# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_globa1 _journal_coden_Cambridge 440 loop_ _publ_author_name 'Chen, Xiao-Ming' 'Liu, Gao-Feng' 'Qiao, Zheng-Ping' 'Wang, He-Zhou' 'Yang, Guang' _publ_contact_author_name 'Prof Xiao-Ming Chen' _publ_contact_author_address ; School of Chemistry & Chemical Engineering Zhongshan University 135 XinGang Xilu GuangZhou 510275 CHINA ; _publ_contact_author_phone '86 20 84113986' _publ_contact_author_fax '86 20 84112245' _publ_contact_author_email cescxm@zsu.edu.cn _publ_requested_joiurnal ' New J. Chem. ' _publ_requested_coeditor_name ? _publ_contact_letter ; Dear Sir or Madam: Please consider this CIF as supplmentary data for a manuscript submitted to New J. Chem. Xiao-Ming Chen ; #================================================================= _publ_section_title ; Synthesis, Structures and Photoluminescence of Three Terbium(III) Dicarboxylate Coordination Polymers ; #============================================================ data_complex_1 _database_code_CSD 156112 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H23 O13 Tb' _chemical_formula_weight 726.40 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.154(5) _cell_length_b 9.530(2) _cell_length_c 21.903(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.57(3) _cell_angle_gamma 90.00 _cell_volume 5618.6(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.717 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 2.586 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.789 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 21383 _diffrn_reflns_av_R_equivalents 0.0199 _diffrn_reflns_av_sigmaI/netI 0.0274 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 4.00 _diffrn_reflns_theta_max 30.01 _reflns_number_total 8103 _reflns_number_gt 5562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+9.6849P] 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 SHELXL _refine_ls_extinction_coef 0.00000(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8103 _refine_ls_number_parameters 380 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0472 _refine_ls_R_factor_gt 0.0256 _refine_ls_wR_factor_ref 0.0589 _refine_ls_wR_factor_gt 0.0536 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.107 _refine_ls_shift/su_mean 0.007 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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.014253(4) 0.247918(13) 0.008710(5) 0.01893(4) Uani 1 d . . . O1 O -0.32829(8) 0.3917(3) -0.46466(12) 0.0561(7) Uani 1 d . . . O2 O -0.34353(8) 0.3352(3) -0.36952(12) 0.0458(6) Uani 1 d . . . H2B H -0.3745 0.3478 -0.3795 0.080 Uiso 1 d R . . O3 O -0.01905(7) 0.0898(2) -0.06574(9) 0.0269(4) Uani 1 d . . . O4 O -0.05324(7) -0.11419(19) -0.09713(9) 0.0282(4) Uani 1 d . . . O5 O -0.10967(7) 0.2550(3) -0.33956(9) 0.0384(5) Uani 1 d . . . O6 O -0.07674(7) 0.6132(2) -0.06076(9) 0.0316(5) Uani 1 d . . . O7 O -0.04762(7) 0.4038(2) -0.03070(9) 0.0309(4) Uani 1 d . . . O8 O -0.46987(7) 0.15793(19) -0.09815(9) 0.0264(4) Uani 1 d . . . O9 O -0.44330(7) 0.34910(19) -0.04809(9) 0.0280(4) Uani 1 d . . . O10 O -0.25442(7) 0.2287(2) -0.18363(10) 0.0400(6) Uani 1 d . . . O1W O 0.04294(7) 0.3720(2) -0.07760(9) 0.0322(5) Uani 1 d . . . H1WA H 0.0253 0.4382 -0.0948 0.080 Uiso 1 d R . . H1WB H 0.0609 0.3281 -0.1001 0.080 Uiso 1 d R . . O2W O 0.08072(6) 0.12258(19) -0.02829(9) 0.0273(4) Uani 1 d . . . H2WA H 0.0738 0.0416 -0.0431 0.080 Uiso 1 d R . . H2WB H 0.1086 0.1259 -0.0056 0.080 Uiso 1 d R . . O3W O -0.5412(2) 0.1223(6) -0.2077(2) 0.219(3) Uani 1 d . . . H3WA H -0.5302 0.1112 -0.1699 0.080 Uiso 1 d R . . H3WB H -0.5157 0.1365 -0.2253 0.080 Uiso 1 d R . . C1 C -0.31366(11) 0.3549(3) -0.41197(16) 0.0378(7) Uani 1 d . . . C2 C -0.26028(10) 0.3296(3) -0.39026(15) 0.0332(7) Uani 1 d . . . C3 C -0.24425(11) 0.2812(3) -0.33133(15) 0.0374(8) Uani 1 d . . . H3A H -0.2680 0.2647 -0.3035 0.080 Uiso 1 d R . . C4 C -0.19416(10) 0.2536(4) -0.31299(13) 0.0372(6) Uani 1 d . . . H4A H -0.1827 0.2174 -0.2728 0.080 Uiso 1 d R . . C5 C -0.16031(10) 0.2769(3) -0.35430(13) 0.0291(6) Uani 1 d . . . C6 C -0.17577(11) 0.3280(4) -0.41286(14) 0.0398(8) Uani 1 d . . . H6A H -0.1517 0.3448 -0.4403 0.080 Uiso 1 d R . . C7 C -0.22567(11) 0.3540(4) -0.43053(15) 0.0411(8) Uani 1 d . . . H7A H -0.2368 0.3903 -0.4708 0.080 Uiso 1 d R . . C8 C -0.09241(10) 0.1929(3) -0.28224(13) 0.0290(6) Uani 1 d . . . C9 C -0.09749(13) 0.0501(3) -0.27452(14) 0.0398(8) Uani 1 d . . . H9A H -0.1120 -0.0073 -0.3081 0.080 Uiso 1 d R . . C10 C -0.08009(12) -0.0087(3) -0.21759(14) 0.0359(7) Uani 1 d . . . H10A H -0.0835 -0.1075 -0.2112 0.080 Uiso 1 d R . . C11 C -0.05822(9) 0.0743(3) -0.16941(12) 0.0215(5) Uani 1 d . . . C12 C -0.05213(11) 0.2172(3) -0.17968(14) 0.0319(7) Uani 1 d . . . H12A H -0.0366 0.2745 -0.1467 0.080 Uiso 1 d R . . C13 C -0.06974(12) 0.2778(3) -0.23626(14) 0.0358(7) Uani 1 d . . . H13A H -0.0653 0.3759 -0.2435 0.080 Uiso 1 d R . . C14 C -0.04219(9) 0.0134(3) -0.10652(12) 0.0198(5) Uani 1 d . . . C15 C -0.08036(9) 0.4813(3) -0.05913(12) 0.0212(5) Uani 1 d . . . C16 C -0.12669(9) 0.4147(3) -0.09209(12) 0.0219(5) Uani 1 d . . . C17 C -0.13995(12) 0.2801(3) -0.07717(16) 0.0376(8) Uani 1 d . . . H17A H -0.1194 0.2290 -0.0458 0.080 Uiso 1 d R . . C18 C -0.18325(12) 0.2196(3) -0.10734(18) 0.0440(9) Uani 1 d . . . H18A H -0.1924 0.1257 -0.0978 0.080 Uiso 1 d R . . C19 C -0.21202(10) 0.2936(3) -0.15190(14) 0.0302(6) Uani 1 d . . . C20 C -0.19929(11) 0.4272(3) -0.16832(15) 0.0383(7) Uani 1 d . . . H20A H -0.2195 0.4752 -0.2010 0.080 Uiso 1 d R . . C21 C -0.15639(11) 0.4877(3) -0.13749(15) 0.0352(7) Uani 1 d . . . H21A H -0.1476 0.5814 -0.1476 0.080 Uiso 1 d R . . C22 C -0.29821(9) 0.2379(3) -0.15775(13) 0.0296(6) Uani 1 d . . . C23 C -0.33754(10) 0.1578(3) -0.18524(14) 0.0347(7) Uani 1 d . . . H23A H -0.3334 0.0988 -0.2196 0.080 Uiso 1 d R . . C24 C -0.38263(10) 0.1604(3) -0.16186(14) 0.0316(6) Uani 1 d . . . H24A H -0.4102 0.1058 -0.1805 0.080 Uiso 1 d R . . C25 C -0.38868(9) 0.2455(3) -0.11152(12) 0.0254(5) Uani 1 d . . . C26 C -0.34880(10) 0.3272(3) -0.08517(14) 0.0320(6) Uani 1 d . . . H26A H -0.3530 0.3869 -0.0511 0.080 Uiso 1 d R . . C27 C -0.30348(10) 0.3237(3) -0.10766(15) 0.0353(7) Uani 1 d . . . H27A H -0.2757 0.3775 -0.0889 0.080 Uiso 1 d R . . C28 C -0.43669(9) 0.2508(3) -0.08542(12) 0.0245(5) Uani 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 Tb1 0.01611(5) 0.01716(6) 