#------------------------------------------------------------------------------ #$Date: 2022-02-04 21:32:17 +0200 (Fri, 04 Feb 2022) $ #$Revision: 272653 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/89/7708946.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_7708946 loop_ _publ_author_name 'Wu, Min-Yu' 'Xu, Jing-Xiang' 'Chen, Yi-Hsin' 'Lu, I-Chung' 'Han, Jeng-Liang' 'Lin, Po-Heng' _publ_section_title ; Self-assembled lanthanide-based helixes: synthetic control of the helical handedness by chirality of the ligand. ; _journal_issue 1 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 69 _journal_page_last 73 _journal_paper_doi 10.1039/d1dt03833h _journal_volume 51 _journal_year 2021 _chemical_absolute_configuration unk _chemical_formula_moiety 'C30 H31 N9 O26 S3 Tb2, 3(H2 O)' _chemical_formula_sum 'C30 H37 N9 O29 S3 Tb2' _chemical_formula_weight 1401.70 _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-10-01 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.02.24 svn.r3390 for Rigaku Oxford Diffraction, GUI svn.r5318) ; _audit_update_record ; 2021-10-19 deposited with the CCDC. 2021-11-24 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 8.4028(7) _cell_length_b 17.0704(15) _cell_length_c 31.728(3) _cell_measurement_reflns_used 9182 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 26.40 _cell_measurement_theta_min 2.71 _cell_volume 4551.0(7) _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 150.15 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71076 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_unetI/netI 0.0280 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 70190 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.243 _diffrn_reflns_theta_max 26.404 _diffrn_reflns_theta_min 2.471 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 3.330 _exptl_absorpt_correction_type none _exptl_crystal_colour yellow _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 2.046 _exptl_crystal_description BLOCK _exptl_crystal_F_000 2760 _refine_diff_density_max 1.387 _refine_diff_density_min -2.244 _refine_diff_density_rms 0.424 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.035(15) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.379 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 673 _refine_ls_number_reflns 9307 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.378 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0283 _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^)+(0.0501P)^2^+14.1284P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0865 _refine_ls_wR_factor_ref 0.1029 _reflns_Friedel_coverage 0.784 _reflns_Friedel_fraction_full 0.998 _reflns_Friedel_fraction_max 0.996 _reflns_number_gt 9240 _reflns_number_total 9307 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL mo_wcl28_0m_a.res in P1 New:P212121 mo_wcl28_0m_pl.res created by SHELXL-2018/3 at 12:07:10 on 01-Oct-2021 CELL 0.71076 8.4028 17.0704 31.728 90 90 90 ZERR 4 0.0007 0.0015 0.003 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H N O S Tb UNIT 120 148 36 116 12 8 SIMU 0.001 0.002 2 O16 O3 ISOR 0.01 0.001 O14 ISOR 0.01 0.001 C20 ISOR 0.00001 0.00002 O3 L.S. 50 PLAN -10 TEMP -123 FREE H18b H18a FREE H17b H17a CONF fmap 2 acta TWIN -1 0 0 0 -1 0 0 0 -1 2 REM REM REM WGHT 0.050100 14.128401 BASF 0.03452 FVAR 0.25973 TB2 6 0.776803 1.011605 0.075806 11.00000 0.01076 0.00728 = 0.00536 0.00073 -0.00233 -0.00046 TB1 6 0.674227 1.194252 -0.096926 11.00000 0.01175 0.01043 = 0.00677 -0.00019 -0.00104 0.00134 S2 5 0.299087 0.952875 -0.009070 11.00000 0.00894 0.03012 = 0.01984 0.00709 -0.00541 -0.00154 S3 5 1.223766 0.973949 0.172986 11.00000 0.01567 0.02168 = 0.02490 -0.00652 -0.00726 0.00257 S1 5 0.391541 1.061352 -0.219783 11.00000 0.02089 0.02291 = 0.01992 -0.01018 -0.00708 0.00407 O12 4 0.582891 0.948952 0.113016 11.00000 0.01751 0.01640 = 0.00842 -0.00042 0.00059 -0.00796 O18 4 0.946417 1.002411 0.016097 11.00000 0.01639 0.02459 = 0.01888 -0.00684 0.00592 0.00114 AFIX 7 H18A 2 1.054625 1.005659 0.018445 11.00000 -1.50000 H18B 2 0.963775 0.969896 0.002672 11.00000 -1.50000 AFIX 0 O3 4 0.589285 1.137620 -0.034739 11.00000 0.01517 0.01515 = 0.01514 0.00002 0.00000 0.00001 O17 4 0.637958 1.103850 0.119737 11.00000 0.02020 0.01766 = 0.01153 0.00215 0.00365 0.00588 AFIX 7 H17A 2 0.655156 1.083130 0.144736 11.00000 -1.50000 H17B 2 0.580637 1.109875 0.141596 11.00000 -1.50000 AFIX 0 O8 4 1.196043 0.989556 -0.124713 11.00000 0.01488 0.07692 = 0.02469 0.00405 -0.00603 -0.00360 O16 4 1.105679 1.186349 0.131581 11.00000 0.02142 0.00686 = 0.01210 0.00436 -0.00093 -0.00341 O22 4 0.107108 0.699555 0.046350 11.00000 0.02202 0.02505 = 0.02223 0.00066 -0.00181 -0.00715 O6 4 0.918015 1.166998 -0.059330 11.00000 0.02300 0.02031 = 0.02969 -0.00605 -0.00937 0.00813 AFIX 7 H6A 2 0.970204 1.210846 -0.054529 11.00000 -1.50000 H6B 2 0.978777 1.135522 -0.074345 11.00000 -1.50000 AFIX 0 O15 4 0.984857 1.103580 0.087381 11.00000 0.01667 0.01912 = 0.00896 0.00170 -0.00202 -0.00716 O13 4 0.871957 0.884525 0.076811 11.00000 0.02213 0.00842 = 0.00962 0.00172 -0.00461 0.00607 O5 4 0.708838 1.300521 -0.049054 11.00000 0.04612 0.01819 = 0.01188 -0.00115 -0.00787 0.00796 AFIX 7 H5A 2 0.703172 1.284022 -0.022184 11.00000 -1.50000 H5B 2 0.632986 1.336795 -0.052847 11.00000 -1.50000 AFIX 0 O2 4 0.394490 1.194778 -0.098041 11.00000 0.01195 0.02337 = 0.00725 0.00099 -0.00182 -0.00045 O4 4 0.876954 1.212912 -0.148007 11.00000 0.01368 0.03633 = 0.01718 0.00254 -0.00363 -0.00040 AFIX 7 H4A 2 0.862900 1.180374 -0.169168 11.00000 -1.50000 H4B 2 0.970634 1.203949 -0.136628 11.00000 -1.50000 AFIX 0 O21 4 0.199079 0.637312 0.101110 11.00000 0.04188 0.01023 = 0.03931 0.00727 0.00112 -0.00899 O1 4 0.740058 1.065671 -0.109881 11.00000 0.01756 0.01439 = 0.01006 -0.00112 -0.00195 0.00261 O7 4 1.010251 1.003781 -0.078481 11.00000 0.04443 0.04465 = 0.01555 0.00159 -0.00740 0.02100 O11 4 0.179062 1.241934 -0.131221 11.00000 0.01259 0.02379 = 0.03241 -0.00936 -0.00262 0.00562 O19 4 0.642241 0.875232 0.185540 11.00000 0.03521 0.03651 = 0.02296 0.00376 -0.01461 -0.00935 O10 4 0.849553 0.939761 -0.291362 11.00000 0.02838 0.05111 = 0.01701 -0.01696 -0.00419 0.00865 O23 4 0.741316 0.757232 0.041633 11.00000 0.02903 0.02493 = 0.01787 -0.00474 -0.00637 -0.00495 O25 4 0.937551 0.623778 0.212732 11.00000 0.08390 0.02430 = 0.03321 0.01804 -0.01035 -0.01563 O9 4 1.063331 0.895568 -0.260733 11.00000 0.02905 0.05431 = 0.04204 -0.01730 0.00717 0.01996 O24 4 0.654115 0.671622 0.085712 11.00000 0.02091 0.02595 = 0.03279 -0.00406 -0.00016 -0.01331 O26 4 1.112115 0.706562 0.235297 11.00000 0.07271 0.03557 = 0.01904 0.00860 -0.01760 0.00153 O20 4 0.482700 0.784257 0.203053 11.00000 0.07408 0.07738 = 0.02938 0.02909 -0.01407 -0.04143 N1 3 0.547738 1.157175 -0.169560 11.00000 0.01576 0.00802 = 0.00902 0.00082 0.00063 0.00126 AFIX 13 H1 2 0.618747 1.176865 -0.192527 11.00000 -1.20000 AFIX 0 N4 3 0.599752 0.950773 0.018089 11.00000 0.00929 0.00650 = 0.00632 0.00420 0.00112 -0.00089 AFIX 13 H4 2 0.634990 0.896261 0.011296 11.00000 -1.20000 AFIX 0 N6 3 0.194334 0.694527 0.076902 11.00000 0.01956 0.01947 = 0.02081 -0.00720 0.01398 -0.00626 N7 3 0.922099 0.998730 0.146651 11.00000 0.01263 0.00885 = 0.01117 -0.00025 0.00413 0.00086 AFIX 13 H7 2 0.849553 0.975405 0.168256 11.00000 -1.20000 AFIX 0 N2 3 1.054268 0.996967 -0.115322 11.00000 0.02307 0.02645 = 0.01394 0.00265 -0.00596 0.00429 N5 3 0.537988 0.829218 0.177136 11.00000 0.01937 0.03030 = 0.01495 0.00355 0.00138 0.00064 C9 1 0.388506 1.195101 -0.174122 11.00000 0.01410 0.01481 = 0.01190 -0.00211 -0.00562 0.00387 AFIX 13 H9 2 0.403657 1.246417 -0.188785 11.00000 -1.20000 AFIX 0 N3 3 0.934314 0.930618 -0.259882 11.00000 0.01959 0.03443 = 0.01793 -0.00732 0.00336 -0.00114 N8 3 0.741013 0.726978 0.076926 11.00000 0.01552 0.01450 = 0.02432 -0.00755 0.00016 0.00050 N9 3 1.010900 0.686079 0.210044 11.00000 0.05389 0.01868 = 0.01009 0.00390 -0.00087 0.00521 C24 1 0.972731 0.737039 0.175050 11.00000 0.02495 0.01371 = 0.01806 0.00390 0.00562 0.00196 C6 1 0.685727 1.033042 -0.179904 11.00000 0.01657 0.01438 = 0.01312 -0.00363 0.00027 0.00101 C10 1 0.314975 1.211093 -0.131306 11.00000 0.01131 0.01095 = 0.01581 0.00152 -0.00167 0.00002 C5 1 0.734865 0.999246 -0.217241 11.00000 0.01418 0.02926 = 0.01583 0.00108 0.00096 -0.00291 AFIX 43 H5 2 0.665977 0.999664 -0.240982 11.00000 -1.20000 AFIX 0 C19 1 0.600543 1.000356 -0.019899 11.00000 0.00932 0.02084 = 0.00411 0.00048 -0.00322 0.00176 AFIX 13 H19 2 0.694873 0.985493 -0.037373 11.00000 -1.20000 AFIX 0 C14 1 0.297838 0.760086 0.086907 11.00000 0.00922 0.01000 = 0.01548 -0.00404 0.00670 -0.00243 C11 1 0.493136 0.889497 0.105387 11.00000 0.01202 0.01486 = 0.01210 -0.00217 0.00075 -0.00251 C4 1 0.886096 0.964153 -0.220488 11.00000 0.01825 0.02515 = 0.01577 -0.00302 0.00487 -0.00010 C25 1 1.036337 0.813844 0.173894 11.00000 0.02368 0.01033 = 0.00788 -0.00094 -0.00176 0.00221 AFIX 43 H25 2 1.102327 0.831873 0.196188 11.00000 -1.20000 AFIX 0 C7 1 0.526992 1.071955 -0.174906 11.00000 0.01585 0.01582 = 0.01661 -0.00290 0.00232 0.00322 AFIX 13 H7A 2 0.473886 1.050455 -0.149181 11.00000 -1.20000 AFIX 0 C17 1 0.435743 0.950937 0.035664 11.00000 0.01662 0.01102 = 0.00799 0.00268 0.00019 -0.00065 AFIX 13 H17 2 0.421307 1.000769 0.051786 11.00000 -1.20000 AFIX 0 C30 1 1.030895 1.125173 0.123686 11.00000 0.00839 0.00893 = 0.01075 -0.00425 -0.00124 -0.00017 C16 1 0.411047 0.883386 0.065980 11.00000 0.01352 0.01289 = 0.00609 0.00004 -0.00271 -0.00146 C27 1 1.059903 0.944879 0.138516 11.00000 