# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2001 # CCDC Number: 186/2271 data_cs034 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34.67 H25.33 N1.33 O8 Tb1.33' _chemical_formula_weight 800.46 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 ? _symmetry_space_group_name_H-M ? 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 16.2103(14) _cell_length_b 17.7707(16) _cell_length_c 17.6211(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.247(2) _cell_angle_gamma 90.00 _cell_volume 4820.8(7) _cell_formula_units_Z 6 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.654 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2360 _exptl_absorpt_coefficient_mu 2.975 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12319 _diffrn_reflns_av_R_equivalents 0.1003 _diffrn_reflns_av_sigmaI/netI 0.0955 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 23.31 _reflns_number_total 3485 _reflns_number_gt 2147 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0190P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3485 _refine_ls_number_parameters 310 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0677 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0763 _refine_ls_wR_factor_gt 0.0708 _refine_ls_goodness_of_fit_ref 0.812 _refine_ls_restrained_S_all 0.812 _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 Tb Tb -0.03780(2) -0.04840(2) 0.345281(18) 0.05031(14) Uani 1 1 d . . . N1 N -0.1279(5) -0.1353(4) 0.4101(3) 0.071(2) Uani 1 1 d . . . O1 O -0.0257(3) -0.1687(3) 0.3019(3) 0.0676(16) Uani 1 1 d . . . C1 C 0.0000 -0.2022(6) 0.2500 0.061(3) Uani 1 2 d S . . O2 O -0.1820(3) -0.0401(3) 0.2568(3) 0.0812(17) Uani 1 1 d . . . C2 C 0.0000 -0.2837(8) 0.2500 0.101(5) Uani 1 2 d S . . O3 O -0.0920(3) -0.0442(3) 0.1879(3) 0.0611(13) Uani 1 1 d . . . C3 C -0.0044(10) -0.3219(7) 0.3134(8) 0.170(6) Uani 1 1 d . . . H3 H -0.0110 -0.2963 0.3572 0.205 Uiso 1 1 calc R . . O4 O -0.0940(3) 0.0254(3) 0.4230(3) 0.0659(16) Uani 1 1 d . . . C4 C 0.001(3) -0.3998(11) 0.3145(19) 0.37(2) Uani 1 1 d . . . H4 H 0.0053 -0.4265 0.3610 0.443 Uiso 1 1 calc R . . O5 O 0.0589(3) -0.0829(3) 0.4617(3) 0.0659(15) Uani 1 1 d . . . C5 C 0.0000 -0.4350(19) 0.2500 0.45(5) Uani 1 2 d S . . H5 H 0.0000 -0.4873 0.2500 0.540 Uiso 1 2 calc SR . . O6 O -0.0208(3) 0.0742(3) 0.3048(3) 0.0644(16) Uani 1 1 d . . . C6 C -0.1664(6) -0.0324(4) 0.1926(4) 0.060(2) Uani 1 1 d . . . C7 C -0.2376(6) -0.0077(6) 0.1207(5) 0.077(3) Uani 1 1 d . . . C8 C -0.3091(11) 0.0106(18) 0.1307(9) 0.41(2) Uani 1 1 d . . . H8 H -0.3155 0.0053 0.1811 0.496 Uiso 1 1 calc R . . C9 C -0.3817(18) 0.040(2) 0.0653(14) 