0.02242(6) -0.00024(6) -0.00151(4) -0.00109(6) O1 0.0324(12) 0.0736(18) 0.0571(17) 0.0136(15) -0.0139(11) 0.0004(12) O2 0.0241(10) 0.0502(14) 0.0611(16) 0.0011(12) -0.0022(11) 0.0041(10) O3 0.0284(10) 0.0272(10) 0.0222(10) -0.0029(8) -0.0072(8) -0.0013(8) O4 0.0300(10) 0.0233(9) 0.0284(11) 0.0051(8) -0.0065(8) -0.0037(8) O5 0.0261(9) 0.0628(14) 0.0254(9) 0.0175(12) 0.0002(7) 0.0067(11) O6 0.0309(10) 0.0222(10) 0.0374(12) 0.0017(9) -0.0109(9) -0.0079(8) O7 0.0213(9) 0.0333(11) 0.0356(11) 0.0020(9) -0.0050(8) 0.0051(8) O8 0.0221(9) 0.0242(9) 0.0330(11) -0.0025(8) 0.0036(8) -0.0052(7) O9 0.0265(9) 0.0218(9) 0.0371(12) -0.0047(8) 0.0094(8) -0.0024(8) O10 0.0225(9) 0.0609(16) 0.0379(11) -0.0254(11) 0.0085(8) -0.0169(10) O1W 0.0406(11) 0.0239(10) 0.0342(12) 0.0040(8) 0.0131(9) 0.0052(9) O2W 0.0208(9) 0.0218(9) 0.0378(11) -0.0040(8) -0.0018(8) 0.0000(7) O3W 0.289(8) 0.192(6) 0.138(5) 0.003(5) -0.107(5) -0.034(6) C1 0.0293(15) 0.0334(16) 0.048(2) 0.0001(14) -0.0061(14) -0.0017(12) C2 0.0248(14) 0.0335(16) 0.0385(17) 0.0009(13) -0.0059(12) 0.0014(12) C3 0.0281(14) 0.047(2) 0.0358(17) 0.0029(13) 0.0009(12) 0.0023(12) C4 0.0303(13) 0.0539(18) 0.0266(13) 0.0082(17) 0.0010(11) 0.0034(17) C5 0.0259(13) 0.0350(17) 0.0248(13) 0.0031(11) -0.0020(10) 0.0018(11) C6 0.0302(16) 0.062(2) 0.0256(16) 0.0106(15) -0.0033(12) 0.0047(15) C7 0.0340(16) 0.057(2) 0.0294(16) 0.0102(15) -0.0066(13) 0.0045(15) C8 0.0218(13) 0.0422(15) 0.0218(14) 0.0097(12) -0.0013(11) 0.0044(11) C9 0.054(2) 0.0393(17) 0.0222(15) -0.0053(13) -0.0103(14) -0.0021(15) C10 0.0533(18) 0.0267(14) 0.0236(15) -0.0015(12) -0.0100(13) -0.0013(13) C11 0.0209(12) 0.0238(12) 0.0184(12) 0.0007(10) -0.0022(10) 0.0000(10) C12 0.0418(16) 0.0234(15) 0.0274(14) 0.0019(10) -0.0066(12) -0.0064(11) C13 0.0442(17) 0.0272(17) 0.0339(16) 0.0080(11) -0.0029(13) -0.0032(12) C14 0.0170(11) 0.0230(12) 0.0181(12) -0.0003(10) -0.0019(9) 0.0015(9) C15 0.0187(11) 0.0244(13) 0.0201(13) 0.0001(10) 0.0007(10) -0.0025(10) C16 0.0163(11) 0.0227(12) 0.0258(13) -0.0017(10) -0.0002(10) -0.0020(9) C17 0.0340(15) 0.0274(17) 0.0482(19) 0.0088(12) -0.0071(14) -0.0077(11) C18 0.0395(17) 0.0298(18) 0.060(2) 0.0059(14) -0.0042(16) -0.0159(13) C19 0.0203(12) 0.0389(15) 0.0321(15) -0.0143(12) 0.0061(11) -0.0094(11) C20 0.0310(15) 0.0374(17) 0.0417(19) 0.0002(14) -0.0139(13) -0.0044(13) C21 0.0331(15) 0.0261(14) 0.0424(19) 0.0028(13) -0.0105(13) -0.0059(12) C22 0.0222(11) 0.0378(16) 0.0292(13) -0.0082(14) 0.0045(10) -0.0056(13) C23 0.0264(14) 0.0441(18) 0.0342(17) -0.0182(14) 0.0065(12) -0.0120(13) C24 0.0231(13) 0.0362(16) 0.0352(17) -0.0117(13) 0.0033(12) -0.0105(11) C25 0.0212(10) 0.0255(12) 0.0295(12) 0.0002(14) 0.0037(9) -0.0034(13) C26 0.0263(14) 0.0346(16) 0.0353(17) -0.0123(13) 0.0046(12) -0.0067(12) C27 0.0224(14) 0.0446(18) 0.0388(18) -0.0147(14) 0.0030(12) -0.0111(12) C28 0.0225(10) 0.0219(11) 0.0287(12) 0.0058(14) 0.0025(9) 0.0019(13) _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 Tb1 O3 2.3146(18) . ? Tb1 O7 2.3221(19) . ? Tb1 O6 2.3284(18) 5_565 ? Tb1 O2W 2.3929(18) . ? Tb1 O9 2.3976(19) 7_455 ? Tb1 O4 2.4403(19) 5 ? Tb1 O1W 2.4429(19) . ? Tb1 O8 2.592(2) 7_455 ? Tb1 C28 2.862(2) 7_455 ? O1 C1 1.221(4) . ? O2 C1 1.325(4) . ? O2 O4 2.843(3) 4_454 ? O3 C14 1.255(3) . ? O4 C14 1.276(3) . ? O4 Tb1 2.4403(19) 5 ? O5 C5 1.386(3) . ? O5 C8 1.411(3) . ? O6 C15 1.262(3) . ? O6 Tb1 2.3284(18) 5_565 ? O7 C15 1.256(3) . ? O8 C28 1.268(3) . ? O8 Tb1 2.592(2) 7_455 ? O8 O3W 2.898(5) . ? O9 C28 1.271(3) . ? O9 Tb1 2.3976(19) 7_455 ? O10 C22 1.386(3) . ? O10 C19 1.407(3) . ? O1W O8 2.776(3) 3 ? O1W O5 2.947(3) 2_554 ? O2W O1 2.675(3) 8_556 ? O2W O9 2.708(3) 3_545 ? O3W O3W 3.090(14) 2_454 ? C1 C2 1.485(4) . ? C2 C3 1.386(4) . ? C2 C7 1.390(4) . ? C3 C4 1.392(4) . ? C4 C5 1.390(4) . ? C5 C6 1.385(4) . ? C6 C7 1.382(4) . ? C8 C13 1.373(4) . ? C8 C9 1.381(4) . ? C9 C10 1.392(4) . ? C10 C11 1.388(4) . ? C11 C12 1.394(4) . ? C11 C14 1.505(3) . ? C12 C13 1.393(4) . ? C15 C16 1.506(3) . ? C16 C21 1.383(4) . ? C16 C17 1.383(4) . ? C17 C18 1.395(4) . ? C18 C19 1.364(5) . ? C19 C20 1.380(4) . ? C20 C21 1.392(4) . ? C22 C23 1.384(4) . ? C22 C27 1.390(4) . ? C23 C24 1.388(4) . ? C24 C25 1.395(4) . ? C25 C26 1.395(4) . ? C25 C28 1.492(3) . ? C26 C27 1.385(4) . ? C28 Tb1 2.862(2) 7_455 ? 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 O3 Tb1 O7 87.60(7) . . ? O3 Tb1 O6 155.07(7) . 5_565 ? O7 Tb1 O6 105.27(7) . 5_565 ? O3 Tb1 O2W 71.26(7) . . ? O7 Tb1 O2W 137.26(7) . . ? O6 Tb1 O2W 85.18(7) 5_565 . ? O3 Tb1 O9 75.20(7) . 7_455 ? O7 Tb1 O9 78.70(7) . 7_455 ? O6 Tb1 O9 127.69(7) 5_565 7_455 ? O2W Tb1 O9 127.37(6) . 7_455 ? O3 Tb1 O4 107.91(7) . 5 ? O7 Tb1 O4 147.79(7) . 5 ? O6 Tb1 O4 72.32(7) 5_565 5 ? O2W Tb1 O4 74.95(7) . 5 ? O9 Tb1 O4 78.36(7) 7_455 5 ? O3 Tb1 O1W 84.53(7) . . ? O7 Tb1 O1W 72.03(7) . . ? O6 Tb1 O1W 79.49(7) 5_565 . ? O2W Tb1 O1W 69.39(7) . . ? O9 Tb1 O1W 144.92(7) 7_455 . ? O4 Tb1 O1W 135.87(7) 5 . ? O3 Tb1 O8 125.48(6) . 7_455 ? O7 Tb1 O8 70.96(7) . 7_455 ? O6 Tb1 O8 79.31(7) 5_565 7_455 ? O2W Tb1 O8 151.08(6) . 7_455 ? O9 Tb1 O8 52.11(6) 7_455 7_455 ? O4 Tb1 O8 77.13(6) 5 7_455 ? O1W Tb1 O8 130.15(6) . 7_455 ? O3 Tb1 C28 99.61(7) . 7_455 ? O7 Tb1 C28 70.32(7) . 7_455 ? O6 Tb1 C28 104.79(8) 5_565 7_455 ? O2W Tb1 C28 147.90(7) . 7_455 ? O9 Tb1 C28 26.11(7) 7_455 7_455 ? O4 Tb1 C28 79.18(7) 5 7_455 ? O1W Tb1 C28 141.87(7) . 7_455 ? O8 Tb1 C28 26.28(7) 7_455 7_455 ? C1 O2 O4 118.01(19) . 4_454 ? C14 O3 Tb1 172.54(17) . . ? C14 O4 Tb1 122.63(16) . 5 ? C5 O5 C8 118.2(2) . . ? C15 O6 Tb1 127.36(17) . 5_565 ? C15 O7 Tb1 172.14(19) . . ? C28 O8 Tb1 88.84(15) . 7_455 ? C28 O8 O3W 130.0(2) . . ? Tb1 O8 O3W 109.84(15) 7_455 . ? C28 O9 Tb1 97.79(15) . 7_455 ? C22 O10 C19 117.4(2) . . ? Tb1 O1W O8 123.70(8) . 3 ? Tb1 O1W O5 125.29(9) . 2_554 ? O8 O1W O5 110.23(9) 3 2_554 ? Tb1 O2W O1 122.34(9) . 8_556 ? Tb1 O2W O9 110.99(8) . 3_545 ? O1 O2W O9 102.77(9) 8_556 3_545 ? O8 O3W O3W 92.2(2) . 