0.01286 0.01414 = 0.00675 -0.00237 0.00045 -0.00049 AFIX 13 H27 2 1.095472 0.954242 0.108863 11.00000 -1.20000 AFIX 0 C26 1 1.002896 0.861573 0.140929 11.00000 0.01363 0.01456 = 0.01080 -0.00342 0.00017 0.00103 C12 1 0.466369 0.828300 0.134839 11.00000 0.01324 0.02174 = 0.01132 0.00473 0.00529 -0.00192 C29 1 0.983319 1.074838 0.161506 11.00000 0.01393 0.00595 = 0.01474 -0.00092 -0.00171 -0.00036 AFIX 13 H29 2 0.896457 1.102313 0.177180 11.00000 -1.20000 AFIX 0 C3 1 0.987443 0.963807 -0.186811 11.00000 0.01986 0.02010 = 0.01817 -0.00624 -0.00092 0.00498 AFIX 43 H3 2 1.090230 0.941086 -0.189273 11.00000 -1.20000 AFIX 0 C18 1 0.448507 0.984402 -0.046119 11.00000 0.01868 0.01827 = 0.01118 -0.00144 -0.00544 0.00329 AFIX 23 H18C 2 0.468591 0.943114 -0.067375 11.00000 -1.20000 H18D 2 0.413774 1.032593 -0.060841 11.00000 -1.20000 AFIX 0 C15 1 0.315434 0.820519 0.057373 11.00000 0.01123 0.01829 = 0.01288 0.00039 0.00451 -0.00184 AFIX 43 H15 2 0.260645 0.817814 0.031223 11.00000 -1.20000 AFIX 0 C23 1 0.877573 0.710537 0.143511 11.00000 0.02649 0.00869 = 0.02037 0.00329 0.00880 -0.00134 AFIX 43 H23 2 0.834108 0.659222 0.144853 11.00000 -1.20000 AFIX 0 C13 1 0.370245 0.763767 0.125217 11.00000 0.01279 0.01429 = 0.01988 0.00284 0.00491 -0.00095 AFIX 43 H13 2 0.355710 0.722976 0.145218 11.00000 -1.20000 AFIX 0 C28 1 1.121352 1.061925 0.191283 11.00000 0.02523 0.00809 = 0.01583 -0.00044 -0.00898 0.00008 AFIX 23 H28A 2 1.082411 1.054598 0.220467 11.00000 -1.20000 H28B 2 1.194223 1.107486 0.190752 11.00000 -1.20000 AFIX 0 C21 1 0.902641 0.836780 0.106673 11.00000 0.01686 0.00586 = 0.00509 -0.00167 0.00016 -0.00074 C2 1 0.939178 0.996787 -0.149133 11.00000 0.02029 0.01430 = 0.00931 -0.00048 -0.00742 -0.00060 C22 1 0.844079 0.758222 0.109512 11.00000 0.01916 0.01169 = 0.01457 -0.00150 -0.00128 -0.00103 C8 1 0.272331 1.143952 -0.201331 11.00000 0.01992 0.02149 = 0.01541 -0.00854 -0.00710 0.00036 AFIX 23 H8A 2 0.230578 1.174474 -0.225449 11.00000 -1.20000 H8B 2 0.181600 1.125437 -0.184098 11.00000 -1.20000 AFIX 0 C1 1 0.786425 1.032572 -0.143456 11.00000 0.01405 0.00902 = 0.01214 0.00205 0.00170 -0.00092 C20 1 0.618062 1.086607 -0.007374 11.00000 0.00880 0.01493 = 0.00885 0.00572 0.00216 0.00182 O14 4 0.662848 1.102522 0.029558 11.00000 0.02313 0.01546 = 0.00455 0.00202 -0.00637 0.00239 AFIX 6 O27 4 0.191763 1.234079 -0.032559 11.00000 0.02351 0.01744 = 0.01759 -0.00310 0.00428 -0.00344 H27A 2 0.176357 1.281859 -0.041269 11.00000 -1.50000 H27B 2 0.261836 1.211414 -0.048650 11.00000 -1.50000 AFIX 6 O28 4 0.432395 0.641412 0.014893 11.00000 0.02585 0.03461 = 0.01823 -0.01089 -0.00561 0.01037 H28C 2 0.434580 0.674375 -0.006060 11.00000 -1.50000 H28D 2 0.526564 0.638429 0.026117 11.00000 -1.50000 AFIX 6 O29 4 0.787196 1.239635 -0.230454 11.00000 0.05145 0.05188 = 0.02197 0.00199 0.01259 0.00185 H29A 2 0.841906 1.235679 -0.253661 11.00000 -1.50000 H29B 2 0.807413 1.284402 -0.218515 11.00000 -1.50000 AFIX 0 HKLF 4 REM mo_wcl28_0m_a.res in P1 New:P212121 REM wR2 = 0.1029, GooF = S = 1.379, Restrained GooF = 1.378 for all data REM R1 = 0.0283 for 9240 Fo > 4sig(Fo) and 0.0308 for all 9307 data REM 673 parameters refined using 18 restraints END WGHT 0.0501 14.1519 REM Highest difference peak 1.387, deepest hole -2.244, 1-sigma level 0.424 Q1 1 0.6849 0.5998 0.0758 11.00000 0.05 1.39 Q2 1 0.7905 0.5815 0.0827 11.00000 0.05 1.30 Q3 1 0.2931 1.0366 0.0741 11.00000 0.05 1.29 Q4 1 1.1956 0.9260 -0.2459 11.00000 0.05 1.22 Q5 1 0.2759 0.9796 -0.2508 11.00000 0.05 1.16 Q6 1 0.8027 0.6188 0.0826 11.00000 0.05 1.15 Q7 1 0.2153 0.9567 -0.0640 11.00000 0.05 1.12 Q8 1 0.1706 1.0781 -0.2469 11.00000 0.05 1.10 Q9 1 0.2982 0.8818 -0.0655 11.00000 0.05 1.09 Q10 1 0.8156 0.5791 0.2373 11.00000 0.05 1.09 REM The information below was added by Olex2. REM REM R1 = 0.0283 for 9240 Fo > 4sig(Fo) and 0.0308 for all 70320 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.39, deepest hole -2.24 REM Mean Shift 0, Max Shift -0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0308 REM R1_gt = 0.0283 REM wR_ref = 0.1029 REM GOOF = 1.379 REM Shift_max = -0.001 REM Shift_mean = 0 REM Reflections_all = 70320 REM Reflections_gt = 9240 REM Parameters = n/a REM Hole = -2.24 REM Peak = 1.39 REM Flack = n/a ; _cod_data_source_file d1dt03833h2.cif _cod_data_source_block mo_wcl28_0m_pl _cod_depositor_comments 'Adding full bibliography for 7708942--7708947.cif.' _cod_database_code 7708946 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.965(15) 0.035(15) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All N(H) groups At 1.5 times of: All O(H,H) groups 3. Uiso/Uaniso restraints and constraints O16 \\sim O3: within 2A with sigma of 0.001 and sigma for terminal atoms of 0.002 Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001 Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.001 Uanis(O3) \\sim Ueq: with sigma of 0.00001 and sigma for terminal atoms of 0.00002 4.a Free rotating group: O27(H27A,H27B), O28(H28C,H28D), O29(H29A,H29B) 4.b Rotating group: O18(H18A,H18B), O17(H17A,H17B), O6(H6A,H6B), O5(H5A,H5B), O4(H4A,H4B) 4.c Ternary CH refined with riding coordinates: N1(H1), N4(H4), N7(H7), C9(H9), C19(H19), C7(H7A), C17(H17), C27(H27), C29(H29) 4.d Secondary CH2 refined with riding coordinates: C18(H18C,H18D), C28(H28A,H28B), C8(H8A,H8B) 4.e Aromatic/amide H refined with riding coordinates: C5(H5), C25(H25), C3(H3), C15(H15), C23(H23), C13(H13) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tb2 Tb 0.77680(5) 1.01161(2) 0.07581(2) 0.00780(11) Uani 1 1 d . . . . . Tb1 Tb 0.67423(5) 1.19425(2) -0.09693(2) 0.00965(11) Uani 1 1 d . . . . . S2 S 0.2991(3) 0.95287(16) -0.00907(8) 0.0196(5) Uani 1 1 d . . . . . S3 S 1.2238(3) 0.97395(15) 0.17299(8) 0.0207(5) Uani 1 1 d . . . . . S1 S 0.3915(3) 1.06135(16) -0.21978(8) 0.0212(5) Uani 1 1 d . . . . . O12 O 0.5829(8) 0.9490(4) 0.1130(2) 0.0141(14) Uani 1 1 d . . . . . O18 O 0.9464(8) 1.0024(4) 0.0161(2) 0.0200(15) Uani 1 1 d . . . . . H18A H 1.054625 1.005659 0.018445 0.030 Uiso 1 1 d GR . . . . H18B H 0.963775 0.969896 0.002672 0.030 Uiso 1 1 d GR . . . . O3 O 0.5893(8) 1.1376(4) -0.0347(2) 0.0152(13) Uani 1 1 d . U . . . O17 O 0.6380(9) 1.1038(4) 0.1197(2) 0.0165(15) Uani 1 1 d . . . . . H17A H 0.655156 1.083130 0.144736 0.025 Uiso 1 1 d GR . . . . H17B H 0.580637 1.109875 0.141596 0.025 Uiso 1 1 d GR . . . . O8 O 1.1960(9) 0.9896(7) -0.1247(3) 0.039(2) Uani 1 1 d . . . . . O16 O 1.1057(8) 1.1863(4) 0.1316(2) 0.0135(13) Uani 1 1 d . U . . . O22 O 0.1071(9) 0.6996(5) 0.0464(2) 0.0231(16) Uani 1 1 d . . . . . O6 O 0.9180(9) 1.1670(4) -0.0593(3) 0.0243(17) Uani 1 1 d . . . . . H6A H 0.970204 1.210846 -0.054529 0.036 Uiso 1 1 d GR . . . . H6B H 0.978777 1.135522 -0.074345 0.036 Uiso 1 1 d GR . . . . O15 O 0.9849(8) 1.1036(4) 0.0874(2) 0.0149(14) Uani 1 1 d . . . . . O13 O 0.8720(8) 0.8845(4) 0.0768(2) 0.0134(13) Uani 1 1 d . . . . . O5 O 0.7088(11) 1.3005(4) -0.0491(2) 0.0254(17) Uani 1 1 d . . . . . H5A H 0.703172 1.284022 -0.022184 0.038 Uiso 1 1 d GR . . . . H5B H 0.632986 1.336795 -0.052847 0.038 Uiso 1 1 d GR . . . . O2 O 0.3945(8) 1.1948(4) -0.0980(2) 0.0142(12) Uani 1 1 d . . . . . O4 O 0.8770(9) 1.2129(5) -0.1480(2) 0.0224(16) Uani 1 1 d . . . . . H4A H 0.862900 1.180374 -0.169168 0.034 Uiso 1 1 d GR . . . . H4B H 0.970634 1.203949 -0.136628 0.034 Uiso 1 1 d GR . . . . O21 O 0.1991(11) 0.6373(4) 0.1011(3) 0.0305(19) Uani 1 1 d . . . . . O1 O 0.7401(8) 1.0657(4) -0.10988(19) 0.0140(13) Uani 1 1 d . . . . . O7 O 1.0103(11) 1.0038(5) -0.0785(2) 0.035(2) Uani 1 1 d . . . . . O11 O 0.1791(9) 1.2419(4) -0.1312(2) 0.0229(16) Uani 1 1 d . . . . . O19 O 0.6422(11) 0.8752(5) 0.1855(3) 0.032(2) Uani 1 1 d . . . . . O10 O 0.8496(10) 0.9398(6) -0.2914(2) 0.032(2) Uani 1 1 d . . . . . O23 O 0.7413(10) 0.7572(4) 0.0416(2) 0.0239(16) Uani 1 1 d . . . . . O25 O 0.9376(15) 0.6238(5) 0.2127(3) 0.047(3) Uani 1 1 d . . . . . O9 O 1.0633(11) 0.8956(6) -0.2607(3) 0.042(2) Uani 1 1 d . . . . . O24 O 0.6541(9) 0.6716(4) 0.0857(2) 0.0265(17) Uani 1 1 d . . . . . O26 O 1.1121(14) 0.7066(5) 0.2353(3) 0.042(2) Uani 1 1 d . . . . . O20 O 0.4827(16) 0.7843(8) 0.2031(3) 0.060(4) Uani 1 1 d . . . . . N1 N 0.5477(10) 1.1572(4) -0.1696(2) 0.0109(15) Uani 1 1 d . . . . . H1 H 0.618747 1.176865 -0.192527 0.013 Uiso 1 1 calc R . . . . N4 N 0.5998(9) 0.9508(4) 0.0181(2) 0.0074(14) Uani 1 1 d . . . . . H4 H 0.634990 0.896261 0.011296 0.009 Uiso 1 1 calc R . . . . N6 N 0.1943(10) 0.6945(5) 0.0769(3) 0.0199(17) Uani 1 1 d . . . . . N7 N 0.9221(9) 0.9987(4) 0.1467(2) 0.0109(15) Uani 1 1 d . . . . . H7 H 0.849553 0.975405 0.168256 0.013 Uiso 1 1 calc R . . . . N2 N 1.0543(11) 0.9970(6) -0.1153(3) 0.0212(19) Uani 1 1 d . . . . . N5 N 0.5380(11) 0.8292(6) 0.1771(3) 0.0215(19) Uani 1 1 d . . . . . C9 C 0.3885(11) 1.1951(6) -0.1741(3) 0.0136(17) Uani 1 1 d . . . . . H9 H 0.403657 1.246417 -0.188785 0.016 Uiso 1 1 calc R . . . . N3 N 0.9343(11) 0.9306(6) -0.2599(3) 0.024(2) Uani 1 1 d . . . . . N8 N 0.7410(10) 0.7270(5) 0.0769(3) 0.0181(17) Uani 1 1 d . . . . . N9 N 1.0109(14) 0.6861(6) 0.2100(3) 0.028(2) Uani 1 1 d . . . . . C24 C 0.9727(13) 0.7370(6) 0.1750(3) 0.019(2) Uani 1 1 d . . . . . C6 C 0.6857(12) 1.0330(5) -0.1799(3) 0.0147(19) Uani 1 1 d . . . . . C10 C 0.3150(11) 1.2111(5) -0.1313(3) 0.0127(18) Uani 1 1 d . . . . . C5 C 0.7349(12) 0.9992(6) -0.2172(3) 0.020(2) Uani 1 1 d . . . . . H5 H 0.665977 0.999664 -0.240982 0.024 Uiso 1 1 calc R . . . . C19 C 0.6005(10) 1.0004(6) -0.0199(3) 0.0114(17) Uani 1 1 d . . . . . H19 H 0.694873 0.985493 -0.037373 0.014 Uiso 1 1 