#------------------------------------------------------------------------------ #$Date: 2026-06-24 00:19:06 +0100 (Wed, 24 Jun 2026) $ #$Revision: 306629 $ #$URL: svn://www.crystallography.net/cod/cif/7/72/11/7721158.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_7721158 loop_ _publ_author_name 'Trifonov, Alexander A.' 'F\'elix, Gautier' 'Lyubov, Dmitry' 'Kallio, Max' 'Vieru, Veacheslav' 'Zakaria, Hamza' 'Vologzhanina, Anna V.' 'Aysin, Rinat R.' 'Larionova, Joulia' 'Guari, Yannick' _publ_section_title ; Stepwise C−H bond activations and assembly of binuclear Ln3+ species coordinated by hexaanionic anti-\h5:\h5-dibenzopentalene-bridged bis(carbazolyl) framework ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D6DT01110A _journal_year 2026 _chemical_formula_moiety 'C88 H92 N2 O4 Tb2, 4(C7 H8)' _chemical_formula_sum 'C116 H124 N2 O4 Tb2' _chemical_formula_weight 1928.00 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_date 2025-04-11 _audit_creation_method ; Olex2 1.5 (compiled 2025.03.04 svn.red2d20d0 for OlexSys, GUI svn.r7188) ; _audit_update_record ; 2026-02-16 deposited with the CCDC. 2026-06-17 downloaded from the CCDC. ; _cell_angle_alpha 102.15(3) _cell_angle_beta 96.57(3) _cell_angle_gamma 106.22(3) _cell_formula_units_Z 2 _cell_length_a 13.439(3) _cell_length_b 15.940(3) _cell_length_c 23.457(5) _cell_measurement_reflns_used 1084 _cell_measurement_temperature 100 _cell_measurement_theta_max 26.63 _cell_measurement_theta_min 2.41 _cell_volume 4636(2) _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.975 _diffrn_measurement_device_type 'Rayonix CCD' _diffrn_measurement_method 'phi scans' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.7517 _diffrn_reflns_av_R_equivalents 0.0422 _diffrn_reflns_av_unetI/netI 0.0338 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.975 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 97366 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.975 _diffrn_reflns_theta_full 26.809 _diffrn_reflns_theta_max 31.125 _diffrn_reflns_theta_min 1.524 _diffrn_source 'Belok beamline of NRC "Kurchatov Institute"' _exptl_absorpt_coefficient_mu 1.803 _exptl_absorpt_correction_T_max 0.911 _exptl_absorpt_correction_T_min 0.873 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details XDS _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 1.381 _exptl_crystal_description prism _exptl_crystal_F_000 1992 _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: toluene' _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.798 _refine_diff_density_min -1.374 _refine_diff_density_rms 0.100 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 1090 _refine_ls_number_reflns 24618 _refine_ls_number_restraints 21 _refine_ls_restrained_S_all 1.044 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0363 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0446P)^2^+7.6271P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.1018 _reflns_Friedel_coverage 0.000 _reflns_number_gt 18708 _reflns_number_total 24618 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d6dt01110a2.cif _cod_data_source_block at2024-77 _cod_original_cell_volume 4635.9(18) _cod_database_code 7721158 _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. ; _shelx_estimated_absorpt_t_max 0.884 _shelx_estimated_absorpt_t_min 0.813 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C57-C58 \\sim C57-C58A with sigma of 0.02 C57-C59 \\sim C57-C59A with sigma of 0.02 C57-C60 \\sim C57-C60A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C83) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.016 Uanis(C24S) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.002 Uanis(C15) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.005 Uiso(C59A) = Uiso(C59) = Uiso(C60A) = Uiso(C60) = Uiso(C58A) = Uiso(C58) Uanis(C25M) = Uanis(C26S) = Uanis(C91) = Uanis(C31S) = Uanis(C90) = Uanis(C89) = Uanis(C30S) = Uanis(C25S) = Uanis(C29S) = Uanis(C24S) = Uanis(C28S) = Uanis(C27S) = Uanis(C22S) = Uanis(C23S) 4. Others Fixed Sof: C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) C22S(0.5) H22A(0.5) H22B(0.5) H22C(0.5) C23S(0.5) C91(0.5) H91(0.5) C90(0.5) H90(0.5) C89(0.5) H89(0.5) C25S(0.5) H25S(0.5) C24S(0.5) H24S(0.5) C59A(0.5) H59D(0.5) H59E(0.5) H59F(0.5) C60A(0.5) H60D(0.5) H60E(0.5) H60F(0.5) C58A(0.5) H58D(0.5) H58E(0.5) H58F(0.5) C25M(0.5) H25A(0.5) H25B(0.5) H25C(0.5) C26S(0.5) C31S(0.5) H31S(0.5) C30S(0.5) H30S(0.5) C29S(0.5) H29S(0.5) C28S(0.5) H28S(0.5) C27S(0.5) H27S(0.5) 5.a Secondary CH2 refined with riding coordinates: C73(H73A,H73B), C74(H74A,H74B), C75(H75A,H75B), C76(H76A,H76B), C77(H77A, H77B), C78(H78A,H78B), C79(H79A,H79B), C80(H80A,H80B), C81(H81A,H81B), C82(H82A,H82B), C83(H83A,H83B), C84(H84A,H84B), C85(H85A,H85B), C86(H86A,H86B), C87(H87A,H87B), C88(H88A,H88B) 5.b Aromatic/amide H refined with riding coordinates: C3(H3), C5(H5), C8(H8), C10(H10), C25(H25), C26(H26), C27(H27), C28(H28), C31(H31), C32(H32), C33(H33), C34(H34), C39(H39), C40(H40), C41(H41), C42(H42), C47(H47), C49(H49), C52(H52), C54(H54), C69(H69), C70(H70), C71(H71), C72(H72), C10S(H10S), C11S(H11S), C12S(H12S), C13S(H13S), C14S(H14S), C91(H91), C90(H90), C89(H89), C25S(H25S), C24S(H24S), C3S(H3S), C4S(H4S), C5S(H5S), C6S(H6S), C7S(H7S), C17S(H17S), C18S(H18S), C19S(H19S), C20S(H20S), C21S(H21S), C31S(H31S), C30S(H30S), C29S(H29S), C28S(H28S), C27S(H27S) 5.c Fitted hexagon refined as free rotating group: C23S(C91,C90,C89,C25S,C24S), C26S(C31S,C30S,C29S,C28S,C27S) 5.d Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C18(H18A,H18B, H18C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C58(H58A,H58B,H58C), C59(H59A, H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,H62C), C63(H63A,H63B,H63C), C64(H64A,H64B,H64C), C8S(H8SA,H8SB,H8SC), C22S(H22A,H22B,H22C), C1S(H1SA,H1SB, H1SC), C15S(H15D,H15E,H15F), C59A(H59D,H59E,H59F), C60A(H60D,H60E,H60F), C58A(H58D,H58E,H58F), C25M(H25A,H25B,H25C) ; _shelx_res_file ; TITL at2024-77_a.res in P-1 at2024-77.res created by SHELXL-2018/3 at 09:26:08 on 11-Apr-2025 REM Old TITL at2024-77 in P-1 REM SHELXT solution in P-1: R1 0.107, Rweak 0.001, Alpha 0.064 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C92 N21 O5 Tb2 CELL 0.7517 13.439 15.94 23.457 102.146 96.569 106.222 ZERR 2 0.0027 0.0032 0.0047 0.03 0.03 0.03 LATT 1 SFAC C H N O Tb DISP C 0.0027 0.0018 12.9072 DISP H 0 0 0.6262 DISP N 0.0051 0.0037 22.3741 DISP O 0.0094 0.0068 37.473 DISP Tb -0.5874 4.5779 20007.0625 UNIT 232 248 4 8 4 SADI C57 C58 C57 C58A SADI C57 C59 C57 C59A SADI C57 C60 C57 C60A EADP C59A C59 C60A C60 C58A C58 ISOR 0.008 0.016 C83 ISOR 0.002 0.002 C24S EADP C25M C26S C91 C31S C90 C89 C30S C25S C29S C24S C28S C27S C22S C23S ISOR 0.005 0.005 C15 L.S. 4 PLAN 14 SIZE 0.07 0.07 0.12 TEMP -173.15 CONF BOND list 4 MORE -1 BOND $H fmap 2 acta OMIT -6 -12 26 OMIT -5 -15 24 OMIT 7 -7 28 REM REM REM WGHT 0.044600 7.627100 FVAR 0.19674 TB1 5 0.542469 0.629686 0.841058 11.00000 0.01807 0.01719 = 0.01856 0.00457 -0.00092 0.00599 O1 4 0.688448 0.704935 0.801507 11.00000 0.02226 0.02428 = 0.02891 0.00826 0.00303 0.00679 N1 3 0.454753 0.721275 0.808961 11.00000 0.02119 0.01976 = 0.02072 0.00320 0.00053 0.00576 C1 1 0.369880 0.688585 0.761868 11.00000 0.02031 0.02144 = 0.01877 0.00559 0.00201 0.00870 TB2 5 0.447498 0.367379 0.657224 11.00000 0.01926 0.01774 = 0.01861 0.00442 -0.00132 0.00667 O2 4 0.444329 0.635268 0.919369 11.00000 0.02798 0.02813 = 0.02085 0.00775 0.00363 0.01044 N2 3 0.532889 0.275281 0.690687 11.00000 0.02218 0.01849 = 0.02188 0.00430 -0.00042 0.00741 C2 1 0.324105 0.597574 0.731045 11.00000 0.01891 0.02096 = 0.02272 0.00627 0.00010 0.00810 O3 4 0.299618 0.293025 0.695469 11.00000 0.02439 0.02354 = 0.02802 0.00728 0.00172 0.00702 C3 1 0.236570 0.576673 0.686517 11.00000 0.02118 0.02168 = 0.02296 0.00367 -0.00113 0.00839 AFIX 43 H3 2 0.203716 0.515463 0.665022 11.00000 -1.20000 AFIX 0 O4 4 0.551156 0.360649 0.581256 11.00000 0.02798 0.03001 = 0.02320 0.00822 0.00332 0.00983 C4 1 0.194865 0.643560 0.672190 11.00000 0.01925 0.02781 = 0.02351 0.00648 -0.00121 0.01097 C5 1 0.242404 0.733095 0.703620 11.00000 0.02334 0.02491 = 0.02580 0.00737 0.00153 0.01271 AFIX 43 H5 2 0.214901 0.778443 0.694411 11.00000 -1.20000 AFIX 0 C6 1 0.330351 0.757021 0.748674 11.00000 0.02141 0.02107 = 0.02307 0.00629 0.00336 0.00871 C7 1 0.394790 0.839020 0.791256 11.00000 0.02325 0.02122 = 0.02143 0.00706 0.00231 0.00768 C8 1 0.396265 0.929147 0.804724 11.00000 0.02686 0.02256 = 0.02604 0.00748 0.00257 0.01160 AFIX 43 H8 2 0.349631 0.947640 0.780206 11.00000 -1.20000 AFIX 0 C9 1 0.465142 0.991837 0.853528 11.00000 0.03137 0.01959 = 0.02654 0.00595 0.00723 0.01045 C10 1 0.534733 0.963303 0.888874 11.00000 0.02896 0.02053 = 0.02229 0.00411 0.00280 0.00760 AFIX 43 H10 2 0.581607 1.006115 0.922432 11.00000 -1.20000 AFIX 0 C11 1 0.537256 0.874251 0.876318 11.00000 0.02440 0.02195 = 0.02237 0.00636 0.00369 0.00625 C12 1 0.466725 0.812312 0.826684 11.00000 0.02264 0.02174 = 0.02145 0.00741 0.00352 0.00868 C13 1 0.097282 0.620565 0.624170 11.00000 0.02120 0.03114 = 0.02607 0.00318 -0.00305 0.01175 C14 1 0.009602 0.644458 0.651749 11.00000 0.02735 0.10016 = 0.04027 0.00228 0.00076 0.02264 AFIX 137 H14A 2 -0.007250 0.610778 0.681702 11.00000 -1.50000 H14B 2 -0.053035 0.628706 0.620935 11.00000 -1.50000 H14C 2 0.032104 0.709420 0.670534 11.00000 -1.50000 AFIX 0 C15 1 0.056573 0.522455 0.591102 11.00000 0.07010 0.05095 = 0.08105 -0.01243 -0.04392 0.03100 AFIX 137 H15A 2 0.111594 0.505739 0.571724 11.00000 -1.50000 H15B 2 -0.005472 0.512273 0.561046 11.00000 -1.50000 H15C 2 0.037066 0.485414 0.618985 11.00000 -1.50000 AFIX 0 C16 1 0.121934 0.675076 0.578950 11.00000 0.03876 0.12400 = 0.04382 0.04821 -0.01034 -0.00516 AFIX 137 H16A 2 0.144236 0.739659 0.598803 11.00000 -1.50000 H16B 2 0.058795 0.660111 0.548620 11.00000 -1.50000 H16C 2 0.178709 0.660704 0.560188 11.00000 -1.50000 AFIX 0 C17 1 0.466099 1.090321 0.871469 11.00000 0.03620 0.02045 = 0.03012 0.00542 0.00496 0.01145 C18 1 0.395224 1.112543 0.824957 11.00000 0.05315 0.02723 = 0.04606 0.00474 -0.00570 0.01901 AFIX 137 H18A 2 0.419720 1.102592 0.787064 11.00000 -1.50000 H18B 2 0.398011 1.175871 0.838025 11.00000 -1.50000 H18C 2 0.322501 1.073412 0.819963 11.00000 -1.50000 AFIX 0 C19 1 0.429036 1.107889 0.930423 11.00000 0.06151 0.03084 = 0.04409 0.00541 0.01982 0.02285 AFIX 137 H19A 2 0.357709 1.066831 0.926609 11.00000 -1.50000 H19B 2 0.428487 1.170534 0.941635 11.00000 -1.50000 H19C 2 0.477023 1.097625 0.961025 11.00000 -1.50000 AFIX 0 C20 1 0.578087 1.153501 0.877413 11.00000 0.04244 0.02283 = 0.05545 0.01177 0.00640 0.00587 AFIX 137 H20A 2 0.624488 1.146165 0.910126 11.00000 -1.50000 H20B 2 0.577453 1.216206 0.885523 11.00000 -1.50000 H20C 2 0.603991 1.138568 0.840393 11.00000 -1.50000 AFIX 0 C21 1 0.605261 0.840406 0.910275 11.00000 0.02739 0.02003 = 0.02371 0.00261 0.00301 0.00440 C22 1 0.655723 0.801568 0.933627 11.00000 0.02514 0.02537 = 0.01914 0.00275 0.00141 0.00422 C23 1 0.712281 0.747745 0.957276 11.00000 0.02363 0.02825 = 0.02539 0.00918 0.00222 0.00836 C24 1 0.684318 0.655966 0.925065 