# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name _publ_author_address 'M. L. P. Reddy' ; Chemical Science and Technology Division National Institute for Interdisciplinary Science and Technology (NIST), Thiruvananthapuram-695 019, India ; 'Shyni Raphael' ; Chemical Science and Technology Division National Institute for Interdisciplinary Science and Technology (NIST), Thiruvananthapuram-695 019, India ; 'Alan H. Cowley' ; The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78701 USA ; 'Kalyan V. Vasudevan' ; The University of Texas at Austin Department of Chemistry and Biochemistry 1 University Station, A5300 Austin, TX 78701 USA ; _publ_contact_author_address ; Chemical Sciences and Technology Division National Institute for Interdisciplinary Science & Technology (NIIST) Thiruvananthapuram-695 019, India ; _publ_contact_author_email 'mlpreddy55@gmail.com ' _publ_contact_author_fax 'AUTHOR FAX' _publ_contact_author_phone 'AUTHOR PHONE' # 1. SUBMISSION DETAILS _publ_contact_author_name 'M.L.P. Reddy' _publ_contact_letter ; Please consider this CIF submission for publication in ; # 2. TITLE AND AUTHOR LIST _publ_section_title ; Article Title ; data_sbkv195b _database_code_depnum_ccdc_archive 'CCDC 756460' #TrackingRef '- sbkv195b_final.cif' _database_code_CSD XXXXXXX _audit_creation_method ; manual editing of the .cif file created by SHELXTL Ver. 6.10 ; _publ_section_synopsis ; ; _publ_section_abstract ; ; _publ_section_comment ; ; _publ_section_references ; Allen, F.H. (2002). Acta Cryst. B58, 380-388. Cremer D. & Pople J.A. (1975). J. Am. Chem. Soc. 97, 1358-1367. Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (1998). SHELXTL/PC. Release 5.10. Siemens Analytical X-ray Instruments, Inc., Madison, WI, USA. Sluis, P. v.d. & Spek, A. L. (1990). SQUEEZE. Acta Cryst. A46, 194-201. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_figure_captions ; ; _publ_section_exptl_prep ; ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C69 H60 N3 O9 Tb' _chemical_formula_sum 'C69 H60 N3 O9 Tb' _chemical_formula_weight 1234.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0030 0.0020 '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 0.0060 0.0030 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0110 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1720 4.1540 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Rhombohedral _symmetry_space_group_name_H-M R-3 _symmetry_space_group_name_Hall ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'z, x, y' 'y, z, x' '-x, -y, -z' '-z, -x, -y' '-y, -z, -x' _cell_length_a 