# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2004 data_global1 _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Ana de Bettencourt-Dias' _publ_contact_author_address ;Department of Chemistry Syracuse University Syracuse, NY 13244-4100 ; _publ_contact_author_email debetten@syr.edu _publ_contact_author_phone 1(315)4432006 _publ_contact_author_fax 1(315)4434070 loop_ _publ_author_name 'de Bettencourt-Dias,A.' S.Viswanathan _publ_section_title ; Luminescent Ln3+ nitrobenzoato complexes: first examples of sensitization of green and red emission ; data_p1bar_1 _database_code_depnum_ccdc_archive 'CCDC 224937' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H53 Eu2 N6 O32.50 S6' _chemical_formula_weight 1946.42 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.372(2) _cell_length_b 17.016(3) _cell_length_c 20.126(4) _cell_angle_alpha 112.99(3) _cell_angle_beta 96.74(3) _cell_angle_gamma 90.22(3) _cell_volume 3555.3(12) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 9543 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 32.73 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.818 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1946 _exptl_absorpt_coefficient_mu 2.023 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4984 _exptl_absorpt_correction_T_max 0.8233 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'APEX CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 35649 _diffrn_reflns_av_R_equivalents 0.0259 _diffrn_reflns_av_sigmaI/netI 0.0390 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.30 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16245 _reflns_number_gt 13977 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0474P)^2^+18.1622P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16245 _refine_ls_number_parameters 1002 _refine_ls_number_restraints 20 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0462 _refine_ls_wR_factor_ref 0.1168 _refine_ls_wR_factor_gt 0.1121 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.002 _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 S2A S 0.2843(5) 0.6436(4) 0.9195(3) 0.0323(5) Uani 0.300(5) 1 d PD A 1 C12A C 0.2058(16) 0.6296(12) 0.8315(8) 0.0206(7) Uani 0.300(5) 1 d PD A 1 H12A H 0.1382 0.6592 0.8239 0.025 Uiso 0.300(5) 1 calc PR A 1 C13A C 0.3728(17) 0.5642(13) 0.8787(10) 0.0206(7) Uani 0.300(5) 1 d PD A 1 H13A H 0.4331 0.5451 0.9048 0.025 Uiso 0.300(5) 1 calc PR A 1 C14A C 0.3491(4) 0.5300(3) 0.8043(3) 0.0206(7) Uani 0.300(5) 1 d PD A 1 C15A C 0.2574(15) 0.5719(12) 0.7795(10) 0.0206(7) Uani 0.300(5) 1 d PD A 1 H15A H 0.2347 0.5595 0.7293 0.025 Uiso 0.300(5) 1 calc PR A 1 S2B S 0.19144(19) 0.63739(15) 0.85508(13) 0.0323(5) Uani 0.700(5) 1 d PD A 2 C12B C 0.3124(7) 0.6338(6) 0.9168(5) 0.0206(7) Uani 0.700(5) 1 d PD A 2 H12B H 0.3240 0.6675 0.9676 0.025 Uiso 0.700(5) 1 calc PR A 2 C13B C 0.2415(7) 0.5577(5) 0.7850(5) 0.0206(7) Uani 0.700(5) 1 d PD A 2 H13B H 0.1998 0.5342 0.7372 0.025 Uiso 0.700(5) 1 calc PR A 2 C14B C 0.3491(4) 0.5300(3) 0.8043(3) 0.0206(7) Uani 0.700(5) 1 d PD A 2 C15B C 0.3864(8) 0.5750(6) 0.8797(5) 0.0206(7) Uani 0.700(5) 1 d PD A 2 H15B H 0.4589 0.5646 0.9028 0.025 Uiso 0.700(5) 1 calc PR A 2 S6A S 1.2950(3) -0.1171(3) 0.18507(12) 0.0272(6) Uani 0.778(5) 1 d PD B 1 C56A C 1.1905(7) -0.1158(5) 0.1152(4) 0.0176(6) Uani 0.778(5) 1 d PD B 1 H56A H 1.1873 -0.1525 0.0652 0.021 Uiso 0.778(5) 1 calc PR B 1 C57A C 1.1135(7) -0.0531(4) 0.1439(4) 0.0176(6) Uani 0.778(5) 1 d PD B 1 H57A H 1.0485 -0.0422 0.1150 0.021 Uiso 0.778(5) 1 calc PR B 1 C58A C 1.1384(4) -0.0058(3) 0.2202(2) 0.0176(6) Uani 0.778(5) 1 d PD B 1 C59A C 1.2367(7) -0.0320(4) 0.2503(4) 0.0176(6) Uani 0.778(5) 1 d PD B 1 H59A H 1.2686 -0.0068 0.3002 0.021 Uiso 0.778(5) 1 calc PR B 1 S6B S 1.2168(6) -0.1202(5) 0.1086(4) 0.0272(6) Uani 0.222(5) 1 d PD B 2 C56B C 1.281(4) -0.112(3) 0.1937(12) 0.0176(6) Uani 0.222(5) 1 d PD B 2 H56B H 1.3430 -0.1457 0.2028 0.021 Uiso 0.222(5) 1 calc PR B 2 C57B C 1.228(2) -0.0494(14) 0.2456(12) 0.0176(6) Uani 0.222(5) 1 d PD B 2 H57B H 1.2499 -0.0356 0.2961 0.021 Uiso 0.222(5) 1 calc PR B 2 C58B C 1.1384(4) -0.0058(3) 0.2202(2) 0.0176(6) Uani 0.222(5) 1 d PD B 2 C59B C 1.122(2) -0.0394(14) 0.1449(10) 0.0176(6) Uani 0.222(5) 1 d PD B 2 H59B H 1.0661 -0.0203 0.1165 0.021 Uiso 0.222(5) 1 calc PR B 2 N2 N 0.6816(4) 0.3392(3) 0.7667(2) 0.0259(9) Uani 1 1 d . A . O5 O 0.7532(4) 0.2985(3) 0.7269(2) 0.0353(7) Uani 1 1 d . . . O6 O 0.6901(4) 0.3544(3) 0.8321(2) 0.0353(7) Uani 1 1 d . . . Eu1 Eu 0.736747(19) 0.383334(13) 0.512611(11) 0.01278(6) Uani 1 1 d . . . Eu2 Eu 0.722415(19) 0.138572(14) 0.489389(11) 0.01408(6) Uani 1 1 d . . . S1 S 0.16197(14) 0.06168(10) -0.00683(8) 0.0348(3) Uani 1 1 d . . . S3 S 0.42398(14) 0.88103(10) 0.99700(9) 0.0400(4) Uani 1 1 d . . . S4 S 1.32531(14) 0.44579(10) 0.99753(7) 0.0339(3) Uani 1 1 d . . . S5 S 1.09233(15) -0.36964(11) 0.03792(9) 0.0414(4) Uani 1 1 d . . . C1 C 0.2271(4) 0.1301(3) 0.1310(2) 0.0160(9) Uani 1 1 d . . . C2 C 0.0592(4) 0.1208(3) 0.0426(2) 0.0174(9) Uani 1 1 d . . . H2 H -0.0181 0.1293 0.0239 0.021 Uiso 1 1 calc R . . C3 C 0.1103(4) 0.1563(3) 0.1189(3) 0.0207(9) Uani 1 1 d . . . H3 H 0.0697 0.1932 0.1569 0.025 Uiso 1 1 calc R . . C4 C 0.2656(5) 0.0786(3) 0.0663(3) 0.0221(10) Uani 1 1 d . . . H4 H 0.3415 0.0552 0.0628 0.027 Uiso 1 1 calc R . . C5 C 0.2983(4) 0.1532(3) 0.2030(2) 0.0153(8) Uani 1 1 d . . . C6 C 0.2581(4) 0.2144(3) 0.2646(2) 0.0161(8) Uani 1 1 d . . . H6 H 0.1859 0.2409 0.2601 0.019 Uiso 1 1 calc R . . C7 C 0.3246(4) 0.2360(3) 0.3320(2) 0.0152(8) Uani 1 1 d . . . C8 C 0.4318(4) 0.2015(3) 0.3424(2) 0.0143(8) Uani 1 1 d . . . C9 C 0.4691(4) 0.1383(3) 0.2809(2) 0.0170(9) Uani 1 1 d . . . H9 H 0.5406 0.1112 0.2857 0.020 Uiso 1 1 calc R . . C10 C 0.4031(4) 0.1146(3) 0.2130(2) 0.0164(9) Uani 1 1 d . . . H10 H 0.4300 0.0711 0.1722 0.020 Uiso 1 1 calc R . . C11 C 0.5150(4) 0.2317(3) 0.4131(2) 0.0150(8) Uani 1 1 d . . . C16 C 0.4159(4) 0.4629(3) 0.7549(2) 0.0178(9) Uani 1 1 d . . . C17 C 0.5159(4) 0.4328(3) 0.7818(2) 0.0189(9) Uani 1 1 d . A . H17 H 0.5412 0.4550 0.8327 0.023 Uiso 1 1 calc R . . C18 C 0.5791(4) 0.3702(3) 0.7343(2) 0.0191(9) Uani 1 1 d . . . C19 C 0.5464(4) 0.3361(3) 0.6591(2) 0.0187(9) Uani 1 1 d . A . C20 C 0.4450(4) 0.3657(3) 0.6330(2) 0.0204(9) Uani 1 1 d . . . H20 H 0.4198 0.3438 0.5821 0.024 Uiso 1 1 calc R A . C21 C 0.3801(4) 0.4265(3) 0.6796(2) 0.0189(9) Uani 1 1 d . A . H21 H 0.3096 0.4440 0.6603 0.023 Uiso 1 1 calc R . . C22 C 0.6129(4) 0.2692(3) 0.6055(2) 0.0187(9) Uani 1 1 d . . . C23 C 0.5201(4) 0.8316(3) 1.0375(2) 0.0170(9) Uani 1 1 d . . . H23 H 0.5340 0.8434 1.0880 0.020 Uiso 1 1 calc R . . C24 C 0.5770(4) 0.7678(3) 0.9803(2) 0.0193(9) Uani 1 1 d . . . H24 H 0.6360 0.7326 0.9894 0.023 Uiso 1 1 calc R . . C25 C 0.5350(4) 0.7634(3) 0.9093(2) 0.0168(9) Uani 1 1 d . . . C26 C 0.4516(4) 0.8224(3) 0.9116(3) 0.0243(10) Uani 1 1 d . . . H26 H 0.4138 0.8293 0.8698 0.029 Uiso 1 1 calc R . . C27 C 0.5715(4) 0.7010(3) 0.8413(2) 0.0136(8) Uani 1 1 d . . . C28 C 0.6770(4) 0.6600(3) 0.8423(2) 0.0147(8) Uani 1 1 d . . . H28 H 0.7275 0.6729 0.8867 0.018 Uiso 1 1 calc R . . C29 C 0.7075(4) 0.6000(3) 0.7777(2) 0.0139(8) Uani 1 1 d . . . C30 C 0.6376(4) 0.5773(3) 0.7107(2) 0.0138(8) Uani 1 1 d . . . C31 C 0.5332(4) 0.6207(3) 0.7110(2) 0.0157(8) Uani 1 1 d . . . H31 H 0.4835 0.6087 0.6664 0.019 Uiso 1 1 calc R . . C32 C 0.5009(4) 0.6807(3) 0.7744(2) 0.0151(8) Uani 1 1 d . . . H32 H 0.4293 0.7088 0.7726 0.018 Uiso 1 1 calc R . . C33 C 0.6684(4) 0.5092(3) 0.6422(2) 0.0153(8) Uani 1 1 d . . . C34 C 1.4203(4) 0.3870(3) 0.9456(3) 0.0233(10) Uani 1 1 d . . . H34 H 1.4986 0.3786 0.9630 0.028 Uiso 1 1 calc R . . C35 C 1.3692(4) 0.3501(3) 0.8706(3) 0.0217(10) Uani 1 1 d . . . H35 H 1.4087 0.3126 0.8323 0.026 Uiso 1 1 calc R . . C36 C 1.2518(4) 0.3767(3) 0.8608(2) 0.0182(9) Uani 1 1 d . . . C37 C 1.2164(5) 0.4285(3) 0.9262(3) 0.0238(10) Uani 1 1 d . . . H37 H 1.1406 0.4519 0.9312 0.029 Uiso 1 1 calc R . . C38 C 1.1781(4) 0.3538(3) 0.7893(2) 0.0161(9) Uani 1 1 d . . . C39 C 1.2142(4) 0.2932(3) 0.7268(2) 0.0165(9) Uani 1 1 d . . . H39 H 1.2858 0.2655 0.7299 0.020 Uiso 1 1 calc R . . C40 C 1.1458(4) 0.2729(3) 0.6600(2) 0.0153(8) Uani 1 1 d . . . C41 C 1.0397(4) 0.3100(3) 0.6519(2) 0.0160(9) Uani 1 1 d . . . C42 C 1.0063(4) 0.3728(3) 0.7145(3) 0.0198(9) Uani 1 1 d . . . H42 H 