#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:26:52 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296449 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249368.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_7249368 loop_ _publ_author_name 'Cui, Wen-Bo' 'Huang, Li' 'Shen, Yuan' 'Yu, Xiao-Yang' 'Li, Zi-Yi' 'Zhang, Hong' _publ_section_title ; Viologen-based Ln-MOF material with photochromicity and photoluminescence for anticounterfeiting ; _journal_issue 41 _journal_name_full CrystEngComm _journal_page_first 5877 _journal_page_last 5882 _journal_paper_doi 10.1039/D4CE00652F _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C40 H24 Cl N4 O18 Tb2, 3(H2 O), 3(O)' _chemical_formula_sum 'C40 H30 Cl N4 O24 Tb2' _chemical_formula_weight 1303.97 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _audit_creation_date 2024-06-04 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2024-06-11 deposited with the CCDC. 2024-09-19 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 101.468(3) _cell_angle_gamma 90 _cell_formula_units_Z 8 _cell_length_a 36.461(3) _cell_length_b 12.5228(9) _cell_length_c 20.6904(14) _cell_measurement_reflns_used 9620 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 24.986 _cell_measurement_theta_min 2.428 _cell_volume 9258.5(12) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_reduction 'SAINT V8.38A (?, 2016)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 298.15 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1685 _diffrn_reflns_av_unetI/netI 0.0978 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_limit_h_max 43 _diffrn_reflns_limit_h_min -43 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_number 39508 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.992 _diffrn_reflns_theta_full 25.114 _diffrn_reflns_theta_max 25.114 _diffrn_reflns_theta_min 2.360 _exptl_absorpt_coefficient_mu 3.181 _exptl_absorpt_correction_type none _exptl_crystal_colour 'clear yellowish green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier yellowish _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.871 _exptl_crystal_description block _exptl_crystal_F_000 5096 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.1 _refine_diff_density_max 2.517 _refine_diff_density_min -2.206 _refine_diff_density_rms 0.233 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.048 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 649 _refine_ls_number_reflns 8184 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.048 _refine_ls_R_factor_all 0.0795 _refine_ls_R_factor_gt 0.0584 _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^)+(0.0830P)^2^+60.9937P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1490 _refine_ls_wR_factor_ref 0.1613 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6356 _reflns_number_total 8184 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00652f2.cif _cod_data_source_block 2 _cod_depositor_comments 'Adding full bibliography for 7249367--7249368.cif.' _cod_database_code 7249368 _shelx_shelxl_version_number 2016/4 _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. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All O(H,H) groups 2.a Free rotating group: O23(H23A,H23B), O21(H21A,H21B), O22(H22A,H22B) 2.b Aromatic/amide H refined with riding coordinates: C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11), C14(H14), C15(H15), C16(H16), C17(H17), C19(H19), C20(H20), C22(H22), C23(H23), C27(H27), C28(H28), C29(H29), C31(H31), C35(H35), C36(H36), C37(H37), C39(H39) ; _shelx_res_file ; TITL 2_a.res in C2/c 2.res created by SHELXL-2016/4 at 20:48:29 on 04-Jun-2024 REM Old TITL 2 in C2/c REM SHELXT solution in C2/c REM R1 0.129, Rweak 0.008, Alpha 0.041, Orientation as input REM Formula found by SHELXT: C39 N11 O18 Tb2 CELL 0.71073 36.4611 12.5228 20.6904 90 101.468 90 ZERR 8 0.0032 0.0009 0.0014 0 0.003 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H Cl N O Tb UNIT 320 240 8 32 192 16 L.S. 4 0 0 PLAN 20 TEMP 19.71 BOND $h conf BOND $H list 4 fmap 2 53 acta OMIT 4 0 0 OMIT 4 0 4 OMIT 4 0 2 REM REM REM WGHT 0.083000 60.993702 FVAR 0.10408 C1 1 0.435336 0.176148 0.430124 11.00000 0.01622 0.02591 = 0.02109 -0.00392 -0.00584 0.00204 C2 1 0.476434 0.163277 0.428395 11.00000 0.01316 0.04503 = 0.02694 -0.00448 0.00353 0.00348 C3 1 0.487145 0.143290 0.369827 11.00000 0.02081 0.07959 = 0.03502 -0.01601 -0.00501 0.00817 AFIX 43 H3 2 0.468986 0.131216 0.332106 11.00000 -1.20000 AFIX 0 C4 1 0.524542 0.140757 0.365833 11.00000 0.01978 0.14297 = 0.02432 -0.02643 -0.00065 0.02316 AFIX 43 H4 2 0.531369 0.128020 0.325541 11.00000 -1.20000 AFIX 0 C5 1 0.551481 0.156995 0.421170 11.00000 0.02495 0.11968 = 0.03960 -0.01075 0.00571 0.01190 AFIX 43 H5 2 0.576634 0.158514 0.418472 11.00000 -1.20000 AFIX 0 C6 1 0.503139 0.177044 0.485286 11.00000 0.01827 0.03878 = 0.02760 -0.00693 -0.00680 0.00195 AFIX 43 H6 2 0.496077 0.189973 0.525360 11.00000 -1.20000 AFIX 0 C7 1 0.540831 0.171238 0.481636 11.00000 0.01930 0.05510 = 0.02900 -0.01207 -0.00739 0.00634 C8 1 0.595711 0.259858 0.540149 11.00000 0.02620 0.09325 = 0.03215 0.00655 0.00014 -0.00899 AFIX 43 H8 2 0.595883 0.300056 0.502416 11.00000 -1.20000 AFIX 0 C9 1 0.568347 0.129718 0.594863 11.00000 0.02860 0.04213 = 0.05705 0.00348 -0.01531 -0.00691 AFIX 43 H9 2 0.550047 0.077709 0.593988 11.00000 -1.20000 AFIX 0 C10 1 0.593925 0.145802 0.652129 11.00000 0.02845 0.03325 = 0.04149 0.00774 -0.01867 -0.01601 AFIX 43 H10 2 0.592273 0.107720 0.690033 11.00000 -1.20000 AFIX 0 C11 1 0.622833 0.275668 0.595548 11.00000 0.02058 0.08342 = 0.03476 0.00079 -0.01061 -0.01030 AFIX 43 H11 2 0.641830 0.324812 0.594502 11.00000 -1.20000 AFIX 0 C12 1 0.622350 0.219737 0.652803 11.00000 0.01521 0.03895 = 0.03086 -0.00053 -0.00708 0.00589 C13 1 0.650716 0.242328 0.714162 11.00000 0.01406 0.02485 = 0.03368 -0.00445 -0.00202 -0.00155 C14 1 0.644705 0.217537 0.775563 11.00000 0.01239 0.03959 = 0.03528 0.00518 -0.00107 -0.00036 AFIX 43 H14 2 0.622785 0.182393 0.779491 11.00000 -1.20000 AFIX 0 C15 1 0.670292 0.243319 0.831655 11.00000 0.01436 0.04228 = 0.02951 0.00013 0.00609 -0.00592 AFIX 43 H15 2 0.665454 0.227826 0.873118 11.00000 -1.20000 AFIX 0 C16 1 0.684803 0.290440 0.710793 11.00000 0.02531 0.03754 = 0.02247 -0.00098 0.00239 -0.00090 AFIX 43 H16 2 0.690231 0.306478 0.669820 11.00000 -1.20000 AFIX 0 C17 1 0.710110 0.314161 0.766221 11.00000 0.01499 0.04985 = 0.01945 -0.00581 0.00495 -0.01447 AFIX 43 H17 2 0.732700 0.346145 0.763018 11.00000 -1.20000 AFIX 0 C18 1 0.729557 0.323200 0.884829 11.00000 0.00744 0.03360 = 0.01821 -0.00153 -0.00553 -0.00317 C19 1 0.717990 0.393468 0.928604 11.00000 0.01621 