18.865(2) _cell_length_b 18.865(2) _cell_length_c 18.865(2) _cell_angle_alpha 117.220(17) _cell_angle_beta 117.220(17) _cell_angle_gamma 117.220(17) _cell_volume 2855.9(48) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 10562 _cell_measurement_theta_min 1.00 _cell_measurement_theta_max 27.48 _exptl_crystal_description Needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.301 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min .925 _exptl_absorpt_correction_T_max .949 _exptl_absorpt_process_details 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa CCD' _diffrn_measurement_method \w-scan _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16805 _diffrn_reflns_av_R_equivalents 0.0976 _diffrn_reflns_av_sigmaI/netI 0.0753 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3450 _reflns_number_gt 2210 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material 'WinGX (Farrugia, J. Appl. Crystallogr., 1999, 32, 837-838)' _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^)+(0.0204P)^2^+3.0007P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3450 _refine_ls_number_parameters 248 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0951 _refine_ls_R_factor_gt 0.0431 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.055 _refine_ls_shift/su_max 0.003 _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 C1 C 1.1950(5) 1.2241(5) 0.3371(5) 0.0406(11) Uani 1 1 d . . . C2 C 1.1650(5) 1.2271(5) 0.3977(5) 0.0344(11) Uani 1 1 d . . . C3 C 1.2805(5) 1.3474(5) 0.5495(5) 0.0433(12) Uani 1 1 d . . . H3 H 1.3772 1.4280 0.6136 0.052 Uiso 1 1 calc R . . C4 C 1.2539(5) 1.3491(5) 0.6060(5) 0.0481(12) Uani 1 1 d . . . H4 H 1.3325 1.4308 0.7081 0.058 Uiso 1 1 calc R . . C5 C 1.1105(5) 1.2297(5) 0.5122(5) 0.0408(12) Uani 1 1 d . . . C6 C 0.9934(5) 1.1108(5) 0.3609(5) 0.0462(12) Uani 1 1 d . . . H6 H 0.8966 1.0316 0.2972 0.055 Uiso 1 1 calc R . . C7 C 1.0219(5) 1.1108(5) 0.3052(5) 0.0427(12) Uani 1 1 d . . . H7 H 0.9431 1.0307 0.2032 0.051 Uiso 1 1 calc R . . C8 C 0.9528(6) 1.1176(6) 0.4891(6) 0.0601(14) Uani 1 1 d . . . H8A H 0.9030 1.0257 0.4141 0.072 Uiso 1 1 calc R . . H8B H 0.8940 1.1112 0.4397 0.072 Uiso 1 1 calc R . . C9 C 0.9700(6) 1.1427(7) 0.5881(7) 0.0693(16) Uani 1 1 d . . . H9A H 0.8724 1.0625 0.5281 0.083 Uiso 1 1 calc R . . H9B H 1.0184 1.2341 0.6611 0.083 Uiso 1 1 calc R . . C10 C 1.0592(5) 1.1517(6) 0.6688(6) 0.0595(15) Uani 1 1 d . . . H10A H 1.0201 1.1103 0.6792 0.071 Uiso 1 1 calc R . . H10B H 1.0453 1.0909 0.6081 0.071 Uiso 1 1 calc R . . C11 C 1.2238(6) 1.3073(6) 0.8208(6) 0.0592(14) Uani 1 1 d . . . H11A