0.9359 0.4017 0.7112 0.024 Uiso 1 1 calc R . . C43 C 1.0740(4) 0.3940(3) 0.7817(2) 0.0188(9) Uani 1 1 d . . . H43 H 1.0487 0.4369 0.8235 0.023 Uiso 1 1 calc R . . C44 C 0.9509(4) 0.2840(3) 0.5832(2) 0.0156(8) Uani 1 1 d . . . C45 C 0.9887(3) -0.3358(3) -0.0127(2) 0.0130(8) Uani 1 1 d . . . H45 H 0.9741 -0.3567 -0.0643 0.016 Uiso 1 1 calc R . . C46 C 0.9263(4) -0.2676(3) 0.0398(3) 0.0224(10) Uani 1 1 d . . . H46 H 0.8646 -0.2376 0.0257 0.027 Uiso 1 1 calc R . . C47 C 0.9685(4) -0.2513(3) 0.1140(3) 0.0183(9) Uani 1 1 d . . . C48 C 1.0586(4) -0.3030(3) 0.1200(3) 0.0236(10) Uani 1 1 d . . . H48 H 1.0973 -0.3013 0.1650 0.028 Uiso 1 1 calc R . . C49 C 0.9257(4) -0.1854(3) 0.1775(2) 0.0154(8) Uani 1 1 d . . . C50 C 0.8220(4) -0.1446(3) 0.1690(2) 0.0158(9) Uani 1 1 d . . . H50 H 0.7788 -0.1593 0.1221 0.019 Uiso 1 1 calc R . . C51 C 0.7829(4) -0.0830(3) 0.2291(2) 0.0149(8) Uani 1 1 d . . . C52 C 0.8408(4) -0.0580(3) 0.2997(2) 0.0155(8) Uani 1 1 d . . . C53 C 0.9430(4) -0.0993(3) 0.3078(2) 0.0182(9) Uani 1 1 d . . . H53 H 0.9852 -0.0847 0.3550 0.022 Uiso 1 1 calc R . . C54 C 0.9855(4) -0.1617(3) 0.2483(3) 0.0170(9) Uani 1 1 d . . . H54 H 1.0559 -0.1887 0.2557 0.020 Uiso 1 1 calc R . . C55 C 0.7976(4) 0.0114(3) 0.3637(2) 0.0165(9) Uani 1 1 d . . . C60 C 1.0655(4) 0.0627(3) 0.2635(2) 0.0138(8) Uani 1 1 d . . . C61 C 0.9719(4) 0.0909(3) 0.2290(2) 0.0162(9) Uani 1 1 d . B . H61 H 0.9570 0.0683 0.1774 0.019 Uiso 1 1 calc R . . C62 C 0.9003(4) 0.1521(3) 0.2703(2) 0.0151(8) Uani 1 1 d . . . C63 C 0.9153(4) 0.1872(3) 0.3459(2) 0.0153(8) Uani 1 1 d . B . C64 C 1.0104(4) 0.1590(3) 0.3797(2) 0.0185(9) Uani 1 1 d . . . H64 H 1.0246 0.1814 0.4314 0.022 Uiso 1 1 calc R B . C65 C 1.0848(4) 0.0987(3) 0.3396(2) 0.0189(9) Uani 1 1 d . B . H65 H 1.1497 0.0818 0.3643 0.023 Uiso 1 1 calc R . . C66 C 0.8396(4) 0.2523(3) 0.3934(2) 0.0147(8) Uani 1 1 d . . . N1 N 0.2724(3) 0.2951(2) 0.3949(2) 0.0182(8) Uani 1 1 d . . . N3 N 0.8224(4) 0.5624(3) 0.7861(2) 0.0231(9) Uani 1 1 d . . . N4 N 1.1961(3) 0.2140(3) 0.5966(2) 0.0201(8) Uani 1 1 d . . . N5 N 0.6709(3) -0.0456(3) 0.2134(2) 0.0179(8) Uani 1 1 d . . . N6 N 0.8020(3) 0.1771(3) 0.2301(2) 0.0193(8) Uani 1 1 d . B . O1 O 0.3055(3) 0.2922(2) 0.45426(18) 0.0254(8) Uani 1 1 d . . . O2 O 0.1965(3) 0.3414(2) 0.38526(19) 0.0307(9) Uani 1 1 d . . . O3 O 0.5575(3) 0.3069(2) 0.43805(17) 0.0171(6) Uani 1 1 d . . . O4 O 0.5401(3) 0.1751(2) 0.43821(16) 0.0172(6) Uani 1 1 d . . . O7 O 0.5945(4) 0.1927(2) 0.59355(19) 0.0277(8) Uani 1 1 d . A . O8 O 0.6805(3) 0.2923(2) 0.56960(16) 0.0182(6) Uani 1 1 d . A . O9 O 0.9106(3) 0.5974(3) 0.7787(2) 0.0342(9) Uani 1 1 d . . . O10 O 0.8225(4) 0.5024(3) 0.8055(2) 0.0333(9) Uani 1 1 d . . . O11 O 0.5960(3) 0.4864(2) 0.58417(16) 0.0185(7) Uani 1 1 d . . . O12 O 0.7658(3) 0.4744(2) 0.64397(17) 0.0189(7) Uani 1 1 d . . . O13 O 1.1679(3) 0.2211(2) 0.53807(18) 0.0254(8) Uani 1 1 d . . . O14 O 1.2661(3) 0.1631(2) 0.6046(2) 0.0313(9) Uani 1 1 d . . . O15 O 0.9233(3) 0.3426(2) 0.56153(16) 0.0165(6) Uani 1 1 d . . . O16 O 0.9077(3) 0.2088(2) 0.55763(17) 0.0190(7) Uani 1 1 d . . . O17 O 0.6765(3) 0.0107(2) 0.19036(18) 0.0238(7) Uani 1 1 d . . . O18 O 0.5784(3) -0.0773(3) 0.21959(19) 0.0266(8) Uani 1 1 d . . . O19 O 0.8588(3) 0.0324(2) 0.42628(16) 0.0181(7) Uani 1 1 d . . . O20 O 0.7056(3) 0.0479(2) 0.35540(17) 0.0187(7) Uani 1 1 d . . . O21 O 0.7162(3) 0.2066(2) 0.26177(18) 0.0226(7) Uani 1 1 d . . . O22 O 0.8093(3) 0.1660(3) 0.16684(19) 0.0329(9) Uani 1 1 d . . . O23 O 0.8416(3) 0.3276(2) 0.39791(17) 0.0190(7) Uani 1 1 d . B . O24 O 0.7803(3) 0.22978(19) 0.43347(16) 0.0149(6) Uani 1 1 d . B . O25 O 0.8856(3) 0.4886(2) 0.52829(17) 0.0186(7) Uani 1 1 d . . . O26 O 0.6567(3) 0.4703(2) 0.44438(17) 0.0202(7) Uani 1 1 d . . . O27 O 0.6004(3) 0.0143(2) 0.46554(17) 0.0172(6) Uani 1 1 d . . . O28 O 0.7828(3) 0.0815(3) 0.5845(2) 0.0323(9) Uani 1 1 d . . . O95 O 0.6604(3) 0.9187(2) 0.55040(17) 0.0173(6) Uani 1 1 d . . . O96 O 0.1549(3) 0.4143(2) 0.55334(18) 0.0181(6) Uani 1 1 d . . . O97 O 0.5338(3) 0.0870(2) 0.65880(19) 0.0249(7) Uani 1 1 d . . . O98 O 0.9636(3) 0.4327(2) 0.34892(19) 0.0240(7) Uani 1 1 d . . . O99 O 0.9121(6) 0.9571(5) 0.5221(4) 0.0254(15) Uani 0.50 1 d P . . 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 S2A 0.0214(10) 0.0346(10) 0.0357(11) 0.0073(9) 0.0063(8) 0.0109(8) C12A 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C13A 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C14A 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C15A 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) S2B 0.0214(10) 0.0346(10) 0.0357(11) 0.0073(9) 0.0063(8) 0.0109(8) C12B 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C13B 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C14B 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) C15B 0.0131(14) 0.0239(17) 0.0270(14) 0.0121(12) 0.0045(11) 0.0002(12) S6A 0.0161(11) 0.0292(10) 0.0346(10) 0.0102(9) 0.0051(8) 0.0084(7) C56A 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C57A 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C58A 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C59A 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) S6B 0.0161(11) 0.0292(10) 0.0346(10) 0.0102(9) 0.0051(8) 0.0084(7) C56B 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C57B 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C58B 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) C59B 0.0137(13) 0.0176(15) 0.0213(13) 0.0071(11) 0.0033(10) 0.0003(11) N2 0.024(2) 0.038(3) 0.017(2) 0.0123(18) 0.0060(17) 0.0130(19) O5 0.0332(15) 0.0560(19) 0.0209(13) 0.0166(13) 0.0132(11) 0.0252(14) O6 0.0332(15) 0.0560(19) 0.0209(13) 0.0166(13) 0.0132(11) 0.0252(14) Eu1 0.01605(11) 0.01372(11) 0.00828(10) 0.00350(8) 0.00345(8) 0.00008(8) Eu2 0.01688(11) 0.01549(11) 0.01055(10) 0.00588(8) 0.00172(8) -0.00101(8) S1 0.0361(8) 0.0391(8) 0.0239(6) 0.0080(6) -0.0005(6) -0.0009(6) S3 0.0344(8) 0.0387(8) 0.0368(8) 0.0019(6) 0.0122(6) 0.0144(6) S4 0.0366(8) 0.0405(8) 0.0193(6) 0.0073(6) -0.0002(5) -0.0031(6) S5 0.0377(8) 0.0444(9) 0.0405(8) 0.0122(7) 0.0147(7) 0.0170(7) C1 0.015(2) 0.016(2) 0.017(2) 0.0067(17) 0.0014(17) -0.0009(16) C2 0.012(2) 0.022(2) 0.022(2) 0.0135(19) -0.0012(17) -0.0024(17) C3 0.021(2) 0.025(2) 0.018(2) 0.0101(19) 0.0028(18) 0.0014(19) C4 0.024(2) 0.023(2) 0.018(2) 0.0075(19) -0.0007(18) -0.0004(19) C5 0.016(2) 0.015(2) 0.015(2) 0.0051(17) 0.0069(16) 0.0017(16) C6 0.014(2) 0.017(2) 0.019(2) 0.0089(18) 0.0023(17) 0.0007(16) C7 0.016(2) 0.014(2) 0.018(2) 0.0066(17) 0.0066(17) 0.0016(16) C8 0.013(2) 0.015(2) 0.017(2) 0.0074(17) 0.0029(16) 0.0004(16) C9 0.016(2) 0.018(2) 0.018(2) 0.0077(18) 0.0045(17) 0.0026(17) C10 0.018(2) 0.017(2) 0.014(2) 0.0052(17) 0.0049(17) 0.0032(17) C11 0.014(2) 0.020(2) 0.015(2) 0.0085(17) 0.0079(16) 0.0029(16) C16 0.016(2) 0.021(2) 0.019(2) 0.0105(18) 0.0023(17) -0.0045(17) C17 0.017(2) 0.029(2) 0.011(2) 0.0077(18) 0.0032(16) 0.0030(18) C18 0.017(2) 0.029(3) 0.013(2) 0.0105(19) 0.0040(17) 0.0037(19) C19 0.022(2) 0.023(2) 0.013(2) 0.0084(18) 0.0068(17) -0.0011(18) C20 0.024(2) 0.026(2) 0.012(2) 0.0093(18) -0.0003(17) -0.0039(19) C21 0.017(2) 0.027(2) 0.017(2) 0.0138(19) -0.0018(17) 0.0008(18) C22 0.023(2) 0.020(2) 0.013(2) 0.0056(17) 0.0045(17) 0.0024(18) C23 0.0078(19) 0.026(2) 0.0116(19) 0.0016(17) -0.0011(15) -0.0023(17) C24 0.015(2) 0.024(2) 0.016(2) 0.0034(18) 0.0050(17) 0.0025(18) C25 0.015(2) 0.017(2) 0.016(2) 0.0040(17) 0.0031(16) 0.0008(17) C26 0.018(2) 0.026(3) 0.025(2) 0.005(2) 0.0050(19) 0.0094(19) C27 0.012(2) 0.014(2) 0.015(2) 0.0054(16) 0.0055(16) 0.0031(16) C28 0.0100(19) 0.020(2) 0.013(2) 0.0053(17) 0.0030(15) 0.0032(16) C29 0.0100(19) 0.017(2) 0.014(2) 0.0043(17) 0.0043(15) 0.0053(16) C30 0.015(2) 0.015(2) 0.0108(19) 0.0042(16) 0.0042(16) 0.0002(16) C31 0.017(2) 0.018(2) 0.013(2) 0.0074(17) -0.0013(16) -0.0014(17) C32 0.012(2) 0.018(2) 0.016(2) 0.0076(17) 0.0017(16) 0.0013(16) C33 0.017(2) 0.018(2) 0.0116(19) 0.0057(17) 0.0044(16) 0.0008(17) C34 0.015(2) 0.031(3) 0.029(3) 0.022(2) -0.0102(19) -0.0065(19) C35 0.025(2) 0.025(2) 0.015(2) 0.0073(19) 0.0013(18) 0.0009(19) C36 0.021(2) 0.018(2) 0.016(2) 0.0074(18) 0.0007(17) -0.0058(18) C37 0.024(2) 0.027(3) 0.017(2) 0.0051(19) -0.0013(19) -0.003(2) C38 0.017(2) 0.018(2) 0.015(2) 0.0070(17) 0.0015(17) -0.0024(17) C39 0.017(2) 0.017(2) 0.015(2) 0.0055(17) 