0.04118 = 0.03027 -0.00042 0.00546 -0.00161 AFIX 43 H19 2 0.693813 0.420923 0.921008 11.00000 -1.20000 AFIX 0 C20 1 0.765213 0.279959 0.893613 11.00000 0.01575 0.02616 = 0.02244 -0.00360 0.00384 0.00269 AFIX 43 H20 2 0.771891 0.233459 0.862858 11.00000 -1.20000 AFIX 0 C21 1 0.790719 0.309224 0.950685 11.00000 0.00924 0.02881 = 0.02053 0.00428 0.00145 -0.00223 C22 1 0.744204 0.420622 0.984074 11.00000 0.02181 0.04759 = 0.01857 -0.01025 0.00752 0.00632 AFIX 43 H22 2 0.737448 0.467972 1.014309 11.00000 -1.20000 AFIX 0 C23 1 0.780045 0.379819 0.996064 11.00000 0.01693 0.03691 = 0.02161 -0.00095 0.00241 0.00201 AFIX 43 H23 2 0.797012 0.399066 1.034040 11.00000 -1.20000 AFIX 0 C24 1 0.829318 0.264406 0.964271 11.00000 0.01934 0.02281 = 0.02231 0.00302 0.00376 -0.00083 C25 1 0.420408 0.513273 0.314276 11.00000 0.01595 0.03770 = 0.02154 0.00568 -0.00079 -0.00430 C26 1 0.404046 0.425402 0.347608 11.00000 0.01680 0.03983 = 0.02292 0.00344 0.00428 0.00292 C27 1 0.448780 0.577560 0.349188 11.00000 0.03401 0.04883 = 0.01827 -0.00428 -0.00240 -0.00030 AFIX 43 H27 2 0.457099 0.566191 0.394133 11.00000 -1.20000 AFIX 0 C28 1 0.464565 0.656824 0.318664 11.00000 0.02691 0.04935 = 0.03105 0.00615 -0.00329 -0.01417 AFIX 43 H28 2 0.483568 0.698963 0.342434 11.00000 -1.20000 AFIX 0 C29 1 0.451887 0.673759 0.251635 11.00000 0.02268 0.04436 = 0.03401 0.00639 0.00839 -0.01232 AFIX 43 H29 2 0.462615 0.727833 0.230777 11.00000 -1.20000 AFIX 0 C30 1 0.423840 0.612518 0.215287 11.00000 0.02158 0.03695 = 0.01593 0.00550 0.00114 -0.00188 C31 1 0.408105 0.532507 0.246755 11.00000 0.01796 0.03970 = 0.02642 -0.00397 0.00402 -0.00401 AFIX 43 H31 2 0.389055 0.490761 0.222771 11.00000 -1.20000 AFIX 0 C32 1 0.410184 0.629343 0.144637 11.00000 0.03204 0.03657 = 0.02818 0.00411 0.00663 -0.00104 C33 1 0.300838 0.288983 0.217132 11.00000 0.02206 0.03196 = 0.02780 0.01279 0.00463 0.00726 C34 1 0.267223 0.323069 0.167162 11.00000 0.01640 0.03867 = 0.02436 0.00840 0.00547 0.01171 C35 1 0.256967 0.270034 0.108956 11.00000 0.02643 0.05820 = 0.03378 -0.00187 -0.00138 0.02462 AFIX 43 H35 2 0.271638 0.214144 0.098799 11.00000 -1.20000 AFIX 0 C36 1 0.224676 0.299049 0.064666 11.00000 0.03869 0.06035 = 0.02595 -0.01111 -0.00434 0.01260 AFIX 43 H36 2 0.217951 0.263403 0.024627 11.00000 -1.20000 AFIX 0 C37 1 0.202676 0.380556 0.080126 11.00000 0.02501 0.04788 = 0.02288 0.00599 -0.00235 0.01751 AFIX 43 H37 2 0.180803 0.398868 0.050772 11.00000 -1.20000 AFIX 0 C38 1 0.212685 0.435101 0.138427 11.00000 0.01577 0.02713 = 0.02820 0.01097 0.00179 0.00981 C39 1 0.245243 0.405496 0.182801 11.00000 0.01855 0.03522 = 0.02123 0.00511 0.00246 -0.00262 AFIX 43 H39 2 0.252119 0.441181 0.222799 11.00000 -1.20000 AFIX 0 C40 1 0.189079 0.525183 0.155235 11.00000 0.02004 0.03263 = 0.01750 0.00175 0.00145 -0.00163 CL1 3 0.343510 0.507597 0.477765 11.00000 0.08133 0.17480 = 0.10298 0.02256 0.01029 -0.01105 N1 4 0.568753 0.185986 0.540324 11.00000 0.01010 0.04964 = 0.03710 -0.00548 -0.00804 0.00377 N2 4 0.702746 0.291781 0.825504 11.00000 0.01291 0.03134 = 0.02307 -0.00072 -0.00347 0.00178 N3 4 0.396226 0.070373 0.229191 11.00000 0.03026 0.04949 = 0.04168 -0.00683 0.01323 -0.00091 N4 4 0.461662 0.495693 0.532367 11.00000 0.11241 0.09737 = 0.08176 0.00300 0.01109 0.04745 O1 5 0.412917 0.149547 0.379918 11.00000 0.00816 0.05521 = 0.02887 -0.00447 -0.00699 0.00165 O2 5 0.427356 0.213394 0.481912 11.00000 0.01275 0.06264 = 0.03218 -0.01104 -0.00296 0.00739 O3 5 0.843487 0.229828 0.916037 11.00000 0.01885 0.03688 = 0.02126 -0.00477 0.00329 0.00006 O4 5 0.847367 0.256188 1.021997 11.00000 0.02054 0.03831 = 0.01709 0.00077 0.00213 0.00713 O5 5 0.303653 0.318229 0.276239 11.00000 0.02274 0.04783 = 0.01364 -0.00052 -0.00483 0.01496 O6 5 0.324744 0.229803 0.200680 11.00000 0.02519 0.05944 = 0.02297 0.00005 0.00077 0.01851 O7 5 0.157440 0.542928 0.120072 11.00000 0.02033 0.04297 = 0.02514 0.00350 -0.00348 0.01292 O8 5 0.201063 0.582726 0.204528 11.00000 0.01065 0.03672 = 0.03307 0.00171 -0.00414 0.00396 O9 5 0.384333 0.357973 0.312089 11.00000 0.05246 0.03821 = 0.04024 -0.00086 0.01174 -0.01535 O10 5 0.410515 0.421815 0.409237 11.00000 0.04641 0.06435 = 0.02472 0.00289 0.00039 -0.02334 O11 5 0.384519 0.571854 0.111362 11.00000 0.05058 0.05492 = 0.02515 0.00548 -0.00349 -0.01897 O12 5 0.425236 0.702103 0.113675 11.00000 0.03583 0.05535 = 0.02905 0.01075 0.00015 -0.01515 O13 5 0.369450 0.036997 0.254579 11.00000 0.02708 0.04413 = 0.03749 -0.00236 0.01073 -0.00024 O14 5 0.404492 0.165382 0.236124 11.00000 0.03743 0.04679 = 0.05019 0.00343 0.01551 -0.00606 O15 5 0.414183 0.007954 0.203143 11.00000 0.09510 0.08320 = 0.13389 -0.02232 0.08690 0.01043 O16 5 0.467640 0.408608 0.528508 11.00000 0.11242 0.09383 = 0.19040 0.00553 -0.01218 -0.03346 O17 5 0.434245 0.525146 0.539496 11.00000 0.08701 0.13592 = 0.12110 -0.00810 -0.00200 -0.04062 O18 5 0.489143 0.571691 0.538388 11.00000 0.10175 0.18047 = 0.41279 0.01724 0.01007 -0.08772 AFIX 6 O23 5 0.292192 0.494204 0.357278 11.00000 0.09167 0.05392 = 0.09725 0.00360 0.04192 0.01290 H23A 2 0.295380 0.464632 0.321847 11.00000 -1.50000 H23B 2 0.268982 0.503910 0.355734 11.00000 -1.50000 AFIX 0 TB1 6 0.355594 0.194984 0.313584 11.00000 0.01125 0.02833 = 0.01586 0.00087 -0.00193 0.00002 TB2 6 0.396290 0.362677 0.505868 11.00000 0.01828 0.03504 = 0.01805 -0.00212 0.00279 -0.00407 O19 5 0.660585 0.107425 0.417143 11.00000 0.11624 0.29562 = 0.07117 0.05677 -0.01525 -0.09816 O20 5 0.516933 0.408045 0.311427 11.00000 0.21555 0.17524 = 0.87209 0.21842 0.27296 0.04239 AFIX 6 O21 5 0.285097 -0.015721 0.157311 11.00000 0.10899 0.10970 = 0.05234 -0.01626 -0.00905 -0.02629 H21A 2 0.292017 0.001657 0.197621 11.00000 -1.50000 H21B 2 0.304147 -0.034235 0.141932 11.00000 -1.50000 AFIX 6 O22 5 0.382122 0.003827 0.508563 11.00000 0.07932 0.07505 = 0.05472 0.01262 0.00630 -0.00184 H22A 2 0.379020 -0.060413 0.519700 11.00000 -1.50000 H22B 2 0.374583 0.004432 0.466942 11.00000 -1.50000 AFIX 0 O24 5 0.525575 0.882423 0.368288 11.00000 0.29677 0.12147 = 0.26741 0.03497 0.16832 0.07601 HKLF 4 REM 2_a.res in C2/c REM R1 = 0.0584 for 6356 Fo > 4sig(Fo) and 0.0795 for all 8184 data REM 649 parameters refined using 0 restraints END WGHT 0.0831 61.0592 REM Highest difference peak 2.517, deepest hole -2.206, 1-sigma level 0.233 Q1 1 0.6433 0.3456 0.4233 11.00000 0.05 2.52 Q2 1 0.3584 0.1878 0.3589 11.00000 0.05 1.77 Q3 1 0.3996 0.3410 0.5568 11.00000 0.05 1.48 Q4 1 0.3998 0.3758 0.5566 11.00000 0.05 1.45 Q5 1 0.3995 0.3596 0.4597 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60.17 -38 6 10 39.05 55.52 38 -6 -10 57.97 44.37 38 -6 -10 30.14 35.15 38 6 -10 -20.06 46.48 -38 -6 9 404.18 