H 1.2589 1.3579 0.8151 0.071 Uiso 1 1 calc R . . H11B H 1.2402 1.3615 0.8890 0.071 Uiso 1 1 calc R . . C12 C 1.3315(5) 1.2963(5) 0.9506(5) 0.0446(12) Uani 1 1 d . . . C13 C 1.2935(5) 1.2959(5) 0.9980(5) 0.0520(13) Uani 1 1 d . . . H13 H 1.2475 1.3066 0.9853 0.062 Uiso 1 1 calc R . . C14 C 1.3261(5) 1.2791(5) 1.0647(5) 0.0539(14) Uani 1 1 d . . . H14 H 1.3026 1.2801 1.0987 0.065 Uiso 1 1 calc R . . C15 C 1.3928(5) 1.2608(5) 1.0829(5) 0.0510(13) Uani 1 1 d . . . H15 H 1.4108 1.2471 1.1261 0.061 Uiso 1 1 calc R . . C16 C 1.4327(5) 1.2629(5) 1.0368(5) 0.0467(12) Uani 1 1 d . . . H16 H 1.4782 1.2516 1.0496 0.056 Uiso 1 1 calc R . . C17 C 1.4033(5) 1.2822(5) 0.9709(5) 0.0402(12) Uani 1 1 d . . . C18 C 1.4280(5) 1.2883(5) 0.9104(5) 0.0461(13) Uani 1 1 d . . . C19 C 1.4931(5) 1.2839(5) 0.8985(5) 0.0565(14) Uani 1 1 d . . . H19 H 1.5348 1.2753 0.9363 0.068 Uiso 1 1 calc R . . C20 C 1.4972(6) 1.2923(6) 0.8313(6) 0.0582(14) Uani 1 1 d . . . H20 H 1.5403 1.2877 0.8227 0.070 Uiso 1 1 calc R . . C21 C 1.4372(6) 1.3075(6) 0.7761(6) 0.0656(16) Uani 1 1 d . . . H21 H 1.4420 1.3143 0.7322 0.079 Uiso 1 1 calc R . . C22 C 1.3705(6) 1.3127(5) 0.7850(5) 0.0595(15) Uani 1 1 d . . . H22 H 1.3293 1.3215 0.7470 0.071 Uiso 1 1 calc R . . C23 C 1.3675(5) 1.3041(5) 0.8538(5) 0.0494(12) Uani 1 1 d . . . N1 N 1.3094(4) 1.3083(4) 0.8784(4) 0.0521(10) Uani 1 1 d . . . O1 O 1.3279(3) 1.3301(3) 0.4268(3) 0.0484(8) Uani 1 1 d . . . O2 O 1.0871(3) 1.1149(3) 0.1983(3) 0.0470(8) Uani 1 1 d . . . O3 O 1.0971(4) 1.2394(3) 0.5801(4) 0.0505(9) Uani 1 1 d . . . Tb1 Tb 1.5000 1.5000 0.5000 0.03698(18) Uani 1 6 d S . . Tb2 Tb 1.0000 1.0000 0.0000 0.03440(18) Uani 1 6 d S . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.040(3) 0.035(3) 0.037(3) 0.031(3) 0.031(3) 0.031(3) C2 0.035(2) 0.030(2) 0.033(2) 0.026(2) 0.028(2) 0.026(2) C3 0.032(3) 0.034(3) 0.034(3) 0.027(3) 0.026(2) 0.024(2) C4 0.040(3) 0.030(3) 0.028(2) 0.022(2) 0.026(2) 0.024(2) C5 0.049(3) 0.041(3) 0.046(3) 0.037(3) 0.042(3) 0.039(3) C6 0.033(3) 0.043(3) 0.042(3) 0.035(3) 0.030(3) 0.029(3) C7 0.037(3) 0.037(3) 0.033(3) 0.028(2) 0.027(2) 0.030(3) C8 0.072(4) 0.087(4) 0.083(4) 0.078(4) 0.070(4) 0.071(4) C9 0.088(4) 0.110(5) 0.103(4) 0.098(4) 0.088(4) 0.091(4) C10 0.064(4) 0.079(4) 0.084(4) 0.075(4) 0.065(4) 0.064(4) C11 0.078(4) 0.071(4) 0.071(4) 0.063(4) 0.066(4) 0.067(4) C12 0.049(3) 0.042(3) 0.046(3) 0.038(3) 0.041(3) 0.038(3) C13 0.059(3) 0.051(3) 0.052(3) 0.043(3) 0.049(3) 0.046(3) C14 0.044(3) 0.039(3) 0.039(3) 0.027(3) 0.036(3) 0.030(3) C15 0.043(3) 0.036(3) 0.037(3) 0.030(3) 0.032(3) 0.027(3) C16 0.038(3) 