# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'M. L. P. Reddy' _publ_contact_author_email MLPREDDY55@GMAIL.COM _publ_section_title ; Synthesis and crystal structures of lanthanide 4-benzyloxy benzoates: Influence of electron-withdrawing and electron-donating groups on luminescent properties ; loop_ _publ_author_name 'M. L. P. Reddy' 'A. Cowley' 'Sarika Sivakumar' 'Kalyan Vasudevan' # Attachment 'sbkv167a_last.cif' data_sbkv167a _database_code_depnum_ccdc_archive 'CCDC 729140' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C88 H82 O22 S2 Tb2' _chemical_formula_sum 'C88 H82 O22 S2 Tb2' _chemical_formula_weight 1873.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/n _symmetry_space_group_name_Hall -p2yn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 8.5769(17) _cell_length_b 17.011(3) _cell_length_c 27.749(6) _cell_angle_alpha 90.00 _cell_angle_beta 91.83(3) _cell_angle_gamma 90.00 _cell_volume 4046.6(14) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 6987 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.538 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1880 _exptl_absorpt_coefficient_mu 1.860 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15337 _diffrn_reflns_av_R_equivalents 0.0780 _diffrn_reflns_av_sigmaI/netI 0.1565 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.49 _reflns_number_total 9147 _reflns_number_gt 5603 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Four water hydrogen atoms are unable to be located due to the presence of the Tb atom. This discrepancy gives rise to a number of related alerts in the checkcif file. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9147 _refine_ls_number_parameters 516 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1239 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.0889 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C43 C 0.1520(8) -0.0565(4) 0.1744(2) 0.0309(16) Uani 1 1 d . . . H43A H 0.2622 -0.0471 0.1731 0.046 Uiso 1 1 calc R . . H43B H 0.1339 -0.1032 0.1927 0.046 Uiso 1 1 calc R . . H43C H 0.1028 -0.0126 0.1894 0.046 Uiso 1 1 calc R . . C44 C -0.1293(7) -0.0613(3) 0.1264(3) 0.0323(18) Uani 1 1 d . . . H44A H -0.1490 -0.0123 0.1423 0.048 Uiso 1 1 calc R . . H44B H -0.1591 -0.1040 0.1468 0.048 Uiso 1 1 calc R . . H44C H -0.1889 -0.0634 0.0966 0.048 Uiso 1 1 calc R . . O1 O 0.5642(4) 0.1058(2) 0.06606(14) 0.0182(9) Uani 1 1 d . . . O2 O 0.4162(4) 0.0913(2) 0.12870(14) 0.0195(9) Uani 1 1 d . . . O4 O 0.2168(4) 0.1838(2) 0.05544(15) 0.0181(9) Uani 1 1 d . . . O5 O 0.0729(4) 0.1114(2) 0.00572(14) 0.0182(10) Uani 1 1 d . . . O7 O 0.4272(5) 0.0818(2) -0.02457(14) 0.0196(10) Uani 1 1 d . . . O8 O 0.5873(5) 0.0643(2) -0.08498(15) 0.0221(10) Uani 1 1 d . . . O10 O 0.2179(4) -0.0471(2) -0.00659(14) 0.0201(9) Uani 1 1 d . . . O11 O 0.1053(4) 0.0087(2) 0.08986(14) 0.0215(10) Uani 1 1 d . . . Tb1 Tb 0.31190(3) 0.052719(15) 0.046253(10) 0.01369(10) Uani 1 1 d . . . S1 S 0.07243(17) -0.06873(8) 0.11463(6) 0.0201(4) Uani 1 1 d . . . C1 C 0.5472(7) 0.1068(3) 0.1114(2) 0.0175(14) Uani 1 1 d . . . C2 C 0.6857(7) 0.1242(3) 0.1432(2) 0.0162(14) Uani 1 1 d . . . C3 C 0.8238(7) 0.1502(3) 0.1238(2) 0.0196(14) Uani 1 1 d . . . H3 H 0.8265 0.1601 0.0909 0.024 Uiso 1 1 calc R . . C4 C 0.9582(7) 0.1619(3) 0.1524(2) 0.0221(15) Uani 1 1 d . . . H4 H 1.0492 0.1806 0.1391 0.027 Uiso 1 1 calc R . . C5 C 0.9528(7) 0.1448(3) 0.2013(2) 0.0194(14) Uani 1 1 d . . . C6 C 0.8148(7) 0.1181(3) 0.2214(2) 0.0230(15) Uani 1 1 d . . . H6 H 0.8120 0.1074 0.2542 0.028 Uiso 1 1 calc R . . C7 C 0.6839(7) 0.1077(3) 0.1924(2) 0.0227(15) Uani 1 1 d . . . H7 H 0.5927 0.0894 0.2058 0.027 Uiso 1 1 calc R . . C8 C 1.2183(7) 0.1840(4) 0.2157(2) 0.0244(15) Uani 1 1 d . . . H8A H 1.1975 0.2310 0.1967 0.029 Uiso 1 1 calc R . . H8B H 1.2663 0.1453 0.1951 0.029 Uiso 1 1 calc R . . C9 C 1.3267(7) 0.2032(3) 0.2581(2) 0.0206(15) Uani 1 1 d . . . C10 C 1.4631(7) 0.2430(4) 0.2495(2) 0.0262(16) Uani 1 1 d . . . H10 H 1.4865 0.2570 0.2181 0.031 Uiso 1 1 calc R . . C11 C 1.5657(8) 0.2621(4) 0.2873(2) 0.0298(17) Uani 1 1 d . . . H11 H 1.6589 0.2876 0.2812 0.036 Uiso 1 1 calc R . . C12 C 1.5295(8) 0.2431(4) 0.3342(3) 0.0293(17) Uani 1 1 d . . . H12 H 1.5970 0.2567 0.3598 0.035 Uiso 1 1 calc R . . C13 C 1.3931(8) 0.2038(4) 0.3426(2) 0.0336(17) Uani 1 1 d . . . H13 H 1.3678 0.1912 0.3740 0.040 Uiso 1 1 calc R . . C14 C 1.2928(7) 0.1830(4) 0.3047(2) 0.0298(17) Uani 1 1 d . . . H14 H 1.2021 0.1551 0.3107 0.036 Uiso 1 1 calc R . . C15 C 0.1017(7) 0.1776(3) 0.0261(2) 0.0159(13) Uani 1 1 d . . . C16 C 0.0049(7) 0.2474(3) 0.0147(2) 0.0144(13) Uani 1 1 d . . . C17 C -0.1258(7) 0.2427(3) -0.0165(2) 0.0189(14) Uani 1 1 d . . . H17 H -0.1563 0.1939 -0.0287 0.023 Uiso 1 1 calc R . . C18 C -0.2107(7) 0.3086(3) -0.0297(2) 0.0192(14) Uani 1 1 d . . . H18 H -0.2989 0.3040 -0.0499 0.023 Uiso 1 1 calc R . . C19 C -0.1636(7) 0.3820(3) -0.0127(2) 0.0200(15) Uani 1 1 d . . . C20 C -0.0368(7) 0.3879(3) 0.0193(2) 0.0225(16) Uani 1 1 d . . . H20 H -0.0065 0.4366 0.0315 0.027 Uiso 1 1 calc R . . C21 C 0.0443(7) 0.3212(3) 0.0329(2) 0.0226(15) Uani 1 1 d . . . H21 H 0.1278 0.3256 0.0549 0.027 Uiso 1 1 calc R . . C22 C -0.3446(7) 0.4500(3) -0.0655(2) 0.0243(15) Uani 1 1 d . . . H22A H -0.4424 0.4284 -0.0548 0.029 Uiso 1 1 calc R . . H22B H -0.3075 0.4172 -0.0913 0.029 Uiso 1 1 calc R . . C23 C -0.3687(7) 0.5325(3) -0.0831(2) 0.0208(15) Uani 1 1 d . . . C24 C -0.4510(8) 0.5866(4) -0.0568(2) 0.0289(16) Uani 1 1 d . . . H24 H -0.4930 0.5715 -0.0277 0.035 Uiso 1 1 calc R . . C25 C -0.4719(8) 0.6626(4) -0.0729(3) 0.0310(17) Uani 1 1 d . . . H25 H -0.5292 0.6981 -0.0552 0.037 Uiso 1 1 calc R . . C26 C -0.4075(8) 0.6858(4) -0.1157(3) 0.0332(18) Uani 1 1 d . . . H26 H -0.4182 0.7375 -0.1263 0.040 Uiso 1 1 calc R . . C27 C -0.3284(9) 0.6327(4) -0.1421(3) 0.042(2) Uani 1 1 d . . . H27 H -0.2876 0.6479 -0.1714 0.051 Uiso 1 1 calc R . . C28 C -0.3077(8) 0.5561(4) -0.1261(2) 0.0329(17) Uani 1 1 d . . . H28 H -0.2524 0.5205 -0.1444 0.039 Uiso 1 1 calc R . . C29 C 0.4918(7) 0.1046(3) -0.0623(2) 0.0150(13) Uani 1 1 d . . . C30 C 0.4486(6) 0.1845(3) -0.0822(2) 0.0142(13) Uani 1 1 d . . . C31 C 0.4830(7) 0.2046(3) -0.1298(2) 0.0197(15) Uani 1 1 d . . . H31 H 0.5365 0.1694 -0.1489 0.024 Uiso 1 1 calc R . . C32 C 0.4375(7) 0.2765(3) -0.1483(2) 