2_454 ? O1 C1 O2 123.4(3) . . ? O1 C1 C2 122.1(3) . . ? O2 C1 C2 114.5(3) . . ? C3 C2 C7 119.4(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 118.9(3) . . ? C2 C3 C4 120.5(3) . . ? C5 C4 C3 119.1(3) . . ? C6 C5 O5 116.1(3) . . ? C6 C5 C4 120.9(3) . . ? O5 C5 C4 123.0(2) . . ? C7 C6 C5 119.3(3) . . ? C6 C7 C2 120.8(3) . . ? C13 C8 C9 122.2(3) . . ? C13 C8 O5 118.1(3) . . ? C9 C8 O5 119.7(3) . . ? C8 C9 C10 118.6(3) . . ? C11 C10 C9 120.8(3) . . ? C10 C11 C12 118.8(3) . . ? C10 C11 C14 121.3(2) . . ? C12 C11 C14 119.9(2) . . ? C11 C12 C13 120.9(3) . . ? C8 C13 C12 118.5(3) . . ? O3 C14 O4 123.0(2) . . ? O3 C14 C11 119.0(2) . . ? O4 C14 C11 118.0(2) . . ? O7 C15 O6 123.2(2) . . ? O7 C15 C16 118.8(2) . . ? O6 C15 C16 118.0(2) . . ? C21 C16 C17 119.4(3) . . ? C21 C16 C15 120.3(2) . . ? C17 C16 C15 120.3(2) . . ? C16 C17 C18 120.0(3) . . ? C19 C18 C17 119.5(3) . . ? C18 C19 C20 121.6(3) . . ? C18 C19 O10 118.7(3) . . ? C20 C19 O10 119.6(3) . . ? C19 C20 C21 118.5(3) . . ? C16 C21 C20 120.8(3) . . ? C23 C22 O10 116.2(2) . . ? C23 C22 C27 120.9(2) . . ? O10 C22 C27 122.9(2) . . ? C22 C23 C24 119.8(3) . . ? C23 C24 C25 120.2(2) . . ? C24 C25 C26 119.0(2) . . ? C24 C25 C28 121.5(2) . . ? C26 C25 C28 119.5(2) . . ? C27 C26 C25 121.1(3) . . ? C26 C27 C22 118.9(3) . . ? O8 C28 O9 120.0(2) . . ? O8 C28 C25 121.6(2) . . ? O9 C28 C25 118.4(2) . . ? O8 C28 Tb1 64.88(13) . 7_455 ? O9 C28 Tb1 56.10(12) . 7_455 ? C25 C28 Tb1 166.65(17) . 7_455 ? _diffrn_measured_fraction_theta_max 0.467 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.467 _refine_diff_density_max 0.777 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.083 #===========================================END data_complex_2 _database_code_CSD 182825 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H32 O19 Tb2' _chemical_formula_weight 1158.52 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' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? 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 8.5937(9) _cell_length_b 29.016(3) _cell_length_c 16.5048(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.279(2) _cell_angle_gamma 90.00 _cell_volume 4115.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colorless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.870 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 3.491 _exptl_absorpt_correction_type Empirical _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_absorpt_correction_T_min 0.5276 _exptl_absorpt_correction_T_max 0.9335 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24040 _diffrn_reflns_av_R_equivalents 0.0291 _diffrn_reflns_av_sigmaI/netI 0.0284 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 27.02 _reflns_number_total 8932 _reflns_number_gt 7552 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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 w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+15.0476P] 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 SHELXL _refine_ls_extinction_coef 0.00002(4) _refine_ls_number_reflns 8932 _refine_ls_number_parameters 568 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0471 _refine_ls_wR_factor_ref 0.1559 _refine_ls_wR_factor_gt 0.1443 _refine_ls_goodness_of_fit_ref 1.184 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.012 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.41108(5) 0.009901(11) 0.37200(2) 0.03609(12) Uani 1 d . . . Tb2 Tb 0.19168(3) 0.014287(9) 0.073402(17) 0.02386(11) Uani 1 d . . . O1 O 0.6445(7) 0.05529(18) 0.3876(3) 0.0447(13) Uani 1 d . . . O2 O 0.8030(9) 0.0510(2) 0.2830(4) 0.077(2) Uani 1 d . . . O3 O 0.8008(5) 0.44287(16) 0.4708(3) 0.0357(11) Uani 1 d . . . O4 O 0.7294(9) 0.4306(2) 0.3441(3) 0.0634(19) Uani 1 d . . . O5 O 1.0406(6) 0.23844(17) 0.4374(4) 0.0563(17) Uani 1 d . . . O6 O 0.2602(7) -0.04388(18) 0.1657(3) 0.0449(13) Uani 1 d . . . O7 O 0.2729(8) -0.0439(2) 0.3000(4) 0.0572(16) Uani 1 d . . . O8 O 0.1609(9) -0.44322(18) 0.2325(3) 0.0574(17) Uani 1 d . . . O9 O 0.2935(6) -0.42178(16) 0.3400(3) 0.0395(12) Uani 1 d . . . O10 O -0.0468(7) -0.23612(18) 0.2417(5) 0.0649(19) Uani 1 d . . . O11 O 0.2804(5) -0.05037(15) -0.0156(3) 0.0310(10) Uani 1 d . . . O12 O 0.0295(5) -0.04814(14) 0.0059(3) 0.0259(9) Uani 1 d . . . O13 O 0.0355(8) -0.45397(18) -0.0495(4) 0.0618(18) Uani 1 d . . . O14 O 0.1644(7) -0.42440(19) 0.0513(3) 0.0495(14) Uani 1 d . . . O15 O 0.0588(8) -0.24433(16) -0.1600(3) 0.0497(15) Uani 1 d . . . O1W O 0.5909(10) -0.0156(2) 0.2668(5) 0.081(3) Uani 1 d U . . H1W1 H 0.6548 -0.0395 0.2721 0.050 Uiso 1 d R . . H1W2 H 0.6490 0.0078 0.2713 0.050 Uiso 1 d R . . O2W O 0.2151(9) -0.0188(3) 0.4648(4) 0.090(3) Uani 1 d U . . H2W1 H 0.1513 -0.0388 0.4458 0.050 Uiso 1 d R . . H2W2 H 0.2442 -0.0288 0.5113 0.050 Uiso 1 d R . . O3W O -0.0388(6) 0.00570(18) 0.1558(3) 0.0389(12) Uani 1 d U . . H3W1 H -0.1016 -0.0204 0.1578 0.050 Uiso 1 d R . . H3W2 H -0.0558 0.0335 0.1862 0.050 Uiso 1 d R . . O4W O 0.4666(6) 0.01905(19) 0.1021(3) 0.0446(13) Uani 1 d U . . H4W1 H 0.5002 -0.0045 0.1283 0.050 Uiso 1 d R . . H4W2 H 0.5486 0.0311 0.0797 0.050 Uiso 1 d R . . C1 C 0.7584(9) 0.0705(2) 0.3453(4) 0.0396(16) Uani 1 d . . . C2 C 0.8323(8) 0.1150(2) 0.3704(4) 0.0324(14) Uani 1 d . . . C3 C 0.7797(10) 0.1390(3) 0.4376(5) 0.0475(19) Uani 1 d . . . H3 H 0.6993 0.1268 0.4684 0.071 Uiso 1 d R . . C4 C 0.8457(10) 0.1810(3) 0.4583(5) 0.0488(19) Uani 1 d . . . H4 H 0.8092 0.1970 0.5032 0.073 Uiso 1 d R . . C5 C 0.9634(8) 0.1986(2) 0.4131(5) 0.0369(16) Uani 1 d . . . C6 C 1.0192(9) 0.1753(3) 0.3463(5) 0.0432(17) Uani 1 d . . . H6 H 1.0996 0.1875 0.3155 0.065 Uiso 1 d R . . C7 C 0.9546(9) 0.1334(3) 0.3248(4) 0.0374(15) Uani 1 d . . . H7 H 0.9911 0.1174 0.2800 0.056 Uiso 1 d R . . C8 C 0.9707(8) 0.2809(2) 0.4281(4) 0.0327(14) Uani 1 d . . . C9 C 1.0134(9) 0.3143(2) 0.4837(5) 0.0414(17) Uani 1 d . . . H9 H 1.0813 0.3069 0.5257 0.062 Uiso 1 d R . . C10 C 0.9558(9) 0.3586(2) 0.4775(4) 0.0377(16) Uani 1 d . . . H10 H 0.9853 0.3810 0.5149 0.057 Uiso 1 d R . . C11 C 0.8554(7) 0.3701(2) 0.4149(4) 0.0261(12) Uani 1 d . . . C12 C 0.8133(9) 0.3362(3) 0.3599(4) 0.0384(16) Uani 1 d . . . H12 H 0.7454 0.3437 0.3178 0.058 Uiso 1 d R . . C13 C 0.8670(9) 0.2917(3) 0.3664(5) 0.0442(18) Uani 1 d . . . H13 H 0.8375 0.2693 0.3290 0.066 Uiso 1 d R . . C14 C 0.7902(8) 0.4178(2) 0.4095(4) 0.0302(13) Uani 1 d . . . C15 C 0.2398(9) -0.0621(2) 0.2323(4) 0.0349(14) Uani 1 d . . . C16 C 0.1741(9) -0.1097(2) 0.2363(4) 0.0346(15) Uani 1 d . . . C17 C 0.1982(10) -0.1411(3) 0.1752(5) 0.0439(17) Uani 1 d . . . H17 H 0.2603 -0.1332 0.1314 0.066 Uiso 1 d R . . C18 C 0.1329(10) -0.1849(3) 0.1793(5) 0.050(2) Uani 1 d . . . H18 H 0.1490 -0.2059 0.1376 0.076 Uiso 1 d R . . C19 C 0.0390(9) -0.1955(2) 0.2426(5) 0.0418(18) Uani 1 d . . . C20 C 0.0171(12) -0.1652(3) 0.3055(5) 0.057(2) Uani 1 d . . . H20 H -0.0450 -0.1732 0.3493 0.086 Uiso 1 d R . . C21 C 0.0841(13) -0.1225(3) 