0.035(3) 0.035(3) 0.027(2) 0.028(2) 0.028(2) C17 0.031(3) 0.027(3) 0.029(3) 0.020(2) 0.023(2) 0.022(2) C18 0.040(3) 0.037(3) 0.039(3) 0.028(3) 0.032(3) 0.032(3) C19 0.051(3) 0.053(3) 0.056(3) 0.044(3) 0.045(3) 0.043(3) C20 0.068(4) 0.063(3) 0.071(4) 0.057(3) 0.064(3) 0.057(3) C21 0.077(4) 0.063(4) 0.065(4) 0.054(3) 0.064(4) 0.057(4) C22 0.071(4) 0.064(4) 0.060(4) 0.055(3) 0.056(3) 0.058(4) C23 0.053(3) 0.046(3) 0.049(3) 0.039(3) 0.044(3) 0.041(3) N1 0.064(3) 0.061(3) 0.059(3) 0.052(2) 0.054(2) 0.056(3) O1 0.0378(19) 0.0421(18) 0.0412(18) 0.0340(17) 0.0326(17) 0.0294(17) O2 0.0429(18) 0.0406(18) 0.0328(18) 0.0293(17) 0.0309(17) 0.0318(17) O3 0.052(2) 0.050(2) 0.052(2) 0.0419(19) 0.0460(19) 0.0423(19) Tb1 0.0276(3) 0.0276(3) 0.0276(3) 0.0209(3) 0.0209(3) 0.0209(3) Tb2 0.0255(3) 0.0255(3) 0.0255(3) 0.0193(3) 0.0193(3) 0.0193(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 C1 O1 1.259(6) . ? C1 O2 1.264(6) . ? C1 C2 1.479(6) . ? C2 C7 1.385(6) . ? C2 C3 1.387(6) . ? C3 C4 1.365(6) . ? C3 H3 0.9300 . ? C4 C5 1.387(7) . ? C4 H4 0.9300 . ? C5 O3 1.365(5) . ? C5 C6 1.378(7) . ? C6 C7 1.383(6) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 O3 1.425(6) . ? C8 C9 1.521(7) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.529(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.516(8) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 N1 1.462(6) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C13 1.379(6) . ? C12 N1 1.389(6) . ? C12 C17 1.413(6) . ? C13 C14 1.377(7) . ? C13 H13 0.9300 . ? C14 C15 1.391(7) . ? C14 H14 0.9300 . ? C15 C16 1.388(6) . ? C15 H15 0.9300 . ? C16 C17 1.398(6) . ? C16 H16 0.9300 . ? C17 C18 1.447(7) . ? C18 C19 1.376(6) . ? C18 C23 1.419(6) . ? C19 C20 1.379(7) . ? C19 H19 0.9300 . ? C20 C21 1.393(7) . ? C20 H20 0.9300 . ? C21 C22 1.383(7) . ? C21 H21 0.9300 . ? C22 C23 1.400(7) . ? C22 H22 0.9300 . ? C23 N1 1.393(6) . ? O1 Tb1 2.247(4) . ? O2 Tb2 2.256(3) . ? Tb1 O1 2.247(4) 6_877 ? Tb1 O1 2.247(4) 2_654 ? Tb1 O1 2.247(4) 4_886 ? Tb1 O1 2.247(4) 5_787 ? Tb1 O1 2.247(4) 3_564 ? Tb2 O2 2.256(3) 2_654 ? Tb2 O2 2.256(3) 6_766 ? Tb2 O2 2.256(3) 3_564 ? Tb2 O2 2.256(3) 4_775 ? Tb2 O2 2.256(3) 5_676 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 122.7(4) . . ? O1 C1 C2 118.2(4) . . ? O2 C1 C2 119.1(4) . . ? C7 C2 C3 118.2(4) . . ? C7 C2 C1 121.3(4) . . ? C3 C2 C1 120.5(4) . . ? C4 C3 C2 120.8(4) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 120.4(4) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? O3 C5 C6 124.5(4) . . ? O3 C5 C4 115.7(4) . . ? C6 C5 C4 119.9(5) . . ? C5 C6 C7 119.1(4) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C6 C7 C2 121.6(4) . . ? C6 C7 H7 119.2 . . ? C2 C7 H7 119.2 . . ? O3 C8 C9 107.9(5) . . ? O3 C8 H8A 110.1 . . ? C9 C8 H8A 110.1 . . ? O3 C8 H8B 110.1 . . ? C9 C8 H8B 110.1 . . ? H8A C8 H8B 108.4 . . ? C8 C9 C10 113.9(4) . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C11 C10 C9 114.3(5) . . ? C11 C10 H10A 108.7 . . ? C9 C10 H10A 108.7 . . ? C11 C10 H10B 108.7 . . ? C9 C10 H10B 108.7 . . ? H10A C10 H10B 107.6 . . ? N1 C11 C10 112.4(4) . . ? N1 C11 H11A 109.1 . . ? C10 C11 H11A 109.1 . . ? N1 C11 H11B 109.1 . . ? C10 C11 H11B 109.1 . . ? H11A C11 H11B 107.9 . . ? C13 C12 N1 129.5(5) . . ? C13 C12 C17 121.8(5) . . ? N1 C12 C17 108.6(4) . . ? C14 C13 C12 117.6(5) . . ? C14 C13 H13 121.2 . . ? C12 C13 H13 121.2 . . ? C13 C14 C15 122.3(5) . . ? C13 C14 H14 118.8 . . ? C15 C14 H14 118.8 . . ? C16 C15 C14 120.1(5) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C15 C16 C17 118.9(5) . . ? C15 C16 H16 120.5 . . ? C17 C16 H16 120.5 . . ? C16 C17 C12 119.2(5) . . ? C16 C17 C18 133.3(5) . . ? C12 C17 C18 107.5(4) . . ? C19 C18 C23 118.2(5) . . ? C19 C18 C17 135.8(5) . . ? C23 C18 C17 106.0(4) . . ? C18 C19 C20 120.7(5) . . ? C18 C19 H19 119.6 . . ? C20 C19 H19 119.6 . . ? C19 C20 C21 120.3(5) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C22 C21 C20 121.5(5) . . ? C22 C21 H21 119.3 . . ? C20 C21 H21 119.3 . . ? C21 C22 C23 117.3(5) . . ? C21 C22 H22 121.4 . . ? C23 C22 H22 121.4 . . ? N1 C23 C22 128.8(5) . . ? N1 C23 C18 109.2(4) . . ? C22 C23 C18 122.0(5) . . ? C12 N1 C23 108.7(4) . . ? C12 N1 C11 126.3(4) . . ? C23 N1 C11 124.5(4) . . ? C1 O1 Tb1 148.1(3) . . ? C1 O2 Tb2 150.0(3) . . ? C5 O3 C8 118.2(4) . . ? O1 Tb1 O1 91.00(16) 6_877 2_654 ? O1 Tb1 O1 89.00(16) 6_877 4_886 ? O1 Tb1 O1 91.00(16) 2_654 4_886 ? O1 Tb1 O1 91.00(16) 6_877 . ? O1 Tb1 O1 89.00(16) 2_654 . ? O1 Tb1 O1 180.000(1) 4_886 . ? O1 Tb1 O1 89.00(16) 6_877 5_787 ? O1 Tb1 O1 180.000(2) 2_654 5_787 ? O1 Tb1 O1 89.00(16) 4_886 5_787 ? O1 Tb1 O1 91.00(16) . 5_787 ? O1 Tb1 O1 180.000(1) 6_877 3_564 ? O1 Tb1 O1 89.00(16) 2_654 3_564 ? O1 Tb1 O1 91.00(16) 4_886 3_564 ? O1 Tb1 O1 89.00(16) . 3_564 ? O1 Tb1 O1 91.00(16) 5_787 3_564 ? O2 Tb2 O2 88.70(16) 2_654 6_766 ? O2 Tb2 O2 91.30(16) 2_654 3_564 ? O2 Tb2 O2 180.00(14) 6_766 3_564 ? O2 Tb2 O2 91.30(16) 2_654 . ? O2 Tb2 O2 88.70(16) 6_766 . ? O2 Tb2 O2 91.30(16) 3_564 . ? O2 Tb2 O2 88.70(16) 2_654 4_775 ? O2 Tb2 O2 91.30(16) 6_766 4_775 ? O2 Tb2 O2 88.70(16) 3_564 4_775 ? O2 Tb2 O2 180.0(3) . 4_775 ? O2 Tb2 O2 180.00(14) 2_654 5_676 ? O2 Tb2 O2 91.30(16) 6_766 5_676 ? O2 Tb2 O2 88.70(16) 3_564 5_676 ? O2 Tb2 O2 88.70(16) . 