 -0.00239 0.00328 AFIX 43 H35 2 1.218579 0.528591 0.246628 11.00000 -1.20000 AFIX 0 C36 1 0.859566 0.492367 0.271523 11.00000 0.03570 0.02600 = 0.02384 0.00124 0.00858 0.01174 AFIX 43 H36 2 0.794511 0.513836 0.302471 11.00000 -1.20000 AFIX 0 C37 1 1.046249 0.429536 0.177681 11.00000 0.02674 0.02377 = 0.02044 0.00511 0.00009 0.00437 AFIX 43 H37 2 1.109672 0.409122 0.145416 11.00000 -1.20000 AFIX 0 C38 1 0.795195 0.421270 0.210339 11.00000 0.02155 0.02245 = 0.03261 0.00283 0.00245 0.00195 AFIX 43 H38 2 0.687112 0.395964 0.200668 11.00000 -1.20000 AFIX 0 C39 1 0.886375 0.387023 0.163497 11.00000 0.03840 0.02042 = 0.01163 0.00451 -0.00367 0.01098 C40 1 0.822027 0.305483 0.101803 11.00000 0.03641 0.01684 = 0.04450 0.01869 -0.01610 -0.01103 C41 1 1.034630 -0.150585 -0.155759 11.00000 0.01934 0.02408 = 0.00581 0.00530 0.00085 0.00359 C42 1 0.967048 -0.215927 -0.231769 11.00000 0.01553 0.01842 = 0.01185 0.00075 -0.00489 0.00301 C43 1 0.846143 -0.209735 -0.273090 11.00000 0.02801 0.01997 = 0.01140 0.00012 -0.00495 0.01047 AFIX 43 H43 2 0.805763 -0.165367 -0.255115 11.00000 -1.20000 AFIX 0 C44 1 1.028861 -0.281876 -0.258093 11.00000 0.01503 0.02382 = 0.01981 0.00814 -0.00372 0.00640 AFIX 43 H44 2 1.113185 -0.285121 -0.229580 11.00000 -1.20000 AFIX 0 C45 1 0.965275 -0.342444 -0.326405 11.00000 0.02640 0.02633 = 0.02172 0.00662 0.00042 0.01394 AFIX 43 H45 2 1.005887 -0.386785 -0.343812 11.00000 -1.20000 AFIX 0 C46 1 0.782312 -0.269772 -0.342462 11.00000 0.02357 0.02495 = 0.02446 0.00900 -0.00422 0.00778 AFIX 43 H46 2 0.700628 -0.264443 -0.370749 11.00000 -1.20000 AFIX 0 C47 1 0.837413 -0.336894 -0.370153 11.00000 0.02159 0.02505 = 0.01536 0.00644 -0.00114 0.00705 C48 1 0.768743 -0.400755 -0.442288 11.00000 0.02606 0.02946 = 0.01894 0.00601 -0.00290 0.00881 C49 1 0.706824 -0.382523 -0.498830 11.00000 0.02256 0.02352 = 0.01725 0.00176 -0.00220 0.00205 C50 1 0.752753 -0.480072 -0.460494 11.00000 0.03269 0.02816 = 0.02292 0.00353 -0.01028 0.00849 AFIX 43 H50 2 0.790342 -0.494591 -0.425478 11.00000 -1.20000 AFIX 0 C51 1 0.681438 -0.541644 -0.530378 11.00000 0.03361 0.02205 = 0.01855 0.00183 -0.00465 0.00729 AFIX 43 H51 2 0.674079 -0.594660 -0.538797 11.00000 -1.20000 AFIX 0 C52 1 0.638343 -0.445213 -0.568947 11.00000 0.02379 0.02502 = 0.02466 0.00562 0.00143 0.00912 C53 1 0.622767 -0.527441 -0.586195 11.00000 0.01958 0.01771 = 0.01493 -0.00145 -0.00239 0.00529 C54 1 0.329300 -0.777518 -0.867662 11.00000 0.02059 0.01559 = 0.01567 0.00898 0.00168 0.00612 C55 1 0.413019 -0.713890 -0.795819 11.00000 0.01868 0.01541 = 0.01889 0.01178 0.00078 0.00300 C56 1 0.535313 -0.720943 -0.755082 11.00000 0.01764 0.01555 = 0.02110 0.00075 0.00486 0.00489 AFIX 43 H56 2 0.571928 -0.766567 -0.773114 11.00000 -1.20000 AFIX 0 C57 1 0.360009 -0.644890 -0.769466 11.00000 0.02917 0.02211 = 0.01730 0.00043 -0.00729 0.01185 AFIX 43 H57 2 0.279078 -0.638986 -0.797679 11.00000 -1.20000 AFIX 0 C58 1 0.428255 -0.585814 -0.701583 11.00000 0.02711 0.02439 = 0.02581 0.00424 -0.00290 0.00986 AFIX 43 H58 2 0.391447 -0.540232 -0.683794 11.00000 -1.20000 AFIX 0 C59 1 0.605392 -0.660229 -0.686752 11.00000 0.02036 0.02233 = 0.01936 0.00154 -0.00272 0.00658 AFIX 43 H59 2 0.689643 -0.665232 -0.659585 11.00000 -1.20000 AFIX 0 C60 1 0.551246 -0.592437 -0.658689 11.00000 0.02490 0.02667 = 0.01339 0.00345 -0.00204 0.00660 O11 4 1.138654 -0.157949 -0.117375 11.00000 0.02105 0.03258 = 0.02746 0.00355 -0.01488 0.00844 HKLF 4 REM 1_a.res in P-1 New: P-1 REM wR2 = 0.1535, GooF = S = 1.036, Restrained GooF = 1.036 for all data REM R1 = 0.0562 for 10392 Fo > 4sig(Fo) and 0.0786 for all 13756 data REM 788 parameters refined using 12 restraints END WGHT 0.0824 14.5807 REM Highest difference peak 4.589, deepest hole -2.938, 1-sigma level 0.259 Q1 1 0.7932 -0.0748 -0.0941 11.00000 0.05 4.59 Q2 1 0.8471 0.0353 -0.0539 11.00000 0.05 4.23 Q3 1 0.6250 0.1700 0.0747 11.00000 0.05 4.14 Q4 1 0.5605 0.0580 0.0299 11.00000 0.05 3.83 Q5 1 0.6611 0.1030 0.0225 11.00000 0.05 3.81 Q6 1 0.9977 0.1371 -0.0206 11.00000 0.05 3.80 Q7 1 1.1129 0.1919 -0.0291 11.00000 0.05 3.48 Q8 1 1.0647 0.2468 0.0184 11.00000 0.05 3.31 Q9 1 0.7393 -0.0118 -0.0400 11.00000 0.05 3.06 Q10 1 0.5113 0.1317 0.0888 11.00000 0.05 2.73 ; _shelx_res_checksum 53736 _shelx_hkl_file ; -2 0 0 37.00 6.50 -2 0 0 29.60 7.00 -2 0 0 31.50 7.00 2 0 0 37.10 7.20 -3 0 0 239.18 13.50 -3 0 0 251.27 13.50 -3 0 0 267.67 21.20 -3 0 0 242.78 18.70 -3 0 0 229.68 18.80 3 0 0 273.57 13.70 3 0 0 222.08 17.50 3 0 0 263.47 20.80 -4 0 0 188.78 12.00 -4 0 0 195.88 22.60 -4 0 0 195.48 18.20 -4 0 0 164.88 11.50 4 0 0 182.48 12.00 4 0 0 174.88 20.80 4 0 0 167.68 20.20 -5 0 0 1743.23 79.89 -5 0 0 1859.21 93.09 -5 0 0 1844.72 88.39 5 0 0 1855.81 91.39 5 0 0 1827.72 89.69 -6 0 0 4.50 5.30 -6 0 0 -2.50 9.90 -6 0 0 16.30 5.30 -7 0 0 -2.00 4.90 -7 0 0 9.60 12.40 -7 0 0 6.50 6.20 7 0 0 10.80 15.00 -8 0 0 79.09 20.00 -8 0 0 93.89 12.10 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17.90 2 -3 22 168.08 40.50 -3 3 -22 -4.80 9.50 -3 3 -22 17.00 19.70 3 -3 22 45.70 25.50 -4 3 -22 -11.70 19.60 -4 3 -22 -9.80 14.10 4 -3 22 101.59 29.10 -7 -2 22 76.19 52.39 6 2 -22 270.87 32.10 -6 -2 22 207.38 49.90 5 2 -22 2.00 11.40 -5 -2 22 -0.90 33.90 4 2 -22 36.70 10.90 -4 -2 22 5.50 33.60 3 2 -22 179.58 25.70 3 2 -22 156.18 21.40 -3 -2 22 163.18 46.40 2 2 -22 31.20 14.50 2 2 -22 2.80 12.20 -2 -2 22 26.20 32.30 1 2 -22 419.76 38.00 -1 -2 22 406.56 62.59 0 2 -22 16.50 16.30 0 2 -22 24.10 11.80 0 -2 22 5.60 28.70 -1 2 -22 246.78 35.40 -1 2 -22 267.07 26.30 1 -2 22 207.48 42.20 -2 2 -22 79.29 15.80 -2 2 -22 70.89 24.60 2 -2 22 137.59 35.60 -3 2 -22 -3.00 9.50 -3 2 -22 -21.70 17.50 3 -2 22 35.60 26.00 7 1 -22 102.49 37.90 6 1 -22 537.15 44.50 -6 -1 22 613.34 82.29 5 1 -22 13.00 9.30 5 1 -22 -7.00 12.40 -5 -1 22 -39.10 30.80 4 1 -22 99.29 20.80 4 1 -22 115.19 17.90 -4 -1 22 106.79 42.90 3 1 -22 -18.10 11.60 3 1 -22 -8.40 11.60 -3 -1 22 5.80 32.00 2 1 -22 20.20 13.40 2 1 -22 -1.50 13.70 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149.09 44.40 3 -3 -22 -0.40 12.90 3 -3 -22 4.10 17.70 -3 3 22 -19.10 