0.3022(5) 0.060(3) Uani 1 d . . . H21 H 0.0680 -0.1015 0.3439 0.090 Uiso 1 d R . . C22 C 0.0329(8) -0.2772(2) 0.2484(5) 0.0403(17) Uani 1 d . . . C23 C -0.0011(10) -0.3104(3) 0.1926(5) 0.0454(18) Uani 1 d . . . H23 H -0.0641 -0.3036 0.1482 0.068 Uiso 1 d R . . C24 C 0.0566(10) -0.3542(2) 0.2023(4) 0.0415(17) Uani 1 d . . . H24 H 0.0327 -0.3771 0.1648 0.062 Uiso 1 d R . . C25 C 0.1497(8) -0.3650(2) 0.2687(4) 0.0298(13) Uani 1 d . . . C26 C 0.1853(10) -0.3308(3) 0.3232(5) 0.0468(19) Uani 1 d . . . H26 H 0.2484 -0.3376 0.3676 0.070 Uiso 1 d R . . C27 C 0.1295(10) -0.2866(3) 0.3129(6) 0.054(2) Uani 1 d . . . H27 H 0.1534 -0.2637 0.3505 0.081 Uiso 1 d R . . C28 C 0.2056(8) -0.4134(2) 0.2807(4) 0.0329(14) Uani 1 d . . . C29 C 0.1499(7) -0.06905(19) -0.0206(3) 0.0222(11) Uani 1 d . . . C30 C 0.1306(6) -0.11633(19) -0.0549(3) 0.0218(11) Uani 1 d . . . C31 C 0.0232(8) -0.1463(2) -0.0219(4) 0.0304(13) Uani 1 d . . . H31 H -0.0354 -0.1370 0.0224 0.046 Uiso 1 d R . . C32 C 0.0044(8) -0.1902(2) -0.0521(4) 0.0345(14) Uani 1 d . . . H32 H -0.0678 -0.2102 -0.0294 0.052 Uiso 1 d R . . C33 C 0.0892(9) -0.2033(2) -0.1191(4) 0.0331(15) Uani 1 d . . . C34 C 0.1963(9) -0.1740(2) -0.1533(4) 0.0361(15) Uani 1 d . . . H34 H 0.2549 -0.1834 -0.1976 0.054 Uiso 1 d R . . C35 C 0.2203(8) -0.1307(2) -0.1203(4) 0.0293(13) Uani 1 d . . . H35 H 0.2926 -0.1107 -0.1430 0.044 Uiso 1 d R . . C36 C 0.0699(8) -0.2858(2) -0.1205(4) 0.0323(14) Uani 1 d . . . C37 C 0.1575(8) -0.2931(2) -0.0507(4) 0.0366(15) Uani 1 d . . . H37 H 0.2101 -0.2687 -0.0264 0.055 Uiso 1 d R . . C38 C 0.1680(8) -0.3369(2) -0.0191(4) 0.0351(15) Uani 1 d . . . H38 H 0.2275 -0.3419 0.0273 0.053 Uiso 1 d R . . C39 C 0.0905(8) -0.3736(2) -0.0543(4) 0.0321(14) Uani 1 d . . . C40 C 0.0024(10) -0.3655(2) -0.1236(5) 0.0449(18) Uani 1 d . . . H40 H -0.0501 -0.3899 -0.1480 0.067 Uiso 1 d R . . C41 C -0.0109(10) -0.3222(3) -0.1559(4) 0.0445(19) Uani 1 d . . . H41 H -0.0704 -0.3172 -0.2022 0.067 Uiso 1 d R . . C42 C 0.0989(9) -0.4202(2) -0.0156(5) 0.0409(16) Uani 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 Tb1 0.0575(2) 0.02088(18) 0.02992(19) -0.00091(11) 0.00205(15) -0.00750(13) Tb2 0.02756(17) 0.01755(16) 0.02649(17) -0.00154(10) 0.00086(11) -0.00311(10) O1 0.061(3) 0.036(3) 0.037(3) -0.010(2) 0.013(2) -0.016(2) O2 0.101(6) 0.059(4) 0.071(4) -0.034(3) 0.052(4) -0.037(4) O3 0.036(3) 0.030(2) 0.041(3) -0.012(2) 0.003(2) 0.0038(19) O4 0.109(5) 0.043(3) 0.038(3) -0.003(2) -0.012(3) 0.033(3) O5 0.046(3) 0.022(3) 0.100(5) -0.011(3) -0.040(3) 0.004(2) O6 0.057(3) 0.032(3) 0.046(3) 0.021(2) 0.002(2) -0.001(2) O7 0.092(5) 0.034(3) 0.045(3) -0.002(2) -0.007(3) -0.026(3) O8 0.108(5) 0.023(3) 0.041(3) -0.004(2) -0.018(3) 0.011(3) O9 0.044(3) 0.027(2) 0.046(3) 0.014(2) -0.008(2) -0.001(2) O10 0.044(3) 0.019(3) 0.131(6) 0.002(3) -0.028(4) -0.002(2) O11 0.027(2) 0.026(2) 0.040(2) -0.0085(18) 0.0025(18) -0.0044(17) O12 0.025(2) 0.022(2) 0.030(2) -0.0051(17) -0.0007(17) 0.0019(16) O13 0.077(4) 0.015(2) 0.093(5) -0.001(3) 0.005(4) -0.011(3) O14 0.068(4) 0.038(3) 0.043(3) 0.014(2) 0.005(3) 0.006(3) O15 0.097(4) 0.016(2) 0.035(3) -0.0026(19) -0.027(3) -0.004(2) O1W 0.090(5) 0.064(5) 0.089(5) -0.046(4) 0.044(4) -0.034(4) O2W 0.076(5) 0.139(8) 0.054(4) -0.041(4) 0.014(4) -0.045(5) O3W 0.044(3) 0.038(3) 0.034(3) -0.012(2) 0.011(2) -0.016(2) O4W 0.033(3) 0.051(3) 0.049(3) 0.020(2) -0.004(2) -0.002(2) C1 0.057(5) 0.028(3) 0.034(4) -0.009(3) 0.013(3) -0.008(3) C2 0.040(4) 0.025(3) 0.032(3) -0.003(3) 0.000(3) -0.003(3) C3 0.058(5) 0.041(4) 0.044(4) -0.014(3) 0.016(4) -0.011(4) C4 0.054(5) 0.043(4) 0.049(5) -0.019(4) 0.004(4) 0.001(4) C5 0.037(4) 0.018(3) 0.056(4) -0.003(3) -0.020(3) 0.004(3) C6 0.046(4) 0.037(4) 0.047(4) 0.001(3) 0.004(3) -0.009(3) C7 0.043(4) 0.035(4) 0.034(4) -0.006(3) 0.006(3) -0.008(3) C8 0.028(3) 0.021(3) 0.049(4) -0.003(3) -0.008(3) 0.001(2) C9 0.048(4) 0.031(4) 0.046(4) -0.003(3) -0.025(3) 0.004(3) C10 0.045(4) 0.030(3) 0.038(4) -0.012(3) -0.014(3) 0.001(3) C11 0.030(3) 0.021(3) 0.027(3) -0.003(2) 0.002(2) 0.003(2) C12 0.047(4) 0.038(4) 0.031(3) -0.007(3) -0.013(3) 0.012(3) C13 0.051(4) 0.035(4) 0.046(4) -0.015(3) -0.019(3) 0.007(3) C14 0.034(3) 0.024(3) 0.033(3) -0.001(2) 0.006(3) 0.006(2) C15 0.045(4) 0.024(3) 0.036(4) 0.002(3) -0.005(3) -0.004(3) C16 0.050(4) 0.024(3) 0.030(3) 0.002(2) -0.010(3) -0.006(3) C17 0.062(5) 0.033(4) 0.036(4) -0.002(3) -0.005(3) -0.001(3) C18 0.063(5) 0.034(4) 0.054(5) -0.018(3) -0.020(4) 0.008(4) C19 0.041(4) 0.016(3) 0.067(5) 0.003(3) -0.020(4) -0.002(3) C20 0.082(6) 0.040(5) 0.050(5) 0.004(4) 0.011(4) -0.026(4) C21 0.106(8) 0.037(4) 0.037(4) -0.011(3) 0.017(4) -0.033(5) C22 0.034(4) 0.014(3) 0.072(5) 0.004(3) -0.010(3) -0.004(2) C23 0.063(5) 0.034(4) 0.040(4) 0.005(3) -0.014(4) 0.008(3) C24 0.066(5) 0.029(4) 0.029(3) -0.002(3) -0.009(3) 0.009(3) C25 0.038(3) 0.023(3) 0.028(3) 0.005(2) 0.000(3) 0.003(3) C26 0.056(5) 0.031(4) 0.053(5) -0.002(3) -0.020(4) 0.001(3) C27 0.056(5) 0.027(4) 0.079(6) -0.010(4) -0.029(5) -0.002(3) C28 0.047(4) 0.024(3) 0.028(3) 0.007(2) 0.002(3) 0.006(3) C29 0.026(3) 0.017(3) 0.023(3) 0.001(2) -0.001(2) 0.001(2) C30 0.022(3) 0.016(3) 0.027(3) -0.002(2) -0.004(2) 0.001(2) C31 0.033(3) 0.024(3) 0.034(3) -0.002(2) 0.001(3) -0.002(2) C32 0.039(4) 0.024(3) 0.041(4) 0.003(3) -0.005(3) -0.007(3) C33 0.053(4) 0.014(3) 0.033(3) -0.003(2) -0.017(3) 0.001(3) C34 0.051(4) 0.026(3) 0.032(3) -0.005(3) -0.002(3) 0.008(3) C35 0.037(3) 0.024(3) 0.027(3) 0.000(2) 0.000(3) 0.001(2) C36 0.048(4) 0.018(3) 0.031(3) -0.002(2) -0.005(3) 0.003(3) C37 0.046(4) 0.024(3) 0.040(4) -0.003(3) -0.017(3) -0.006(3) C38 0.040(4) 0.030(3) 0.036(4) 0.004(3) -0.009(3) -0.001(3) C39 0.045(4) 0.020(3) 0.032(3) 0.000(2) 0.002(3) -0.004(3) C40 0.068(5) 0.022(3) 0.045(4) -0.004(3) -0.012(4) -0.014(3) C41 0.069(5) 0.028(4) 0.036(4) -0.001(3) -0.023(4) -0.006(3) C42 0.048(4) 0.027(3) 0.048(4) 0.006(3) 0.006(3) 0.003(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 Tb1 O8 2.279(5) 2 ? Tb1 O7 2.291(5) . ? Tb1 O13 2.333(6) 4_656 ? Tb1 O14 2.380(5) 2 ? Tb1 O1 2.412(5) . ? Tb1 O2W 2.429(7) . ? Tb1 O1W 2.444(6) . ? Tb1 O13 3.144(7) 2 ? Tb2 O3 2.304(4) 4_565 ? Tb2 O9 2.344(5) 2 ? Tb2 O6 2.346(5) . ? Tb2 O4W 2.411(5) . ? Tb2 O3W 2.421(5) . ? Tb2 O12 2.503(4) 3 ? Tb2 O11 2.504(4) . ? Tb2 O12 2.540(4) . ? O1 C1 1.283(9) . ? O2 C1 1.235(9) . ? O3 C14 1.249(8) . ? O3 Tb2 2.304(4) 4_666 ? O4 C14 1.253(9) . ? O5 C8 1.378(8) . ? O5 C5 