0.0037(17) -0.0006(17) C40 0.017(2) 0.014(2) 0.013(2) 0.0037(16) 0.0044(16) -0.0012(16) C41 0.018(2) 0.014(2) 0.016(2) 0.0054(17) 0.0018(17) -0.0015(17) C42 0.019(2) 0.022(2) 0.018(2) 0.0074(19) 0.0046(18) 0.0051(18) C43 0.025(2) 0.018(2) 0.012(2) 0.0035(17) 0.0046(17) 0.0009(18) C44 0.017(2) 0.020(2) 0.0100(19) 0.0048(17) 0.0043(16) 0.0019(17) C45 0.0055(18) 0.021(2) 0.0127(19) 0.0066(17) 0.0040(15) 0.0043(15) C46 0.019(2) 0.026(2) 0.021(2) 0.007(2) 0.0069(18) 0.0051(19) C47 0.015(2) 0.019(2) 0.023(2) 0.0081(18) 0.0091(18) 0.0023(17) C48 0.017(2) 0.028(3) 0.028(3) 0.012(2) 0.0082(19) 0.0081(19) C49 0.013(2) 0.016(2) 0.019(2) 0.0082(17) 0.0051(16) 0.0028(16) C50 0.0103(19) 0.024(2) 0.013(2) 0.0072(18) 0.0016(16) 0.0021(17) C51 0.012(2) 0.017(2) 0.016(2) 0.0067(17) 0.0025(16) 0.0022(16) C52 0.017(2) 0.016(2) 0.013(2) 0.0044(17) 0.0021(16) -0.0021(17) C53 0.018(2) 0.019(2) 0.017(2) 0.0080(18) -0.0026(17) -0.0042(17) C54 0.012(2) 0.017(2) 0.024(2) 0.0113(18) -0.0011(17) 0.0009(16) C55 0.023(2) 0.015(2) 0.0111(19) 0.0048(16) 0.0030(17) -0.0029(17) C60 0.0107(19) 0.016(2) 0.015(2) 0.0066(17) 0.0022(15) -0.0001(16) C61 0.017(2) 0.020(2) 0.0116(19) 0.0049(17) 0.0037(16) -0.0002(17) C62 0.012(2) 0.023(2) 0.013(2) 0.0096(17) 0.0020(16) 0.0027(17) C63 0.017(2) 0.015(2) 0.013(2) 0.0042(17) 0.0044(16) 0.0001(16) C64 0.023(2) 0.021(2) 0.0106(19) 0.0059(17) -0.0001(17) 0.0013(18) C65 0.020(2) 0.021(2) 0.017(2) 0.0097(18) -0.0023(17) -0.0001(18) C66 0.016(2) 0.018(2) 0.0086(18) 0.0034(16) 0.0012(15) 0.0004(16) N1 0.0190(19) 0.0194(19) 0.0170(18) 0.0066(15) 0.0071(15) 0.0042(15) N3 0.019(2) 0.031(2) 0.0105(17) -0.0005(16) 0.0024(15) 0.0122(17) N4 0.0155(19) 0.024(2) 0.0158(19) 0.0022(16) 0.0038(15) -0.0010(16) N5 0.0170(19) 0.022(2) 0.0106(17) 0.0015(15) 0.0024(14) 0.0056(15) N6 0.0163(19) 0.027(2) 0.0151(18) 0.0074(16) 0.0044(15) 0.0064(16) O1 0.0281(19) 0.034(2) 0.0163(16) 0.0108(15) 0.0090(14) 0.0083(15) O2 0.035(2) 0.032(2) 0.0227(18) 0.0070(16) 0.0067(16) 0.0224(17) O3 0.0177(16) 0.0172(15) 0.0150(15) 0.0045(12) 0.0028(12) 0.0009(12) O4 0.0205(16) 0.0179(15) 0.0137(15) 0.0062(12) 0.0039(12) 0.0010(13) O7 0.043(2) 0.0209(18) 0.0215(17) 0.0083(14) 0.0150(16) -0.0025(16) O8 0.0223(17) 0.0214(16) 0.0127(14) 0.0076(13) 0.0057(12) -0.0014(13) O9 0.0131(17) 0.052(3) 0.0233(18) -0.0014(17) 0.0045(14) 0.0018(16) O10 0.039(2) 0.041(2) 0.0209(18) 0.0115(17) 0.0077(16) 0.0251(18) O11 0.0231(17) 0.0194(16) 0.0105(14) 0.0040(12) 0.0002(12) 0.0006(13) O12 0.0181(16) 0.0222(17) 0.0135(15) 0.0034(13) 0.0033(12) 0.0024(13) O13 0.0211(17) 0.039(2) 0.0129(16) 0.0056(15) 0.0050(13) 0.0003(15) O14 0.029(2) 0.034(2) 0.0234(18) 0.0023(16) 0.0061(15) 0.0127(16) O15 0.0168(15) 0.0201(16) 0.0138(15) 0.0077(13) 0.0030(12) 0.0039(12) O16 0.0236(17) 0.0153(15) 0.0152(15) 0.0036(12) -0.0010(13) -0.0003(13) O17 0.0280(19) 0.0248(18) 0.0195(17) 0.0095(14) 0.0032(14) 0.0108(14) O18 0.0138(16) 0.043(2) 0.0192(17) 0.0082(16) 0.0032(13) -0.0003(15) O19 0.0210(16) 0.0172(16) 0.0119(14) 0.0010(12) 0.0027(12) 0.0041(13) O20 0.0182(16) 0.0224(17) 0.0149(15) 0.0063(13) 0.0035(12) 0.0035(13) O21 0.0185(17) 0.0275(18) 0.0219(17) 0.0087(14) 0.0067(13) 0.0105(14) O22 0.029(2) 0.060(3) 0.0168(17) 0.0218(18) 0.0067(15) 0.0203(19) O23 0.0243(17) 0.0169(16) 0.0171(15) 0.0060(13) 0.0102(13) 0.0030(13) O24 0.0178(15) 0.0177(15) 0.0091(13) 0.0049(12) 0.0031(11) 0.0008(12) O25 0.0196(16) 0.0175(16) 0.0193(16) 0.0075(13) 0.0043(13) 0.0005(13) O26 0.0228(17) 0.0215(17) 0.0176(16) 0.0097(13) 0.0001(13) 0.0002(13) O27 0.0158(15) 0.0184(16) 0.0195(16) 0.0088(13) 0.0053(12) 0.0030(12) O28 0.028(2) 0.044(2) 0.034(2) 0.0288(19) -0.0081(16) -0.0076(17) O95 0.0142(15) 0.0178(16) 0.0205(16) 0.0079(13) 0.0030(12) 0.0033(12) O96 0.0153(15) 0.0201(16) 0.0225(16) 0.0117(14) 0.0046(13) 0.0051(12) O97 0.0231(18) 0.0308(19) 0.0226(17) 0.0127(15) 0.0016(14) -0.0001(15) O98 0.0209(17) 0.0309(19) 0.0230(17) 0.0139(15) 0.0014(14) 0.0001(14) O99 0.025(4) 0.026(4) 0.026(4) 0.013(3) -0.003(3) 0.004(3) _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 S2A C13A 1.687(19) . ? S2A C12A 1.813(15) . ? C12A C15A 1.32(2) . ? C12A H12A 0.9500 . ? C13A C14A 1.371(17) . ? C13A H13A 0.9500 . ? C14A C15A 1.416(16) . ? C14A C16 1.472(7) . ? C15A H15A 0.9500 . ? S2B C13B 1.689(9) . ? S2B C12B 1.760(8) . ? C12B C15B 1.355(13) . ? C12B H12B 0.9500 . ? C13B H13B 0.9500 . ? C15B H15B 0.9500 . ? S6A C59A 1.728(8) . ? S6A C56A 1.738(7) . ? C56A C57A 1.373(12) . ? C56A H56A 0.9500 . ? C57A C58A 1.421(9) . ? C57A H57A 0.9500 . ? C58A C59A 1.366(9) . ? C58A C60 1.480(6) . ? C59A H59A 0.9500 . ? S6B C59B 1.728(19) . ? S6B C56B 1.736(18) . ? C56B C57B 1.37(2) . ? C56B H56B 0.9500 . ? C57B H57B 0.9500 . ? C59B H59B 0.9500 . ? N2 O5 1.228(5) . ? N2 O6 1.229(5) . ? N2 C18 1.468(6) . ? Eu1 O25 2.363(3) . ? Eu1 O8 2.383(3) . ? Eu1 O3 2.416(3) . ? Eu1 O15 2.451(3) . ? Eu1 O12 2.468(3) . ? Eu1 O26 2.492(3) . ? Eu1 O11 2.510(3) . ? Eu1 O24 2.560(3) . ? Eu1 O23 2.568(3) . ? Eu2 O24 2.375(3) . ? Eu2 O27 2.378(3) . ? Eu2 O4 2.399(3) . ? Eu2 O16 2.402(3) . ? Eu2 O19 2.444(3) . ? Eu2 O28 2.495(4) . ? Eu2 O20 2.513(3) . ? Eu2 O8 2.563(3) . ? Eu2 O7 2.564(4) . ? S1 C2 1.693(5) . ? S1 C4 1.702(5) . ? S3 C26 1.684(5) . ? S3 C23 1.703(5) . ? S4 C34 1.649(6) . ? S4 C37 1.712(5) . ? S5 C48 1.688(5) . ? S5 C45 1.715(4) . ? C1 C4 1.380(7) . ? C1 C3 1.427(6) . ? C1 C5 1.479(6) . ? C2 C3 1.458(6) . ? C2 H2 0.9500 . ? C3 H3 0.9500 . ? C4 H4 0.9500 . ? C5 C10 1.394(6) . ? C5 C6 1.400(6) . ? C6 C7 1.384(6) . ? C6 H6 0.9500 . ? C7 C8 1.384(6) . ? C7 N1 1.466(6) . ? C8 C9 1.399(6) . ? C8 C11 1.513(6) . ? C9 C10 1.386(6) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 O3 1.248(5) . ? C11 O4 1.271(5) . ? C16 C17 1.387(7) . ? C16 C21 1.402(6) . ? C17 C18 1.392(7) . ? C17 H17 0.9500 . ? C18 C19 1.395(6) . ? C19 C20 1.389(7) . ? C19 C22 1.507(6) . ? C20 C21 1.380(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 O7 1.241(6) . ? C22 O8 1.271(5) . ? C23 C24 1.458(6) . ? C23 H23 0.9500 . ? C24 C25 1.426(6) . ? C24 H24 0.9500 . ? C25 C26 1.375(6) . ? C25 C27 1.474(6) . ? C26 H26 0.9500 . ? C27 C28 1.392(6) . ? C27 C32 1.400(6) . ? C28 C29 1.386(6) . ? C28 H28 0.9500 . ? C29 C30 1.393(6) . ? C29 N3 1.477(6) . ? C30 C31 1.400(6) . ? C30 C33 1.495(6) . ? C31 C32 1.378(6) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 O12 1.261(5) . ? C33 O11 1.269(5) . ? C34 C35 1.435(6) . ? C34 H34 0.9500 . ? C35 C36 1.428(7) . ? C35 H35 0.9500 . ? C36 C37 1.376(7) . ? C36 C38 1.485(6) . ? C37 H37 0.9500 . ? C38 C39 1.387(6) . ? C38 C43 1.392(7) . ? C39 C40 1.387(6) . ? C39 H39 0.9500 . ? C40 C41 1.387(6) . ? C40 N4 1.461(6) . ? C41 C42 1.391(6) . ? C41 C44 1.523(6) . ? C42 C43 1.386(6) . ? C42 H42 0.9500 . ? C43 H43 0.9500 . ? C44 O16 1.252(5) . ? C44 O15 1.261(5) . ? C45 C46 1.480(6) . ? C45 H45 0.9500 . ? C46 C47 1.430(7) . ? C46 H46 0.9500 . ? C47 C48 1.377(7) . ? C47 C49 1.469(6) . ? C48 H48 0.9500 . ? C49 C50 1.397(6) . ? C49 C54 1.406(6) . ? C50 C51 1.379(6) . ? C50 H50 0.9500 . ? C51 C52 1.393(6) . ? C51 N5 1.482(6) . ? C52 C53 1.386(6) . ? C52 C55 1.503(6) . ? C53 C54 1.392(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 O20 1.246(6) . ? C55 O19 1.281(5) . ? C60 C61 1.390(6) . ? C60 C65 1.400(6) . ? C61 C62 1.389(6) . ? C61 H61 0.9500 . ? C62 C63 1.389(6) . ? C62 N6 1.465(6) . ? C63 C64 1.396(6) . ? C63 C66 1.501(6) . ? C64 C65 1.393(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C66 O23 1.248(5) . ? C66 O24 1.273(5) . ? N1 O2 1.221(5) . ? N1 O1 1.230(5) . ? N3 O9 1.219(6) . ? N3 O10 1.227(6) . ? N4 O14 1.222(5) . ? N4 O13 1.236(5) . ? N5 O17 1.220(5) . ? N5 O18 1.222(5) . ? N6 O22 1.225(5) . ? N6 O21 1.229(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 C13A S2A C12A 90.3(8) . . ? C15A C12A S2A 109.4(13) . . ? C15A C12A H12A 125.3 . . ? S2A C12A H12A 125.3 . . ? C14A C13A S2A 113.4(12) . . ? C14A C13A H13A 123.3 . . ? S2A C13A H13A 123.3 . . ? C13A C14A C15A 111.6(9) . . ? C13A C14A C16 125.0(9) . . ? C15A C14A C16 123.2(8) . . ? C12A C15A C14A 114.9(14) . . ? C12A C15A H15A 122.5 . . ? C14A C15A H15A 122.5 . . ? C13B S2B C12B 92.1(4) . . ? C15B C12B S2B 108.6(7) . . ? C15B C12B H12B 125.7 . . ? S2B C12B H12B 125.7 . . ? S2B C13B H13B 123.4 . . ? C12B C15B H15B 122.0 . . ? C59A S6A C56A 93.1(4) . . ? C57A C56A S6A 108.9(6) . . ? C57A C56A H56A 125.6 . . ? S6A C56A H56A 