0.0193(14) Uani 1 1 d . . . H32 H 0.4605 0.2894 -0.1798 0.023 Uiso 1 1 calc R . . C33 C 0.3575(7) 0.3301(3) -0.1202(2) 0.0190(14) Uani 1 1 d . . . C34 C 0.3257(7) 0.3121(3) -0.0729(2) 0.0185(14) Uani 1 1 d . . . H34 H 0.2749 0.3482 -0.0537 0.022 Uiso 1 1 calc R . . C35 C 0.3704(6) 0.2401(3) -0.0546(2) 0.0174(14) Uani 1 1 d . . . H35 H 0.3479 0.2279 -0.0229 0.021 Uiso 1 1 calc R . . C36 C 0.2116(8) 0.4508(3) -0.1200(2) 0.0275(15) Uani 1 1 d . . . H36A H 0.2645 0.4758 -0.0926 0.033 Uiso 1 1 calc R . . H36B H 0.1226 0.4220 -0.1085 0.033 Uiso 1 1 calc R . . C37 C 0.1584(7) 0.5120(4) -0.1563(2) 0.0260(16) Uani 1 1 d . . . C38 C 0.0602(8) 0.4914(4) -0.1941(3) 0.0375(19) Uani 1 1 d . . . H38 H 0.0269 0.4396 -0.1973 0.045 Uiso 1 1 calc R . . C39 C 0.0099(9) 0.5476(4) -0.2277(3) 0.045(2) Uani 1 1 d . . . H39 H -0.0587 0.5334 -0.2528 0.054 Uiso 1 1 calc R . . C40 C 0.0613(10) 0.6240(4) -0.2239(3) 0.046(2) Uani 1 1 d . . . H40 H 0.0291 0.6615 -0.2465 0.056 Uiso 1 1 calc R . . C41 C 0.1606(10) 0.6439(4) -0.1862(3) 0.055(2) Uani 1 1 d . . . H41 H 0.1956 0.6955 -0.1832 0.066 Uiso 1 1 calc R . . C42 C 0.2096(9) 0.5890(4) -0.1526(3) 0.042(2) Uani 1 1 d . . . H42 H 0.2773 0.6037 -0.1274 0.050 Uiso 1 1 calc R . . O3 O 1.0762(5) 0.1536(3) 0.23350(14) 0.0286(11) Uani 1 1 d . . . O6 O -0.2314(5) 0.4515(2) -0.02602(15) 0.0253(10) Uani 1 1 d . . . O9 O 0.3157(5) 0.3985(2) -0.14333(15) 0.0255(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C43 0.037(4) 0.032(4) 0.022(4) 0.006(3) -0.010(3) 0.000(3) C44 0.021(4) 0.025(4) 0.052(5) 0.020(3) 0.013(3) 0.005(3) O1 0.016(2) 0.027(2) 0.011(2) -0.0019(18) 0.0009(19) 0.0000(19) O2 0.013(2) 0.025(2) 0.020(3) 0.0013(19) -0.0002(19) 0.0007(19) O4 0.014(2) 0.014(2) 0.026(3) -0.0028(18) -0.004(2) 0.0030(18) O5 0.019(2) 0.012(2) 0.024(3) 0.0017(18) 0.000(2) -0.0005(18) O7 0.024(2) 0.017(2) 0.017(2) 0.0050(18) -0.002(2) -0.0054(19) O8 0.019(2) 0.019(2) 0.029(3) 0.0044(19) 0.002(2) 0.0013(19) O10 0.017(2) 0.019(2) 0.024(2) -0.0027(19) 0.0012(18) 0.0017(19) O11 0.020(2) 0.021(2) 0.024(3) 0.0016(19) 0.003(2) -0.0026(19) Tb1 0.01103(15) 0.01334(15) 0.01664(16) 0.00180(14) -0.00042(11) -0.00040(14) S1 0.0164(8) 0.0183(8) 0.0256(9) 0.0025(7) 0.0007(7) -0.0015(7) C1 0.018(4) 0.011(3) 0.024(4) -0.002(3) 0.003(3) 0.005(3) C2 0.013(3) 0.014(3) 0.022(4) -0.003(3) -0.001(3) 0.001(3) C3 0.029(4) 0.018(3) 0.012(3) -0.001(3) 0.000(3) -0.004(3) C4 0.018(4) 0.028(4) 0.020(4) -0.003(3) 0.002(3) -0.009(3) C5 0.012(3) 0.027(3) 0.019(4) -0.005(3) -0.006(3) 0.004(3) C6 0.023(4) 0.034(4) 0.012(4) 0.003(3) 0.000(3) -0.004(3) C7 0.019(4) 0.030(4) 0.018(4) -0.005(3) 0.002(3) -0.002(3) C8 0.018(4) 0.040(4) 0.015(4) -0.002(3) -0.001(3) 0.001(3) C9 0.016(3) 0.021(3) 0.024(4) -0.004(3) -0.005(3) 0.006(3) C10 0.024(4) 0.032(4) 0.022(4) 0.002(3) -0.004(3) 0.003(3) C11 0.019(4) 0.029(4) 0.040(5) 0.000(3) -0.009(4) -0.004(3) C12 0.031(4) 0.024(4) 0.032(5) -0.006(3) -0.015(3) 0.015(3) C13 0.030(4) 0.050(5) 0.021(4) -0.004(3) -0.001(3) 0.004(4) C14 0.016(4) 0.048(4) 0.025(4) -0.008(3) -0.002(3) -0.001(3) C15 0.014(3) 0.018(3) 0.016(3) 0.004(3) 0.006(3) -0.004(3) C16 0.013(3) 0.012(3) 0.018(4) 0.003(3) 0.001(3) 0.000(3) C17 0.021(4) 0.011(3) 0.024(4) -0.003(3) 0.002(3) 0.000(3) C18 0.012(3) 0.020(3) 0.026(4) -0.003(3) -0.005(3) -0.003(3) C19 0.016(3) 0.021(3) 0.023(4) 0.009(3) -0.002(3) 0.006(3) C20 0.024(4) 0.006(3) 0.036(4) -0.005(3) -0.014(3) 0.000(3) C21 0.018(3) 0.027(4) 0.023(4) 0.003(3) -0.006(3) 0.001(3) C22 0.022(3) 0.020(3) 0.031(4) -0.001(3) -0.009(3) 0.003(3) C23 0.021(4) 0.015(3) 0.026(4) 0.000(3) -0.008(3) 0.003(3) C24 0.036(4) 0.026(4) 0.024(4) 0.003(3) -0.006(3) 0.000(3) C25 0.035(4) 0.024(4) 0.033(4) -0.009(3) -0.007(4) 0.006(3) C26 0.040(5) 0.012(3) 0.047(5) 0.003(3) -0.017(4) -0.005(3) C27 0.066(6) 0.025(4) 0.037(5) 0.010(3) 0.011(4) 0.003(4) C28 0.034(4) 0.027(4) 0.037(4) -0.002(4) 0.009(3) 0.009(3) C29 0.010(3) 0.016(3) 0.018(4) 0.003(3) -0.007(3) -0.006(3) C30 0.006(3) 0.017(3) 0.020(4) 0.005(3) -0.004(3) -0.002(2) C31 0.020(4) 0.023(3) 0.017(4) 0.000(3) 0.001(3) 0.002(3) C32 0.021(3) 0.021(3) 0.016(4) 0.009(3) 0.004(3) 0.006(3) C33 0.015(3) 0.014(3) 0.028(4) 0.001(3) -0.006(3) -0.002(3) C34 0.020(3) 0.015(3) 0.020(4) -0.003(3) 0.003(3) 0.002(3) C35 0.014(3) 0.026(3) 0.012(3) 0.000(3) 0.002(3) -0.004(3) C36 0.036(4) 0.023(3) 0.023(4) 0.004(3) 0.001(3) 0.008(3) C37 0.024(4) 0.023(4) 0.030(4) -0.005(3) -0.001(3) 0.005(3) C38 0.038(5) 0.032(4) 0.042(5) -0.001(4) -0.005(4) 0.004(4) C39 0.053(5) 0.050(5) 0.030(5) 0.005(4) -0.010(4) 0.009(4) C40 0.057(6) 0.041(5) 0.041(5) 0.010(4) -0.001(4) 0.022(4) C41 0.075(7) 0.021(4) 0.068(7) 0.012(4) -0.006(5) 0.006(4) C42 0.051(5) 0.026(4) 0.047(5) -0.002(4) -0.021(4) -0.005(4) O3 0.019(2) 0.050(3) 0.017(3) 0.002(2) -0.002(2) -0.011(2) O6 0.022(2) 0.014(2) 0.039(3) 0.004(2) -0.015(2) 0.002(2) O9 0.030(3) 0.020(2) 0.027(3) 0.010(2) 0.002(2) 0.009(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 C43 S1 1.785(6) . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 S1 1.776(6) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? O1 C1 1.272(7) . ? O1 Tb1 2.392(4) . ? O2 C1 1.263(7) . ? O2 Tb1 2.517(4) . ? O4 C15 1.263(7) . ? O4 Tb1 2.390(3) . ? O5 C15 1.281(6) . ? O5 Tb1 2.513(4) . ? O7 C29 1.261(7) . ? O7 Tb1 2.282(4) . ? O8 C29 1.254(7) . ? O8 Tb1 2.409(4) 3_655 ? O10 Tb1 2.368(4) . ? O11 S1 1.517(4) . ? O11 Tb1 2.302(4) . ? Tb1 O8 2.409(4) 3_655 ? Tb1 C1 2.821(6) . ? Tb1 C15 2.830(6) . ? C1 C2 1.487(8) . ? C2 C3 1.389(8) . ? C2 C7 1.394(8) . ? C3 C4 1.392(8) . ? C3 H3 0.9300 . ? C4 C5 1.390(8) . ? C4 H4 0.9300 . ? C5 O3 1.371(7) . ? C5 C6 1.399(8) . ? C6 C7 1.370(8) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.427(7) . ? C8 C9 1.512(8) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C14 1.378(9) . ? C9 C10 1.379(8) . ? C10 C11 1.388(8) . ? C10 H10 0.9300 . ? C11 C12 1.386(9) . ? C11 H11 0.9300 . ? C12 C13 1.373(9) . ? C12 H12 0.9300 . ? C13 C14 1.384(9) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.478(8) . ? C16 C21 1.389(8) . ? C16 C17 1.397(8) . ? C17 C18 1.381(8) . ? C17 H17 0.9300 . ? C18 C19 1.390(8) . ? C18 H18 0.9300 . ? C19 O6 1.363(6) . ? C19 C20 1.386(8) . ? C20 C21 1.377(8) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 O6 1.440(7) . ? C22 C23 1.497(8) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C28 1.378(9) . ? C23 C24 1.382(8) . ? C24 C25 1.378(8) . ? C24 H24 0.9300 . ? C25 C26 1.383(9) . ? C25 H25 0.9300 . ? C26 C27 1.359(9) . ? C26 H26 0.9300 . ? C27 C28 1.387(8) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.508(8) . ? C30 C35 1.402(8) . ? C30 C31 1.405(8) . ? C31 C32 1.377(8) . ? C31 H31 0.9300 . ? C32 C33 1.393(8) . ? C32 H32 0.9300 . ? C33 O9 1.371(7) . ? C33 C34 1.385(8) . ? C34 C35 1.375(8) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 O9 1.430(7) . ? C36 C37 1.511(8) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.368(9) . ? C37 C42 1.385(9) . ? C38 C39 1.394(9) . ? C38 H38 0.9300 . ? C39 C40 1.375(10) . ? C39 H39 0.9300 . ? C40 C41 1.370(11) . ? C40 H40 0.9300 . ? C41 C42 1.375(9) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? 