28.30 2 -3 -22 128.89 20.40 2 -3 -22 91.59 32.70 -2 3 22 82.29 35.30 1 -3 -22 18.70 12.30 1 -3 -22 17.30 20.30 -1 3 22 -11.30 26.80 -1 3 22 14.00 12.10 0 -3 -22 196.78 23.70 0 3 22 237.18 57.79 0 3 22 238.18 27.30 -5 4 22 38.80 62.09 4 -4 -22 0.20 17.00 4 -4 -22 -7.30 12.30 -4 4 22 -39.10 27.20 -4 4 22 -8.40 10.90 3 -4 -22 5.70 13.10 3 -4 -22 10.20 19.10 -3 4 22 15.60 30.30 -3 4 22 34.20 15.20 2 -4 -22 423.86 37.30 -2 4 22 454.25 60.09 -2 4 22 495.85 40.30 1 -4 -22 76.59 25.30 1 -4 -22 73.59 16.80 -1 4 22 76.09 18.10 0 20 -23 77.99 23.60 0 -20 23 -7.20 30.90 -1 20 -23 61.09 23.30 1 -20 23 16.50 31.30 -2 -19 23 4.20 29.20 -1 -19 23 -18.30 29.30 0 19 -23 51.49 29.00 -1 19 -23 346.07 39.00 1 -19 23 219.68 44.00 -2 19 -23 15.10 17.10 -2 19 -23 3.60 16.60 2 -19 23 -14.60 27.30 2 18 -23 40.30 22.80 -2 -18 23 41.00 30.30 1 18 -23 62.59 21.20 -1 -18 23 35.60 32.80 0 18 -23 47.10 19.80 0 -18 23 -21.00 27.60 -1 18 -23 454.05 41.00 1 -18 23 303.27 54.59 -2 18 -23 272.97 38.70 -2 18 -23 190.48 29.40 2 -18 23 164.48 39.70 -3 18 -23 48.40 20.00 -3 18 -23 10.20 17.10 3 -18 23 6.50 24.10 3 17 -23 136.99 33.70 -3 -17 23 91.89 36.80 2 17 -23 89.89 21.50 -2 -17 23 54.89 33.00 1 17 -23 91.69 22.40 -1 -17 23 12.40 29.90 0 17 -23 -0.50 14.90 0 -17 23 -22.80 28.40 -1 17 -23 77.89 21.40 1 -17 23 33.80 31.20 -2 17 -23 90.89 22.80 -2 17 -23 70.89 18.40 2 -17 23 21.40 28.70 -3 17 -23 318.37 37.60 -3 17 -23 343.67 36.80 3 -17 23 335.27 47.80 -4 17 -23 60.79 21.90 -4 17 -23 39.10 20.40 4 -17 23 89.09 25.00 -4 -16 23 -21.00 26.90 3 16 -23 13.70 17.30 -3 -16 23 -13.40 26.30 2 16 -23 242.38 34.50 -2 -16 23 237.28 44.10 1 16 -23 21.50 17.00 -1 -16 23 -27.50 28.70 0 16 -23 3.70 16.70 0 -16 23 -26.80 26.10 -1 16 -23 18.90 14.90 -1 16 -23 14.00 17.80 1 -16 23 -1.00 28.60 -2 16 -23 -8.60 14.90 2 -16 23 -35.30 23.70 -3 16 -23 723.53 52.49 -3 16 -23 756.82 53.29 3 -16 23 674.63 63.79 -4 16 -23 175.58 28.30 -4 16 -23 154.58 27.90 4 15 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33.20 4 13 -23 26.40 16.10 -4 -13 23 1.20 26.40 3 13 -23 39.70 18.70 -3 -13 23 37.50 31.50 2 13 -23 52.69 19.40 -2 -13 23 8.40 29.00 1 13 -23 -9.90 12.90 -1 -13 23 -21.70 30.20 0 13 -23 467.25 39.60 0 -13 23 418.56 77.29 -1 13 -23 396.96 37.20 1 -13 23 319.37 55.49 -2 13 -23 4.60 13.90 -2 13 -23 -12.50 13.00 2 -13 23 -30.70 25.70 -3 13 -23 51.89 19.70 -3 13 -23 114.79 20.50 3 -13 23 89.19 34.10 -4 13 -23 4.80 16.80 -4 13 -23 54.39 17.50 5 12 -23 134.49 25.20 -5 -12 23 146.89 39.60 4 12 -23 263.97 32.90 -4 -12 23 203.08 46.00 3 12 -23 58.39 19.60 -3 -12 23 77.49 33.70 2 12 -23 44.40 19.00 -2 -12 23 22.70 29.40 1 12 -23 62.49 19.10 -1 -12 23 30.00 32.40 0 12 -23 149.49 23.30 0 12 -23 120.09 19.70 -1 12 -23 295.27 32.10 -1 12 -23 289.57 39.90 1 -12 23 353.86 60.59 -2 12 -23 51.69 17.30 -2 12 -23 84.89 19.10 2 -12 23 60.39 41.40 -3 12 -23 -5.50 15.10 -3 12 -23 -8.20 13.90 -4 12 -23 92.89 19.40 -4 12 -23 68.59 23.10 4 -12 23 121.09 31.00 -6 -11 23 193.18 63.99 5 11 -23 29.70 16.60 -5 -11 23 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-0.1803 9 -3 8 -4.4947 -0.0716 9 -3 9 -2.9019 -0.0810 9 -3 10 9.8201 -0.1740 9 -3 11 13.0915 0.5398 9 -3 12 0.5848 1.4874 9 -2 0 -1.5624 -0.0235 9 -2 1 0.0592 -0.0386 9 -2 2 -0.8767 0.0007 9 -2 3 0.9506 0.0271 9 -2 4 5.4322 0.0400 9 -2 5 6.4299 0.0526 9 -2 6 5.0927 0.0973 9 -2 7 6.8282 0.1391 9 -2 8 5.4837 0.1481 9 -2 9 -5.1506 0.1695 9 -2 10 -10.7448 -0.0579 9 -2 11 -0.9957 -0.5501 9 -1 0 0.5078 -0.0581 9 -1 1 0.7752 -0.0427 9 -1 2 -0.4524 0.0741 9 -1 3 -5.2668 0.1362 9 -1 4 -6.5805 0.1365 9 -1 5 -3.5721 0.1969 9 -1 6 -3.6432 0.1941 9 -1 7 -5.1567 0.0699 9 -1 8 -0.1438 -0.0271 9 -1 9 5.1049 -0.0954 9 -1 10 -0.2701 -0.1915 9 -1 11 -7.0057 -0.3270 9 0 0 -0.6613 -0.0294 9 0 1 -2.1237 -0.0922 9 0 2 0.3212 -0.1107 9 0 3 1.6564 -0.0454 9 0 4 -1.6905 -0.0857 9 0 5 -2.6165 -0.1879 9 0 6 1.3991 -0.1530 9 0 7 2.6917 -0.1171 9 0 8 0.6662 -0.1069 9 0 9 3.1562 0.1463 9 0 10 7.1386 0.5276 9 1 0 3.9265 0.0495 9 1 1 5.2580 -0.0660 9 1 2 4.4302 -0.1529 9 1 3 5.9836 -0.1413 9 1 4 6.5892 -0.1151 9 1 5 1.8439 -0.1621 9 1 6 -3.2663 -0.0945 9 1 7 -4.8343 0.1727 9 1 8 -6.7961 0.2565 9 1 9 -8.6521 0.0270 9 2 0 -6.1976 0.2020 9 2 1 -6.7204 0.2161 9 2 2 -6.2339 -0.0103 9 2 3 -6.0434 -0.0721 9 2 4 -2.8368 0.1683 9 2 5 2.4043 0.3070 9 2 6 5.8976 0.0790 9 2 7 8.4999 -0.2055 9 2 8 10.0182 -0.2636 9 3 0 4.8663 -0.1953 9 3 1 3.2418 0.1349 9 3 2 2.0192 0.4225 9 3 3 1.8124 0.2463 9 3 4 -0.1873 -0.0351 9 3 5 -3.5130 -0.0678 9 3 6 -6.6784 -0.0204 9 3 7 -8.4508 -0.0492 9 4 0 -1.2978 -0.0380 9 4 1 1.8650 -0.1884 9 4 2 0.6528 -0.1488 9 4 3 -1.8294 -0.1028 9 4 4 -0.4605 -0.1972 9 4 5 3.2868 -0.1334 9 4 6 5.2021 0.0893 9 5 0 -2.3859 -0.0595 9 5 1 -2.9814 -0.3273 9 5 2 2.0054 -0.3098 9 5 3 3.9506 0.0548 9 5 4 0.0546 0.2105 9 5 5 -3.2092 0.0611 9 6 0 3.7003 0.2289 9 6 1 -0.3615 0.3955 9 6 2 -5.4602 0.1956 9 6 3 -3.6954 0.0497 9 7 0 -1.7518 -0.0143 9 7 1 3.7539 0.0776 9 7 2 5.8247 -0.0113 9 8 0 0.0914 -0.2533 10 -16 2 -0.0688 -0.4476 10 -16 3 3.0595 0.4587 10 -16 4 1.8387 0.0673 10 -16 5 -1.7128 -1.0777 10 -15 0 3.1812 1.7927 10 -15 1 2.9395 0.8518 10 -15 2 -0.3364 -0.0216 10 -15 3 -0.3440 0.1370 10 -15 4 3.6770 0.7098 10 -15 5 5.2737 1.1310 10 -15 6 5.2468 1.0473 10 -15 7 7.2331 0.5051 10 -14 0 -3.5991 -0.5754 10 -14 1 -1.9392 0.1586 10 -14 2 -1.3461 0.0664 10 -14 3 -5.0379 -0.0660 10 -14 4 -6.1822 0.0165 10 -14 5 -3.2458 0.0528 10 -14 6 -4.0570 0.1617 10 -14 7 -6.2577 0.5700 10 -14 8 -1.7226 1.1937 10 -14 9 3.1314 1.2781 10 -13 0 1.6183 -0.4533 10 -13 1 1.2133 -0.3075 10 -13 2 4.2213 -0.3030 10 -13 3 5.3980 -0.5178 10 -13 4 0.0735 -0.4865 10 -13 5 -2.8963 -0.2301 10 -13 6 1.3566 -0.1362 10 -13 7 2.1108 -0.4685 10 -13 8 -3.7402 -0.5835 10 -13 9 -5.1132 0.5122 10 -12 0 -0.8907 -0.0228 10 -12 1 -3.2013 0.0184 10 -12 2 -4.2845 0.2000 10 -12 3 1.0795 0.0254 10 -12 4 7.2841 -0.2392 10 -12 5 4.7971 -0.3555 10 -12 6 -0.7629 -0.2065 10 -12 7 1.2364 0.0365 10 -12 8 5.6481 -0.5036 10 -12 9 3.3977 -1.5965 10 -12 10 -1.9310 -1.4682 10 -11 0 4.6059 0.4762 10 -11 1 5.0007 0.1499 10 -11 2 0.2648 0.3279 10 -11 3 -6.4527 