125.6 . . ? C56A C57A C58A 114.7(6) . . ? C56A C57A H57A 122.6 . . ? C58A C57A H57A 122.6 . . ? C59A C58A C57A 112.4(5) . . ? C59A C58A C60 123.1(5) . . ? C57A C58A C60 124.4(5) . . ? C58A C59A S6A 110.8(5) . . ? C58A C59A H59A 124.6 . . ? S6A C59A H59A 124.6 . . ? C59B S6B C56B 93.1(10) . . ? C57B C56B S6B 108.3(16) . . ? C57B C56B H56B 125.9 . . ? S6B C56B H56B 125.9 . . ? C56B C57B H57B 121.6 . . ? S6B C59B H59B 124.0 . . ? O5 N2 O6 123.5(4) . . ? O5 N2 C18 118.3(4) . . ? O6 N2 C18 118.2(4) . . ? O25 Eu1 O8 139.75(11) . . ? O25 Eu1 O3 144.52(11) . . ? O8 Eu1 O3 75.72(11) . . ? O25 Eu1 O15 72.19(11) . . ? O8 Eu1 O15 74.58(11) . . ? O3 Eu1 O15 135.06(11) . . ? O25 Eu1 O12 74.27(11) . . ? O8 Eu1 O12 75.39(11) . . ? O3 Eu1 O12 128.38(11) . . ? O15 Eu1 O12 74.26(11) . . ? O25 Eu1 O26 72.62(11) . . ? O8 Eu1 O26 143.33(11) . . ? O3 Eu1 O26 73.82(11) . . ? O15 Eu1 O26 142.09(11) . . ? O12 Eu1 O26 108.92(11) . . ? O25 Eu1 O11 95.45(11) . . ? O8 Eu1 O11 86.52(11) . . ? O3 Eu1 O11 83.88(11) . . ? O15 Eu1 O11 126.63(10) . . ? O12 Eu1 O11 52.61(11) . . ? O26 Eu1 O11 70.44(11) . . ? O25 Eu1 O24 115.42(11) . . ? O8 Eu1 O24 71.64(10) . . ? O3 Eu1 O24 69.87(11) . . ? O15 Eu1 O24 69.18(11) . . ? O12 Eu1 O24 135.77(10) . . ? O26 Eu1 O24 115.17(10) . . ? O11 Eu1 O24 149.04(10) . . ? O25 Eu1 O23 73.40(11) . . ? O8 Eu1 O23 121.98(11) . . ? O3 Eu1 O23 88.18(11) . . ? O15 Eu1 O23 79.92(11) . . ? O12 Eu1 O23 143.41(11) . . ? O26 Eu1 O23 76.98(11) . . ? O11 Eu1 O23 147.40(10) . . ? O24 Eu1 O23 50.61(10) . . ? O24 Eu2 O27 141.61(11) . . ? O24 Eu2 O4 75.01(11) . . ? O27 Eu2 O4 79.65(11) . . ? O24 Eu2 O16 74.30(11) . . ? O27 Eu2 O16 140.12(11) . . ? O4 Eu2 O16 138.25(11) . . ? O24 Eu2 O19 90.79(11) . . ? O27 Eu2 O19 82.33(11) . . ? O4 Eu2 O19 127.73(11) . . ? O16 Eu2 O19 80.23(11) . . ? O24 Eu2 O28 145.03(11) . . ? O27 Eu2 O28 70.99(12) . . ? O4 Eu2 O28 136.12(12) . . ? O16 Eu2 O28 70.88(12) . . ? O19 Eu2 O28 80.34(13) . . ? O24 Eu2 O20 73.84(11) . . ? O27 Eu2 O20 72.02(11) . . ? O4 Eu2 O20 75.02(11) . . ? O16 Eu2 O20 121.47(11) . . ? O19 Eu2 O20 52.74(11) . . ? O28 Eu2 O20 122.83(13) . . ? O24 Eu2 O8 71.72(10) . . ? O27 Eu2 O8 125.92(11) . . ? O4 Eu2 O8 71.32(11) . . ? O16 Eu2 O8 72.61(11) . . ? O19 Eu2 O8 150.71(11) . . ? O28 Eu2 O8 100.40(12) . . ? O20 Eu2 O8 136.67(10) . . ? O24 Eu2 O7 120.62(11) . . ? O27 Eu2 O7 78.45(11) . . ? O4 Eu2 O7 74.59(12) . . ? O16 Eu2 O7 97.84(12) . . ? O19 Eu2 O7 147.05(11) . . ? O28 Eu2 O7 68.21(13) . . ? O20 Eu2 O7 140.67(12) . . ? O8 Eu2 O7 50.58(10) . . ? C2 S1 C4 95.0(2) . . ? C26 S3 C23 95.4(2) . . ? C34 S4 C37 94.0(2) . . ? C48 S5 C45 96.1(2) . . ? C4 C1 C3 111.1(4) . . ? C4 C1 C5 123.7(4) . . ? C3 C1 C5 125.2(4) . . ? C3 C2 S1 108.0(3) . . ? C3 C2 H2 126.0 . . ? S1 C2 H2 126.0 . . ? C1 C3 C2 113.4(4) . . ? C1 C3 H3 123.3 . . ? C2 C3 H3 123.3 . . ? C1 C4 S1 112.4(4) . . ? C1 C4 H4 123.8 . . ? S1 C4 H4 123.8 . . ? C10 C5 C6 117.9(4) . . ? C10 C5 C1 122.8(4) . . ? C6 C5 C1 119.3(4) . . ? C7 C6 C5 119.3(4) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C8 C7 C6 123.6(4) . . ? C8 C7 N1 119.9(4) . . ? C6 C7 N1 116.4(4) . . ? C7 C8 C9 116.5(4) . . ? C7 C8 C11 125.2(4) . . ? C9 C8 C11 118.1(4) . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C5 121.6(4) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? O3 C11 O4 126.7(4) . . ? O3 C11 C8 117.6(4) . . ? O4 C11 C8 115.5(4) . . ? C17 C16 C21 117.8(4) . . ? C17 C16 C14A 120.8(4) . . ? C21 C16 C14A 121.4(4) . . ? C16 C17 C18 120.1(4) . . ? C16 C17 H17 120.0 . . ? C18 C17 H17 120.0 . . ? C17 C18 C19 122.3(4) . . ? C17 C18 N2 117.1(4) . . ? C19 C18 N2 120.6(4) . . ? C20 C19 C18 117.0(4) . . ? C20 C19 C22 118.7(4) . . ? C18 C19 C22 124.2(4) . . ? C21 C20 C19 121.3(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C20 C21 C16 121.4(4) . . ? C20 C21 H21 119.3 . . ? C16 C21 H21 119.3 . . ? O7 C22 O8 121.4(4) . . ? O7 C22 C19 119.6(4) . . ? O8 C22 C19 118.8(4) . . ? C24 C23 S3 107.4(3) . . ? C24 C23 H23 126.3 . . ? S3 C23 H23 126.3 . . ? C25 C24 C23 113.2(4) . . ? C25 C24 H24 123.4 . . ? C23 C24 H24 123.4 . . ? C26 C25 C24 111.4(4) . . ? C26 C25 C27 123.9(4) . . ? C24 C25 C27 124.6(4) . . ? C25 C26 S3 112.6(4) . . ? C25 C26 H26 123.7 . . ? S3 C26 H26 123.7 . . ? C28 C27 C32 118.2(4) . . ? C28 C27 C25 120.6(4) . . ? C32 C27 C25 121.2(4) . . ? C29 C28 C27 119.3(4) . . ? C29 C28 H28 120.3 . . ? C27 C28 H28 120.3 . . ? C28 C29 C30 123.6(4) . . ? C28 C29 N3 113.9(4) . . ? C30 C29 N3 122.5(4) . . ? C29 C30 C31 116.0(4) . . ? C29 C30 C33 123.0(4) . . ? C31 C30 C33 121.0(4) . . ? C32 C31 C30 121.6(4) . . ? C32 C31 H31 119.2 . . ? C30 C31 H31 119.2 . . ? C31 C32 C27 121.3(4) . . ? C31 C32 H32 119.3 . . ? C27 C32 H32 119.3 . . ? O12 C33 O11 121.4(4) . . ? O12 C33 C30 118.7(4) . . ? O11 C33 C30 119.9(4) . . ? C35 C34 S4 111.1(4) . . ? C35 C34 H34 124.5 . . ? S4 C34 H34 124.5 . . ? C36 C35 C34 111.7(4) . . ? C36 C35 H35 124.2 . . ? C34 C35 H35 124.2 . . ? C37 C36 C35 111.4(4) . . ? C37 C36 C38 123.9(4) . . ? C35 C36 C38 124.7(4) . . ? C36 C37 S4 111.8(4) . . ? C36 C37 H37 124.1 . . ? S4 C37 H37 124.1 . . ? C39 C38 C43 117.7(4) . . ? C39 C38 C36 120.3(4) . . ? C43 C38 C36 121.9(4) . . ? C38 C39 C40 120.1(4) . . ? C38 C39 H39 120.0 . . ? C40 C39 H39 120.0 . . ? C39 C40 C41 122.9(4) . . ? C39 C40 N4 116.1(4) . . ? C41 C40 N4 120.9(4) . . ? C40 C41 C42 116.5(4) . . ? C40 C41 C44 126.7(4) . . ? C42 C41 C44 116.5(4) . . ? C43 C42 C41 121.2(4) . . ? C43 C42 H42 119.4 . . ? C41 C42 H42 119.4 . . ? C42 C43 C38 121.5(4) . . ? C42 C43 H43 119.2 . . ? C38 C43 H43 119.2 . . ? O16 C44 O15 127.4(4) . . ? O16 C44 C41 116.4(4) . . ? O15 C44 C41 116.0(4) . . ? C46 C45 S5 106.5(3) . . ? C46 C45 H45 126.8 . . ? S5 C45 H45 126.8 . . ? C47 C46 C45 113.1(4) . . ? C47 C46 H46 123.4 . . ? C45 C46 H46 123.4 . . ? C48 C47 C46 112.1(4) . . ? C48 C47 C49 122.9(4) . . ? C46 C47 C49 125.0(4) . . ? C47 C48 S5 112.2(4) . . ? C47 C48 H48 123.9 . . ? S5 C48 H48 123.9 . . ? C50 C49 C54 117.7(4) . . ? C50 C49 C47 120.3(4) . . ? C54 C49 C47 122.0(4) . . ? C51 C50 C49 119.6(4) . . ? C51 C50 H50 120.2 . . ? C49 C50 H50 120.2 . . ? C50 C51 C52 123.8(4) . . ? C50 C51 N5 114.6(4) . . ? C52 C51 N5 121.6(4) . . ? C53 C52 C51 116.3(4) . . ? C53 C52 C55 121.5(4) . . ? C51 C52 C55 122.3(4) . . ? C52 C53 C54 121.6(4) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C53 C54 C49 121.0(4) . . ? C53 C54 H54 119.5 . . ? C49 C54 H54 119.5 . . ? O20 C55 O19 121.4(4) . . ? O20 C55 C52 120.6(4) . . ? O19 C55 C52 118.1(4) . . ? C61 C60 C65 118.0(4) . . ? C61 C60 C58A 120.3(4) . . ? C65 C60 C58A 121.7(4) . . ? C62 C61 C60 119.8(4) . . ? C62 C61 H61 120.1 . . ? C60 C61 H61 120.1 . . ? C61 C62 C63 123.5(4) . . ? C61 C62 N6 116.5(4) . . ? C63 C62 N6 119.9(4) . . ? C62 C63 C64 116.0(4) . . ? C62 C63 C66 125.9(4) . . ? C64 C63 C66 118.1(4) . . ? C65 C64 C63 121.6(4) . . ? C65 C64 H64 119.2 . . ? C63 C64 H64 119.2 . . ? C64 C65 C60 121.0(4) . . ? C64 C65 H65 119.5 . . ? C60 C65 H65 119.5 . . ? O23 C66 O24 120.8(4) . . ? O23 C66 C63 121.6(4) . . ? O24 C66 C63 117.4(4) . . ? O2 N1 O1 123.9(4) . . ? O2 N1 C7 118.9(4) . . ? O1 N1 C7 117.1(4) . . ? O9 N3 O10 125.0(4) . . ? O9 N3 C29 117.5(4) . . ? O10 N3 C29 117.3(4) . . ? O14 N4 O13 123.8(4) . . ? O14 N4 C40 118.9(4) . . ? O13 N4 C40 117.2(4) . . ? O17 N5 O18 124.3(4) . . ? O17 N5 C51 117.9(4) . . ? O18 N5 C51 117.6(4) . . ? O22 N6 O21 124.1(4) . . ? O22 N6 C62 118.3(4) . . ? O21 N6 C62 117.7(4) . . ? C11 O3 Eu1 136.3(3) . . ? C11 O4 Eu2 132.8(3) . . ? C22 O7 Eu2 94.4(3) . . ? C22 O8 Eu1 152.8(3) . . ? C22 O8 Eu2 93.7(3) . . ? Eu1 O8 Eu2 108.15(12) . . ? C33 O11 Eu1 91.9(3) . . ? C33 O12 Eu1 94.0(3) . . ? C44 O15 Eu1 134.1(3) . . ? C44 O16 Eu2 135.0(3) . . ? C55 O19 Eu2 94.1(3) . . ? C55 O20 Eu2 91.8(3) . . ? C66 O23 Eu1 94.0(3) . . ? C66 O24 Eu2 155.5(3) . . ? C66 O24 Eu1 93.7(3) . . ? Eu2 O24 Eu1 108.49(11) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 6.595 _refine_diff_density_min -2.852 _refine_diff_density_rms 0.164 data_p1bar_2 _database_code_depnum_ccdc_archive 'CCDC 224938' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C66 H53 N6 O32.50 S6 Tb2' _chemical_formula_weight 1960.