calc R . . . . C14 C 0.2978(11) 0.7601(5) 0.0869(3) 0.0116(17) Uani 1 1 d . . . . . C11 C 0.4931(11) 0.8895(6) 0.1054(3) 0.0130(18) Uani 1 1 d . . . . . C4 C 0.8861(13) 0.9642(6) -0.2205(3) 0.020(2) Uani 1 1 d . . . . . C25 C 1.0363(12) 0.8138(6) 0.1739(3) 0.0140(18) Uani 1 1 d . . . . . H25 H 1.102327 0.831873 0.196188 0.017 Uiso 1 1 calc R . . . . C7 C 0.5270(12) 1.0720(6) -0.1749(3) 0.0161(19) Uani 1 1 d . . . . . H7A H 0.473886 1.050455 -0.149181 0.019 Uiso 1 1 calc R . . . . C17 C 0.4357(11) 0.9509(5) 0.0357(3) 0.0119(17) Uani 1 1 d . . . . . H17 H 0.421307 1.000769 0.051786 0.014 Uiso 1 1 calc R . . . . C30 C 1.0309(11) 1.1252(5) 0.1237(3) 0.0094(17) Uani 1 1 d . . . . . C16 C 0.4110(11) 0.8834(5) 0.0660(3) 0.0108(18) Uani 1 1 d . . . . . C27 C 1.0599(11) 0.9449(5) 0.1385(3) 0.0112(17) Uani 1 1 d . . . . . H27 H 1.095472 0.954242 0.108863 0.013 Uiso 1 1 calc R . . . . C26 C 1.0029(12) 0.8616(6) 0.1409(3) 0.0130(18) Uani 1 1 d . . . . . C12 C 0.4664(12) 0.8283(6) 0.1348(3) 0.0154(19) Uani 1 1 d . . . . . C29 C 0.9833(11) 1.0748(5) 0.1615(3) 0.0115(18) Uani 1 1 d . . . . . H29 H 0.896457 1.102313 0.177180 0.014 Uiso 1 1 calc R . . . . C3 C 0.9874(13) 0.9638(6) -0.1868(3) 0.019(2) Uani 1 1 d . . . . . H3 H 1.090230 0.941086 -0.189273 0.023 Uiso 1 1 calc R . . . . C18 C 0.4485(12) 0.9844(6) -0.0461(3) 0.0160(19) Uani 1 1 d . . . . . H18C H 0.468591 0.943114 -0.067375 0.019 Uiso 1 1 calc R . . . . H18D H 0.413774 1.032593 -0.060841 0.019 Uiso 1 1 calc R . . . . C15 C 0.3154(11) 0.8205(5) 0.0574(3) 0.0141(18) Uani 1 1 d . . . . . H15 H 0.260645 0.817814 0.031223 0.017 Uiso 1 1 calc R . . . . C23 C 0.8776(13) 0.7105(5) 0.1435(3) 0.019(2) Uani 1 1 d . . . . . H23 H 0.834108 0.659222 0.144853 0.022 Uiso 1 1 calc R . . . . C13 C 0.3702(12) 0.7638(6) 0.1252(3) 0.0157(19) Uani 1 1 d . . . . . H13 H 0.355710 0.722976 0.145218 0.019 Uiso 1 1 calc R . . . . C28 C 1.1214(13) 1.0619(5) 0.1913(3) 0.016(2) Uani 1 1 d . . . . . H28A H 1.082411 1.054598 0.220467 0.020 Uiso 1 1 calc R . . . . H28B H 1.194223 1.107486 0.190752 0.020 Uiso 1 1 calc R . . . . C21 C 0.9026(11) 0.8368(5) 0.1067(3) 0.0093(17) Uani 1 1 d . . . . . C2 C 0.9392(12) 0.9968(6) -0.1491(3) 0.0146(18) Uani 1 1 d . . . . . C22 C 0.8441(12) 0.7582(5) 0.1095(3) 0.0151(19) Uani 1 1 d . . . . . C8 C 0.2723(13) 1.1440(6) -0.2013(3) 0.019(2) Uani 1 1 d . . . . . H8A H 0.230578 1.174474 -0.225449 0.023 Uiso 1 1 calc R . . . . H8B H 0.181600 1.125437 -0.184098 0.023 Uiso 1 1 calc R . . . . C1 C 0.7864(12) 1.0326(5) -0.1435(3) 0.0117(17) Uani 1 1 d . . . . . C20 C 0.6181(11) 1.0866(5) -0.0074(3) 0.0109(17) Uani 1 1 d . U . . . O14 O 0.6628(9) 1.1025(4) 0.02956(19) 0.0144(13) Uani 1 1 d . U . . . O27 O 0.1918(9) 1.2341(4) -0.0326(2) 0.0195(15) Uani 1 1 d . . . . . H27A H 0.176357 1.281859 -0.041269 0.029 Uiso 1 1 d G . . . . H27B H 0.261836 1.211414 -0.048650 0.029 Uiso 1 1 d G . . . . O28 O 0.4324(10) 0.6414(5) 0.0149(2) 0.0262(18) Uani 1 1 d . . . . . H28C H 0.434580 0.674375 -0.006060 0.039 Uiso 1 1 d G . . . . H28D H 0.526564 0.638429 0.026117 0.039 Uiso 1 1 d G . . . . O29 O 0.7872(13) 1.2396(6) -0.2305(3) 0.042(2) Uani 1 1 d . . . . . H29A H 0.841906 1.235679 -0.253661 0.063 Uiso 1 1 d G . . . . H29B H 0.807413 1.284402 -0.218515 0.063 Uiso 1 1 d G . . . . 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 Tb2 0.01076(19) 0.00728(18) 0.00536(18) 0.00073(14) -0.00233(15) -0.00046(14) Tb1 0.0117(2) 0.01043(19) 0.00677(19) -0.00019(15) -0.00104(15) 0.00134(15) S2 0.0089(11) 0.0301(13) 0.0198(12) 0.0071(10) -0.0054(9) -0.0015(9) S3 0.0157(11) 0.0217(12) 0.0249(12) -0.0065(9) -0.0073(10) 0.0026(10) S1 0.0209(12) 0.0229(12) 0.0199(12) -0.0102(10) -0.0071(10) 0.0041(10) O12 0.018(3) 0.016(3) 0.008(3) 0.000(2) 0.001(3) -0.008(3) O18 0.016(3) 0.025(4) 0.019(3) -0.007(3) 0.006(3) 0.001(3) O3 0.0152(13) 0.0152(13) 0.0151(13) 0.00002(14) 0.00000(14) 0.00001(14) O17 0.020(4) 0.018(3) 0.012(3) 0.002(3) 0.004(3) 0.006(3) O8 0.015(4) 0.077(7) 0.025(4) 0.004(4) -0.006(3) -0.004(4) O16 0.021(3) 0.007(3) 0.012(3) 0.004(2) -0.001(3) -0.003(3) O22 0.022(4) 0.025(4) 0.022(4) 0.001(3) -0.002(3) -0.007(3) O6 0.023(4) 0.020(4) 0.030(4) -0.006(3) -0.009(3) 0.008(3) O15 0.017(3) 0.019(3) 0.009(3) 0.002(2) -0.002(2) -0.007(3) O13 0.022(3) 0.008(3) 0.010(3) 0.002(2) -0.005(3) 0.006(2) O5 0.046(5) 0.018(3) 0.012(3) -0.001(3) -0.008(3) 0.008(4) O2 0.012(3) 0.023(3) 0.007(3) 0.001(3) -0.002(2) 0.000(3) O4 0.014(3) 0.036(4) 0.017(4) 0.003(3) -0.004(3) 0.000(3) O21 0.042(5) 0.010(3) 0.039(5) 0.007(3) 0.001(4) -0.009(3) O1 0.018(3) 0.014(3) 0.010(3) -0.001(2) -0.002(3) 0.003(3) O7 0.044(5) 0.045(5) 0.016(4) 0.002(4) -0.007(4) 0.021(4) O11 0.013(3) 0.024(4) 0.032(4) -0.009(3) -0.003(3) 0.006(3) O19 0.035(5) 0.037(5) 0.023(4) 0.004(3) -0.015(4) -0.009(4) O10 