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 S1 C43 H43A 109.5 . . ? S1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S1 C44 H44A 109.5 . . ? S1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C1 O1 Tb1 95.8(3) . . ? C1 O2 Tb1 90.2(4) . . ? C15 O4 Tb1 96.7(3) . . ? C15 O5 Tb1 90.5(3) . . ? C29 O7 Tb1 174.5(4) . . ? C29 O8 Tb1 117.4(4) . 3_655 ? S1 O11 Tb1 132.7(2) . . ? O7 Tb1 O11 152.25(14) . . ? O7 Tb1 O10 76.74(13) . . ? O11 Tb1 O10 80.79(13) . . ? O7 Tb1 O4 92.77(13) . . ? O11 Tb1 O4 88.63(13) . . ? O10 Tb1 O4 128.62(13) . . ? O7 Tb1 O1 72.68(14) . . ? O11 Tb1 O1 135.04(14) . . ? O10 Tb1 O1 134.47(13) . . ? O4 Tb1 O1 86.13(13) . . ? O7 Tb1 O8 113.82(14) . 3_655 ? O11 Tb1 O8 76.61(13) . 3_655 ? O10 Tb1 O8 78.13(14) . 3_655 ? O4 Tb1 O8 147.32(14) . 3_655 ? O1 Tb1 O8 84.28(13) . 3_655 ? O7 Tb1 O5 84.16(13) . . ? O11 Tb1 O5 74.57(13) . . ? O10 Tb1 O5 75.57(12) . . ? O4 Tb1 O5 53.21(12) . . ? O1 Tb1 O5 132.19(12) . . ? O8 Tb1 O5 143.49(12) 3_655 . ? O7 Tb1 O2 125.09(13) . . ? O11 Tb1 O2 82.20(13) . . ? O10 Tb1 O2 148.66(13) . . ? O4 Tb1 O2 76.83(13) . . ? O1 Tb1 O2 53.14(13) . . ? O8 Tb1 O2 72.42(13) 3_655 . ? O5 Tb1 O2 124.35(13) . . ? O7 Tb1 C1 99.24(16) . . ? O11 Tb1 C1 108.41(16) . . ? O10 Tb1 C1 148.57(14) . . ? O4 Tb1 C1 82.37(14) . . ? O1 Tb1 C1 26.67(14) . . ? O8 Tb1 C1 75.16(14) 3_655 . ? O5 Tb1 C1 135.58(14) . . ? O2 Tb1 C1 26.60(14) . . ? O7 Tb1 C15 87.59(15) . . ? O11 Tb1 C15 81.47(15) . . ? O10 Tb1 C15 102.34(15) . . ? O4 Tb1 C15 26.32(14) . . ? O1 Tb1 C15 109.12(15) . . ? O8 Tb1 C15 157.73(15) 3_655 . ? O5 Tb1 C15 26.91(14) . . ? O2 Tb1 C15 100.91(15) . . ? C1 Tb1 C15 108.67(16) . . ? O11 S1 C44 102.6(3) . . ? O11 S1 C43 104.4(3) . . ? C44 S1 C43 99.6(3) . . ? O2 C1 O1 120.3(6) . . ? O2 C1 C2 121.3(6) . . ? O1 C1 C2 118.4(5) . . ? O2 C1 Tb1 63.2(3) . . ? O1 C1 Tb1 57.5(3) . . ? C2 C1 Tb1 170.8(4) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 120.6(6) . . ? C7 C2 C1 120.5(5) . . ? C2 C3 C4 121.7(6) . . ? C2 C3 H3 119.1 . . ? C4 C3 H3 119.1 . . ? C5 C4 C3 118.2(6) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? O3 C5 C4 124.4(5) . . ? O3 C5 C6 114.9(5) . . ? C4 C5 C6 120.7(6) . . ? C7 C6 C5 119.7(6) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 120.9(6) . . ? C6 C7 H7 119.6 . . ? C2 C7 H7 119.6 . . ? O3 C8 C9 108.6(5) . . ? O3 C8 H8A 110.0 . . ? C9 C8 H8A 110.0 . . ? O3 C8 H8B 110.0 . . ? C9 C8 H8B 110.0 . . ? H8A C8 H8B 108.4 . . ? C14 C9 C10 119.4(6) . . ? C14 C9 C8 122.3(6) . . ? C10 C9 C8 118.4(6) . . ? C9 C10 C11 120.3(6) . . ? C9 C10 H10 119.8 . . ? C11 C10 H10 119.8 . . ? C12 C11 C10 120.1(6) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C13 C12 C11 119.3(6) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 120.6(7) . . ? C12 C13 H13 119.7 . . ? C14 C13 H13 119.7 . . ? C9 C14 C13 120.3(6) . . ? C9 C14 H14 119.8 . . ? C13 C14 H14 119.8 . . ? O4 C15 O5 119.6(5) . . ? O4 C15 C16 119.6(5) . . ? O5 C15 C16 120.9(5) . . ? O4 C15 Tb1 57.0(3) . . ? O5 C15 Tb1 62.6(3) . . ? C16 C15 Tb1 174.6(4) . . ? C21 C16 C17 117.3(5) . . ? C21 C16 C15 121.3(5) . . ? C17 C16 C15 121.4(5) . . ? C18 C17 C16 121.6(5) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C19 119.7(5) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? O6 C19 C20 115.5(5) . . ? O6 C19 C18 124.8(5) . . ? C20 C19 C18 119.7(5) . . ? C21 C20 C19 119.7(5) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? C20 C21 C16 122.0(6) . . ? C20 C21 H21 119.0 . . ? C16 C21 H21 119.0 . . ? O6 C22 C23 108.3(5) . . ? O6 C22 H22A 110.0 . . ? C23 C22 H22A 110.0 . . ? O6 C22 H22B 110.0 . . ? C23 C22 H22B 110.0 . . ? H22A C22 H22B 108.4 . . ? C28 C23 C24 118.5(6) . . ? C28 C23 C22 120.2(6) . . ? C24 C23 C22 121.3(6) . . ? C25 C24 C23 121.1(6) . . ? C25 C24 H24 119.5 . . ? C23 C24 H24 119.5 . . ? C24 C25 C26 119.8(6) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C27 C26 C25 119.5(6) . . ? C27 C26 H26 120.2 . . ? C25 C26 H26 120.2 . . ? C26 C27 C28 120.8(7) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C23 C28 C27 120.3(6) . . ? C23 C28 H28 119.8 . . ? C27 C28 H28 119.8 . . ? O8 C29 O7 124.0(5) . . ? O8 C29 C30 117.8(5) . . ? O7 C29 C30 118.2(5) . . ? C35 C30 C31 117.8(5) . . ? C35 C30 C29 121.6(5) . . ? C31 C30 C29 120.5(5) . . ? C32 C31 C30 120.1(5) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.8(6) . . ? C31 C32 H32 119.6 . . ? C33 C32 H32 119.6 . . ? O9 C33 C34 125.0(5) . . ? O9 C33 C32 114.9(5) . . ? C34 C33 C32 120.1(5) . . ? C35 C34 C33 119.0(5) . . ? C35 C34 H34 120.5 . . ? C33 C34 H34 120.5 . . ? C34 C35 C30 122.3(6) . . ? C34 C35 H35 118.9 . . ? C30 C35 H35 118.9 . . ? O9 C36 C37 107.8(5) . . ? O9 C36 H36A 110.1 . . ? C37 C36 H36A 110.1 . . ? O9 C36 H36B 110.1 . . ? C37 C36 H36B 110.1 . . ? H36A C36 H36B 108.5 . . ? C38 C37 C42 119.0(6) . . ? C38 C37 C36 120.0(6) . . ? C42 C37 C36 121.0(6) . . ? C37 C38 C39 120.3(7) . . ? C37 C38 H38 119.8 . . ? C39 C38 H38 119.8 . . ? C40 C39 C38 120.4(7) . . ? C40 C39 H39 119.8 . . ? C38 C39 H39 119.8 . . ? C41 C40 C39 118.8(7) . . ? C41 C40 H40 120.6 . . ? C39 C40 H40 120.6 . . ? C40 C41 C42 121.2(7) . . ? C40 C41 H41 119.4 . . ? C42 C41 H41 119.4 . . ? C41 C42 C37 120.2(7) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? C5 O3 C8 117.6(5) . . ? C19 O6 C22 117.5(4) . . ? C33 O9 C36 118.3(5) . . ? 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 C29 O7 Tb1 O11 118(4) . . . . ? C29 O7 Tb1 O10 155(4) . . . . ? C29 O7 Tb1 O4 26(4) . . . . ? C29 O7 Tb1 O1 -59(4) . . . . ? C29 O7 Tb1 O8 -135(4) . . . 