0.58(4) Uani 1 1 d . . . H9 H -0.4316 0.0558 0.0757 0.696 Uiso 1 1 calc R . . C10 C -0.3778(11) 0.0438(15) -0.0125(12) 0.289(14) Uani 1 1 d . . . H10 H -0.4229 0.0621 -0.0553 0.347 Uiso 1 1 calc R . . C11 C -0.3063(10) 0.0199(7) -0.0188(6) 0.141(5) Uani 1 1 d . . . H11 H -0.2994 0.0188 -0.0692 0.169 Uiso 1 1 calc R . . C12 C -0.2357(7) -0.0053(7) 0.0483(6) 0.133(5) Uani 1 1 d . . . H12 H -0.1851 -0.0210 0.0387 0.159 Uiso 1 1 calc R . . C13 C -0.0993(5) 0.0802(5) 0.4649(4) 0.053(2) Uani 1 1 d . . . C14 C -0.1545(5) 0.1448(5) 0.4279(5) 0.064(2) Uani 1 1 d . . . C15 C -0.2118(6) 0.1387(6) 0.3527(6) 0.096(3) Uani 1 1 d . . . H15 H -0.2169 0.0941 0.3239 0.116 Uiso 1 1 calc R . . C16 C -0.2622(9) 0.2011(10) 0.3203(7) 0.145(6) Uani 1 1 d . . . H16 H -0.3029 0.1980 0.2697 0.174 Uiso 1 1 calc R . . C17 C -0.2528(11) 0.2639(9) 0.3603(10) 0.167(8) Uani 1 1 d . . . H17 H -0.2873 0.3046 0.3366 0.200 Uiso 1 1 calc R . . C18 C -0.1963(10) 0.2730(8) 0.4333(8) 0.145(6) Uani 1 1 d . . . H18 H -0.1908 0.3188 0.4600 0.174 Uiso 1 1 calc R . . C19 C -0.1465(7) 0.2116(6) 0.4674(6) 0.101(3) Uani 1 1 d . . . H19 H -0.1066 0.2159 0.5183 0.121 Uiso 1 1 calc R . . C20 C -0.1915(8) -0.1754(6) 0.3689(5) 0.130(5) Uani 1 1 d . . . H20 H -0.2046 -0.1745 0.3136 0.156 Uiso 1 1 calc R . . C21 C -0.2425(8) -0.2203(6) 0.4008(5) 0.150(6) Uani 1 1 d . . . H21 H -0.2898 -0.2462 0.3673 0.180 Uiso 1 1 calc R . . C22 C -0.2227(6) -0.2261(5) 0.4819(4) 0.070(2) Uani 1 1 d . . . C23 C -0.1573(6) -0.1831(5) 0.5236(5) 0.088(3) Uani 1 1 d . . . H23 H -0.1426 -0.1824 0.5791 0.106 Uiso 1 1 calc R . . C24 C -0.1112(6) -0.1401(6) 0.4873(4) 0.096(3) Uani 1 1 d . . . H24 H -0.0649 -0.1123 0.5196 0.115 Uiso 1 1 calc R . . C25 C 0.0000 0.1059(7) 0.2500 0.059(3) Uani 1 2 d S . . C26 C 0.0000 0.1910(6) 0.2500 0.061(3) Uani 1 2 d S . . C27 C -0.0349(7) 0.2302(6) 0.2981(5) 0.095(3) Uani 1 1 d . . . H27 H -0.0587 0.2043 0.3321 0.114 Uiso 1 1 calc R . . C28 C -0.0360(9) 0.3079(6) 0.2979(7) 0.139(5) Uani 1 1 d . . . H28 H -0.0615 0.3336 0.3307 0.166 Uiso 1 1 calc R . . C29 C 0.0000 0.3468(10) 0.2500 0.163(8) Uani 1 2 d S . . H29 H 0.0000 0.3991 0.2500 0.195 Uiso 1 2 calc SR . . 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 Tb 0.0602(3) 0.0571(2) 0.03751(18) 0.0009(2) 0.02083(16) -0.0038(3) N1 0.092(6) 0.084(6) 0.046(4) -0.004(4) 0.032(4) -0.028(5) O1 0.088(4) 0.062(4) 0.061(3) 0.000(3) 0.035(3) -0.012(3) C1 0.079(9) 0.039(8) 0.063(7) 0.000 0.020(7) 0.000 O2 0.064(4) 0.136(5) 0.047(3) 0.002(3) 0.021(3) -0.016(4) C2 0.151(15) 0.039(10) 0.113(12) 0.000 0.043(11) 0.000 O3 0.055(3) 0.075(4) 0.056(3) -0.001(3) 0.021(3) 0.005(3) C3 