0.4987 10 -11 4 -6.9553 0.2989 10 -11 5 -0.8068 0.0640 10 -11 6 2.1476 -0.1603 10 -11 7 -1.7059 -0.0848 10 -11 8 -4.3408 0.4704 10 -11 9 -1.5200 0.5016 10 -11 10 2.3847 -0.3147 10 -10 0 -7.2495 0.0236 10 -10 1 -2.3874 0.0332 10 -10 2 3.6776 -0.1117 10 -10 3 5.4006 0.1227 10 -10 4 1.0101 0.3163 10 -10 5 -4.4066 0.3141 10 -10 6 -3.6346 0.2897 10 -10 7 2.3572 0.1043 10 -10 8 5.7141 0.0811 10 -10 9 3.5564 0.4093 10 -10 10 -0.6937 0.2889 10 -9 0 3.7949 -0.4006 10 -9 1 -2.2468 -0.3128 10 -9 2 -4.3840 -0.3676 10 -9 3 -1.4856 -0.2733 10 -9 4 4.2440 0.0190 10 -9 5 6.8619 0.1308 10 -9 6 1.2252 0.1434 10 -9 7 -7.4045 0.0892 10 -9 8 -9.2614 -0.1344 10 -9 9 -3.2851 -0.0453 10 -9 10 4.5559 0.3449 10 -8 0 1.1550 0.0390 10 -8 1 4.6349 0.1334 10 -8 2 3.9094 -0.0518 10 -8 3 -0.5823 -0.4178 10 -8 4 -5.5526 -0.4402 10 -8 5 -3.8437 -0.2668 10 -8 6 5.0399 -0.2051 10 -8 7 10.1216 -0.0875 10 -8 8 5.0501 -0.0719 10 -8 9 -4.8602 -0.1873 10 -8 10 -11.6723 0.1249 10 -7 0 -2.8941 0.2301 10 -7 1 -5.4065 0.1865 10 -7 2 -4.2415 0.3618 10 -7 3 0.3887 0.2094 10 -7 4 3.2597 -0.1308 10 -7 5 -0.3075 -0.1602 10 -7 6 -4.4466 -0.0635 10 -7 7 -1.5729 0.0140 10 -7 8 5.2466 0.1660 10 -7 9 10.1923 -0.0141 10 -7 10 10.1604 -0.3488 10 -6 0 2.7414 0.0070 10 -6 1 4.8395 -0.0005 10 -6 2 3.0644 0.1645 10 -6 3 -0.9532 0.4265 10 -6 4 -3.3538 0.3645 10 -6 5 -4.0520 0.1590 10 -6 6 -6.1102 0.0817 10 -6 7 -7.5187 -0.0996 10 -6 8 -5.7201 -0.1900 10 -6 9 -3.2652 0.0310 10 -6 10 -0.8362 -0.1058 10 -5 0 -0.6182 -0.1561 10 -5 1 -0.4598 -0.2201 10 -5 2 1.5564 -0.2530 10 -5 3 5.1089 -0.0512 10 -5 4 9.5515 0.1341 10 -5 5 12.4785 0.0158 10 -5 6 10.0678 -0.0371 10 -5 7 2.3225 0.1319 10 -5 8 -3.9975 0.0151 10 -5 9 -5.6411 -0.2079 10 -4 0 -3.7619 -0.0138 10 -4 1 -5.0163 -0.0600 10 -4 2 -6.2219 -0.2678 10 -4 3 -10.0211 -0.3624 10 -4 4 -13.4473 -0.1185 10 -4 5 -10.0462 0.1360 10 -4 6 -0.4600 0.0163 10 -4 7 6.1635 -0.0439 10 -4 8 6.0756 0.3560 10 -4 9 5.2154 0.5979 10 -3 0 4.8514 0.1634 10 -3 1 5.2381 0.2617 10 -3 2 6.9156 0.2038 10 -3 3 10.1103 -0.0213 10 -3 4 7.9671 -0.2109 10 -3 5 -0.3171 -0.1090 10 -3 6 -4.5397 0.1215 10 -3 7 -0.0196 -0.0893 10 -3 8 3.0273 -0.5736 10 -2 0 -0.2957 -0.1072 10 -2 1 -1.6641 0.0350 10 -2 2 -5.1388 0.1903 10 -2 3 -5.6469 0.1786 10 -2 4 -0.0222 0.0999 10 -2 5 2.6295 -0.0361 10 -2 6 -5.1778 -0.0114 10 -2 7 -12.8344 0.3778 10 -1 0 -3.1278 -0.1819 10 -1 1 0.0959 -0.2554 10 -1 2 2.5350 -0.0063 10 -1 3 -0.6173 0.1033 10 -1 4 -3.5612 -0.0272 10 -1 5 3.8066 -0.1233 10 -1 6 15.1582 -0.3598 10 -1 7 14.2933 -0.6468 10 0 0 2.8122 0.3698 10 0 1 1.5919 -0.0653 10 0 2 3.9384 -0.3506 10 0 3 8.3736 -0.1292 10 0 4 4.2451 0.0181 10 0 5 -8.5130 0.0446 10 0 6 -13.5270 0.3484 10 1 0 -4.2876 0.0255 10 1 1 -6.9714 0.4179 10 1 2 -12.4497 0.2274 10 1 3 -12.9889 0.1289 10 1 4 -1.9505 0.4450 10 1 5 8.4845 0.4392 10 2 0 6.4104 -0.3326 10 2 1 9.7119 -0.0407 10 2 2 13.7184 0.1430 10 2 3 8.6050 -0.3157 10 2 4 -2.8595 -0.7048 10 3 0 -2.2549 -0.4350 10 3 1 -4.8829 -0.6947 10 3 2 -6.8393 -0.2587 10 4 0 -4.4879 1.3296 10 4 1 -0.0522 0.6275 11 -11 0 3.0606 0.2016 11 -11 1 1.4716 -0.3961 11 -11 2 -0.0171 -0.7934 11 -10 0 0.2264 0.7273 11 -10 1 1.1376 0.7626 11 -10 2 1.7476 1.0741 11 -10 3 3.6913 1.2632 11 -10 4 4.7003 0.5995 11 -9 0 -2.3091 -0.0272 11 -9 1 -0.8595 -0.0708 11 -9 2 -2.6162 -0.3706 11 -9 3 -5.5730 -0.0321 11 -9 4 -4.6628 0.5273 11 -8 0 -0.5630 -0.4338 11 -8 1 -1.2162 -0.0798 11 -8 2 2.9475 -0.1112 11 -8 3 4.1063 -0.3357 11 -8 4 1.2798 -0.0412 11 -7 0 4.4639 -0.2210 11 -7 1 1.1150 -0.1236 11 -7 2 -1.6980 0.0393 11 -7 3 1.1661 -0.1942 11 -7 4 3.1036 -0.4034 11 -6 0 -4.1098 0.0781 11 -6 1 0.0340 -0.1938 11 -6 2 -2.7454 0.0338 11 -6 3 -6.8220 0.1410 11 -6 4 -4.6086 -0.3063 11 -5 0 0.1985 0.5876 11 -5 1 0.5473 0.2089 11 -5 2 6.2851 -0.0534 11 -5 3 6.4879 0.2441 11 -5 4 0.9930 0.5815 11 -4 0 3.1540 0.0030 11 -4 1 -0.7439 0.3104 11 -4 2 -3.5821 0.1131 11 -4 3 -0.6696 -0.0388 11 -3 0 -3.4653 -0.5871 11 -3 1 -1.0143 -0.1662 11 -3 2 -1.3184 -0.1207 11 -2 0 0.8981 -0.4038 11 -2 1 1.5868 -0.4303 11 -1 0 1.7199 1.3673 0 0 0 0.0 0.0 ; _shelx_fab_checksum 53923 _platon_squeeze_void_probe_radius 1.20 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 Tb1 Tb 0.60065(4) 0.11823(2) 0.05222(2) 0.01453(10) Uani 1 1 d . . . . . S1 S 0.9831(4) -0.19038(18) -0.56569(13) 0.0442(7) Uani 1 1 d . . . . . N1 N 0.8833(10) -0.1753(5) -0.6258(4) 0.0335(18) Uani 1 1 d . . . . . O1 O 0.5141(7) -0.1328(4) -0.9521(3) 0.0287(14) Uani 1 1 d . . . . . C1 C 0.6236(9) -0.1517(5) -0.9260(4) 0.0182(16) Uani 1 1 d . U . . . Tb2 Tb 0.82318(4) -0.02122(2) -0.07393(2) 0.01446(10) Uani 1 1 d . . . . . S2 S 1.4084(3) 0.77050(15) 0.35738(13) 0.0353(5) Uani 1 1 d . . . . . N2 N 0.9455(10) -0.1274(5) -0.4941(4) 0.0353(19) Uani 1 1 d . . . . . O2 O 0.7261(7) -0.1792(4) -0.9583(3) 0.0320(15) Uani 1 1 d . . . . . C2 C 0.6384(10) -0.1404(5) -0.8493(4) 0.0226(17) Uani 1 1 d . . . . . Tb3 Tb 1.03786(4) 0.18880(2) -0.00576(2) 0.01686(10) Uani 1 1 d . . . . . S3 S 0.6415(4) -0.32090(16) -0.57259(14) 0.0447(7) Uani 1 1 d . . . . . N3 N 1.2787(9) 0.6838(5) 0.3188(4) 0.0307(17) Uani 1 1 d . . . . . O3 O 0.9165(8) 0.1760(4) -0.1211(3) 0.0324(15) Uani 1 1 d . . . . . C3 C 0.7272(12) -0.1766(6) -0.8226(5) 0.037(2) Uani 1 1 d . . . . . H3 H 0.773008 -0.213476 -0.853399 0.045 Uiso 1 1 calc R U . . . N4 N 1.3954(9) 0.7962(4) 0.4400(4) 0.0293(17) Uani 1 1 d . . . . . O4 O 0.9628(7) 0.0641(4) -0.1260(3) 0.0232(12) Uani 1 1 d . . . . . C4 C 0.5605(13) -0.0912(7) -0.8042(5) 0.042(3) Uani 1 1 d . . . . . H4 H 0.490327 -0.069589 -0.821948 0.050 Uiso 1 1 calc R U . . . N5 N 0.7173(10) -0.3088(5) -0.4944(4) 0.0339(18) Uani 1 1 d . . . . . O5 O 1.6471(7) 0.9509(4) 0.8236(3) 0.0293(14) Uani 1 1 d . . . . . C5 C 0.5884(13) -0.0743(7) -0.7316(5) 0.043(3) Uani 1 1 d . . . . . H5 H 0.538230 -0.039657 -0.701140 0.051 Uiso 1 1 calc R U . . . N6 N 0.5933(10) -0.4166(5) -0.6170(4) 0.0329(18) Uani 1 1 d . . . . . O6 O 1.4089(7) 0.9133(4) 0.8466(3) 0.0293(14) Uani 1 1 d . . . . . C6 C 0.7516(12) -0.1606(6) -0.7513(5) 0.038(2) Uani 1 1 d . . . . . H6 H 0.813556 -0.186888 -0.735177 