Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2002 data_rw3d _database_code_CSD 167051 _journal_coden_Cambridge 182 _publ_requested_journal 'Chemical Communications' loop_ _publ_author_name 'Wang, Suning' 'Song, Datong' 'Wang, Bo-Jie' _publ_contact_author_name 'Prof Suning Wang' _publ_contact_author_address ; Prof Suning Wang Department of Chemistry Queen's University Kingston Ontario K7L 3N6 CANADA ; _publ_contact_author_email 'WANGS@CHEM.QUEENSU.CA' _publ_section_title ; Toward Constructing Nanoscale Hydroxo-lanthanide Clusters: Syntheses and Characterization of Novel Tetradeca-nuclear Hydroxo-lanthanide Clusters ; _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Tb14(OH)18(acac)24 _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C122 H190.6 O66 Tb14' _chemical_formula_weight 4937.6 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 Tetragonal _symmetry_space_group_name_H-M I4/mmm loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-y, x, z' 'y, -x, z' '-x, y, -z' 'x, -y, -z' 'y, x, -z' '-y, -x, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-y+1/2, x+1/2, z+1/2' 'y+1/2, -x+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z+1/2' 'y+1/2, x+1/2, -z+1/2' '-y+1/2, -x+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z' 'y, -x, -z' '-y, x, -z' 'x, -y, z' '-x, y, z' '-y, -x, z' 'y, x, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, y+1/2, -z+1/2' 'y+1/2, -x+1/2, -z+1/2' '-y+1/2, x+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1/2' '-y+1/2, -x+1/2, z+1/2' 'y+1/2, x+1/2, z+1/2' _cell_length_a 21.090(4) _cell_length_b 21.090(4) _cell_length_c 21.213(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9436(3) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max .2 _exptl_crystal_size_mid .3 _exptl_crystal_size_min .5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.738 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4721 _exptl_absorpt_coefficient_mu 5.241 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.677 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 34150 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0269 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 28.33 _reflns_number_total 3210 _reflns_number_gt 2487 _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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+172.