0.028(4) 0.051(5) 0.017(4) -0.017(4) -0.004(3) 0.009(4) O23 0.029(4) 0.025(4) 0.018(4) -0.005(3) -0.006(3) -0.005(3) O25 0.084(8) 0.024(5) 0.033(5) 0.018(4) -0.010(5) -0.016(5) O9 0.029(5) 0.054(6) 0.042(6) -0.017(5) 0.007(4) 0.020(4) O24 0.021(4) 0.026(4) 0.033(4) -0.004(3) 0.000(3) -0.013(3) O26 0.073(7) 0.036(5) 0.019(4) 0.009(4) -0.018(4) 0.002(5) O20 0.074(8) 0.077(8) 0.029(5) 0.029(5) -0.014(5) -0.041(7) N1 0.016(4) 0.008(3) 0.009(4) 0.001(3) 0.001(3) 0.001(3) N4 0.009(3) 0.007(3) 0.006(3) 0.004(3) 0.001(3) -0.001(3) N6 0.020(4) 0.019(4) 0.021(4) -0.007(4) 0.014(4) -0.006(4) N7 0.013(4) 0.009(4) 0.011(3) 0.000(3) 0.004(3) 0.001(3) N2 0.023(4) 0.026(5) 0.014(4) 0.003(4) -0.006(3) 0.004(4) N5 0.019(5) 0.030(5) 0.015(4) 0.004(4) 0.001(4) 0.001(4) C9 0.014(4) 0.015(4) 0.012(4) -0.002(4) -0.006(3) 0.004(4) N3 0.020(4) 0.034(5) 0.018(4) -0.007(4) 0.003(4) -0.001(4) N8 0.016(4) 0.015(4) 0.024(4) -0.008(3) 0.000(4) 0.000(3) N9 0.054(6) 0.019(4) 0.010(4) 0.004(4) -0.001(4) 0.005(5) C24 0.025(6) 0.014(5) 0.018(5) 0.004(4) 0.006(4) 0.002(4) C6 0.017(5) 0.014(4) 0.013(4) -0.004(3) 0.000(4) 0.001(4) C10 0.011(4) 0.011(4) 0.016(4) 0.002(3) -0.002(4) 0.000(3) C5 0.014(4) 0.029(5) 0.016(4) 0.001(4) 0.001(4) -0.003(4) C19 0.009(4) 0.021(5) 0.004(4) 0.000(3) -0.003(3) 0.002(4) C14 0.009(4) 0.010(4) 0.015(4) -0.004(3) 0.007(3) -0.002(3) C11 0.012(4) 0.015(4) 0.012(5) -0.002(3) 0.001(3) -0.003(3) C4 0.018(5) 0.025(5) 0.016(5) -0.003(4) 0.005(4) 0.000(4) C25 0.024(5) 0.010(4) 0.008(4) -0.001(3) -0.002(3) 0.002(4) C7 0.016(5) 0.016(5) 0.017(5) -0.003(4) 0.002(4) 0.003(4) C17 0.017(4) 0.011(4) 0.008(4) 0.003(3) 0.000(4) -0.001(4) C30 0.008(4) 0.009(4) 0.011(4) -0.004(3) -0.001(3) 0.000(3) C16 0.014(4) 0.013(4) 0.006(4) 0.000(3) -0.003(3) -0.001(3) C27 0.013(4) 0.014(4) 0.007(4) -0.002(3) 0.000(3) 0.000(4) C26 0.014(4) 0.015(4) 0.011(4) -0.003(3) 0.000(4) 0.001(4) C12 0.013(5) 0.022(5) 0.011(4) 0.005(4) 0.005(4) -0.002(4) C29 0.014(4) 0.006(4) 0.015(4) -0.001(3) -0.002(4) 0.000(3) C3 0.020(5) 0.020(5) 0.018(5) -0.006(4) -0.001(4) 0.005(4) C18 0.019(5) 0.018(4) 0.011(4) -0.001(4) -0.005(4) 0.003(4) C15 0.011(4) 0.018(4) 0.013(4) 0.000(4) 0.005(3) -0.002(4) C23 0.026(5) 0.009(4) 0.020(5) 0.003(4) 0.009(4) -0.001(4) C13 0.013(5) 0.014(4) 0.020(5) 0.003(4) 0.005(4) -0.001(4) C28 0.025(5) 0.008(4) 0.016(5) 0.000(3) -0.009(4) 0.000(4) C21 0.017(4) 0.006(4) 0.005(4) -0.002(3) 0.000(3) -0.001(3) C2 0.020(5) 0.014(4) 0.009(4) 0.000(3) -0.007(4) -0.001(4) C22 0.019(5) 0.012(4) 0.015(5) -0.001(3) -0.001(4) -0.001(4) C8 0.020(5) 0.021(5) 0.015(5) -0.009(4) -0.007(4) 0.000(4) C1 0.014(4) 0.009(4) 0.012(4) 0.002(3) 0.002(4) -0.001(3) C20 0.009(4) 0.015(4) 0.009(4) 0.006(3) 0.002(3) 0.002(3) O14 0.023(3) 0.015(3) 0.005(3) 0.002(2) -0.006(3) 0.002(3) O27 0.024(4) 0.017(3) 0.018(3) -0.003(3) 0.004(3) -0.003(3) O28 0.026(4) 0.035(4) 0.018(4) -0.011(3) -0.006(3) 0.010(3) O29 0.051(6) 0.052(6) 0.022(4) 0.002(4) 0.013(4) 0.002(5) 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 O12 Tb2 O18 144.2(3) . . ? O12 Tb2 O17 70.1(2) . . ? O12 Tb2 O15 139.1(2) . . ? O12 Tb2 O13 78.4(2) . . ? O12 Tb2 N4 76.5(2) . . ? O12 Tb2 N7 81.2(2) . . ? O12 Tb2 O14 110.1(3) . . ? O18 Tb2 O17 142.8(2) . . ? O18 Tb2 O15 74.1(2) . . ? O18 Tb2 N4 75.7(2) . . ? O18 Tb2 N7 114.0(2) . . ? O17 Tb2 N4 113.3(2) . . ? O17 Tb2 N7 77.3(2) . . ? O15 Tb2 O17 80.5(2) . . ? O15 Tb2 N4 143.1(2) . . ? O15 Tb2 N7 64.6(2) . . ? O13 Tb2 O18 75.0(3) . . ? O13 Tb2 O17 140.7(2) . . ? O13 Tb2 O15 111.3(2) . . ? O13 Tb2 N4 80.3(2) . . ? O13 Tb2 N7 75.1(2) . . ? O13 Tb2 O14 140.6(2) . . ? N7 Tb2 N4 149.5(2) . . ? O14 Tb2 O18 77.8(3) . . ? O14 Tb2 O17 74.4(2) . . ? O14 Tb2 O15 87.7(2) . . ? O14 Tb2 N4 65.5(2) . . ? O14 Tb2 N7 143.1(2) . . ? O3 Tb1 O16 132.6(2) . 3_475 ? O3 Tb1 O6 76.1(3) . . ? O3 Tb1 O5 79.2(2) . . ? O3 Tb1 O2 72.9(2) . . ? O3 Tb1 O4 149.5(3) . . ? O3 Tb1 N1 121.7(2) . . ? O16 Tb1 O6 126.6(3) 3_475 . ? O16 Tb1 N1 72.7(2) 3_475 . ? O6 Tb1 N1 137.1(3) . . ? O5 Tb1 O16 70.9(2) . 3_475 ? O5 Tb1 O6 74.2(3) . . ? O5 Tb1 N1 142.7(2) . . ? O2 Tb1 O16 75.4(2) . 3_475 ? O2 Tb1 O6 148.9(3) . . ? O2 Tb1 O5 97.4(3) . . ? O2 Tb1 O4 135.0(2) . . ? O2 Tb1 N1 65.3(2) . . ? O4 Tb1 O16 75.2(2) . 3_475 ? O4 Tb1 O6 75.8(3) . . ? O4 Tb1 O5 104.2(3) . . ? O4 Tb1 N1 73.9(3) . . ? O1 Tb1 O3 80.1(2) . . ? O1 Tb1 O16 142.2(2) . 3_475 ? O1 Tb1 O6 72.6(2) . . ? O1 Tb1 O5 144.2(2) . . ? O1 Tb1 O2 104.0(2) . . ? O1 Tb1 O4 80.4(3) . . ? O1 Tb1 N1 73.1(2) . . ? C18 S2 C17 94.3(4) . . ? C28 S3 C27 93.4(4) . . ? C8 S1 C7 90.9(4) . . ? C11 O12 Tb2 133.7(6) . . ? C20 O3 Tb1 145.4(6) . . ? C30 O16 Tb1 138.2(6) . 