0.292(19) 0.057(9) 0.163(12) 0.038(8) 0.074(13) -0.005(10) O4 0.080(4) 0.069(4) 0.054(3) 0.001(3) 0.028(3) 0.012(3) C4 0.74(6) 0.10(2) 0.31(4) 0.07(2) 0.23(4) 0.02(4) O5 0.061(4) 0.096(4) 0.038(3) 0.003(3) 0.012(3) 0.004(3) C5 0.88(11) 0.03(2) 0.47(11) 0.000 0.26(10) 0.000 O6 0.094(4) 0.052(4) 0.058(3) -0.002(3) 0.040(3) 0.002(3) C6 0.073(6) 0.063(6) 0.044(4) -0.001(4) 0.020(4) -0.010(5) C7 0.042(5) 0.138(8) 0.050(5) 0.000(5) 0.013(5) -0.005(5) C8 0.119(13) 1.01(7) 0.080(10) 0.06(2) -0.006(10) 0.20(2) C9 0.31(3) 1.29(11) 0.145(19) 0.07(3) 0.08(2) 0.44(5) C10 0.120(13) 0.58(4) 0.168(17) 0.02(2) 0.047(13) 0.129(19) C11 0.150(12) 0.192(14) 0.071(7) 0.036(8) 0.021(9) 0.019(10) C12 0.115(9) 0.214(13) 0.074(7) 0.016(8) 0.038(7) 0.056(9) C13 0.045(5) 0.072(6) 0.048(5) -0.001(4) 0.022(4) 0.001(4) C14 0.069(6) 0.072(7) 0.053(5) 0.008(5) 0.025(5) 0.017(5) C15 0.093(8) 0.119(9) 0.074(6) 0.024(6) 0.022(6) 0.035(7) C16 0.130(11) 0.206(17) 0.093(9) 0.049(10) 0.025(8) 0.092(12) C17 0.224(19) 0.144(15) 0.156(14) 0.061(13) 0.094(15) 0.118(14) C18 0.216(17) 0.118(11) 0.115(10) 0.023(10) 0.071(11) 0.081(11) C19 0.138(10) 0.083(8) 0.092(7) 0.009(7) 0.052(7) 0.049(7) C20 0.184(12) 0.166(12) 0.046(5) -0.026(6) 0.047(7) -0.116(10) C21 0.223(14) 0.183(12) 0.054(6) -0.029(7) 0.057(8) -0.145(11) C22 0.090(7) 0.075(7) 0.054(5) -0.001(4) 0.035(5) -0.027(5) C23 0.084(7) 0.134(9) 0.046(5) 0.006(5) 0.020(5) -0.037(6) C24 0.084(7) 0.156(10) 0.052(5) 0.002(6) 0.027(5) -0.044(7) C25 0.065(9) 0.070(9) 0.046(6) 0.000 0.022(6) 0.000 C26 0.084(9) 0.041(8) 0.062(7) 0.000 0.030(7) 0.000 C27 0.142(10) 0.070(8) 0.095(7) -0.002(6) 0.068(7) 0.010(7) C28 0.237(15) 0.064(9) 0.145(11) -0.026(8) 0.103(10) 0.023(9) C29 0.28(3) 0.058(13) 0.189(19) 0.000 0.134(19) 0.000 _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 Tb O5 2.242(5) . ? Tb O4 2.281(5) . ? Tb O1 2.299(5) . ? Tb O6 2.336(5) . ? Tb O3 2.354(5) 2 ? Tb O2 2.374(5) . ? Tb N1 2.621(6) . ? Tb O3 2.635(4) . ? Tb C6 2.855(8) . ? Tb Tb 3.9184(6) 2 ? N1 C20 1.277(10) . ? N1 C24 1.303(8) . ? O1 C1 1.266(6) . ? C1 O1 1.266(6) 2 ? C1 C2 1.448(15) . ? O2 C6 1.243(8) . ? C2 C3 1.328(12) 2 ? C2 C3 1.328(12) . ? O3 C6 1.252(8) . ? O3 Tb 2.354(5) 2 ? C3 C4 1.39(2) . ? O4 C13 1.242(8) . ? C4 C5 1.29(2) . ? O5 C13 1.254(8) 5_556 ? C5 C4 1.29(2) 2 ? O6 C25 1.251(7) . ? C6 C7 1.488(10) . ? C7 C8 1.267(16) . ? C7 C12 1.288(11) . ? C8 C9 1.46(2) . ? C9 C10 1.39(2) . ? C10 C11 1.271(17) . ? C11 C12 1.435(13) . ? C13 O5 1.254(8) 5_556 ? C13 C14 1.477(10) . ? C14 C19 1.362(12) . ? C14 C15 1.363(10) . ? C15 C16 1.389(14) . ? C16 C17 1.303(18) . ? C17 C18 1.335(18) . ? C18 C19 1.379(13) . ? C20 C21 1.390(11) . ? C21 C22 1.367(10) . ? C22 C23 1.327(10) . ? C22 C22 1.504(14) 7_446 ? C23 C24 1.362(10) . ? C25 O6 1.251(7) 2 ? C25 C26 1.514(14) . ? C26 C27 1.350(9) . ? C26 C27 1.350(9) 2 ? C27 C28 1.380(12) . ? C28 C29 1.356(13) . ? C29 C28 1.356(13) 2 ? 