11.00000 0.02342 0.02420 = 0.02645 0.00797 0.00171 0.00706 C25 1 0.741774 0.606410 0.948472 11.00000 0.02437 0.02688 = 0.02483 0.00841 0.00223 0.00613 AFIX 43 H25 2 0.726920 0.544534 0.928843 11.00000 -1.20000 AFIX 0 C26 1 0.820026 0.643448 0.999354 11.00000 0.02434 0.03483 = 0.02826 0.01172 0.00013 0.01183 AFIX 43 H26 2 0.857645 0.607017 1.013109 11.00000 -1.20000 AFIX 0 C27 1 0.843191 0.733141 1.029958 11.00000 0.02475 0.03600 = 0.02671 0.00775 -0.00174 0.00843 AFIX 43 H27 2 0.895466 0.757909 1.065036 11.00000 -1.20000 AFIX 0 C28 1 0.789516 0.786181 1.008954 11.00000 0.02830 0.02912 = 0.02482 0.00450 0.00073 0.00703 AFIX 43 H28 2 0.804762 0.847821 1.029260 11.00000 -1.20000 AFIX 0 C29 1 0.376155 0.533438 0.748238 11.00000 0.02035 0.01917 = 0.01864 0.00244 -0.00167 0.00692 C30 1 0.357268 0.486596 0.793206 11.00000 0.01908 0.01894 = 0.02227 0.00281 -0.00208 0.00347 C31 1 0.273418 0.471619 0.825124 11.00000 0.02278 0.02707 = 0.02514 0.00537 0.00354 0.00578 AFIX 43 H31 2 0.216668 0.494625 0.817284 11.00000 -1.20000 AFIX 0 C32 1 0.274223 0.423896 0.867339 11.00000 0.02529 0.03470 = 0.02532 0.00881 0.00581 0.00316 AFIX 43 H32 2 0.217101 0.413711 0.888118 11.00000 -1.20000 AFIX 0 C33 1 0.358194 0.389236 0.880870 11.00000 0.03270 0.02894 = 0.02632 0.01356 0.00331 0.00422 AFIX 43 H33 2 0.356949 0.357147 0.910765 11.00000 -1.20000 AFIX 0 C34 1 0.441107 0.401828 0.851014 11.00000 0.02904 0.02324 = 0.02355 0.00891 -0.00004 0.00659 AFIX 43 H34 2 0.497233 0.378696 0.860152 11.00000 -1.20000 AFIX 0 C35 1 0.442143 0.449735 0.806375 11.00000 0.02198 0.01743 = 0.02144 0.00531 0.00089 0.00538 C36 1 0.514268 0.472147 0.767163 11.00000 0.02125 0.01749 = 0.02311 0.00471 0.00027 0.00818 C37 1 0.611837 0.463341 0.750810 11.00000 0.01951 0.01899 = 0.01990 0.00284 -0.00225 0.00616 C38 1 0.630636 0.511192 0.706085 11.00000 0.01975 0.01947 = 0.02240 0.00459 -0.00031 0.00480 C39 1 0.714590 0.527198 0.674378 11.00000 0.02115 0.02854 = 0.02835 0.00701 0.00242 0.00650 AFIX 43 H39 2 0.772107 0.505141 0.682350 11.00000 -1.20000 AFIX 0 C40 1 0.712495 0.574731 0.632069 11.00000 0.02530 0.03381 = 0.02867 0.01042 0.00625 0.00299 AFIX 43 H40 2 0.769668 0.585694 0.611376 11.00000 -1.20000 AFIX 0 C41 1 0.627706 0.608027 0.618233 11.00000 0.03145 0.02943 = 0.02845 0.01372 0.00343 0.00461 AFIX 43 H41 2 0.628364 0.639844 0.588209 11.00000 -1.20000 AFIX 0 C42 1 0.544900 0.594592 0.647888 11.00000 0.02750 0.02259 = 0.02739 0.00840 -0.00116 0.00682 AFIX 43 H42 2 0.488055 0.616810 0.638551 11.00000 -1.20000 AFIX 0 C43 1 0.544924 0.547275 0.692574 11.00000 0.02189 0.01935 = 0.02079 0.00606 0.00151 0.00654 C44 1 0.472595 0.523671 0.731703 11.00000 0.02084 0.01668 = 0.02044 0.00305 -0.00091 0.00657 C45 1 0.619151 0.308683 0.737114 11.00000 0.02044 0.02194 = 0.01908 0.00436 0.00112 0.00825 C46 1 0.665157 0.399925 0.767482 11.00000 0.02041 0.02092 = 0.02106 0.00400 -0.00044 0.00814 C47 1 0.755741 0.421752 0.809635 11.00000 0.01942 0.02233 = 0.02357 0.00521 0.00047 0.00789 AFIX 43 H47 2 0.788571 0.483074 0.830906 11.00000 -1.20000 AFIX 0 C48 1 0.801179 0.355516 0.822116 11.00000 0.01800 0.02642 = 0.02488 0.00641 -0.00094 0.00940 C49 1 0.752572 0.265538 0.791534 11.00000 0.02232 0.02232 = 0.02830 0.00821 0.00114 0.01088 AFIX 43 H49 2 0.781658 0.220533 0.799774 11.00000 -1.20000 AFIX 0 C50 1 0.661050 0.240953 0.748694 11.00000 0.02181 0.02067 = 0.02138 0.00510 0.00202 0.00952 C51 1 0.596142 0.158554 0.706187 11.00000 0.02120 0.02209 = 0.02276 0.00612 0.00254 0.00845 C52 1 0.595818 0.068860 0.691786 11.00000 0.02717 0.02326 = 0.02596 0.00787 0.00354 0.01183 AFIX 43 H52 2 0.644253 0.050552 0.715208 11.00000 -1.20000 AFIX 0 C53 1 0.525029 0.006059 0.643351 11.00000 0.03000 0.01942 = 0.02787 0.00518 0.00576 0.00882 C54 1 0.454349 0.034538 0.608872 11.00000 0.02677 0.02190 = 0.02445 0.00525 0.00369 0.00667 AFIX 43 H54 2 0.407261 -0.008026 0.575288 11.00000 -1.20000 AFIX 0 C55 1 0.451113 0.123329 0.622381 11.00000 0.02432 0.02182 = 0.02148 0.00421 0.00205 0.00803 C56 1 0.522154 0.184959 0.672104 11.00000 0.02237 0.01956 = 0.02020 0.00531 0.00300 0.00743 C57 1 0.900945 0.382930 0.869508 11.00000 0.02000 0.03044 = 0.03143 0.00322 -0.00448 0.01114 PART 1 C58 1 0.877318 0.408233 0.929430 10.50000 0.04282 AFIX 137 H58A 2 0.846631 0.457620 0.932051 10.50000 -1.50000 H58B 2 0.942520 0.427944 0.958893 10.50000 -1.50000 H58C 2 0.827100 0.355952 0.937171 10.50000 -1.50000 AFIX 0 PART 2 C59 1 0.966568 0.480523 0.882536 10.50000 0.04282 AFIX 137 H59A 2 0.984978 0.494803 0.845688 10.50000 -1.50000 H59B 2 1.031171 0.491345 0.910833 10.50000 -1.50000 H59C 2 0.926305 0.518998 0.899575 10.50000 -1.50000 AFIX 0 PART 1 C60 1 0.955138 0.310535 0.863881 10.50000 0.04282 AFIX 137 H60A 2 0.916084 0.261206 0.879420 10.50000 -1.50000 H60B 2 1.027319 0.336593 0.886564 10.50000 -1.50000 H60C 2 0.956976 0.287095 0.822027 10.50000 -1.50000 AFIX 0 PART 0 C61 1 0.523482 -0.092326 0.624764 11.00000 0.03831 0.02164 = 0.03479 0.00304 0.00184 0.01121 C62 1 0.593259 -0.115428 0.671053 11.00000 0.08646 0.02852 = 0.06216 0.00193 -0.02155 0.03112 AFIX 137 H62A 2 0.666799 -0.078969 0.674733 11.00000 -1.50000 H62B 2 0.586948 -0.179667 0.658790 11.00000 -1.50000 H62C 2 0.570904 -0.102506 0.709404 11.00000 -1.50000 AFIX 0 C63 1 0.560383 -0.109368 0.565648 11.00000 0.06383 0.03098 = 0.05000 0.00553 0.02082 0.02376 AFIX 137 H63A 2 0.513128 -0.097640 0.535411 11.00000 -1.50000 H63B 2 0.559543 -0.172333 0.553759 11.00000 -1.50000 H63C 2 0.632238 -0.069105 0.569711 11.00000 -1.50000 AFIX 0 C64 1 0.411456 -0.155125 0.618773 11.00000 0.05441 0.02315 = 0.07291 0.01567 0.01604 0.00697 AFIX 137 H64A 2 0.386497 -0.141541 0.656256 11.00000 -1.50000 H64B 2 0.411369 -0.218032 0.609234 11.00000 -1.50000 H64C 2 0.364714 -0.146047 0.586990 11.00000 -1.50000 AFIX 0 C65 1 0.383157 0.157573 0.588195 11.00000 0.02704 0.02047 = 0.02486 0.00015 0.00270 0.00601 C66 1 0.333559 0.195466 0.563979 11.00000 0.02712 0.02627 = 0.02157 0.00261 0.00153 0.00557 C67 1 0.279426 0.250005 0.539236 11.00000 0.02557 0.02864 = 0.02464 0.00799 0.00189 0.00972 C68 1 0.309496 0.342342 0.571308 11.00000 0.02516 0.02793 = 0.02674 0.00881 0.00343 0.00844 C69 1 0.255415 0.393188 0.547099 11.00000 0.02544 0.02688 = 0.02434 0.00699 0.00217 0.00650 AFIX 43 H69 2 0.272140 0.455409 0.566413 11.00000 -1.20000 AFIX 0 C70 1 0.177785 0.357417 0.495846 11.00000 0.02509 0.03686 = 0.02518 0.01284 0.00125 0.01186 AFIX 43 H70 2 0.142372 0.394933 0.481599 11.00000 -1.20000 AFIX 0 C71 1 0.152257 0.267274 0.465692 11.00000 0.02847 0.03916 = 0.02446 0.00701 -0.00231 0.01074 AFIX 43 H71 2 0.100274 0.243134 0.430476 11.00000 -1.20000 AFIX 0 C72 1 0.203088 0.212722 0.487291 11.00000 0.03163 0.03111 = 0.02400 0.00305 -0.00225 0.01150 AFIX 43 H72 2 0.186377 0.150848 0.467130 11.00000 -1.20000 AFIX 0 C73 1 0.686185 0.777847 0.773565 11.00000 0.03005 0.02861 = 0.03647 0.01536 0.00675 0.00776 AFIX 23 H73A 2 0.689696 0.832998 0.803603 11.00000 -1.20000 H73B 2 0.620663 0.760266 0.743816 11.00000 -1.20000 AFIX 0 C74 1 0.780958 0.794203 0.744296 11.00000 0.03730 0.03161 = 0.04251 0.01419 0.01507 0.00856 AFIX 23 H74A 2 0.811304 0.859264 0.746571 11.00000 -1.20000 H74B 2 0.761999 0.760013 0.702081 11.00000 -1.20000 AFIX 0 C75 1 0.858102 0.761519 0.778434 11.00000 0.03103 0.05408 = 0.05079 0.02216 0.01363 0.01304 AFIX 23 H75A 2 0.888259 0.723606 0.750862 11.00000 -1.20000 H75B 2 0.916405 0.813374 0.804080 11.00000 -1.20000 AFIX 0 C76 1 0.797237 0.707366 0.815351 11.00000 0.02047 0.04581 = 0.04723 0.02159 0.00470 0.00867 AFIX 23 H76A 2 0.802261 0.645323 0.806045 11.00000 -1.20000 H76B 2 0.825898 0.735751 0.858055 11.00000 -1.20000 AFIX 0 C77 1 0.468001 0.617580 0.976534 11.00000 0.03697 0.03783 = 0.02349 0.01188 0.00285 0.01389 AFIX 23 H77A 2 0.524413 0.669614 1.003449 11.00000 -1.20000 H77B 2 0.491290 0.563247 0.972232 11.00000 -1.20000 AFIX 0 C78 1 0.366706 0.602769 1.000397 11.00000 0.04390 0.04393 = 0.02918 0.01499 0.00991 0.01318 AFIX 23 H78A 2 0.381035 0.630215 1.043669 11.00000 -1.20000 H78B 2 0.328875 0.537429 0.992755 11.00000 -1.20000 AFIX 0 C79 1 0.302143 0.648331 0.967570 11.00000 0.03702 0.05007 = 0.04150 0.01708 0.01617 0.01851 AFIX 23 H79A 2 0.233143 0.604559 0.946447 11.00000 -1.20000 H79B 2 0.289778 0.698676 0.995545 11.00000 -1.20000 AFIX 0 C80 1 0.366966 0.683199 0.924076 11.00000 0.03111 0.03629 = 0.03280 0.01346 0.00977 0.01655 AFIX 23 H80A 2 0.321707 0.670933 0.884969 11.00000 -1.20000 H80B 2 0.402356 0.749129 0.938718 11.00000 -1.20000 AFIX 0 C81 1 0.300701 0.222177 0.725760 11.00000 0.03334 0.02715 = 0.03306 0.01284 0.00706 0.00804 AFIX 23 H81A 2 0.362197 0.243166 0.758613 11.00000 -1.20000 H81B 2 0.304480 0.167687 0.697782 11.00000 -1.20000 AFIX 0 C82 1 0.198700 0.201392 0.749575 11.00000 0.04282 0.03073 = 0.04011 0.01043 0.01534 0.00799 AFIX 23 H82A 2 0.167087 0.135511 0.743921 11.00000 -1.20000 H82B 2 0.210919 0.231666 0.792332 11.00000 -1.20000 AFIX 0 C83 1 0.129226 0.237548 0.714023 11.00000 0.04088 0.07901 = 0.10442 0.05866 0.02983 0.02644 AFIX 23 H83A 2 0.071223 0.187060 0.686929 11.00000 -1.20000 H83B 2 0.097909 0.275586 0.740722 11.00000 -1.20000 AFIX 0 C84 1 0.191639 0.290743 0.680083 11.00000 0.02169 0.07580 = 0.05739 0.03824 0.00654 0.01274 AFIX 23 H84A 2 0.165247 0.263311 0.637087 11.00000 -1.20000 H84B 2 0.186773 0.352835 0.689461 11.00000 -1.20000 AFIX 0 C85 1 0.531291 0.378747 0.523728 11.00000 0.04092 0.03436 = 0.02442 0.00922 0.00273 0.01334 AFIX 23 H85A 2 0.507379 0.432690 0.527218 11.00000 -1.20000 H85B 2 0.476543 0.326539 0.495863 11.00000 -1.20000 AFIX 0 C86 1 0.635017 0.394830 0.502435 11.00000 0.05183 0.04127 = 0.03047 0.01247 0.01420 0.01340 AFIX 23 H86A 2 0.672212 0.460350 0.510463 11.00000 -1.20000 H86B 2 0.623811 0.367498 0.459279 11.00000 -1.20000 AFIX 0 C87 1 0.697987 0.350200 0.536946 11.00000 0.04024 0.05937 = 0.04580 0.02531 0.02018 0.02101 AFIX 23 H87A 2 0.712748 0.300364 0.509794 11.00000 -1.20000 H87B 2 0.765812 0.394602 0.559249 11.00000 -1.20000 AFIX 0 C88 1 0.630179 0.314338 0.578983 11.00000 0.03377 0.03965 = 0.03356 0.01412 0.01201 0.01878 AFIX 23 H88A 2 0.596322 0.248226 0.564184 11.00000 -1.20000 H88B 2 0.673120 0.327296 0.618882 11.00000 -1.20000 AFIX 0 C8S 1 0.087189 0.685018 0.825688 11.00000 0.06925 0.09308 = 0.04996 0.01326 0.01169 0.04188 AFIX 137 H8SA 2 0.088139 0.718682 0.795171 11.00000 -1.50000 H8SB 2 0.014936 0.647006 0.823611 11.00000 -1.50000 H8SC 2 0.132785 0.646843 0.819026 11.00000 -1.50000 AFIX 0 C9S 1 0.126418 0.749904 0.885587 11.00000 0.04778 0.05328 = 0.04297 0.02335 0.01325 0.03119 C10S 1 0.225723 0.815856 0.898948 11.00000 0.04416 0.06769 = 0.06180 0.04275 0.02727 0.03134 AFIX 43 H10S 2 0.267705 0.820392 0.869103 11.00000 -1.20000 AFIX 0 C11S 1 0.263331 0.873871 0.954238 11.00000 0.04080 0.05025 = 0.07490 0.02243 0.01592 0.01555 AFIX 43 H11S 2 0.331628 0.916985 0.962749 11.00000 -1.20000 AFIX 0 C12S 1 0.202659 0.869780 0.997184 11.00000 0.04711 0.05721 = 0.06414 0.00593 0.01138 0.02098 AFIX 43 H12S 2 0.228571 0.910305 1.035434 11.00000 -1.20000 AFIX 0 C13S 1 0.103792 0.806749 0.984908 11.00000 0.04154 0.06325 = 0.04888 0.01613 