3_655 ? C29 O7 Tb1 O5 78(4) . . . . ? C29 O7 Tb1 O2 -50(4) . . . . ? C29 O7 Tb1 C1 -57(4) . . . . ? C29 O7 Tb1 C15 52(4) . . . . ? S1 O11 Tb1 O7 101.9(4) . . . . ? S1 O11 Tb1 O10 65.7(3) . . . . ? S1 O11 Tb1 O4 -164.8(3) . . . . ? S1 O11 Tb1 O1 -81.6(3) . . . . ? S1 O11 Tb1 O8 -14.2(3) . . . 3_655 ? S1 O11 Tb1 O5 143.2(3) . . . . ? S1 O11 Tb1 O2 -87.9(3) . . . . ? S1 O11 Tb1 C1 -83.3(3) . . . . ? S1 O11 Tb1 C15 169.8(3) . . . . ? C15 O4 Tb1 O7 78.9(3) . . . . ? C15 O4 Tb1 O11 -73.4(3) . . . . ? C15 O4 Tb1 O10 3.7(4) . . . . ? C15 O4 Tb1 O1 151.3(3) . . . . ? C15 O4 Tb1 O8 -135.6(3) . . . 3_655 ? C15 O4 Tb1 O5 -1.7(3) . . . . ? C15 O4 Tb1 O2 -155.7(3) . . . . ? C15 O4 Tb1 C1 177.9(4) . . . . ? C1 O1 Tb1 O7 174.8(3) . . . . ? C1 O1 Tb1 O11 -3.5(4) . . . . ? C1 O1 Tb1 O10 -135.2(3) . . . . ? C1 O1 Tb1 O4 80.7(3) . . . . ? C1 O1 Tb1 O8 -68.0(3) . . . 3_655 ? C1 O1 Tb1 O5 110.1(3) . . . . ? C1 O1 Tb1 O2 4.3(3) . . . . ? C1 O1 Tb1 C15 93.7(3) . . . . ? C15 O5 Tb1 O7 -96.2(3) . . . . ? C15 O5 Tb1 O11 101.8(3) . . . . ? C15 O5 Tb1 O10 -174.0(3) . . . . ? C15 O5 Tb1 O4 1.7(3) . . . . ? C15 O5 Tb1 O1 -36.0(4) . . . . ? C15 O5 Tb1 O8 140.8(3) . . . 3_655 ? C15 O5 Tb1 O2 32.8(4) . . . . ? C15 O5 Tb1 C1 1.0(4) . . . . ? C1 O2 Tb1 O7 -15.3(4) . . . . ? C1 O2 Tb1 O11 170.2(3) . . . . ? C1 O2 Tb1 O10 112.6(3) . . . . ? C1 O2 Tb1 O4 -99.4(3) . . . . ? C1 O2 Tb1 O1 -4.3(3) . . . . ? C1 O2 Tb1 O8 91.9(3) . . . 3_655 ? C1 O2 Tb1 O5 -124.5(3) . . . . ? C1 O2 Tb1 C15 -110.1(3) . . . . ? Tb1 O11 S1 C44 -166.2(3) . . . . ? Tb1 O11 S1 C43 90.3(4) . . . . ? Tb1 O2 C1 O1 7.5(5) . . . . ? Tb1 O2 C1 C2 -170.9(5) . . . . ? Tb1 O1 C1 O2 -7.9(5) . . . . ? Tb1 O1 C1 C2 170.5(4) . . . . ? O7 Tb1 C1 O2 167.4(3) . . . . ? O11 Tb1 C1 O2 -10.2(3) . . . . ? O10 Tb1 C1 O2 -113.0(4) . . . . ? O4 Tb1 C1 O2 75.8(3) . . . . ? O1 Tb1 C1 O2 172.4(5) . . . . ? O8 Tb1 C1 O2 -80.3(3) 3_655 . . . ? O5 Tb1 C1 O2 76.3(4) . . . . ? C15 Tb1 C1 O2 76.8(3) . . . . ? O7 Tb1 C1 O1 -5.0(3) . . . . ? O11 Tb1 C1 O1 177.4(3) . . . . ? O10 Tb1 C1 O1 74.6(4) . . . . ? O4 Tb1 C1 O1 -96.6(3) . . . . ? O8 Tb1 C1 O1 107.3(3) 3_655 . . . ? O5 Tb1 C1 O1 -96.1(3) . . . . ? O2 Tb1 C1 O1 -172.4(5) . . . . ? C15 Tb1 C1 O1 -95.6(3) . . . . ? O7 Tb1 C1 C2 -71(3) . . . . ? O11 Tb1 C1 C2 111(3) . . . . ? O10 Tb1 C1 C2 9(3) . . . . ? O4 Tb1 C1 C2 -163(3) . . . . ? O1 Tb1 C1 C2 -66(3) . . . . ? O8 Tb1 C1 C2 41(3) 3_655 . . . ? O5 Tb1 C1 C2 -162(3) . . . . ? O2 Tb1 C1 C2 121(3) . . . . ? C15 Tb1 C1 C2 -162(3) . . . . ? O2 C1 C2 C3 -172.2(5) . . . . ? O1 C1 C2 C3 9.5(8) . . . . ? Tb1 C1 C2 C3 71(3) . . . . ? O2 C1 C2 C7 13.8(8) . . . . ? O1 C1 C2 C7 -164.5(5) . . . . ? Tb1 C1 C2 C7 -103(3) . . . . ? C7 C2 C3 C4 -1.5(8) . . . . ? C1 C2 C3 C4 -175.6(5) . . . . ? C2 C3 C4 C5 1.6(9) . . . . ? C3 C4 C5 O3 -180.0(5) . . . . ? C3 C4 C5 C6 -1.2(9) . . . . ? O3 C5 C6 C7 179.6(5) . . . . ? C4 C5 C6 C7 0.7(9) . . . . ? C5 C6 C7 C2 -0.6(9) . . . . ? C3 C2 C7 C6 1.0(9) . . . . ? C1 C2 C7 C6 175.1(5) . . . . ? O3 C8 C9 C14 7.8(8) . . . . ? O3 C8 C9 C10 -171.6(5) . . . . ? C14 C9 C10 C11 0.3(9) . . . . ? C8 C9 C10 C11 179.8(6) . . . . ? C9 C10 C11 C12 -1.7(9) . . . . ? C10 C11 C12 C13 1.3(9) . . . . ? C11 C12 C13 C14 0.4(9) . . . . ? C10 C9 C14 C13 1.4(9) . . . . ? C8 C9 C14 C13 -178.0(6) . . . . ? C12 C13 C14 C9 -1.8(10) . . . . ? Tb1 O4 C15 O5 3.1(6) . . . . ? Tb1 O4 C15 C16 -175.1(4) . . . . ? Tb1 O5 C15 O4 -2.9(5) . . . . ? Tb1 O5 C15 C16 175.3(5) . . . . ? O7 Tb1 C15 O4 -101.2(3) . . . . ? O11 Tb1 C15 O4 104.4(3) . . . . ? O10 Tb1 C15 O4 -177.1(3) . . . . ? O1 Tb1 C15 O4 -30.5(4) . . . . ? O8 Tb1 C15 O4 94.2(5) 3_655 . . . ? O5 Tb1 C15 O4 177.0(5) . . . . ? O2 Tb1 C15 O4 24.1(3) . . . . ? C1 Tb1 C15 O4 -2.2(4) . . . . ? O7 Tb1 C15 O5 81.8(3) . . . . ? O11 Tb1 C15 O5 -72.6(3) . . . . ? O10 Tb1 C15 O5 6.0(3) . . . . ? O4 Tb1 C15 O5 -177.0(5) . . . . ? O1 Tb1 C15 O5 152.6(3) . . . . ? O8 Tb1 C15 O5 -82.8(5) 3_655 . . . ? O2 Tb1 C15 O5 -152.9(3) . . . . ? C1 Tb1 C15 O5 -179.2(3) . . . . ? O7 Tb1 C15 C16 -49(4) . . . . ? O11 Tb1 C15 C16 156(4) . . . . ? O10 Tb1 C15 C16 -125(4) . . . . ? O4 Tb1 C15 C16 52(4) . . . . ? O1 Tb1 C15 C16 21(5) . . . . ? O8 Tb1 C15 C16 146(4) 3_655 . . . ? O5 Tb1 C15 C16 -131(5) . . . . ? O2 Tb1 C15 C16 76(4) . . . . ? C1 Tb1 C15 C16 50(5) . . . . ? O4 C15 C16 C21 4.7(8) . . . . ? O5 C15 C16 C21 -173.5(5) . . . . ? Tb1 C15 C16 C21 -45(5) . . . . ? O4 C15 C16 C17 -178.2(5) . . . . ? O5 C15 C16 C17 3.6(8) . . . . ? Tb1 C15 C16 C17 133(4) . . . . ? C21 C16 C17 C18 1.4(9) . . . . ? C15 C16 C17 C18 -175.8(5) . . . . ? C16 C17 C18 C19 1.7(9) . . . . ? C17 C18 C19 O6 175.1(6) . . . . ? C17 C18 C19 C20 -3.3(9) . . . . ? O6 C19 C20 C21 -176.7(6) . . . . ? C18 C19 C20 C21 1.8(10) . . . . ? C19 C20 C21 C16 1.4(10) . . . . ? C17 C16 C21 C20 -3.0(9) . . . . ? C15 C16 C21 C20 174.2(6) . . . . ? O6 C22 C23 C28 106.3(7) . . . . ? O6 C22 C23 C24 -73.3(7) . . . . ? C28 C23 C24 C25 -0.1(10) . . . . ? C22 C23 C24 C25 179.5(6) . . . . ? C23 C24 C25 C26 -1.1(10) . . . . ? C24 C25 C26 C27 2.1(10) . . . . ? C25 C26 C27 C28 -1.9(11) . . . . ? C24 C23 C28 C27 0.3(10) . . . . ? C22 C23 C28 C27 -179.3(6) . . . . ? C26 C27 C28 C23 0.7(11) . . . . ? Tb1 O8 C29 O7 -11.7(7) 3_655 . . . ? Tb1 O8 C29 C30 169.9(3) 3_655 . . . ? Tb1 O7 C29 O8 145(4) . . . . ? Tb1 O7 C29 C30 -37(4) . . . . ? O8 C29 C30 C35 -166.2(5) . . . . ? O7 C29 C30 C35 15.4(8) . . . . ? O8 C29 C30 C31 15.3(8) . . . . ? O7 C29 C30 C31 -163.1(5) . . . . ? C35 C30 C31 C32 -1.2(8) . . . . ? C29 C30 C31 C32 177.4(5) . . . . ? C30 C31 C32 C33 0.1(9) . . . . ? C31 C32 C33 O9 -178.5(5) . . . . ? C31 C32 C33 C34 1.4(9) . . . . ? O9 C33 C34 C35 178.0(5) . . . . ? C32 C33 C34 C35 -1.8(9) . . . . ? C33 C34 C35 C30 0.7(9) . . . . ? C31 C30 C35 C34 0.8(8) . . . . ? C29 C30 C35 C34 -177.8(5) . . . . ? O9 C36 C37 C38 70.1(8) . . . . ? O9 C36 C37 C42 -108.9(7) . . . . ? C42 C37 C38 C39 -1.4(11) . . . . ? C36 C37 C38 C39 179.7(6) . . . . ? C37 C38 C39 C40 1.5(11) . . . . ? C38 C39 C40 C41 -0.9(12) . . . . ? C39 C40 C41 C42 0.3(13) . . . . ? C40 C41 C42 C37 -0.2(13) . . . . ? C38 C37 C42 C41 0.7(11) . . . . ? C36 C37 C42 C41 179.7(7) . . . . ? C4 C5 O3 C8 1.5(8) . . . . ? C6 C5 O3 C8 -177.3(5) . . . . ? C9 C8 O3 C5 169.3(5) . . . . ? C20 C19 O6 C22 169.0(5) . . . . ? C18 C19 O6 C22 -9.4(9) . . . . ? C23 C22 O6 C19 -163.9(5) . . . . ? C34 C33 O9 C36 -10.0(8) . . . . ? C32 C33 O9 C36 169.8(5) . . . . ? C37 C36 O9 C33 -168.5(5) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.146 _refine_diff_density_min -0.882 _refine_diff_density_rms 0.216 # Attachment 'sbkv168a_last.cif' data_sbkv168a _database_code_depnum_ccdc_archive 'CCDC 734105' _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C92 H94 O30 Tb2' _chemical_formula_sum 'C92 H94 O30 Tb2' _chemical_formula_weight 1997.