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 O5 Tb O4 84.51(17) . . ? O5 Tb O1 86.69(18) . . ? O4 Tb O1 145.66(17) . . ? O5 Tb O6 114.77(18) . . ? O4 Tb O6 75.82(16) . . ? O1 Tb O6 137.29(15) . . ? O5 Tb O3 79.20(16) . 2 ? O4 Tb O3 133.35(18) . 2 ? O1 Tb O3 76.76(18) . 2 ? O6 Tb O3 72.19(18) . 2 ? O5 Tb O2 151.67(17) . . ? O4 Tb O2 82.07(18) . . ? O1 Tb O2 90.46(19) . . ? O6 Tb O2 85.87(19) . . ? O3 Tb O2 127.45(15) 2 . ? O5 Tb N1 76.4(2) . . ? O4 Tb N1 72.27(19) . . ? O1 Tb N1 73.41(18) . . ? O6 Tb N1 144.9(2) . . ? O3 Tb N1 142.2(2) 2 . ? O2 Tb N1 75.8(2) . . ? O5 Tb O3 151.38(16) . . ? O4 Tb O3 123.45(17) . . ? O1 Tb O3 73.21(16) . . ? O6 Tb O3 71.59(16) . . ? O3 Tb O3 76.53(17) 2 . ? O2 Tb O3 51.11(15) . . ? N1 Tb O3 115.35(18) . . ? O5 Tb C6 169.8(2) . . ? O4 Tb C6 101.4(2) . . ? O1 Tb C6 83.8(2) . . ? O6 Tb C6 75.0(2) . . ? O3 Tb C6 102.0(2) 2 . ? O2 Tb C6 25.43(19) . . ? N1 Tb C6 97.3(2) . . ? O3 Tb C6 25.97(16) . . ? O5 Tb Tb 117.87(12) . 2 ? O4 Tb Tb 143.61(12) . 2 ? O1 Tb Tb 68.45(11) . 2 ? O6 Tb Tb 68.86(11) . 2 ? O3 Tb Tb 40.87(11) 2 2 ? O2 Tb Tb 86.87(11) . 2 ? N1 Tb Tb 137.74(14) . 2 ? O3 Tb Tb 35.76(11) . 2 ? C6 Tb Tb 61.59(17) . 2 ? C20 N1 C24 115.1(7) . . ? C20 N1 Tb 122.8(5) . . ? C24 N1 Tb 122.1(6) . . ? C1 O1 Tb 139.4(6) . . ? O1 C1 O1 123.8(10) . 2 ? O1 C1 C2 118.1(5) . . ? O1 C1 C2 118.1(5) 2 . ? C6 O2 Tb 99.5(5) . . ? C3 C2 C3 118.6(16) 2 . ? C3 C2 C1 120.7(8) 2 . ? C3 C2 C1 120.7(8) . . ? C6 O3 Tb 167.4(5) . 2 ? C6 O3 Tb 86.9(4) . . ? Tb O3 Tb 103.36(17) 2 . ? C2 C3 C4 120.1(18) . . ? C13 O4 Tb 157.4(5) . . ? C5 C4 C3 119(3) . . ? C13 O5 Tb 157.3(5) 5_556 . ? C4 C5 C4 122(4) . 2 ? C25 O6 Tb 137.9(6) . . ? O2 C6 O3 121.2(7) . . ? O2 C6 C7 118.8(8) . . ? O3 C6 C7 120.0(6) . . ? O2 C6 Tb 55.1(4) . . ? O3 C6 Tb 67.2(4) . . ? C7 C6 Tb 166.9(6) . . ? C8 C7 C12 115.9(11) . . ? C8 C7 C6 117.2(10) . . ? C12 C7 C6 126.8(9) . . ? C7 C8 C9 121.7(16) . . ? C10 C9 C8 121.5(19) . . ? C11 C10 C9 113.0(18) . . ? C10 C11 C12 123.1(14) . . ? C7 C12 C11 124.5(11) . . ? O4 C13 O5 122.2(8) . 5_556 ? O4 C13 C14 119.5(7) . . ? O5 C13 C14 118.3(7) 5_556 . ? C19 C14 C15 119.6(9) . . ? C19 C14 C13 120.3(8) . . ? C15 C14 C13 120.1(9) . . ? C14 C15 C16 118.0(11) . . ? C17 C16 C15 120.4(14) . . ? C16 C17 C18 123.7(15) . . ? C17 C18 C19 117.1(14) . . ? C14 C19 C18 121.2(11) . . ? N1 C20 C21 124.5(8) . . ? C22 C21 C20 119.5(9) . . ? C23 C22 C21 114.9(7) . . ? C23 C22 C22 124.4(9) . 