0.01686 0.02296 AFIX 43 H13S 2 0.061749 0.804424 1.014809 11.00000 -1.20000 AFIX 0 C14S 1 0.065401 0.747261 0.929904 11.00000 0.03720 0.05036 = 0.04788 0.02315 0.01349 0.01534 AFIX 43 H14S 2 -0.002855 0.704221 0.922024 11.00000 -1.20000 AFIX 0 PART 1 C22S 1 0.021199 1.021847 0.563519 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 137 H22A 2 -0.000163 0.973635 0.526676 10.50000 -1.50000 H22B 2 0.078402 1.072541 0.559142 10.50000 -1.50000 H22C 2 -0.039092 1.042358 0.571993 10.50000 -1.50000 AFIX 66 C23S 1 0.058834 0.986454 0.613929 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 C91 1 -0.010422 0.954877 0.649977 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H91 2 -0.082133 0.952524 0.641506 10.50000 -1.20000 AFIX 65 C90 1 0.025244 0.926742 0.698421 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H90 2 -0.022090 0.905160 0.723058 10.50000 -1.20000 AFIX 65 C89 1 0.130167 0.930184 0.710816 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H89 2 0.154543 0.910955 0.743926 10.50000 -1.20000 AFIX 65 C25S 1 0.199425 0.961761 0.674768 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H25S 2 0.271136 0.964114 0.683240 10.50000 -1.20000 AFIX 65 C24S 1 0.163760 0.989897 0.626324 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H24S 2 0.211095 1.011479 0.601687 10.50000 -1.20000 AFIX 0 PART 0 C1S 1 0.933074 0.349875 0.677419 11.00000 0.07977 0.09454 = 0.05232 0.00632 0.01576 0.04721 AFIX 137 H1SA 2 0.899169 0.395955 0.673614 11.00000 -1.50000 H1SB 2 1.009422 0.375698 0.680759 11.00000 -1.50000 H1SC 2 0.918257 0.329225 0.712972 11.00000 -1.50000 AFIX 0 C2S 1 0.890735 0.271320 0.623640 11.00000 0.04453 0.05680 = 0.04850 0.02653 0.01668 0.02918 C3S 1 0.796136 0.206602 0.620128 11.00000 0.05540 0.06827 = 0.07147 0.04215 0.03686 0.03367 AFIX 43 H3S 2 0.759797 0.211541 0.652501 11.00000 -1.20000 AFIX 0 C4S 1 0.753355 0.135873 0.571620 11.00000 0.03911 0.05641 = 0.11060 0.03959 0.03066 0.01628 AFIX 43 H4S 2 0.687589 0.092520 0.570236 11.00000 -1.20000 AFIX 0 C5S 1 0.805497 0.126891 0.524183 11.00000 0.04574 0.05036 = 0.07647 0.00790 -0.00107 0.01408 AFIX 43 H5S 2 0.775502 0.077794 0.490041 11.00000 -1.20000 AFIX 0 C6S 1 0.901284 0.189789 0.526922 11.00000 0.04228 0.05386 = 0.04839 0.01851 0.01601 0.02106 AFIX 43 H6S 2 0.937948 0.184013 0.494736 11.00000 -1.20000 AFIX 0 C7S 1 0.943543 0.260796 0.576291 11.00000 0.03310 0.04652 = 0.04734 0.01973 0.01364 0.01431 AFIX 43 H7S 2 1.010032 0.303505 0.578151 11.00000 -1.20000 AFIX 0 C15S 1 -0.204442 1.042635 0.828874 11.00000 0.05610 0.04279 = 0.08406 0.01144 0.00381 0.01745 AFIX 137 H15D 2 -0.216030 1.092151 0.857202 11.00000 -1.50000 H15E 2 -0.266934 0.989147 0.819864 11.00000 -1.50000 H15F 2 -0.191671 1.060792 0.792284 11.00000 -1.50000 AFIX 0 C16S 1 -0.112338 1.021325 0.854824 11.00000 0.05846 0.03382 = 0.06443 -0.00486 -0.00596 0.01586 C17S 1 -0.015485 1.051108 0.834247 11.00000 0.04861 0.05603 = 0.07409 -0.00544 0.01747 0.00779 AFIX 43 H17S 2 -0.009632 1.086766 0.806303 11.00000 -1.20000 AFIX 0 C18S 1 0.068314 1.026999 0.855779 11.00000 0.06203 0.07159 = 0.06957 0.00742 0.00663 0.01352 AFIX 43 H18S 2 0.132546 1.044853 0.841710 11.00000 -1.20000 AFIX 0 C19S 1 0.061544 0.976337 0.898309 11.00000 0.06922 0.05859 = 0.09848 -0.00960 -0.02691 0.02963 AFIX 43 H19S 2 0.120181 0.959344 0.912513 11.00000 -1.20000 AFIX 0 C20S 1 -0.030906 0.951798 0.918997 11.00000 0.06436 0.05821 = 0.07649 0.01813 -0.00504 0.02095 AFIX 43 H20S 2 -0.035628 0.920561 0.949395 11.00000 -1.20000 AFIX 0 C21S 1 -0.118223 0.972968 0.895141 11.00000 0.06254 0.04063 = 0.06017 0.00563 0.00588 0.01394 AFIX 43 H21S 2 -0.183293 0.952476 0.907904 11.00000 -1.20000 AFIX 0 PART 1 C59A 1 0.982578 0.467688 0.858150 10.50000 0.04282 AFIX 137 H59D 2 0.994242 0.453369 0.817226 10.50000 -1.50000 H59E 2 1.049494 0.483473 0.885638 10.50000 -1.50000 H59F 2 0.954696 0.518861 0.864532 10.50000 -1.50000 AFIX 0 PART 2 C60A 1 0.971714 0.326639 0.852453 10.50000 0.04282 AFIX 137 H60D 2 0.934926 0.263166 0.849949 10.50000 -1.50000 H60E 2 1.036315 0.347805 0.882493 10.50000 -1.50000 H60F 2 0.989808 0.332431 0.813855 10.50000 -1.50000 AFIX 0 C58A 1 0.865931 0.368615 0.927167 10.50000 0.04282 AFIX 137 H58D 2 0.808802 0.394488 0.933718 10.50000 -1.50000 H58E 2 0.925603 0.398367 0.960247 10.50000 -1.50000 H58F 2 0.840852 0.303775 0.924647 10.50000 -1.50000 AFIX 0 C25M 1 -0.122504 0.989236 0.654175 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 137 H25A 2 -0.174052 0.928825 0.645283 10.50000 -1.50000 H25B 2 -0.140349 1.020851 0.624848 10.50000 -1.50000 H25C 2 -0.123709 1.023383 0.693917 10.50000 -1.50000 AFIX 66 C26S 1 -0.024361 0.981798 0.652061 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 C31S 1 0.021214 0.939087 0.688609 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H31S 2 -0.016753 0.912996 0.715660 10.50000 -1.20000 AFIX 65 C30S 1 0.122339 0.934550 0.685578 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H30S 2 0.153486 0.905358 0.710557 10.50000 -1.20000 AFIX 65 C29S 1 0.177890 0.972724 0.645998 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H29S 2 0.247004 0.969623 0.643926 10.50000 -1.20000 AFIX 65 C28S 1 0.132316 1.015436 0.609449 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H28S 2 0.170284 1.041526 0.582398 10.50000 -1.20000 AFIX 65 C27S 1 0.031191 1.019974 0.612480 10.50000 0.05311 0.05393 = 0.05404 0.00726 0.01220 0.01041 AFIX 43 H27S 2 0.000044 1.049165 0.587501 10.50000 -1.20000 AFIX 0 HKLF 4 REM at2024-77_a.res in P-1 REM wR2 = 0.1018, GooF = S = 1.038, Restrained GooF = 1.044 for all data REM R1 = 0.0363 for 18708 Fo > 4sig(Fo) and 0.0523 for all 24618 data REM 1090 parameters refined using 21 restraints END WGHT 0.0428 7.0937 REM Highest difference peak 1.798, deepest hole -1.374, 1-sigma level 0.100 Q1 1 -0.1330 1.0662 0.7908 11.00000 0.05 1.45 Q2 1 0.8792 0.3074 0.9145 11.00000 0.05 1.27 Q3 1 -0.1772 1.0019 0.8708 11.00000 0.05 1.27 Q4 1 0.9051 0.4628 0.9271 11.00000 0.05 1.06 Q5 1 -0.0580 1.0127 0.8859 11.00000 0.05 1.06 Q6 1 -0.0361 1.0789 0.8003 11.00000 0.05 0.87 Q7 1 -0.0652 1.0254 0.6045 11.00000 0.05 0.83 Q8 1 0.9935 0.3761 0.8471 11.00000 0.05 0.81 Q9 1 0.1017 0.9755 0.6471 11.00000 0.05 0.80 Q10 1 0.2917 0.3767 0.5602 11.00000 0.05 0.69 Q11 1 0.0944 0.5389 0.5709 11.00000 0.05 0.67 Q12 1 0.5777 0.7060 0.8334 11.00000 0.05 0.66 Q13 1 0.0961 1.0291 0.5980 11.00000 0.05 0.66 Q14 1 0.5883 0.6362 0.8411 11.00000 0.05 0.62 ; _shelx_res_checksum 60383 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.54247(2) 0.62969(2) 0.84106(2) 0.01820(4) Uani 1 1 d . . . . . O1 O 0.68845(15) 0.70493(14) 0.80151(10) 0.0252(4) Uani 1 1 d . . . . . N1 N 0.45475(17) 0.72128(16) 0.80896(11) 0.0213(5) Uani 1 1 d . . . . . C1 C 0.3699(2) 0.68859(18) 0.76187(12) 0.0198(5) Uani 1 1 d . . . . . Tb2 Tb 0.44750(2) 0.36738(2) 0.65722(2) 0.01879(4) Uani 1 1 d . . . . . O2 O 0.44433(16) 0.63527(14) 0.91937(9) 0.0251(4) Uani 1 1 d . . . . . N2 N 0.53289(17) 0.27528(15) 0.69069(11) 0.0211(5) Uani 1 1 d . . . . . C2 C 0.3241(2) 0.59757(18) 0.73104(13) 0.0207(5) Uani 1 1 d . . . . . O3 O 0.29962(15) 0.29303(14) 0.69547(10) 0.0256(4) Uani 1 1 d . . . . . C3 C 0.2366(2) 0.57667(19) 0.68652(13) 0.0223(5) Uani 1 1 d . . . . . H3 H 0.203716 0.515463 0.665022 0.027 Uiso 1 1 calc R U . . . O4 O 0.55116(16) 0.36065(15) 0.58126(9) 0.0268(4) Uani 1 1 d . . . . . C4 C 0.1949(2) 0.6436(2) 0.67219(13) 0.0232(6) Uani 1 1 d . . . . . C5 C 0.2424(2) 0.7331(2) 0.70362(13) 0.0237(6) Uani 1 1 d . . . . . H5 H 0.214901 0.778443 0.694411 0.028 Uiso 1 1 calc R U . . . C6 C 0.3304(2) 0.75702(19) 0.74867(13) 0.0214(5) Uani 1 1 d . . . . . C7 C 0.3948(2) 0.83902(19) 0.79126(13) 0.0217(5) Uani 1 1 d . . . . . C8 C 0.3963(2) 0.92915(19) 0.80472(13) 0.0243(6) Uani 1 1 d . . . . . H8 H 0.349631 0.947640 0.780206 0.029 Uiso 1 1 calc R U . . . C9 C 0.4651(2) 0.99184(19) 0.85353(14) 0.0251(6) Uani 1 1 d . . . . . C10 C 0.5347(2) 0.96330(19) 0.88887(13) 0.0243(6) Uani 1 1 d . . . . . H10 H 0.581607 1.006115 0.922432 0.029 Uiso 1 1 calc R U . . . C11 C 0.5373(2) 0.87425(19) 0.87632(13) 0.0231(6) Uani 1 1 d . . . . . C12 C 0.4667(2) 0.81231(19) 0.82668(13) 0.0213(5) Uani 1 1 d . . . . . C13 C 0.0973(2) 0.6206(2) 0.62417(14) 0.0266(6) Uani 1 1 d . . . . . C14 C 0.0096(3) 0.6445(4) 0.65175(19) 0.0583(13) Uani 1 1 d . . . . . H14A H -0.007250 0.610778 0.681702 0.087 Uiso 1 1 calc R U . . . H14B H -0.053035 0.628706 0.620935 0.087 Uiso 1 1 calc R U . . . H14C H 0.032104 0.709420 0.670534 0.087 Uiso 1 1 calc R U . . . C15 C 0.0566(4) 0.5225(3) 0.5911(2) 0.0743(16) Uani 1 1 d . U . . . H15A H 0.111594 0.505739 0.571724 0.111 Uiso 1 1 calc R U . . . H15B H -0.005472 0.512273 0.561046 0.111 Uiso 1 1 calc R U . . . H15C H 0.037066 0.485414 0.618985 0.111 Uiso 1 1 calc R U . . . C16 C 0.1219(3) 0.6751(4) 0.5789(2) 0.0726(17) Uani 1 1 d . . . . . H16A H 0.144236 0.739659 0.598803 0.109 Uiso 1 1 calc R U . . . H16B H 0.058795 0.660111 0.548620 0.109 Uiso 1 1 calc R U . . . H16C H 0.178709 0.660704 0.560188 0.109 Uiso 1 1 calc R U . . . C17 C 0.4661(2) 1.0903(2) 0.87147(15) 0.0286(6) Uani 1 1 d . . . . . C18 C 0.3952(3) 1.1125(2) 0.82496(18) 0.0427(9) Uani 1 1 d . . . . . H18A H 0.419720 1.102592 0.787064 0.064 Uiso 1 1 calc R U . . . H18B H 0.398011 1.175871 0.838025 0.064 Uiso 1 1 calc R U . . . H18C H 0.322501 1.073412 0.819963 0.064 Uiso 1 1 calc R U . . . C19 C 0.4290(3) 1.1079(3) 0.93042(18) 0.0435(9) Uani 1 1 d . . . . . H19A H 0.357709 1.066831 0.926609 0.065 Uiso 1 1 calc R U . . . H19B H 0.428487 1.170534 0.941635 0.065 Uiso 1 1 calc R U . . . H19C H 0.477023 1.097625 0.961025 0.065 Uiso 1 1 calc R U . . . C20 C 0.5781(3) 1.1535(2) 0.87741(19) 0.0411(8) Uani 1 1 d . . . . . H20A H 0.624488 1.146165 0.910126 0.062 Uiso 1 1 calc R U . . . H20B H 0.577453 1.216206 0.885523 0.062 Uiso 1 1 calc R U . . . H20C H 0.603991 1.138568 0.840393 0.062 Uiso 1 1 calc R U . . . C21 C 0.6053(2) 0.84041(19) 0.91028(13) 0.0250(6) Uani 1 1 d . . . . . C22 C 0.6557(2) 0.8016(2) 0.93363(13) 0.0247(6) Uani 1 1 d . . . . . C23 C 0.7123(2) 0.7477(2) 0.95728(14) 0.0255(6) Uani 1 1 d . . . . . C24 C 0.6843(2) 0.6560(2) 0.92506(14) 0.0248(6) Uani 1 1 d . . . . . C25 C 0.7418(2) 0.6064(2) 0.94847(14) 0.0257(6) Uani 1 1 d . . . . . H25 H 0.726920 0.544534 0.928843 0.031 Uiso 1 1 calc R U . . . C26 C 0.8200(2) 0.6434(2) 0.99935(14) 0.0284(6) Uani 1 1 d . . . . . H26 H 0.857645 0.607017 1.013109 0.034 Uiso 1 1 calc R U . . . C27 C 0.8432(2) 0.7331(2) 1.02996(14) 0.0300(6) Uani 1 1 d . . . . . H27 H 0.895466 0.757909 1.065036 0.036 Uiso 1 1 calc R U . . . C28 C 0.7895(2) 0.7862(2) 1.00895(14) 0.0285(6) Uani 1 1 d . . . . . H28 H 0.804762 0.847821 1.029260 0.034 Uiso 1 1 calc R U . . . C29 C 0.3762(2) 0.53344(18) 0.74824(12) 0.0200(5) Uani 1 1 d . . . . . C30 C 0.3573(2) 0.48660(18) 0.79321(13) 0.0215(5) Uani 1 1 d . . . . . C31 C 0.2734(2) 0.4716(2) 0.82512(13) 0.0257(6) Uani 1 1 d . . . . . H31 H 0.216668 0.494625 0.817284 0.031 Uiso 1 1 calc R U . . . C32 C 0.2742(2) 0.4239(2) 0.86734(14) 0.0295(6) Uani 1 1 d . . . . . H32 H 0.217101 0.413711 0.888118 0.035 Uiso 1 1 calc R U . . . C33 C 0.3582(2) 0.3892(2) 0.88087(14) 0.0296(6) Uani 1 1 d . . . . . H33 H 0.356949 0.357147 0.910765 0.036 Uiso 1 1 calc R U . . . C34 C 0.4411(2) 0.4018(2) 0.85101(13) 0.0256(6) Uani 1 1 d . . . . . H34 H 0.497233 0.378696 0.860152 0.031 Uiso 1 1 calc R U . . . C35 C 0.4421(2) 0.44974(18) 0.80637(12) 0.0207(5) Uani 1 1 d . . . . . C36 C 0.5143(2) 0.47215(18) 0.76716(13) 0.0206(5) Uani 1 1 d . . . . . C37 C 0.6118(2) 0.46334(18) 0.75081(12) 0.0203(5) Uani 1 1 d . . . . . C38 C 0.6306(2) 0.51119(18) 0.70608(13) 0.0213(5) Uani 1 1 d . . . . . C39 C 0.7146(2) 0.5272(2) 0.67438(14) 0.0265(6) Uani 1 1 d . . . . . H39 H 0.772107 0.505141 0.682350 0.032 Uiso 1 1 calc R U . . . C40 C 0.7125(2) 0.5747(2) 0.63207(15) 0.0301(6) Uani 1 1 d . . . . . H40 H 0.769668 0.585694 0.611376 0.036 Uiso 1 1 calc R U . . . C41 C 0.6277(2) 0.6080(2) 0.61823(15) 0.0300(6) Uani 1 1 d . . . . . H41 H 0.628364 0.639844 0.588209 0.036 Uiso 1 1 calc R U . . . C42 C 0.5449(2) 0.5946(2) 0.64789(14) 0.0262(6) Uani 1 1 d . . . . . H42 H 0.488055 0.616810 0.638551 0.031 Uiso 1 1 calc R U . . . C43 C 0.5449(2) 0.54727(18) 0.69257(12) 0.0207(5) Uani 1 1 d . . . . . C44 C 0.4726(2) 0.52367(18) 0.73170(12) 0.0198(5) Uani 1 1 d . . . . . C45 C 0.6192(2) 0.30868(19) 0.73711(12) 0.0205(5) Uani 1 1 d . . . . . C46 C 0.6652(2) 0.39992(19) 0.76748(12) 0.0210(5) Uani 1 1 d . . . . . C47 C 0.7557(2) 0.42175(19) 0.80963(13) 0.0219(5) Uani 1 1 d . . . . . H47 H 0.788571 0.483074 0.830906 0.026 Uiso 1 1 calc R U . . . C48 C 0.8012(2) 0.3555(2) 0.82212(13) 0.0230(6) Uani 1 1 d . . . . . C49 C 0.7526(2) 0.26554(19) 0.79153(13) 0.0235(6) Uani 1 1 d . . . . . H49 H 0.781658 0.220533 0.799774 0.028 Uiso 1 1 calc R U . . . C50 C 0.6611(2) 0.24095(19) 0.74869(13) 0.0209(5) Uani 1 1 d . . . . . C51 C 0.5961(2) 0.15855(19) 0.70619(13) 0.0217(5) Uani 1 1 d . . . . . C52 C 0.5958(2) 0.06886(19) 0.69179(13) 0.0245(6) Uani 1 1 d . . . . . H52 H 0.644253 0.050552 0.715208 0.029 Uiso 1 1 calc R U . . . C53 C 0.5250(2) 0.00606(19) 0.64335(14) 0.0256(6) Uani 1 1 d . . . . . C54 C 0.4543(2) 0.03454(19) 0.60887(13) 0.0248(6) Uani 1 1 d . . . . . H54 H 0.407261 -0.008026 0.575288 0.030 Uiso 1 1 calc R U . . . C55 C 0.4511(2) 0.12333(19) 0.62238(13) 0.0227(5) Uani 1 1 d . . . . . C56 C 0.5222(2) 0.18496(18) 0.67210(12) 0.0206(5) Uani 1 1 d . . . . . C57 C 0.9009(2) 0.3829(2) 0.86951(14) 0.0281(6) Uani 1 1 d D . . . . C58 C 0.8773(6) 0.4082(6) 0.9294(3) 0.0428(7) Uiso 0.5 1 d D . P A 1 H58A H 0.846631 0.457620 0.932051 0.064 Uiso 0.5 1 calc R U P A 1 H58B H 0.942520 0.427944 0.958893 0.064 Uiso 0.5 1 calc R U P A 1 H58C H 0.827100 0.355952 0.937171 0.064 Uiso 0.5 1 calc R U P A 1 C59 C 0.9666(6) 0.4805(5) 0.8825(4) 0.0428(7) Uiso 0.5 1 d D . P A 2 H59A H 0.984978 0.494803 0.845688 0.064 Uiso 0.5 1 calc R U P A 2 H59B H 1.031171 0.491345 0.910833 0.064 Uiso 0.5 1 calc R U P A 2 H59C H 0.926305 0.518998 0.899575 0.064 Uiso 0.5 1 calc R U P A 2 C60 C 0.9551(7) 0.3105(6) 0.8639(4) 0.0428(7) Uiso 0.5 1 d D . P A 1 H60A H 0.916084 0.261206 0.879420 0.064 Uiso 0.5 1 calc R U P A 1 H60B H 1.027319 0.336593 0.886564 0.064 Uiso 0.5 1 calc R U P A 1 H60C H 0.956976 0.287095 0.822027 0.064 Uiso 0.5 1 calc R U P A 1 C61 C 0.5235(3) -0.0923(2) 0.62476(16) 0.0322(7) Uani 1 1 d . . . . . C62 C 0.5933(4) -0.1154(3) 0.6711(2) 0.0607(14) Uani 1 1 d . . . . . H62A H 0.666799 -0.078969 0.674733 0.091 Uiso 1 1 calc R U . . . H62B H 0.586948 -0.179667 0.658790 0.091 Uiso 1 1 calc R U . . . H62C H 0.570904 -0.102506 0.709404 0.091 Uiso 1 1 calc R U . . . C63 C 0.5604(3) -0.1094(3) 0.56565(19) 0.0462(9) Uani 1 1 d . . . . . H63A H 0.513128 -0.097640 0.535411 0.069 Uiso 1 1 calc R U . . . H63B H 0.559543 -0.172333 0.553759 0.069 Uiso 1 1 calc R U . . . H63C H 0.632238 -0.069105 0.569711 0.069 Uiso 1 1 calc R U . . . C64 C 0.4115(3) -0.1551(2) 0.6188(2) 0.0503(10) Uani 1 1 d . . . . . H64A H 0.386497 -0.141541 0.656256 0.076 Uiso 1 1 calc R U . . . H64B H 0.411369 -0.218032 0.609234 0.076 Uiso 1 1 calc R U . . . H64C H 0.364714 -0.146047 0.586990 0.076 Uiso 1 1 calc R U . . . C65 C 0.3832(2) 0.15757(19) 0.58819(14) 0.0255(6) Uani 1 1 d . . . . . C66 C 0.3336(2) 0.1955(2) 0.56398(13) 0.0264(6) Uani 1 1 d . . . . . C67 C 0.2794(2) 0.2500(2) 0.53924(14) 0.0261(6) Uani 1 1 d . . . . . C68 C 0.3095(2) 0.3423(2) 0.57131(14) 0.0264(6) Uani 1 1 d . . . . . C69 C 0.2554(2) 0.3932(2) 0.54710(14) 0.0260(6) Uani 1 1 d . . . . . H69 H 0.272140 0.455409 0.566413 0.031 Uiso 1 1 calc R U . . . C70 C 0.1778(2) 0.3574(2) 0.49585(14) 0.0281(6) Uani 1 1 d . . . . . H70 H 0.142372 0.394933 0.481599 0.034 Uiso 1 1 calc R U . . . C71 C 0.1523(2) 0.2673(2) 0.46569(14) 0.0314(7) Uani 1 1 d . . . . . H71 H 0.100274 0.243134 0.430476 0.038 Uiso 1 1 calc R U . . . C72 C 0.2031(2) 0.2127(2) 0.48729(14) 0.0298(6) Uani 1 1 d . . . . . H72 H 0.186377 0.150848 0.467130 0.036 Uiso 1 1 calc R U . . . C73 C 0.6862(2) 0.7778(2) 0.77356(15) 0.0308(7) Uani 1 1 d . . . . . H73A H 0.689696 0.832998 0.803603 0.037 Uiso 1 1 calc R U . . . H73B H 0.620663 0.760266 0.743816 0.037 Uiso 1 1 calc R U . . . C74 C 0.7810(3) 0.7942(2) 0.74430(17) 0.0362(7) Uani 1 1 d . . . . . H74A H 0.811304 0.859264 0.746571 0.043 Uiso 1 1 calc R U . . . H74B H 0.761999 0.760013 0.702081 0.043 Uiso 1 1 calc R U . . . C75 C 0.8581(3) 0.7615(3) 0.77843(19) 0.0435(9) Uani 1 1 d . . . . . H75A H 0.888259 0.723606 0.750862 0.052 Uiso 1 1 calc R U . . . H75B H 0.916405 0.813374 0.804080 0.052 Uiso 1 1 calc R U . . . C76 C 0.7972(2) 0.7074(3) 0.81535(17) 0.0368(8) Uani 1 1 d . . . . . H76A H 0.802261 0.645323 0.806045 0.044 Uiso 1 1 calc R U . . . H76B H 0.825898 0.735751 0.858055 0.044 Uiso 1 1 calc R U . . . C77 C 0.4680(3) 0.6176(2) 0.97653(14) 0.0319(7) Uani 1 1 d . . . . . H77A H 0.524413 0.669614 1.003449 0.038 Uiso 1 1 calc R U . . . H77B H 0.491290 0.563247 0.972232 0.038 Uiso 1 1 calc R U . . . C78 C 0.3667(3) 0.6028(3) 1.00040(16) 0.0380(8) Uani 1 1 d . . . . . H78A H 0.381035 0.630215 1.043669 0.046 Uiso 1 1 calc R U . . . H78B H 0.328875 0.537429 0.992755 0.046 Uiso 1 1 calc R U . . . C79 C 0.3021(3) 0.6483(3) 0.96757(18) 0.0402(8) Uani 1 1 d . . . . . H79A H 0.233143 0.604559 0.946447 0.048 Uiso 1 1 calc R U . . . H79B H 0.289778 0.698676 0.995545 0.048 Uiso 1 1 calc R U . . . C80 C 0.3670(2) 0.6832(2) 0.92408(15) 0.0311(7) Uani 1 1 d . . . . . H80A H 0.321707 0.670933 0.884969 0.037 Uiso 1 1 calc R U . . . H80B H 0.402356 0.749129 0.938718 0.037 Uiso 1 1 calc R U . . . C81 C 0.3007(2) 0.2222(2) 0.72576(15) 0.0306(6) Uani 1 1 d . . . . . H81A H 0.362197 0.243166 0.758613 0.037 Uiso 1 1 calc R U . . . H81B H 0.304480 0.167687 0.697782 0.037 Uiso 1 1 calc R U . . . C82 C 0.1987(3) 0.2014(2) 0.74958(17) 0.0378(8) Uani 1 1 d . . . . . H82A H 0.167087 0.135511 0.743921 0.045 Uiso 1 1 calc R U . . . H82B H 0.210919 0.231666 0.792332 0.045 Uiso 1 1 calc R U . . . C83 C 0.1292(3) 0.2375(4) 0.7140(3) 0.0662(14) Uani 1 1 d . U . . . H83A H 0.071223 0.187060 0.686929 0.079 Uiso 1 1 calc R U . . . H83B H 0.097909 0.275586 0.740722 0.079 Uiso 1 1 calc R U . . . C84 C 0.1916(3) 0.2907(3) 0.6801(2) 0.0489(10) Uani 1 1 d . . . . . H84A H 0.165247 0.263311 0.637087 0.059 Uiso 1 1 calc R U . . . H84B H 0.186773 0.352835 0.689461 0.059 Uiso 1 1 calc R U . . . C85 C 0.5313(3) 0.3787(2) 0.52373(14) 0.0329(7) Uani 1 1 d . . . . . H85A H 0.507379 0.432690 0.527218 0.039 Uiso 1 1 calc R U . . . H85B H 0.476543 0.326539 0.495863 0.039 Uiso 1 1 calc R U . . . C86 C 0.6350(3) 0.3948(3) 0.50243(17) 0.0403(8) Uani 1 1 d . . . . . H86A H 0.672212 0.460350 0.510463 0.048 Uiso 1 1 calc R U . . . H86B H 0.623811 0.367498 0.459279 0.048 Uiso 1 1 calc R U . . . C87 C 0.6980(3) 0.3502(3) 0.53695(19) 0.0444(9) Uani 1 1 d . . . . . H87A H 0.712748 0.300364 0.509794 0.053 Uiso 1 1 calc R U . . . H87B H 0.765812 0.394602 0.559249 0.053 Uiso 1 1 calc R U . . . C88 C 0.6302(3) 0.3143(2) 0.57898(16) 0.0329(7) Uani 1 1 d . . . . . H88A H 0.596322 0.248226 0.564184 0.039 Uiso 1 1 calc R U . . . H88B H 0.673120 0.327296 0.618882 0.039 Uiso 1 1 calc R U . . . C8S C 0.0872(4) 0.6850(4) 0.8257(2) 0.0680(14) Uani 1 1 d . . . . . H8SA H 0.088139 0.718682 0.795171 0.102 Uiso 1 1 calc R U . . . H8SB H 0.014936 0.647006 0.823611 0.102 Uiso 1 1 calc R U . . . H8SC H 0.132785 0.646843 0.819026 0.102 Uiso 1 1 calc R U . . . C9S C 0.1264(3) 0.7499(3) 0.88559(18) 0.0426(9) Uani 1 1 d . . . . . C10S C 0.2257(3) 0.8159(3) 0.8989(2) 0.0493(11) Uani 1 1 d . . . . . H10S H 0.267705 0.820392 0.869103 0.059 Uiso 1 1 calc R U . . . C11S C 0.2633(3) 0.8739(3) 0.9542(2) 0.0536(11) Uani 1 1 d . . . . . H11S H 0.331628 0.916985 0.962749 0.064 Uiso 1 1 calc R U . . . C12S C 0.2027(3) 0.8698(3) 0.9972(2) 0.0566(11) Uani 1 1 d . . . . . H12S H 0.228571 0.910305 1.035434 0.068 Uiso 1 1 calc R U . . . C13S C 0.1038(3) 0.8067(3) 0.9849(2) 0.0488(10) Uani 1 1 d . . . . . H13S H 0.061749 0.804424 1.014809 0.059 Uiso 1 1 calc R U . . . C14S C 0.0654(3) 0.7473(3) 0.92990(19) 0.0426(9) Uani 1 1 d . . . . . H14S H -0.002855 0.704221 0.922024 0.051 Uiso 1 1 calc R U . . . C22S C 0.0212(7) 1.0218(6) 0.5635(4) 0.0559(7) Uani 0.5 1 d . . P B 1 H22A H -0.000163 0.973635 0.526676 0.084 Uiso 0.5 1 calc R U P B 1 H22B H 0.078402 1.072541 0.559142 0.084 Uiso 0.5 1 calc R U P B 1 H22C H -0.039092 1.042358 0.571993 0.084 Uiso 0.5 1 calc R U P B 1 C23S C 0.0588(5) 0.9865(5) 0.6139(3) 0.0559(7) Uani 0.5 1 d G . P B 1 C91 C -0.0104(4) 0.9549(5) 0.6500(3) 0.0559(7) Uani 0.5 1 d G . P B 1 H91 H -0.082133 0.952524 0.641506 0.067 Uiso 0.5 1 calc R U P B 1 C90 C 0.0252(5) 0.9267(5) 0.6984(3) 0.0559(7) Uani 0.5 1 d G . P B 1 H90 H -0.022090 0.905160 0.723058 0.067 Uiso 0.5 1 calc R U P B 1 C89 C 0.1302(5) 0.9302(5) 0.7108(3) 0.0559(7) Uani 0.5 1 d G . P B 1 H89 H 0.154543 0.910955 0.743926 0.067 Uiso 0.5 1 calc R U P B 1 C25S C 0.1994(4) 0.9618(5) 0.6748(3) 0.0559(7) Uani 0.5 1 d G . P B 1 H25S H 0.271136 0.964114 0.683240 0.067 Uiso 0.5 1 calc R U P B 1 C24S C 0.1638(4) 0.9899(5) 0.6263(3) 0.0559(7) Uani 0.5 1 d G U P B 1 H24S H 0.211095 1.011479 0.601687 0.067 Uiso 0.5 1 calc R U P B 1 C1S C 0.9331(5) 0.3499(4) 0.6774(2) 0.0729(16) Uani 1 1 d . . . . . H1SA H 0.899169 0.395955 0.673614 0.109 Uiso 1 1 calc R U . . . H1SB H 1.009422 0.375698 0.680759 0.109 Uiso 1 1 calc R U . . . H1SC H 0.918257 0.329225 0.712972 0.109 Uiso 1 1 calc R U . . . C2S C 0.8907(3) 0.2713(3) 0.62364(19) 0.0444(9) Uani 1 1 d . . . . . C3S C 0.7961(4) 0.2066(3) 0.6201(2) 0.0560(12) Uani 1 1 d . . . . . H3S H 0.759797 0.211541 0.652501 0.067 Uiso 1 1 calc R U . . . C4S C 0.7534(3) 0.1359(3) 0.5716(3) 0.0641(14) Uani 1 1 d . . . . . H4S H 0.687589 0.092520 0.570236 0.077 Uiso 1 1 calc R U . . . C5S C 0.8055(3) 0.1269(3) 0.5242(2) 0.0600(12) Uani 1 1 d . . . . . H5S H 0.775502 0.077794 0.490041 0.072 Uiso 1 1 calc R U . . . C6S C 0.9013(3) 0.1898(3) 0.52692(19) 0.0454(9) Uani 1 1 d . . . . . H6S H 0.937948 0.184013 0.494736 0.054 Uiso 1 1 calc R U . . . C7S C 0.9435(3) 0.2608(3) 0.57629(18) 0.0402(8) Uani 1 1 d . . . . . H7S H 1.010032 0.303505 0.578151 0.048 Uiso 1 1 calc R U . . . C15S C -0.2044(4) 1.0426(3) 0.8289(2) 