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.416(2) _cell_length_b 16.896(3) _cell_length_c 20.075(4) _cell_angle_alpha 113.09(3) _cell_angle_beta 96.85(3) _cell_angle_gamma 90.46(3) _cell_volume 3530.1(12) _cell_formula_units_Z 2 _cell_measurement_temperature 89(2) _cell_measurement_reflns_used 8965 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 33.02 _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.844 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1954 _exptl_absorpt_coefficient_mu 2.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7276 _exptl_absorpt_correction_T_max 0.8952 _exptl_absorpt_process_details 'SADABS SHELXL-97 (Sheldrick, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 89(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 'APEX CCD detector' _diffrn_measurement_method 'Phi and omega scans' _diffrn_detector_area_resol_mean 8.3 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.001 _diffrn_reflns_number 47390 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 27.50 _reflns_number_total 16131 _reflns_number_gt 12277 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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. ; _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^)+(0.0623P)^2^+6.3318P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16131 _refine_ls_number_parameters 997 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0689 _refine_ls_R_factor_gt 0.0485 _refine_ls_wR_factor_ref 0.1275 _refine_ls_wR_factor_gt 0.1173 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _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 S6A S -0.2172(5) 0.6409(5) 0.4165(4) 0.0329(6) Uani 0.301(5) 1 d PD A 1 C42A C -0.2384(17) 0.5670(13) 0.2753(11) 0.0207(8) Uani 0.301(5) 1 d PD A 1 H42A H -0.2579 0.5525 0.2244 0.025 Uiso 0.301(5) 1 calc PR A 1 C43A C -0.1491(4) 0.5285(4) 0.3035(3) 0.0207(8) Uani 0.301(5) 1 d PD A 1 C44A C -0.1107(19) 0.5781(13) 0.3768(11) 0.0207(8) Uani 0.301(5) 1 d PD A 1 H44A H -0.0345 0.5767 0.4012 0.025 Uiso 0.301(5) 1 calc PR A 1 C45A C -0.2955(18) 0.6270(14) 0.3262(9) 0.0207(8) Uani 0.301(5) 1 d PD A 1 H45A H -0.3625 0.6560 0.3171 0.025 Uiso 0.301(5) 1 calc PR A 1 S6B S -0.3063(2) 0.63513(17) 0.35381(15) 0.0329(6) Uani 0.699(5) 1 d PD A 2 C42B C -0.1187(9) 0.5666(6) 0.3797(6) 0.0207(8) Uani 0.699(5) 1 d PD A 2 H42B H -0.0547 0.5479 0.4036 0.025 Uiso 0.699(5) 1 calc PR A 2 C43B C -0.1491(4) 0.5285(4) 0.3035(3) 0.0207(8) Uani 0.699(5) 1 d PD A 2 C44B C -0.2566(8) 0.5567(6) 0.2836(6) 0.0207(8) Uani 0.699(5) 1 d PD A 2 H44B H -0.2975 0.5338 0.2353 0.025 Uiso 0.699(5) 1 calc PR A 2 C45B C -0.1869(9) 0.6333(7) 0.4188(6) 0.0207(8) Uani 0.699(5) 1 d PD A 2 H45B H -0.1725 0.6698 0.4692 0.025 Uiso 0.699(5) 1 calc PR A 2 S3A S 0.7950(2) -0.11711(18) -0.31620(13) 0.0275(6) Uani 0.745(5) 1 d PD B 1 C13A C 0.6884(8) -0.1136(6) -0.3851(5) 0.0189(8) Uani 0.745(5) 1 d PD B 1 H13A H 0.6852 -0.1494 -0.4355 0.023 Uiso 0.745(5) 1 calc PR B 1 C14A C 0.6112(8) -0.0529(6) -0.3566(5) 0.0189(8) Uani 0.745(5) 1 d PD B 1 H14A H 0.5452 -0.0429 -0.3852 0.023 Uiso 0.745(5) 1 calc PR B 1 C15A C 0.6377(4) -0.0060(3) -0.2807(3) 0.0189(8) Uani 0.745(5) 1 d PD B 1 C16A C 0.7316(8) -0.0387(6) -0.2515(6) 0.0189(8) Uani 0.745(5) 1 d PD B 1 H16A H 0.7576 -0.0192 -0.2006 0.023 Uiso 0.745(5) 1 calc PR B 1 S3B S 0.7177(6) -0.1217(5) -0.3922(4) 0.0275(6) Uani 0.255(5) 1 d PD B 2 C13B C 0.780(3) -0.1019(19) -0.3030(11) 0.0189(8) Uani 0.255(5) 1 d PD B 2 H13B H 0.8336 -0.1388 -0.2911 0.023 Uiso 0.255(5) 1 calc PR B 2 C14B C 0.745(2) -0.0277(15) -0.2518(14) 0.0189(8) Uani 0.255(5) 1 d PD B 2 H14B H 0.7867 0.0038 -0.2044 0.023 Uiso 0.255(5) 1 calc PR B 2 C15B C 0.6377(4) -0.0060(3) -0.2807(3) 0.0189(8) Uani 0.255(5) 1 d PD B 2 C16B C 0.624(2) -0.0434(15) -0.3573(12) 0.0189(8) Uani 0.255(5) 1 d PD B 2 H16B H 0.5679 -0.0261 -0.3870 0.023 Uiso 0.255(5) 1 calc PR B 2 S2A S 0.5925(3) -0.3696(3) -0.46314(12) 0.0327(6) Uani 0.855(6) 1 d PD C 1 C9A C 0.5605(6) -0.3007(4) -0.3796(4) 0.0187(7) Uani 0.855(6) 1 d PD C 1 H9A H 0.6012 -0.2972 -0.3343 0.022 Uiso 0.855(6) 1 calc PR C 1 C10A C 0.4682(5) -0.2509(3) -0.3863(3) 0.0187(7) Uani 0.855(6) 1 d PD C 1 C11A C 0.4251(7) -0.2692(4) -0.4615(4) 0.0187(7) Uani 0.855(6) 1 d PD C 1 H11A H 0.3593 -0.2430 -0.4764 0.022 Uiso 0.855(6) 1 calc PR C 1 C12A C 0.4897(8) -0.3290(5) -0.5100(5) 0.0187(7) Uani 0.855(6) 1 d PD C 1 H12A H 0.4790 -0.3453 -0.5614 0.022 Uiso 0.855(6) 1 calc PR C 1 S2B S 0.4872(15) -0.3486(8) -0.5196(8) 0.0327(6) Uani 0.145(6) 1 d PD C 2 C9B C 0.438(4) -0.257(2) -0.4575(11) 0.0187(7) Uani 0.145(6) 1 d PD C 2 H9B H 0.3950 -0.2151 -0.4699 0.022 Uiso 0.145(6) 1 calc PR C 2 C10B C 0.4682(5) -0.2509(3) -0.3863(3) 0.0187(7) Uani 0.145(6) 1 d PD C 2 C11B C 0.547(3) -0.318(2) -0.3869(16) 0.0187(7) Uani 0.145(6) 1 d PD C 2 H11B H 0.5679 -0.3324 -0.3459 0.022 Uiso 0.145(6) 1 calc PR C 2 C12B C 0.589(5) -0.359(5) -0.4535(17) 0.0187(7) Uani 0.145(6) 1 d PD C 2 H12B H 0.6607 -0.3875 -0.4611 0.022 Uiso 0.145(6) 1 calc PR C 2 Tb1 Tb 0.22315(2) 0.137837(15) -0.010726(13) 0.01368(7) Uani 1 1 d . . . Tb2 Tb 0.24038(2) 0.382010(15) 0.012664(12) 0.01449(7) Uani 1 1 d . . . S1 S -0.33715(15) 0.06166(11) -0.50590(9) 0.0346(4) Uani 1 1 d . . . S4 S 0.82564(15) 0.44479(11) 0.49801(9) 0.0347(4) Uani 1 1 d . . . S5 S -0.07830(16) 0.88010(12) 0.49392(11) 0.0437(5) Uani 1 1 d . . . C2 C 0.2952(5) 0.0117(3) -0.1362(3) 0.0179(11) Uani 1 1 d . . . C3 C 0.3391(5) -0.0583(3) -0.2005(3) 0.0146(10) Uani 1 1 d . C . C4 C 0.4416(4) -0.0990(3) -0.1922(3) 0.0166(10) Uani 1 1 d . . . H4 H 0.4834 -0.0840 -0.1447 0.020 Uiso 1 1 calc R . . C5 C 0.4845(5) -0.1609(3) -0.2514(3) 0.0170(11) Uani 1 1 d . C . H5 H 0.5553 -0.1871 -0.2438 0.020 Uiso 1 1 calc R . . C6 C 0.4248(4) -0.1854(3) -0.3225(3) 0.0147(10) Uani 1 1 d . . . C7 C 0.3217(4) -0.1452(3) -0.3311(3) 0.0144(10) Uani 1 1 d . C . H7 H 0.2791 -0.1599 -0.3784 0.017 Uiso 1 1 calc R . . C8 C 0.2816(4) -0.0840(3) -0.2710(3) 0.0159(10) Uani 1 1 d . . . C17 C 0.5649(4) 0.0615(3) -0.2371(3) 0.0165(10) Uani 1 1 d . . . C18 C 0.4707(4) 0.0903(3) -0.2714(3) 0.0155(10) Uani 1 1 d . B . H18 H 0.4558 0.0681 -0.3232 0.019 Uiso 1 1 calc R . . C19 C 0.3998(5) 0.1504(3) -0.2303(3) 0.0154(10) Uani 1 1 d . . . C20 C 0.4151(5) 0.1854(3) -0.1541(3) 0.0168(11) Uani 1 1 d . B . C21 C 0.5089(5) 0.1575(3) -0.1197(3) 0.0183(11) Uani 1 1 d . . . H21 H 0.5227 0.1798 -0.0679 0.022 Uiso 1 1 calc R B . C22 C 0.5828(5) 0.0976(3) -0.1603(3) 0.0183(11) Uani 1 1 d . B . H22 H 0.6472 0.0805 -0.1354 0.022 Uiso 1 1 calc R . . C23 C 0.3390(5) 0.2506(3) -0.1063(3) 0.0170(11) Uani 1 1 d . . . C24 C 0.0190(4) 0.2313(3) -0.0858(3) 0.0142(10) Uani 1 1 d . . . C25 C -0.0652(4) 0.2015(3) -0.1562(3) 0.0144(10) Uani 1 1 d . . . C26 C -0.0285(5) 0.1384(3) -0.2184(3) 0.0160(10) Uani 1 1 d . . . H26 H 0.0430 0.1114 -0.2140 0.019 Uiso 1 1 calc R . . C27 C -0.0951(5) 0.1148(3) -0.2863(3) 0.0164(10) Uani 1 1 d . . . H27 H -0.0690 0.0711 -0.3275 0.020 Uiso 1 1 calc R . . C28 C -0.1995(5) 0.1535(3) -0.2954(3) 0.0154(10) Uani 1 1 d . . . C29 C -0.2383(5) 0.2145(3) -0.2332(3) 0.0161(10) Uani 1 1 d . . . H29 H -0.3104 0.2411 -0.2372 0.019 Uiso 1 1 calc R . . C30 C -0.1722(4) 0.2360(3) -0.1662(3) 0.0137(10) Uani 1 1 d . . . C31 C -0.2705(5) 0.1303(3) -0.3674(3) 0.0180(11) Uani 1 1 d . . . C32 C -0.2333(5) 0.0785(3) -0.4331(3) 0.0225(12) Uani 1 1 d . . . H32 H -0.1578 0.0551 -0.4370 0.027 Uiso 1 1 calc R . . C33 C -0.4372(4) 0.1210(3) -0.4556(3) 0.0170(11) Uani 1 1 d . . . H33 H -0.5143 0.1298 -0.4741 0.020 Uiso 1 1 calc R . . C34 C -0.3870(5) 0.1562(3) -0.3798(3) 0.0209(11) Uani 1 1 d . . . H34 H -0.4275 0.1931 -0.3417 0.025 Uiso 1 1 calc R . . C35 C 0.1171(5) 0.2685(3) 0.1055(3) 0.0199(11) Uani 1 1 d . . . C36 C -0.0498(5) 0.3647(4) 0.1320(3) 0.0227(12) Uani 1 1 d . . . H36 H -0.0741 0.3427 0.0808 0.027 Uiso 1 1 calc R . . C37 C 0.0512(5) 0.3355(3) 0.1591(3) 0.0186(11) Uani 1 1 d . . . C38 C 0.0820(5) 0.3691(3) 0.2342(3) 0.0179(11) Uani 1 1 d . . . C39 C 0.0189(5) 0.4316(4) 0.2812(3) 0.0183(11) Uani 1 1 d . A . H39 H 0.0441 0.4542 0.3323 0.022 Uiso 1 1 calc R . . C40 C -0.0821(4) 0.4616(3) 0.2538(3) 0.0160(10) Uani 1 1 d . . . C41 C -0.1153(5) 0.4255(3) 0.1787(3) 0.0202(11) Uani 1 1 d . A . H41 H -0.1851 0.4430 0.1588 0.024 Uiso 1 1 calc R . . C46 C 0.1723(5) 0.5073(3) 0.1407(3) 0.0174(11) Uani 1 1 d . . . C47 C 0.1408(5) 0.5759(3) 0.2091(3) 0.0152(10) Uani 1 1 d . . . C48 C 0.2087(4) 0.5994(3) 0.2766(3) 0.0146(10) Uani 1 1 d . . . C49 C 0.1760(4) 0.6590(3) 0.3407(3) 0.0149(10) Uani 1 1 d . . . H49 H 0.2253 0.6724 