66.89 -38 6 9 427.03 67.49 38 -6 -9 506.39 58.96 38 6 -9 239.14 56.37 -38 -6 8 126.35 57.37 -38 6 8 213.70 60.04 38 -6 -8 275.19 50.62 38 6 -8 135.94 49.76 -38 -6 7 266.29 60.98 -38 6 7 96.12 53.99 38 -6 -7 171.70 47.34 38 6 -7 148.78 49.58 -38 -6 6 11.48 55.01 -38 6 6 15.71 51.34 38 -6 -6 -29.42 42.04 38 6 -6 -8.84 45.21 -38 -6 5 113.30 51.64 -38 6 5 115.66 54.33 38 -6 -5 45.83 44.11 38 6 -5 55.11 45.76 -38 -6 4 94.09 50.41 -38 6 4 9.30 48.14 38 -6 -4 48.26 43.86 38 6 -4 7.56 46.67 -38 -6 3 116.85 51.13 -38 6 3 185.96 57.57 38 -6 -3 75.03 46.17 38 6 -3 72.76 49.99 -38 -6 2 207.10 58.09 -38 6 2 249.91 56.52 38 -6 -2 363.10 61.89 38 6 -2 226.75 55.69 -38 -6 1 5.63 49.21 -38 6 1 46.27 53.44 38 -6 -1 -5.00 45.54 38 6 -1 99.81 53.55 -38 -6 0 -13.53 47.09 -38 6 0 30.17 53.87 38 -6 0 -26.47 44.10 38 6 0 -67.78 50.66 -38 -6 -1 192.51 53.43 -38 6 -1 82.65 52.73 38 -6 1 324.59 63.31 38 6 1 153.12 56.44 -38 -6 -2 -10.99 46.90 -38 6 -2 -26.74 56.37 38 -6 2 -0.66 52.09 -39 -1 14 123.57 58.24 -39 1 14 39.32 56.94 39 -1 -14 27.55 70.45 39 -1 -14 -32.10 44.59 39 1 -14 -31.66 40.81 39 1 -14 22.66 45.82 -39 -1 13 573.95 74.62 -39 1 13 898.28 91.85 39 -1 -13 376.30 57.63 39 -1 -13 312.96 54.11 39 1 -13 390.70 53.94 -39 -1 12 232.78 58.24 -39 1 12 374.46 62.30 39 -1 -12 74.47 42.22 39 1 -12 152.76 46.15 -39 -1 11 -36.72 44.23 -39 1 11 -1.70 47.18 39 -1 -11 5.32 37.56 39 1 -11 44.91 40.67 -39 -1 10 43.07 46.72 -39 1 10 75.91 52.45 39 -1 -10 37.73 37.28 39 1 -10 95.82 42.62 -39 -1 9 36.83 49.68 -39 1 9 -21.31 43.89 39 -1 -9 101.92 41.25 39 1 -9 -17.20 40.54 -39 -1 8 -17.72 46.46 -39 1 8 40.57 45.17 39 -1 -8 52.93 39.69 39 1 -8 3.09 37.95 -39 -1 7 517.74 62.97 -39 1 7 388.45 58.34 39 -1 -7 373.36 53.30 39 1 -7 288.47 52.53 -39 -1 6 850.84 82.86 -39 1 6 974.32 84.61 39 -1 -6 778.24 76.23 39 1 -6 465.30 56.78 -39 -1 5 371.32 56.49 -39 1 5 236.63 51.32 39 -1 -5 286.30 50.48 39 1 -5 181.13 44.44 -39 -1 4 -14.26 43.86 -39 1 4 18.18 40.85 39 -1 -4 11.22 40.68 39 1 -4 71.15 40.32 -39 -1 3 177.30 48.52 -39 1 3 136.35 45.09 39 -1 -3 213.20 46.81 39 1 -3 157.30 44.35 -39 -1 2 148.06 45.89 -39 1 2 -30.26 41.90 39 -1 -2 79.00 40.18 39 1 -2 123.32 43.25 -39 -1 1 159.64 45.27 -39 1 1 141.08 47.06 39 -1 -1 220.37 46.83 39 1 -1 244.01 51.71 -39 -1 0 237.00 47.47 -39 1 0 318.85 52.23 39 -1 0 206.89 48.00 39 1 0 284.47 53.38 -39 -1 -1 179.77 46.63 -39 1 -1 195.22 48.49 39 -1 1 144.72 44.53 39 1 1 250.91 52.15 -39 -1 -2 -27.46 40.75 -39 1 -2 -10.92 43.65 39 -1 2 40.01 43.28 39 1 2 44.87 39.90 -39 -1 -3 5.66 41.86 -39 1 -3 606.50 74.88 39 -1 3 440.77 61.84 39 1 3 433.76 60.76 -39 1 -4 124.08 47.38 39 -1 4 71.27 50.77 39 1 4 169.31 54.27 -39 1 -5 35.39 45.83 39 -1 5 227.69 56.04 39 1 5 123.87 51.80 39 -1 6 221.20 58.18 39 1 6 205.90 58.86 -39 -3 13 -45.69 56.98 -39 3 13 95.67 56.13 39 -3 -13 24.16 86.82 39 3 -13 38.13 45.66 -39 -3 12 602.44 73.41 -39 3 12 497.48 66.27 39 -3 -12 460.48 55.11 39 -3 -12 437.97 66.95 39 3 -12 481.09 60.36 -39 -3 11 143.84 54.95 -39 3 11 96.77 53.22 39 -3 -11 60.38 42.20 39 3 -11 27.13 43.03 -39 -3 10 -1.17 49.96 -39 3 10 22.14 50.34 39 -3 -10 73.41 41.24 39 3 -10 -33.94 43.00 -39 -3 9 19.51 49.34 -39 3 9 73.91 47.75 39 -3 -9 34.08 38.90 39 3 -9 38.56 44.67 -39 -3 8 252.63 56.06 -39 3 8 95.34 45.87 39 -3 -8 112.26 44.49 39 3 -8 -55.60 40.80 -39 -3 7 42.48 47.48 -39 3 7 59.17 43.90 39 -3 -7 51.10 41.72 39 3 -7 1.62 39.65 -39 -3 6 698.51 82.77 -39 3 6 573.47 65.98 39 -3 -6 692.57 67.65 39 3 -6 411.91 57.29 -39 -3 5 79.85 47.10 -39 3 5 278.74 56.53 39 -3 -5 154.53 45.47 39 3 -5 180.19 45.59 -39 -3 4 27.72 44.56 -39 3 4 1.18 43.54 39 -3 -4 -8.26 39.00 39 3 -4 40.53 41.60 -39 -3 3 -54.91 41.78 -39 3 3 69.50 44.70 39 -3 -3 40.95 38.19 39 3 -3 -4.19 41.63 -39 -3 2 351.92 56.23 -39 3 2 230.29 50.53 39 -3 -2 321.76 56.00 39 3 -2 265.18 48.57 -39 -3 1 74.29 43.40 -39 3 1 -59.17 44.10 39 -3 -1 -18.13 40.95 39 3 -1 3.95 40.23 -39 -3 0 894.08 82.09 -39 3 0 727.57 81.76 39 -3 0 915.97 85.15 39 3 0 682.46 77.94 -39 -3 -1 170.05 48.07 -39 3 -1 119.72 47.72 39 -3 1 215.88 51.33 39 3 1 209.42 56.15 -39 -3 -2 90.50 45.20 -39 3 -2 46.63 46.78 39 -3 2 121.06 52.51 39 3 2 64.35 49.17 -39 -3 -3 -20.12 47.67 -39 3 -3 67.86 49.96 39 -3 3 -8.75 45.75 39 3 3 85.85 50.97 -39 3 -4 417.78 61.61 39 -3 4 758.55 90.86 39 3 4 740.76 77.17 -39 3 -5 -24.93 50.31 -39 -5 11 104.79 61.84 -39 5 11 8.56 57.43 39 -5 -11 121.01 45.35 39 -5 -11 88.45 41.72 39 5 -11 23.68 47.54 -39 -5 10 56.07 62.84 -39 5 10 -10.05 54.77 39 -5 -10 52.74 42.15 39 5 -10 86.24 49.47 -39 -5 9 74.18 59.39 -39 5 9 -40.99 49.33 39 -5 -9 95.22 44.70 39 5 -9 -11.63 47.48 -39 -5 8 179.14 60.30 -39 5 8 120.28 57.01 39 -5 -8 224.63 49.26 39 5 -8 102.28 48.70 -39 -5 7 66.94 53.50 -39 5 7 -55.94 50.08 39 -5 -7 81.51 44.80 39 5 -7 -42.65 43.00 -39 -5 6 303.53 61.71 -39 5 6 230.42 59.72 39 -5 -6 159.62 47.93 39 5 -6 102.45 48.53 -39 -5 5 3.24 51.73 -39 5 5 -20.15 52.91 39 -5 -5 39.80 45.19 39 5 -5 -18.74 45.73 -39 -5 4 377.73 62.21 -39 5 4 246.21 58.10 39 -5 -4 455.50 61.32 39 5 -4 286.04 53.86 -39 -5 3 -9.49 48.61 -39 5 3 3.48 50.45 39 -5 -3 77.90 48.44 39 5 -3 75.03 49.77 -39 -5 2 -14.68 49.05 -39 5 2 54.99 48.16 39 -5 -2 21.20 44.01 39 5 -2 14.78 47.96 -39 -5 1 38.56 47.84 -39 5 1 109.15 55.39 39 -5 -1 73.09 50.87 39 5 -1 94.31 52.53 -39 -5 0 70.12 49.58 -39 5 0 57.89 52.92 39 -5 0 149.18 54.76 39 5 0 194.48 53.72 -39 -5 -1 8.06 46.79 -39 5 -1 38.22 53.86 39 -5 1 13.29 48.14 39 5 1 74.85 51.18 -39 -5 -2 481.97 60.56 -39 5 -2 397.82 66.45 39 -5 2 823.89 91.86 39 5 2 506.99 67.52 -40 0 13 5.88 55.38 40 0 -13 26.57 42.19 -40 0 12 132.17 55.05 40 0 -12 148.69 45.63 -40 0 11 51.45 52.49 40 0 -11 3.65 39.45 -40 0 10 524.09 65.12 40 0 -10 288.70 52.30 -40 0 9 62.79 50.11 40 0 -9 30.36 39.61 -40 0 8 48.56 47.86 40 0 -8 -4.05 37.35 -40 0 7 -22.71 46.49 40 0 -7 16.15 41.84 -40 0 6 71.01 45.43 40 0 -6 35.98 39.91 -40 0 5 -59.08 44.86 40 0 -5 -29.44 42.09 -40 0 4 1265.59 89.53 40 0 -4 1342.10 86.04 -40 0 3 -9.14 43.09 40 0 -3 4.13 39.30 -40 0 2 169.93 49.94 40 0 -2 93.17 45.15 -40 0 1 38.48 43.27 40 0 -1 15.76 41.02 -40 0 0 362.04 56.01 40 0 0 417.94 57.64 -40 0 -1 26.70 42.22 40 0 1 -6.96 43.21 -40 0 -2 490.50 59.33 40 0 2 495.45 60.08 -40 0 -3 8.34 44.86 40 0 3 56.63 46.85 -40 0 -4 26.81 45.90 40 0 4 29.50 50.08 -40 -2 13 95.32 63.51 -40 2 13 135.79 64.56 40 -2 -13 49.27 43.51 40 -2 -13 104.12 48.84 40 2 -13 -13.39 42.54 -40 -2 12 336.99 67.65 -40 2 12 191.27 62.89 40 -2 -12 249.31 47.65 40 2 -12 249.16 50.42 -40 -2 11 741.02 78.10 -40 2 11 1132.50 97.39 40 -2 -11 832.39 77.54 40 2 -11 554.25 61.16 -40 -2 10 92.32 55.18 -40 2 10 81.19 52.62 40 -2 -10 158.35 45.22 40 2 -10 117.87 47.32 -40 -2 9 91.47 50.29 -40 