0.0621(13) Uani 1 1 d . . . . . H15D H -0.216030 1.092151 0.857202 0.093 Uiso 1 1 calc R U . . . H15E H -0.266934 0.989147 0.819864 0.093 Uiso 1 1 calc R U . . . H15F H -0.191671 1.060792 0.792284 0.093 Uiso 1 1 calc R U . . . C16S C -0.1123(4) 1.0213(3) 0.8548(2) 0.0561(12) Uani 1 1 d . . . . . C17S C -0.0155(4) 1.0511(3) 0.8342(2) 0.0643(13) Uani 1 1 d . . . . . H17S H -0.009632 1.086766 0.806303 0.077 Uiso 1 1 calc R U . . . C18S C 0.0683(4) 1.0270(4) 0.8558(3) 0.0714(14) Uani 1 1 d . . . . . H18S H 0.132546 1.044853 0.841710 0.086 Uiso 1 1 calc R U . . . C19S C 0.0615(4) 0.9763(4) 0.8983(3) 0.0816(19) Uani 1 1 d . . . . . H19S H 0.120181 0.959344 0.912513 0.098 Uiso 1 1 calc R U . . . C20S C -0.0309(4) 0.9518(4) 0.9190(3) 0.0673(14) Uani 1 1 d . . . . . H20S H -0.035628 0.920561 0.949395 0.081 Uiso 1 1 calc R U . . . C21S C -0.1182(4) 0.9730(3) 0.8951(2) 0.0565(11) Uani 1 1 d . . . . . H21S H -0.183293 0.952476 0.907904 0.068 Uiso 1 1 calc R U . . . C59A C 0.9826(6) 0.4677(5) 0.8582(4) 0.0428(7) Uiso 0.5 1 d D . P A 1 H59D H 0.994242 0.453369 0.817226 0.064 Uiso 0.5 1 calc R U P A 1 H59E H 1.049494 0.483473 0.885638 0.064 Uiso 0.5 1 calc R U P A 1 H59F H 0.954696 0.518861 0.864532 0.064 Uiso 0.5 1 calc R U P A 1 C60A C 0.9717(7) 0.3266(6) 0.8525(4) 0.0428(7) Uiso 0.5 1 d D . P A 2 H60D H 0.934926 0.263166 0.849949 0.064 Uiso 0.5 1 calc R U P A 2 H60E H 1.036315 0.347805 0.882493 0.064 Uiso 0.5 1 calc R U P A 2 H60F H 0.989808 0.332431 0.813855 0.064 Uiso 0.5 1 calc R U P A 2 C58A C 0.8659(6) 0.3686(6) 0.9272(3) 0.0428(7) Uiso 0.5 1 d D . P A 2 H58D H 0.808802 0.394488 0.933718 0.064 Uiso 0.5 1 calc R U P A 2 H58E H 0.925603 0.398367 0.960247 0.064 Uiso 0.5 1 calc R U P A 2 H58F H 0.840852 0.303775 0.924647 0.064 Uiso 0.5 1 calc R U P A 2 C25M C -0.1225(7) 0.9892(6) 0.6542(4) 0.0559(7) Uani 0.5 1 d . . P C 2 H25A H -0.174052 0.928825 0.645283 0.084 Uiso 0.5 1 calc R U P C 2 H25B H -0.140349 1.020851 0.624848 0.084 Uiso 0.5 1 calc R U P C 2 H25C H -0.123709 1.023383 0.693917 0.084 Uiso 0.5 1 calc R U P C 2 C26S C -0.0244(4) 0.9818(5) 0.6521(3) 0.0559(7) Uani 0.5 1 d G . P C 2 C31S C 0.0212(5) 0.9391(5) 0.6886(3) 0.0559(7) Uani 0.5 1 d G . P C 2 H31S H -0.016753 0.912996 0.715660 0.067 Uiso 0.5 1 calc R U P C 2 C30S C 0.1223(5) 0.9345(5) 0.6856(3) 0.0559(7) Uani 0.5 1 d G . P C 2 H30S H 0.153486 0.905358 0.710557 0.067 Uiso 0.5 1 calc R U P C 2 C29S C 0.1779(4) 0.9727(5) 0.6460(3) 0.0559(7) Uani 0.5 1 d G . P C 2 H29S H 0.247004 0.969623 0.643926 0.067 Uiso 0.5 1 calc R U P C 2 C28S C 0.1323(5) 1.0154(4) 0.6094(3) 0.0559(7) Uani 0.5 1 d G . P C 2 H28S H 0.170284 1.041526 0.582398 0.067 Uiso 0.5 1 calc R U P C 2 C27S C 0.0312(5) 1.0200(4) 0.6125(3) 0.0559(7) Uani 0.5 1 d G . P C 2 H27S H 0.000044 1.049165 0.587501 0.067 Uiso 0.5 1 calc R U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.01807(6) 0.01719(7) 0.01856(7) 0.00457(5) -0.00092(5) 0.00599(4) O1 0.0223(9) 0.0243(10) 0.0289(11) 0.0083(9) 0.0030(8) 0.0068(7) N1 0.0212(10) 0.0198(11) 0.0207(12) 0.0032(9) 0.0005(8) 0.0058(8) C1 0.0203(11) 0.0214(13) 0.0188(13) 0.0056(10) 0.0020(9) 0.0087(9) Tb2 0.01926(6) 0.01774(7) 0.01861(8) 0.00442(5) -0.00132(5) 0.00667(5) O2 0.0280(10) 0.0281(11) 0.0209(11) 0.0077(8) 0.0036(8) 0.0104(8) N2 0.0222(10) 0.0185(11) 0.0219(12) 0.0043(9) -0.0004(9) 0.0074(8) C2 0.0189(11) 0.0210(13) 0.0227(14) 0.0063(11) 0.0001(10) 0.0081(9) O3 0.0244(9) 0.0235(10) 0.0280(11) 0.0073(9) 0.0017(8) 0.0070(8) C3 0.0212(11) 0.0217(13) 0.0230(14) 0.0037(11) -0.0011(10) 0.0084(10) O4 0.0280(10) 0.0300(11) 0.0232(11) 0.0082(9) 0.0033(8) 0.0098(8) C4 0.0192(11) 0.0278(14) 0.0235(14) 0.0065(11) -0.0012(10) 0.0110(10) C5 0.0233(12) 0.0249(14) 0.0258(15) 0.0074(11) 0.0015(10) 0.0127(10) C6 0.0214(11) 0.0211(13) 0.0231(14) 0.0063(11) 0.0034(10) 0.0087(9) C7 0.0233(12) 0.0212(13) 0.0214(14) 0.0071(11) 0.0023(10) 0.0077(10) C8 0.0269(13) 0.0226(14) 0.0260(15) 0.0075(11) 0.0026(11) 0.0116(10) C9 0.0314(14) 0.0196(13) 0.0265(15) 0.0060(11) 0.0072(11) 0.0105(10) C10 0.0290(13) 0.0205(13) 0.0223(15) 0.0041(11) 0.0028(11) 0.0076(10) C11 0.0244(12) 0.0220(13) 0.0224(14) 0.0064(11) 0.0037(10) 0.0062(10) C12 0.0226(12) 0.0217(13) 0.0214(14) 0.0074(11) 0.0035(10) 0.0087(10) C13 0.0212(12) 0.0311(15) 0.0261(15) 0.0032(12) -0.0031(10) 0.0118(11) C14 0.0273(16) 0.100(4) 0.040(2) 0.002(2) 0.0008(15) 0.023(2) C15 0.070(3) 0.051(2) 0.081(3) -0.012(2) -0.044(2) 0.031(2) C16 0.039(2) 0.124(5) 0.044(3) 0.048(3) -0.0103(18) -0.005(2) C17 0.0362(15) 0.0205(14) 0.0301(17) 0.0054(12) 0.0050(12) 0.0115(11) C18 0.053(2) 0.0272(17) 0.046(2) 0.0047(15) -0.0057(17) 0.0190(15) C19 0.062(2) 0.0308(18) 0.044(2) 0.0054(16) 0.0198(18) 0.0229(16) C20 0.0424(18) 0.0228(16) 0.055(2) 0.0118(15) 0.0064(16) 0.0059(13) C21 0.0274(13) 0.0200(13) 0.0237(15) 0.0026(11) 0.0030(11) 0.0044(10) C22 0.0251(12) 0.0254(14) 0.0191(14) 0.0027(11) 0.0014(10) 0.0042(10) C23 0.0236(12) 0.0282(15) 0.0254(15) 0.0092(12) 0.0022(11) 0.0084(10) C24 0.0234(12) 0.0242(14) 0.0264(15) 0.0080(12) 0.0017(10) 0.0071(10) C25 0.0244(12) 0.0269(15) 0.0248(15) 0.0084(12) 0.0022(11) 0.0061(10) C26 0.0243(13) 0.0348(16) 0.0283(16) 0.0117(13) 0.0001(11) 0.0118(11) C27 0.0248(13) 0.0360(17) 0.0267(16) 0.0078(13) -0.0017(11) 0.0084(12) C28 0.0283(13) 0.0291(15) 0.0248(16) 0.0045(12) 0.0007(11) 0.0070(11) C29 0.0203(11) 0.0192(12) 0.0186(13) 0.0024(10) -0.0017(9) 0.0069(9) C30 0.0191(11) 0.0189(12) 0.0223(14) 0.0028(10) -0.0021(9) 0.0035(9) C31 0.0228(12) 0.0271(14) 0.0251(15) 0.0054(12) 0.0035(10) 0.0058(10) C32 0.0253(13) 0.0347(17) 0.0253(16) 0.0088(13) 0.0058(11) 0.0032(11) C33 0.0327(14) 0.0289(15) 0.0263(16) 0.0136(13) 0.0033(12) 0.0042(12) C34 0.0290(13) 0.0232(14) 0.0235(15) 0.0089(11) 0.0000(11) 0.0066(10) C35 0.0220(11) 0.0174(12) 0.0214(14) 0.0053(10) 0.0009(10) 0.0054(9) C36 0.0212(11) 0.0175(12) 0.0231(14) 0.0047(10) 0.0003(10) 0.0082(9) C37 0.0195(11) 0.0190(12) 0.0199(13) 0.0028(10) -0.0023(9) 0.0062(9) C38 0.0198(11) 0.0195(13) 0.0224(14) 0.0046(10) -0.0003(10) 0.0048(9) C39 0.0212(12) 0.0285(15) 0.0284(16) 0.0070(12) 0.0024(11) 0.0065(10) C40 0.0253(13) 0.0338(16) 0.0287(17) 0.0104(13) 0.0062(11) 0.0030(11) C41 0.0315(14) 0.0294(16) 0.0284(17) 0.0137(13) 0.0034(12) 0.0046(12) C42 0.0275(13) 0.0226(14) 0.0274(16) 0.0084(12) -0.0012(11) 0.0068(10) C43 0.0219(11) 0.0194(13) 0.0208(14) 0.0061(10) 0.0015(10) 0.0065(9) C44 0.0208(11) 0.0167(12) 0.0204(14) 0.0031(10) -0.0009(9) 0.0066(9) C45 0.0204(11) 0.0219(13) 0.0191(13) 0.0044(10) 0.0011(9) 0.0082(9) C46 0.0204(11) 0.0209(13) 0.0211(14) 0.0040(10) -0.0004(10) 0.0081(9) C47 0.0194(11) 0.0223(13) 0.0236(14) 0.0052(11) 0.0005(10) 0.0079(9) C48 0.0180(11) 0.0264(14) 0.0249(15) 0.0064(11) -0.0009(10) 0.0094(10) C49 0.0223(12) 0.0223(13) 0.0283(15) 0.0082(11) 0.0011(10) 0.0109(10) C50 0.0218(11) 0.0207(13) 0.0214(14) 0.0051(11) 0.0020(10) 0.0095(9) C51 0.0212(11) 0.0221(13) 0.0228(14) 0.0061(11) 0.0025(10) 0.0085(10) C52 0.0272(13) 0.0233(14) 0.0260(15) 0.0079(12) 0.0035(11) 0.0118(10) C53 0.0300(13) 0.0194(13) 0.0279(16) 0.0052(12) 0.0058(11) 0.0088(10) C54 0.0268(13) 0.0219(14) 0.0244(15) 0.0053(11) 0.0037(11) 0.0067(10) C55 0.0243(12) 0.0218(13) 0.0215(14) 0.0042(11) 0.0021(10) 0.0080(10) C56 0.0224(11) 0.0196(13) 0.0202(14) 0.0053(10) 0.0030(10) 0.0074(9) C57 0.0200(12) 0.0304(15) 0.0314(16) 0.0032(12) -0.0045(11) 0.0111(11) C61 0.0383(16) 0.0216(14) 0.0348(18) 0.0030(13) 0.0018(13) 0.0112(12) C62 0.086(3) 0.0285(19) 0.062(3) 0.0019(18) -0.022(2) 0.031(2) C63 0.064(2) 0.0310(18) 0.050(2) 0.0055(17) 0.0208(19) 0.0238(17) C64 0.054(2) 0.0231(17) 0.073(3) 0.0157(18) 0.016(2) 0.0070(15) C65 0.0270(13) 0.0205(13) 0.0249(15) 0.0001(11) 0.0027(11) 0.0060(10) C66 0.0271(13) 0.0263(14) 0.0216(15) 0.0026(12) 0.0015(11) 0.0056(11) C67 0.0256(13) 0.0286(15) 0.0246(15) 0.0080(12) 0.0019(11) 0.0097(11) C68 0.0252(13) 0.0279(15) 0.0267(16) 0.0088(12) 0.0034(11) 0.0084(11) C69 0.0254(13) 0.0269(15) 0.0243(15) 0.0070(12) 0.0022(11) 0.0065(11) C70 0.0251(13) 0.0369(17) 0.0252(16) 0.0128(13) 0.0012(11) 0.0119(12) C71 0.0285(14) 0.0392(18) 0.0245(16) 0.0070(13) -0.0023(11) 0.0107(12) C72 0.0316(14) 0.0311(16) 0.0240(16) 0.0030(12) -0.0022(11) 0.0115(12) C73 0.0300(14) 0.0286(16) 0.0365(18) 0.0154(14) 0.0068(12) 0.0078(11) C74 0.0373(16) 0.0316(17) 0.043(2) 0.0142(15) 0.0151(14) 0.0086(13) C75 0.0310(16) 0.054(2) 0.051(2) 0.0222(19) 0.0136(15) 0.0130(15) C76 0.0205(13) 0.046(2) 0.047(2) 0.0216(17) 0.0047(13) 0.0087(12) C77 0.0370(16) 0.0378(18) 0.0235(16) 0.0119(13) 0.0028(12) 0.0139(13) C78 0.0439(18) 0.044(2) 0.0292(18) 0.0150(15) 0.0099(14) 0.0132(15) C79 0.0370(17) 0.050(2) 0.041(2) 0.0171(17) 0.0162(15) 0.0185(15) C80 0.0311(14) 0.0363(17) 0.0328(18) 0.0135(14) 0.0098(12) 0.0166(12) C81 0.0333(15) 0.0272(15) 0.0331(18) 0.0128(13) 0.0071(12) 0.0080(12) C82 0.0428(18) 0.0307(17) 0.040(2) 0.0104(15) 0.0153(15) 0.0080(14) C83 0.041(2) 0.079(3) 0.104(4) 0.059(3) 0.030(2) 0.026(2) C84 0.0217(14) 0.076(3) 0.057(3) 0.038(2) 0.0065(15) 0.0127(16) C85 0.0409(17) 0.0344(17) 0.0244(16) 0.0092(13) 0.0027(13) 0.0133(13) C86 0.052(2) 0.041(2) 0.0305(19) 0.0125(16) 0.0142(15) 0.0134(16) C87 0.0402(18) 0.059(3) 0.046(2) 0.025(2) 0.0202(16) 0.0210(17) C88 0.0338(15) 0.0396(18) 0.0336(18) 0.0141(15) 0.0120(13) 0.0188(13) C8S 0.069(3) 0.093(4) 0.050(3) 0.013(3) 0.012(2) 0.042(3) C9S 0.048(2) 0.053(2) 0.043(2) 0.0233(18) 0.0133(16) 0.0312(18) C10S 0.044(2) 0.068(3) 0.062(3) 0.043(2) 0.0273(19) 0.0313(19) C11S 0.041(2) 0.050(2) 0.075(3) 0.022(2) 0.016(2) 0.0155(17) C12S 0.047(2) 0.057(3) 0.064(3) 0.006(2) 0.011(2) 0.0210(19) C13S 0.0415(19) 0.063(3) 0.049(2) 0.016(2) 0.0169(17) 0.0230(18) C14S 0.0372(17) 0.050(2) 0.048(2) 0.0232(19) 0.0135(16) 0.0153(16) C22S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C23S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C91 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C90 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C89 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C25S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C24S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C1S 0.080(4) 0.095(4) 0.052(3) 0.006(3) 0.016(3) 0.047(3) C2S 0.0445(19) 0.057(2) 0.049(2) 0.027(2) 0.0167(17) 0.0292(18) C3S 0.055(2) 0.068(3) 0.071(3) 0.042(3) 0.037(2) 0.034(2) C4S 0.039(2) 0.056(3) 0.111(5) 0.040(3) 0.031(2) 0.0163(19) C5S 0.046(2) 0.050(3) 0.076(3) 0.008(2) -0.001(2) 0.0141(19) C6S 0.0423(19) 0.054(2) 0.048(2) 0.0185(19) 0.0160(17) 0.0211(17) C7S 0.0331(16) 0.047(2) 0.047(2) 0.0197(18) 0.0136(15) 0.0143(14) C15S 0.056(3) 0.043(2) 0.084(4) 0.011(2) 0.004(2) 0.0175(19) C16S 0.058(2) 0.034(2) 0.064(3) -0.0049(19) -0.006(2) 0.0159(18) C17S 0.049(2) 0.056(3) 0.074(3) -0.005(2) 0.017(2) 0.008(2) C18S 0.062(3) 0.072(4) 0.070(4) 0.007(3) 0.007(3) 0.014(3) C19S 0.069(3) 0.059(3) 0.098(5) -0.010(3) -0.027(3) 0.030(3) C20S 0.064(3) 0.058(3) 0.076(4) 0.018(3) -0.005(3) 0.021(2) C21S 0.063(3) 0.041(2) 0.060(3) 0.006(2) 0.006(2) 0.0139(19) C25M 