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_space_group_name_Hall -p2ybc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 19.359(4) _cell_length_b 23.771(5) _cell_length_c 9.4710(19) _cell_angle_alpha 90.00 _cell_angle_beta 91.62(3) _cell_angle_gamma 90.00 _cell_volume 4356.6(15) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7250 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 25.03 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2032 _exptl_absorpt_coefficient_mu 1.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.904 _exptl_absorpt_correction_T_max 0.935 _exptl_absorpt_process_details 'Denzo and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14335 _diffrn_reflns_av_R_equivalents 0.0532 _diffrn_reflns_av_sigmaI/netI 0.0780 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 25.02 _reflns_number_total 7664 _reflns_number_gt 5414 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. A number of solvent hydrogen atoms are unable to be located due to the presence of the Tb atom. These missing H atoms gives rise to a number of related alerts in the checkcif file. Additionally, the structure formula is reported as that of the dimeric unit. As such, a number of related alerts are generated pertaining to the structural solution as a dimer versus that of the monomer. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0249P)^2^+22.0250P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7664 _refine_ls_number_parameters 544 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0913 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1100 _refine_ls_goodness_of_fit_ref 1.148 _refine_ls_restrained_S_all 1.148 _refine_ls_shift/su_max 0.028 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.4500(4) 0.8982(3) 0.7344(7) 0.0232(16) Uani 1 1 d . . . C2 C 0.4246(4) 0.8394(3) 0.7162(7) 0.0269(17) Uani 1 1 d . . . C3 C 0.3693(4) 0.8273(3) 0.6257(9) 0.0339(19) Uani 1 1 d . . . H3 H 0.3459 0.8563 0.5791 0.041 Uiso 1 1 calc R . . C4 C 0.3488(5) 0.7723(3) 0.6042(10) 0.042(2) Uani 1 1 d . . . H4 H 0.3114 0.7647 0.5432 0.051 Uiso 1 1 calc R . . C5 C 0.3821(5) 0.7293(3) 0.6702(10) 0.042(2) Uani 1 1 d . . . C6 C 0.4376(5) 0.7412(3) 0.7644(9) 0.0341(19) Uani 1 1 d . . . C7 C 0.4586(4) 0.7956(3) 0.7852(8) 0.0354(19) Uani 1 1 d . . . H7 H 0.4959 0.8032 0.8462 0.042 Uiso 1 1 calc R . . C8 C 0.5294(6) 0.7059(4) 0.9161(14) 0.079(4) Uani 1 1 d . . . H8A H 0.5655 0.7210 0.8598 0.118 Uiso 1 1 calc R . . H8B H 0.5448 0.6713 0.9589 0.118 Uiso 1 1 calc R . . H8C H 0.5182 0.7324 0.9884 0.118 Uiso 1 1 calc R . . C9 C 0.3196(6) 0.6563(4) 0.5382(15) 0.078(4) Uani 1 1 d . . . H9A H 0.3257 0.6166 0.5187 0.093 Uiso 1 1 calc R . . H9B H 0.3305 0.6768 0.4531 0.093 Uiso 1 1 calc R . . C10 C 0.2461(6) 0.6663(5) 0.5695(15) 0.069(3) Uani 1 1 d . . . C11 C 0.2245(9) 0.6551(5) 0.6995(16) 0.099(5) Uani 1 1 d . . . H11 H 0.2568 0.6464 0.7707 0.118 Uiso 1 1 calc R . . C12 C 0.1521(12) 0.6562(12) 0.731(3) 0.181(12) Uani 1 1 d . . . H12 H 0.1352 0.6436 0.8166 0.217 Uiso 1 1 calc R . . C13 C 0.1093(12) 0.6778(9) 0.623(3) 0.180(13) Uani 1 1 d . . . H13 H 0.0642 0.6866 0.6458 0.216 Uiso 1 1 calc R . . C14 C 0.1292(8) 0.6885(7) 0.470(3) 0.144(8) Uani 1 1 d . . . H14 H 0.0980 0.6977 0.3971 0.173 Uiso 1 1 calc R . . C15 C 0.2013(8) 0.6825(6) 0.454(2) 0.114(6) Uani 1 1 d . . . H15 H 0.2200 0.6893 0.3662 0.136 Uiso 1 1 calc R . . C16 C 0.3764(3) 1.0018(3) 1.0052(7) 0.0191(15) Uani 1 1 d . . . C17 C 0.3037(3) 0.9946(3) 0.9527(7) 0.0222(15) Uani 1 1 d . . . C18 C 0.2507(4) 0.9922(4) 1.0437(7) 0.0338(18) Uani 1 1 d . . . H18 H 0.2598 0.9972 1.1398 0.041 Uiso 1 1 calc R . . C19 C 0.1840(4) 0.9825(4) 0.9965(8) 0.044(2) Uani 1 1 d . . . H19 H 0.1482 0.9822 1.0600 0.053 Uiso 1 1 calc R . . C20 C 0.1702(4) 0.9731(4) 0.8531(8) 0.036(2) Uani 1 1 d . . . C21 C 0.2238(3) 0.9761(3) 0.7585(7) 0.0249(16) Uani 1 1 d . . . C22 C 0.2907(3) 0.9878(3) 0.8062(7) 0.0253(15) Uani 1 1 d . . . H22 H 0.3263 0.9912 0.7429 0.030 Uiso 1 1 calc R . . C23 C 0.2572(4) 0.9719(4) 0.5187(7) 0.0355(19) Uani 1 1 d . . . H23A H 0.2745 1.0098 0.5197 0.053 Uiso 1 1 calc R . . H23B H 0.2382 0.9633 0.4265 0.053 Uiso 1 1 calc R . . H23C H 0.2942 0.9463 0.5415 0.053 Uiso 1 1 calc R . . C24 C 0.0506(4) 0.9582(5) 0.8912(9) 0.052(3) Uani 1 1 d . . . H24A H 0.0473 0.9937 0.9411 0.063 Uiso 1 1 calc R . . H24B H 0.0584 0.9286 0.9602 0.063 Uiso 1 1 calc R . . C25 C -0.0155(4) 0.9472(4) 0.8080(9) 0.040(2) Uani 1 1 d . . . C26 C -0.0357(4) 0.9802(4) 0.6952(9) 0.041(2) Uani 1 1 d . . . H26 H -0.0072 1.0093 0.6666 0.049 Uiso 1 1 calc R . . C27 C -0.0975(4) 0.9707(4) 0.6241(9) 0.040(2) Uani 1 1 d . . . H27 H -0.1106 0.9933 0.5476 0.048 Uiso 1 1 calc R . . C28 C -0.1402(4) 0.9278(4) 0.6662(9) 0.045(2) Uani 1 1 d . . . H28 H -0.1817 0.9210 0.6175 0.054 Uiso 1 1 calc R . . C29 C -0.1213(4) 0.8953(4) 0.7796(10) 0.049(2) Uani 1 1 d . . . H29 H -0.1505 0.8669 0.8096 0.059 Uiso 1 1 calc R . . C30 C -0.0586(5) 0.9045(4) 0.8501(10) 0.051(2) Uani 1 1 d . . . H30 H -0.0456 0.8819 0.9263 0.061 Uiso 1 1 calc R . . C31 C 0.5952(3) 0.9339(3) 0.4918(7) 0.0195(15) Uani 1 1 d . . . C32 C 0.6470(3) 0.8919(3) 0.5429(7) 0.0193(15) Uani 1 1 d . . . C33 C 0.6870(4) 0.8636(3) 0.4493(8) 0.0286(18) Uani 1 1 d . . . H33 H 0.6835 0.8729 0.3540 0.034 Uiso 1 1 calc R . . C34 C 0.7325(4) 0.8213(3) 0.4926(7) 0.0284(17) Uani 1 1 d . . . H34 H 0.7593 0.8026 0.4275 0.034 Uiso 1 1 calc R . . C35 C 0.7372(4) 0.8077(3) 0.6358(7) 0.0253(16) Uani 1 1 d . . . C36 C 0.6963(4) 0.8360(3) 0.7315(7) 0.0258(16) Uani 1 1 d . . . C37 C 0.6533(4) 0.8784(3) 0.6880(7) 0.0266(17) Uani 1 1 d . . . H37 H 0.6282 0.8984 0.7537 0.032 Uiso 1 1 calc R . . C38 C 0.6659(5) 0.8462(4) 0.9742(8) 0.043(2) Uani 1 1 d . . . H38A H 0.6798 0.8849 0.9815 0.064 Uiso 1 1 calc R . . H38B H 0.6733 0.8280 1.0638 0.064 Uiso 1 