2 9 73.59 54.75 40 -2 -9 157.46 47.09 40 2 -9 89.66 47.23 -40 -2 8 55.53 48.88 -40 2 8 107.14 50.89 40 -2 -8 -57.86 37.52 40 2 -8 -44.91 41.15 -40 -2 7 76.01 51.08 -40 2 7 214.23 56.06 40 -2 -7 135.75 45.49 40 2 -7 78.02 44.32 -40 -2 6 53.97 48.70 -40 2 6 154.72 51.59 40 -2 -6 33.42 44.24 40 2 -6 70.06 41.69 -40 -2 5 862.51 87.26 -40 2 5 819.16 86.85 40 -2 -5 767.77 75.56 40 2 -5 668.16 75.53 -40 -2 4 288.44 53.57 -40 2 4 287.87 58.48 40 -2 -4 288.11 52.69 40 2 -4 214.89 48.57 -40 -2 3 4.20 44.73 -40 2 3 56.55 46.61 40 -2 -3 12.27 40.69 40 2 -3 -5.96 40.57 -40 -2 2 220.53 52.95 -40 2 2 42.05 48.63 40 -2 -2 147.43 43.87 40 2 -2 125.35 45.92 -40 -2 1 470.03 63.01 -40 2 1 364.80 55.26 40 -2 -1 466.40 60.10 40 2 -1 301.26 53.72 -40 -2 0 80.26 50.07 -40 2 0 51.78 48.57 40 -2 0 181.03 52.08 40 2 0 253.56 51.86 -40 -2 -1 243.01 55.18 -40 2 -1 213.01 56.51 40 -2 1 212.13 49.90 40 2 1 230.32 53.04 -40 -2 -2 208.79 50.04 -40 2 -2 176.59 52.72 40 -2 2 287.57 60.76 40 2 2 295.84 53.72 -40 -2 -3 -0.90 44.95 -40 2 -3 35.52 48.53 40 -2 3 43.27 49.59 40 2 3 14.93 50.82 -40 -2 -4 -23.91 43.21 -40 2 -4 67.82 53.52 40 -2 4 88.34 51.16 40 2 4 51.58 55.54 -40 -4 11 572.44 81.94 -40 4 11 440.66 70.94 40 -4 -11 502.84 60.55 40 4 -11 444.93 60.38 -40 -4 10 128.39 64.02 -40 4 10 0.85 57.61 40 -4 -10 68.82 44.12 40 4 -10 23.72 44.61 -40 -4 9 -54.12 58.47 -40 4 9 77.56 56.69 40 -4 -9 9.14 42.68 40 4 -9 -12.25 46.13 -40 -4 8 87.40 56.90 -40 4 8 79.06 56.51 40 -4 -8 110.98 47.37 40 4 -8 128.43 49.41 -40 -4 7 22.48 51.93 -40 4 7 -2.33 53.57 40 -4 -7 -15.71 43.06 40 4 -7 -8.90 44.95 -40 -4 6 106.69 52.64 -40 4 6 28.20 53.41 40 -4 -6 -30.57 39.19 40 4 -6 -37.44 46.05 -40 -4 5 260.67 58.51 -40 4 5 298.80 62.39 40 -4 -5 279.50 50.45 40 4 -5 188.52 53.22 -40 -4 4 25.12 50.60 -40 4 4 41.73 50.01 40 -4 -4 46.46 45.00 40 4 -4 25.60 47.52 -40 -4 3 224.26 54.31 -40 4 3 125.22 56.48 40 -4 -3 187.30 48.74 40 4 -3 211.49 52.21 -40 -4 2 20.55 49.62 -40 4 2 6.15 52.55 40 -4 -2 121.45 49.24 40 4 -2 -47.39 44.93 -40 -4 1 123.10 52.36 -40 4 1 250.69 59.43 40 -4 -1 242.05 57.90 40 4 -1 158.95 53.28 -40 -4 0 12.75 46.60 -40 4 0 48.00 53.55 40 -4 0 16.94 50.55 40 4 0 13.94 46.85 -40 -4 -1 151.01 54.17 -40 4 -1 83.94 55.54 40 -4 1 160.19 56.01 40 4 1 159.77 56.23 -40 -4 -2 192.06 52.62 -40 4 -2 115.37 57.76 40 -4 2 57.29 53.86 40 4 2 125.19 51.47 -41 -1 12 65.26 58.59 -41 1 12 -85.05 57.48 41 -1 -12 17.13 43.02 41 1 -12 -22.72 43.42 -41 -1 11 64.28 61.41 -41 1 11 -24.87 56.55 41 -1 -11 15.38 40.54 41 1 -11 16.00 44.93 -41 -1 10 177.70 58.44 -41 1 10 166.90 57.91 41 -1 -10 90.79 43.69 41 1 -10 51.79 44.21 -41 -1 9 797.95 79.42 -41 1 9 719.00 78.56 41 -1 -9 812.64 80.09 41 1 -9 544.34 63.95 -41 -1 8 106.23 52.50 -41 1 8 20.03 52.46 41 -1 -8 69.56 43.26 41 1 -8 59.35 44.65 -41 -1 7 -3.28 51.04 -41 1 7 2.33 52.39 41 -1 -7 19.65 43.45 41 1 -7 -12.98 44.59 -41 -1 6 150.58 51.87 -41 1 6 65.34 51.20 41 -1 -6 101.78 47.03 41 1 -6 16.04 42.77 -41 -1 5 97.47 53.24 -41 1 5 85.11 52.46 41 -1 -5 143.15 46.63 41 1 -5 118.15 47.90 -41 -1 4 8.09 49.21 -41 1 4 167.27 50.89 41 -1 -4 42.39 44.92 41 1 -4 100.12 49.57 -41 -1 3 1316.56 94.83 -41 1 3 1002.73 93.79 41 -1 -3 1217.92 88.17 41 1 -3 973.95 86.43 -41 -1 2 -1.32 46.58 -41 1 2 40.51 46.48 41 -1 -2 13.20 43.79 41 1 -2 56.23 48.65 -41 -1 1 75.16 49.09 -41 1 1 88.40 49.35 41 -1 -1 42.28 45.82 41 1 -1 63.95 45.89 -41 -1 0 -22.46 48.00 -41 1 0 48.92 45.54 41 -1 0 117.42 45.96 41 1 0 -61.57 45.47 -41 -1 -1 559.03 64.94 -41 1 -1 448.77 62.69 41 -1 1 455.49 61.21 41 1 1 358.60 59.00 -41 -1 -2 -9.49 46.48 -41 1 -2 30.86 47.06 41 -1 2 -69.87 48.21 41 1 2 27.88 53.29 -41 -1 -3 130.82 53.99 -41 1 -3 234.79 54.46 41 -1 3 213.76 59.78 41 1 3 212.06 57.57 -41 -3 10 294.14 68.19 -41 3 10 278.15 70.47 41 -3 -10 364.29 57.21 41 3 -10 310.20 57.68 -41 -3 9 -70.92 57.01 -41 3 9 -32.59 53.22 41 -3 -9 -53.02 40.51 41 3 -9 -21.12 48.21 -41 -3 8 158.30 60.92 -41 3 8 28.05 55.20 41 -3 -8 149.55 49.65 41 3 -8 46.92 49.57 -41 -3 7 169.05 62.31 -41 3 7 196.14 61.95 41 -3 -7 160.87 51.79 41 3 -7 105.63 52.18 -41 -3 6 130.53 55.86 -41 3 6 126.34 56.45 41 -3 -6 140.29 45.76 41 3 -6 31.55 48.63 -41 -3 5 219.60 58.05 -41 3 5 150.11 55.25 41 -3 -5 200.20 52.74 41 3 -5 149.02 51.11 -41 -3 4 -67.50 52.17 -41 3 4 17.19 52.13 41 -3 -4 -21.08 42.22 41 3 -4 26.30 43.34 -41 -3 3 131.29 54.00 -41 3 3 78.60 50.06 41 -3 -3 4.92 44.40 41 3 -3 32.17 47.03 -41 -3 2 293.12 59.11 -41 3 2 167.58 57.40 41 -3 -2 394.27 61.99 41 3 -2 271.65 59.60 -41 -3 1 365.58 63.57 -41 3 1 233.72 58.94 41 -3 -1 343.05 62.51 41 3 -1 214.13 59.60 -41 -3 0 422.72 65.03 -41 3 0 277.17 61.85 41 -3 0 393.88 64.61 41 3 0 213.70 57.46 -41 -3 -1 95.30 51.16 -41 3 -1 62.84 53.31 41 -3 1 -24.80 46.61 41 3 1 -67.92 47.39 -42 0 10 261.61 68.83 42 0 -10 210.41 51.73 -42 0 9 38.79 60.43 42 0 -9 35.97 42.44 -42 0 8 631.71 76.79 42 0 -8 728.97 83.68 -42 0 7 57.47 54.89 42 0 -7 8.61 47.40 -42 0 6 -6.19 54.39 42 0 -6 -26.63 45.50 -42 0 5 32.92 50.84 42 0 -5 67.30 46.81 -42 0 4 777.84 95.05 42 0 -4 729.01 85.04 -42 0 3 -10.52 50.43 42 0 -3 -35.55 45.24 -42 0 2 460.47 64.79 42 0 -2 413.82 63.32 -42 0 1 -104.43 50.24 42 0 -1 48.23 49.86 -42 0 0 155.10 54.54 42 0 0 119.64 52.42 -42 0 -1 -5.12 48.02 42 0 1 71.28 51.27 -42 -2 9 64.19 65.03 -42 2 9 -16.29 59.81 42 -2 -9 -14.47 41.97 42 2 -9 -46.47 47.82 -42 -2 8 121.48 61.34 -42 2 8 166.29 64.51 42 -2 -8 75.57 48.22 42 2 -8 95.68 50.14 -42 -2 7 298.30 63.28 -42 2 7 487.50 72.69 42 -2 -7 334.99 58.66 42 2 -7 142.11 50.26 -42 -2 6 174.43 59.08 -42 2 6 250.13 63.74 42 -2 -6 56.77 46.18 42 2 -6 128.70 48.87 -42 -2 5 114.14 56.76 -42 2 5 57.42 54.46 42 -2 -5 66.79 50.89 42 2 -5 56.57 47.75 -42 -2 4 6.88 53.06 -42 2 4 -54.66 52.29 42 -2 -4 -44.14 44.08 42 2 -4 12.49 51.62 -42 -2 3 160.19 58.27 -42 2 3 214.39 61.43 42 -2 -3 190.36 55.97 42 2 -3 101.01 48.81 -42 -2 2 25.61 56.57 -42 2 2 42.02 51.62 42 -2 -2 34.70 46.72 42 2 -2 78.19 50.71 -42 -2 1 463.90 65.85 -42 2 1 480.56 70.65 42 -2 -1 357.34 58.44 42 2 -1 368.98 62.25 -42 -2 0 227.69 55.82 -42 2 0 155.13 57.35 42 -2 0 283.94 61.04 42 2 0 184.87 56.24 -43 -1 7 203.74 64.42 -43 1 7 118.11 60.14 43 -1 -7 234.41 54.35 43 1 -7 188.39 54.83 -43 -1 6 295.23 66.23 -43 1 6 291.36 65.88 43 -1 -6 356.56 60.60 43 1 -6 224.80 57.15 -43 -1 5 538.00 78.09 -43 1 5 618.47 79.72 43 -1 -5 507.98 65.45 43 1 -5 498.81 66.03 -43 -1 4 159.25 61.54 -43 1 4 11.42 56.04 43 -1 -4 44.04 49.70 43 1 -4 -30.64 47.11 -43 -1 3 103.12 58.49 -43 1 3 138.89 56.30 43 -1 -3 180.33 54.70 43 1 -3 180.02 55.22 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 8282 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4353(2) 0.1761(7) 0.4301(4) 0.0224(19) Uani 