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000043(10) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3210 _refine_ls_number_parameters 185 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0731 _refine_ls_R_factor_gt 0.0566 _refine_ls_wR_factor_ref 0.1480 _refine_ls_wR_factor_gt 0.1409 _refine_ls_goodness_of_fit_ref 1.170 _refine_ls_restrained_S_all 1.170 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.09411(3) 0.09411(3) 0.5000 0.0363(2) Uani 1 4 d S . . Tb2 Tb 0.0000 0.12025(3) 0.23904(3) 0.0456(2) Uani 1 2 d S . . Tb3 Tb 0.0000 0.0000 0.37031(4) 0.0315(3) Uani 1 8 d S . . O1 O 0.0000 0.1896(5) 0.3247(5) 0.066(3) Uani 1 2 d S . . O2 O -0.0673(4) 0.2007(4) 0.2076(4) 0.072(2) Uani 1 1 d . . . O3 O 0.1310(3) 0.1310(3) 0.3983(4) 0.050(2) Uani 1 2 d S . . O4 O 0.0949(5) 0.2059(4) 0.5000 0.056(3) Uani 1 2 d S . . O5 O 0.0785(4) 0.0785(4) 0.1640(4) 0.056(2) Uani 1 2 d S . . O6 O 0.0000 0.0000 0.2250(7) 0.042(4) Uani 1 8 d S . . O7 O 0.0685(3) 0.0685(3) 0.3067(4) 0.0419(19) Uani 1 2 d S . . H7 H 0.0964 0.0964 0.3311 0.050 Uiso 1 2 calc SR . . O8 O 0.0000 0.0940(4) 0.4345(3) 0.0389(17) Uani 1 2 d S . . H8 H 0.0000 0.1317 0.4074 0.047 Uiso 1 2 calc SR . . C1 C 0.0000 0.2796(11) 0.3873(9) 0.039(5) Uani 0.50 2 d SP . . C2 C 0.0177(10) 0.2458(11) 0.3265(10) 0.063(7) Uani 0.50 1 d P . . C3 C -0.0471(11) 0.2851(11) 0.2812(10) 0.066(6) Uani 0.50 1 d P . . C4 C -0.0720(13) 0.2588(15) 0.2263(13) 0.082(8) Uani 0.50 1 d P . . C5 C -0.1139(10) 0.2961(9) 0.1701(14) 0.166(11) Uani 1 1 d . . . C6 C -0.0966(12) 0.2148(12) 0.1581(13) 0.077(7) Uani 0.50 1 d P . . C7 C 0.1958(14) 0.1758(14) 0.3194(10) 0.071(12) Uani 0.50 1 d P . . C8 C 0.164(2) 0.180(2) 0.3832(8) 0.057(17) Uani 0.50 1 d P . . C9 C 0.1711(13) 0.2280(12) 0.4186(10) 0.076(7) Uani 0.50 1 d P . . C10 C 0.1363(13) 0.2430(10) 0.4725(11) 0.074(7) Uani 0.50 1 d P . . C11 C 0.1384(15) 0.3112(11) 0.5000 0.117(9) Uani 1 2 d S . . C12 C 0.1172(13) 0.1741(16) 0.1136(11) 0.089(9) Uani 0.50 1 d P . . C13 C 0.0559(16) 0.1378(14) 0.0739(11) 0.096(10) Uani 0.50 1 d P . . C14 C 0.1084(7) 0.1084(7) 0.1195(7) 0.071(5) Uani 1 2 d S . . C15 C 0.0000 0.5000 0.287(6) 0.25(7) Uiso 0.50 4 d SP . . C16 C 0.049(4) 0.5000 0.530(4) 0.27(6) Uiso 0.50 2 d SP . . 