0.3858 0.018 Uiso 1 1 calc R . . C50 C 0.0710(4) 0.6993(3) 0.3389(3) 0.0133(10) Uani 1 1 d . . . C51 C 0.0023(4) 0.6782(3) 0.2719(3) 0.0164(11) Uani 1 1 d . . . H51 H -0.0694 0.7057 0.2695 0.020 Uiso 1 1 calc R . . C52 C 0.0359(5) 0.6182(3) 0.2085(3) 0.0179(11) Uani 1 1 d . . . H52 H -0.0133 0.6052 0.1634 0.021 Uiso 1 1 calc R . . C53 C -0.0499(5) 0.8214(4) 0.4087(3) 0.0249(12) Uani 1 1 d . . . H53 H -0.0872 0.8281 0.3665 0.030 Uiso 1 1 calc R . . C54 C 0.0335(4) 0.7625(3) 0.4070(3) 0.0180(11) Uani 1 1 d . . . C55 C 0.0750(4) 0.7684(3) 0.4785(3) 0.0178(11) Uani 1 1 d . . . H55 H 0.1344 0.7339 0.4883 0.021 Uiso 1 1 calc R . . C56 C 0.0176(4) 0.8324(3) 0.5352(3) 0.0169(10) Uani 1 1 d . . . H56 H 0.0315 0.8450 0.5860 0.020 Uiso 1 1 calc R . . C57 C 0.4512(5) 0.2831(3) 0.0832(3) 0.0155(10) Uani 1 1 d . . . C58 C 0.5392(5) 0.3093(3) 0.1515(3) 0.0151(10) Uani 1 1 d . . . C59 C 0.6460(5) 0.2729(3) 0.1596(3) 0.0170(11) Uani 1 1 d . . . C60 C 0.5068(5) 0.3715(3) 0.2149(3) 0.0190(11) Uani 1 1 d . . . H60 H 0.4362 0.3999 0.2119 0.023 Uiso 1 1 calc R . . C61 C 0.5739(5) 0.3932(3) 0.2819(3) 0.0191(11) Uani 1 1 d . . . H61 H 0.5487 0.4362 0.3239 0.023 Uiso 1 1 calc R . . C62 C 0.7145(5) 0.2931(3) 0.2262(3) 0.0158(10) Uani 1 1 d . . . H62 H 0.7864 0.2659 0.2288 0.019 Uiso 1 1 calc R . . C63 C 0.6786(5) 0.3531(3) 0.2894(3) 0.0160(10) Uani 1 1 d . . . C64 C 0.7522(5) 0.3757(3) 0.3606(3) 0.0174(11) Uani 1 1 d . . . C65 C 0.7171(5) 0.4282(4) 0.4267(3) 0.0241(12) Uani 1 1 d . . . H65 H 0.6420 0.4521 0.4318 0.029 Uiso 1 1 calc R . . C66 C 0.8684(5) 0.3497(4) 0.3707(3) 0.0226(12) Uani 1 1 d . . . H66 H 0.9075 0.3127 0.3319 0.027 Uiso 1 1 calc R . . C67 C 0.9201(5) 0.3848(4) 0.4450(3) 0.0219(12) Uani 1 1 d . . . H67 H 0.9978 0.3754 0.4620 0.026 Uiso 1 1 calc R . . N1 N -0.2232(4) 0.2951(3) -0.1026(2) 0.0196(10) Uani 1 1 d . . . N2 N 0.1827(4) 0.3387(3) 0.2673(3) 0.0246(11) Uani 1 1 d . . . N3 N 0.3239(4) 0.5628(3) 0.2863(2) 0.0222(10) Uani 1 1 d . . . N4 N 0.6955(4) 0.2148(3) 0.0954(3) 0.0219(10) Uani 1 1 d . . . N5 N 0.3031(4) 0.1762(3) -0.2702(2) 0.0203(10) Uani 1 1 d . B . N6 N 0.1696(4) -0.0477(3) -0.2873(2) 0.0181(9) Uani 1 1 d . C . O1 O 0.3557(3) 0.0330(2) -0.0732(2) 0.0189(8) Uani 1 1 d . . . O2 O 0.2036(3) 0.0471(2) -0.1449(2) 0.0195(8) Uani 1 1 d . . . O3 O 0.1749(4) 0.0090(2) -0.3101(2) 0.0244(9) Uani 1 1 d . . . O4 O 0.0780(3) -0.0806(3) -0.2813(2) 0.0263(9) Uani 1 1 d . . . O5 O 0.3415(4) 0.3273(2) -0.1013(2) 0.0215(8) Uani 1 1 d . B . O6 O 0.2810(3) 0.2284(2) -0.06620(19) 0.0162(7) Uani 1 1 d . B . O7 O 0.3106(4) 0.1650(3) -0.3336(2) 0.0326(10) Uani 1 1 d . . . O8 O 0.2181(3) 0.2065(2) -0.2383(2) 0.0236(9) Uani 1 1 d . . . O9 O 0.4239(3) 0.3420(2) 0.06085(19) 0.0173(8) Uani 1 1 d . . . O10 O 0.4065(3) 0.2077(2) 0.0575(2) 0.0191(8) Uani 1 1 d . . . O11 O 0.6663(4) 0.2213(3) 0.0369(2) 0.0294(10) Uani 1 1 d . . . O12 O 0.7662(4) 0.1644(3) 0.1031(2) 0.0336(10) Uani 1 1 d . . . O13 O 0.0627(3) 0.3067(2) -0.0611(2) 0.0183(8) Uani 1 1 d . . . O14 O 0.0436(3) 0.1745(2) -0.06128(19) 0.0173(8) Uani 1 1 d . . . O15 O -0.1886(4) 0.2938(3) -0.0428(2) 0.0261(9) Uani 1 1 d . . . O16 O -0.3007(4) 0.3404(3) -0.1120(2) 0.0323(10) Uani 1 1 d . . . O17 O 0.1838(3) 0.2917(2) 0.06914(18) 0.0166(7) Uani 1 1 d . . . O18 O 0.0995(4) 0.1915(2) 0.0936(2) 0.0265(9) Uani 1 1 d . . . O19 O 0.2546(4) 0.2986(3) 0.2282(2) 0.0349(8) Uani 1 1 d . . . O20 O 0.1906(4) 0.3536(3) 0.3327(2) 0.0349(8) Uani 1 1 d . . . O21 O 0.1012(3) 0.4851(2) 0.08220(19) 0.0216(8) Uani 1 1 d . . . O22 O 0.2695(3) 0.4735(2) 0.1434(2) 0.0203(8) Uani 1 1 d . . . O23 O 0.4117(3) 0.5990(3) 0.2792(2) 0.0331(10) Uani 1 1 d . . . O24 O 0.3243(4) 0.5031(3) 0.3062(2) 0.0324(10) Uani 1 1 d . . . O25 O 0.3866(3) 0.4883(2) 0.0294(2) 0.0181(8) Uani 1 1 d . . . O26 O 0.1617(4) 0.4681(2) -0.0560(2) 0.0236(8) Uani 1 1 d . . . O27 O 0.1010(3) 0.0155(2) -0.03419(19) 0.0159(7) Uani 1 1 d . . . O28 O 0.2847(4) 0.0798(3) 0.0820(2) 0.0308(10) Uani 1 1 d . . . O90 O 0.1587(3) 0.9190(2) 0.0505(2) 0.0172(8) Uani 1 1 d . . . O91 O 0.5366(3) 0.5689(3) 0.1519(2) 0.0237(9) Uani 1 1 d . . . O92 O 0.3457(3) 0.5847(2) 0.9460(2) 0.0199(8) Uani 1 1 d . . . O93 O 0.9656(3) 0.9140(3) 0.8415(2) 0.0238(8) Uani 1 1 d . . . O94 O 0.4153(7) 0.9569(5) 0.0205(5) 0.0277(18) Uani 0.50 1 d P . . 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 S6A 0.0189(11) 0.0325(12) 0.0433(14) 0.0100(11) 0.0062(10) 0.0089(9) C42A 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C43A 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C44A 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C45A 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) S6B 0.0189(11) 0.0325(12) 0.0433(14) 0.0100(11) 0.0062(10) 0.0089(9) C42B 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C43B 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C44B 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) C45B 0.0115(16) 0.0251(17) 0.0293(17) 0.0150(14) 0.0029(13) -0.0010(14) S3A 0.0131(11) 0.0259(13) 0.0422(13) 0.0110(10) 0.0071(9) 0.0083(8) C13A 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C14A 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C15A 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C16A 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) S3B 0.0131(11) 0.0259(13) 0.0422(13) 0.0110(10) 0.0071(9) 0.0083(8) C13B 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C14B 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C15B 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) C16B 0.0110(16) 0.0193(16) 0.0281(16) 0.0109(13) 0.0042(13) -0.0010(13) S2A 0.0277(10) 0.0334(15) 0.0351(11) 0.0082(10) 0.0149(9) 0.0165(9) C9A 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C10A 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C11A 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C12A 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) S2B 0.0277(10) 0.0334(15) 0.0351(11) 0.0082(10) 0.0149(9) 0.0165(9) C9B 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C10B 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C11B 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) C12B 0.0120(15) 0.0162(16) 0.0267(17) 0.0067(13) 0.0047(12) 0.0009(13) Tb1 0.01492(13) 0.01355(12) 0.01313(12) 0.00583(9) 0.00240(9) -0.00343(9) Tb2 0.01952(14) 0.01254(12) 0.01123(12) 0.00422(9) 0.00340(9) -0.00411(10) S1 0.0330(9) 0.0367(9) 0.0296(8) 0.0095(7) 0.0006(7) -0.0023(7) S4 0.0349(9) 0.0393(9) 0.0248(8) 0.0086(7) 0.0001(7) -0.0062(7) S5 0.0337(10) 0.0371(9) 0.0542(11) 0.0075(8) 0.0188(9) 0.0142(8) C2 0.026(3) 0.015(2) 0.014(2) 0.007(2) 0.004(2) -0.006(2) C3 0.015(3) 0.012(2) 0.018(3) 0.0071(19) 0.004(2) -0.0014(19) C4 0.013(2) 0.017(2) 0.019(3) 0.007(2) -0.003(2) -0.006(2) C5 0.009(2) 0.016(2) 0.029(3) 0.012(2) 0.001(2) -0.0003(19) C6 0.009(2) 0.013(2) 0.025(3) 0.010(2) 0.005(2) -0.0020(19) C7 0.009(2) 0.017(2) 0.016(2) 0.006(2) 0.0012(19) -0.0019(19) C8 0.012(2) 0.018(2) 0.019(3) 0.009(2) 0.002(2) 0.000(2) C17 0.012(2) 0.018(2) 0.023(3) 0.012(2) 0.000(2) -0.005(2) C18 0.011(2) 0.022(3) 0.014(2) 0.008(2) 0.0026(19) -0.001(2) C19 0.013(2) 0.021(2) 0.015(2) 0.010(2) 0.0010(19) 0.001(2) C20 0.020(3) 0.015(2) 0.016(3) 0.007(2) 0.005(2) -0.004(2) C21 0.021(3) 0.021(3) 0.015(2) 0.010(2) -0.002(2) -0.003(2) C22 0.015(3) 0.023(3) 0.020(3) 0.012(2) -0.003(2) -0.003(2) C23 0.018(3) 0.018(2) 0.011(2) 0.003(2) 0.000(2) -0.001(2) C24 0.011(2) 0.016(2) 0.017(2) 0.007(2) 0.0066(19) 0.0017(19) C25 0.015(2) 0.014(2) 0.020(3) 0.011(2) 0.007(2) 0.0014(19) C26 0.013(2) 0.017(2) 0.020(3) 0.008(2) 0.006(2) 0.004(2) C27 0.019(3) 0.014(2) 0.018(3) 0.006(2) 0.006(2) 0.004(2) C28 0.018(3) 0.010(2) 0.018(3) 0.0049(19) 0.005(2) -0.0011(19) C29 0.013(2) 0.012(2) 0.026(3) 0.010(2) 0.007(2) 0.0011(19) C30 0.013(2) 0.012(2) 0.019(3) 0.0062(19) 0.009(2) 0.0027(19) C31 0.020(3) 0.015(2) 0.020(3) 0.007(2) 0.004(2) -0.002(2) C32 0.023(3) 0.020(3) 0.023(3) 0.008(2) 0.000(2) -0.002(2) C33 0.008(2) 0.020(3) 0.029(3) 0.016(2) 0.001(2) -0.002(2) C34 0.015(3) 0.022(3) 0.027(3) 0.012(2) 0.003(2) -0.001(2) C35 0.026(3) 0.021(3) 0.011(2) 0.005(2) 0.005(2) -0.002(2) C36 0.026(3) 0.027(3) 0.015(3) 0.009(2) -0.001(2) -0.007(2) C37 0.018(3) 0.020(3) 0.019(3) 0.009(2) 0.005(2) -0.001(2) C38 0.015(3) 0.027(3) 0.013(2) 0.008(2) 0.004(2) 0.001(2) C39 0.014(3) 0.030(3) 0.011(2) 0.009(2) -0.0015(19) -0.003(2) C40 