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C26S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C31S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C30S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C29S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C28S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) C27S 0.0531(11) 0.0539(13) 0.0540(13) 0.0073(11) 0.0122(10) 0.0104(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0027 0.0018 '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 0.0051 0.0037 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0094 0.0068 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.5874 4.5779 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 C22 74.54(8) . . ? O1 Tb1 C24 81.29(9) . . ? O1 Tb1 C29 108.63(8) . . ? O1 Tb1 C30 134.45(8) . . ? O1 Tb1 C35 124.06(8) . . ? O1 Tb1 C36 93.17(9) . . ? O1 Tb1 C44 85.08(8) . . ? N1 Tb1 O1 87.39(8) . . ? N1 Tb1 O2 85.27(8) . . ? N1 Tb1 C22 81.29(9) . . ? N1 Tb1 C24 133.08(9) . . ? N1 Tb1 C29 68.08(8) . . ? N1 Tb1 C30 87.05(8) . . ? N1 Tb1 C35 116.81(8) . . ? N1 Tb1 C36 116.61(8) . . ? N1 Tb1 C44 85.40(8) . . ? O2 Tb1 O1 147.25(8) . . ? O2 Tb1 C22 72.82(8) . . ? O2 Tb1 C24 80.68(9) . . ? O2 Tb1 C29 98.05(8) . . ? O2 Tb1 C30 76.98(9) . . ? O2 Tb1 C35 87.42(9) . . ? O2 Tb1 C36 118.59(9) . . ? O2 Tb1 C44 125.92(8) . . ? C24 Tb1 C22 51.79(9) . . ? C24 Tb1 C29 158.10(9) . . ? C24 Tb1 C30 131.69(9) . . ? C24 Tb1 C35 107.04(9) . . ? C24 Tb1 C36 109.40(9) . . ? C24 Tb1 C44 137.92(9) . . ? C29 Tb1 C22 148.80(8) . . ? C29 Tb1 C30 29.66(8) . . ? C30 Tb1 C22 148.34(8) . . ? C35 Tb1 C22 152.41(8) . . ? C35 Tb1 C29 51.12(8) . . ? C35 Tb1 C30 30.64(8) . . ? C36 Tb1 C22 158.26(8) . . ? C36 Tb1 C29 51.92(8) . . ? C36 Tb1 C30 50.59(9) . . ? C36 Tb1 C35 31.17(9) . . ? C36 Tb1 C44 31.93(8) . . ? C44 Tb1 C22 156.04(9) . . ? C44 Tb1 C29 30.58(8) . . ? C44 Tb1 C30 49.42(9) . . ? C44 Tb1 C35 51.31(9) . . ? C73 O1 Tb1 122.16(17) . . ? C76 O1 Tb1 127.53(19) . . ? C76 O1 C73 108.0(2) . . ? C1 N1 Tb1 122.47(18) . . ? C12 N1 Tb1 133.78(18) . . ? C12 N1 C1 103.7(2) . . ? N1 C1 C2 125.0(2) . . ? N1 C1 C6 112.8(2) . . ? C2 C1 C6 122.2(2) . . ? N2 Tb2 O3 87.27(8) . . ? N2 Tb2 O4 84.37(8) . . ? N2 Tb2 C36 84.97(8) . . ? N2 Tb2 C37 68.17(8) . . ? N2 Tb2 C38 87.88(8) . . ? N2 Tb2 C43 117.63(8) . . ? N2 Tb2 C44 116.32(8) . . ? N2 Tb2 C66 81.68(9) . . ? N2 Tb2 C68 133.23(10) . . ? O3 Tb2 O4 147.58(8) . . ? O3 Tb2 C36 84.60(9) . . ? O3 Tb2 C37 108.77(8) . . ? O3 Tb2 C38 134.28(8) . . ? O3 Tb2 C43 123.04(8) . . ? O3 Tb2 C44 92.12(8) . . ? O3 Tb2 C66 74.35(8) . . ? O3 Tb2 C68 81.97(9) . . ? O4 Tb2 C36 125.57(8) . . ? O4 Tb2 C37 97.01(8) . . ? O4 Tb2 C38 76.70(9) . . ? O4 Tb2 C43 88.30(9) . . ? O4 Tb2 C44 119.61(9) . . ? O4 Tb2 C66 73.47(8) . . ? O4 Tb2 C68 81.20(9) . . ? C36 Tb2 C37 30.80(8) . . ? C36 Tb2 C38 49.68(9) . . ? C36 Tb2 C43 51.61(9) . . ? C36 Tb2 C66 155.49(9) . . ? C37 Tb2 C38 29.84(8) . . ? C37 Tb2 C66 149.26(8) . . ? C38 Tb2 C66 149.16(9) . . ? C43 Tb2 C37 51.48(8) . . ? C43 Tb2 C38 30.80(8) . . ? C43 Tb2 C66 152.44(9) . . ? C44 Tb2 C36 31.92(8) . . ? C44 Tb2 C37 52.07(8) . . ? C44 Tb2 C38 50.71(8) . . ? C44 Tb2 C43 31.31(9) . . ? C44 Tb2 C66 157.40(8) . . ? C68 Tb2 C36 138.31(9) . . ? C68 Tb2 C37 157.65(9) . . ? C68 Tb2 C38 130.59(10) . . ? C68 Tb2 C43 106.17(10) . . ? C68 Tb2 C44 109.48(10) . . ? C68 Tb2 C66 51.58(10) . . ? C77 O2 Tb1 128.13(18) . . ? C77 O2 C80 106.6(2) . . ? C80 O2 Tb1 123.04(18) . . ? C45 N2 Tb2 122.23(18) . . ? C56 N2 Tb2 133.54(18) . . ? C56 N2 C45 104.1(2) . . ? C1 C2 C29 116.3(2) . . ? C3 C2 C1 117.1(2) . . ? C3 C2 C29 126.6(3) . . ? C81 O3 Tb2 122.61(17) . . ? C84 O3 Tb2 127.3(2) . . ? C84 O3 C81 108.2(2) . . ? C2 C3 H3 118.9 . . ? C2 C3 C4 122.2(3) . . ? C4 C3 H3 118.9 . . ? C85 O4 Tb2 127.79(18) . . ? C85 O4 C88 106.8(2) . . ? C88 O4 Tb2 123.62(18) . . ? C3 C4 C13 122.4(3) . . ? C5 C4 C3 119.1(2) . . ? C5 C4 C13 118.5(2) . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(3) . . ? C6 C5 H5 119.7 . . ? C1 C6 C7 105.2(2) . . ? C5 C6 C1 118.9(3) . . ? C5 C6 C7 135.8(3) . . ? C8 C7 C6 135.3(3) . . ? C8 C7 C12 119.5(3) . . ? C12 C7 C6 105.0(2) . . ? C7 C8 H8 119.7 . . ? C9 C8 C7 120.7(3) . . ? C9 C8 H8 119.7 . . ? C8 C9 C10 118.8(3) . . ? C8 C9 C17 122.4(3) . . ? C10 C9 C17 118.8(3) . . ? C9 C10 H10 118.8 . . ? C11 C10 C9 122.4(3) . . ? C11 C10 H10 118.8 . . ? C10 C11 C12 117.6(3) . . ? C10 C11 C21 125.5(3) . . ? C12 C11 C21 116.9(3) . . ? N1 C12 C7 113.1(2) . . ? N1 C12 C11 125.8(2) . . ? C11 C12 C7 121.0(3) . . ? C14 C13 C4 109.8(3) . . ? C14 C13 C16 107.7(4) . . ? C15 C13 C4 113.5(3) . . ? C15 C13 C14 107.9(4) . . ? C15 C13 C16 107.5(4) . . ? C16 C13 C4 110.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C9 112.0(3) . . ? C18 C17 C20 107.0(3) . . ? C19 C17 C9 109.4(3) . . ? C19 C17 C18 109.1(3) . . ? C19 C17 C20 109.7(3) . . ? C20 C17 C9 109.6(3) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C11 171.6(3) . . ? C21 C22 Tb1 90.4(2) . . ? C21 C22 C23 174.8(3) . . ? C23 C22 Tb1 84.43(18) . . ? C24 C23 C22 115.9(3) . . ? C28 C23 C22 120.6(3) . . ? C28 C23 C24 123.6(3) . . ? C23 C24 Tb1 107.90(19) . . ? C25 C24 Tb1 137.7(2) . . ? C25 C24 C23 114.4(3) . . ? C24 C25 H25 118.4 . . ? C26 C25 C24 123.1(3) . . ? C26 C25 H25 118.4 . . ? C25 C26 H26 119.8 . . ? C27 C26 C25 120.4(3) . . ? C27 C26 H26 119.8 . . ? C26 C27 H27 120.3 . . ? C28 C27 C26 119.4(3) . . ? C28 C27 H27 120.3 . . ? C23 C28 H28 120.4 . . ? C27 C28 C23 119.1(3) . . ? C27 C28 H28 120.4 . . ? C2 C29 Tb1 108.04(17) . . ? C30 C29 Tb1 75.97(15) . . ? C30 C29 C2 128.1(3) . . ? C30 C29 C44 105.8(2) . . ? C44 C29 Tb1 70.45(14) . . ? C44 C29 C2 124.6(3) . . ? C29 C30 Tb1 74.37(15) . . ? C29 C30 C35 110.4(2) . . ? C31 C30 Tb1 120.38(19) . . ? C31 C30 C29 131.4(3) . . ? C31 C30 C35 118.2(3) . . ? C35 C30 Tb1 71.53(14) . . ? C30 C31 H31 120.0 . . ? C32 C31 C30 119.9(3) . . ? C32 C31 H31 120.0 . . ? C31 C32 H32 119.1 . . ? C31 C32 C33 121.8(3) . . ? C33 C32 H32 119.1 . . ? C32 C33 H33 119.8 . . ? C34 C33 C32 120.4(3) . . ? C34 C33 H33 119.8 . . ? C33 C34 H34 120.3 . . ? C33 C34 C35 119.4(3) . . ? C35 C34 H34 120.3 . . ? C30 C35 Tb1 77.83(15) . . ? C34 C35 Tb1 116.63(19) . . ? C34 C35 C30 120.3(3) . . ? C34 C35 C36 132.8(2) . . ? C36 C35 Tb1 71.73(15) . . ? C36 C35 C30 106.9(2) . . ? Tb1 C36 Tb2 147.96(11) . . ? C35 C36 Tb1 77.10(16) . . ? C35 C36 Tb2 113.30(18) . . ? C35 C36 C37 143.4(2) . . ? C35 C36 C44 106.8(2) . . ? C37 C36 Tb1 111.86(18) . . ? C37 C36 Tb2 78.57(16) . . ? C37 C36 C44 109.8(2) . . ? C44 C36 Tb1 74.86(15) . . ? C44 C36 Tb2 73.12(16) . . ? C36 C37 Tb2 70.63(15) . . ? C36 C37 C46 125.2(3) . . ? C38 C37 Tb2 75.75(15) . . ? C38 C37 C36 105.7(2) . . ? C38 C37 C46 127.7(3) . . ? C46 C37 Tb2 108.15(17) . . ? C37 C38 Tb2 74.41(15) . . ? C37 C38 C43 110.7(2) . . ? C39 C38 Tb2 120.1(2) . . ? C39 C38 C37 131.4(3) . . ? C39 C38 C43 118.0(3) . . ? C43 C38 Tb2 71.52(15) . . ? C38 C39 H39 120.2 . . ? C40 C39 C38 119.7(3) . . ? C40 C39 H39 120.2 . . ? C39 C40 H40 118.9 . . ? C39 C40 C41 122.1(3) . . ? C41 C40 H40 118.9 . . ? C40 C41 H41 119.8 . . ? C42 C41 C40 120.4(3) . . ? C42 C41 H41 119.8 . . ? C41 C42 H42 120.4 . . ? C41 C42 C43 119.3(3) . . ? C43 C42 H42 120.4 . . ? C38 C43 Tb2 77.68(15) . . ? C42 C43 Tb2 116.05(19) . . ? C42 C43 C38 120.6(3) . . ? C42 C43 C44 132.9(2) . . ? C44 C43 Tb2 71.89(15) . . ? C44 C43 C38 106.5(2) . . ? Tb2 C44 Tb1 148.16(11) . . ? C29 C44 Tb1 78.97(16) . . ? C29 C44 Tb2 113.39(18) . . ? C29 C44 C36 110.0(2) . . ? C29 C44 C43 142.7(3) . . ? C36 C44 Tb1 73.21(15) . . ? C36 C44 Tb2 74.96(15) . . ? C43 C44 Tb1 111.90(17) . . ? C43 C44 Tb2 76.80(16) . . ? C43 C44 C36 107.3(2) . . ? N2 C45 C46 125.0(2) . . ? N2 C45 C50 112.5(2) . . ? C46 C45 C50 122.4(2) . . ? C45 C46 C37 116.3(2) . . ? C47 C46 C37 126.7(3) . . ? C47 C46 C45 117.1(2) . . ? C46 C47 H47 118.9 . . ? C46 C47 C48 122.3(3) . . ? C48 C47 H47 118.9 . . ? C47 C48 C57 120.3(3) . . ? C49 C48 C47 119.0(2) . . ? C49 C48 C57 120.7(2) . . ? C48 C49 H49 119.8 . . ? C48 C49 C50 120.4(2) . . ? C50 C49 H49 119.8 . . ? C45 C50 C51 105.4(2) . . ? C49 C50 C45 119.0(3) . . ? C49 C50 C51 135.5(3) . . ? C52 C51 C50 135.5(2) . . ? C52 C51 C56 119.5(3) . . ? C56 C51 C50 104.8(2) . . ? C51 C52 H52 119.7 . . ? C53 C52 C51 120.5(3) . . ? C53 C52 H52 119.7 . . ? C52 C53 C54 119.0(3) . . ? C52 C53 C61 122.5(3) . . ? C54 C53 C61 118.5(3) . . ? C53 C54 H54 118.9 . . ? C55 C54 C53 122.2(3) . . ? C55 C54 H54 118.9 . . ? C54 C55 C56 117.6(3) . . ? C54 C55 C65 125.1(3) . . ? C56 C55 C65 117.2(3) . . ? N2 C56 C51 113.1(2) . . ? N2 C56 C55 125.7(2) . . ? C55 C56 C51 121.1(3) . . ? C48 C57 C59A 107.7(4) . . ? C58 C57 C48 110.8(4) . . ? C58 C57 C60 111.9(5) . . ? C58 C57 C59A 108.7(5) . . ? C59 C57 C48 114.6(4) . . ? C59 C57 C60A 107.3(5) . . ? C59 C57 C58A 106.3(5) . . ? C60 C57 C48 112.2(4) . . ? C60 C57 C59A 105.4(5) . . ? C60A C57 C48 111.4(4) . . ? C60A C57 C58A 109.7(5) . . ? C58A C57 C48 107.4(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58B 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.4 . . ? C57 C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 C53 111.8(3) . . ? C62 C61 C64 106.7(3) . . ? C63 C61 C53 109.4(3) . . ? C63 C61 C62 109.6(3) . . ? C63 C61 C64 109.7(3) . . ? C64 C61 C53 109.6(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62B 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63B 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64B 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C66 C65 C55 172.4(3) . . ? C65 C66 Tb2 89.4(2) . . ? C65 C66 C67 174.0(3) . . ? C67 C66 Tb2 84.68(18) . . ? C68 C67 C66 115.3(3) . . ? C72 C67 C66 121.1(3) . . ? C72 C67 C68 123.5(3) . . ? C67 C68 Tb2 108.4(2) . . ? C69 C68 Tb2 137.3(2) . . ? C69 C68 C67 114.3(3) . . ? C68 C69 H69 118.3 . . ? C68 C69 C70 123.3(3) . . ? C70 C69 H69 118.3 . . ? C69 C70 H70 119.9 . . ? C71 C70 C69 120.2(3) . . ? C71 C70 H70 119.9 . . ? C70 C71 H71 120.2 . . ? C72 C71 C70 119.5(3) . . ? C72 C71 H71 120.2 . . ? C67 C72 H72 120.5 . . ? C71 C72 C67 119.1(3) . . ? C71 C72 H72 120.5 . . ? O1 C73 H73A 110.5 . . ? O1 C73 H73B 110.5 . . ? O1 C73 C74 105.9(3) . . ? H73A C73 H73B 108.7 . . ? C74 C73 H73A 110.5 . . ? C74 C73 H73B 110.5 . . ? C73 C74 H74A 110.7 . . ? C73 C74 H74B 110.7 . . ? C73 C74 C75 105.1(3) . . ? H74A C74 H74B 108.8 . . ? C75 C74 H74A 110.7 . . ? C75 C74 H74B 110.7 . . ? C74 C75 H75A 110.4 . . ? C74 C75 H75B 110.4 . . ? H75A C75 H75B 108.6 . . ? C76 C75 C74 106.4(3) . . ? C76 C75 H75A 110.4 . . ? C76 C75 H75B 110.4 . . ? O1 C76 C75 107.4(3) . . ? O1 C76 H76A 110.2 . . ? O1 C76 H76B 110.2 . . ? C75 C76 H76A 110.2 . . ? C75 C76 H76B 110.2 . . ? H76A C76 H76B 108.5 . . ? O2 C77 H77A 110.6 . . ? O2 C77 H77B 110.6 . . ? O2 C77 C78 105.6(3) . . ? H77A C77 H77B 108.8 . . ? C78 C77 H77A 110.6 . . ? C78 C77 H77B 110.6 . . ? C77 C78 H78A 110.7 . . ? C77 C78 H78B 110.7 . . ? C77 C78 C79 105.4(3) . . ? H78A C78 H78B 108.8 . . ? C79 C78 H78A 110.7 . . ? C79 C78 H78B 110.7 . . ? C78 C79 H79A 110.6 . . ? C78 C79 H79B 110.6 . . ? H79A C79 H79B 108.8 . . ? C80 C79 C78 105.5(3) . . ? C80 C79 H79A 110.6 . . ? C80 C79 H79B 110.6 . . ? O2 C80 C79 105.9(3) . . ? O2 C80 H80A 110.6 . . ? O2 C80 H80B 110.6 . . ? C79 C80 H80A 110.6 . . ? C79 C80 H80B 110.6 . . ? H80A C80 H80B 108.7 . . ? O3 C81 H81A 110.5 . . ? O3 C81 H81B 110.5 . . ? O3 C81 C82 106.1(3) . . ? H81A C81 H81B 108.7 . . ? C82 C81 H81A 110.5 . . ? C82 C81 H81B 110.5 . . ? C81 C82 H82A 110.9 . . ? C81 C82 H82B 110.9 . . ? H82A C82 H82B 108.9 . . ? C83 C82 C81 104.3(3) . . ? C83 C82 H82A 110.9 . . ? C83 C82 H82B 110.9 . . ? C82 C83 H83A 109.9 . . ? C82 C83 H83B 109.9 . . ? H83A C83 H83B 108.3 . . ? C84 C83 C82 108.8(3) . . ? C84 C83 H83A 109.9 . . ? C84 C83 H83B 109.9 . . ? O3 C84 C83 108.1(3) . . ? O3 C84 H84A 110.1 . . ? O3 C84 H84B 110.1 . . ? C83 C84 H84A 110.1 . . ? C83 C84 H84B 110.1 . . ? H84A C84 H84B 108.4 . . ? O4 C85 H85A 110.6 . . ? O4 C85 H85B 110.6 . . ? O4 C85 C86 105.6(3) . . ? H85A C85 H85B 108.8 . . ? C86 C85 H85A 110.6 . . ? C86 C85 H85B 110.6 . . ? C85 C86 H86A 110.6 . . ? C85 C86 H86B 110.6 . . ? C85 C86 C87 105.5(3) . . ? H86A C86 H86B 108.8 . . ? C87 C86 H86A 110.6 . . ? C87 C86 H86B 110.6 . . ? C86 C87 H87A 110.6 . . ? C86 C87 H87B 110.6 . . ? H87A C87 H87B 108.7 . . ? C88 C87 C86 105.7(3) . . ? C88 C87 H87A 110.6 . . ? C88 C87 H87B 110.6 . . ? O4 C88 C87 105.7(3) . . ? O4 C88 H88A 110.6 . . ? O4 C88 H88B 110.6 . . ? C87 C88 H88A 110.6 . . ? C87 C88 H88B 110.6 . . ? H88A C88 H88B 108.7 . . ? H8SA C8S H8SB 109.5 . . ? H8SA C8S H8SC 109.5 . . ? H8SB C8S H8SC 109.5 . . ? C9S C8S H8SA 109.5 . . ? C9S C8S H8SB 109.5 . . ? C9S C8S H8SC 109.5 . . ? C10S C9S C8S 120.9(4) . . ? C14S C9S C8S 121.3(4) . . ? C14S C9S C10S 117.8(4) . . ? C9S C10S H10S 119.4 . . ? C11S C10S C9S 121.2(4) . . ? C11S C10S H10S 119.4 . . ? C10S C11S H11S 120.0 . . ? C12S C11S C10S 120.1(4) . . ? C12S C11S H11S 120.0 . . ? C11S C12S H12S 120.0 . . ? C11S C12S C13S 119.9(5) . . ? C13S C12S H12S 120.0 . . ? C12S C13S H13S 119.6 . . ? C14S C13S C12S 120.8(4) . . ? C14S C13S H13S 119.6 . . ? C9S C14S H14S 119.9 . . ? C13S C14S C9S 120.2(4) . . ? C13S C14S H14S 119.9 . . ? H22A C22S H22B 109.5 . . ? H22A C22S H22C 109.5 . . ? H22B C22S H22C 109.5 . . ? C23S C22S H22A 109.5 . . ? C23S C22S H22B 109.5 . . ? C23S C22S H22C 109.5 . . ? C91 C23S C22S 119.7(5) . . ? C91 C23S C24S 120.0 . . ? C24S C23S C22S 120.2(5) . . ? C23S C91 H91 120.0 . . ? C23S C91 C90 120.0 . . ? C90 C91 H91 120.0 . . ? C91 C90 H90 120.0 . . ? C91 C90 C89 120.0 . . ? C89 C90 H90 120.0 . . ? C90 C89 H89 120.0 . . ? C25S C89 C90 120.0 . . ? C25S C89 H89 120.0 . . ? C89 C25S H25S 120.0 . . ? C89 C25S C24S 120.0 . . ? C24S C25S H25S 120.0 . . ? C23S C24S H24S 120.0 . . ? C25S C24S C23S 120.0 . . ? C25S C24S H24S 120.0 . . ? H1SA C1S H1SB 109.5 . . ? H1SA C1S H1SC 109.5 . . ? H1SB C1S H1SC 109.5 . . ? C2S C1S H1SA 109.5 . . ? C2S C1S H1SB 109.5 . . ? C2S C1S H1SC 109.5 . . ? C3S C2S C1S 119.8(4) . . ? C3S C2S C7S 117.8(4) . . ? C7S C2S C1S 122.5(4) . . ? C2S C3S H3S 119.1 . . ? C4S C3S C2S 121.8(4) . . ? C4S C3S H3S 119.1 . . ? C3S C4S H4S 120.0 . . ? C3S C4S C5S 120.1(4) . . ? C5S C4S H4S 120.0 . . ? C4S C5S H5S 120.3 . . ? C6S C5S C4S 119.4(5) . . ? C6S C5S H5S 120.3 . . ? C5S C6S H6S 120.1 . . ? C7S C6S C5S 119.8(4) . . ? C7S C6S H6S 120.1 . . ? C2S C7S H7S 119.4 . . ? C6S C7S C2S 121.2(4) . . ? C6S C7S H7S 119.4 . . ? H15D C15S H15E 109.5 . . ? H15D C15S H15F 109.5 . . ? H15E C15S H15F 109.5 . . ? C16S C15S H15D 109.5 . . ? C16S C15S H15E 109.5 . . ? C16S C15S H15F 109.5 . . ? C17S C16S C15S 118.3(5) . . ? C21S C16S C15S 121.8(5) . . ? C21S C16S C17S 119.9(5) . . ? C16S C17S H17S 120.8 . . ? C18S C17S C16S 118.3(5) . . ? C18S C17S H17S 120.8 . . ? C17S C18S H18S 119.3 . . ? C17S C18S C19S 121.4(5) . . ? C19S C18S H18S 119.3 . . ? C18S C19S H19S 120.5 . . ? C20S C19S C18S 119.0(5) . . ? C20S C19S H19S 120.5 . . ? C19S C20S H20S 120.2 . . ? C19S C20S C21S 119.7(5) . . ? C21S C20S H20S 120.2 . . ? C16S C21S C20S 121.6(5) . . ? C16S C21S H21S 119.2 . . ? C20S C21S H21S 119.2 . . ? C57 C59A H59D 109.4 . . ? C57 C59A H59E 109.5 . . ? C57 C59A H59F 109.5 . . ? H59D C59A H59E 109.5 . . ? H59D C59A H59F 109.5 . . ? H59E C59A H59F 109.5 . . ? C57 C60A H60D 109.5 . . ? C57 C60A H60E 109.5 . . ? C57 C60A H60F 109.5 . . ? H60D C60A H60E 109.5 . . ? H60D C60A H60F 109.5 . . ? H60E C60A H60F 109.5 . . ? C57 C58A H58D 109.5 . . ? C57 C58A H58E 109.5 . . ? C57 C58A H58F 109.5 . . ? H58D C58A H58E 109.5 . . ? H58D C58A H58F 109.5 . . ? H58E C58A H58F 109.5 . . ? H25A C25M H25B 109.5 . . ? H25A C25M H25C 109.5 . . ? H25B C25M H25C 109.5 . . ? C26S C25M H25A 109.5 . . ? C26S C25M H25B 109.5 . . ? C26S C25M H25C 109.5 . . ? C25M C26S C31S 122.1(6) . . ? C25M C26S C27S 117.9(6) . . ? C31S C26S C27S 120.0 . . ? C26S C31S H31S 120.0 . . ? C26S C31S C30S 120.0 . . ? C30S C31S H31S 120.0 . . ? C31S C30S H30S 120.0 . . ? C29S C30S C31S 120.0 . . ? C29S C30S H30S 120.0 . . ? C30S C29S H29S 120.0 . . ? C28S C29S C30S 120.0 . . ? C28S C29S H29S 120.0 . . ? C29S C28S H28S 120.0 . . ? C27S C28S C29S 120.0 . . ? C27S C28S H28S 120.0 . . ? C26S C27S H27S 120.0 . . ? C28S C27S C26S 120.0 . . ? C28S C27S H27S 120.0 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.391(2) . ? Tb1 N1 2.304(2) . ? Tb1 O2 2.382(2) . ? Tb1 C22 2.991(3) . ? Tb1 C24 2.458(3) . ? Tb1 C29 2.767(3) . ? Tb1 C30 2.787(3) . ? Tb1 C35 2.704(3) . ? Tb1 C36 2.634(3) . ? Tb1 C44 2.656(3) . ? O1 C73 1.455(4) . ? O1 C76 1.449(3) . ? N1 C1 1.389(3) . ? N1 C12 1.380(4) . ? C1 C2 1.401(4) . ? C1 C6 1.413(4) . ? Tb2 N2 2.304(2) . ? Tb2 O3 2.387(2) . ? Tb2 O4 2.387(2) . ? Tb2 C36 2.658(3) . ? Tb2 C37 2.762(3) . ? Tb2 C38 2.779(3) . ? Tb2 C43 2.698(3) . ? Tb2 C44 2.634(3) . ? Tb2 C66 3.001(3) . ? Tb2 C68 2.460(3) . ? O2 C77 1.446(4) . ? O2 C80 1.453(3) . ? N2 C45 1.391(3) . ? N2 C56 1.374(3) . ? C2 C3 1.393(3) . ? C2 C29 1.485(4) . ? O3 C81 1.458(4) . ? O3 C84 1.443(4) . ? C3 H3 0.9500 . ? C3 C4 1.416(4) . ? O4 C85 1.449(4) . ? O4 C88 1.453(4) . ? C4 C5 1.389(4) . ? C4 C13 1.531(4) . ? C5 H5 0.9500 . ? C5 C6 1.397(4) . ? C6 C7 1.441(4) . ? C7 C8 1.398(4) . ? C7 C12 1.415(4) . ? C8 H8 0.9500 . ? C8 C9 1.388(4) . ? C9 C10 1.410(4) . ? C9 C17 1.533(4) . ? C10 H10 0.9500 . ? C10 C11 1.399(4) . ? C11 C12 1.403(4) . ? C11 C21 1.432(4) . ? C13 C14 1.508(5) . ? C13 C15 1.504(5) . ? C13 C16 1.516(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.529(5) . ? C17 C19 1.520(5) . ? C17 C20 1.531(5) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.198(4) . ? C22 C23 1.446(4) . ? C23 C24 1.420(4) . ? C23 C28 1.402(4) . ? C24 C25 1.396(4) . ? C25 H25 0.9500 . ? C25 C26 1.396(4) . ? C26 H26 0.9500 . ? C26 C27 1.387(5) . ? C27 H27 0.9500 . ? C27 C28 1.383(4) . ? C28 H28 0.9500 . ? C29 C30 1.422(4) . ? C29 C44 1.434(4) . ? C30 C31 1.416(4) . ? C30 C35 1.453(4) . ? C31 H31 0.9500 . ? C31 C32 1.371(4) . ? C32 H32 0.9500 . ? C32 C33 1.421(4) . ? C33 H33 0.9500 . ? C33 C34 1.373(4) . ? C34 H34 0.9500 . ? C34 C35 1.419(4) . ? C35 C36 1.436(4) . ? C36 C37 1.443(4) . ? C36 C44 1.455(4) . ? C37 C38 1.427(4) . ? C37 C46 1.482(4) . ? C38 C39 1.415(4) . ? C38 C43 1.457(4) . ? C39 H39 0.9500 . ? C39 C40 1.372(4) . ? C40 H40 0.9500 . ? C40 C41 1.418(4) . ? C41 H41 0.9500 . ? C41 C42 1.369(4) . ? C42 H42 0.9500 . ? C42 C43 1.414(4) . ? C43 C44 1.440(4) . ? C45 C46 1.402(4) . ? C45 C50 1.409(4) . ? C46 C47 1.387(3) . ? C47 H47 0.9500 . ? C47 C48 1.422(4) . ? C48 C49 1.391(4) . ? C48 C57 1.533(4) . ? C49 H49 0.9500 . ? C49 C50 1.399(4) . ? C50 C51 1.446(4) . ? C51 C52 1.397(4) . ? C51 C56 1.414(4) . ? C52 H52 0.9500 . ? C52 C53 1.393(4) . ? C53 C54 1.408(4) . ? C53 C61 1.530(4) . ? C54 H54 0.9500 . ? C54 C55 1.398(4) . ? C55 C56 1.406(4) . ? C55 C65 1.439(4) . ? C57 C58 1.475(8) . ? C57 C59 1.504(8) . ? C57 C60 1.519(8) . ? C57 C59A 1.578(8) . ? C57 C60A 1.511(8) . ? C57 C58A 1.523(8) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.524(5) . ? C61 C63 1.522(5) . ? C61 C64 1.529(5) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 C66 1.189(4) . ? C66 C67 1.446(4) . ? C67 C68 1.424(4) . ? C67 C72 1.400(4) . ? C68 C69 1.391(4) . ? C69 H69 0.9500 . ? C69 C70 1.397(4) . ? C70 H70 0.9500 . ? C70 C71 1.387(5) . ? C71 H71 0.9500 . ? C71 C72 1.385(4) . ? C72 H72 0.9500 . ? C73 H73A 0.9900 . ? C73 H73B 0.9900 . ? C73 C74 1.500(4) . ? C74 H74A 0.9900 . ? C74 H74B 0.9900 . ? C74 C75 1.508(5) . ? C75 H75A 0.9900 . ? C75 H75B 0.9900 . ? C75 C76 1.499(5) . ? C76 H76A 0.9900 . ? C76 H76B 0.9900 . ? C77 H77A 0.9900 . ? C77 H77B 0.9900 . ? C77 C78 1.508(5) . ? C78 H78A 0.9900 . ? C78 H78B 0.9900 . ? C78 C79 1.519(5) . ? C79 H79A 0.9900 . ? C79 H79B 0.9900 . ? C79 C80 1.510(5) . ? C80 H80A 0.9900 . ? C80 H80B 0.9900 . ? C81 H81A 0.9900 . ? C81 H81B 0.9900 . ? C81 C82 1.517(5) . ? C82 H82A 0.9900 . ? C82 H82B 0.9900 . ? C82 C83 1.491(6) . ? C83 H83A 0.9900 . ? C83 H83B 0.9900 . ? C83 C84 1.448(5) . ? C84 H84A 0.9900 . ? C84 H84B 0.9900 . ? C85 H85A 0.9900 . ? C85 H85B 0.9900 . ? C85 C86 1.507(5) . ? C86 H86A 0.9900 . ? C86 H86B 0.9900 . ? C86 C87 1.516(5) . ? C87 H87A 0.9900 . ? C87 H87B 0.9900 . ? C87 C88 1.510(5) . ? C88 H88A 0.9900 . ? C88 H88B 0.9900 . ? C8S H8SA 0.9800 . ? C8S H8SB 0.9800 . ? C8S H8SC 0.9800 . ? C8S C9S 1.495(6) . ? C9S C10S 1.402(6) . ? C9S C14S 1.396(5) . ? C10S H10S 0.9500 . ? C10S C11S 1.370(7) . ? C11S H11S 0.9500 . ? C11S C12S 1.367(6) . ? C12S H12S 0.9500 . ? C12S C13S 1.379(6) . ? C13S H13S 0.9500 . ? C13S C14S 1.375(6) . ? C14S H14S 0.9500 . ? C22S H22A 0.9800 . ? C22S H22B 0.9800 . ? C22S H22C 0.9800 . ? C22S C23S 1.509(11) . ? C23S C91 1.3900 . ? C23S C24S 1.3900 . ? C91 H91 0.9500 . ? C91 C90 1.3900 . ? C90 H90 0.9500 . ? C90 C89 1.3900 . ? C89 H89 0.9500 . ? C89 C25S 1.3900 . ? C25S H25S 0.9500 . ? C25S C24S 1.3900 . ? C24S H24S 0.9500 . ? C1S H1SA 0.9800 . ? C1S H1SB 0.9800 . ? C1S H1SC 0.9800 . ? C1S C2S 1.502(7) . ? C2S C3S 1.377(6) . ? C2S C7S 1.391(5) . ? C3S H3S 0.9500 . ? C3S C4S 1.358(7) . ? C4S H4S 0.9500 . ? C4S C5S 1.385(7) . ? C5S H5S 0.9500 . ? C5S C6S 1.378(6) . ? C6S H6S 0.9500 . ? C6S C7S 1.372(6) . ? C7S H7S 0.9500 . ? C15S H15D 0.9800 . ? C15S H15E 0.9800 . ? C15S H15F 0.9800 . ? C15S C16S 1.472(6) . ? C16S C17S 1.431(7) . ? C16S C21S 1.336(7) . ? C17S H17S 0.9500 . ? C17S C18S 1.365(7) . ? C18S H18S 0.9500 . ? C18S C19S 1.405(8) . ? C19S H19S 0.9500 . ? C19S C20S 1.371(8) . ? C20S H20S 0.9500 . ? C20S C21S 1.398(7) . ? C21S H21S 0.9500 . ? C59A H59D 0.9800 . ? C59A H59E 0.9800 . ? C59A H59F 0.9800 . ? C60A H60D 0.9800 . ? C60A H60E 0.9800 . ? C60A H60F 0.9800 . ? C58A H58D 0.9800 . ? C58A H58E 0.9800 . ? C58A H58F 0.9800 . ? C25M H25A 0.9800 . ? C25M H25B 0.9800 . ? C25M H25C 0.9800 . ? C25M C26S 1.362(10) . ? C26S C31S 1.3900 . ? C26S C27S 1.3900 . ? C31S H31S 0.9500 . ? C31S C30S 1.3900 . ? C30S H30S 0.9500 . ? C30S C29S 1.3900 . ? C29S H29S 0.9500 . ? C29S C28S 1.3900 . ? C28S H28S 0.9500 . ? C28S C27S 1.3900 . ? C27S H27S 0.9500 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Tb1 O1 C73 C74 -169.0(2) . . . . ? Tb1 O1 C76 C75 178.9(2) . . . . ? Tb1 N1 C1 C2 3.9(4) . . . . ? Tb1 N1 C1 C6 -178.14(18) . . . . ? Tb1 N1 C12 C7 177.7(2) . . . . ? Tb1 N1 C12 C11 -5.9(4) . . . . ? Tb1 O2 C77 C78 -163.2(2) . . . . ? Tb1 O2 C80 C79 164.0(2) . . . . ? Tb1 C22 C23 C24 1.1(3) . . . . ? Tb1 C22 C23 C28 -179.0(3) . . . . ? Tb1 C24 C25 C26 -179.5(2) . . . . ? Tb1 C29 C30 C31 117.0(3) . . . . ? Tb1 C29 C30 C35 -62.91(19) . . . . ? Tb1 C29 C44 Tb2 149.17(15) . . . . ? Tb1 C29 C44 C36 67.41(19) . . . . ? Tb1 C29 C44 C43 -111.8(4) . . . . ? Tb1 C30 C31 C32 -83.8(3) . . . . ? Tb1 C30 C35 C34 113.9(3) . . . . ? Tb1 C30 C35 C36 -66.38(18) . . . . ? Tb1 C35 C36 Tb2 -148.02(14) . . . . ? Tb1 C35 C36 C37 109.4(4) . . . . ? Tb1 C35 C36 C44 -69.57(18) . . . . ? Tb1 C36 C37 Tb2 -148.29(15) . . . . ? Tb1 C36 C37 C38 -80.0(2) . . . . ? Tb1 C36 C37 C46 112.7(3) . . . . ? Tb1 C36 C44 Tb2 178.97(8) . . . . ? Tb1 C36 C44 C29 -71.2(2) . . . . ? Tb1 C36 C44 C43 108.31(19) . . . . ? O1 C73 C74 C75 -24.9(4) . . . . ? N1 C1 C2 C3 177.4(3) . . . . ? N1 C1 C2 C29 -4.3(4) . . . . ? N1 C1 C6 C5 -177.7(3) . . . . ? N1 C1 C6 C7 -0.6(3) . . . . ? C1 N1 C12 C7 -2.0(3) . . . . ? C1 N1 C12 C11 174.4(3) . . . . ? C1 C2 C3 C4 0.3(4) . . . . ? C1 C2 C29 Tb1 2.4(3) . . . . ? C1 C2 C29 C30 88.5(4) . . . . ? C1 C2 C29 C44 -75.9(4) . . . . ? C1 C6 C7 C8 -177.0(3) . . . . ? C1 C6 C7 C12 -0.6(3) . . . . ? Tb2 N2 C45 C46 -1.6(4) . . . . ? Tb2 N2 C45 C50 -177.89(18) . . . . ? Tb2 N2 C56 C51 178.1(2) . . . . ? Tb2 N2 C56 C55 2.1(4) . . . . ? Tb2 O3 C81 C82 173.1(2) . . . . ? Tb2 O3 C84 C83 179.8(3) . . . . ? Tb2 O4 C85 C86 161.9(2) . . . . ? Tb2 O4 C88 C87 -163.0(2) . . . . ? Tb2 C36 C37 C38 68.31(19) . . . . ? Tb2 C36 C37 C46 -99.0(3) . . . . ? Tb2 C36 C44 Tb1 -178.97(8) . . . . ? Tb2 C36 C44 C29 109.8(2) . . . . ? Tb2 C36 C44 C43 -70.66(19) . . . . ? Tb2 C37 C38 C39 -116.6(3) . . . . ? Tb2 C37 C38 C43 62.80(19) . . . . ? Tb2 C37 C46 C45 -4.4(3) . . . . ? Tb2 C37 C46 C47 175.3(2) . . . . ? Tb2 C38 C39 C40 83.2(3) . . . . ? Tb2 C38 C43 C42 -113.1(3) . . . . ? Tb2 C38 C43 C44 66.63(18) . . . . ? Tb2 C43 C44 Tb1 147.79(13) . . . . ? Tb2 C43 C44 C29 -111.4(4) . . . . ? Tb2 C43 C44 C36 69.39(18) . . . . ? Tb2 C66 C67 C68 -0.5(3) . . . . ? Tb2 C66 C67 C72 179.5(3) . . . . ? Tb2 C68 C69 C70 -179.6(2) . . . . ? O2 C77 C78 C79 -21.8(4) . . . . ? N2 C45 C46 C37 4.4(4) . . . . ? N2 C45 C46 C47 -175.2(3) . . . . ? N2 C45 C50 C49 175.7(3) . . . . ? N2 C45 C50 C51 0.1(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? C2 C1 C6 C7 177.4(3) . . . . ? C2 C3 C4 C5 -0.2(5) . . . . ? C2 C3 C4 C13 -178.7(3) . . . . ? C2 C29 C30 Tb1 -102.1(3) . . . . ? C2 C29 C30 C31 14.9(5) . . . . ? C2 C29 C30 C35 -165.0(3) . . . . ? C2 C29 C44 Tb1 98.9(3) . . . . ? C2 C29 C44 Tb2 -112.0(3) . . . . ? C2 C29 C44 C36 166.3(2) . . . . ? C2 C29 C44 C43 -12.9(6) . . . . ? O3 C81 C82 C83 19.3(4) . . . . ? C3 C2 C29 Tb1 -179.4(2) . . . . ? C3 C2 C29 C30 -93.4(4) . . . . ? C3 C2 C29 C44 102.3(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C3 C4 C13 C14 116.3(4) . . . . ? C3 C4 C13 C15 -4.6(5) . . . . ? C3 C4 C13 C16 -125.2(4) . . . . ? O4 C85 C86 C87 21.5(4) . . . . ? C4 C5 C6 C1 -0.2(4) . . . . ? C4 C5 C6 C7 -176.1(3) . . . . ? C5 C4 C13 C14 -62.2(4) . . . . ? C5 C4 C13 C15 176.9(4) . . . . ? C5 C4 C13 C16 56.3(4) . . . . ? C5 C6 C7 C8 -0.7(6) . . . . ? C5 C6 C7 C12 175.7(3) . . . . ? C6 C1 C2 C3 -0.4(4) . . . . ? C6 C1 C2 C29 178.0(3) . . . . ? C6 C7 C8 C9 173.9(3) . . . . ? C6 C7 C12 N1 1.7(3) . . . . ? C6 C7 C12 C11 -175.0(3) . . . . ? C7 C8 C9 C10 0.9(5) . . . . ? C7 C8 C9 C17 -177.3(3) . . . . ? C8 C7 C12 N1 178.7(3) . . . . ? C8 C7 C12 C11 2.1(4) . . . . ? C8 C9 C10 C11 0.4(5) . . . . ? C8 C9 C17 C18 -8.2(4) . . . . ? C8 C9 C17 C19 112.9(4) . . . . ? C8 C9 C17 C20 -126.8(3) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C9 C10 C11 C21 -179.7(3) . . . . ? C10 C9 C17 C18 173.7(3) . . . . ? C10 C9 C17 C19 -65.2(4) . . . . ? C10 C9 C17 C20 55.0(4) . . . . ? C10 C11 C12 N1 -177.1(3) . . . . ? C10 C11 C12 C7 -0.9(4) . . . . ? C12 N1 C1 C2 -176.4(3) . . . . ? C12 N1 C1 C6 1.6(3) . . . . ? C12 C7 C8 C9 -2.1(4) . . . . ? C13 C4 C5 C6 178.7(3) . . . . ? C17 C9 C10 C11 178.6(3) . . . . ? C21 C11 C12 N1 2.3(4) . . . . ? C21 C11 C12 C7 178.5(3) . . . . ? C22 C23 C24 Tb1 -1.3(3) . . . . ? C22 C23 C24 C25 178.9(3) . . . . ? C22 C23 C28 C27 -179.1(3) . . . . ? C23 C24 C25 C26 0.2(4) . . . . ? C24 C23 C28 C27 0.9(5) . . . . ? C24 C25 C26 C27 1.0(5) . . . . ? C25 C26 C27 C28 -1.3(5) . . . . ? C26 C27 C28 C23 0.4(5) . . . . ? C28 C23 C24 Tb1 178.7(3) . . . . ? C28 C23 C24 C25 -1.1(5) . . . . ? C29 C2 C3 C4 -177.8(3) . . . . ? C29 C30 C31 C32 -179.5(3) . . . . ? C29 C30 C35 Tb1 64.7(2) . . . . ? C29 C30 C35 C34 178.6(2) . . . . ? C29 C30 C35 C36 -1.7(3) . . . . ? C30 C29 C44 Tb1 -68.39(18) . . . . ? C30 C29 C44 Tb2 80.8(2) . . . . ? C30 C29 C44 C36 -1.0(3) . . . . ? C30 C29 C44 C43 179.8(3) . . . . ? C30 C31 C32 C33 0.7(5) . . . . ? C30 C35 C36 Tb1 70.60(19) . . . . ? C30 C35 C36 Tb2 -77.4(2) . . . . ? C30 C35 C36 C37 180.0(4) . . . . ? C30 C35 C36 C44 1.0(3) . . . . ? C31 C30 C35 Tb1 -115.2(2) . . . . ? C31 C30 C35 C34 -1.3(4) . . . . ? C31 C30 C35 C36 178.4(2) . . . . ? C31 C32 C33 C34 -0.9(5) . . . . ? C32 C33 C34 C35 -0.1(5) . . . . ? C33 C34 C35 Tb1 92.3(3) . . . . ? C33 C34 C35 C30 1.2(4) . . . . ? C33 C34 C35 C36 -178.5(3) . . . . ? C34 C35 C36 Tb1 -109.7(3) . . . . ? C34 C35 C36 Tb2 102.3(3) . . . . ? C34 C35 C36 C37 -0.3(6) . . . . ? C34 C35 C36 C44 -179.3(3) . . . . ? C35 C30 C31 C32 0.4(4) . . . . ? C35 C36 C37 Tb2 113.9(4) . . . . ? C35 C36 C37 C38 -177.8(4) . . . . ? C35 C36 C37 C46 14.9(6) . . . . ? C35 C36 C44 Tb1 71.14(19) . . . . ? C35 C36 C44 Tb2 -109.9(2) . . . . ? C35 C36 C44 C29 0.0(3) . . . . ? C35 C36 C44 C43 179.5(2) . . . . ? C36 C37 C38 Tb2 -64.75(18) . . . . ? C36 C37 C38 C39 178.7(3) . . . . ? C36 C37 C38 C43 -1.9(3) . . . . ? C36 C37 C46 C45 74.4(4) . . . . ? C36 C37 C46 C47 -106.0(4) . . . . ? C37 C36 C44 Tb1 -108.2(2) . . . . ? C37 C36 C44 Tb2 70.8(2) . . . . ? C37 C36 C44 C29 -179.4(2) . . . . ? C37 C36 C44 C43 0.1(3) . . . . ? C37 C38 C39 C40 178.7(3) . . . . ? C37 C38 C43 Tb2 -64.6(2) . . . . ? C37 C38 C43 C42 -177.7(3) . . . . ? C37 C38 C43 C44 2.0(3) . . . . ? C37 C46 C47 C48 -179.6(3) . . . . ? C38 C37 C46 C45 -90.1(3) . . . . ? C38 C37 C46 C47 89.5(4) . . . . ? C38 C39 C40 C41 -0.7(5) . . . . ? C38 C43 C44 Tb1 77.1(2) . . . . ? C38 C43 C44 Tb2 -70.66(19) . . . . ? C38 C43 C44 C29 177.9(3) . . . . ? C38 C43 C44 C36 -1.3(3) . . . . ? C39 C38 C43 Tb2 114.9(2) . . . . ? C39 C38 C43 C42 1.7(4) . . . . ? C39 C38 C43 C44 -178.5(2) . . . . ? C39 C40 C41 C42 1.0(5) . . . . ? C40 C41 C42 C43 0.1(5) . . . . ? C41 C42 C43 Tb2 -92.2(3) . . . . ? C41 C42 C43 C38 -1.5(4) . . . . ? C41 C42 C43 C44 178.8(3) . . . . ? C42 C43 C44 Tb1 -103.1(3) . . . . ? C42 C43 C44 Tb2 109.1(3) . . . . ? C42 C43 C44 C29 -2.3(6) . . . . ? C42 C43 C44 C36 178.5(3) . . . . ? C43 C38 C39 C40 -0.6(4) . . . . ? C44 C29 C30 Tb1 64.56(18) . . . . ? C44 C29 C30 C31 -178.5(3) . . . . ? C44 C29 C30 C35 1.7(3) . . . . ? C44 C36 C37 Tb2 -67.19(19) . . . . ? C44 C36 C37 C38 1.1(3) . . . . ? C44 C36 C37 C46 -166.2(2) . . . . ? C45 N2 C56 C51 2.0(3) . . . . ? C45 N2 C56 C55 -174.0(3) . . . . ? C45 C46 C47 C48 0.0(4) . . . . ? C45 C50 C51 C52 177.3(3) . . . . ? C45 C50 C51 C56 1.1(3) . . . . ? C46 C37 C38 Tb2 102.1(3) . . . . ? C46 C37 C38 C39 -14.5(5) . . . . ? C46 C37 C38 C43 164.9(3) . . . . ? C46 C45 C50 C49 -0.8(4) . . . . ? C46 C45 C50 C51 -176.4(3) . . . . ? C46 C47 C48 C49 -0.8(5) . . . . ? C46 C47 C48 C57 -179.5(3) . . . . ? C47 C48 C49 C50 0.7(4) . . . . ? C47 C48 C57 C58 71.2(5) . . . . ? C47 C48 C57 C59 -22.7(5) . . . . ? C47 C48 C57 C60 -163.0(4) . . . . ? C47 C48 C57 C59A -47.5(5) . . . . ? C47 C48 C57 C60A -144.8(4) . . . . ? C47 C48 C57 C58A 95.1(5) . . . . ? C48 C49 C50 C45 0.0(4) . . . . ? C48 C49 C50 C51 173.9(3) . . . . ? C49 C48 C57 C58 -107.6(5) . . . . ? C49 C48 C57 C59 158.5(4) . . . . ? C49 C48 C57 C60 18.3(5) . . . . ? C49 C48 C57 C59A 133.7(4) . . . . ? C49 C48 C57 C60A 36.5(5) . . . . ? C49 C48 C57 C58A -83.6(5) . . . . ? C49 C50 C51 C52 2.8(6) . . . . ? C49 C50 C51 C56 -173.4(3) . . . . ? C50 C45 C46 C37 -179.6(3) . . . . ? C50 C45 C46 C47 0.7(4) . . . . ? C50 C51 C52 C53 -174.2(3) . . . . ? C50 C51 C56 N2 -2.0(3) . . . . ? C50 C51 C56 C55 174.2(3) . . . . ? C51 C52 C53 C54 0.5(5) . . . . ? C51 C52 C53 C61 178.3(3) . . . . ? C52 C51 C56 N2 -178.9(3) . . . . ? C52 C51 C56 C55 -2.7(4) . . . . ? C52 C53 C54 C55 -1.5(5) . . . . ? C52 C53 C61 C62 10.0(5) . . . . ? C52 C53 C61 C63 -111.6(4) . . . . ? C52 C53 C61 C64 128.1(3) . . . . ? C53 C54 C55 C56 0.4(4) . . . . ? C53 C54 C55 C65 178.1(3) . . . . ? C54 C53 C61 C62 -172.1(3) . . . . ? C54 C53 C61 C63 66.3(4) . . . . ? C54 C53 C61 C64 -54.1(4) . . . . ? C54 C55 C56 N2 177.4(3) . . . . ? C54 C55 C56 C51 1.7(4) . . . . ? C56 N2 C45 C46 175.1(3) . . . . ? C56 N2 C45 C50 -1.2(3) . . . . ? C56 C51 C52 C53 1.6(4) . . . . ? C57 C48 C49 C50 179.5(3) . . . . ? C61 C53 C54 C55 -179.4(3) . . . . ? C65 C55 C56 N2 -0.5(4) . . . . ? C65 C55 C56 C51 -176.2(3) . . . . ? C66 C67 C68 Tb2 0.7(3) . . . . ? C66 C67 C68 C69 -179.2(3) . . . . ? C66 C67 C72 C71 179.1(3) . . . . ? C67 C68 C69 C70 0.2(5) . . . . ? C68 C67 C72 C71 -0.9(5) . . . . ? C68 C69 C70 C71 -1.1(5) . . . . ? C69 C70 C71 C72 1.0(5) . . . . ? C70 C71 C72 C67 -0.1(5) . . . . ? C72 C67 C68 Tb2 -179.3(3) . . . . ? C72 C67 C68 C69 0.8(5) . . . . ? C73 O1 C76 C75 -18.4(4) . . . . ? C73 C74 C75 C76 13.7(4) . . . . ? C74 C75 C76 O1 2.4(4) . . . . ? C76 O1 C73 C74 27.2(3) . . . . ? C77 O2 C80 C79 -31.6(3) . . . . ? C77 C78 C79 C80 2.8(4) . . . . ? C78 C79 C80 O2 17.1(4) . . . . ? C80 O2 C77 C78 33.5(3) . . . . ? C81 O3 C84 C83 15.5(5) . . . . ? C81 C82 C83 C84 -10.2(5) . . . . ? C82 C83 C84 O3 -2.9(6) . . . . ? C84 O3 C81 C82 -21.8(4) . . . . ? C85 O4 C88 C87 31.1(4) . . . . ? C85 C86 C87 C88 -2.8(4) . . . . ? C86 C87 C88 O4 -16.8(4) . . . . ? C88 O4 C85 C86 -33.0(3) . . . . ? C8S C9S C10S C11S -178.2(4) . . . . ? C8S C9S C14S C13S 179.0(4) . . . . ? C9S C10S C11S C12S -1.8(6) . . . . ? C10S C9S C14S C13S -1.3(6) . . . . ? C10S C11S C12S C13S 0.4(7) . . . . ? C11S C12S C13S C14S 0.4(7) . . . . ? C12S C13S C14S C9S 0.1(6) . . . . ? C14S C9S C10S C11S 2.2(6) . . . . ? C22S C23S C91 C90 -176.5(7) . . . . ? C22S C23S C24S C25S 176.5(7) . . . . ? C23S C91 C90 C89 0.0 . . . . ? C91 C23S C24S C25S 0.0 . . . . ? C91 C90 C89 C25S 0.0 . . . . ? C90 C89 C25S C24S 0.0 . . . . ? C89 C25S C24S C23S 0.0 . . . . ? C24S C23S C91 C90 0.0 . . . . ? C1S C2S C3S C4S 178.0(4) . . . . ? C1S C2S C7S C6S -177.9(4) . . . . ? C2S C3S C4S C5S 0.6(7) . . . . ? C3S C2S C7S C6S 1.9(6) . . . . ? C3S C4S C5S C6S 0.6(7) . . . . ? C4S C5S C6S C7S -0.4(7) . . . . ? C5S C6S C7S C2S -0.8(6) . . . . ? C7S C2S C3S C4S -1.9(6) . . . . ? C15S C16S C17S C18S -176.3(5) . . . . ? C15S C16S C21S C20S 179.0(5) . . . . ? C16S C17S C18S C19S -1.7(8) . . . . ? C17S C16S C21S C20S 1.3(7) . . . . ? C17S C18S C19S C20S -0.8(8) . . . . ? C18S C19S C20S C21S 3.6(8) . . . . ? C19S C20S C21S C16S -3.9(8) . . . . ? C21S C16S C17S C18S 1.5(7) . . . . ? C25M C26S C31S C30S -178.9(8) . . . . ? C25M C26S C27S C28S 178.9(8) . . . . ? C26S C31S C30S C29S 0.0 . . . . ? C31S C26S C27S C28S 0.0 . . . . ? C31S C30S C29S C28S 0.0 . . . . ? C30S C29S C28S C27S 0.0 . . . . ? C29S C28S C27S C26S 0.0 . . . . ? C27S C26S C31S C30S 0.0 . . . . ?