Electronic Supplementary Material for CrystEngComm This Journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_cambridge 1350 _publ_section_title ;Structural Variations in Rare Earth-Benzoate Complexes: Part II - Yttrium and Terbium ; _publ_contact_author_name 'Prof. Peter Junk' _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU loop_ _publ_author_name 'Peter Junk' G.Deacon 'Stefanie Hein' 'Thomas Justel' 'Winnie Lee' 'David Turner' # Attachment '1a.CIF' data_1a _database_code_depnum_ccdc_archive 'CCDC 649804' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tris(benzoato)(dimethylsulphoxide)yttrium(III)] ; _chemical_name_common '[Y(BA)3(DMSO)]n' _chemical_melting_point ? _chemical_formula_moiety C23H21O7S1Y1 _chemical_formula_sum C23H21O7S1Y1 _chemical_formula_weight 530.37 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting tetragonal _symmetry_space_group_name_H-M P42/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 22.2733(12) _cell_length_b 22.2733(12) _cell_length_c 8.9917(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4460.8(4) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 2.751 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.4372 _exptl_absorpt_correction_T_max 0.7020 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD' _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 36895 _diffrn_reflns_av_R_equivalents 0.1452 _diffrn_reflns_av_sigmaI/netI 0.1101 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 27.49 _reflns_number_total 5114 _reflns_number_gt 3597 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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. TWIN matrix 0 1 0 1 0 0 0 0 -1 used for tetragonal twin. ; _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^)+(0.0257P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5114 _refine_ls_number_parameters 318 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0917 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0661 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.996 _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 Y1 Y -0.004486(17) 0.471475(16) 0.22475(3) 0.01070(9) Uani 1 1 d . . . O1 O -0.05960(11) 0.47083(13) 0.4376(3) 0.0168(6) Uani 1 1 d . . . C1 C -0.09504(15) 0.5034(2) 0.5114(4) 0.0139(8) Uani 1 1 d U . . S1A S 0.03188(9) 0.33005(8) 0.38514(18) 0.0202(6) Uani 0.576(3) 1 d P A 1 S1B S -0.02522(14) 0.33797(12) 0.4290(3) 0.0265(9) Uani 0.424(3) 1 d P A 2 O2 O -0.07847(11) 0.53648(12) 0.6190(3) 0.0163(6) Uani 1 1 d . . . C2 C -0.16078(15) 0.5017(2) 0.4774(4) 0.0136(8) Uani 1 1 d U . . O3 O -0.07296(13) 0.43131(13) 0.0641(3) 0.0162(7) Uani 1 1 d . . . C3 C -0.18319(18) 0.45864(19) 0.3781(4) 0.0217(11) Uani 1 1 d . . . H3 H -0.1567 0.4317 0.3293 0.026 Uiso 1 1 calc R . . O4 O -0.05105(11) 0.44301(12) -0.1781(3) 0.0179(7) Uani 1 1 d . . . C4 C -0.2443(2) 0.4558(2) 0.3520(5) 0.0336(13) Uani 1 1 d . . . H4 H -0.2597 0.4266 0.2851 0.040 Uiso 1 1 calc R . . O5 O 0.05795(12) 0.44018(13) 0.0437(3) 0.0172(7) Uani 1 1 d . . . C5 C -0.28288(18) 0.4945(3) 0.4211(4) 0.0336(12) Uani 1 1 d . . . H5 H -0.3248 0.4916 0.4035 0.040 Uiso 1 1 calc R . . O6 O 0.07711(11) 0.45296(12) -0.1959(3) 0.0151(6) Uani 1 1 d . . . C6 C -0.2608(2) 0.5377(2) 0.5164(4) 0.0334(13) Uani 1 1 d . . . H6 H -0.2875 0.5655 0.5617 0.040 Uiso 1 1 calc R . . O7 O -0.00501(13) 0.37007(11) 0.2892(3) 0.0201(6) Uani 1 1 d . . . C7 C -0.19934(19) 0.5407(2) 0.5466(4) 0.0252(11) Uani 1 1 d . . . H7 H -0.1844 0.5697 0.6147 0.030 Uiso 1 1 calc R . . C8 C -0.08263(18) 0.42311(17) -0.0738(4) 