3_575 ? C30 O15 Tb2 123.8(6) . . ? C21 O13 Tb2 132.8(6) . . ? C10 O2 Tb1 122.4(6) . . ? C1 O1 Tb1 130.5(6) . . ? C9 N1 Tb1 110.2(5) . . ? C7 N1 Tb1 112.8(6) . . ? C7 N1 C9 108.1(7) . . ? C19 N4 Tb2 110.3(5) . . ? C19 N4 C17 108.1(7) . . ? C17 N4 Tb2 105.5(5) . . ? O22 N6 O21 124.5(9) . . ? O22 N6 C14 118.7(8) . . ? O21 N6 C14 116.8(9) . . ? C27 N7 Tb2 105.6(5) . . ? C29 N7 Tb2 111.7(5) . . ? C29 N7 C27 109.0(7) . . ? O8 N2 C2 117.8(9) . . ? O7 N2 O8 121.9(9) . . ? O7 N2 C2 120.3(9) . . ? O19 N5 O20 122.6(10) . . ? O19 N5 C12 120.4(9) . . ? O20 N5 C12 117.0(10) . . ? N1 C9 C10 110.9(7) . . ? N1 C9 C8 111.7(8) . . ? C10 C9 C8 109.8(8) . . ? O10 N3 O9 123.2(10) . . ? O10 N3 C4 119.4(9) . . ? O9 N3 C4 117.3(10) . . ? O23 N8 C22 119.5(8) . . ? O24 N8 O23 122.0(9) . . ? O24 N8 C22 118.5(9) . . ? O25 N9 C24 117.5(10) . . ? O26 N9 O25 123.4(10) . . ? O26 N9 C24 119.1(10) . . ? C25 C24 N9 119.5(10) . . ? C23 C24 N9 119.7(9) . . ? C23 C24 C25 120.8(9) . . ? C5 C6 C7 122.8(9) . . ? C5 C6 C1 120.9(9) . . ? C1 C6 C7 116.3(8) . . ? O2 C10 C9 119.1(8) . . ? O11 C10 O2 124.3(9) . . ? O11 C10 C9 116.6(8) . . ? C6 C5 C4 120.7(9) . . ? N4 C19 C18 109.6(7) . . ? N4 C19 C20 109.9(7) . . ? C20 C19 C18 112.8(8) . . ? C15 C14 N6 119.0(8) . . ? C13 C14 N6 119.9(8) . . ? C13 C14 C15 121.1(8) . . ? O12 C11 C16 120.3(8) . . ? O12 C11 C12 123.3(9) . . ? C12 C11 C16 116.4(8) . . ? C5 C4 N3 119.3(10) . . ? C3 C4 N3 120.3(10) . . ? C3 C4 C5 120.5(9) . . ? C26 C25 C24 119.9(9) . . ? N1 C7 S1 105.1(7) . . ? N1 C7 C6 110.1(8) . . ? C6 C7 S1 115.3(7) . . ? N4 C17 S2 106.9(6) . . ? N4 C17 C16 111.3(7) . . ? C16 C17 S2 114.9(7) . . ? O16 C30 O15 125.5(9) . . ? O16 C30 C29 116.5(8) . . ? O15 C30 C29 118.0(8) . . ? C11 C16 C17 115.6(8) . . ? C15 C16 C11 121.0(8) . . ? C15 C16 C17 123.4(8) . . ? N7 C27 S3 108.2(6) . . ? N7 C27 C26 109.0(8) . . ? C26 C27 S3 117.8(7) . . ? C25 C26 C27 122.8(9) . . ? C25 C26 C21 121.8(9) . . ? C21 C26 C27 115.3(8) . . ? C11 C12 N5 121.9(9) . . ? C13 C12 N5 116.3(9) . . ? C13 C12 C11 121.8(9) . . ? N7 C29 C30 109.6(7) . . ? N7 C29 C28 109.8(7) . . ? C28 C29 C30 111.8(8) . . ? C4 C3 C2 119.5(10) . . ? C19 C18 S2 106.1(6) . . ? C16 C15 C14 120.4(9) . . ? C24 C23 C22 120.0(9) . . ? C14 C13 C12 119.3(9) . . ? C29 C28 S3 106.4(6) . . ? O13 C21 C26 119.4(8) . . ? O13 C21 C22 125.1(8) . . ? C22 C21 C26 115.4(8) . . ? C3 C2 N2 116.5(9) . . ? C3 C2 C1 123.0(9) . . ? C1 C2 N2 120.4(8) . . ? C23 C22 N8 117.5(9) . . ? C23 C22 C21 122.1(9) . . ? C21 C22 N8 120.3(8) . . ? C9 C8 S1 105.4(7) . . ? O1 C1 C6 119.6(9) . . ? O1 C1 C2 124.8(8) . . ? C6 C1 C2 115.5(8) . . ? O3 C20 C19 118.0(8) . . ? O3 C20 O14 123.5(9) . . ? O14 C20 C19 118.5(8) . . ? C20 O14 Tb2 124.2(6) . . ? 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 Tb2 O12 2.279(7) . ? Tb2 O18 2.376(7) . ? Tb2 O17 2.405(7) . ? Tb2 O15 2.378(7) . ? Tb2 O13 2.312(6) . ? Tb2 N4 2.578(7) . ? Tb2 N7 2.567(8) . ? Tb2 O14 2.341(6) . ? Tb1 O3 2.310(7) . ? Tb1 O16 2.386(6) 3_475 ? Tb1 O6 2.416(8) . ? Tb1 O5 2.384(7) . ? Tb1 O2 2.351(6) . ? Tb1 O4 2.373(7) . ? Tb1 O1 2.301(6) . ? Tb1 N1 2.616(8) . ? S2 C17 1.826(10) . ? S2 C18 1.802(10) . ? S3 C27 1.827(10) . ? S3 C28 1.826(10) . ? S1 C7 1.832(11) . ? S1 C8 1.826(10) . ? O12 C11 1.287(11) . ? O3 C20 1.253(11) . ? O8 N2 1.235(12) . ? O16 C30 1.244(11) . ? O22 N6 1.218(12) . ? O15 C30 1.270(11) . ? O13 C21 1.276(11) . ? O2 C10 1.280(11) . ? O21 N6 1.243(12) . ? O1 C1 1.267(11) . ? O7 N2 1.232(12) . ? O11 C10 1.258(13) . ? O19 N5 1.206(12) . ? O10 N3 1.237(13) . ? O23 N8 1.233(12) . ? O25 N9 1.232(14) . ? O9 N3 1.239(13) . ? O24 N8 1.226(11) . ? O26 N9 1.220(14) . ? O20 N5 1.217(13) . ? N1 C9 1.493(12) . ? N1 C7 1.475(12) . ? N4 C19 1.473(11) . ? N4 C17 1.487(12) . ? N6 C14 1.452(11) . ? N7 C27 1.501(12) . ? N7 C29 1.475(11) . ? N2 C2 1.444(12) . ? N5 C12 1.471(13) . ? C9 C10 1.517(13) . ? C9 C8 1.569(13) . ? N3 C4 1.433(13) . ? N8 C22 1.450(12) . ? N9 C24 1.447(13) . ? C24 C25 1.416(14) . ? C24 C23 1.358(16) . ? C6 C5 1.381(14) . ? C6 C7 1.498(13) . ? C6 C1 1.433(13) . ? C5 C4 1.409(15) . ? C19 C18 1.549(12) . ? C19 C20 1.532(13) . ? C14 C15 1.401(13) . ? C14 C13 1.361(14) . ? C11 C16 1.432(12) . ? C11 C12 1.420(13) . ? C4 C3 1.366(15) . ? C25 C26 1.355(14) . ? C17 C16 1.516(12) . ? C30 C29 1.529(13) . ? C16 C15 1.368(13) . ? C27 C26 1.503(13) . ? C26 C21 1.439(13) . ? C12 C13 1.400(14) . ? C29 C28 1.512(13) . ? C3 C2 1.382(14) . ? C23 C22 1.380(14) . ? C21 C22 1.431(12) . ? C2 C1 1.433(13) . ? C20 O14 1.260(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 Tb2 O12 C11 C16 -47.4(13) . . . . ? Tb2 O12 C11 C12 134.1(8) . . . . ? Tb2 O15 C30 O16 -159.4(7) . . . . ? Tb2 O15 C30 C29 16.9(11) . . . . ? Tb2 O13 C21 C26 -51.6(12) . . . . ? Tb2 O13 C21 C22 128.1(8) . . . . ? Tb2 N4 C19 C18 -156.8(6) . . . . ? Tb2 N4 C19 C20 -32.3(8) . . . . ? Tb2 N4 C17 S2 154.2(4) . . . . ? Tb2 N4 C17 C16 -79.6(7) . . . . ? Tb2 N7 C27 S3 147.9(4) . . . . ? Tb2 N7 C27 