0.046 Uiso 1 1 calc R U . . . O7 O 0.6900(7) 0.2617(3) 0.0972(3) 0.0251(13) Uani 1 1 d . . . . . C7 C 0.6876(10) -0.1071(5) -0.7032(4) 0.0233(17) Uani 1 1 d . . . . . O8 O 0.9138(7) 0.2831(4) 0.0573(3) 0.0326(15) Uani 1 1 d . . . . . C8 C 0.7228(10) -0.0819(5) -0.6244(4) 0.0242(18) Uani 1 1 d . . . . . O9 O 0.3705(7) -0.8421(3) -0.8936(3) 0.0227(12) Uani 1 1 d . . . . . C9 C 0.6705(11) -0.0227(6) -0.5764(4) 0.031(2) Uani 1 1 d . . . . . H9 H 0.608620 0.002330 -0.594341 0.037 Uiso 1 1 calc R U . . . C10 C 0.8182(10) -0.1163(5) -0.5906(4) 0.0240(18) Uani 1 1 d . . . . . O10 O 0.2098(6) -0.7672(3) -0.8969(3) 0.0225(12) Uani 1 1 d . . . . . C11 C 0.8516(10) -0.0896(5) -0.5143(4) 0.0244(18) Uani 1 1 d . . . . . C13 C 0.7922(10) -0.0277(5) -0.4674(4) 0.0258(18) Uani 1 1 d . . . . . O13 O 1.0575(5) 0.0699(3) 0.0011(3) 0.0104(7) Uani 1 1 d . U . . . C12 C 0.7037(11) 0.0030(6) -0.5019(5) 0.032(2) Uani 1 1 d . . . . . H12 H 0.662501 0.043980 -0.473824 0.039 Uiso 1 1 calc R U . . . O12 O 0.9779(7) -0.0915(3) -0.1389(3) 0.0244(13) Uani 1 1 d . . . . . C14 C 0.8255(11) 0.0038(6) -0.3882(5) 0.0284(19) Uani 1 1 d . . . . . O14 O 0.6441(5) -0.0116(3) 0.0031(3) 0.0104(7) Uani 1 1 d . . . . . C15 C 0.8943(11) -0.0336(6) -0.3514(5) 0.030(2) Uani 1 1 d . . . . . H15 H 0.919900 -0.081044 -0.377439 0.036 Uiso 1 1 calc R U . . . O15 O 0.7752(6) 0.1074(3) -0.0290(3) 0.0145(10) Uani 1 1 d . . . . . C16 C 0.7879(13) 0.0739(7) -0.3462(5) 0.041(3) Uani 1 1 d . . . . . H16 H 0.742325 0.100299 -0.368779 0.049 Uiso 1 1 calc R U . . . C17 C 0.8154(12) 0.1056(6) -0.2725(5) 0.038(2) Uani 1 1 d . . . . . H17 H 0.787558 0.152372 -0.246256 0.046 Uiso 1 1 calc R U . . . C18 C 0.9247(11) -0.0015(6) -0.2773(5) 0.032(2) Uani 1 1 d . . . . . H18 H 0.972610 -0.026855 -0.254261 0.038 Uiso 1 1 calc R U . . . C19 C 0.8847(11) 0.0680(5) -0.2373(4) 0.0262(18) Uani 1 1 d . . . . . C20 C 0.9212(10) 0.1045(5) -0.1578(4) 0.0231(17) Uani 1 1 d . . . . . O1W O 1.1712(9) 0.3163(4) -0.0017(5) 0.052(2) Uani 1 1 d . . . . . H1WA H 1.125366 0.357998 -0.001713 0.078 Uiso 1 1 d R U . . . H1WB H 1.281787 0.336649 0.000458 0.078 Uiso 1 1 d R U . . . C21 C 1.4988(10) 0.9198(5) 0.8055(4) 0.0234(17) Uani 1 1 d . . . . . C25 C 1.4619(10) 0.8261(6) 0.6028(4) 0.0286(19) Uani 1 1 d . . . . . H25 H 1.529383 0.817702 0.570317 0.034 Uiso 1 1 calc R U . . . C24 C 1.2646(10) 0.8583(6) 0.7005(4) 0.0273(19) Uani 1 1 d . . . . . H24 H 1.197200 0.870323 0.732778 0.033 Uiso 1 1 calc R U . . . C23 C 1.5256(9) 0.8705(5) 0.6759(4) 0.0249(18) Uani 1 1 d . . . . . H23 H 1.635276 0.891158 0.691787 0.030 Uiso 1 1 calc R U . . . C22 C 1.4273(9) 0.8842(5) 0.7254(4) 0.0192(16) Uani 1 1 d . . . . . C28 C 1.2278(10) 0.7335(5) 0.5023(4) 0.0236(17) Uani 1 1 d . . . . . C27 C 1.2985(9) 0.7942(5) 0.5778(4) 0.0197(16) Uani 1 1 d . . . . . C26 C 1.2014(11) 0.8144(6) 0.6273(5) 0.030(2) Uani 1 1 d . . . . . H26 H 1.091692 0.798261 0.611205 0.036 Uiso 1 1 calc R U . . . C29 C 1.2837(9) 0.7354(5) 0.4405(4) 0.0227(17) Uani 1 1 d . . . . . C30 C 1.1064(11) 0.6677(5) 0.4888(5) 0.0288(19) Uani 1 1 d . . . . . H30 H 1.065346 0.663791 0.527187 0.035 Uiso 1 1 calc R U . . . C31 C 1.2159(9) 0.6712(5) 0.3707(4) 0.0233(17) Uani 1 1 d . . . . . C32 C 1.0404(11) 0.6052(5) 0.4191(5) 0.032(2) Uani 1 1 d . . . . . H32 H 0.957543 0.562459 0.414240 0.038 Uiso 1 1 calc R U . . . C33 C 1.0893(10) 0.6034(5) 0.3594(4) 0.0237(17) Uani 1 1 d . . . . . C34 C 1.0206(10) 0.5325(5) 0.2876(5) 0.0260(18) Uani 1 1 d . . . . . C35 C 1.1122(10) 0.5013(5) 0.2386(5) 0.0278(19) Uani 1 1 d . . . . . H35 H 1.218579 0.528591 0.246628 0.033 Uiso 1 1 calc R U . . . C36 C 0.8596(11) 0.4924(5) 0.2715(5) 0.031(2) Uani 1 1 d . . . . . H36 H 0.794511 0.513836 0.302471 0.037 Uiso 1 1 calc R U . . . C37 C 1.0462(10) 0.4295(5) 0.1777(5) 0.0260(18) Uani 1 1 d . . . . . H37 H 1.109672 0.409122 0.145416 0.031 Uiso 1 1 calc R U . . . C38 C 0.7952(10) 0.4213(5) 0.2103(5) 0.030(2) Uani 1 1 d . . . . . H38 H 0.687112 0.395964 0.200668 0.035 Uiso 1 1 calc R U . . . C39 C 0.8864(11) 0.3870(5) 0.1635(4) 0.0245(18) Uani 1 1 d . . . . . C40 C 0.8220(12) 0.3055(5) 0.1018(6) 0.036(2) Uani 1 1 d . . . . . C41 C 1.0346(9) -0.1506(5) -0.1558(4) 0.0174(16) Uani 1 1 d . . . . . C42 C 0.9670(9) -0.2159(5) -0.2318(4) 0.0181(16) Uani 1 1 d . . . . . C43 C 0.8461(10) -0.2097(5) -0.2731(4) 0.0221(17) Uani 1 1 d . . . . . H43 H 0.805763 -0.165367 -0.255115 0.027 Uiso 1 1 calc R U . . . C44 C 1.0289(9) -0.2819(5) -0.2581(4) 0.0204(16) Uani 1 1 d . . . . . H44 H 1.113185 -0.285121 -0.229580 0.024 Uiso 1 1 calc R U . . . C45 C 0.9653(10) -0.3424(5) -0.3264(4) 0.0254(18) Uani 1 1 d . . . . . H45 H 1.005887 -0.386785 -0.343812 0.030 Uiso 1 1 calc R U . . . C46 C 0.7823(10) -0.2698(5) -0.3425(5) 0.0254(18) Uani 1 1 d . . . . . H46 H 0.700628 -0.264443 -0.370749 0.031 Uiso 1 1 calc R U . . . C47 C 0.8374(10) -0.3369(5) -0.3702(4) 0.0217(17) Uani 1 1 d . . . . . C48 C 0.7687(10) -0.4008(5) -0.4423(4) 0.0267(19) Uani 1 1 d . . . . . C49 C 0.7068(10) -0.3825(5) -0.4988(4) 0.0247(18) Uani 1 1 d . . . . . C50 C 0.7528(11) -0.4801(5) -0.4605(5) 0.032(2) Uani 1 1 d . . . . . H50 H 0.790342 -0.494591 -0.425478 0.038 Uiso 1 1 calc R U . . . C51 C 0.6814(11) -0.5416(5) -0.5304(4) 0.0280(19) Uani 1 1 d . . . . . H51 H 0.674079 -0.594660 -0.538797 0.034 Uiso 1 1 calc R U . . . C52 C 0.6383(10) -0.4452(5) -0.5689(5) 0.0261(18) Uani 1 1 d . . . . . C53 C 0.6228(9) -0.5274(5) -0.5862(4) 0.0208(17) Uani 1 1 d . . . . . C54 C 0.3293(9) -0.7775(4) -0.8677(4) 0.0165(15) Uani 1 1 d . . . . . C55 C 0.4130(9) -0.7139(4) -0.7958(4) 0.0167(15) Uani 1 1 d . . . . . C56 C 0.5353(9) -0.7209(5) -0.7551(4) 0.0204(16) Uani 1 1 d . . . . . H56 H 0.571928 -0.766567 -0.773114 0.025 Uiso 1 1 calc R U . . . C57 C 0.3600(10) -0.6449(5) -0.7695(4) 0.0258(18) Uani 1 1 d . . . . . H57 H 0.279078 -0.638986 -0.797679 0.031 Uiso 1 1 calc R U . . . C58 C 0.4283(10) -0.5858(5) -0.7016(5) 0.0282(19) Uani 1 1 d . . . . . H58 H 0.391447 -0.540232 -0.683794 0.034 Uiso 1 1 calc R U . . . C59 C 0.6054(10) -0.6602(5) -0.6868(4) 0.0237(18) Uani 1 1 d . . . . . H59 H 