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 0.0392(3) 0.0392(3) 0.0305(3) 0.000 0.000 -0.0043(3) Tb2 0.0555(4) 0.0483(4) 0.0331(3) 0.0077(2) 0.000 0.000 Tb3 0.0351(4) 0.0351(4) 0.0242(4) 0.000 0.000 0.000 O1 0.103(9) 0.047(6) 0.048(5) 0.005(5) 0.000 0.000 O2 0.081(6) 0.067(5) 0.066(5) 0.005(4) -0.018(4) 0.014(4) O3 0.057(3) 0.057(3) 0.036(4) 0.001(3) 0.001(3) -0.010(5) O4 0.086(7) 0.037(5) 0.046(5) 0.000 0.000 -0.010(5) O5 0.064(4) 0.064(4) 0.040(4) 0.010(3) 0.010(3) 0.001(5) O6 0.047(6) 0.047(6) 0.033(8) 0.000 0.000 0.000 O7 0.047(3) 0.047(3) 0.032(4) 0.001(2) 0.001(2) -0.002(4) O8 0.052(5) 0.036(4) 0.030(3) 0.002(3) 0.000 0.000 C1 0.055(15) 0.040(13) 0.023(9) -0.012(9) 0.000 0.000 C2 0.064(19) 0.067(13) 0.059(10) 0.004(10) -0.012(9) -0.001(10) C3 0.070(14) 0.069(14) 0.058(11) 0.004(11) -0.005(11) 0.026(12) C4 0.076(17) 0.09(2) 0.076(15) 0.010(15) -0.025(13) -0.002(15) C5 0.129(16) 0.101(14) 0.27(3) 0.084(17) 0.031(18) 0.038(13) C6 0.077(16) 0.069(15) 0.085(16) 0.024(13) -0.018(14) 0.027(13) C7 0.07(2) 0.08(2) 0.064(10) 0.003(11) 0.010(11) -0.01(2) C8 0.046(19) 0.08(4) 0.046(7) 0.019(14) -0.011(12) -0.02(3) C9 0.097(18) 0.078(16) 0.052(11) 0.010(11) -0.001(12) -0.034(14) C10 0.12(2) 0.036(10) 0.067(12) 0.004(9) -0.019(13) -0.008(12) C11 0.19(3) 0.076(14) 0.089(14) 0.000 0.000 -0.041(16) C12 0.088(18) 0.13(2) 0.052(12) 0.041(15) 0.004(12) -0.011(17) C13 0.14(3) 0.10(2) 0.046(11) 0.040(13) 0.016(15) 0.011(19) C14 0.088(7) 0.088(7) 0.038(7) 0.019(6) 0.019(6) 0.009(10) _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 O4 2.357(9) . ? Tb1 O4 2.357(9) 7_556 ? Tb1 O8 2.423(4) . ? Tb1 O8 2.423(4) 4 ? Tb1 O8 2.423(4) 19_556 ? Tb1 O8 2.423(4) 18_556 ? Tb1 O3 2.423(8) 18_556 ? Tb1 O3 2.423(8) . ? Tb1 Tb3 3.9304(10) . ? Tb1 Tb3 3.9304(10) 17_556 ? Tb1 Tb1 3.9697(13) 3 ? Tb1 Tb1 3.9697(13) 19_556 ? Tb2 O2 2.310(8) 22 ? Tb2 O2 2.310(8) . ? Tb2 O7 2.311(5) 3 ? Tb2 O7 2.311(5) . ? Tb2 O1 2.333(10) . ? Tb2 O5 2.460(6) 3 ? Tb2 O5 2.460(6) . ? Tb2 O6 2.554(2) . ? Tb2 Tb2 3.5867(11) 3 ? Tb2 Tb2 3.5867(11) 4 ? Tb2 Tb3 3.7664(11) . ? Tb3 O8 2.406(8) 4 ? Tb3 O8 2.406(8) . ? Tb3 O8 2.406(8) 3 ? Tb3 O8 2.406(8) 2 ? Tb3 O7 2.448(8) 2 ? Tb3 O7 2.448(8) . ? Tb3 O7 2.448(8) 4 ? Tb3 O7 2.448(8) 3 ? Tb3 