1.391(8) . ? O6 C15 1.234(8) . ? O7 C15 1.266(9) . ? O8 C28 1.237(9) . ? O8 Tb1 2.279(5) 2_545 ? O9 C28 1.257(8) . ? O9 Tb2 2.344(5) 2_545 ? O10 C22 1.379(8) . ? O10 C19 1.389(8) . ? O11 C29 1.248(7) . ? O12 C29 1.278(7) . ? O12 Tb2 2.503(4) 3 ? O13 C42 1.251(10) . ? O13 Tb1 2.333(6) 4 ? O14 C42 1.242(9) . ? O14 Tb1 2.380(5) 2_545 ? O15 C36 1.372(8) . ? O15 C33 1.393(7) . ? O1W H1W1 0.8898 . ? O1W H1W2 0.8444 . ? O2W H2W1 0.8570 . ? O2W H2W2 0.8575 . ? O3W H3W1 0.9292 . ? O3W H3W2 0.9622 . ? O4W H4W1 0.8570 . ? O4W H4W2 0.8709 . ? C1 C2 1.499(9) . ? C2 C3 1.387(10) . ? C2 C7 1.400(10) . ? C3 C4 1.388(11) . ? C3 H3 0.9300 . ? C4 C5 1.359(12) . ? C4 H4 0.9299 . ? C5 C6 1.381(11) . ? C6 C7 1.382(10) . ? C6 H6 0.9301 . ? C7 H7 0.9301 . ? C8 C9 1.384(9) . ? C8 C13 1.387(10) . ? C9 C10 1.380(10) . ? C9 H9 0.9301 . ? C10 C11 1.384(9) . ? C10 H10 0.9299 . ? C11 C12 1.386(9) . ? C11 C14 1.497(8) . ? C12 C13 1.375(10) . ? C12 H12 0.9301 . ? C13 H13 0.9300 . ? C15 C16 1.492(9) . ? C16 C21 1.389(11) . ? C16 C17 1.378(10) . ? C17 C18 1.390(11) . ? C17 H17 0.9299 . ? C18 C19 1.358(12) . ? C18 H18 0.9299 . ? C19 C20 1.375(12) . ? C20 C21 1.368(11) . ? C20 H20 0.9301 . ? C21 H21 0.9299 . ? C22 C23 1.362(11) . ? C22 C27 1.375(11) . ? C23 C24 1.374(10) . ? C23 H23 0.9299 . ? C24 C25 1.390(9) . ? C24 H24 0.9300 . ? C25 C26 1.373(10) . ? C25 C28 1.495(9) . ? C26 C27 1.381(11) . ? C26 H26 0.9301 . ? C27 H27 0.9298 . ? C29 C30 1.494(8) . ? C30 C31 1.382(9) . ? C30 C35 1.392(8) . ? C31 C32 1.376(9) . ? C31 H31 0.9300 . ? C32 C33 1.381(10) . ? C32 H32 0.9300 . ? C33 C34 1.375(10) . ? C34 C35 1.386(9) . ? C34 H34 0.9301 . ? C35 H35 0.9300 . ? C36 C37 1.389(9) . ? C36 C41 1.390(9) . ? C37 C38 1.377(9) . ? C37 H37 0.9300 . ? C38 C39 1.382(9) . ? C38 H38 0.9301 . ? C39 C40 1.389(10) . ? C39 C42 1.498(9) . ? C40 C41 1.370(10) . ? C40 H40 0.9301 . ? C41 H41 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 O8 Tb1 O7 82.9(2) 2 . ? O8 Tb1 O13 163.2(2) 2 4_656 ? O7 Tb1 O13 92.8(2) . 4_656 ? O8 Tb1 O14 81.4(2) 2 2 ? O7 Tb1 O14 132.8(2) . 2 ? O13 Tb1 O14 112.8(2) 4_656 2 ? O8 Tb1 O1 88.7(2) 2 . ? O7 Tb1 O1 148.9(2) . . ? O13 Tb1 O1 86.7(2) 4_656 . ? O14 Tb1 O1 74.61(19) 2 . ? O8 Tb1 O2W 119.7(3) 2 . ? O7 Tb1 O2W 74.6(2) . . ? O13 Tb1 O2W 74.3(3) 4_656 . ? O14 Tb1 O2W 75.4(2) 2 . ? O1 Tb1 O2W 134.3(2) . . ? O8 Tb1 O1W 79.2(3) 2 . ? O7 Tb1 O1W 75.7(2) . . ? O13 Tb1 O1W 83.9(3) 4_656 . ? O14 Tb1 O1W 142.6(2) 2 . ? O1 Tb1 O1W 73.3(2) . . ? O2W Tb1 O1W 141.9(3) . . ? O8 Tb1 O13 122.95(17) 2 2 ? O7 Tb1 O13 141.63(19) . 2 ? O13 Tb1 O13 69.5(2) 4_656 2 ? O14 Tb1 O13 43.62(18) 2 2 ? O1 Tb1 O13 66.48(17) . 2 ? O2W Tb1 O13 68.0(2) . 2 ? O1W Tb1 O13 132.3(2) . 2 ? O3 Tb2 O9 89.99(18) 4_565 2 ? O3 Tb2 O6 139.78(18) 4_565 . ? O9 Tb2 O6 99.3(2) 2 . ? O3 Tb2 O4W 73.24(17) 4_565 . ? O9 Tb2 O4W 77.56(19) 2 . ? O6 Tb2 O4W 70.81(18) . . ? O3 Tb2 O3W 143.66(18) 4_565 . ? O9 Tb2 O3W 77.36(17) 2 . ? O6 Tb2 O3W 76.4(2) . . ? O4W Tb2 O3W 134.33(18) . . ? O3 Tb2 O12 73.43(15) 4_565 3 ? O9 Tb2 O12 92.68(15) 2 3 ? O6 Tb2 O12 143.99(17) . 3 ? O4W Tb2 O12 145.19(16) . 3 ? O3W Tb2 O12 73.31(17) . 3 ? O3 Tb2 O11 81.20(16) 4_565 . ? O9 Tb2 O11 159.15(16) 2 . ? O6 Tb2 O11 76.45(18) . . ? O4W Tb2 O11 81.80(17) . . ? O3W Tb2 O11 120.32(15) . . ? O12 Tb2 O11 102.72(14) 3 . ? O3 Tb2 O12 106.65(16) 4_565 . ? O9 Tb2 O12 149.30(16) 2 . ? O6 Tb2 O12 84.68(17) . . ? O4W Tb2 O12 131.46(17) . . ? O3W Tb2 O12 74.02(15) . . ? O12 Tb2 O12 68.70(15) 3 . ? O11 Tb2 O12 51.40(14) . . ? C1 O1 Tb1 139.9(5) . . ? C14 O3 Tb2 151.8(4) . 4_666 ? C8 O5 C5 120.2(5) . . ? C15 O6 Tb2 148.3(5) . . ? C15 O7 Tb1 148.8(5) . . ? C28 O8 Tb1 170.9(5) . 2_545 ? C28 O9 Tb2 131.2(5) . 2_545 ? C22 O10 C19 118.0(6) . . ? C29 O11 Tb2 95.1(3) . . ? C29 O12 Tb2 128.4(4) . 3 ? C29 O12 Tb2 92.6(3) . . ? Tb2 O12 Tb2 111.30(15) 3 . ? C42 O13 Tb1 172.0(6) . 4 ? C42 O14 Tb1 115.3(5) . 2_545 ? C36 O15 C33 120.5(5) . . ? Tb1 O1W H1W1 123.9 . . ? Tb1 O1W H1W2 94.0 . . ? H1W1 O1W H1W2 104.6 . . ? Tb1 O2W H2W1 116.5 . . ? Tb1 O2W H2W2 118.7 . . ? H2W1 O2W H2W2 106.4 . . ? Tb2 O3W H3W1 125.5 . . ? Tb2 O3W H3W2 109.4 . . ? H3W1 O3W H3W2 125.1 . . ? Tb2 O4W H4W1 112.4 . . ? Tb2 O4W H4W2 137.2 . . ? H4W1 O4W H4W2 105.2 . . ? O2 C1 O1 122.5(7) . . ? O2 C1 C2 119.5(6) . . ? O1 C1 C2 118.0(6) . . ? C3 C2 C7 119.2(6) . . ? C3 C2 C1 120.9(6) . . ? C7 C2 C1 119.8(6) . . ? C4 C3 C2 120.2(7) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 119.5 . . ? C5 C4 C3 120.0(7) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 119.7 . . ? C4 C5 C6 121.1(7) . . ? C4 C5 O5 120.6(7) . . ? C6 C5 O5 118.1(7) . . ? C5 C6 C7 119.7(7) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 119.6 . . ? C6 C7 C2 119.9(7) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 119.7 . . ? O5 C8 C9 116.0(6) . . ? O5 C8 C13 124.2(6) . . ? C9 C8 C13 119.7(6) . . ? C10 C9 C8 120.7(6) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.6 . . ? C9 C10 C11 120.1(6) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 119.6 . . ? C12 C11 C10 118.6(6) . . ? C12 C11 C14 121.4(6) . . ? C10 C11 C14 120.0(6) . . ? C13 C12 C11 121.9(6) . . ? C13 C12 H12 119.1 . . ? C11 C12 H12 119.0 . . ? C12 C13 C8 119.0(6) . . ? C12 C13 H13 120.9 . . ? C8 C13 H13 120.1 . . ? O4 C14 O3 123.7(6) . . ? O4 C14 C11 118.7(6) . . ? O3 C14 C11 117.6(6) . . ? O6 C15 O7 125.1(7) . . ? O6 C15 C16 119.4(6) . . ? O7 C15 C16 115.5(6) . . ? C21 C16 C17 118.8(7) . . ? C21 C16 C15 119.7(6) . . ? C17 C16 C15 121.5(7) . . ? C16 C17 C18 120.4(8) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 120.0 . . ? C19 C18 C17 119.2(7) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.0 . . ? C18 C19 C20 121.3(7) . . ? C18 C19 O10 120.1(7) . . ? C20 C19 O10 118.4(8) . . ? C21 C20 C19 119.4(8) . . ? C21 C20 H20 120.0 . . ? C19 C20 H20 120.6 . . ? C20 C21 C16 120.7(7) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 119.3 . . ? C23 C22 C27 120.7(7) . . ? C23 C22 O10 116.9(7) . . ? C27 C22 O10 122.0(7) . . ? C22 C23 C24 119.9(7) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 119.7 . . ? C23 C24 C25 120.5(7) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 119.3 . . ? C26 C25 C24 118.6(6) . . ? C26 C25 C28 121.4(6) . . ? C24 C25 C28 120.0(6) . . ? C25 C26 C27 121.1(7) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.6 . . ? C22 C27 C26 119.1(7) . . ? C22 C27 H27 120.4 . . ? C26 C27 H27 120.4 . . ? O8 C28 O9 123.3(6) . . ? O8 C28 C25 118.2(6) . . ? O9 