5_676 ? O2 Tb2 O2 91.30(16) 4_775 5_676 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C7 -176.8(4) . . . . ? O2 C1 C2 C7 2.2(6) . . . . ? O1 C1 C2 C3 3.2(6) . . . . ? O2 C1 C2 C3 -177.8(4) . . . . ? C7 C2 C3 C4 1.8(7) . . . . ? C1 C2 C3 C4 -178.2(4) . . . . ? C2 C3 C4 C5 0.3(7) . . . . ? C3 C4 C5 O3 176.8(4) . . . . ? C3 C4 C5 C6 -2.3(7) . . . . ? O3 C5 C6 C7 -176.9(4) . . . . ? C4 C5 C6 C7 2.1(7) . . . . ? C5 C6 C7 C2 0.1(7) . . . . ? C3 C2 C7 C6 -2.0(7) . . . . ? C1 C2 C7 C6 178.0(4) . . . . ? O3 C8 C9 C10 -60.8(6) . . . . ? C8 C9 C10 C11 91.6(6) . . . . ? C9 C10 C11 N1 -166.0(4) . . . . ? N1 C12 C13 C14 178.6(5) . . . . ? C17 C12 C13 C14 -0.9(7) . . . . ? C12 C13 C14 C15 -1.0(7) . . . . ? C13 C14 C15 C16 1.7(8) . . . . ? C14 C15 C16 C17 -0.6(7) . . . . ? C15 C16 C17 C12 -1.2(7) . . . . ? C15 C16 C17 C18 -179.3(5) . . . . ? C13 C12 C17 C16 2.0(7) . . . . ? N1 C12 C17 C16 -177.7(4) . . . . ? C13 C12 C17 C18 -179.4(5) . . . . ? N1 C12 C17 C18 0.9(5) . . . . ? C16 C17 C18 C19 -3.1(10) . . . . ? C12 C17 C18 C19 178.5(6) . . . . ? C16 C17 C18 C23 177.6(5) . . . . ? C12 C17 C18 C23 -0.8(5) . . . . ? C23 C18 C19 C20 -1.0(8) . . . . ? C17 C18 C19 C20 179.8(6) . . . . ? C18 C19 C20 C21 0.9(8) . . . . ? C19 C20 C21 C22 -0.9(8) . . . . ? C20 C21 C22 C23 0.9(8) . . . . ? C21 C22 C23 N1 179.3(5) . . . . ? C21 C22 C23 C18 -1.0(8) . . . . ? C19 C18 C23 N1 -179.1(4) . . . . ? C17 C18 C23 N1 0.3(5) . . . . ? C19 C18 C23 C22 1.0(7) . . . . ? C17 C18 C23 C22 -179.5(5) . . . . ? C13 C12 N1 C23 179.6(5) . . . . ? C17 C12 N1 C23 -0.8(5) . . . . ? C13 C12 N1 C11 -7.3(8) . . . . ? C17 C12 N1 C11 172.3(4) . . . . ? C22 C23 N1 C12 -179.9(5) . . . . ? C18 C23 N1 C12 0.3(5) . . . . ? C22 C23 N1 C11 6.8(8) . . . . ? C18 C23 N1 C11 -173.0(4) . . . . ? C10 C11 N1 C12 -83.0(6) . . . . ? C10 C11 N1 C23 89.1(6) . . . . ? O2 C1 O1 Tb1 48.5(8) . . . . ? C2 C1 O1 Tb1 -132.5(5) . . . . ? O1 C1 O2 Tb2 -3.1(9) . . . . ? C2 C1 O2 Tb2 178.0(4) . . . . ? C6 C5 O3 C8 1.2(7) . . . . ? C4 C5 O3 C8 -177.8(4) . . . . ? C9 C8 O3 C5 169.9(4) . . . . ? C1 O1 Tb1 O1 -174.8(5) . . . 6_877 ? C1 O1 Tb1 O1 -83.8(5) . . . 2_654 ? C1 O1 Tb1 O1 26(100) . . . 4_886 ? C1 O1 Tb1 O1 96.2(5) . . . 5_787 ? C1 O1 Tb1 O1 5.2(5) . . . 3_564 ? C1 O2 Tb2 O2 35.1(6) . . . 2_654 ? C1 O2 Tb2 O2 123.8(5) . . . 6_766 ? C1 O2 Tb2 O2 -56.2(5) . . . 3_564 ? C1 O2 Tb2 O2 -45(100) . . . 4_775 ? C1 O2 Tb2 O2 -144.9(6) . . . 5_676 ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.943 _refine_diff_density_min -0.810 _refine_diff_density_rms 0.139