0.009(2) 0.022(3) 0.020(3) 0.012(2) 0.003(2) -0.003(2) C41 0.018(3) 0.023(3) 0.024(3) 0.016(2) -0.002(2) -0.001(2) C46 0.022(3) 0.015(2) 0.018(3) 0.008(2) 0.006(2) -0.002(2) C47 0.017(3) 0.015(2) 0.015(2) 0.007(2) 0.002(2) -0.004(2) C48 0.009(2) 0.019(2) 0.016(2) 0.009(2) -0.0009(19) -0.0002(19) C49 0.010(2) 0.018(2) 0.017(2) 0.006(2) 0.0027(19) 0.0042(19) C50 0.008(2) 0.016(2) 0.018(2) 0.009(2) 0.0021(19) -0.0003(19) C51 0.004(2) 0.021(3) 0.030(3) 0.017(2) -0.002(2) -0.0004(19) C52 0.016(3) 0.021(3) 0.018(3) 0.010(2) -0.002(2) -0.007(2) C53 0.017(3) 0.026(3) 0.030(3) 0.008(2) 0.008(2) 0.007(2) C54 0.010(2) 0.016(2) 0.028(3) 0.008(2) 0.004(2) 0.0023(19) C55 0.009(2) 0.017(2) 0.024(3) 0.005(2) 0.004(2) 0.0048(19) C56 0.006(2) 0.020(3) 0.018(3) 0.001(2) 0.0003(19) -0.0022(19) C57 0.016(3) 0.018(2) 0.014(2) 0.007(2) 0.005(2) -0.001(2) C58 0.018(3) 0.014(2) 0.015(2) 0.0065(19) 0.002(2) -0.007(2) C59 0.018(3) 0.017(2) 0.017(3) 0.006(2) 0.007(2) -0.004(2) C60 0.019(3) 0.020(3) 0.019(3) 0.010(2) 0.002(2) 0.002(2) C61 0.027(3) 0.014(2) 0.017(3) 0.005(2) 0.006(2) 0.000(2) C62 0.012(2) 0.016(2) 0.019(3) 0.006(2) 0.003(2) -0.0014(19) C63 0.015(3) 0.014(2) 0.021(3) 0.008(2) 0.004(2) -0.003(2) C64 0.019(3) 0.015(2) 0.017(3) 0.005(2) 0.002(2) -0.006(2) C65 0.022(3) 0.027(3) 0.019(3) 0.005(2) -0.001(2) -0.007(2) C66 0.022(3) 0.023(3) 0.021(3) 0.008(2) 0.002(2) -0.001(2) C67 0.011(3) 0.028(3) 0.035(3) 0.025(3) -0.007(2) -0.004(2) N1 0.017(2) 0.021(2) 0.021(2) 0.0075(19) 0.0053(19) -0.0019(19) N2 0.021(2) 0.039(3) 0.019(2) 0.014(2) 0.0082(19) 0.014(2) N3 0.015(2) 0.029(3) 0.015(2) -0.0001(19) 0.0013(18) 0.007(2) N4 0.014(2) 0.024(2) 0.022(2) 0.0017(19) 0.0079(19) -0.0027(19) N5 0.020(2) 0.023(2) 0.020(2) 0.0096(19) 0.0057(19) 0.0046(19) N6 0.013(2) 0.025(2) 0.013(2) 0.0046(18) 0.0014(17) 0.0065(18) O1 0.021(2) 0.0163(18) 0.0183(19) 0.0062(15) 0.0002(15) -0.0021(15) O2 0.018(2) 0.0217(19) 0.0184(19) 0.0069(15) 0.0047(15) 0.0025(16) O3 0.023(2) 0.025(2) 0.025(2) 0.0099(17) 0.0038(17) 0.0122(17) O4 0.0077(18) 0.043(2) 0.026(2) 0.0109(19) 0.0030(15) -0.0013(17) O5 0.032(2) 0.0167(18) 0.0175(19) 0.0066(15) 0.0110(16) -0.0031(16) O6 0.0178(19) 0.0175(17) 0.0142(17) 0.0063(14) 0.0055(14) -0.0032(14) O7 0.028(2) 0.056(3) 0.023(2) 0.023(2) 0.0116(18) 0.023(2) O8 0.020(2) 0.027(2) 0.024(2) 0.0095(17) 0.0076(17) 0.0117(17) O9 0.0199(19) 0.0161(17) 0.0175(18) 0.0079(15) 0.0046(15) -0.0011(15) O10 0.021(2) 0.0161(17) 0.0199(19) 0.0075(15) 0.0014(15) -0.0043(15) O11 0.023(2) 0.045(3) 0.015(2) 0.0056(18) 0.0066(16) -0.0064(19) O12 0.029(2) 0.036(2) 0.028(2) 0.0017(19) 0.0098(19) 0.009(2) O13 0.021(2) 0.0128(17) 0.0203(19) 0.0054(14) 0.0043(15) -0.0015(15) O14 0.0184(19) 0.0167(17) 0.0172(18) 0.0071(14) 0.0031(15) -0.0040(15) O15 0.025(2) 0.036(2) 0.022(2) 0.0136(18) 0.0083(17) 0.0100(18) O16 0.030(2) 0.034(2) 0.030(2) 0.0078(19) 0.0071(19) 0.022(2) O17 0.023(2) 0.0156(17) 0.0122(17) 0.0059(14) 0.0052(15) -0.0019(15) O18 0.041(3) 0.0160(18) 0.026(2) 0.0094(16) 0.0160(19) -0.0017(17) O19 0.0272(17) 0.056(2) 0.0261(16) 0.0177(15) 0.0134(13) 0.0244(15) O20 0.0272(17) 0.056(2) 0.0261(16) 0.0177(15) 0.0134(13) 0.0244(15) O21 0.028(2) 0.0201(19) 0.0131(18) 0.0039(15) -0.0019(16) -0.0039(16) O22 0.024(2) 0.0180(18) 0.0161(18) 0.0026(15) 0.0076(16) 0.0021(16) O23 0.013(2) 0.045(3) 0.028(2) 0.000(2) 0.0043(17) 0.0017(18) O24 0.034(3) 0.039(3) 0.026(2) 0.0142(19) 0.0060(19) 0.025(2) O25 0.0177(19) 0.0157(17) 0.0237(19) 0.0100(15) 0.0060(15) -0.0002(14) O26 0.027(2) 0.023(2) 0.023(2) 0.0124(16) -0.0011(17) -0.0048(17) O27 0.0118(17) 0.0151(17) 0.0213(19) 0.0075(15) 0.0039(14) -0.0005(14) O28 0.025(2) 0.043(3) 0.033(2) 0.027(2) -0.0081(18) -0.0116(19) O90 0.0158(18) 0.0149(17) 0.0203(19) 0.0062(15) 0.0030(15) -0.0002(14) O91 0.020(2) 0.029(2) 0.027(2) 0.0162(18) 0.0038(17) 0.0008(17) O92 0.0143(19) 0.0221(19) 0.027(2) 0.0134(16) 0.0043(16) 0.0001(15) O93 0.019(2) 0.031(2) 0.023(2) 0.0125(17) 0.0012(16) 0.0000(17) O94 0.028(5) 0.022(4) 0.032(5) 0.012(4) -0.001(4) 0.001(3) _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 S6A C44A 1.682(18) . ? S6A C45A 1.848(16) . ? C42A C45A 1.36(2) . ? C42A C43A 1.395(18) . ? C42A H42A 0.9500 . ? C43A C44A 1.39(2) . ? C43A C40 1.474(8) . ? C44A H44A 0.9500 . ? C45A H45A 0.9500 . ? S6B C44B 1.674(10) . ? S6B C45B 1.781(10) . ? C42B C45B 1.398(14) . ? C42B H42B 0.9500 . ? C44B H44B 0.9500 . ? C45B H45B 0.9500 . ? S3A C16A 1.691(10) . ? S3A C13A 1.749(9) . ? C13A C14A 1.354(13) . ? C13A H13A 0.9500 . ? C14A C15A 1.407(12) . ? C14A H14A 0.9500 . ? C15A C16A 1.383(12) . ? C15A C17 1.470(7) . ? C16A H16A 0.9500 . ? S3B C16B 1.688(19) . ? S3B C13B 1.748(17) . ? C13B C14B 1.37(2) . ? C13B H13B 0.9500 . ? C14B H14B 0.9500 . ? C16B H16B 0.9500 . ? S2A C9A 1.710(7) . ? S2A C12A 1.729(9) . ? C9A C10A 1.380(9) . ? C9A H9A 0.9500 . ? C10A C11A 1.440(9) . ? C10A C6 1.469(7) . ? C11A C12A 1.388(12) . ? C11A H11A 0.9500 . ? C12A H12A 0.9500 . ? S2B C9B 1.72(2) . ? S2B C12B 1.72(2) . ? C9B H9B 0.9500 . ? C11B C12B 1.39(2) . ? C11B H11B 0.9500 . ? C12B H12B 0.9500 . ? Tb1 O27 2.340(3) . ? Tb1 O6 2.348(3) . ? Tb1 O14 2.373(4) . ? Tb1 O10 2.379(4) . ? Tb1 O1 2.398(4) . ? Tb1 O28 2.460(4) . ? Tb1 O2 2.503(4) . ? Tb1 O18 2.536(4) . ? Tb1 O17 2.540(4) . ? Tb2 O25 2.339(3) . ? Tb2 O17 2.355(3) . ? Tb2 O13 2.385(4) . ? Tb2 O9 2.416(4) . ? Tb2 O22 2.448(4) . ? Tb2 O26 2.473(4) . ? Tb2 O21 2.484(4) . ? Tb2 O5 2.531(4) . ? Tb2 O6 2.536(4) . ? S1 C33 1.682(6) . ? S1 C32 1.696(6) . ? S4 C67 1.664(6) . ? S4 C65 1.709(6) . ? S5 C53 1.679(6) . ? S5 C56 1.690(6) . ? C2 O2 1.236(7) . ? C2 O1 1.279(6) . ? C2 C3 1.511(7) . ? C3 C8 1.384(7) . ? C3 C4 1.386(7) . ? C4 C5 1.385(7) . ? C4 H4 0.9500 . ? C5 C6 1.405(7) . ? C5 H5 0.9500 . ? C6 C7 1.390(7) . ? C7 C8 1.378(7) . ? C7 H7 0.9500 . ? C8 N6 1.479(7) . ? C17 C18 1.400(7) . ? C17 C22 1.406(7) . ? C18 C19 1.373(7) . ? C18 H18 0.9500 . ? C19 C20 1.394(7) . ? C19 N5 1.456(7) . ? C20 C21 1.390(8) . ? C20 C23 1.508(7) . ? C21 C22 1.390(8) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 O6 1.260(6) . ? C23 O5 1.260(6) . ? C24 O13 1.247(6) . ? C24 O14 1.259(6) . ? C24 C25 1.510(7) . ? C25 C30 1.384(7) . ? C25 C26 1.400(7) . ? C26 C27 1.384(7) . ? C26 H26 0.9500 . ? C27 C28 1.392(7) . ? C27 H27 0.9500 . ? C28 C29 1.396(7) . ? C28 C31 1.474(7) . ? C29 C30 1.371(7) . ? C29 H29 0.9500 . ? C30 N1 1.468(6) . ? C31 C32 1.385(7) . ? C31 C34 1.427(8) . ? C32 H32 0.9500 . ? C33 C34 1.440(8) . ? C33 H33 0.9500 . ? C34 H34 0.9500 . ? C35 O18 1.238(6) . ? C35 O17 1.273(6) . ? C35 C37 1.502(7) . ? C36 C41 1.384(8) . ? C36 C37 1.393(8) . ? C36 H36 0.9500 . ? C37 C38 1.384(7) . ? C38 C39 1.385(7) . ? C38 N2 1.457(7) . ? C39 C40 1.402(7) . ? C39 H39 0.9500 . ? C40 C41 1.388(7) . ? C41 H41 0.9500 . ? C46 O22 1.256(7) . ? C46 O21 1.265(6) . ? C46 C47 1.496(7) . ? C47 C48 1.385(7) . ? C47 C52 1.400(8) . ? C48 C49 1.384(7) . ? C48 N3 1.482(7) . ? C49 C50 1.387(7) . ? C49 H49 0.9500 . ? C50 C51 1.386(7) . ? C50 C54 1.481(7) . ? C51 C52 1.381(7) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 C54 1.376(8) . ? C53 H53 0.9500 . ? C54 C55 1.421(8) . ? C55 C56 1.455(7) . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 O10 1.249(6) . ? C57 O9 1.268(6) . ? C57 C58 1.508(7) . ? C58 C60 1.389(7) . ? C58 C59 1.391(8) . ? C59 C62 1.380(7) . ? C59 N4 1.460(7) . ? C60 C61 1.376(8) . ? C60 H60 0.9500 . ? C61 C63 1.400(8) . ? C61 H61 0.9500 . ? C62 C63 1.388(7) . ? C62 H62 0.9500 . ? C63 C64 1.474(7) . ? C64 C65 1.386(7) . ? C64 C66 1.418(8) . ? C65 H65 0.9500 . ? C66 C67 1.419(8) . ? C66 H66 0.9500 . ? C67 H67 0.9500 . ? N1 O16 1.221(6) . ? N1 O15 1.227(6) . ? N2 O19 1.222(6) . ? N2 O20 1.229(6) . ? N3 O23 1.221(6) . ? N3 O24 1.222(6) . ? N4 O12 1.218(6) . ? N4 O11 1.230(6) . ? N5 O7 1.226(6) . ? N5 O8 1.229(6) . ? N6 O3 1.216(6) . ? N6 O4 1.220(6) . ? 