C28 C25 118.4(6) . . ? O11 C29 O12 120.0(5) . . ? O11 C29 C30 121.5(5) . . ? O12 C29 C30 118.5(5) . . ? C31 C30 C35 119.4(6) . . ? C31 C30 C29 120.1(5) . . ? C35 C30 C29 120.5(5) . . ? C32 C31 C30 121.1(6) . . ? C32 C31 H31 119.4 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 118.9(6) . . ? C31 C32 H32 120.6 . . ? C33 C32 H32 120.4 . . ? C34 C33 C32 121.0(6) . . ? C34 C33 O15 117.0(6) . . ? C32 C33 O15 121.7(6) . . ? C33 C34 C35 119.9(6) . . ? C33 C34 H34 120.6 . . ? C35 C34 H34 119.6 . . ? C34 C35 C30 119.6(6) . . ? C34 C35 H35 120.4 . . ? C30 C35 H35 119.9 . . ? O15 C36 C37 124.3(6) . . ? O15 C36 C41 115.7(6) . . ? C37 C36 C41 120.0(6) . . ? C38 C37 C36 119.2(6) . . ? C38 C37 H37 120.6 . . ? C36 C37 H37 120.2 . . ? C37 C38 C39 121.4(6) . . ? C37 C38 H38 119.4 . . ? C39 C38 H38 119.1 . . ? C38 C39 C40 118.4(6) . . ? C38 C39 C42 119.6(6) . . ? C40 C39 C42 121.9(6) . . ? C41 C40 C39 121.2(6) . . ? C41 C40 H40 119.5 . . ? C39 C40 H40 119.3 . . ? C40 C41 C36 119.6(7) . . ? C40 C41 H41 120.5 . . ? C36 C41 H41 119.9 . . ? O14 C42 O13 121.1(7) . . ? O14 C42 C39 119.2(7) . . ? O13 C42 C39 119.7(7) . . ? 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 O8 Tb1 O1 C1 -52.2(8) 2 . . . ? O7 Tb1 O1 C1 21.7(10) . . . . ? O13 Tb1 O1 C1 111.6(8) 4_656 . . . ? O14 Tb1 O1 C1 -133.7(8) 2 . . . ? O2W Tb1 O1 C1 175.7(8) . . . . ? O1W Tb1 O1 C1 26.9(8) . . . . ? O13 Tb1 O1 C1 -179.3(8) 2 . . . ? O3 Tb2 O6 C15 151.1(9) 4_565 . . . ? O9 Tb2 O6 C15 50.0(10) 2 . . . ? O4W Tb2 O6 C15 123.3(10) . . . . ? O3W Tb2 O6 C15 -24.5(9) . . . . ? O12 Tb2 O6 C15 -57.8(11) 3 . . . ? O11 Tb2 O6 C15 -150.8(10) . . . . ? O12 Tb2 O6 C15 -99.3(10) . . . . ? O8 Tb1 O7 C15 43.8(11) 2 . . . ? O13 Tb1 O7 C15 -119.9(11) 4_656 . . . ? O14 Tb1 O7 C15 115.0(11) 2 . . . ? O1 Tb1 O7 C15 -31.7(14) . . . . ? O2W Tb1 O7 C15 167.2(12) . . . . ? O1W Tb1 O7 C15 -36.9(11) . . . . ? O13 Tb1 O7 C15 -179.8(10) 2 . . . ? O3 Tb2 O11 C29 -125.2(4) 4_565 . . . ? O9 Tb2 O11 C29 168.8(5) 2 . . . ? O6 Tb2 O11 C29 88.5(4) . . . . ? O4W Tb2 O11 C29 160.6(4) . . . . ? O3W Tb2 O11 C29 23.4(4) . . . . ? O12 Tb2 O11 C29 -54.5(4) 3 . . . ? O12 Tb2 O11 C29 -5.6(3) . . . . ? O3 Tb2 O12 C29 69.1(4) 4_565 . . . ? O9 Tb2 O12 C29 -170.6(4) 2 . . . ? O6 Tb2 O12 C29 -71.5(4) . . . . ? O4W Tb2 O12 C29 -13.0(4) . . . . ? O3W Tb2 O12 C29 -148.8(4) . . . . ? O12 Tb2 O12 C29 133.3(4) 3 . . . ? O11 Tb2 O12 C29 5.4(3) . . . . ? O3 Tb2 O12 Tb2 -64.1(2) 4_565 . . 3 ? O9 Tb2 O12 Tb2 56.1(4) 2 . . 3 ? O6 Tb2 O12 Tb2 155.3(2) . . . 3 ? O4W Tb2 O12 Tb2 -146.25(18) . . . 3 ? O3W Tb2 O12 Tb2 77.9(2) . . . 3 ? O12 Tb2 O12 Tb2 0.0 3 . . 3 ? O11 Tb2 O12 Tb2 -127.8(2) . . . 3 ? Tb1 O1 C1 O2 -26.1(14) . . . . ? Tb1 O1 C1 C2 150.1(6) . . . . ? O2 C1 C2 C3 176.7(9) . . . . ? O1 C1 C2 C3 0.5(11) . . . . ? O2 C1 C2 C7 -2.3(12) . . . . ? O1 C1 C2 C7 -178.6(7) . . . . ? C7 C2 C3 C4 1.4(13) . . . . ? C1 C2 C3 C4 -177.7(8) . . . . ? C2 C3 C4 C5 -0.8(13) . . . . ? C3 C4 C5 C6 0.1(12) . . . . ? C3 C4 C5 O5 -173.8(7) . . . . ? C8 O5 C5 C4 -75.6(10) . . . . ? C8 O5 C5 C6 110.3(8) . . . . ? C4 C5 C6 C7 0.0(12) . . . . ? O5 C5 C6 C7 174.0(7) . . . . ? C5 C6 C7 C2 0.7(12) . . . . ? C3 C2 C7 C6 -1.3(12) . . . . ? C1 C2 C7 C6 177.7(7) . . . . ? C5 O5 C8 C9 150.8(8) . . . . ? C5 O5 C8 C13 -31.3(12) . . . . ? O5 C8 C9 C10 176.9(7) . . . . ? C13 C8 C9 C10 -1.1(12) . . . . ? C8 C9 C10 C11 -0.6(12) . . . . ? C9 C10 C11 C12 0.8(11) . . . . ? C9 C10 C11 C14 178.6(7) . . . . ? C10 C11 C12 C13 0.7(12) . . . . ? C14 C11 C12 C13 -177.1(7) . . . . ? C11 C12 C13 C8 -2.4(13) . . . . ? O5 C8 C13 C12 -175.3(7) . . . . ? C9 C8 C13 C12 2.5(12) . . . . ? Tb2 O3 C14 O4 62.0(13) 4_666 . . . ? Tb2 O3 C14 C11 -118.5(9) 4_666 . . . ? C12 C11 C14 O4 -18.2(10) . . . . ? C10 C11 C14 O4 164.0(7) . . . . ? C12 C11 C14 O3 162.3(7) . . . . ? C10 C11 C14 O3 -15.5(10) . . . . ? Tb2 O6 C15 O7 -67.8(14) . . . . ? Tb2 O6 C15 C16 113.4(9) . . . . ? Tb1 O7 C15 O6 -20.4(17) . . . . ? Tb1 O7 C15 C16 158.4(8) . . . . ? O6 C15 C16 C21 -149.5(8) . . . . ? O7 C15 C16 C21 31.6(11) . . . . ? O6 C15 C16 C17 29.3(11) . . . . ? O7 C15 C16 C17 -149.6(8) . . . . ? C21 C16 C17 C18 0.3(12) . . . . ? C15 C16 C17 C18 -178.5(7) . . . . ? C16 C17 C18 C19 3.0(12) . . . . ? C17 C18 C19 C20 -5.1(12) . . . . ? C17 C18 C19 O10 169.9(7) . . . . ? C22 O10 C19 C18 69.0(10) . . . . ? C22 O10 C19 C20 -115.9(9) . . . . ? C18 C19 C20 C21 3.8(14) . . . . ? O10 C19 C20 C21 -171.3(9) . . . . ? C19 C20 C21 C16 -0.3(16) . . . . ? C17 C16 C21 C20 -1.7(14) . . . . ? C15 C16 C21 C20 177.2(9) . . . . ? C19 O10 C22 C23 -130.0(8) . . . . ? C19 O10 C22 C27 57.0(12) . . . . ? C27 C22 C23 C24 2.5(13) . . . . ? O10 C22 C23 C24 -170.7(8) . . . . ? C22 C23 C24 C25 0.0(13) . . . . ? C23 C24 C25 C26 -1.5(12) . . . . ? C23 C24 C25 C28 177.1(7) . . . . ? C24 C25 C26 C27 0.5(13) . . . . ? C28 C25 C26 C27 -178.1(8) . . . . ? C23 C22 C27 C26 -3.4(14) . . . . ? O10 C22 C27 C26 169.3(8) . . . . ? C25 C26 C27 C22 2.0(14) . . . . ? Tb1 O8 C28 O9 -133(3) 2_545 . . . ? Tb1 O8 C28 C25 48(4) 2_545 . . . ? Tb2 O9 C28 O8 -36.1(11) 2_545 . . . ? Tb2 O9 C28 C25 142.6(5) 2_545 . . . ? C26 C25 C28 O8 175.2(8) . . . . ? C24 C25 C28 O8 -3.3(10) . . . . ? C26 C25 C28 O9 -3.6(10) . . . . ? C24 C25 C28 O9 177.9(7) . . . . ? Tb2 O11 C29 O12 10.1(6) . . . . ? Tb2 O11 C29 C30 -168.2(5) . . . . ? Tb2 O12 C29 O11 110.1(6) 3 . . . ? Tb2 O12 C29 O11 -9.9(6) . . . . ? Tb2 O12 C29 C30 -71.6(6) 3 . . . ? Tb2 O12 C29 C30 168.4(4) . . . . ? O11 C29 C30 C31 142.7(6) . . . . ? O12 C29 C30 C31 -35.5(8) . . . . ? O11 C29 C30 C35 -37.2(8) . . . . ? O12 C29 C30 C35 144.5(6) . . . . ? C35 C30 C31 C32 0.6(9) . . . . ? C29 C30 C31 C32 -179.4(6) . . . . ? C30 C31 C32 C33 -3.4(10) . . . . ? C31 C32 C33 C34 3.1(10) . . . . ? C31 C32 C33 O15 -170.0(6) . . . . ? C36 O15 C33 C34 126.9(7) . . . . ? C36 O15 C33 C32 -59.7(10) . . . . ? C32 C33 C34 C35 0.0(10) . . . . ? O15 C33 C34 C35 173.4(6) . . . . ? C33 C34 C35 C30 -2.8(10) . . . . ? C31 C30 C35 C34 2.6(9) . . . . ? C29 C30 C35 C34 -177.5(6) . . . . ? C33 O15 C36 C37 -22.6(12) . . . . ? C33 O15 C36 C41 159.0(7) . . . . ? O15 C36 C37 C38 -175.9(7) . . . . ? C41 C36 C37 C38 2.4(12) . . . . ? C36 C37 C38 C39 -1.4(12) . . . . ? C37 C38 C39 C40 0.8(11) . . . . ? C37 C38 C39 C42 -177.1(7) . . . . ? C38 C39 C40 C41 -1.4(12) . . . . ? C42 C39 C40 C41 176.5(8) . . . . ? C39 C40 C41 C36 2.4(13) . . . . ? O15 C36 C41 C40 175.5(8) . . . . ? C37 C36 C41 C40 -3.0(12) . . . . ? Tb1 