1 1 d . . . . . C2 C 0.4764(3) 0.1633(8) 0.4284(4) 0.028(2) Uani 1 1 d . . . . . C3 C 0.4871(3) 0.1433(10) 0.3698(5) 0.047(3) Uani 1 1 d . . . . . H3 H 0.468986 0.131216 0.332106 0.056 Uiso 1 1 calc R . . . . C4 C 0.5245(3) 0.1408(12) 0.3658(5) 0.063(4) Uani 1 1 d . . . . . H4 H 0.531369 0.128020 0.325541 0.076 Uiso 1 1 calc R . . . . C5 C 0.5515(3) 0.1570(11) 0.4212(6) 0.062(4) Uani 1 1 d . . . . . H5 H 0.576634 0.158514 0.418472 0.074 Uiso 1 1 calc R . . . . C6 C 0.5031(3) 0.1770(7) 0.4853(5) 0.030(2) Uani 1 1 d . . . . . H6 H 0.496077 0.189973 0.525360 0.036 Uiso 1 1 calc R . . . . C7 C 0.5408(3) 0.1712(8) 0.4816(5) 0.036(2) Uani 1 1 d . . . . . C8 C 0.5957(3) 0.2599(11) 0.5401(5) 0.051(3) Uani 1 1 d . . . . . H8 H 0.595883 0.300056 0.502416 0.062 Uiso 1 1 calc R . . . . C9 C 0.5683(3) 0.1297(8) 0.5949(6) 0.046(3) Uani 1 1 d . . . . . H9 H 0.550047 0.077709 0.593988 0.055 Uiso 1 1 calc R . . . . C10 C 0.5939(3) 0.1458(7) 0.6521(5) 0.038(3) Uani 1 1 d . . . . . H10 H 0.592273 0.107720 0.690033 0.046 Uiso 1 1 calc R . . . . C11 C 0.6228(3) 0.2757(10) 0.5955(5) 0.048(3) Uani 1 1 d . . . . . H11 H 0.641830 0.324812 0.594502 0.058 Uiso 1 1 calc R . . . . C12 C 0.6223(3) 0.2197(7) 0.6528(5) 0.030(2) Uani 1 1 d . . . . . C13 C 0.6507(2) 0.2423(7) 0.7142(4) 0.0251(19) Uani 1 1 d . . . . . C14 C 0.6447(3) 0.2175(7) 0.7756(5) 0.030(2) Uani 1 1 d . . . . . H14 H 0.622785 0.182393 0.779491 0.036 Uiso 1 1 calc R . . . . C15 C 0.6703(2) 0.2433(8) 0.8317(5) 0.028(2) Uani 1 1 d . . . . . H15 H 0.665454 0.227826 0.873118 0.034 Uiso 1 1 calc R . . . . C16 C 0.6848(3) 0.2904(7) 0.7108(4) 0.029(2) Uani 1 1 d . . . . . H16 H 0.690231 0.306478 0.669820 0.035 Uiso 1 1 calc R . . . . C17 C 0.7101(3) 0.3142(8) 0.7662(4) 0.028(2) Uani 1 1 d . . . . . H17 H 0.732700 0.346145 0.763018 0.033 Uiso 1 1 calc R . . . . C18 C 0.7296(2) 0.3232(7) 0.8848(4) 0.0209(18) Uani 1 1 d . . . . . C19 C 0.7180(3) 0.3935(7) 0.9286(4) 0.029(2) Uani 1 1 d . . . . . H19 H 0.693813 0.420923 0.921008 0.035 Uiso 1 1 calc R . . . . C20 C 0.7652(2) 0.2800(6) 0.8936(4) 0.0214(19) Uani 1 1 d . . . . . H20 H 0.771891 0.233459 0.862858 0.026 Uiso 1 1 calc R . . . . C21 C 0.7907(2) 0.3092(7) 0.9507(4) 0.0197(18) Uani 1 1 d . . . . . C22 C 0.7442(3) 0.4206(8) 0.9841(4) 0.029(2) Uani 1 1 d . . . . . H22 H 0.737448 0.467972 1.014309 0.035 Uiso 1 1 calc R . . . . C23 C 0.7800(3) 0.3798(7) 0.9961(4) 0.025(2) Uani 1 1 d . . . . . H23 H 0.797012 0.399066 1.034040 0.030 Uiso 1 1 calc R . . . . C24 C 0.8293(2) 0.2644(7) 0.9643(4) 0.0215(19) Uani 1 1 d . . . . . C25 C 0.4204(2) 0.5133(7) 0.3143(4) 0.026(2) Uani 1 1 d . . . . . C26 C 0.4040(2) 0.4254(7) 0.3476(4) 0.026(2) Uani 1 1 d . . . . . C27 C 0.4488(3) 0.5776(8) 0.3492(4) 0.035(2) Uani 1 1 d . . . . . H27 H 0.457099 0.566191 0.394133 0.042 Uiso 1 1 calc R . . . . C28 C 0.4646(3) 0.6568(8) 0.3187(5) 0.037(2) Uani 1 1 d . . . . . H28 H 0.483568 0.698963 0.342434 0.044 Uiso 1 1 calc R . . . . C29 C 0.4519(3) 0.6738(8) 0.2516(5) 0.033(2) Uani 1 1 d . . . . . H29 H 0.462615 0.727833 0.230777 0.040 Uiso 1 1 calc R . . . . C30 C 0.4238(3) 0.6125(7) 0.2153(4) 0.025(2) Uani 1 1 d . . . . . C31 C 0.4081(2) 0.5325(7) 0.2468(4) 0.028(2) Uani 1 1 d . . . . . H31 H 0.389055 0.490761 0.222771 0.034 Uiso 1 1 calc R . . . . C32 C 0.4102(3) 0.6293(8) 0.1446(5) 0.032(2) Uani 1 1 d . . . . . C33 C 0.3008(3) 0.2890(7) 0.2171(4) 0.027(2) Uani 1 1 d . . . . . C34 C 0.2672(3) 0.3231(7) 0.1672(4) 0.026(2) Uani 1 1 d . . . . . C35 C 0.2570(3) 0.2700(9) 0.1090(5) 0.040(3) Uani 1 1 d . . . . . H35 H 0.271638 0.214144 0.098799 0.049 Uiso 1 1 calc R . . . . C36 C 0.2247(3) 0.2990(9) 0.0647(5) 0.043(3) Uani 1 1 d . . . . . H36 H 0.217951 0.263403 0.024627 0.052 Uiso 1 1 calc R . . . . C37 C 0.2027(3) 0.3806(8) 0.0801(4) 0.033(2) Uani 1 1 d . . . . . H37 H 0.180803 0.398868 0.050772 0.039 Uiso 1 1 calc R . . . . C38 C 0.2127(2) 0.4351(7) 0.1384(4) 0.0241(19) Uani 1 1 d . . . . . C39 C 0.2452(2) 0.4055(7) 0.1828(4) 0.025(2) Uani 1 1 d . . . . . H39 H 0.252119 0.441181 0.222799 0.030 Uiso 1 1 calc R . . . . C40 C 0.1891(2) 0.5252(7) 0.1552(4) 0.0237(19) Uani 1 1 d . . . . . Cl1 Cl 0.34351(14) 0.5076(5) 0.4778(3) 0.1208(18) Uani 1 1 d . . . . . N1 N 0.5688(2) 0.1860(7) 0.5403(4) 0.0340(19) Uani 1 1 d . . . . . N2 N 0.7027(2) 0.2918(6) 0.8255(4) 0.0234(16) Uani 1 1 d . . . . . N3 N 0.3962(2) 0.0704(7) 0.2292(4) 0.040(2) Uani 1 1 d . . . . . N4 N 0.4617(6) 0.4957(15) 0.5324(8) 0.098(6) Uani 1 1 d . . . . . O1 O 0.41292(17) 0.1495(5) 0.3799(3) 0.0322(15) Uani 1 1 d . . . . . O2 O 0.42736(18) 0.2134(6) 0.4819(3) 0.0369(17) Uani 1 1 d . . . . . O3 O 0.84349(17) 0.2298(5) 0.9160(3) 0.0258(14) Uani 1 1 d . . . . . O4 O 0.84737(17) 0.2562(5) 1.0220(3) 0.0255(13) Uani 1 1 d . . . . . O5 O 0.30365(17) 0.3182(5) 0.2762(3) 0.0292(15) Uani 1 1 d . . . . . O6 O 0.32474(18) 0.2298(6) 0.2007(3) 0.0364(17) Uani 1 1 d . . . . . O7 O 0.15744(17) 0.5429(5) 0.1201(3) 0.0306(15) Uani 1 1 d . . . . . O8 O 0.20106(16) 0.5827(5) 0.2045(3) 0.0280(14) Uani 1 1 d . . . . . O9 O 0.3843(2) 0.3580(5) 0.3121(3) 0.0433(18) Uani 1 1 d . . . . . O10 O 0.4105(2) 0.4218(6) 0.4092(3) 0.0461(19) Uani 1 1 d . . . . . O11 O 0.3845(2) 0.5719(6) 0.1114(3) 0.0451(19) Uani 1 1 d . . . . . O12 O 0.4252(2) 0.7021(6) 0.1137(3) 0.0409(18) Uani 1 1 d . . . . . O13 O 0.36945(18) 0.0370(5) 0.2546(3) 0.0356(16) Uani 1 1 d . . . . . O14 O 0.4045(2) 0.1654(6) 0.2361(4) 0.0439(18) Uani 1 1 d . . . . . O15 O 0.4142(3) 0.0080(8) 0.2031(6) 0.095(4) Uani 1 1 d . . . . . O16 O 0.4676(5) 0.4086(12) 0.5285(8) 0.138(6) Uani 1 1 d . . . . . O17 O 0.4342(4) 0.5251(13) 0.5395(7) 0.118(5) Uani 1 1 d . . . . . O18 O 0.4891(5) 0.5717(16) 0.5384(13) 0.237(12) Uani 1 1 d . . . . . O23 O 0.2922(3) 0.4942(8) 0.3573(5) 0.078(3) Uani 1 1 d . . . . . H23A H 0.295380 0.464632 0.321847 0.117 Uiso 1 1 d G . . . . H23B H 0.268982 0.503910 0.355734 0.117 Uiso 1 1 d G . . . . Tb1 Tb 0.35559(2) 0.19498(3) 0.31358(2) 0.01912(14) Uani 1 1 d . . . . . Tb2 Tb 0.39629(2) 0.36268(3) 0.50587(2) 0.02390(15) Uani 1 1 d . . . . . O19 O 0.6606(4) 0.1074(15) 0.4171(6) 0.166(8) Uani 1 1 d . . . . . O20 O 0.5169(7) 0.4080(18) 0.3114(19) 0.40(3) Uani 1 1 d . . . . . O21 O 0.2851(3) -0.0157(11) 0.1573(5) 0.094(4) Uani 1 1 d . . . . . H21A H 0.292017 0.001657 0.197621 0.141 Uiso 1 1 d G . . . . H21B H 0.304147 -0.034235 0.141932 0.141 Uiso 1 1 d G . . . . O22 O 0.3821(3) 0.0038(7) 0.5086(4) 0.071(3) Uani 1 1 d . . . . . H22A H 0.379020 -0.060413 0.519700 0.106 Uiso 1 1 d G . . . . H22B H 0.374583 0.004432 0.466942 0.106 Uiso 1 1 d G . . . . O24 O 0.5256(7) 0.8824(13) 0.3683(10) 0.213(10) 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 C1 0.016(5) 