Tb2 3.7664(11) 2 ? Tb3 Tb2 3.7664(11) 3 ? Tb3 Tb2 3.7664(11) 4 ? O1 C2 1.24(2) 22 ? O1 C2 1.24(2) . ? O2 C6 1.25(2) . ? O2 C4 1.29(3) . ? O3 C8 1.28(2) . ? O3 C8 1.28(2) 24 ? O4 C10 1.31(3) 18_556 ? O4 C10 1.31(3) . ? O5 C14 1.299(17) . ? O5 Tb2 2.460(6) 4 ? O6 Tb2 2.554(2) 4 ? O6 Tb2 2.554(2) 2 ? O6 Tb2 2.554(2) 3 ? O7 Tb2 2.311(5) 4 ? O8 Tb1 2.423(4) 3 ? C1 C2 1.52(3) . ? C1 C2 1.52(3) 22 ? C2 C2 0.75(4) 22 ? C2 C3 1.41(3) 22 ? C2 C3 1.87(3) . ? C3 C4 1.39(3) . ? C3 C2 1.41(3) 22 ? C3 C3 1.99(5) 22 ? C4 C5 1.68(3) . ? C4 C6 1.79(4) . ? C5 C6 1.77(3) . ? C6 C12 1.35(4) 22 ? C7 C7 0.60(7) 24 ? C7 C8 1.42(2) 24 ? C7 C8 1.51(4) . ? C8 C8 0.46(14) 24 ? C8 C9 1.28(4) . ? C8 C7 1.42(2) 24 ? C8 C9 1.55(6) 24 ? C9 C10 1.39(3) . ? C9 C8 1.55(6) 24 ? C9 C9 1.70(6) 24 ? C10 C10 1.17(5) 18_556 ? C10 C11 1.55(3) . ? C11 C10 1.55(3) 18_556 ? C12 C6 1.35(4) 22 ? C12 C14 1.40(3) . ? C12 C12 1.70(6) 24 ? C12 C13 1.72(4) . ? C13 C14 1.60(3) . ? C14 C12 1.40(3) 24 ? C14 C13 1.60(3) 24 ? C15 C15 1.6(3) 27_455 ? C16 C16 1.27(18) 18_556 ? 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 O4 Tb1 O4 89.1(5) . 7_556 ? O4 Tb1 O8 90.4(3) . . ? O4 Tb1 O8 145.01(14) 7_556 . ? O4 Tb1 O8 145.01(14) . 4 ? O4 Tb1 O8 90.4(3) 7_556 4 ? O8 Tb1 O8 70.7(4) . 4 ? O4 Tb1 O8 145.01(14) . 19_556 ? O4 Tb1 O8 90.4(3) 7_556 19_556 ? O8 Tb1 O8 109.1(4) . 19_556 ? O8 Tb1 O8 70.0(3) 4 19_556 ? O4 Tb1 O8 90.4(3) . 18_556 ? O4 Tb1 O8 145.01(14) 7_556 18_556 ? O8 Tb1 O8 70.0(3) . 18_556 ? O8 Tb1 O8 109.1(4) 4 18_556 ? O8 Tb1 O8 70.7(4) 19_556 18_556 ? O4 Tb1 O3 71.10(17) . 18_556 ? O4 Tb1 O3 71.10(17) 7_556 18_556 ? O8 Tb1 O3 140.75(18) . 18_556 ? O8 Tb1 O3 140.75(18) 4 18_556 ? O8 Tb1 O3 75.7(2) 19_556 18_556 ? O8 Tb1 O3 75.7(2) 18_556 18_556 ? O4 Tb1 O3 71.10(17) . . ? O4 Tb1 O3 71.10(17) 7_556 . ? O8 Tb1 O3 75.7(2) . . ? O8 Tb1 O3 75.7(2) 4 . ? O8 Tb1 O3 140.75(18) 19_556 . ? O8 Tb1 O3 140.75(18) 18_556 . ? O3 Tb1 O3 125.9(4) 18_556 . ? O4 Tb1 Tb3 120.58(16) . . ? O4 Tb1 Tb3 120.58(16) 7_556 . ? O8 Tb1 Tb3 35.36(18) . . ? O8 Tb1 Tb3 35.36(18) 4 . ? O8 Tb1 Tb3 89.26(16) 19_556 . ? O8 Tb1 Tb3 89.26(16) 18_556 . ? O3 Tb1 Tb3 161.5(2) 18_556 . ? O3 Tb1 Tb3 72.6(2) . . ? O4 Tb1 Tb3 120.58(16) . 17_556 ? O4 Tb1 Tb3 120.58(16) 7_556 17_556 ? O8 Tb1 Tb3 89.26(16) . 