7_446 ? C21 C22 C22 120.6(10) . 7_446 ? C22 C23 C24 121.6(7) . . ? N1 C24 C23 124.2(8) . . ? O6 C25 O6 126.5(11) 2 . ? O6 C25 C26 116.7(6) 2 . ? O6 C25 C26 116.7(6) . . ? C27 C26 C27 117.9(12) . 2 ? C27 C26 C25 121.1(6) . . ? C27 C26 C25 121.1(6) 2 . ? C26 C27 C28 121.5(10) . . ? C29 C28 C27 120.2(12) . . ? C28 C29 C28 118.7(17) 2 . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.31 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.165 _refine_diff_density_min -0.478 _refine_diff_density_rms 0.089 data_cs040a _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C23 H25 O9 Tb' _chemical_formula_weight 604.35 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 Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8547(16) _cell_length_b 9.8709(16) _cell_length_c 14.718(3) _cell_angle_alpha 92.620(3) _cell_angle_beta 95.352(3) _cell_angle_gamma 113.621(3) _cell_volume 1168.6(4) _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 needle _exptl_crystal_colour colourless _exptl_crystal_size_max .1 _exptl_crystal_size_mid .1 _exptl_crystal_size_min .6 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.718 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 3.076 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _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 8470 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0685 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -4 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 28.35 _reflns_number_total 5395 _reflns_number_gt 4351 _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^)+(0.0060P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5395 _refine_ls_number_parameters 314 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0385 _refine_ls_R_factor_gt 0.0275 _refine_ls_wR_factor_ref 0.0501 _refine_ls_wR_factor_gt 0.0482 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.869 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.52999(2) 0.756719(16) 0.489569(12) 0.02814(5) Uani 1 1 d . . . O1 O 0.3739(3) 0.5330(2) 0.40971(18) 0.0421(6) Uani 1 1 d . . . C1 C 0.1671(4) 0.3844(3) 0.2919(2) 0.0327(8) Uani 1 1 d . . . O2 O 0.2820(3) 0.2900(2) 0.40991(17) 0.0406(6) Uani 1 1 d . . . C2 C 0.1854(5) 0.5047(4) 0.2410(3) 0.0509(11) Uani 1 1 d . . . H2 H 0.2696 0.5976 0.2598 0.061 Uiso 1 1 calc R . . O3 O 0.5334(3) 0.9272(2) 0.60090(16) 0.0374(6) Uani 1 1 d . . . C3 C 0.0787(7) 0.4852(6) 0.1632(3) 0.0762(15) Uani 1 1 d . . . H3 H 0.0918 0.5653 0.1290 0.091 Uiso 1 1 calc R . . O4 O 0.5164(3) 0.8780(2) 0.35864(17) 0.0418(6) Uani 