O14 C42 O13 -20.0(10) 2_545 . . . ? Tb1 O14 C42 C39 157.5(5) 2_545 . . . ? Tb1 O13 C42 O14 -175(4) 4 . . . ? Tb1 O13 C42 C39 7(5) 4 . . . ? C38 C39 C42 O14 6.1(11) . . . . ? C40 C39 C42 O14 -171.7(7) . . . . ? C38 C39 C42 O13 -176.4(7) . . . . ? C40 C39 C42 O13 5.8(12) . . . . ? _diffrn_measured_fraction_theta_max 0.975 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.975 _refine_diff_density_max 3.077 _refine_diff_density_min -1.298 _refine_diff_density_rms 0.256 #===========================================END data_complex_3 _database_code_CSD 156113 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C62 H40 N4 O15 Tb2' _chemical_formula_weight 1398.82 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 C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 30.896(11) _cell_length_b 10.183(7) _cell_length_c 20.432(13) _cell_angle_alpha 90.00 _cell_angle_beta 118.75 _cell_angle_gamma 90.00 _cell_volume 5636(6) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7.5 _cell_measurement_theta_max 15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.649 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2760 _exptl_absorpt_coefficient_mu 2.562 _exptl_absorpt_correction_type \y-scan _exptl_absorpt_correction_T_min 0.757 _exptl_absorpt_correction_T_max 0.571 _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'Siemens R3m' _diffrn_measurement_method '\w scan' _diffrn_standards_number 2 _diffrn_standards_decay_% none _diffrn_reflns_number 4634 _diffrn_reflns_av_R_equivalents 0.0371 _diffrn_reflns_av_sigmaI/netI 0.0387 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 27.02 _reflns_number_total 4520 _reflns_number_gt 3526 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXTL-plus (Sheldrick, 1990)' _computing_cell_refinement 'SHELXTL-plus (Sheldrick, 1990)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0609P)^2^+10.3105P] 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 SHELXL _refine_ls_extinction_coef 0.00018(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4520 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0916 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.004 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.707286(12) 0.58790(3) 0.438700(15) 0.02898(15) Uani 1 d . . . O1 O 0.76878(18) 0.6519(5) 0.4067(2) 0.0428(13) Uani 1 d . . . O2 O 0.80172(18) 0.8468(4) 0.4580(2) 0.0411(12) Uani 1 d . . . O3 O 1.11903(18) 1.0472(5) 0.3959(2) 0.0428(12) Uani 1 d . . . O4 O 1.1724(2) 0.8947(4) 0.4633(3) 0.0440(13) Uani 1 d . . . O5 O 0.9774(2) 0.6089(5) 0.4170(4) 0.0629(18) Uani 1 d . . . O6 O 0.80707(18) 0.6897(4) 0.5728(2) 0.0408(12) Uani 1 d . . . O7 O 0.77738(17) 0.4868(5) 0.5365(2) 0.0411(12) Uani 1 d . . . O8 O 1.0000 0.3356(6) 0.7500 0.050(2) Uani 1 d S . . N1 N 0.6590(2) 0.6039(5) 0.2935(3) 0.0404(15) Uani 1 d . . . N2 N 0.7203(2) 0.4002(5) 0.3634(3) 0.0394(15) Uani 1 d . . . C1 C 0.8033(3) 0.7358(7) 0.4313(3) 0.0342(19) Uani 1 d . . . C2 C 0.8487(3) 0.7015(6) 0.4264(3) 0.0312(18) Uani 1 d . . . C3 C 0.8502(3) 0.6041(6) 0.3798(4) 0.045(2) Uani 1 d . . . H3A H 0.8210 0.5537 0.3499 0.080 Uiso 1 d R . . C4 C 0.8927(4) 0.5780(7) 0.3755(5) 0.051(2) Uani 1 d . . . H4A H 0.8930 0.5122 0.3420 0.080 Uiso 1 d R . . C5 C 0.9354(3) 0.6484(7) 0.4203(4) 0.045(2) Uani 1 d . . . C6 C 0.9354(3) 0.7425(7) 0.4684(4) 0.045(2) Uani 1 d . . . H6A H 0.9656 0.7876 0.5002 0.080 Uiso 1 d R . . C7 C 0.8933(3) 0.7719(7) 0.4716(4) 0.042(2) Uani 1 d . . . H7A H 0.8939 0.8400 0.5044 0.080 Uiso 1 d R . . C8 C 1.0138(3) 0.7025(7) 0.4283(4) 0.045(2) Uani 1 d . . . C9 C 1.0623(3) 0.6580(7) 0.4658(4) 0.046(2) Uani 1 d . . . H9A H 1.0697 0.5736 0.4897 0.080 Uiso 1 d R . . C10 C 1.0993(3) 0.7367(7) 0.4683(4) 0.0412(18) Uani 1 d . . . H10A H 1.1330 0.7072 0.4932 0.080 Uiso 1 d R . . C11 C 1.0889(3) 0.8592(7) 0.4341(4) 0.0348(17) Uani 1 d . . . C12 C 1.0407(3) 0.9056(7) 0.3995(4) 0.044(2) Uani 1 d . . . H12A H 1.0343 0.9918 0.3779 0.080 Uiso 1 d R . . C13 C 1.0024(3) 0.8265(7) 0.3956(4) 0.047(2) Uani 1 d . . . H13A H 0.9689 0.8566 0.3713 0.080 Uiso 1 d R . . C14 C 1.1289(3) 0.9395(6) 0.4313(3) 0.0362(19) Uani 1 d . . . C15 C 0.8117(3) 0.5651(6) 0.5751(3) 0.0336(17) Uani 1 d . . . C16 C 0.8620(2) 0.5094(6) 0.6252(3) 0.0304(16) Uani 1 d . . . C17 C 0.8677(3) 0.3861(6) 0.6602(4) 0.0412(19) Uani 1 d . . . H17A H 0.8388 0.3399 0.6537 0.080 Uiso 1 d R . . C18 C 0.9143(3) 0.3346(7) 0.7039(4) 0.0410(19) Uani 1 d . . . H18A H 0.9186 0.2523 0.7293 0.080 Uiso 1 d R . . C19 C 0.9552(3) 0.4021(6) 0.7115(3) 0.0369(18) Uani 1 d . . . C20 C 0.9510(3) 0.5223(7) 0.6771(4) 0.0394(18) Uani 1 d . . . H20A H 0.9799 0.5665 0.6823 0.080 Uiso 1 d R . . C21 C 0.9042(3) 0.5758(6) 0.6356(4) 0.0389(18) Uani 1 d . . . H21A H 0.9007 0.6613 0.6139 0.080 Uiso 1 d R . . C22 C 0.6232(3) 0.6928(8) 0.2586(4) 0.058(2) Uani 1 d . . . H22A H 0.6172 0.7541 0.2890 0.080 Uiso 1 d R . . C23 C 0.5935(3) 0.7007(8) 0.1819(4) 0.066(3) Uani 1 d . . . H23A H 0.5693 0.7690 0.1599 0.080 Uiso 1 d R . . C24 C 0.6008(3) 0.6111(8) 0.1379(4) 0.063(3) Uani 1 d . . . H24A H 0.5805 0.6132 0.0846 0.080 Uiso 1 d R . . C25 C 0.6375(3) 0.5168(8) 0.1724(4) 0.058(2) Uani 1 d . . . H25A H 0.6425 0.4513 0.1429 0.080 Uiso 1 d R . . C26 C 0.6665(3) 0.5170(7) 0.2500(3) 0.0389(18) Uani 1 d . . . C27 C 0.7055(3) 0.4167(7) 0.2899(4) 0.0416(19) Uani 1 d . . . C28 C 0.7257(3) 0.3445(10) 0.2539(5) 0.075(3) Uani 1 d . . . H28A H 0.7169 0.3639 0.2030 0.080 Uiso 1 d R . . C29 C 0.7588(4) 0.2451(11) 0.2917(5) 0.093(4) Uani 1 d . . . H29A H 0.7734 0.1948 0.2676 0.080 Uiso 1 d R . . C30 C 0.7720(3) 0.2208(8) 0.3661(5) 0.068(3) Uani 1 d . . . H30A H 0.7924 0.1472 0.3925 0.080 Uiso 1 d R . . C31 C 0.7535(3) 0.3030(7) 0.4004(4) 0.048(2) Uani 1 d . . . H31A H 0.7646 0.2925 0.4528 0.080 Uiso 1 d R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Tb1 0.0209(3) 0.03454(17) 0.03132(16) -0.00102(13) 0.01237(13) -0.00271(14) O1 0.034(3) 0.053(3) 0.045(3) -0.008(2) 0.022(2) -0.012(2) O2 0.039(3) 0.047(3) 0.043(2) -0.007(2) 0.025(2) -0.006(2) O3 0.031(3) 0.053(3) 0.044(3) 0.009(2) 0.017(2) -0.004(2) O4 0.028(4) 0.043(3) 0.066(3) -0.002(2) 0.027(3) -0.008(2) O5 0.042(5) 0.047(3) 0.128(5) -0.016(3) 0.064(4) -0.017(3) O6 0.043(3) 0.032(2) 0.047(3) 0.0093(19) 0.022(2) 0.009(2) O7 0.021(3) 0.052(3) 0.039(2) 0.001(2) 0.005(2) -0.003(2) O8 0.025(5) 0.042(4) 0.059(4) 0.000 0.001(3) 0.000 N1 0.042(4) 0.042(3) 0.036(3) 0.001(2) 0.018(3) 0.000(3) N2 0.032(4) 