17_556 ? O8 Tb1 Tb3 89.26(16) 4 17_556 ? O8 Tb1 Tb3 35.36(18) 19_556 17_556 ? O8 Tb1 Tb3 35.36(18) 18_556 17_556 ? O3 Tb1 Tb3 72.6(2) 18_556 17_556 ? O3 Tb1 Tb3 161.5(2) . 17_556 ? Tb3 Tb1 Tb3 88.85(3) . 17_556 ? O4 Tb1 Tb1 90.4(3) . 3 ? O4 Tb1 Tb1 179.6(3) 7_556 3 ? O8 Tb1 Tb1 34.98(14) . 3 ? O8 Tb1 Tb1 89.95(19) 4 3 ? O8 Tb1 Tb1 89.95(19) 19_556 3 ? O8 Tb1 Tb1 34.98(14) 18_556 3 ? O3 Tb1 Tb1 108.76(14) 18_556 3 ? O3 Tb1 Tb1 108.76(14) . 3 ? Tb3 Tb1 Tb1 59.668(9) . 3 ? Tb3 Tb1 Tb1 59.668(9) 17_556 3 ? O4 Tb1 Tb1 179.6(3) . 19_556 ? O4 Tb1 Tb1 90.4(3) 7_556 19_556 ? O8 Tb1 Tb1 89.95(19) . 19_556 ? O8 Tb1 Tb1 34.98(14) 4 19_556 ? O8 Tb1 Tb1 34.98(14) 19_556 19_556 ? O8 Tb1 Tb1 89.95(19) 18_556 19_556 ? O3 Tb1 Tb1 108.76(14) 18_556 19_556 ? O3 Tb1 Tb1 108.76(14) . 19_556 ? Tb3 Tb1 Tb1 59.668(9) . 19_556 ? Tb3 Tb1 Tb1 59.668(9) 17_556 19_556 ? Tb1 Tb1 Tb1 90.0 3 19_556 ? O2 Tb2 O2 75.9(4) 22 . ? O2 Tb2 O7 155.6(3) 22 3 ? O2 Tb2 O7 98.1(3) . 3 ? O2 Tb2 O7 98.1(3) 22 . ? O2 Tb2 O7 155.6(3) . . ? O7 Tb2 O7 77.4(4) 3 . ? O2 Tb2 O1 76.4(3) 22 . ? O2 Tb2 O1 76.4(3) . . ? O7 Tb2 O1 79.2(2) 3 . ? O7 Tb2 O1 79.2(2) . . ? O2 Tb2 O5 119.3(3) 22 3 ? O2 Tb2 O5 70.3(3) . 3 ? O7 Tb2 O5 79.2(2) 3 3 ? O7 Tb2 O5 130.8(3) . 3 ? O1 Tb2 O5 136.8(3) . 3 ? O2 Tb2 O5 70.3(3) 22 . ? O2 Tb2 O5 119.3(3) . . ? O7 Tb2 O5 130.8(3) 3 . ? O7 Tb2 O5 79.2(2) . . ? O1 Tb2 O5 136.8(3) . . ? O5 Tb2 O5 84.6(5) 3 . ? O2 Tb2 O6 134.1(3) 22 . ? O2 Tb2 O6 134.1(3) . . ? O7 Tb2 O6 66.6(3) 3 . ? O7 Tb2 O6 66.6(3) . . ? O1 Tb2 O6 135.5(4) . . ? O5 Tb2 O6 64.5(3) 3 . ? O5 Tb2 O6 64.5(3) . . ? O2 Tb2 Tb2 162.5(2) 22 3 ? O2 Tb2 Tb2 94.8(2) . 3 ? O7 Tb2 Tb2 39.10(15) 3 3 ? O7 Tb2 Tb2 96.2(2) . 3 ? O1 Tb2 Tb2 116.32(15) . 3 ? O5 Tb2 Tb2 43.19(15) 3 3 ? O5 Tb2 Tb2 102.9(2) . 3 ? O6 Tb2 Tb2 45.39(4) . 3 ? O2 Tb2 Tb2 94.8(2) 22 4 ? O2 Tb2 Tb2 162.5(2) . 4 ? O7 Tb2 Tb2 96.2(2) 3 4 ? O7 Tb2 Tb2 39.10(15) . 4 ? O1 Tb2 Tb2 116.32(15) . 4 ? O5 Tb2 Tb2 102.9(2) 3 4 ? O5 Tb2 Tb2 43.19(15) . 4 ? O6 Tb2 Tb2 45.39(4) . 4 ? Tb2 Tb2 Tb2 90.0 3 4 ? O2 Tb2 Tb3 135.1(2) 22 . ? O2 Tb2 Tb3 135.1(2) . . ? O7 Tb2 Tb3 39.0(2) 3 . ? O7 Tb2 Tb3 39.0(2) . . ? O1 Tb2 Tb3 81.2(2) . . ? O5 Tb2 Tb3 103.73(15) 3 . ? O5 Tb2 Tb3 103.73(15) . . ? O6 Tb2 Tb3 54.4(3) . . ? Tb2 Tb2 Tb3 61.566(9) 3 . ? Tb2 Tb2 Tb3 61.566(9) 4 . ? O8 Tb3 O8 71.30(18) 4 . ? O8 Tb3 O8 111.0(4) 4 3 ? O8 Tb3 O8 71.30(18) . 