0.026(4) 0.021(5) -0.004(4) -0.006(4) 0.002(4) C2 0.013(5) 0.045(6) 0.027(5) -0.004(4) 0.004(4) 0.003(4) C3 0.021(6) 0.080(8) 0.035(6) -0.016(5) -0.005(5) 0.008(5) C4 0.020(6) 0.143(13) 0.024(6) -0.026(7) -0.001(5) 0.023(7) C5 0.025(6) 0.120(11) 0.040(7) -0.011(7) 0.006(5) 0.012(7) C6 0.018(5) 0.039(5) 0.028(5) -0.007(4) -0.007(4) 0.002(4) C7 0.019(5) 0.055(6) 0.029(5) -0.012(5) -0.007(4) 0.006(5) C8 0.026(6) 0.093(9) 0.032(6) 0.007(6) 0.000(5) -0.009(6) C9 0.029(6) 0.042(6) 0.057(7) 0.003(5) -0.015(5) -0.007(5) C10 0.028(6) 0.033(5) 0.041(6) 0.008(4) -0.019(5) -0.016(4) C11 0.021(6) 0.083(9) 0.035(6) 0.001(6) -0.011(5) -0.010(6) C12 0.015(5) 0.039(5) 0.031(5) -0.001(4) -0.007(4) 0.006(4) C13 0.014(5) 0.025(4) 0.034(5) -0.004(4) -0.002(4) -0.002(4) C14 0.012(5) 0.040(5) 0.035(5) 0.005(4) -0.001(4) 0.000(4) C15 0.014(5) 0.042(5) 0.030(5) 0.000(4) 0.006(4) -0.006(4) C16 0.025(5) 0.038(5) 0.022(5) -0.001(4) 0.002(4) -0.001(4) C17 0.015(5) 0.050(6) 0.019(5) -0.006(4) 0.005(4) -0.014(4) C18 0.007(4) 0.034(5) 0.018(4) -0.002(4) -0.006(3) -0.003(4) C19 0.016(5) 0.041(5) 0.030(5) 0.000(4) 0.005(4) -0.002(4) C20 0.016(5) 0.026(4) 0.022(5) -0.004(3) 0.004(4) 0.003(4) C21 0.009(4) 0.029(4) 0.021(4) 0.004(3) 0.001(3) -0.002(4) C22 0.022(5) 0.048(6) 0.019(4) -0.010(4) 0.008(4) 0.006(4) C23 0.017(5) 0.037(5) 0.022(5) -0.001(4) 0.002(4) 0.002(4) C24 0.019(5) 0.023(4) 0.022(5) 0.003(3) 0.004(4) -0.001(4) C25 0.016(5) 0.038(5) 0.022(5) 0.006(4) -0.001(4) -0.004(4) C26 0.017(5) 0.040(5) 0.023(5) 0.003(4) 0.004(4) 0.003(4) C27 0.034(6) 0.049(6) 0.018(5) -0.004(4) -0.002(4) 0.000(5) C28 0.027(6) 0.049(6) 0.031(6) 0.006(4) -0.003(4) -0.014(5) C29 0.023(5) 0.044(6) 0.034(6) 0.006(4) 0.008(4) -0.012(4) C30 0.022(5) 0.037(5) 0.016(4) 0.005(4) 0.001(4) -0.002(4) C31 0.018(5) 0.040(5) 0.026(5) -0.004(4) 0.004(4) -0.004(4) C32 0.032(6) 0.037(5) 0.028(5) 0.004(4) 0.007(4) -0.001(5) C33 0.022(5) 0.032(5) 0.028(5) 0.013(4) 0.005(4) 0.007(4) C34 0.016(5) 0.039(5) 0.024(5) 0.008(4) 0.005(4) 0.012(4) C35 0.026(6) 0.058(7) 0.034(6) -0.002(5) -0.001(5) 0.025(5) C36 0.039(6) 0.060(7) 0.026(5) -0.011(5) -0.004(5) 0.013(6) C37 0.025(5) 0.048(6) 0.023(5) 0.006(4) -0.002(4) 0.018(5) C38 0.016(5) 0.027(4) 0.028(5) 0.011(4) 0.002(4) 0.010(4) C39 0.019(5) 0.035(5) 0.021(4) 0.005(4) 0.002(4) -0.003(4) C40 0.020(5) 0.033(5) 0.017(4) 0.002(4) 0.001(4) -0.002(4) Cl1 0.081(3) 0.175(5) 0.103(4) 0.023(3) 0.010(3) -0.011(3) N1 0.010(4) 0.050(5) 0.037(5) -0.005(4) -0.008(3) 0.004(4) N2 0.013(4) 0.031(4) 0.023(4) -0.001(3) -0.003(3) 0.002(3) N3 0.030(5) 0.049(5) 0.042(5) -0.007(4) 0.013(4) -0.001(4) N4 0.112(16) 0.097(12) 0.082(10) 0.003(8) 0.011(10) 0.047(12) O1 0.008(3) 0.055(4) 0.029(4) -0.004(3) -0.007(3) 0.002(3) O2 0.013(3) 0.063(5) 0.032(4) -0.011(3) -0.003(3) 0.007(3) O3 0.019(3) 0.037(3) 0.021(3) -0.005(3) 0.003(3) 0.000(3) O4 0.021(3) 0.038(3) 0.017(3) 0.001(3) 0.002(3) 0.007(3) O5 0.023(4) 0.048(4) 0.014(3) -0.001(3) -0.005(3) 0.015(3) O6 0.025(4) 0.059(4) 0.023(3) 0.000(3) 0.001(3) 0.019(3) O7 0.020(3) 0.043(4) 0.025(3) 0.003(3) -0.003(3) 0.013(3) O8 0.011(3) 0.037(3) 0.033(4) 0.002(3) -0.004(3) 0.004(3) O9 0.052(5) 0.038(4) 0.040(4) -0.001(3) 0.012(4) -0.015(4) O10 0.046(5) 0.064(5) 0.025(4) 0.003(3) 0.000(3) -0.023(4) O11 0.051(5) 0.055(4) 0.025(4) 0.005(3) -0.003(3) -0.019(4) O12 0.036(4) 0.055(4) 0.029(4) 0.011(3) 0.000(3) -0.015(4) O13 0.027(4) 0.044(4) 0.037(4) -0.002(3) 0.011(3) 0.000(3) O14 0.037(5) 0.047(4) 0.050(5) 0.003(3) 0.016(4) -0.006(4) O15 0.095(8) 0.083(7) 0.134(10) -0.022(6) 0.087(8) 0.010(6) O16 0.112(12) 0.094(10) 0.190(16) 0.006(10) -0.012(11) -0.033(10) O17 0.087(10) 0.136(12) 0.121(11) -0.008(9) -0.002(9) -0.041(10) O18 0.102(14) 0.180(18) 0.41(4) 0.017(19) 0.010(17) -0.088(14) O23 0.092(8) 0.054(6) 0.097(8) 0.004(5) 0.042(6) 0.013(6) Tb1 0.0112(2) 0.0283(2) 0.0159(2) 0.00087(16) -0.00193(16) 0.00002(17) Tb2 0.0183(3) 0.0350(3) 0.0181(2) -0.00212(17) 0.00279(18) -0.00407(18) O19 0.116(11) 0.30(2) 0.071(8) 0.057(11) -0.015(8) -0.098(13) O20 0.22(3) 0.175(18) 0.87(9) 0.22(3) 0.27(4) 0.042(19) O21 0.109(9) 0.110(9) 0.052(6) -0.016(6) -0.009(6) -0.026(8) O22 0.079(7) 0.075(6) 0.055(6) 0.013(4) 0.006(5) -0.002(6) O24 0.30(3) 0.121(13) 0.27(2) 0.035(13) 0.17(2) 0.076(15) 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C2 116.4(8) . . ? O1 C1 O2 126.3(9) . . ? O2 C1 C2 117.3(7) . . ? C3 C2 C1 119.9(8) . . ? C3 C2 C6 120.0(9) . . ? C6 C2 C1 120.0(8) . . ? C2 C3 H3 119.5 . . ? C2 C3 C4 121.0(10) . . ? C4 C3 H3 119.5 . . ? C3 C4 H4 120.0 . . ? C5 C4 C3 120.0(10) . . ? C5 C4 H4 120.0 . . ? C4 C5 H5 120.4 . . ? C4 C5 C7 119.3(11) . . ? C7 C5 H5 120.4 . . ? C2 C6 H6 120.6 . . ? C2 C6 C7 118.9(9) . . ? C7 C6 H6 120.6 . . ? C5 C7 N1 120.0(10) . . ? C6 C7 C5 120.6(9) . . ? C6 C7 N1 119.3(9) . . ? C11 C8 H8 120.0 . . ? N1 C8 H8 120.0 . . ? N1 C8 C11 120.1(11) . . ? C10 C9 H9 118.8 . . ? N1 C9 H9 118.8 . . ? N1 C9 C10 122.3(10) . . ? C9 C10 H10 120.5 . . ? C9 C10 C12 119.1(10) . . ? C12 C10 H10 120.5 . . ? C8 C11 H11 119.5 . . ? C8 C11 C12 121.0(11) . . ? C12 C11 H11 119.5 . . ? C10 C12 C13 121.6(9) . . ? C11 C12 C10 117.9(9) . . ? C11 C12 C13 120.5(9) . . ? C14 C13 C12 122.3(8) . . ? C14 C13 C16 117.0(8) . . ? C16 C13 C12 120.8(9) . . ? C13 C14 H14 119.2 . . ? C13 C14 C15 121.6(9) . . ? C15 C14 H14 119.2 . . ? C14 C15 H15 120.5 . . ? N2 C15 C14 118.9(8) . . ? N2 C15 H15 120.5 . . ? C13 C16 H16 119.5 . . ? C17 C16 C13 121.1(9) . . ? C17 C16 H16 119.5 . . ? C16 C17 H17 119.9 . . ? N2 C17 C16 120.3(8) . . ? N2 C17 H17 119.9 . . ? C19 C18 N2 118.6(7) . . ? C20 C18 C19 124.1(8) . . ? C20 C18 N2 117.2(8) . . ? C18 C19 H19 121.7 . . ? C22 C19 C18 116.6(8) . . ? C22 C19 H19 121.7 . . ? C18 C20 H20 121.4 . . ? C18 C20 C21 117.2(8) . . ? C21 C20 H20 121.4 . . ? C20 C21 C23 120.3(8) . . ? C20 C21 C24 120.4(8) . . ? C23 C21 C24 119.3(8) . . ? C19 C22 H22 118.9 . . ? C23 C22 C19 122.2(8) . . ? C23 C22 H22 118.9 . . ? C21 C23 H23 120.2 . . ? C22 C23 C21 119.6(8) . . ? C22 C23 H23 120.2 . . ? C21 C24 Tb2 166.4(6) . 8_556 ? O3 C24 C21 119.4(8) . . ? O3 C24 Tb2 66.5(5) . 8_556 ? O4 C24 C21 120.7(8) . . ? O4 C24 O3 119.9(8) . . ? O4 C24 Tb2 54.4(4) . 8_556 ? C27 C25 C26 120.8(8) . . ? C27 C25 C31 118.4(8) . . ? C31 C25 C26 120.8(8) . . ? O9 C26 C25 117.7(8) . . ? O9 C26 O10 123.1(9) . . ? O10 C26 C25 119.2(8) . . ? C25 C27 H27 119.4 . . ? C28 C27 C25 121.2(9) . . ? C28 C27 H27 119.4 . . ? C27 C28 H28 120.4 . . ? C27 C28 C29 119.1(9) . . ? C29 C28 H28 120.4 . . ? C28 C29 H29 119.2 . . ? C30 C29 C28 121.6(8) . . ? C30 C29 H29 119.2 . . ? C29 C30 C31 118.7(8) . . ? C29 C30 C32 122.3(8) . . ? C31 C30 C32 119.0(8) . . ? C25 C31 H31 119.5 . . ? C30 C31 C25 121.0(8) . . ? C30 C31 H31 119.5 . . ? C30 C32 Tb2 168.6(7) . 