1 1 d . . . C4 C -0.0461(7) 0.3504(6) 0.1352(3) 0.0803(16) Uani 1 1 d . . . H4 H -0.1180 0.3392 0.0824 0.096 Uiso 1 1 calc R . . O5 O 0.7015(3) 0.7060(2) 0.38693(17) 0.0369(6) Uani 1 1 d . . . C5 C -0.0665(6) 0.2308(5) 0.1843(3) 0.0659(13) Uani 1 1 d . . . H5 H -0.1520 0.1387 0.1649 0.079 Uiso 1 1 calc R . . O6 O 0.9080(3) 0.9144(3) 0.36032(18) 0.0467(7) Uani 1 1 d . . . C6 C 0.0405(5) 0.2475(4) 0.2631(3) 0.0478(10) Uani 1 1 d . . . H6 H 0.0270 0.1666 0.2965 0.057 Uiso 1 1 calc R . . C7 C 0.2825(4) 0.4049(3) 0.3761(2) 0.0288(7) Uani 1 1 d . . . O7 O 0.2583(3) 0.7664(3) 0.4739(2) 0.0454(8) Uani 1 1 d . . . H7A H 0.256(5) 0.835(4) 0.484(3) 0.061(15) Uiso 1 1 d . . . O8 O 0.3629(3) 0.5995(3) 0.60076(19) 0.0459(8) Uani 1 1 d . . . H8A H 0.359(5) 0.529(4) 0.607(3) 0.054(14) Uiso 1 1 d . . . C8 C 0.5840(4) 1.0115(3) 0.7571(2) 0.0345(8) Uani 1 1 d . . . O9 O 0.7952(4) 0.9809(3) 0.5054(2) 0.0366(6) Uani 1 1 d . . . H9A H 0.845(4) 0.978(4) 0.469(2) 0.025(12) Uiso 1 1 d . . . H9B H 0.855(5) 0.977(4) 0.554(3) 0.053(14) Uiso 1 1 d . . . C9 C 0.6522(5) 0.9114(4) 0.7804(3) 0.0467(10) Uani 1 1 d . . . H9C H 0.6630 0.8488 0.7347 0.056 Uiso 1 1 calc R . . C10 C 0.7038(6) 0.9038(5) 0.8698(3) 0.0660(13) Uani 1 1 d . . . H10 H 0.7499 0.8367 0.8846 0.079 Uiso 1 1 calc R . . C11 C 0.6878(6) 0.9934(6) 0.9366(3) 0.0757(15) Uani 1 1 d . . . H11 H 0.7214 0.9863 0.9974 0.091 Uiso 1 1 calc R . . C12 C 0.6229(6) 1.0943(5) 0.9166(3) 0.0692(13) Uani 1 1 d . . . H12 H 0.6144 1.1564 0.9634 0.083 Uiso 1 1 calc R . . C13 C 0.5698(5) 1.1045(4) 0.8264(3) 0.0499(10) Uani 1 1 d . . . H13 H 0.5252 1.1729 0.8125 0.060 Uiso 1 1 calc R . . C14 C 0.5308(4) 1.0209(3) 0.6601(2) 0.0304(8) Uani 1 1 d . . . C15 C 0.7798(5) 0.7293(4) 0.2374(3) 0.0388(9) Uani 1 1 d . . . C16 C 0.8959(6) 0.8028(5) 0.1808(3) 0.0546(11) Uani 1 1 d . . . H16 H 0.9860 0.8902 0.2035 0.066 Uiso 1 1 calc R . . C17 C 0.8807(6) 0.7490(6) 0.0914(3) 0.0699(14) Uani 1 1 d . . . H17 H 0.9601 0.7998 0.0539 0.084 Uiso 1 1 calc R . . C18 C 0.7503(7) 0.6219(6) 0.0578(3) 0.0715(14) Uani 1 1 d . . . H18 H 0.7404 0.5844 -0.0026 0.086 Uiso 1 1 calc R . . C19 C 0.6323(6) 0.5484(5) 0.1132(3) 0.0708(14) Uani 1 1 d . . . H19 H 0.5419 0.4616 0.0898 0.085 Uiso 1 1 calc R . . C20 C 0.6468(5) 0.6018(4) 0.2020(3) 0.0497(10) Uani 1 1 d . . . H20 H 0.5661 0.5515 0.2389 0.060 Uiso 1 1 calc R . . C21 C 0.7982(5) 0.7882(4) 0.3349(3) 0.0356(8) Uani 1 1 d . . . C22 C 0.0992(5) 0.6721(4) 0.4354(3) 0.0695(15) Uani 1 1 d . . . H22 H 0.0818 0.6925 0.3731 0.104 Uiso 1 1 calc R . . H22A H 0.0195 0.6875 0.4696 0.104 Uiso 1 1 calc R . . H22B H 0.0864 0.5709 0.4368 0.104 Uiso 1 1 calc