0.689643 -0.665232 -0.659585 0.028 Uiso 1 1 calc R U . . . C60 C 0.5512(10) -0.5924(5) -0.6587(4) 0.0240(18) Uani 1 1 d . . . . . O11 O 1.1387(7) -0.1579(4) -0.1174(3) 0.0316(15) 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 Tb1 0.01092(17) 0.01753(19) 0.01172(17) 0.00369(14) -0.00066(14) 0.00394(14) S1 0.0587(17) 0.0615(18) 0.0264(12) 0.0221(12) 0.0062(12) 0.0399(15) N1 0.049(5) 0.037(4) 0.022(4) 0.016(3) 0.004(4) 0.024(4) O1 0.026(3) 0.049(4) 0.022(3) 0.020(3) 0.008(3) 0.019(3) C1 0.012(3) 0.030(4) 0.009(3) 0.009(3) -0.006(3) 0.001(3) Tb2 0.01140(18) 0.01853(19) 0.01059(17) 0.00402(14) -0.00123(14) 0.00471(14) S2 0.0399(14) 0.0328(13) 0.0287(12) 0.0139(10) 0.0032(11) 0.0017(11) N2 0.036(4) 0.053(5) 0.024(4) 0.020(4) 0.002(4) 0.022(4) O2 0.024(3) 0.053(4) 0.022(3) 0.018(3) 0.006(3) 0.014(3) C2 0.026(4) 0.032(5) 0.017(4) 0.017(4) 0.006(3) 0.010(4) Tb3 0.01533(18) 0.01925(19) 0.01358(18) 0.00553(15) -0.00083(14) 0.00499(14) S3 0.072(2) 0.0317(13) 0.0288(13) 0.0119(11) -0.0030(13) 0.0192(13) N3 0.035(4) 0.031(4) 0.024(4) 0.011(3) 0.005(3) 0.006(3) O3 0.049(4) 0.032(4) 0.015(3) 0.010(3) 0.001(3) 0.014(3) C3 0.045(6) 0.051(6) 0.020(4) 0.010(4) 0.004(4) 0.034(5) N4 0.025(4) 0.027(4) 0.027(4) 0.008(3) -0.004(3) 0.003(3) O4 0.025(3) 0.035(3) 0.017(3) 0.018(3) 0.004(2) 0.011(3) C4 0.065(7) 0.063(7) 0.018(4) 0.024(5) 0.012(5) 0.044(6) N5 0.050(5) 0.026(4) 0.017(4) 0.004(3) -0.004(4) 0.010(4) O5 0.025(3) 0.032(3) 0.021(3) 0.010(3) -0.012(3) -0.002(3) C5 0.062(7) 0.056(7) 0.017(4) 0.011(4) 0.011(5) 0.039(6) N6 0.041(5) 0.032(4) 0.023(4) 0.010(3) -0.005(3) 0.015(4) O6 0.033(3) 0.047(4) 0.013(3) 0.014(3) 0.005(3) 0.018(3) C6 0.053(6) 0.058(7) 0.019(4) 0.021(5) 0.011(4) 0.037(5) O7 0.025(3) 0.025(3) 0.017(3) 0.002(2) 0.001(2) 0.007(3) C7 0.021(4) 0.033(5) 0.013(4) 0.008(3) -0.001(3) 0.008(4) O8 0.033(3) 0.027(3) 0.032(3) 0.003(3) 0.013(3) 0.014(3) C8 0.022(4) 0.037(5) 0.019(4) 0.019(4) 0.000(3) 0.005(4) O9 0.025(3) 0.017(3) 0.018(3) 0.002(2) 0.002(2) 0.003(2) C9 0.038(5) 0.044(6) 0.014(4) 0.013(4) 0.003(4) 0.015(4) C10 0.029(5) 0.028(4) 0.019(4) 0.013(4) 0.005(4) 0.010(4) O10 0.021(3) 0.025(3) 0.014(3) 0.003(2) -0.004(2) 0.006(2) C11 0.026(4) 0.033(5) 0.018(4) 0.015(4) 0.001(4) 0.009(4) C13 0.023(4) 0.037(5) 0.017(4) 0.012(4) -0.001(4) 0.008(4) O13 0.0091(10) 0.0114(10) 0.0108(10) 0.0048(8) 0.0019(8) 0.0030(8) C12 0.039(5) 0.037(5) 0.022(4) 0.009(4) 0.004(4) 0.017(4) O12 0.029(3) 0.028(3) 0.018(3) 0.006(2) 0.006(3) 0.018(3) C14 0.028(5) 0.035(5) 0.022(4) 0.014(4) 0.002(4) 0.007(4) O14 0.0091(10) 0.0114(10) 0.0108(10) 0.0048(8) 0.0019(8) 0.0030(8) C15 0.037(5) 0.032(5) 0.018(4) 0.008(4) 0.000(4) 0.009(4) O15 0.009(2) 0.022(3) 0.014(2) 0.009(2) 0.003(2) 0.004(2) C16 0.054(6) 0.058(7) 0.023(5) 0.020(5) 0.011(5) 0.033(6) C17 0.045(6) 0.048(6) 0.023(5) 0.012(4) 0.003(4) 0.024(5) C18 0.037(5) 0.030(5) 0.022(4) 0.010(4) -0.007(4) 0.006(4) C19 0.035(5) 0.031(5) 0.015(4) 0.013(4) 0.002(4) 0.008(4) C20 0.020(4) 0.036(5) 0.010(4) 0.009(3) -0.002(3) 0.007(4) O1W 0.040(4) 0.045(5) 0.076(6) 0.032(4) 0.014(4) 0.009(4) C21 0.021(4) 0.025(4) 0.018(4) 0.006(3) -0.006(3) 0.006(3) C25 0.026(4) 0.042(5) 0.015(4) 0.010(4) 0.006(4) 0.009(4) C24 0.020(4) 0.042(5) 0.017(4) 0.011(4) 0.005(3) 0.008(4) C23 0.012(4) 0.033(5) 0.022(4) 0.009(4) 0.001(3) 0.002(3) C22 0.020(4) 0.023(4) 0.007(3) 0.004(3) -0.008(3) 0.001(3) C28 0.020(4) 0.028(4) 0.020(4) 0.009(4) -0.002(3) 0.009(3) C27 0.018(4) 0.022(4) 0.017(4) 0.007(3) -0.001(3) 0.008(3) C26 0.021(4) 0.038(5) 0.023(4) 0.009(4) 0.003(4) 0.003(4) C29 0.019(4) 0.022(4) 0.022(4) 0.006(3) -0.003(3) 0.004(3) C30 0.030(5) 0.036(5) 0.017(4) 0.013(4) 0.001(4) 0.003(4) C31 0.019(4) 0.030(4) 0.017(4) 0.006(3) -0.004(3) 0.010(3) C32 0.031(5) 0.025(5) 0.030(5) 0.007(4) -0.003(4) 0.002(4) C33 0.023(4) 0.022(4) 0.019(4) 0.004(3) 0.001(3) 0.004(3) C34 0.023(4) 0.018(4) 0.026(4) 0.003(3) -0.005(4) 0.001(3) C35 0.023(4) 0.026(5) 0.025(4) 0.006(4) -0.002(4) 0.003(4) C36 0.036(5) 0.026(5) 0.024(4) 0.001(4) 0.009(4) 0.012(4) C37 0.027(4) 0.024(4) 0.020(4) 0.005(3) 0.000(4) 0.004(4) C38 0.022(4) 0.022(4) 0.033(5) 0.003(4) 0.002(4) 0.002(4) C39 0.038(5) 0.020(4) 0.012(4) 0.005(3) -0.004(4) 0.011(4) C40 0.036(5) 0.017(4) 0.045(6) 0.019(4) -0.016(5) -0.011(4) C41 0.019(4) 0.024(4) 0.006(3) 0.005(3) 0.001(3) 0.004(3) C42 0.016(4) 0.018(4) 0.012(3) 0.001(3) -0.005(3) 0.003(3) C43 0.028(4) 0.020(4) 0.011(4) 0.000(3) -0.005(3) 0.010(3) C44 0.015(4) 0.024(4) 0.020(4) 0.008(3) -0.004(3) 0.006(3) C45 0.026(4) 0.026(4) 0.022(4) 0.007(4) 0.000(4) 0.014(4) C46 0.024(4) 0.025(4) 0.024(4) 0.009(4) -0.004(4) 0.008(4) C47 0.022(4) 0.025(4) 0.015(4) 0.006(3) -0.001(3) 0.007(3) C48 0.026(4) 0.029(5) 0.019(4) 0.006(4) -0.003(4) 0.009(4) C49 0.023(4) 0.024(4) 0.017(4) 0.002(3) -0.002(3) 0.002(3) C50 0.033(5) 0.028(5) 0.023(4) 0.004(4) -0.010(4) 0.008(4) C51 0.034(5) 0.022(4) 0.019(4) 0.002(3) -0.005(4) 0.007(4) C52 0.024(4) 0.025(4) 0.025(4) 0.006(4) 0.001(4) 0.009(4) C53 0.020(4) 0.018(4) 0.015(4) -0.001(3) -0.002(3) 0.005(3) C54 0.021(4) 0.016(4) 0.016(4) 0.009(3) 0.002(3) 0.006(3) C55 0.019(4) 0.015(4) 0.019(4) 0.012(3) 0.001(3) 0.003(3) C56 0.018(4) 0.016(4) 0.021(4) 0.001(3) 0.005(3) 0.005(3) C57 0.029(5) 0.022(4) 0.017(4) 0.000(3) -0.007(4) 0.012(4) C58 0.027(5) 0.024(4) 0.026(4) 0.004(4) -0.003(4) 0.010(4) C59 0.020(4) 0.022(4) 0.019(4) 0.002(3) -0.003(3) 0.007(3) C60 0.025(4) 0.027(4) 0.013(4) 0.003(3) -0.002(3) 0.007(4) O11 0.021(3) 0.033(3) 0.027(3) 0.004(3) -0.015(3) 0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 _geom_angle_publ_flag O1 Tb1 Tb2 91.05(14) 2_654 2_655 ? O1 Tb1 O6 153.9(2) 2_654 2_766 ? O1 Tb1 O7 80.3(2) 2_654 . ? O1 Tb1 O9 86.43(19) 2_654 1_566 ? O1 Tb1 O14 104.83(19) 2_654 . ? O1 Tb1 O14 73.81(19) 2_654 2_655 ? O1 Tb1 O15 69.70(18) 2_654 . ? O6 Tb1 Tb2 63.13(15) 2_766 2_655 ? O6 Tb1 O9 71.49(19) 2_766 1_566 ? O6 Tb1 O14 84.84(19) 2_766 2_655 ? O7 Tb1 Tb2 118.66(14) . 2_655 ? O7 Tb1 O6 108.0(2) . 2_766 ? O7 Tb1 O9 79.44(18) . 1_566 ? O7 Tb1 O14 138.88(17) . 2_655 ? O9 Tb1 Tb2 39.28(12) 1_566 2_655 ? O14 Tb1 Tb2 33.24(11) 2_655 2_655 ? O14 Tb1 Tb2 89.16(11) . 