6_565 ? O11 C32 C30 121.9(8) . . ? O11 C32 O12 118.0(8) . . ? O11 C32 Tb2 60.2(5) . 6_565 ? O12 C32 C30 120.1(9) . . ? O12 C32 Tb2 58.6(5) . 6_565 ? C34 C33 Tb1 169.9(6) . . ? O5 C33 C34 118.9(8) . . ? O5 C33 Tb1 61.3(4) . . ? O6 C33 C34 120.2(8) . . ? O6 C33 O5 120.8(8) . . ? O6 C33 Tb1 60.2(4) . . ? C35 C34 C33 120.9(8) . . ? C35 C34 C39 120.1(8) . . ? C39 C34 C33 118.9(8) . . ? C34 C35 H35 119.9 . . ? C34 C35 C36 120.3(9) . . ? C36 C35 H35 119.9 . . ? C35 C36 H36 120.1 . . ? C37 C36 C35 119.9(9) . . ? C37 C36 H36 120.1 . . ? C36 C37 H37 119.7 . . ? C38 C37 C36 120.6(9) . . ? C38 C37 H37 119.7 . . ? C37 C38 C39 119.2(8) . . ? C37 C38 C40 120.9(8) . . ? C39 C38 C40 119.9(8) . . ? C34 C39 C38 120.0(8) . . ? C34 C39 H39 120.0 . . ? C38 C39 H39 120.0 . . ? C38 C40 Tb1 179.8(7) . 4 ? O7 C40 C38 120.1(8) . . ? O7 C40 Tb1 59.7(5) . 4 ? O8 C40 C38 119.8(8) . . ? O8 C40 O7 120.1(8) . . ? O8 C40 Tb1 60.4(4) . 4 ? C8 N1 C7 118.7(9) . . ? C9 N1 C7 121.6(9) . . ? C9 N1 C8 119.7(9) . . ? C15 N2 C18 119.4(7) . . ? C17 N2 C15 121.2(8) . . ? C17 N2 C18 119.4(7) . . ? O13 N3 Tb1 53.9(4) . . ? O14 N3 O13 117.5(8) . . ? O14 N3 Tb1 63.8(5) . . ? O15 N3 O13 120.0(9) . . ? O15 N3 O14 122.3(9) . . ? O15 N3 Tb1 169.4(8) . . ? O16 N4 O18 122(2) . . ? O16 N4 Tb2 65.6(14) . . ? O17 N4 O16 122(3) . . ? O17 N4 O18 114.9(19) . . ? O17 N4 Tb2 58.6(14) . . ? O18 N4 Tb2 170.2(14) . . ? C1 O1 Tb1 142.8(6) . . ? C1 O2 Tb2 134.2(6) . . ? C24 O3 Tb1 135.6(5) . 8_556 ? C24 O3 Tb2 87.2(5) . 8_556 ? Tb1 O3 Tb2 123.0(2) 8_556 8_556 ? C24 O4 Tb2 100.6(5) . 8_556 ? C33 O5 Tb1 91.8(5) . . ? C33 O6 Tb1 93.4(5) . . ? C40 O7 Tb1 94.1(5) . 4 ? C40 O8 Tb1 93.3(5) . 4 ? C26 O9 Tb1 143.5(6) . . ? C26 O10 Tb2 150.9(6) . . ? C32 O11 Tb2 93.0(6) . 6_565 ? C32 O12 Tb2 94.0(6) . 6_565 ? N3 O13 Tb1 101.2(5) . . ? N3 O14 Tb1 91.6(5) . . ? N4 O16 Tb2 91.5(16) . . ? N4 O17 Tb2 99.1(16) . . ? H23A O23 H23B 109.6 . . ? C33 Tb1 C40 96.8(3) . 4_545 ? C33 Tb1 N3 99.9(3) . . ? C40 Tb1 N3 96.7(2) 4_545 . ? O1 Tb1 C33 162.8(3) . . ? O1 Tb1 C40 99.9(2) . 4_545 ? O1 Tb1 N3 73.9(2) . . ? O1 Tb1 O3 83.0(2) . 8_455 ? O1 Tb1 O5 152.5(2) . . ? O1 Tb1 O6 143.3(2) . . ? O1 Tb1 O7 74.4(2) . 4_545 ? O1 Tb1 O8 125.2(2) . 4_545 ? O1 Tb1 O13 81.1(2) . . ? O1 Tb1 O14 71.9(2) . . ? O3 Tb1 C33 103.4(2) 8_455 . ? O3 Tb1 C40 83.1(2) 8_455 4_545 ? O3 Tb1 N3 156.6(2) 8_455 . ? O3 Tb1 O5 76.61(19) 8_455 . ? O3 Tb1 O7 74.0(2) 8_455 4_545 ? O3 Tb1 O8 93.5(2) 8_455 4_545 ? O3 Tb1 O14 147.1(2) 8_455 . ? O5 Tb1 C33 26.9(2) . . ? O5 Tb1 C40 95.8(2) . 4_545 ? O5 Tb1 N3 126.5(2) . . ? O5 Tb1 O7 116.3(2) . 4_545 ? O5 Tb1 O8 74.9(2) . 4_545 ? O5 Tb1 O14 118.0(2) . . ? O6 Tb1 C33 26.4(2) . . ? O6 Tb1 C40 100.2(2) . 4_545 ? O6 Tb1 N3 73.5(2) . . ? O6 Tb1 O3 129.7(2) . 8_455 ? O6 Tb1 O5 53.1(2) . . ? O6 Tb1 O7 125.2(2) . 4_545 ? O6 Tb1 O8 75.0(2) . 4_545 ? O6 Tb1 O13 76.4(2) . . ? O6 Tb1 O14 71.4(2) . . ? O7 Tb1 C33 122.6(2) 4_545 . ? O7 Tb1 C40 26.3(2) 4_545 4_545 ? O7 Tb1 N3 95.5(2) 4_545 . ? O7 Tb1 O8 52.5(2) 4_545 4_545 ? O7 Tb1 O14 117.3(2) 4_545 . ? O8 Tb1 C33 70.9(2) 4_545 . ? O8 Tb1 C40 26.3(2) 4_545 4_545 ? O8 Tb1 N3 96.5(2) 4_545 . ? O8 Tb1 O14 118.2(2) 4_545 . ? O9 Tb1 C33 83.0(3) . . ? O9 Tb1 C40 162.8(3) . 4_545 ? O9 Tb1 N3 100.2(3) . . ? O9 Tb1 O1 82.3(3) . . ? O9 Tb1 O3 80.2(2) . 8_455 ? O9 Tb1 O5 76.2(3) . . ? O9 Tb1 O6 87.3(3) . . ? O9 Tb1 O7 147.0(2) . 4_545 ? O9 Tb1 O8 151.1(3) . 4_545 ? O9 Tb1 O13 125.1(2) . . ? O9 Tb1 O14 75.7(2) . . ? O13 Tb1 C33 100.1(2) . . ? O13 Tb1 C40 71.9(2) . 4_545 ? O13 Tb1 N3 24.9(2) . . ? O13 Tb1 O3 147.4(2) . 8_455 ? O13 Tb1 O5 125.5(2) . . ? O13 Tb1 O7 74.4(2) . 4_545 ? O13 Tb1 O8 73.2(2) . 4_545 ? O13 Tb1 O14 49.5(2) . . ? O14 Tb1 C33 95.6(3) . . ? O14 Tb1 C40 121.3(2) . 4_545 ? O14 Tb1 N3 24.6(2) . . ? C32 Tb2 C24 107.0(3) 6_566 8_455 ? C32 Tb2 N4 79.1(4) 6_566 . ? Cl1 Tb2 C24 77.1(2) . 8_455 ? Cl1 Tb2 C32 100.2(2) . 6_566 ? Cl1 Tb2 N4 100.7(3) . . ? Cl1 Tb2 O3 75.49(18) . 8_455 ? N4 Tb2 C24 173.8(4) . 8_455 ? O2 Tb2 C24 84.9(2) . 8_455 ? O2 Tb2 C32 104.7(3) . 6_566 ? O2 Tb2 Cl1 152.7(2) . . ? O2 Tb2 N4 95.0(4) . . ? O2 Tb2 O3 79.3(2) . 8_455 ? O2 Tb2 O4 86.4(2) . 8_455 ? O2 Tb2 O11 130.4(2) . 6_566 ? O2 Tb2 O12 77.4(2) . 6_566 ? O2 Tb2 O16 72.6(4) . . ? O2 Tb2 O17 117.2(5) . . ? O3 Tb2 C24 26.3(2) 8_455 8_455 ? O3 Tb2 C32 133.3(2) 8_455 6_566 ? O3 Tb2 N4 147.6(3) 8_455 . ? O4 Tb2 C24 25.0(2) 8_455 8_455 ? O4 Tb2 C32 82.4(2) 8_455 6_566 ? O4 Tb2 Cl1 85.82(19) 8_455 . ? O4 Tb2 N4 161.2(3) 8_455 . ? O4 Tb2 O3 51.08(18) 8_455 8_455 ? O4 Tb2 O11 79.4(2) 8_455 6_566 ? O4 Tb2 O12 82.1(2) 8_455 6_566 ? O4 Tb2 O16 148.6(4) 8_455 . ? O4 Tb2 O17 149.2(4) 8_455 . ? O10 Tb2 C24 104.0(2) . 8_455 ? O10 Tb2 C32 148.6(3) . 6_566 ? O10 Tb2 Cl1 82.3(2) . . ? O10 Tb2 N4 69.8(4) . . ? O10 Tb2 O2 82.4(3) . . ? O10 Tb2 O3 77.8(2) . 8_455 ? O10 Tb2 O4 128.9(2) . 8_455 ? O10 Tb2 O11 141.4(3) . 6_566 ? O10 Tb2 O12 141.7(3) . 6_566 ? O10 Tb2 O16 72.2(4) . . ? O10 Tb2 O17 76.6(4) . . ? O11 Tb2 C24 99.3(3) 6_566 8_455 ? O11 Tb2 C32 26.8(2) 6_566 6_566 ? O11 Tb2 Cl1 73.5(2) 6_566 . ? O11 Tb2 N4 85.5(4) 6_566 . ? O11 Tb2 O3 122.5(2) 6_566 8_455 ? O11 Tb2 O16 96.4(4) 6_566 . ? O11 Tb2 O17 70.3(4) 6_566 . ? O12 Tb2 C24 106.1(2) 6_566 8_455 ? O12 Tb2 C32 27.3(2) 6_566 6_566 ? O12 Tb2 Cl1 127.2(2) 6_566 . ? O12 Tb2 N4 79.9(4) 6_566 . ? O12 Tb2 O3 128.5(2) 6_566 8_455 ? O12 Tb2 O11 53.8(2) 6_566 6_566 ? O12 Tb2 O16 70.8(4) 6_566 . ? O12 Tb2 O17 84.2(4) 6_566 . ? O16 Tb2 C24 157.5(4) . 8_455 ? O16 Tb2 C32 80.7(4) . 6_566 ? O16 Tb2 Cl1 123.2(4) . . ? O16 Tb2 N4 22.9(4) . . ? O16 Tb2 O3 141.0(4) . 8_455 ? O17 Tb2 C24 157.5(4) . 8_455 ? O17 Tb2 C32 73.0(4) . 6_566 ? O17 Tb2 Cl1 80.7(4) . . ? O17 Tb2 N4 22.3(4) . . ? O17 Tb2 O3 147.0(4) . 8_455 ? O17 Tb2 O16 44.7(5) . . ? H21A O21 H21B 109.3 . . ? H22A O22 H22B 104.4 . . ? 