0.042(3) 0.044(3) -0.006(2) 0.018(3) -0.004(3) C1 0.024(5) 0.050(4) 0.028(3) 0.000(3) 0.013(3) -0.006(3) C2 0.021(5) 0.044(4) 0.035(3) -0.001(3) 0.019(3) -0.005(3) C3 0.039(6) 0.044(4) 0.056(4) -0.008(3) 0.026(4) -0.011(3) C4 0.050(7) 0.046(4) 0.078(5) -0.013(4) 0.046(5) -0.008(4) C5 0.042(7) 0.043(4) 0.069(5) 0.002(3) 0.042(4) -0.008(4) C6 0.028(6) 0.058(4) 0.055(4) -0.007(4) 0.024(4) -0.011(4) C7 0.033(6) 0.049(4) 0.048(4) -0.009(3) 0.023(3) -0.011(4) C8 0.031(6) 0.052(4) 0.065(5) -0.007(4) 0.035(4) -0.011(4) C9 0.041(6) 0.050(4) 0.053(4) -0.005(3) 0.029(4) -0.005(4) C10 0.030(5) 0.055(4) 0.044(4) -0.003(3) 0.022(3) -0.006(4) C11 0.015(5) 0.050(4) 0.048(4) -0.008(3) 0.023(3) -0.014(3) C12 0.036(6) 0.048(4) 0.056(4) -0.001(3) 0.027(4) -0.008(4) C13 0.029(5) 0.054(4) 0.069(5) -0.007(4) 0.031(4) -0.006(4) C14 0.034(6) 0.045(4) 0.033(3) -0.010(3) 0.019(3) -0.015(3) C15 0.022(5) 0.047(4) 0.032(3) 0.003(3) 0.013(3) -0.004(3) C16 0.017(4) 0.037(3) 0.036(3) 0.002(2) 0.011(3) -0.003(3) C17 0.028(5) 0.047(4) 0.045(4) 0.001(3) 0.014(3) -0.007(3) C18 0.024(5) 0.048(4) 0.040(3) 0.002(3) 0.007(3) -0.002(3) C19 0.019(5) 0.044(4) 0.033(3) 0.003(3) 0.001(3) 0.005(3) C20 0.019(5) 0.046(4) 0.047(4) -0.004(3) 0.011(3) -0.008(3) C21 0.029(5) 0.040(4) 0.041(3) 0.002(3) 0.012(3) 0.000(3) C22 0.069(6) 0.056(5) 0.045(4) 0.001(3) 0.023(4) 0.013(4) C23 0.063(6) 0.065(5) 0.049(4) 0.013(4) 0.012(4) 0.019(4) C24 0.067(7) 0.079(6) 0.034(4) 0.001(4) 0.018(4) -0.001(5) C25 0.061(6) 0.063(5) 0.037(4) -0.012(3) 0.014(4) -0.003(4) C26 0.031(5) 0.050(4) 0.038(3) -0.011(3) 0.019(3) -0.011(3) C27 0.033(5) 0.044(4) 0.044(4) -0.011(3) 0.016(3) -0.004(3) C28 0.069(8) 0.103(7) 0.046(4) -0.022(5) 0.023(5) 0.021(6) C29 0.084(8) 0.116(8) 0.064(6) -0.027(6) 0.024(5) 0.044(7) C30 0.060(7) 0.063(5) 0.065(5) -0.018(4) 0.017(4) 0.019(4) C31 0.040(5) 0.050(4) 0.047(4) -0.009(3) 0.014(4) -0.001(4) _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 Tb1 O6 2.298(4) 7_666 ? Tb1 O2 2.353(5) 7_666 ? Tb1 O7 2.362(4) . ? Tb1 O1 2.379(5) . ? Tb1 O4 2.410(5) 3_445 ? Tb1 O3 2.465(5) 3_445 ? Tb1 N2 2.603(6) . ? Tb1 N1 2.607(5) . ? Tb1 C14 2.795(7) 3_445 ? O1 C1 1.266(8) . ? O2 C1 1.266(8) . ? O2 Tb1 2.353(5) 7_666 ? O3 C14 1.267(8) . ? O3 Tb1 2.465(5) 3 ? O4 C14 1.262(9) . ? O4 Tb1 2.410(5) 3 ? O5 C5 1.388(10) . ? O5 C8 1.407(9) . ? O6 C15 1.275(7) . ? O6 Tb1 2.298(4) 7_666 ? O7 C15 1.255(8) . ? O8 C19 1.394(7) 2_756 ? O8 C19 1.394(7) . ? N1 C22 1.339(9) . ? N1 C26 1.351(8) . ? N2 C27 1.355(9) . ? N2 C31 1.362(9) . ? C1 C2 1.495(10) . ? C2 C3 1.392(9) . ? C2 C7 1.430(10) . ? C3 C4 1.382(12) . ? C4 C5 1.391(11) . ? C5 C6 1.374(10) . ? C6 C7 1.363(11) . ? C8 C9 1.391(11) . ? C8 C13 1.392(10) . ? C9 C10 1.377(10) . ? C10 C11 1.389(9) . ? C11 C12 1.388(10) . ? C11 C14 1.508(10) . ? C12 C13 1.401(10) . ? C14 Tb1 2.795(7) 3 ? C15 C16 1.503(9) . ? C16 C21 1.391(9) . ? C16 C17 1.413(8) . ? C17 C18 1.381(9) . ? C18 C19 1.381(10) . ? C19 C20 1.385(9) . ? C20 C21 1.387(9) . ? C22 C23 1.386(10) . ? C23 C24 1.373(11) . ? C24 C25 1.393(11) . ? C25 C26 1.396(9) . ? C26 C27 1.489(10) . ? C27 C28 1.382(11) . ? C28 C29 1.380(12) . ? C29 C30 1.393(12) . ? C30 C31 1.379(11) . ? 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 O6 Tb1 O2 73.31(16) 7_666 7_666 ? O6 Tb1 O7 124.69(17) 7_666 . ? O2 Tb1 O7 79.64(17) 7_666 . ? O6 Tb1 O1 80.92(17) 7_666 . ? O2 Tb1 O1 128.60(16) 7_666 . ? O7 Tb1 O1 79.84(17) . . ? O6 Tb1 O4 137.90(18) 7_666 3_445 ? O2 Tb1 O4 77.62(17) 7_666 3_445 ? O7 Tb1 O4 77.77(17) . 3_445 ? O1 Tb1 O4 141.08(17) . 3_445 ? O6 Tb1 O3 90.19(17) 7_666 3_445 ? O2 Tb1 O3 77.19(16) 7_666 3_445 ? O7 Tb1 O3 129.39(16) . 3_445 ? O1 Tb1 O3 147.33(15) . 3_445 ? O4 Tb1 O3 53.64(17) 3_445 3_445 ? O6 Tb1 N2 137.77(17) 7_666 . ? O2 Tb1 N2 148.85(17) 7_666 . ? O7 Tb1 N2 80.81(17) . . ? O1 Tb1 N2 70.59(17) . . ? O4 Tb1 N2 74.69(19) 3_445 . ? O3 Tb1 N2 97.24(18) 3_445 . ? O6 Tb1 N1 81.11(16) 7_666 . ? O2 Tb1 N1 138.85(18) 7_666 . ? O7 Tb1 N1 141.27(18) . . ? O1 Tb1 N1 76.44(18) . . ? O4 Tb1 N1 102.71(18) 3_445 . ? O3 Tb1 N1 71.13(17) 3_445 . ? N2 Tb1 N1 62.64(17) . . ? O6 Tb1 C14 114.1(2) 7_666 3_445 ? O2 Tb1 C14 74.24(17) 7_666 3_445 ? O7 Tb1 C14 103.18(19) . 3_445 ? O1 Tb1 C14 156.74(17) . 3_445 ? O4 Tb1 C14 26.77(18) 3_445 3_445 ? O3 Tb1 C14 26.96(17) 3_445 3_445 ? N2 Tb1 C14 86.98(19) . 3_445 ? N1 Tb1 C14 88.02(18) . 3_445 ? C1 O1 Tb1 134.9(5) . . ? C1 O2 Tb1 133.2(4) . 7_666 ? C14 O3 Tb1 91.2(4) . 3 ? C14 O4 Tb1 93.9(4) . 3 ? C5 O5 C8 119.3(6) . . ? C15 O6 Tb1 175.6(5) . 7_666 ? C15 O7 Tb1 114.1(4) . . ? C19 O8 C19 121.9(7) 2_756 . ? C22 N1 C26 116.9(6) . . ? C22 N1 Tb1 121.5(5) . . ? C26 N1 Tb1 121.5(4) . . ? C27 N2 C31 117.8(6) . . ? C27 N2 Tb1 119.9(4) . . ? C31 N2 Tb1 119.7(4) . . ? O2 C1 O1 125.1(7) . . ? O2 C1 C2 118.0(6) . . ? O1 C1 C2 116.9(6) . . ? C3 C2 C7 117.2(8) . . ? C3 C2 C1 123.7(6) . . ? C7 C2 C1 119.1(6) . . ? C4 C3 C2 121.9(7) . . ? C3 C4 C5 119.2(8) . . ? C6 C5 O5 124.0(7) . . ? C6 C5 C4 120.2(9) . . ? O5 C5 C4 115.6(7) . . ? C7 C6 C5 121.0(7) . . ? C6 C7 C2 120.4(7) . . ? C9 C8 C13 121.1(7) . . ? C9 C8 O5 115.8(7) . . ? C13 C8 O5 122.6(7) . . ? C10 C9 C8 119.1(7) . . ? C9 C10 C11 121.1(7) . . ? C12 C11 C10 119.7(7) . . ? C12 C11 C14 119.7(7) . . ? C10 C11 C14 120.6(7) . . ? C11 C12 C13 120.1(7) . . ? C8 C13 C12 118.9(7) . . ? O4 C14 O3 120.9(7) . . ? O4 C14 C11 118.1(6) . . ? O3 C14 C11 120.9(7) . . ? O4 C14 Tb1 59.4(4) . 3 ? O3 C14 Tb1 61.9(4) . 3 ? C11 C14 Tb1 175.4(4) . 3 ? O7 C15 O6 124.3(6) . . ? O7 C15 C16 118.2(6) . . ? O6 C15 C16 117.5(6) . . ? C21 C16 C17 118.3(6) . . ? C21 C16 C15 120.5(6) . . ? C17 C16 C15 121.1(6) . . ? C18 C17 C16 120.1(7) . . ? C19 C18 C17 119.8(6) . . ? C18 C19 C20 121.6(6) . . ? C18 C19 O8 115.4(6) . . ? C20 C19 O8 122.8(7) . . ? C19 C20 C21 118.3(7) . . ? C20 C21 C16 121.8(6) . . ? N1 C22 C23 124.6(7) . . ? C24 C23 C22 118.4(8) . . ? C23 C24 C25 118.5(7) . . ? C24 C25 C26 119.7(7) . . ? N1 C26 C25 121.9(7) . . ? N1 C26 C27 116.1(6) . . ? C25 C26 C27 121.9(6) . . ? N2 C27 C28 121.8(7) . . ? N2 C27 C26 116.4(6) . . ? C28 C27 C26 121.9(7) . . ? C29 C28 C27 119.6(8) . . ? C28 C29 C30 119.4(8) . . ? C31 C30 C29 118.1(8) . . ? N2 C31 C30 123.0(7) . . ? _diffrn_measured_fraction_theta_max 0.347 _diffrn_reflns_theta_full 27.02 _diffrn_measured_fraction_theta_full 0.347 _refine_diff_density_max 0.978 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.115 #_eof #End of Crystallographic Information File