1 calc R . . H38C H 0.6178 0.8443 0.9473 0.064 Uiso 1 1 calc R . . C39 C 0.8302(4) 0.7432(3) 0.5991(9) 0.0350(19) Uani 1 1 d . . . H39A H 0.8581 0.7728 0.5588 0.042 Uiso 1 1 calc R . . H39B H 0.8080 0.7221 0.5229 0.042 Uiso 1 1 calc R . . C40 C 0.8737(4) 0.7056(3) 0.6909(8) 0.0327(19) Uani 1 1 d . . . C41 C 0.8616(5) 0.6480(4) 0.6992(10) 0.046(2) Uani 1 1 d . . . H41 H 0.8266 0.6319 0.6433 0.055 Uiso 1 1 calc R . . C42 C 0.9005(6) 0.6144(4) 0.7886(11) 0.059(3) Uani 1 1 d . . . H42 H 0.8916 0.5760 0.7928 0.071 Uiso 1 1 calc R . . C43 C 0.9534(5) 0.6374(4) 0.8730(11) 0.055(3) Uani 1 1 d . . . H43 H 0.9796 0.6148 0.9340 0.066 Uiso 1 1 calc R . . C44 C 0.9660(5) 0.6939(4) 0.8646(10) 0.054(3) Uani 1 1 d . . . H44 H 1.0007 0.7097 0.9218 0.064 Uiso 1 1 calc R . . C45 C 0.9279(5) 0.7284(4) 0.7721(10) 0.048(2) Uani 1 1 d . . . H45 H 0.9386 0.7664 0.7646 0.058 Uiso 1 1 calc R . . O1 O 0.4262(2) 0.93670(18) 0.6546(4) 0.0208(10) Uani 1 1 d . . . O2 O 0.4970(2) 0.9094(2) 0.8261(5) 0.0252(11) Uani 1 1 d . . . O3 O 0.4690(3) 0.6953(2) 0.8275(7) 0.0533(17) Uani 1 1 d . . . O4 O 0.3692(3) 0.6729(2) 0.6515(7) 0.0500(16) Uani 1 1 d . . . O5 O 0.4242(2) 1.0065(2) 0.9199(5) 0.0244(11) Uani 1 1 d . . . O6 O 0.2046(3) 0.9666(2) 0.6203(5) 0.0361(13) Uani 1 1 d . . . O7 O 0.1065(3) 0.9601(3) 0.7960(5) 0.0427(15) Uani 1 1 d . . . O8 O 0.5639(2) 0.9637(2) 0.5790(5) 0.0248(11) Uani 1 1 d . . . O9 O 0.7054(3) 0.8188(2) 0.8709(5) 0.0334(13) Uani 1 1 d . . . O10 O 0.7793(3) 0.7667(2) 0.6913(5) 0.0312(12) Uani 1 1 d . . . O11 O 0.6127(2) 0.9982(2) 0.8630(4) 0.0257(11) Uani 1 1 d . . . O12 O 0.5718(3) 1.0794(2) 0.6259(5) 0.0293(12) Uani 1 1 d . . . O13 O 0.5129(3) 1.0970(2) 0.8879(5) 0.0291(12) Uani 1 1 d . . . O14 O 0.4165(3) 1.0621(2) 0.6399(5) 0.0262(11) Uani 1 1 d . . . Tb1 Tb 0.504773(17) 1.010061(13) 0.75012(4) 0.01892(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(4) 0.025(4) 0.021(4) -0.003(3) 0.009(3) 0.003(3) C2 0.032(4) 0.024(4) 0.025(4) 0.006(3) 0.007(3) -0.003(3) C3 0.030(5) 0.028(4) 0.043(5) 0.001(4) -0.001(4) -0.001(3) C4 0.041(5) 0.028(5) 0.058(6) -0.002(4) -0.010(4) -0.001(4) C5 0.042(5) 0.024(5) 0.059(6) -0.004(4) 0.014(4) -0.006(4) C6 0.045(5) 0.020(4) 0.037(5) 0.004(3) 0.007(4) 0.005(4) C7 0.047(5) 0.032(5) 0.027(4) -0.001(4) 0.004(4) 0.002(4) C8 0.072(8) 0.036(6) 0.127(11) 0.028(6) -0.030(7) 0.018(5) C9 0.053(7) 0.045(6) 0.135(11) -0.040(7) 0.000(7) -0.013(5) C10 0.050(7) 0.055(7) 0.103(10) -0.015(7) 0.012(7) -0.010(5) C11 0.120(13) 0.079(9) 0.101(10) -0.003(8) 0.066(9) -0.027(8) C12 0.098(18) 0.26(3) 0.18(2) -0.04(2) -0.002(16) 0.021(18) C13 0.128(19) 0.138(17) 0.28(3) -0.09(2) 0.14(2) -0.040(15) C14 0.044(9) 0.125(14) 0.26(3) -0.039(15) 0.000(12) 0.003(8) C15 0.076(11) 0.096(11) 0.170(17) -0.029(11) 0.004(11) -0.018(8) C16 0.020(3) 0.016(4) 0.021(4) 0.000(3) -0.004(3) -0.001(3) C17 0.020(3) 0.026(4) 0.020(3) 0.002(3) -0.002(3) -0.001(3) C18 0.025(4) 0.062(5) 0.013(3) 0.000(4) -0.001(3) -0.006(4) C19 0.023(4) 0.081(7) 0.028(4) -0.004(4) 0.005(3) -0.011(4) C20 0.020(4) 0.058(6) 0.029(4) 0.002(4) -0.006(3) -0.007(4) C21 0.018(4) 0.034(4) 0.022(4) 0.000(3) -0.004(3) -0.002(3) C22 0.024(4) 0.034(4) 0.018(3) -0.005(3) 0.000(3) -0.002(3) C23 0.025(4) 0.060(6) 0.021(4) -0.006(4) 0.000(3) 0.003(4) C24 0.023(5) 0.101(8) 0.033(5) -0.003(5) 0.005(4) -0.016(5) C25 0.022(4) 0.061(6) 0.036(4) -0.001(4) 0.001(3) -0.007(4) C26 0.031(4) 0.048(5) 0.046(5) -0.012(4) 0.003(4) -0.010(4) C27 0.032(5) 0.048(5) 0.041(5) -0.001(4) -0.005(4) -0.003(4) C28 0.025(5) 0.055(6) 0.053(6) -0.017(5) -0.011(4) 0.003(4) C29 0.028(5) 0.057(6) 0.062(6) 0.007(5) -0.006(4) -0.008(4) C30 0.037(5) 0.070(7) 0.047(5) 0.012(5) -0.005(4) 0.000(5) C31 0.020(4) 0.018(4) 0.020(4) -0.002(3) -0.001(3) -0.005(3) C32 0.021(4) 0.021(4) 0.016(3) -0.002(3) 0.000(3) 0.001(3) C33 0.028(4) 0.033(4) 0.025(4) 0.004(3) -0.006(3) 0.006(3) C34 0.031(4) 0.031(4) 0.023(4) -0.004(3) 0.003(3) 0.006(3) C35 0.021(4) 0.026(4) 0.029(4) 0.001(3) -0.001(3) 0.004(3) C36 0.023(4) 0.030(4) 0.024(4) 0.001(3) 0.000(3) 0.005(3) C37 0.032(4) 0.029(4) 0.018(4) -0.004(3) -0.005(3) 0.006(3) C38 0.054(6) 0.050(5) 0.024(4) -0.002(4) 0.000(4) 0.024(4) C39 0.028(5) 0.037(5) 0.040(5) 0.000(4) 0.008(4) 0.015(4) C40 0.032(5) 0.037(5) 0.030(4) -0.003(4) 0.012(3) 0.015(4) C41 0.044(6) 0.045(6) 0.049(6) 0.006(4) 0.000(4) 0.005(4) C42 0.066(7) 0.040(6) 0.070(7) 0.011(5) -0.008(6) 0.020(5) C43 0.050(6) 0.055(6) 0.059(6) 0.020(5) -0.003(5) 0.020(5) C44 0.036(5) 0.067(7) 0.057(6) 0.012(5) -0.008(4) 0.011(5) C45 0.037(5) 0.043(5) 0.063(6) 0.001(5) -0.006(5) 0.009(4) O1 0.026(3) 0.022(3) 0.015(2) 0.002(2) -0.0008(19) 0.002(2) O2 0.027(3) 0.030(3) 0.018(2) 0.007(2) 0.000(2) -0.002(2) O3 0.059(4) 0.025(3) 0.075(4) 0.004(3) -0.002(3) 0.010(3) O4 0.049(4) 0.024(3) 0.077(5) -0.006(3) 0.007(3) -0.006(3) O5 0.017(2) 0.036(3) 0.020(2) 0.001(2) 0.0035(18) -0.001(2) O6 0.023(3) 0.065(4) 0.019(3) -0.005(3) -0.005(2) -0.004(3) O7 0.019(3) 0.081(4) 0.029(3) -0.010(3) 0.002(2) -0.008(3) O8 0.030(3) 0.027(3) 0.018(2) 0.001(2) 0.001(2) 0.005(2) O9 0.041(3) 0.042(3) 0.017(3) 0.008(2) -0.001(2) 0.019(3) O10 0.031(3) 0.038(3) 0.026(3) 0.005(2) 0.006(2) 0.012(2) O11 0.023(2) 0.042(3) 0.012(2) 0.000(2) -0.0020(18) 0.002(2) O12 0.039(3) 0.029(3) 0.020(3) 0.000(2) 0.002(2) -0.008(2) O13 0.043(3) 0.031(3) 0.013(2) -0.002(2) 0.002(2) -0.001(2) O14 0.033(3) 0.031(3) 0.014(2) -0.002(2) -0.003(2) 0.010(2) Tb1 0.02132(18) 0.02071(17) 0.01469(16) 0.00031(18) -0.00019(11) 0.00124(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.265(8) . ? C1 O2 1.269(8) . ? C1 C2 1.489(10) . ? C1 Tb1 2.865(7) . ? C2 C3 1.383(11) . ? C2 C7 1.386(11) . ? C3 C4 1.379(11) . ? C3 H3 0.9300 . ? C4 C5 1.353(12) . ? C4 H4 0.9300 . ? C5 O4 1.375(9) . ? C5 C6 1.406(12) . ? C6 C7 1.367(11) . ? C6 O3 1.378(9) . ? C7 H7 0.9300 . ? C8 O3 1.442(12) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 O4 1.473(13) . ? C9 C10 1.481(16) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.338(17) . ? C10 C15 1.43(2) . ? C11 C12 1.44(3) . ? C11 H11 0.9300 . ? C12 C13 1.40(3) . ? C12 H12 0.9300 . ? C13 C14 1.53(3) . ? C13 H13 0.9300 . ? C14 C15 1.42(2) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 O5 1.250(8) . ? C16 O11 1.260(8) 3_677 ? C16 C17 1.489(9) . ? C17 C18 1.360(10) . ? C17 C22 1.412(9) . ? C18 C19 