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 C1 C2 1.515(12) . ? C1 O1 1.233(10) . ? C1 O2 1.255(11) . ? C2 C3 1.368(14) . ? C2 C6 1.381(13) . ? C3 H3 0.9300 . ? C3 C4 1.383(15) . ? C4 H4 0.9300 . ? C4 C5 1.367(15) . ? C5 H5 0.9300 . ? C5 C7 1.393(15) . ? C6 H6 0.9300 . ? C6 C7 1.393(14) . ? C7 N1 1.433(12) . ? C8 H8 0.9300 . ? C8 C11 1.371(14) . ? C8 N1 1.350(14) . ? C9 H9 0.9300 . ? C9 C10 1.369(14) . ? C9 N1 1.333(14) . ? C10 H10 0.9300 . ? C10 C12 1.388(13) . ? C11 H11 0.9300 . ? C11 C12 1.379(14) . ? C12 C13 1.496(12) . ? C13 C14 1.367(13) . ? C13 C16 1.395(13) . ? C14 H14 0.9300 . ? C14 C15 1.375(13) . ? C15 H15 0.9300 . ? C15 N2 1.358(11) . ? C16 H16 0.9300 . ? C16 C17 1.354(13) . ? C17 H17 0.9300 . ? C17 N2 1.336(11) . ? C18 C19 1.387(12) . ? C18 C20 1.387(12) . ? C18 N2 1.463(11) . ? C19 H19 0.9300 . ? C19 C22 1.382(13) . ? C20 H20 0.9300 . ? C20 C21 1.399(12) . ? C21 C23 1.400(12) . ? C21 C24 1.489(12) . ? C22 H22 0.9300 . ? C22 C23 1.379(12) . ? C23 H23 0.9300 . ? C24 O3 1.287(10) . ? C24 O4 1.248(10) . ? C24 Tb2 2.898(9) 8_556 ? C25 C26 1.485(12) . ? C25 C27 1.394(13) . ? C25 C31 1.401(12) . ? C26 O9 1.249(11) . ? C26 O10 1.251(10) . ? C27 H27 0.9300 . ? C27 C28 1.364(14) . ? C28 H28 0.9300 . ? C28 C29 1.388(13) . ? C29 H29 0.9300 . ? C29 C30 1.376(13) . ? C30 C31 1.380(12) . ? C30 C32 1.463(12) . ? C31 H31 0.9300 . ? C32 O11 1.270(12) . ? C32 O12 1.297(11) . ? C32 Tb2 2.816(9) 6_565 ? C33 C34 1.500(12) . ? C33 O5 1.261(11) . ? C33 O6 1.242(11) . ? C33 Tb1 2.787(9) . ? C34 C35 1.361(14) . ? C34 C39 1.384(12) . ? C35 H35 0.9300 . ? C35 C36 1.389(14) . ? C36 H36 0.9300 . ? C36 C37 1.375(13) . ? C37 H37 0.9300 . ? C37 C38 1.371(13) . ? C38 C39 1.399(12) . ? C38 C40 1.501(12) . ? C39 H39 0.9300 . ? C40 O7 1.255(10) . ? C40 O8 1.254(10) . ? C40 Tb1 2.830(9) 4 ? Cl1 Tb2 2.625(6) . ? N3 O13 1.268(10) . ? N3 O14 1.229(11) . ? N3 O15 1.213(11) . ? N3 Tb1 2.951(8) . ? N4 O16 1.118(18) . ? N4 O17 1.103(19) . ? N4 O18 1.37(2) . ? N4 Tb2 2.87(2) . ? O1 Tb1 2.331(6) . ? O2 Tb2 2.291(7) . ? O3 Tb1 2.439(6) 8_556 ? O3 Tb2 2.661(6) 8_556 ? O4 Tb2 2.397(6) 8_556 ? O5 Tb1 2.446(6) . ? O6 Tb1 2.422(6) . ? O7 Tb1 2.448(6) 4 ? O8 Tb1 2.465(6) 4 ? O9 Tb1 2.297(7) . ? O10 Tb2 2.286(7) . ? O11 Tb2 2.448(7) 6_565 ? O12 Tb2 2.411(7) 6_565 ? O13 Tb1 2.430(7) . ? O14 Tb1 2.650(7) . ? O16 Tb2 2.614(15) . ? O17 Tb2 2.481(13) . ? O23 H23A 0.8497 . ? O23 H23B 0.8492 . ? Tb1 C40 2.830(9) 4_545 ? Tb1 O3 2.439(6) 8_455 ? Tb1 O7 2.449(6) 4_545 ? Tb1 O8 2.465(6) 4_545 ? Tb2 C24 2.898(9) 8_455 ? Tb2 C32 2.816(9) 6_566 ? Tb2 O3 2.661(6) 8_455 ? Tb2 O4 2.397(6) 8_455 ? Tb2 O11 2.448(7) 6_566 ? Tb2 O12 2.411(7) 6_566 ? O21 H21A 0.8503 . ? O21 H21B 0.8517 . ? O22 H22A 0.8505 . ? O22 H22B 0.8503 . ? 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 C1 C2 C3 C4 174.1(11) . . . . ? C1 C2 C6 C7 -176.1(9) . . . . ? C2 C1 O1 Tb1 -143.1(8) . . . . ? C2 C1 O2 Tb2 118.8(8) . . . . ? C2 C3 C4 C5 1(2) . . . . ? C2 C6 C7 C5 3.1(16) . . . . ? C2 C6 C7 N1 179.7(9) . . . . ? C3 C2 C6 C7 0.6(15) . . . . ? C3 C4 C5 C7 3(2) . . . . ? C4 C5 C7 C6 -5(2) . . . . ? C4 C5 C7 N1 178.6(12) . . . . ? C5 C7 N1 C8 50.0(15) . . . . ? C5 C7 N1 C9 -130.9(12) . . . . ? C6 C2 C3 C4 -2.6(18) . . . . ? C6 C7 N1 C8 -126.6(11) . . . . ? C6 C7 N1 C9 52.5(14) . . . . ? C8 C11 C12 C10 1.1(17) . . . . ? C8 C11 C12 C13 -176.3(10) . . . . ? C9 C10 C12 C11 1.6(16) . . . . ? C9 C10 C12 C13 178.9(10) . . . . ? C10 C9 N1 C7 -177.3(10) . . . . ? C10 C9 N1 C8 1.8(17) . . . . ? C10 C12 C13 C14 -19.5(14) . . . . ? C10 C12 C13 C16 160.6(9) . . . . ? C11 C8 N1 C7 -179.9(11) . . . . ? C11 C8 N1 C9 1.0(17) . . . . ? C11 C12 C13 C14 157.7(10) . . . . ? C11 C12 C13 C16 -22.1(14) . . . . ? C12 C13 C14 C15 -176.9(9) . . . . ? C12 C13 C16 C17 177.9(9) . . . . ? C13 C14 C15 N2 -1.9(14) . . . . ? C13 C16 C17 N2 -0.1(14) . . . . ? C14 C13 C16 C17 -2.0(14) . . . . ? C14 C15 N2 C17 -0.2(13) . . . . ? C14 C15 N2 C18 177.7(8) . . . . ? C16 C13 C14 C15 3.0(13) . . . . ? C16 C17 N2 C15 1.2(14) . . . . ? C16 C17 N2 C18 -176.7(8) . . . . ? C18 C19 C22 C23 -0.5(14) . . . . ? C18 C20 C21 C23 -0.3(12) . . . . ? C18 C20 C21 C24 178.8(7) . . . . ? C19 C18 C20 C21 0.5(13) . . . . ? C19 C18 N2 C15 -58.8(11) . . . . ? C19 C18 N2 C17 119.2(10) . . . . ? C19 C22 C23 C21 0.6(14) . . . . ? C20 C18 C19 C22 -0.1(14) . . . . ? C20 C18 N2 C15 121.1(9) . . . . ? C20 C18 N2 C17 -60.9(11) . . . . ? C20 C21 C23 C22 -0.2(13) . . . . ? C20 C21 C24 O3 23.6(12) . . . . ? C20 C21 C24 O4 -153.5(8) . . . . ? C20 C21 C24 Tb2 -89(3) . . . 8_556 ? C21 C24 O3 Tb1 57.0(11) . . . 8_556 ? C21 C24 O3 Tb2 -166.2(7) . . . 8_556 ? C21 C24 O4 Tb2 164.8(6) . . . 8_556 ? C23 C21 C24 O3 -157.2(8) . . . . ? C23 C21 C24 O4 25.7(12) . . . . ? C23 C21 C24 Tb2 90(3) . . . 8_556 ? C24 C21 C23 C22 -179.3(8) . . . . ? C25 C26 O9 Tb1 168.9(8) . . . . ? C25 C26 O10 Tb2 161.0(10) . . . . ? C25 C27 C28 C29 0.3(16) . . . . ? C26 C25 C27 C28 178.5(9) . . . . ? C26 C25 C31 C30 -178.5(8) . . . . ? C27 C25 C26 O9 -166.2(9) . . . . ? C27 C25 C26 O10 13.7(14) . . . . ? C27 C25 C31 C30 0.5(14) . . . . ? C27 C28 C29 C30 -0.1(16) . . . . ? C28 C29 C30 C31 0.0(15) . . . . ? C28 C29 C30 C32 -180.0(9) . . . . ? C29 C30 C31 C25 -0.3(14) . . . . ? C29 C30 C32 O11 179.4(10) . . . . ? C29 C30 C32 O12 1.9(15) . . . . ? C29 C30 C32 Tb2 82(4) . . . 6_565 ? C30 C32 O11 Tb2 -167.0(8) . . . 6_565 ? C30 C32 O12 Tb2 166.9(8) . . . 6_565 ? C31 C25 C26 O9 12.8(13) . . . . ? C31 C25 C26 O10 -167.3(9) . . . . ? C31 C25 C27 C28 -0.6(15) . . . . ? C31 C30 C32 O11 -0.6(14) . . . . ? C31 C30 C32 O12 -178.1(9) . . . . ? C31 C30 C32 Tb2 -98(3) . . . 6_565 ? C32 C30 C31 C25 179.7(9) . . . . ? C33 C34 C35 C36 176.6(10) . . . . ? C33 C34 C39 C38 -176.7(8) . . . . ? C34 C33 O5 Tb1 168.5(7) . . . . ? C34 C33 O6 Tb1 -168.4(7) . . . . ? C34 C35 C36 C37 -1.0(18) . . . . ? C35 C34 C39 C38 -0.7(14) . . . . ? C35 C36 C37 C38 1.3(17) . . . . ? C36 C37 C38 C39 -1.3(15) . . . . ? C36 C37 C38 C40 179.2(9) . . . . ? C37 C38 C39 C34 1.0(13) . . . . ? C37 C38 C40 O7 9.1(13) . . . . ? C37 C38 C40 O8 -170.9(9) . . . . ? C38 C40 O7 Tb1 -179.9(7) . . . 4 ? C38 C40 O8 Tb1 179.9(7) . . . 4 ? C39 C34 C35 C36 0.7(16) . . . . ? C39 C38 C40 O7 -170.5(8) . . . . ? C39 C38 C40 O8 9.6(12) . . . . ? C40 C38 C39 C34 -179.4(8) . . . . ? N1 C8 C11 C12 -2.4(19) . . . . ? N1 C9 C10 C12 -3.0(17) . . . . ? N2 C18 C19 C22 179.8(8) . . . . ? N2 C18 C20 C21 -179.4(7) . . . . ? O1 C1 C2 C3 12.2(14) . . . . ? O1 C1 C2 C6 -171.0(9) . . . . ? O1 C1 O2 Tb2 -60.6(13) . . . . ? O2 C1 C2 C3 -167.2(10) . . . . ? O2 C1 C2 C6 9.5(14) . . . . ? O2 C1 O1 Tb1 36.2(16) . . . . ? O3 C24 O4 Tb2 -12.3(9) . . . 8_556 ? O4 C24 O3 Tb1 -125.9(7) . . . 8_556 ? O4 C24 O3 Tb2 10.9(8) . . . 8_556 ? O5 C33 C34 C35 -160.2(9) . . . . ? O5 C33 C34 C39 15.8(13) . . . . ? O5 C33 O6 Tb1 9.1(9) . . . . ? O6 C33 C34 C35 17.3(14) . . . . ? O6 C33 C34 C39 -166.7(9) . . . . ? O6 C33 O5 Tb1 -9.0(9) . . . . ? O7 C40 O8 Tb1 -0.1(9) . . . 4 ? O8 C40 O7 Tb1 0.1(9) . . . 4 ? O9 C26 O10 Tb2 -19(2) . . . . ? O10 C26 O9 Tb1 -10.9(17) . . . . ? O11 C32 O12 Tb2 -10.7(10) . . . 6_565 ? O12 C32 O11 Tb2 10.6(9) . . . 6_565 ? O13 N3 O14 Tb1 5.0(9) . . . . ? O14 N3 O13 Tb1 -5.6(9) . . . . ? O15 N3 O13 Tb1 169.6(10) . . . . ? O15 N3 O14 Tb1 -170.1(11) . . . . ? O16 N4 O17 Tb2 -18(2) . . . . ? O17 N4 O16 Tb2 16(2) . . . . ? O18 N4 O16 Tb2 -173.5(19) . . . . ? O18 N4 O17 Tb2 171.7(16) . . . . ? Tb1 C33 C34 C35 -72(4) . . . . ? Tb1 C33 C34 C39 104(4) . . . . ? Tb2 C24 O3 Tb1 -136.8(7) 8_556 . . 8_556 ?