3 ? O8 Tb3 O8 71.30(18) 4 2 ? O8 Tb3 O8 111.0(4) . 2 ? O8 Tb3 O8 71.30(18) 3 2 ? O8 Tb3 O7 142.97(6) 4 2 ? O8 Tb3 O7 142.97(6) . 2 ? O8 Tb3 O7 79.9(2) 3 2 ? O8 Tb3 O7 79.9(2) 2 2 ? O8 Tb3 O7 79.9(2) 4 . ? O8 Tb3 O7 79.9(2) . . ? O8 Tb3 O7 142.97(6) 3 . ? O8 Tb3 O7 142.97(6) 2 . ? O7 Tb3 O7 113.1(4) 2 . ? O8 Tb3 O7 79.9(2) 4 4 ? O8 Tb3 O7 142.97(6) . 4 ? O8 Tb3 O7 142.97(6) 3 4 ? O8 Tb3 O7 79.9(2) 2 4 ? O7 Tb3 O7 72.33(18) 2 4 ? O7 Tb3 O7 72.33(18) . 4 ? O8 Tb3 O7 142.97(6) 4 3 ? O8 Tb3 O7 79.9(2) . 3 ? O8 Tb3 O7 79.9(2) 3 3 ? O8 Tb3 O7 142.97(6) 2 3 ? O7 Tb3 O7 72.33(18) 2 3 ? O7 Tb3 O7 72.33(18) . 3 ? O7 Tb3 O7 113.1(4) 4 3 ? O8 Tb3 Tb2 114.75(12) 4 2 ? O8 Tb3 Tb2 166.81(18) . 2 ? O8 Tb3 Tb2 114.75(12) 3 2 ? O8 Tb3 Tb2 82.16(18) 2 2 ? O7 Tb3 Tb2 36.42(11) 2 2 ? O7 Tb3 Tb2 89.43(17) . 2 ? O7 Tb3 Tb2 36.42(11) 4 2 ? O7 Tb3 Tb2 89.43(17) 3 2 ? O8 Tb3 Tb2 166.81(18) 4 3 ? O8 Tb3 Tb2 114.75(12) . 3 ? O8 Tb3 Tb2 82.16(18) 3 3 ? O8 Tb3 Tb2 114.75(12) 2 3 ? O7 Tb3 Tb2 36.42(11) 2 3 ? O7 Tb3 Tb2 89.43(17) . 3 ? O7 Tb3 Tb2 89.43(17) 4 3 ? O7 Tb3 Tb2 36.42(11) 3 3 ? Tb2 Tb3 Tb2 56.868(19) 2 3 ? O8 Tb3 Tb2 114.75(12) 4 . ? O8 Tb3 Tb2 82.16(18) . . ? O8 Tb3 Tb2 114.75(12) 3 . ? O8 Tb3 Tb2 166.81(18) 2 . ? O7 Tb3 Tb2 89.43(17) 2 . ? O7 Tb3 Tb2 36.42(11) . . ? O7 Tb3 Tb2 89.43(17) 4 . ? O7 Tb3 Tb2 36.42(11) 3 . ? Tb2 Tb3 Tb2 84.66(3) 2 . ? Tb2 Tb3 Tb2 56.868(19) 3 . ? O8 Tb3 Tb2 82.16(18) 4 4 ? O8 Tb3 Tb2 114.75(12) . 4 ? O8 Tb3 Tb2 166.81(18) 3 4 ? O8 Tb3 Tb2 114.75(12) 2 4 ? O7 Tb3 Tb2 89.43(17) 2 4 ? O7 Tb3 Tb2 36.42(11) . 4 ? O7 Tb3 Tb2 36.42(11) 4 4 ? O7 Tb3 Tb2 89.43(17) 3 4 ? Tb2 Tb3 Tb2 56.868(19) 2 4 ? Tb2 Tb3 Tb2 84.66(3) 3 4 ? Tb2 Tb3 Tb2 56.868(19) . 4 ? C2 O1 C2 34.9(19) 22 . ? C2 O1 Tb2 128.4(12) 22 . ? C2 O1 Tb2 128.4(12) . . ? C6 O2 C4 89.6(17) . . ? C6 O2 Tb2 136.0(14) . . ? C4 O2 Tb2 130.9(12) . . ? C8 O3 C8 21(6) . 24 ? C8 O3 Tb1 130.9(10) . . ? C8 O3 Tb1 130.9(10) 24 . ? C10 O4 C10 53(2) 18_556 . ? C10 O4 Tb1 127.0(12) 18_556 . ? C10 O4 Tb1 127.0(12) . . ? C14 O5 Tb2 128.6(4) . . ? C14 O5 Tb2 128.6(4) . 4 ? Tb2 O5 Tb2 93.6(3) . 4 ? Tb2 O6 Tb2 89.22(8) . 4 ? Tb2 O6 Tb2 166.6(7) . 2 ? Tb2 O6 Tb2 89.22(8) 4 2 ? Tb2 O6 Tb2 89.22(8) . 