1.375(10) . ? C18 H18 0.9300 . ? C19 C20 1.395(11) . ? C19 H19 0.9300 . ? C20 O7 1.368(8) . ? C20 C21 1.393(10) . ? C21 O6 1.369(8) . ? C21 C22 1.387(9) . ? C22 H22 0.9300 . ? C23 O6 1.425(9) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 O7 1.429(10) . ? C24 C25 1.507(11) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.373(12) . ? C25 C30 1.379(12) . ? C26 C27 1.376(11) . ? C26 H26 0.9300 . ? C27 C28 1.379(12) . ? C27 H27 0.9300 . ? C28 C29 1.364(12) . ? C28 H28 0.9300 . ? C29 C30 1.385(12) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 O8 1.258(8) . ? C31 O14 1.265(8) 3_676 ? C31 C32 1.486(9) . ? C32 C33 1.370(10) . ? C32 C37 1.413(9) . ? C33 C34 1.390(10) . ? C33 H33 0.9300 . ? C34 C35 1.395(10) . ? C34 H34 0.9300 . ? C35 O10 1.365(8) . ? C35 C36 1.393(10) . ? C36 C37 1.364(10) . ? C36 O9 1.388(8) . ? C37 H37 0.9300 . ? C38 O9 1.417(9) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 O10 1.448(9) . ? C39 C40 1.492(11) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 C41 1.392(12) . ? C40 C45 1.393(12) . ? C41 C42 1.374(12) . ? C41 H41 0.9300 . ? C42 C43 1.393(14) . ? C42 H42 0.9300 . ? C43 C44 1.368(13) . ? C43 H43 0.9300 . ? C44 C45 1.396(12) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? O1 Tb1 2.469(4) . ? O2 Tb1 2.504(5) . ? O5 Tb1 2.273(4) . ? O8 Tb1 2.292(5) . ? O11 C16 1.260(8) 3_677 ? O11 Tb1 2.337(4) . ? O12 Tb1 2.423(5) . ? O13 Tb1 2.446(5) . ? O14 C31 1.265(8) 3_676 ? O14 Tb1 2.332(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 119.9(6) . . ? O1 C1 C2 119.8(6) . . ? O2 C1 C2 120.3(6) . . ? O1 C1 Tb1 59.2(3) . . ? O2 C1 Tb1 60.8(3) . . ? C2 C1 Tb1 175.6(5) . . ? C3 C2 C7 118.9(7) . . ? C3 C2 C1 120.9(7) . . ? C7 C2 C1 120.0(7) . . ? C4 C3 C2 120.3(7) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.1(8) . . ? C5 C4 H4 119.4 . . ? C3 C4 H4 119.5 . . ? C4 C5 O4 126.5(9) . . ? C4 C5 C6 119.1(7) . . ? O4 C5 C6 114.3(8) . . ? C7 C6 O3 124.1(8) . . ? C7 C6 C5 120.0(7) . . ? O3 C6 C5 115.8(7) . . ? C6 C7 C2 120.5(8) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 C10 114.9(10) . . ? O4 C9 H9A 108.5 . . ? C10 C9 H9A 108.5 . . ? O4 C9 H9B 108.5 . . ? C10 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? C11 C10 C15 124.0(14) . . ? C11 C10 C9 118.6(14) . . ? C15 C10 C9 117.1(13) . . ? C10 C11 C12 121.2(19) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 114(3) . . ? C13 C12 H12 122.8 . . ? C11 C12 H12 122.8 . . ? C12 C13 C14 127(2) . . ? C12 C13 H13 116.7 . . ? C14 C13 H13 116.6 . . ? C15 C14 C13 111.1(19) . . ? C15 C14 H14 124.4 . . ? C13 C14 H14 124.5 . . ? C14 C15 C10 121.6(18) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? O5 C16 O11 122.3(6) . 3_677 ? O5 C16 C17 120.2(6) . . ? O11 C16 C17 117.5(6) 3_677 . ? C18 C17 C22 120.1(6) . . ? C18 C17 C16 121.1(6) . . ? C22 C17 C16 118.8(6) . . ? C17 C18 C19 121.3(6) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C19 C20 119.7(7) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? O7 C20 C21 115.9(6) . . ? O7 C20 C19 124.6(7) . . ? C21 C20 C19 119.5(6) . . ? O6 C21 C22 124.8(6) . . ? O6 C21 C20 114.8(6) . . ? C22 C21 C20 120.4(6) . . ? C21 C22 C17 118.8(6) . . ? C21 C22 H22 120.6 . . ? C17 C22 H22 120.6 . . ? O6 C23 H23A 109.5 . . ? O6 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O6 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O7 C24 C25 108.8(7) . . ? O7 C24 H24A 109.9 . . ? C25 C24 H24A 109.9 . . ? O7 C24 H24B 109.9 . . ? C25 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C26 C25 C30 118.9(7) . . ? C26 C25 C24 121.8(8) . . ? C30 C25 C24 119.3(8) . . ? C25 C26 C27 120.8(8) . . ? C25 C26 H26 119.6 . . ? C27 C26 H26 119.6 . . ? C26 C27 C28 119.9(8) . . ? C26 C27 H27 120.0 . . ? C28 C27 H27 120.0 . . ? C29 C28 C27 119.8(8) . . ? C29 C28 H28 120.1 . . ? C27 C28 H28 120.1 . . ? C28 C29 C30 120.1(9) . . ? C28 C29 H29 119.9 . . ? C30 C29 H29 119.9 . . ? C25 C30 C29 120.4(9) . . ? C25 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? O8 C31 O14 121.9(6) . 3_676 ? O8 C31 C32 119.9(6) . . ? O14 C31 C32 118.2(6) 3_676 . ? C33 C32 C37 118.8(6) . . ? C33 C32 C31 120.5(6) . . ? C37 C32 C31 120.6(6) . . ? C32 C33 C34 122.0(7) . . ? C32 C33 H33 119.0 . . ? C34 C33 H33 119.0 . . ? C33 C34 C35 118.5(7) . . ? C33 C34 H34 120.7 . . ? C35 C34 H34 120.7 . . ? O10 C35 C36 115.9(6) . . ? O10 C35 C34 124.2(6) . . ? C36 C35 C34 119.9(6) . . ? C37 C36 O9 124.3(6) . . ? C37 C36 C35 120.9(6) . . ? O9 C36 C35 114.8(6) . . ? C36 C37 C32 119.8(7) . . ? C36 C37 H37 120.1 . . ? C32 C37 H37 120.1 . . ? O9 C38 H38A 109.5 . . ? O9 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? O9 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? O10 C39 C40 105.2(6) . . ? O10 C39 H39A 110.7 . . ? C40 C39 H39A 110.7 . . ? O10 C39 H39B 110.7 . . ? C40 C39 H39B 110.7 . . ? H39A C39 H39B 108.8 . . ? C41 C40 C45 118.6(8) . . ? C41 C40 C39 122.0(8) . . ? C45 C40 C39 119.4(7) . . ? C42 C41 C40 121.1(9) . . ? C42 C41 H41 119.5 . . ? C40 C41 H41 119.5 . . ? C41 C42 C43 120.4(9) . . ? C41 C42 H42 119.8 . . ? C43 C42 H42 119.8 . . ? C44 C43 C42 118.9(8) . . ? C44 C43 H43 120.6 . . ? C42 C43 H43 120.6 . . ? C43 C44 C45 121.4(9) . . ? C43 C44 H44 119.3 . . ? C45 C44 H44 119.3 . . ? C40 C45 C44 119.6(9) . . ? C40 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C1 O1 Tb1 94.7(4) . . ? C1 O2 Tb1 93.0(4) . . ? C6 O3 C8 117.0(7) . . ? C5 O4 C9 117.8(8) . . ? C16 O5 Tb1 174.5(4) . . ? C21 O6 C23 116.8(5) . . ? C20 O7 C24 116.6(6) . . ? C31 O8 Tb1 174.3(4) . . ? C36 O9 C38 117.8(5) . . ? C35 O10 C39 116.9(6) . . ? C16 O11 Tb1 125.1(4) 3_677 . ? C31 O14 Tb1 126.1(4) 3_676 . ? O5 Tb1 O8 148.06(18) . . ? O5 Tb1 O14 80.06(16) . . ? O8 Tb1 O14 108.20(16) . . ? O5 Tb1 O11 107.12(15) . . ? O8 Tb1 O11 78.92(16) . . ? O14 Tb1 O11 154.57(17) . . ? O5 Tb1 O12 139.11(17) . . ? O8 Tb1 O12 72.48(17) . . ? O14 Tb1 O12 79.48(17) . . ? O11 Tb1 O12 79.65(17) . . ? O5 Tb1 O13 71.90(17) . . ? O8 Tb1 O13 139.19(17) . . ? O14 Tb1 O13 80.00(16) . . ? O11 Tb1 O13 79.31(17) . . ? O12 Tb1 O13 69.93(16) . . ? O5 Tb1 O1 78.75(16) . . ? O8 Tb1 O1 73.53(16) . . ? O14 Tb1 O1 76.95(16) . . ? O11 Tb1 O1 128.04(16) . . ? O12 Tb1 O1 129.46(15) . . ? O13 Tb1 O1 145.25(17) . . ? O5 Tb1 O2 73.35(16) . . ? O8 Tb1 O2 77.25(16) . . ? O14 Tb1 O2 125.87(17) . . ? O11 Tb1 O2 79.25(16) . . ? O12 Tb1 O2 145.79(17) . . ? O13 Tb1 O2 131.09(15) . . ? O1 Tb1 O2 52.34(14) . . ? O5 Tb1 C1 75.06(18) . . ? O8 Tb1 C1 73.06(18) . . ? O14 Tb1 C1 101.73(19) . . ? O11 Tb1 C1 103.69(19) . . ? O12 Tb1 C1 143.97(18) . . ? O13 Tb1 C1 146.09(18) . . ? O1 Tb1 C1 26.12(17) . . ? O2 Tb1 C1 26.24(17) . . ? 