R . . C23 C 0.2675(5) 0.6323(4) 0.6636(3) 0.0547(11) Uani 1 1 d . . . H23 H 0.3381 0.6833 0.7189 0.082 Uiso 1 1 calc R . . H23A H 0.1817 0.5416 0.6776 0.082 Uiso 1 1 calc R . . H23B H 0.2180 0.6941 0.6370 0.082 Uiso 1 1 calc 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 0.03141(10) 0.02008(7) 0.03239(10) -0.00292(5) -0.00297(7) 0.01193(6) O1 0.0383(16) 0.0297(12) 0.0520(17) -0.0147(11) -0.0075(13) 0.0118(11) C1 0.034(2) 0.0342(17) 0.033(2) -0.0030(14) -0.0032(16) 0.0185(16) O2 0.0378(16) 0.0336(12) 0.0493(17) 0.0069(11) -0.0050(12) 0.0153(11) C2 0.057(3) 0.050(2) 0.049(3) 0.0114(19) -0.001(2) 0.025(2) O3 0.0447(16) 0.0304(11) 0.0342(15) -0.0089(10) 0.0005(12) 0.0144(11) C3 0.096(4) 0.090(4) 0.057(3) 0.023(3) -0.006(3) 0.055(4) O4 0.0578(19) 0.0386(13) 0.0383(16) 0.0067(11) 0.0048(13) 0.0292(13) C4 0.083(4) 0.115(4) 0.054(3) -0.007(3) -0.025(3) 0.060(4) O5 0.0402(16) 0.0301(11) 0.0437(16) 0.0030(10) 0.0125(12) 0.0161(11) C5 0.053(3) 0.068(3) 0.063(3) -0.023(2) -0.019(2) 0.020(2) O6 0.0451(17) 0.0361(13) 0.0515(18) -0.0001(12) 0.0094(14) 0.0084(13) C6 0.040(3) 0.041(2) 0.056(3) -0.0086(18) -0.009(2) 0.0139(18) C7 0.027(2) 0.0297(16) 0.032(2) -0.0022(14) 0.0017(15) 0.0145(15) O7 0.0375(17) 0.0276(13) 0.070(2) -0.0063(13) -0.0069(14) 0.0163(12) O8 0.0556(19) 0.0314(13) 0.062(2) 0.0107(13) 0.0231(15) 0.0246(14) C8 0.033(2) 0.0314(16) 0.034(2) 0.0022(14) 0.0031(16) 0.0085(16) O9 0.0325(17) 0.0326(12) 0.0438(19) -0.0039(12) 0.0022(15) 0.0136(12) C9 0.050(3) 0.046(2) 0.046(3) 0.0090(17) -0.002(2) 0.022(2) C10 0.066(4) 0.078(3) 0.057(3) 0.025(3) 0.000(3) 0.033(3) C11 0.070(4) 0.106(4) 0.042(3) 0.022(3) -0.005(3) 0.027(3) C12 0.076(4) 0.076(3) 0.037(3) -0.013(2) 0.008(2) 0.014(3) C13 0.061(3) 0.046(2) 0.039(3) -0.0035(17) 0.007(2) 0.019(2) C14 0.030(2) 0.0270(15) 0.034(2) 0.0009(14) 0.0035(16) 0.0109(15) C15 0.037(2) 0.0420(19) 0.041(2) 0.0054(17) 0.0055(18) 0.0198(18) C16 0.052(3) 0.058(2) 0.051(3) 0.006(2) 0.009(2) 0.019(2) C17 0.070(4) 0.091(4) 0.049(3) 0.010(3) 0.015(3) 0.032(3) C18 0.081(4) 0.098(4) 0.038(3) -0.006(3) -0.001(3) 0.041(3) C19 0.064(4) 0.076(3) 0.056(3) -0.006(3) -0.013(3) 0.016(3) C20 0.046(3) 0.054(2) 0.043(3) 0.0036(19) 0.001(2) 0.015(2) C21 0.035(2) 0.0329(18) 0.043(2) 0.0038(16) 0.0067(18) 0.0183(17) C22 0.043(3) 0.050(2) 0.107(4) -0.024(2) -0.017(3) 0.018(2) C23 0.056(3) 0.044(2) 0.064(3) 0.0050(19) 0.015(2) 0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.276(2) . ? Tb1 O3 2.283(2) . ? Tb1 O2 2.322(2) 2_666 ? Tb1 O4 2.333(2) . ? Tb1 O5 2.410(2) . ? Tb1 O7 2.436(3) . ? Tb1 O8 2.474(3) . ? Tb1 O9 2.481(3) . ? O1 C7 1.244(4) . ? C1 C6 1.381(5) . ? C1 