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 C44A S6A C45A 90.9(10) . . ? C45A C42A C43A 115.0(16) . . ? C45A C42A H42A 122.5 . . ? C43A C42A H42A 122.5 . . ? C44A C43A C42A 111.6(10) . . ? C44A C43A C40 125.3(9) . . ? C42A C43A C40 120.0(9) . . ? C43A C44A S6A 110.7(14) . . ? C43A C44A H44A 124.6 . . ? S6A C44A H44A 124.6 . . ? C42A C45A S6A 106.6(14) . . ? C42A C45A H45A 126.7 . . ? S6A C45A H45A 126.7 . . ? C44B S6B C45B 94.0(5) . . ? C45B C42B H42B 121.5 . . ? S6B C44B H44B 123.6 . . ? C42B C45B S6B 105.3(8) . . ? C42B C45B H45B 127.3 . . ? S6B C45B H45B 127.3 . . ? C16A S3A C13A 91.3(5) . . ? C14A C13A S3A 110.6(7) . . ? C14A C13A H13A 124.7 . . ? S3A C13A H13A 124.7 . . ? C13A C14A C15A 113.8(9) . . ? C13A C14A H14A 123.1 . . ? C15A C14A H14A 123.1 . . ? C16A C15A C14A 111.3(6) . . ? C16A C15A C17 124.3(6) . . ? C14A C15A C17 123.9(6) . . ? C15A C16A S3A 112.6(7) . . ? C15A C16A H16A 123.7 . . ? S3A C16A H16A 123.7 . . ? C16B S3B C13B 88.5(11) . . ? C14B C13B S3B 113.3(17) . . ? C14B C13B H13B 123.3 . . ? S3B C13B H13B 123.3 . . ? C13B C14B H14B 125.5 . . ? S3B C16B H16B 123.0 . . ? C9A S2A C12A 93.2(4) . . ? C10A C9A S2A 111.5(5) . . ? C10A C9A H9A 124.3 . . ? S2A C9A H9A 124.3 . . ? C9A C10A C11A 112.1(5) . . ? C9A C10A C6 122.3(5) . . ? C11A C10A C6 125.6(5) . . ? C12A C11A C10A 112.9(7) . . ? C12A C11A H11A 123.6 . . ? C10A C11A H11A 123.6 . . ? C11A C12A S2A 110.0(6) . . ? C11A C12A H12A 125.0 . . ? S2A C12A H12A 125.0 . . ? C9B S2B C12B 91.9(15) . . ? S2B C9B H9B 124.6 . . ? C12B C11B H11B 123.5 . . ? C11B C12B S2B 107(2) . . ? C11B C12B H12B 126.4 . . ? S2B C12B H12B 126.4 . . ? O27 Tb1 O6 141.51(12) . . ? O27 Tb1 O14 79.23(12) . . ? O6 Tb1 O14 75.10(12) . . ? O27 Tb1 O10 140.32(13) . . ? O6 Tb1 O10 74.47(12) . . ? O14 Tb1 O10 138.29(12) . . ? O27 Tb1 O1 83.04(12) . . ? O6 Tb1 O1 90.44(12) . . ? O14 Tb1 O1 127.75(12) . . ? O10 Tb1 O1 80.21(13) . . ? O27 Tb1 O28 71.25(13) . . ? O6 Tb1 O28 144.67(13) . . ? O14 Tb1 O28 136.83(13) . . ? O10 Tb1 O28 70.47(13) . . ? O1 Tb1 O28 79.59(14) . . ? O27 Tb1 O2 72.08(12) . . ? O6 Tb1 O2 73.75(12) . . ? O14 Tb1 O2 74.63(13) . . ? O10 Tb1 O2 122.05(12) . . ? O1 Tb1 O2 53.16(13) . . ? O28 Tb1 O2 122.40(14) . . ? O27 Tb1 O18 78.05(12) . . ? O6 Tb1 O18 121.11(12) . . ? O14 Tb1 O18 75.14(13) . . ? O10 Tb1 O18 97.28(13) . . ? O1 Tb1 O18 146.74(12) . . ? O28 Tb1 O18 68.54(14) . . ? O2 Tb1 O18 140.66(13) . . ? O27 Tb1 O17 125.61(12) . . ? O6 Tb1 O17 71.69(11) . . ? O14 Tb1 O17 71.32(12) . . ? O10 Tb1 O17 72.45(13) . . ? O1 Tb1 O17 150.40(12) . . ? O28 Tb1 O17 101.21(13) . . ? O2 Tb1 O17 136.31(12) . . ? O18 Tb1 O17 50.96(11) . . ? O25 Tb2 O17 139.79(13) . . ? O25 Tb2 O13 144.36(13) . . ? O17 Tb2 O13 75.78(12) . . ? O25 Tb2 O9 72.31(12) . . ? O17 Tb2 O9 75.04(12) . . ? O13 Tb2 O9 135.61(12) . . ? O25 Tb2 O22 73.80(13) . . ? O17 Tb2 O22 75.37(12) . . ? O13 Tb2 O22 128.04(13) . . ? O9 Tb2 O22 74.50(13) . . ? O25 Tb2 O26 72.56(13) . . ? O17 Tb2 O26 143.14(13) . . ? O13 Tb2 O26 73.33(12) . . ? O9 Tb2 O26 141.82(12) . . ? O22 Tb2 O26 109.15(13) . . ? O25 Tb2 O21 94.76(12) . . ? O17 Tb2 O21 86.82(12) . . ? O13 Tb2 O21 83.06(12) . . ? O9 Tb2 O21 127.46(12) . . ? O22 Tb2 O21 53.15(13) . . ? O26 Tb2 O21 70.02(13) . . ? O25 Tb2 O5 73.96(12) . . ? O17 Tb2 O5 122.57(12) . . ? O13 Tb2 O5 88.17(13) . . ? O9 Tb2 O5 80.26(13) . . ? O22 Tb2 O5 143.73(13) . . ? O26 Tb2 O5 76.13(13) . . ? O21 Tb2 O5 146.13(12) . . ? O25 Tb2 O6 116.41(12) . . ? O17 Tb2 O6 71.65(11) . . ? O13 Tb2 O6 69.98(12) . . ? O9 Tb2 O6 69.46(12) . . ? O22 Tb2 O6 135.98(12) . . ? O26 Tb2 O6 114.76(12) . . ? O21 Tb2 O6 148.68(12) . . ? O5 Tb2 O6 51.15(11) . . ? C33 S1 C32 94.6(3) . . ? C67 S4 C65 93.9(3) . . ? C53 S5 C56 95.6(3) . . ? O2 C2 O1 121.6(5) . . ? O2 C2 C3 120.5(5) . . ? O1 C2 C3 118.0(5) . . ? C8 C3 C4 116.2(5) . . ? C8 C3 C2 122.1(5) . . ? C4 C3 C2 121.6(5) . . ? C5 C4 C3 121.8(5) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 120.9(5) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C7 C6 C5 117.6(5) . . ? C7 C6 C10A 120.3(5) . . ? C5 C6 C10A 122.1(5) . . ? C8 C7 C6 119.8(5) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C3 123.6(5) . . ? C7 C8 N6 114.5(4) . . ? C3 C8 N6 121.8(5) . . ? C18 C17 C22 117.0(5) . . ? C18 C17 C15A 120.5(5) . . ? C22 C17 C15A 122.5(5) . . ? C19 C18 C17 120.2(5) . . ? C19 C18 H18 119.9 . . ? C17 C18 H18 119.9 . . ? C18 C19 C20 123.4(5) . . ? C18 C19 N5 116.7(5) . . ? C20 C19 N5 119.9(5) . . ? C21 C20 C19 116.7(5) . . ? C21 C20 C23 117.6(5) . . ? C19 C20 C23 125.7(5) . . ? C20 C21 C22 120.8(5) . . ? C20 C21 H21 119.6 . . ? C22 C21 H21 119.6 . . ? C21 C22 C17 121.9(5) . . ? C21 C22 H22 119.1 . . ? C17 C22 H22 119.1 . . ? O6 C23 O5 120.5(5) . . ? O6 C23 C20 117.9(5) . . ? O5 C23 C20 121.2(5) . . ? O13 C24 O14 126.9(5) . . ? O13 C24 C25 117.4(4) . . ? O14 C24 C25 115.5(4) . . ? C30 C25 C26 116.5(5) . . ? C30 C25 C24 125.7(5) . . ? C26 C25 C24 117.7(4) . . ? C27 C26 C25 120.9(5) . . ? C27 C26 H26 119.6 . . ? C25 C26 H26 119.6 . . ? C26 C27 C28 121.4(5) . . ? C26 C27 H27 119.3 . . ? C28 C27 H27 119.3 . . ? C27 C28 C29 117.9(5) . . ? C27 C28 C31 122.2(5) . . ? C29 C28 C31 119.9(5) . . ? C30 C29 C28 119.8(5) . . ? C30 C29 H29 120.1 . . ? C28 C29 H29 120.1 . . ? C29 C30 C25 123.5(5) . . ? C29 C30 N1 116.7(5) . . ? C25 C30 N1 119.7(5) . . ? C32 C31 C34 110.3(5) . . ? C32 C31 C28 124.2(5) . . ? C34 C31 C28 125.5(5) . . ? C31 C32 S1 112.6(4) . . ? C31 C32 H32 123.7 . . ? S1 C32 H32 123.7 . . ? C34 C33 S1 108.9(4) . . ? C34 C33 H33 125.6 . . ? S1 C33 H33 125.6 . . ? C31 C34 C33 113.6(5) . . ? C31 C34 H34 123.2 . . ? C33 C34 H34 123.2 . . ? O18 C35 O17 120.9(5) . . ? O18 C35 C37 120.0(5) . . ? O17 C35 C37 118.9(5) . . ? C41 C36 C37 120.8(5) . . ? C41 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 117.2(5) . . ? C38 C37 C35 124.6(5) . . ? C36 C37 C35 118.1(5) . . ? C37 C38 C39 122.3(5) . . ? C37 C38 N2 120.7(5) . . ? C39 C38 N2 116.9(5) . . ? C38 C39 C40 120.3(5) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 117.2(5) . . ? C41 C40 C43A 122.3(5) . . ? C39 C40 C43A 120.6(5) . . ? C36 C41 C40 122.0(5) . . ? C36 C41 H41 119.0 . . ? C40 C41 H41 119.0 . . ? O22 C46 O21 122.2(5) . . ? O22 C46 C47 118.4(5) . . ? O21 C46 C47 119.5(5) . . ? C48 C47 C52 115.9(5) . . ? C48 C47 C46 123.3(5) . . ? C52 C47 C46 120.8(5) . . ? C49 C48 C47 123.4(5) . . ? C49 C48 N3 114.0(4) . . ? C47 C48 N3 122.6(5) . . ? C48 C49 C50 119.7(5) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C51 C50 C49 118.1(5) . . ? C51 C50 C54 121.2(5) . . ? C49 C50 C54 120.7(5) . . ? C52 C51 C50 121.4(5) . . ? C52 C51 H51 119.3 . . ? C50 C51 H51 119.3 . . ? C51 C52 C47 121.5(5) . . ? C51 C52 H52 119.3 . . ? C47 C52 H52 119.3 . . ? C54 C53 S5 112.4(5) . . ? C54 C53 H53 123.8 . . ? S5 C53 H53 123.8 . . ? C53 C54 C55 111.1(5) . . ? C53 C54 C50 124.0(5) . . ? C55 C54 C50 124.9(5) . . ? C54 C55 C56 113.5(5) . . ? C54 C55 H55 123.3 . . ? C56 C55 H55 123.3 . . ? C55 C56 S5 107.4(4) . . ? C55 C56 H56 126.3 . . ? S5 C56 H56 126.3 . . ? O10 C57 O9 126.6(5) . . ? O10 C57 C58 116.9(4) . . ? O9 C57 C58 116.3(4) . . ? C60 C58 C59 115.8(5) . . ? C60 C58 C57 117.1(5) . . ? C59 C58 C57 126.9(5) . . ? C62 C59 C58 123.2(5) . . ? C62 C59 N4 116.3(5) . . ? C58 C59 N4 120.3(5) . . ? C61 C60 C58 122.1(5) . . ? C61 C60 H60 118.9 . . ? C58 C60 H60 118.9 . . ? C60 C61 C63 121.3(5) . . ? C60 C61 H61 119.4 . . ? C63 C61 H61 119.4 . . ? C59 C62 C63 120.2(5) . . ? C59 C62 H62 119.9 . . ? C63 C62 H62 119.9 . . ? C62 C63 C61 117.3(5) . . ? C62 C63 C64 120.4(5) . . ? C61 C63 C64 122.2(5) . . ? C65 C64 C66 111.0(5) . . ? C65 C64 C63 123.7(5) . . ? C66 C64 C63 125.2(5) . . ? C64 C65 S4 111.6(5) . . ? C64 C65 H65 124.2 . . ? S4 C65 H65 124.2 . . ? C64 C66 C67 112.8(5) . . ? C64 C66 H66 123.6 . . ? C67 C66 H66 123.6 . . ? C66 C67 S4 110.6(4) . . ? C66 C67 H67 124.7 . . ? S4 C67 H67 124.7 . . ? O16 N1 O15 123.3(5) . . ? O16 N1 C30 118.7(5) . . ? O15 N1 C30 117.9(5) . . ? O19 N2 O20 123.2(5) . . ? O19 N2 C38 118.2(5) . . ? O20 N2 C38 118.6(4) . . ? O23 N3 O24 125.3(5) . . ? O23 N3 C48 117.3(5) . . ? O24 N3 C48 117.2(5) . . ? O12 N4 O11 123.5(5) . . ? O12 N4 C59 118.5(5) . . ? O11 N4 C59 118.0(5) . . ? O7 N5 O8 124.2(5) . . ? O7 N5 C19 118.1(4) . . ? O8 N5 C19 117.7(4) . . ? O3 N6 O4 124.7(5) . . ? O3 N6 C8 117.6(4) . . ? O4 N6 C8 117.5(4) . . ? C2 O1 Tb1 94.5(3) . . ? C2 O2 Tb1 90.7(3) . . ? C23 O5 Tb2 93.9(3) . . ? C23 O6 Tb1 155.7(3) . . ? C23 O6 Tb2 93.7(3) . . ? Tb1 O6 Tb2 108.52(13) . . ? C57 O9 Tb2 133.9(3) . . ? C57 O10 Tb1 135.5(3) . . ? C24 O13 Tb2 136.2(3) . . ? C24 O14 Tb1 132.9(3) . . ? C35 O17 Tb2 153.3(4) . . ? C35 O17 Tb1 93.5(3) . . ? Tb2 O17 Tb1 108.14(13) . . ? C35 O18 Tb1 94.6(3) . . ? C46 O21 Tb2 91.4(3) . . ? C46 O22 Tb2 93.3(3) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 6.244 _refine_diff_density_min -2.140 _refine_diff_density_rms 0.187