2_655 ? O14 Tb1 O6 79.66(18) . 2_766 ? O14 Tb1 O7 151.87(18) . . ? O14 Tb1 O9 128.01(17) . 1_566 ? O14 Tb1 O9 67.72(16) 2_655 1_566 ? O14 Tb1 O14 67.41(18) . 2_655 ? O15 Tb1 Tb2 144.11(12) . 2_655 ? O15 Tb1 O6 133.57(19) . 2_766 ? O15 Tb1 O7 88.58(18) . . ? O15 Tb1 O9 154.86(18) . 1_566 ? O15 Tb1 O14 110.88(16) . 2_655 ? O15 Tb1 O14 68.28(17) . . ? O11 Tb1 O1 133.5(2) 2_755 2_654 ? O11 Tb1 Tb2 135.25(17) 2_755 2_655 ? O11 Tb1 O6 72.1(2) 2_755 2_766 ? O11 Tb1 O7 73.5(2) 2_755 . ? O11 Tb1 O9 124.3(2) 2_755 1_566 ? O11 Tb1 O14 83.85(19) 2_755 . ? O11 Tb1 O14 146.07(19) 2_755 2_655 ? O11 Tb1 O15 71.8(2) 2_755 . ? N2 S1 N1 100.7(4) . . ? C10 N1 S1 106.5(6) . . ? C1 O1 Tb1 146.1(5) . 2_654 ? O1 C1 O2 124.9(7) . . ? O1 C1 C2 118.9(7) . . ? O2 C1 C2 116.2(7) . . ? O4 Tb2 O9 143.19(18) . 2_644 ? O5 Tb2 O4 75.1(2) 1_444 . ? O5 Tb2 O9 74.4(2) 1_444 2_644 ? O5 Tb2 O13 141.10(19) 1_444 . ? O5 Tb2 O13 148.00(19) 1_444 2_755 ? O5 Tb2 O14 98.4(2) 1_444 . ? O5 Tb2 O15 85.2(2) 1_444 . ? O13 Tb2 O4 126.18(17) 2_755 . ? O13 Tb2 O4 66.97(17) . . ? O13 Tb2 O9 75.92(17) 2_755 2_644 ? O13 Tb2 O9 143.91(17) . 2_644 ? O13 Tb2 O13 68.06(19) . 2_755 ? O13 Tb2 O14 103.33(16) . . ? O13 Tb2 O14 81.37(16) 2_755 . ? O13 Tb2 O15 123.32(16) 2_755 . ? O13 Tb2 O15 73.34(16) . . ? O12 Tb2 O4 74.6(2) . . ? O12 Tb2 O5 91.7(2) . 1_444 ? O12 Tb2 O9 86.2(2) . 2_644 ? O12 Tb2 O13 74.63(18) . 2_755 ? O12 Tb2 O13 86.41(19) . . ? O12 Tb2 O14 148.52(19) . . ? O12 Tb2 O15 142.06(19) . . ? O14 Tb2 O4 136.85(18) . . ? O14 Tb2 O9 68.15(17) . 2_644 ? O14 Tb2 O15 68.89(16) . . ? O15 Tb2 O4 68.08(17) . . ? O15 Tb2 O9 128.52(17) . 2_644 ? N4 S2 N3 100.9(4) . . ? C11 N2 S1 107.2(6) . . ? C1 O2 Tb3 161.7(6) . 2_754 ? C3 C2 C1 122.1(8) . . ? C3 C2 C4 118.2(8) . . ? C4 C2 C1 119.7(7) . . ? O2 Tb3 O3 91.5(2) 2_754 . ? O2 Tb3 O4 75.1(2) 2_754 . ? O2 Tb3 O8 141.0(2) 2_754 . ? O2 Tb3 O10 78.6(2) 2_754 1_666 ? O2 Tb3 O13 79.8(2) 2_754 . ? O2 Tb3 O15 139.6(2) 2_754 . ? O2 Tb3 O1W 71.7(3) 2_754 . ? O3 Tb3 O4 52.36(19) . . ? O8 Tb3 O3 93.5(2) . . ? O8 Tb3 O4 135.5(2) . . ? O8 Tb3 O10 85.6(2) . 1_666 ? O8 Tb3 O13 130.4(2) . . ? O8 Tb3 O15 78.7(2) . . ? O8 Tb3 O1W 71.6(2) . . ? O10 Tb3 O3 162.5(2) 1_666 . ? O10 Tb3 O4 135.86(18) 1_666 . ? O10 Tb3 O13 75.72(18) 1_666 . ? O10 Tb3 O15 120.80(18) 1_666 . ? O10 Tb3 O1W 84.9(2) 1_666 . ? O13 Tb3 O3 116.96(19) . . ? O13 Tb3 O4 65.20(17) . . ? O13 Tb3 O15 72.78(17) . . ? O13 Tb3 O1W 148.2(2) . . ? O15 Tb3 O3 75.9(2) . . ? O15 Tb3 O4 66.77(17) . . ? O15 Tb3 O1W 139.0(2) . . ? O1W Tb3 O3 78.3(3) . . ? O1W Tb3 O4 118.5(2) . . ? N6 S3 N5 101.8(4) . . ? C31 N3 S2 106.7(6) . . ? C20 O3 Tb3 96.9(5) . . ? C2 C3 H3 119.1 . . ? C2 C3 C6 121.8(8) . . ? C6 C3 H3 119.1 . . ? C29 N4 S2 106.2(6) . . ? Tb2 O4 Tb3 92.10(17) . . ? C20 O4 Tb2 134.9(5) . . ? C20 O4 Tb3 90.5(5) . . ? C2 C4 H4 120.4 . . ? C2 C4 C5 119.2(9) . . ? C5 C4 H4 120.4 . . ? C49 N5 S3 106.6(6) . . ? C21 O5 Tb2 130.2(6) . 1_666 ? C4 C5 H5 118.7 . . ? C7 C5 C4 122.5(9) . . ? C7 C5 H5 118.7 . . ? C52 N6 S3 105.6(6) . . ? C21 O6 Tb1 140.6(5) . 2_766 ? C3 C6 H6 119.0 . . ? C7 C6 C3 122.0(9) . . ? C7 C6 H6 119.0 . . ? C40 O7 Tb1 129.8(6) . . ? C5 C7 C8 120.1(8) . . ? C6 C7 C5 115.9(8) . . ? C6 C7 C8 124.0(8) . . ? C40 O8 Tb3 149.7(6) . . ? C9 C8 C7 123.2(8) . . ? C9 C8 C10 113.1(7) . . ? C10 C8 C7 123.7(8) . . ? Tb1 O9 Tb2 102.18(19) 1_544 2_644 ? C54 O9 Tb1 135.2(5) . 1_544 ? C54 O9 Tb2 121.6(5) . 2_644 ? C8 C9 H9 117.8 . . ? C8 C9 C12 124.4(9) . . ? C12 C9 H9 117.8 . . ? N1 C10 C8 124.8(8) . . ? N1 C10 C11 113.1(7) . . ? C11 C10 C8 122.1(8) . . ? C54 O10 Tb3 143.4(5) . 1_444 ? N2 C11 C10 112.5(8) . . ? N2 C11 C13 125.7(8) . . ? C13 C11 C10 121.8(7) . . ? C11 C13 C14 124.3(7) . . ? C12 C13 C11 113.8(8) . . ? C12 C13 C14 121.9(8) . . ? Tb2 O13 Tb2 111.94(19) . 2_755 ? Tb2 O13 Tb3 101.90(18) . . ? Tb2 O13 Tb3 142.9(2) 2_755 . ? C9 C12 H12 117.6 . . ? C13 C12 C9 124.9(9) . . ? C13 C12 H12 117.6 . . ? C41 O12 Tb2 148.3(5) . . ? C15 C14 C13 123.6(8) . . ? C16 C14 C13 120.0(8) . . ? C16 C14 C15 116.4(8) . . ? Tb1 O14 Tb1 112.59(18) . 2_655 ? Tb2 O14 Tb1 111.84(19) . . ? Tb2 O14 Tb1 112.28(19) . 2_655 ? C14 C15 H15 119.2 . . ? C18 C15 C14 121.6(9) . . ? C18 C15 H15 119.2 . . ? Tb1 O15 Tb2 110.9(2) . . ? Tb1 O15 Tb3 127.5(2) . . ? Tb3 O15 Tb2 99.49(17) . . ? C14 C16 H16 118.7 . . ? C17 C16 C14 122.5(9) . . ? C17 C16 H16 118.7 . . ? C16 C17 H17 120.0 . . ? C16 C17 C19 120.1(9) . . ? C19 C17 H17 120.0 . . ? C15 C18 H18 119.8 . . ? C15 C18 C19 120.5(9) . . ? C19 C18 H18 119.8 . . ? C17 C19 C20 119.9(8) . . ? C18 C19 C17 119.0(8) . . ? C18 C19 C20 121.1(8) . . ? O3 C20 O4 119.6(7) . . ? O3 C20 C19 121.0(7) . . ? O4 C20 C19 119.3(8) . . ? Tb3 O1W H1WA 127.7 . . ? Tb3 O1W H1WB 127.8 . . ? H1WA O1W H1WB 104.5 . . ? O5 C21 C22 116.0(7) . . ? O6 C21 O5 125.7(8) . . ? O6 C21 C22 118.3(7) . . ? C23 C25 H25 119.7 . . ? C23 C25 C27 120.7(8) . . ? C27 C25 H25 119.7 . . ? C22 C24 H24 119.9 . . ? C22 C24 C26 120.1(8) . . ? C26 C24 H24 119.9 . . ? C25 C23 H23 119.6 . . ? C22 C23 C25 120.7(7) . . ? C22 C23 H23 119.6 . . ? C24 C22 C21 121.0(7) . . ? C24 C22 C23 118.8(7) . . ? C23 C22 C21 120.0(7) . . ? C29 C28 C27 124.9(8) . . ? C30 C28 C27 119.8(8) . . ? C30 C28 C29 115.2(7) . . ? C25 C27 C28 122.0(7) . . ? C26 C27 C25 117.7(8) . . ? C26 C27 C28 119.9(7) . . ? C24 C26 H26 119.3 . . ? C27 C26 C24 121.5(8) . . ? C27 C26 H26 119.3 . . ? N4 C29 C28 125.9(8) . . ? N4 C29 C31 113.2(8) . . ? C31 C29 C28 120.8(8) . . ? C28 C30 H30 118.6 . . ? C28 C30 C32 122.9(8) . . ? C32 C30 H30 118.6 . . ? N3 C31 C29 113.0(8) . . ? N3 C31 C33 125.2(7) . . ? C33 C31 C29 121.8(8) . . ? C30 C32 H32 117.8 . . ? C33 C32 C30 124.5(9) . . ? C33 C32 H32 117.8 . . ? C31 C33 C34 123.6(7) . . ? C32 C33 C31 114.8(8) . . ? C32 C33 C34 121.5(8) . . ? C35 C34 C33 122.9(8) . . ? C35 C34 C36 118.1(8) . . ? C36 C34 C33 118.9(8) . . ? C34 C35 H35 119.9 . . ? C34 C35 C37 120.3(8) . . ? C37 C35 H35 119.9 . . ? C34 C36 H36 119.5 . . ? C38 C36 C34 120.9(8) . . ? C38 C36 H36 119.5 . . ? C35 C37 H37 119.2 . . ? C35 C37 C39 121.5(8) . . ? C39 C37 H37 119.2 . . ? C36 