C2 1.395(5) . ? C1 C7 1.481(5) . ? O2 C7 1.258(3) . ? O2 Tb1 2.322(2) 2_666 ? C2 C3 1.368(6) . ? O3 C14 1.250(4) . ? C3 C4 1.359(7) . ? O4 C14 1.259(3) 2_676 ? C4 C5 1.372(6) . ? O5 C21 1.265(4) . ? C5 C6 1.386(6) . ? O6 C21 1.248(4) . ? O7 C22 1.387(5) . ? O8 C23 1.419(4) . ? C8 C9 1.389(4) . ? C8 C13 1.390(5) . ? C8 C14 1.481(5) . ? C9 C10 1.367(6) . ? C10 C11 1.348(6) . ? C11 C12 1.365(6) . ? C12 C13 1.387(6) . ? C14 O4 1.259(3) 2_676 ? C15 C20 1.371(5) . ? C15 C16 1.376(5) . ? C15 C21 1.493(5) . ? C16 C17 1.370(6) . ? C17 C18 1.352(7) . ? C18 C19 1.374(6) . ? C19 C20 1.362(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 144.92(9) . . ? O1 Tb1 O2 104.30(8) . 2_666 ? O3 Tb1 O2 87.37(8) . 2_666 ? O1 Tb1 O4 90.51(9) . . ? O3 Tb1 O4 100.80(8) . . ? O2 Tb1 O4 141.33(9) 2_666 . ? O1 Tb1 O5 72.60(8) . . ? O3 Tb1 O5 142.46(8) . . ? O2 Tb1 O5 77.97(9) 2_666 . ? O4 Tb1 O5 72.71(8) . . ? O1 Tb1 O7 79.64(8) . . ? O3 Tb1 O7 72.08(9) . . ? O2 Tb1 O7 143.42(9) 2_666 . ? O4 Tb1 O7 73.74(9) . . ? O5 Tb1 O7 135.69(9) . . ? O1 Tb1 O8 74.45(10) . . ? O3 Tb1 O8 77.17(8) . . ? O2 Tb1 O8 74.60(9) 2_666 . ? O4 Tb1 O8 144.05(9) . . ? O5 Tb1 O8 129.66(7) . . ? O7 Tb1 O8 71.55(9) . . ? O1 Tb1 O9 145.85(10) . . ? O3 Tb1 O9 69.08(9) . . ? O2 Tb1 O9 72.97(9) 2_666 . ? O4 Tb1 O9 74.93(10) . . ? O5 Tb1 O9 73.60(9) . . ? O7 Tb1 O9 123.37(8) . . ? O8 Tb1 O9 133.59(11) . . ? C7 O1 Tb1 172.3(2) . . ? C6 C1 C2 119.2(3) . . ? C6 C1 C7 120.9(3) . . ? C2 C1 C7 119.8(3) . . ? C7 O2 Tb1 133.7(2) . 2_666 ? C3 C2 C1 119.7(4) . . ? C14 O3 Tb1 177.9(2) . . ? C4 C3 C2 120.9(4) . . ? C14 O4 Tb1 134.3(2) 2_676 . ? C3 C4 C5 120.4(4) . . ? C21 O5 Tb1 130.92(19) . . ? C4 C5 C6 119.8(4) . . ? C1 C6 C5 120.0(4) . . ? O1 C7 O2 123.4(3) . . ? O1 C7 C1 119.1(3) . . ? O2 C7 C1 117.5(3) . . ? C22 O7 Tb1 135.8(2) . . ? C23 O8 Tb1 129.4(2) . . ? C9 C8 C13 118.7(4) . . ? C9 C8 C14 120.6(3) . . ? C13 C8 C14 120.7(3) . . ? C10 C9 C8 120.8(4) . . ? C11 C10 C9 120.0(4) . . ? C10 C11 C12 121.0(5) . . ? C11 C12 C13 120.1(4) . . ? C12 C13 C8 119.3(4) . . ? O3 C14 O4 123.2(3) . 2_676 ? O3 C14 C8 118.4(3) . . ? O4 C14 C8 118.4(3) 2_676 . ? C20 C15 C16 118.6(4) . . ? C20 C15 C21 120.9(3) . . ? C16 C15 C21 120.5(4) . . ? C17 C16 C15 120.9(4) . . ? C18 C17 C16 119.9(5) . . ? C17 C18 C19 119.8(5) . . ? C20 C19 C18 120.4(5) . . ? C19 C20 C15 120.3(4) . . ? O6 C21 O5 124.0(3) . . ? O6 C21 C15 118.3(3) . . ? O5 C21 C15 117.7(3) . . ? _diffrn_measured_fraction_theta_max 0.926 _diffrn_reflns_theta_full 28.35 _diffrn_measured_fraction_theta_full 0.926 _refine_diff_density_max 1.544 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.091