C26 -82.9(7) . . . . ? Tb2 N7 C29 C30 -32.9(8) . . . . ? Tb2 N7 C29 C28 -156.1(6) . . . . ? Tb1 O3 C20 C19 -69.5(14) . . . . ? Tb1 O3 C20 O14 109.4(12) . . . . ? Tb1 O16 C30 O15 12.7(15) 3_575 . . . ? Tb1 O16 C30 C29 -163.7(6) 3_575 . . . ? Tb1 O2 C10 O11 -150.6(7) . . . . ? Tb1 O2 C10 C9 27.4(11) . . . . ? Tb1 O1 C1 C6 -60.6(11) . . . . ? Tb1 O1 C1 C2 116.0(9) . . . . ? Tb1 N1 C9 C10 -25.8(9) . . . . ? Tb1 N1 C9 C8 -148.7(6) . . . . ? Tb1 N1 C7 S1 165.2(4) . . . . ? Tb1 N1 C7 C6 -70.1(8) . . . . ? S2 C17 C16 C11 -167.5(7) . . . . ? S2 C17 C16 C15 11.6(12) . . . . ? S3 C27 C26 C25 17.7(13) . . . . ? S3 C27 C26 C21 -165.4(7) . . . . ? O12 C11 C16 C17 -1.0(13) . . . . ? O12 C11 C16 C15 179.9(9) . . . . ? O12 C11 C12 N5 1.2(15) . . . . ? O12 C11 C12 C13 -178.8(9) . . . . ? O3 C20 O14 Tb2 -164.2(7) . . . . ? O8 N2 C2 C3 20.3(15) . . . . ? O8 N2 C2 C1 -157.0(10) . . . . ? O16 C30 C29 N7 -170.0(8) . . . . ? O16 C30 C29 C28 -48.0(11) . . . . ? O22 N6 C14 C15 -11.3(12) . . . . ? O22 N6 C14 C13 165.8(9) . . . . ? O15 C30 C29 N7 13.4(11) . . . . ? O15 C30 C29 C28 135.4(9) . . . . ? O13 C21 C22 N8 -0.1(14) . . . . ? O13 C21 C22 C23 -177.7(10) . . . . ? O21 N6 C14 C15 170.2(8) . . . . ? O21 N6 C14 C13 -12.7(13) . . . . ? O7 N2 C2 C3 -159.2(10) . . . . ? O7 N2 C2 C1 23.5(15) . . . . ? O19 N5 C12 C11 -12.4(15) . . . . ? O19 N5 C12 C13 167.7(10) . . . . ? O10 N3 C4 C5 7.1(16) . . . . ? O10 N3 C4 C3 -171.2(11) . . . . ? O23 N8 C22 C23 -160.7(9) . . . . ? O23 N8 C22 C21 21.6(13) . . . . ? O25 N9 C24 C25 170.9(11) . . . . ? O25 N9 C24 C23 -9.7(16) . . . . ? O9 N3 C4 C5 -175.1(11) . . . . ? O9 N3 C4 C3 6.5(16) . . . . ? O24 N8 C22 C23 20.3(13) . . . . ? O24 N8 C22 C21 -157.4(9) . . . . ? O26 N9 C24 C25 -8.8(16) . . . . ? O26 N9 C24 C23 170.6(11) . . . . ? O20 N5 C12 C11 164.7(12) . . . . ? O20 N5 C12 C13 -15.3(15) . . . . ? N1 C9 C10 O2 2.9(12) . . . . ? N1 C9 C10 O11 -178.9(8) . . . . ? N1 C9 C8 S1 -4.7(9) . . . . ? N4 C19 C18 S2 27.8(9) . . . . ? N4 C19 C20 O3 -166.0(8) . . . . ? N4 C19 C20 O14 15.1(11) . . . . ? N4 C17 C16 C11 70.8(10) . . . . ? N4 C17 C16 C15 -110.2(10) . . . . ? N6 C14 C15 C16 179.5(8) . . . . ? N6 C14 C13 C12 -178.3(8) . . . . ? N7 C27 C26 C25 -106.0(10) . . . . ? N7 C27 C26 C21 70.9(10) . . . . ? N7 C29 C28 S3 32.9(9) . . . . ? N2 C2 C1 O1 -0.4(14) . . . . ? N2 C2 C1 C6 176.4(9) . . . . ? N5 C12 C13 C14 178.7(9) . . . . ? C9 N1 C7 S1 43.1(8) . . . . ? C9 N1 C7 C6 167.9(8) . . . . ? N3 C4 C3 C2 179.7(10) . . . . ? N9 C24 C25 C26 179.1(10) . . . . ? N9 C24 C23 C22 -178.3(10) . . . . ? C24 C25 C26 C27 177.1(9) . . . . ? C24 C25 C26 C21 0.4(15) . . . . ? C24 C23 C22 N8 -179.6(9) . . . . ? C24 C23 C22 C21 -2.0(16) . . . . ? C6 C5 C4 N3 -179.1(10) . . . . ? C6 C5 C4 C3 -0.8(16) . . . . ? C10 C9 C8 S1 -128.1(7) . . . . ? C5 C6 C7 S1 7.2(13) . . . . ? C5 C6 C7 N1 -111.5(11) . . . . ? C5 C6 C1 O1 178.3(9) . . . . ? C5 C6 C1 C2 1.4(13) . . . . ? C5 C4 C3 C2 1.3(16) . . . . ? C19 N4 C17 S2 36.2(8) . . . . ? C19 N4 C17 C16 162.4(7) . . . . ? C19 C20 O14 Tb2 14.6(12) . . . . ? C11 C16 C15 C14 -0.9(14) . . . . ? C11 C12 C13 C14 -1.3(15) . . . . ? C4 C3 C2 N2 -177.8(10) . . . . ? C4 C3 C2 C1 -0.6(16) . . . . ? C25 C24 C23 C22 1.1(16) . . . . ? C25 C26 C21 O13 178.5(9) . . . . ? C25 C26 C21 C22 -1.2(14) . . . . ? C7 S1 C8 C9 25.0(7) . . . . ? C7 N1 C9 C10 97.9(9) . . . . ? C7 N1 C9 C8 -25.0(10) . . . . ? C7 C6 C5 C4 179.3(9) . . . . ? C7 C6 C1 O1 -1.6(13) . . . . ? C7 C6 C1 C2 -178.6(8) . . . . ? C17 S2 C18 C19 -5.6(7) . . . . ? C17 N4 C19 C18 -41.9(9) . . . . ? C17 N4 C19 C20 82.6(8) . . . . ? C17 C16 C15 C14 -179.9(8) . . . . ? C30 C29 C28 S3 -89.0(8) . . . . ? C16 C11 C12 N5 -177.3(9) . . . . ? C16 C11 C12 C13 2.6(14) . . . . ? C27 S3 C28 C29 -14.0(7) . . . . ? C27 N7 C29 C30 83.4(8) . . . . ? C27 N7 C29 C28 -39.8(10) . . . . ? C27 C26 C21 O13 1.6(13) . . . . ? C27 C26 C21 C22 -178.2(8) . . . . ? C26 C21 C22 N8 179.6(9) . . . . ? C26 C21 C22 C23 2.0(14) . . . . ? C12 C11 C16 C17 177.6(8) . . . . ? C12 C11 C16 C15 -1.5(14) . . . . ? C29 N7 C27 S3 27.7(8) . . . . ? C29 N7 C27 C26 157.0(7) . . . . ? C3 C2 C1 O1 -177.5(9) . . . . ? C3 C2 C1 C6 -0.8(14) . . . . ? C18 S2 C17 N4 -17.1(7) . . . . ? C18 S2 C17 C16 -141.2(7) . . . . ? C18 C19 C20 O3 -43.4(11) . . . . ? C18 C19 C20 O14 137.6(9) . . . . ? C15 C14 C13 C12 -1.3(14) . . . . ? C23 C24 C25 C26 -0.3(16) . . . . ? C13 C14 C15 C16 2.4(14) . . . . ? C28 S3 C27 N7 -7.4(7) . . . . ? C28 S3 C27 C26 -131.5(7) . . . . ? C8 S1 C7 N1 -40.2(7) . . . . ? C8 S1 C7 C6 -161.6(8) . . . . ? C8 C9 C10 O2 126.8(9) . . . . ? C8 C9 C10 O11 -55.0(11) . . . . ? C1 C6 C5 C4 -0.7(15) . . . . ? C1 C6 C7 S1 -172.9(7) . . . . ? C1 C6 C7 N1 68.4(11) . . . . ? C20 C19 C18 S2 -95.0(8) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.965(15) 2 0.035(15)