C38 H38 119.2 . . ? C39 C38 C36 121.6(8) . . ? C39 C38 H38 119.2 . . ? C37 C39 C40 120.6(8) . . ? C38 C39 C37 117.3(8) . . ? C38 C39 C40 121.9(8) . . ? O7 C40 O8 123.5(8) . . ? O7 C40 C39 120.3(10) . . ? O8 C40 C39 116.2(8) . . ? O12 C41 C42 114.8(7) . . ? O11 C41 O12 125.6(7) . . ? O11 C41 C42 119.6(7) . . ? C43 C42 C41 119.6(7) . . ? C43 C42 C44 120.6(7) . . ? C44 C42 C41 119.8(7) . . ? C42 C43 H43 120.0 . . ? C42 C43 C46 120.0(7) . . ? C46 C43 H43 120.0 . . ? C42 C44 H44 119.9 . . ? C45 C44 C42 120.1(7) . . ? C45 C44 H44 119.9 . . ? C44 C45 H45 120.1 . . ? C44 C45 C47 119.8(7) . . ? C47 C45 H45 120.1 . . ? C43 C46 H46 119.3 . . ? C47 C46 C43 121.4(8) . . ? C47 C46 H46 119.3 . . ? C45 C47 C48 120.3(7) . . ? C46 C47 C45 118.1(7) . . ? C46 C47 C48 121.6(7) . . ? C49 C48 C47 120.6(8) . . ? C50 C48 C47 123.7(8) . . ? C50 C48 C49 115.6(8) . . ? N5 C49 C48 126.0(8) . . ? N5 C49 C52 113.4(8) . . ? C52 C49 C48 120.4(8) . . ? C48 C50 H50 118.5 . . ? C48 C50 C51 123.0(9) . . ? C51 C50 H50 118.5 . . ? C50 C51 H51 118.2 . . ? C53 C51 C50 123.6(8) . . ? C53 C51 H51 118.2 . . ? N6 C52 C49 112.5(8) . . ? N6 C52 C53 124.8(8) . . ? C53 C52 C49 122.6(8) . . ? C51 C53 C52 114.7(7) . . ? C51 C53 C60 122.6(8) . . ? C52 C53 C60 122.7(8) . . ? O9 C54 C55 119.7(7) . . ? O10 C54 O9 123.0(7) . . ? O10 C54 C55 116.9(7) . . ? C56 C55 C54 122.9(7) . . ? C56 C55 C57 120.0(7) . . ? C57 C55 C54 117.1(7) . . ? C55 C56 H56 119.9 . . ? C55 C56 C59 120.2(7) . . ? C59 C56 H56 119.9 . . ? C55 C57 H57 120.3 . . ? C58 C57 C55 119.4(8) . . ? C58 C57 H57 120.3 . . ? C57 C58 H58 119.2 . . ? C57 C58 C60 121.5(8) . . ? C60 C58 H58 119.2 . . ? C56 C59 H59 119.6 . . ? C60 C59 C56 120.7(8) . . ? C60 C59 H59 119.6 . . ? C58 C60 C53 120.1(8) . . ? C59 C60 C53 121.8(7) . . ? C59 C60 C58 118.1(7) . . ? C41 O11 Tb1 152.0(6) . 2_755 ? 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 Tb1 O1 2.363(6) 2_654 ? Tb1 Tb2 3.9453(5) 2_655 ? Tb1 O6 2.410(6) 2_766 ? Tb1 O7 2.397(6) . ? Tb1 O9 2.515(6) 1_566 ? Tb1 O14 2.375(5) . ? Tb1 O14 2.413(5) 2_655 ? Tb1 O15 2.369(5) . ? Tb1 O11 2.343(6) 2_755 ? S1 N1 1.608(8) . ? S1 N2 1.604(8) . ? N1 C10 1.339(11) . ? O1 C1 1.242(9) . ? C1 O2 1.252(9) . ? C1 C2 1.509(10) . ? Tb2 O4 2.472(5) . ? Tb2 O5 2.305(6) 1_444 ? Tb2 O9 2.555(5) 2_644 ? Tb2 O13 2.313(5) . ? Tb2 O13 2.333(5) 2_755 ? Tb2 O12 2.260(5) . ? Tb2 O14 2.337(5) . ? Tb2 O15 2.370(5) . ? S2 N3 1.611(8) . ? S2 N4 1.609(8) . ? N2 C11 1.336(11) . ? O2 Tb3 2.291(6) 2_754 ? C2 C3 1.352(12) . ? C2 C4 1.378(12) . ? Tb3 O3 2.421(6) . ? Tb3 O4 2.551(6) . ? Tb3 O8 2.300(6) . ? Tb3 O10 2.318(5) 1_666 ? Tb3 O13 2.345(5) . ? Tb3 O15 2.369(5) . ? Tb3 O1W 2.408(7) . ? S3 N5 1.600(8) . ? S3 N6 1.597(8) . ? N3 C31 1.340(11) . ? O3 C20 1.266(10) . ? C3 H3 0.9300 . ? C3 C6 1.373(12) . ? N4 C29 1.349(11) . ? O4 C20 1.275(10) . ? C4 H4 0.9300 . ? C4 C5 1.395(12) . ? N5 C49 1.339(11) . ? O5 C21 1.261(10) . ? C5 H5 0.9300 . ? C5 C7 1.382(12) . ? N6 C52 1.375(11) . ? O6 C21 1.245(10) . ? C6 H6 0.9300 . ? C6 C7 1.368(12) . ? O7 C40 1.245(11) . ? C7 C8 1.487(11) . ? O8 C40 1.289(12) . ? C8 C9 1.365(12) . ? C8 C10 1.448(11) . ? O9 C54 1.266(9) . ? C9 H9 0.9300 . ? C9 C12 1.403(12) . ? C10 C11 1.435(11) . ? O10 C54 1.250(9) . ? C11 C13 1.423(12) . ? C13 C12 1.365(12) . ? C13 C14 1.482(11) . ? C12 H12 0.9300 . ? O12 C41 1.252(9) . ? C14 C15 1.403(12) . ? C14 C16 1.389(13) . ? C15 H15 0.9300 . ? C15 C18 1.381(12) . ? C16 H16 0.9300 . ? C16 C17 1.375(12) . ? C17 H17 0.9300 . ? C17 C19 1.386(12) . ? C18 H18 0.9300 . ? C18 C19 1.382(12) . ? C19 C20 1.480(11) . ? O1W H1WA 0.9566 . ? O1W H1WB 0.9561 . ? C21 C22 1.527(10) . ? C25 H25 0.9300 . ? C25 C23 1.390(11) . ? C25 C27 1.390(12) . ? C24 H24 0.9300 . ? C24 C22 1.381(11) . ? C24 C26 1.391(12) . ? C23 H23 0.9300 . ? C23 C22 1.389(11) . ? C28 C27 1.489(11) . ? C28 C29 1.431(12) . ? C28 C30 1.365(12) . ? C27 C26 1.389(11) . ? C26 H26 0.9300 . ? C29 C31 1.429(11) . ? C30 H30 0.9300 . ? C30 C32 1.413(12) . ? C31 C33 1.428(12) . ? C32 H32 0.9300 . ? C32 C33 1.344(12) . ? C33 C34 1.501(11) . ? C34 C35 1.382(12) . ? C34 C36 1.393(12) . ? C35 H35 0.9300 . ? C35 C37 1.385(11) . ? C36 H36 0.9300 . ? C36 C38 1.379(12) . ? C37 H37 0.9300 . ? C37 C39 1.399(12) . ? C38 H38 0.9300 . ? C38 C39 1.368(12) . ? C39 C40 1.494(12) . ? C41 C42 1.519(10) . ? C41 O11 1.220(9) . ? C42 C43 1.353(11) . ? C42 C44 1.391(11) . ? C43 H43 0.9300 . ? C43 C46 1.391(11) . ? C44 H44 0.9300 . ? C44 C45 1.379(11) . ? C45 H45 0.9300 . ? C45 C47 1.422(11) . ? C46 H46 0.9300 . ? C46 C47 1.376(11) . ? C47 C48 1.458(11) . ? C48 C49 1.440(12) . ? C48 C50 1.359(12) . ? C49 C52 1.423(11) . ? C50 H50 0.9300 . ? C50 C51 1.417(11) . ? C51 H51 0.9300 . ? C51 C53 1.369(12) . ? C52 C53 1.417(11) . ? C53 C60 1.473(10) . ? C54 C55 1.477(10) . ? C55 C56 1.364(11) . ? C55 C57 1.393(11) . ? C56 H56 0.9300 . ? C56 C59 1.389(11) . ? C57 H57 0.9300 . ? C57 C58 1.370(11) . ? C58 H58 0.9300 . ? C58 C60 1.390(12) . ? C59 H59 0.9300 . ? C59 C60 1.383(11) . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O1 C1 O2 -4.6(16) 2_654 . . . ? Tb1 O1 C1 C2 174.6(7) 2_654 . . . ? Tb1 O6 C21 O5 -40.1(14) 2_766 . . . ? Tb1 O6 C21 C22 137.0(7) 2_766 . . . ? Tb1 O7 C40 O8 31.4(13) . . . . ? Tb1 O7 C40 C39 -145.1(6) . . . . ? Tb1 O9 C54 O10 112.2(8) 1_544 . . . ? Tb1 O9 C54 C55 -74.8(9) 1_544 . . . ? S1 N1 C10 C8 177.7(7) . . . . ? S1 N1 C10 C11 -2.5(10) . . . . ? S1 N2 C11 C10 -0.6(10) . . . . ? S1 N2 C11 C13 -178.8(8) . . . . ? N1 S1 N2 C11 -0.8(8) . . . . ? N1 C10 C11 N2 2.2(11) . . . . ? N1 C10 C11 C13 -179.5(8) . . . . ? O1 C1 O2 Tb3 105.0(17) . . . 2_754 ? O1 C1 C2 C3 163.6(9) . . . . ? O1 C1 C2 C4 -16.9(13) . . . . ? C1 C2 C3 C6 174.1(9) . . . . ? C1 C2 C4 C5 -173.2(10) . . . . ? Tb2 O4 C20 O3 85.9(10) . . . . ? Tb2 O4 C20 C19 -96.2(9) . . . . ? Tb2 O5 C21 O6 17.0(13) 1_666 . . . ? Tb2 O5 C21 C22 -160.1(5) 1_666 . . . ? Tb2 O9 C54 O10 -53.5(9) 2_644 . . . ? Tb2 O9 C54 C55 119.4(6) 2_644 . . . ? Tb2 O12 C41 C42 109.4(9) . . . . ? Tb2 O12 C41 O11 -72.3(13) . . . . ? S2 N3 C31 C29 -1.0(9) . . . . ? S2 N3 C31 C33 176.2(7) . . . . ? S2 N4 C29 C28 -177.3(7) . . . . ? S2 N4 C29 C31 -0.3(9) . . . . ? N2 S1 N1 C10 2.0(8) . . . . ? N2 C11 C13 C12 177.5(9) . . . . ? N2 C11 C13 C14 -0.5(15) . . . . ? O2 C1 C2 C3 -17.1(13) . . . . ? O2 C1 C2 C4 162.4(9) . . . . ? C2 C1 O2 Tb3 -74(2) . . . 