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 O1 C1 C2 C3 -8.2(11) . . . . ? O2 C1 C2 C3 174.2(7) . . . . ? Tb1 C1 C2 C3 -83(7) . . . . ? O1 C1 C2 C7 168.7(7) . . . . ? O2 C1 C2 C7 -9.0(11) . . . . ? Tb1 C1 C2 C7 94(7) . . . . ? C7 C2 C3 C4 -0.4(12) . . . . ? C1 C2 C3 C4 176.5(8) . . . . ? C2 C3 C4 C5 -0.2(14) . . . . ? C3 C4 C5 O4 -176.0(9) . . . . ? C3 C4 C5 C6 1.3(14) . . . . ? C4 C5 C6 C7 -1.8(13) . . . . ? O4 C5 C6 C7 175.8(8) . . . . ? C4 C5 C6 O3 -180.0(8) . . . . ? O4 C5 C6 O3 -2.3(12) . . . . ? O3 C6 C7 C2 179.3(8) . . . . ? C5 C6 C7 C2 1.3(12) . . . . ? C3 C2 C7 C6 -0.2(12) . . . . ? C1 C2 C7 C6 -177.0(7) . . . . ? O4 C9 C10 C11 -40.6(15) . . . . ? O4 C9 C10 C15 145.1(11) . . . . ? C15 C10 C11 C12 3(2) . . . . ? C9 C10 C11 C12 -171.1(16) . . . . ? C10 C11 C12 C13 -9(3) . . . . ? C11 C12 C13 C14 13(4) . . . . ? C12 C13 C14 C15 -10(3) . . . . ? C13 C14 C15 C10 2(2) . . . . ? C11 C10 C15 C14 1(2) . . . . ? C9 C10 C15 C14 174.6(12) . . . . ? O5 C16 C17 C18 -176.6(7) . . . . ? O11 C16 C17 C18 4.5(10) 3_677 . . . ? O5 C16 C17 C22 6.1(10) . . . . ? O11 C16 C17 C22 -172.7(6) 3_677 . . . ? C22 C17 C18 C19 0.8(13) . . . . ? C16 C17 C18 C19 -176.4(8) . . . . ? C17 C18 C19 C20 2.1(14) . . . . ? C18 C19 C20 O7 176.4(8) . . . . ? C18 C19 C20 C21 -2.8(14) . . . . ? O7 C20 C21 O6 1.1(11) . . . . ? C19 C20 C21 O6 -179.6(8) . . . . ? O7 C20 C21 C22 -178.7(7) . . . . ? C19 C20 C21 C22 0.6(12) . . . . ? O6 C21 C22 C17 -177.5(7) . . . . ? C20 C21 C22 C17 2.3(11) . . . . ? C18 C17 C22 C21 -3.0(11) . . . . ? C16 C17 C22 C21 174.3(6) . . . . ? O7 C24 C25 C26 -53.9(12) . . . . ? O7 C24 C25 C30 129.4(9) . . . . ? C30 C25 C26 C27 -0.7(13) . . . . ? C24 C25 C26 C27 -177.4(8) . . . . ? C25 C26 C27 C28 0.2(13) . . . . ? C26 C27 C28 C29 0.9(13) . . . . ? C27 C28 C29 C30 -1.6(14) . . . . ? C26 C25 C30 C29 0.0(14) . . . . ? C24 C25 C30 C29 176.8(9) . . . . ? C28 C29 C30 C25 1.1(15) . . . . ? O8 C31 C32 C33 -172.7(7) . . . . ? O14 C31 C32 C33 8.0(10) 3_676 . . . ? O8 C31 C32 C37 10.7(10) . . . . ? O14 C31 C32 C37 -168.7(6) 3_676 . . . ? C37 C32 C33 C34 1.2(11) . . . . ? C31 C32 C33 C34 -175.5(7) . . . . ? C32 C33 C34 C35 0.1(11) . . . . ? C33 C34 C35 O10 179.3(7) . . . . ? C33 C34 C35 C36 0.4(11) . . . . ? O10 C35 C36 C37 178.7(7) . . . . ? C34 C35 C36 C37 -2.3(11) . . . . ? O10 C35 C36 O9 1.0(9) . . . . ? C34 C35 C36 O9 -180.0(7) . . . . ? O9 C36 C37 C32 -178.9(7) . . . . ? C35 C36 C37 C32 3.6(11) . . . . ? C33 C32 C37 C36 -3.1(11) . . . . ? C31 C32 C37 C36 173.7(6) . . . . ? O10 C39 C40 C41 96.1(9) . . . . ? O10 C39 C40 C45 -83.3(9) . . . . ? C45 C40 C41 C42 2.1(13) . . . . ? C39 C40 C41 C42 -177.4(8) . . . . ? C40 C41 C42 C43 -0.1(16) . . . . ? C41 C42 C43 C44 -0.4(16) . . . . ? C42 C43 C44 C45 -1.0(16) . . . . ? C41 C40 C45 C44 -3.4(13) . . . . ? C39 C40 C45 C44 176.1(8) . . . . ? C43 C44 C45 C40 3.0(15) . . . . ? O2 C1 O1 Tb1 2.5(7) . . . . ? C2 C1 O1 Tb1 -175.1(6) . . . . ? O1 C1 O2 Tb1 -2.5(7) . . . . ? C2 C1 O2 Tb1 175.1(6) . . . . ? C7 C6 O3 C8 -2.7(13) . . . . ? C5 C6 O3 C8 175.3(9) . . . . ? C4 C5 O4 C9 7.0(14) . . . . ? C6 C5 O4 C9 -170.4(8) . . . . ? C10 C9 O4 C5 -75.0(13) . . . . ? O11 C16 O5 Tb1 149(4) 3_677 . . . ? C17 C16 O5 Tb1 -29(5) . . . . ? C22 C21 O6 C23 -3.2(11) . . . . ? C20 C21 O6 C23 177.0(7) . . . . ? C21 C20 O7 C24 -178.5(8) . . . . ? C19 C20 O7 C24 2.2(13) . . . . ? C25 C24 O7 C20 176.3(8) . . . . ? O14 C31 O8 Tb1 131(4) 3_676 . . . ? C32 C31 O8 Tb1 -48(5) . . . . ? C37 C36 O9 C38 1.8(11) . . . . ? C35 C36 O9 C38 179.4(7) . . . . ? C36 C35 O10 C39 -170.1(7) . . . . ? C34 C35 O10 C39 10.9(10) . . . . ? C40 C39 O10 C35 173.3(6) . . . . ? C16 O5 Tb1 O8 -41(5) . . . . ? C16 O5 Tb1 O14 67(5) . . . . ? C16 O5 Tb1 O11 -138(5) . . . . ? C16 O5 Tb1 O12 128(5) . . . . ? C16 O5 Tb1 O13 150(5) . . . . ? C16 O5 Tb1 O1 -11(5) . . . . ? C16 O5 Tb1 O2 -65(5) . . . . ? C16 O5 Tb1 C1 -38(5) . . . . ? C31 O8 Tb1 O5 -25(5) . . . . ? C31 O8 Tb1 O14 -125(4) . . . . ? C31 O8 Tb1 O11 80(4) . . . . ? C31 O8 Tb1 O12 162(4) . . . . ? C31 O8 Tb1 O13 139(4) . . . . ? C31 O8 Tb1 O1 -56(4) . . . . ? C31 O8 Tb1 O2 -2(4) . . . . ? C31 O8 Tb1 C1 -28(4) . . . . ? C31 O14 Tb1 O5 -150.9(5) 3_676 . . . ? C31 O14 Tb1 O8 -2.8(6) 3_676 . . . ? C31 O14 Tb1 O11 99.9(6) 3_676 . . . ? C31 O14 Tb1 O12 64.6(5) 3_676 . . . ? C31 O14 Tb1 O13 135.9(6) 3_676 . . . ? C31 O14 Tb1 O1 -70.3(5) 3_676 . . . ? C31 O14 Tb1 O2 -90.0(6) 3_676 . . . ? C31 O14 Tb1 C1 -78.6(5) 3_676 . . . ? C16 O11 Tb1 O5 -9.3(5) 3_677 . . . ? C16 O11 Tb1 O8 -157.0(5) 3_677 . . . ? C16 O11 Tb1 O14 93.8(6) 3_677 . . . ? C16 O11 Tb1 O12 129.1(5) 3_677 . . . ? C16 O11 Tb1 O13 57.8(5) 3_677 . . . ? C16 O11 Tb1 O1 -98.3(5) 3_677 . . . ? C16 O11 Tb1 O2 -78.0(5) 3_677 . . . ? C16 O11 Tb1 C1 -87.6(5) 3_677 . . . ? C1 O1 Tb1 O5 -79.0(4) . . . . ? C1 O1 Tb1 O8 85.0(4) . . . . ? C1 O1 Tb1 O14 -161.2(4) . . . . ? C1 O1 Tb1 O11 24.1(4) . . . . ? C1 O1 Tb1 O12 134.5(4) . . . . ? C1 O1 Tb1 O13 -111.5(4) . . . . ? C1 O1 Tb1 O2 -1.4(4) . . . . ? C1 O2 Tb1 O5 89.9(4) . . . . ? C1 O2 Tb1 O8 -77.5(4) . . . . ? C1 O2 Tb1 O14 25.9(5) . . . . ? C1 O2 Tb1 O11 -158.4(4) . . . . ? C1 O2 Tb1 O12 -105.6(4) . . . . ? C1 O2 Tb1 O13 136.2(4) . . . . ? C1 O2 Tb1 O1 1.4(4) . . . . ? O1 C1 Tb1 O5 94.9(4) . . . . ? O2 C1 Tb1 O5 -82.6(4) . . . . ? C2 C1 Tb1 O5 172(7) . . . . ? O1 C1 Tb1 O8 -87.0(4) . . . . ? O2 C1 Tb1 O8 95.5(4) . . . . ? C2 C1 Tb1 O8 -10(7) . . . . ? O1 C1 Tb1 O14 18.7(4) . . . . ? O2 C1 Tb1 O14 -158.8(4) . . . . ? C2 C1 Tb1 O14 96(7) . . . . ? O1 C1 Tb1 O11 -160.7(4) . . . . ? O2 C1 Tb1 O11 21.8(4) . . . . ? C2 C1 Tb1 O11 -83(7) . . . . ? O1 C1 Tb1 O12 -69.5(5) . . . . ? O2 C1 Tb1 O12 113.0(4) . . . . ? C2 C1 Tb1 O12 8(7) . . . . ? O1 C1 Tb1 O13 108.1(4) . . . . ? O2 C1 Tb1 O13 -69.3(5) . . . . ? C2 C1 Tb1 O13 -175(7) . . . . ? O2 C1 Tb1 O1 -177.5(7) . . . . ? C2 C1 Tb1 O1 77(7) . . . . ? O1 C1 Tb1 O2 177.5(7) . . . . ? C2 C1 Tb1 O2 -105(7) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.021 _refine_diff_density_min -0.870 _refine_diff_density_rms 0.137