3 ? Tb2 O6 Tb2 166.6(7) 4 3 ? Tb2 O6 Tb2 89.22(8) 2 3 ? Tb2 O7 Tb2 101.8(3) . 4 ? Tb2 O7 Tb3 104.6(3) . . ? Tb2 O7 Tb3 104.6(3) 4 . ? Tb3 O8 Tb1 109.0(2) . 3 ? Tb3 O8 Tb1 109.0(2) . . ? Tb1 O8 Tb1 110.0(3) 3 . ? C2 C1 C2 28.4(15) . 22 ? C2 C2 O1 72.5(10) 22 . ? C2 C2 C3 116.1(13) 22 22 ? O1 C2 C3 132(2) . 22 ? C2 C2 C1 75.8(8) 22 . ? O1 C2 C1 113.6(18) . . ? C3 C2 C1 114(2) 22 . ? C2 C2 C3 42.9(10) 22 . ? O1 C2 C3 100.9(15) . . ? C3 C2 C3 73(2) 22 . ? C1 C2 C3 92.8(14) . . ? C4 C3 C2 120(2) . 22 ? C4 C3 C2 122(2) . . ? C2 C3 C2 21.0(12) 22 . ? C4 C3 C3 112.1(16) . 22 ? C2 C3 C3 63.9(13) 22 22 ? C2 C3 C3 42.9(10) . 22 ? O2 C4 C3 127(2) . . ? O2 C4 C5 105.5(19) . . ? C3 C4 C5 127(3) . . ? O2 C4 C6 44.3(12) . . ? C3 C4 C6 171(3) . . ? C5 C4 C6 61.2(14) . . ? C4 C5 C6 62.6(15) . . ? O2 C6 C12 126(2) . 22 ? O2 C6 C5 102(2) . . ? C12 C6 C5 131(2) 22 . ? O2 C6 C4 46.1(14) . . ? C12 C6 C4 171(2) 22 . ? C5 C6 C4 56.2(15) . . ? C7 C7 C8 87(3) 24 24 ? C7 C7 C8 70(3) 24 . ? C8 C7 C8 18(5) 24 . ? C8 C8 C9 119(3) 24 . ? C8 C8 O3 80(3) 24 . ? C9 C8 O3 124(2) . . ? C8 C8 C7 93(3) 24 24 ? C9 C8 C7 110(3) . 24 ? O3 C8 C7 121.7(18) . 24 ? C8 C8 C7 70(3) 24 . ? C9 C8 C7 121.2(19) . . ? O3 C8 C7 115(3) . . ? C7 C8 C7 23(3) 24 . ? C8 C8 C9 46(2) 24 24 ? C9 C8 C9 73(2) . 24 ? O3 C8 C9 105(4) . 24 ? C7 C8 C9 110(3) 24 24 ? C7 C8 C9 93(3) . 24 ? C8 C9 C10 127(2) . . ? C8 C9 C8 15(5) . 24 ? C10 C9 C8 130.8(19) . 24 ? C8 C9 C9 61(3) . 24 ? C10 C9 C9 122.2(14) . 24 ? C8 C9 C9 46(2) 24 24 ? C10 C10 O4 63.5(10) 18_556 . ? C10 C10 C9 145.1(15) 18_556 . ? O4 C10 C9 125.5(19) . . ? C10 C10 C11 67.9(9) 18_556 . ? O4 C10 C11 114(2) . . ? C9 C10 C11 120(2) . . ? C10 C11 C10 44.2(18) 18_556 . ? C6 C12 C14 121.7(19) 22 . ? C6 C12 C12 132.7(17) 22 24 ? C14 C12 C12 52.8(13) . 24 ? C6 C12 C13 113(2) 22 . ? C14 C12 C13 60.4(16) . . ? C12 C12 C13 102.5(15) 24 . ? C14 C13 C12 49.8(15) . . ? O5 C14 C12 127.4(14) . . ? O5 C14 C12 127.4(14) . 24 ? C12 C14 C12 74(3) . 24 ? O5 C14 C13 107.0(14) . . ? C12 C14 C13 69.8(16) . . ? C12 C14 C13 125.5(18) 24 . ? O5 C14 C13 107.0(14) . 24 ? C12 C14 C13 125.5(18) . 24 ? C12 C14 C13 69.8(16) 24 24 ? C13 C14 C13 100(2) . 24 ? _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 4.844 _refine_diff_density_min -1.656 _refine_diff_density_rms 0.202