2_754 ? C2 C3 C6 C7 0.0(18) . . . . ? C2 C4 C5 C7 -2.2(18) . . . . ? Tb3 O3 C20 O4 8.1(8) . . . . ? Tb3 O3 C20 C19 -169.8(7) . . . . ? Tb3 O4 C20 O3 -7.6(8) . . . . ? Tb3 O4 C20 C19 170.3(7) . . . . ? Tb3 O8 C40 O7 -48.2(17) . . . . ? Tb3 O8 C40 C39 128.4(10) . . . . ? Tb3 O10 C54 O9 -22.6(13) 1_444 . . . ? Tb3 O10 C54 C55 164.3(6) 1_444 . . . ? S3 N5 C49 C48 176.1(8) . . . . ? S3 N5 C49 C52 1.5(10) . . . . ? S3 N6 C52 C49 1.1(9) . . . . ? S3 N6 C52 C53 -177.7(7) . . . . ? N3 S2 N4 C29 -0.3(7) . . . . ? N3 C31 C33 C32 -177.0(8) . . . . ? N3 C31 C33 C34 6.5(13) . . . . ? C3 C2 C4 C5 6.3(16) . . . . ? C3 C6 C7 C5 4.1(16) . . . . ? C3 C6 C7 C8 -174.0(10) . . . . ? N4 S2 N3 C31 0.8(7) . . . . ? N4 C29 C31 N3 0.9(10) . . . . ? N4 C29 C31 C33 -176.4(7) . . . . ? C4 C2 C3 C6 -5.4(16) . . . . ? C4 C5 C7 C6 -3.0(17) . . . . ? C4 C5 C7 C8 175.1(10) . . . . ? N5 S3 N6 C52 -0.2(7) . . . . ? N5 C49 C52 N6 -1.7(11) . . . . ? N5 C49 C52 C53 177.1(8) . . . . ? O5 C21 C22 C24 -171.3(8) . . . . ? O5 C21 C22 C23 14.7(12) . . . . ? C5 C7 C8 C9 -4.7(14) . . . . ? C5 C7 C8 C10 176.5(9) . . . . ? N6 S3 N5 C49 -0.7(8) . . . . ? N6 C52 C53 C51 177.5(8) . . . . ? N6 C52 C53 C60 -1.6(14) . . . . ? O6 C21 C22 C24 11.3(12) . . . . ? O6 C21 C22 C23 -162.6(8) . . . . ? C6 C7 C8 C9 173.3(10) . . . . ? C6 C7 C8 C10 -5.5(14) . . . . ? C7 C8 C9 C12 -179.1(9) . . . . ? C7 C8 C10 N1 -1.2(14) . . . . ? C7 C8 C10 C11 179.1(8) . . . . ? C8 C9 C12 C13 -0.1(17) . . . . ? C8 C10 C11 N2 -178.1(8) . . . . ? C8 C10 C11 C13 0.2(13) . . . . ? O9 C54 C55 C56 0.2(11) . . . . ? O9 C54 C55 C57 -178.6(7) . . . . ? C9 C8 C10 N1 179.9(9) . . . . ? C9 C8 C10 C11 0.2(12) . . . . ? C10 C8 C9 C12 -0.2(14) . . . . ? C10 C11 C13 C12 -0.5(13) . . . . ? C10 C11 C13 C14 -178.5(8) . . . . ? O10 C54 C55 C56 173.6(7) . . . . ? O10 C54 C55 C57 -5.3(11) . . . . ? C11 C13 C12 C9 0.5(14) . . . . ? C11 C13 C14 C15 -12.3(14) . . . . ? C11 C13 C14 C16 167.9(9) . . . . ? C13 C14 C15 C18 179.3(9) . . . . ? C13 C14 C16 C17 179.7(10) . . . . ? C12 C13 C14 C15 169.8(9) . . . . ? C12 C13 C14 C16 -9.9(14) . . . . ? O12 C41 C42 C43 -4.9(11) . . . . ? O12 C41 C42 C44 175.7(7) . . . . ? O12 C41 O11 Tb1 -63.9(15) . . . 2_755 ? C14 C13 C12 C9 178.6(9) . . . . ? C14 C15 C18 C19 1.5(15) . . . . ? C14 C16 C17 C19 0.7(17) . . . . ? C15 C14 C16 C17 -0.1(16) . . . . ? C15 C18 C19 C17 -0.9(15) . . . . ? C15 C18 C19 C20 -178.0(9) . . . . ? C16 C14 C15 C18 -0.9(14) . . . . ? C16 C17 C19 C18 -0.1(16) . . . . ? C16 C17 C19 C20 177.0(9) . . . . ? C17 C19 C20 O3 -12.4(14) . . . . ? C17 C19 C20 O4 169.7(9) . . . . ? C18 C19 C20 O3 164.7(9) . . . . ? C18 C19 C20 O4 -13.1(13) . . . . ? C25 C23 C22 C21 169.2(8) . . . . ? C25 C23 C22 C24 -4.9(13) . . . . ? C25 C27 C26 C24 -6.4(13) . . . . ? C23 C25 C27 C28 -167.8(8) . . . . ? C23 C25 C27 C26 5.9(13) . . . . ? C22 C24 C26 C27 1.2(14) . . . . ? C28 C27 C26 C24 167.4(8) . . . . ? C28 C29 C31 N3 178.1(7) . . . . ? C28 C29 C31 C33 0.7(12) . . . . ? C28 C30 C32 C33 0.3(15) . . . . ? C27 C25 C23 C22 -0.4(14) . . . . ? C27 C28 C29 N4 -8.1(13) . . . . ? C27 C28 C29 C31 175.1(7) . . . . ? C27 C28 C30 C32 -175.8(8) . . . . ? C26 C24 C22 C21 -169.6(8) . . . . ? C26 C24 C22 C23 4.5(13) . . . . ? C29 C28 C27 C25 -40.5(12) . . . . ? C29 C28 C27 C26 146.0(9) . . . . ? C29 C28 C30 C32 0.4(13) . . . . ? C29 C31 C33 C32 0.0(12) . . . . ? C29 C31 C33 C34 -176.5(8) . . . . ? C30 C28 C27 C25 135.4(9) . . . . ? C30 C28 C27 C26 -38.2(12) . . . . ? C30 C28 C29 N4 175.9(8) . . . . ? C30 C28 C29 C31 -0.9(12) . . . . ? C30 C32 C33 C31 -0.6(14) . . . . ? C30 C32 C33 C34 176.1(9) . . . . ? C31 C33 C34 C35 37.7(13) . . . . ? C31 C33 C34 C36 -147.2(9) . . . . ? C32 C33 C34 C35 -138.6(10) . . . . ? C32 C33 C34 C36 36.5(13) . . . . ? C33 C34 C35 C37 171.2(8) . . . . ? C33 C34 C36 C38 -171.9(9) . . . . ? C34 C35 C37 C39 0.5(14) . . . . ? C34 C36 C38 C39 0.5(15) . . . . ? C35 C34 C36 C38 3.4(14) . . . . ? C35 C37 C39 C38 3.4(13) . . . . ? C35 C37 C39 C40 -173.3(8) . . . . ? C36 C34 C35 C37 -3.9(13) . . . . ? C36 C38 C39 C37 -3.9(14) . . . . ? C36 C38 C39 C40 172.7(9) . . . . ? C37 C39 C40 O7 166.4(8) . . . . ? C37 C39 C40 O8 -10.3(12) . . . . ? C38 C39 C40 O7 -10.1(13) . . . . ? C38 C39 C40 O8 173.2(8) . . . . ? C41 C42 C43 C46 -179.2(8) . . . . ? C41 C42 C44 C45 178.3(8) . . . . ? C42 C41 O11 Tb1 114.3(11) . . . 2_755 ? C42 C43 C46 C47 1.2(13) . . . . ? C42 C44 C45 C47 0.7(13) . . . . ? C43 C42 C44 C45 -1.1(13) . . . . ? C43 C46 C47 C45 -1.7(13) . . . . ? C43 C46 C47 C48 178.7(8) . . . . ? C44 C42 C43 C46 0.2(13) . . . . ? C44 C45 C47 C46 0.7(13) . . . . ? C44 C45 C47 C48 -179.7(8) . . . . ? C45 C47 C48 C49 -147.1(8) . . . . ? C45 C47 C48 C50 35.4(13) . . . . ? C46 C47 C48 C49 32.5(13) . . . . ? C46 C47 C48 C50 -145.0(9) . . . . ? C47 C48 C49 N5 6.4(14) . . . . ? C47 C48 C49 C52 -179.3(8) . . . . ? C47 C48 C50 C51 178.1(9) . . . . ? C48 C49 C52 N6 -176.7(8) . . . . ? C48 C49 C52 C53 2.1(13) . . . . ? C48 C50 C51 C53 0.4(15) . . . . ? C49 C48 C50 C51 0.5(14) . . . . ? C49 C52 C53 C51 -1.1(13) . . . . ? C49 C52 C53 C60 179.7(8) . . . . ? C50 C48 C49 N5 -176.0(9) . . . . ? C50 C48 C49 C52 -1.7(13) . . . . ? C50 C51 C53 C52 -0.1(13) . . . . ? C50 C51 C53 C60 179.1(8) . . . . ? C51 C53 C60 C58 147.5(9) . . . . ? C51 C53 C60 C59 -34.0(13) . . . . ? C52 C53 C60 C58 -33.4(13) . . . . ? C52 C53 C60 C59 145.1(9) . . . . ? C54 C55 C56 C59 -177.6(7) . . . . ? C54 C55 C57 C58 176.7(8) . . . . ? C55 C56 C59 C60 0.8(13) . . . . ? C55 C57 C58 C60 1.1(14) . . . . ? C56 C55 C57 C58 -2.2(13) . . . . ? C56 C59 C60 C53 179.6(8) . . . . ? C56 C59 C60 C58 -1.9(13) . . . . ? C57 C55 C56 C59 1.2(12) . . . . ? C57 C58 C60 C53 179.5(9) . . . . ? C57 C58 C60 C59 0.9(14) . . . . ? O11 C41 C42 C43 176.7(8) . . . . ? O11 C41 C42 C44 -2.8(12) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.277 0.500 1.000 567.0 102.8 ?