0.0105(9) Uani 1 1 d . . . C9 C -0.13797(17) 0.38727(18) -0.1109(4) 0.0122(9) Uani 1 1 d . . . C10 C -0.15762(17) 0.38329(16) -0.2569(4) 0.0152(9) Uani 1 1 d . . . H10 H -0.1342 0.4004 -0.3343 0.018 Uiso 1 1 calc R . . C11 C -0.21090(19) 0.35479(17) -0.2907(4) 0.0198(10) Uani 1 1 d . . . H11 H -0.2245 0.3534 -0.3908 0.024 Uiso 1 1 calc R . . C12 C -0.24458(19) 0.32825(18) -0.1790(5) 0.0249(11) Uani 1 1 d . . . H12 H -0.2814 0.3089 -0.2020 0.030 Uiso 1 1 calc R . . C13 C -0.2239(2) 0.3302(2) -0.0317(5) 0.0260(11) Uani 1 1 d . . . H13 H -0.2460 0.3112 0.0454 0.031 Uiso 1 1 calc R . . C14 C -0.17147(18) 0.36003(18) -0.0002(4) 0.0175(9) Uani 1 1 d . . . H14 H -0.1579 0.3620 0.0999 0.021 Uiso 1 1 calc R . . C15 C 0.08968(18) 0.43268(18) -0.0698(4) 0.0137(10) Uani 1 1 d . . . C16 C 0.14640(17) 0.39627(17) -0.0526(4) 0.0134(9) Uani 1 1 d . . . C17 C 0.16168(18) 0.37194(18) 0.0847(4) 0.0183(9) Uani 1 1 d . . . H17 H 0.1356 0.3768 0.1674 0.022 Uiso 1 1 calc R . . C18 C 0.2150(2) 0.34057(19) 0.1007(5) 0.0273(11) Uani 1 1 d . . . H18 H 0.2257 0.3241 0.1945 0.033 Uiso 1 1 calc R . . C19 C 0.25236(19) 0.3333(2) -0.0198(5) 0.0296(12) Uani 1 1 d . . . H19 H 0.2888 0.3118 -0.0081 0.035 Uiso 1 1 calc R . . C20 C 0.23796(18) 0.35671(19) -0.1569(5) 0.0245(11) Uani 1 1 d . . . H20 H 0.2641 0.3514 -0.2393 0.029 Uiso 1 1 calc R . . C21 C 0.18459(18) 0.38814(17) -0.1726(4) 0.0186(10) Uani 1 1 d . . . H21 H 0.1741 0.4043 -0.2669 0.022 Uiso 1 1 calc R . . C22A C 0.0171(6) 0.3537(7) 0.5736(16) 0.015(3) Uani 0.576(3) 1 d PU A 1 H22A H 0.0364 0.3927 0.5916 0.022 Uiso 0.576(3) 1 calc PR A 1 H22B H 0.0333 0.3239 0.6431 0.022 Uiso 0.576(3) 1 calc PR A 1 H22C H -0.0263 0.3575 0.5886 0.022 Uiso 0.576(3) 1 calc PR A 1 C22B C 0.0339(8) 0.3536(11) 0.569(3) 0.025(5) Uani 0.424(3) 1 d PU A 2 H22D H 0.0305 0.3953 0.6026 0.038 Uiso 0.424(3) 1 calc PR A 2 H22E H 0.0735 0.3472 0.5241 0.038 Uiso 0.424(3) 1 calc PR A 2 H22F H 0.0289 0.3265 0.6539 0.038 Uiso 0.424(3) 1 calc PR A 2 C23A C -0.0069(6) 0.2623(5) 0.3936(15) 0.006(3) Uani 0.576(3) 1 d PU A 1 H23A H -0.0062 0.2430 0.2957 0.009 Uiso 0.576(3) 1 calc PR A 1 H23B H -0.0486 0.2699 0.4230 0.009 Uiso 0.576(3) 1 calc PR A 1 H23C H 0.0121 0.2359 0.4669 0.009 Uiso 0.576(3) 1 calc PR A 1 C23B C -0.0059(15) 0.2613(13) 0.413(3) 0.072(11) Uani 0.424(3) 1 d PU A 2 H23D H -0.0294 0.2430 0.3324 0.108 Uiso 0.424(3) 1 calc PR A 2 H23E H -0.0145 0.2407 0.5065 0.108 Uiso 0.424(3) 1 calc PR A 2 H23F H 0.0370 0.2577 0.3898 0.108 Uiso 0.424(3) 1 calc PR A 2 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 Y1 0.0092(2) 0.0134(2) 0.00957(14) -0.00029(15) -0.00034(16) 0.0006(2) O1 0.0126(15) 0.0247(16) 0.0130(14) 0.0024(13) 0.0038(11) 0.0017(14) C1 0.0113(19) 0.0155(19) 0.0148(19) 0.0097(18) 0.0009(16) -0.004(2) S1A 0.0219(13) 0.0199(11) 0.0187(10) 0.0012(8) 0.0001(9) 0.0013(10) S1B 0.0283(19) 0.0209(16) 0.0304(16) 0.0001(11) 0.0057(14) -0.0002(14) O2 0.0125(15) 0.0232(17) 0.0133(14) -0.0010(13) -0.0041(11) -0.0010(13) C2 0.0127(19) 0.021(2) 0.0075(17) 0.0111(19) -0.0012(15) -0.003(2) O3 0.0188(16) 0.0170(16) 0.0129(14) -0.0019(12) -0.0057(12) -0.0013(13) C3 0.017(3) 0.021(3) 0.026(2) 0.005(2) -0.0050(19) -0.005(2) O4 0.0130(15) 0.0227(16) 0.0182(14) -0.0021(13) 0.0066(12) -0.0023(13) C4 0.030(3) 0.039(3) 0.032(3) 0.005(2) -0.014(2) -0.018(3) O5 0.0120(16) 0.0280(18) 0.0114(14) -0.0023(13) 0.0028(12) 0.0035(13) C5 0.009(2) 0.066(4) 0.025(2) 0.012(3) -0.0023(19) -0.008(3) O6 0.0153(16) 0.0192(17) 0.0108(14) 0.0000(12) 0.0013(11) -0.0006(12) C6 0.017(3) 0.063(4) 0.020(2) 0.006(2) 0.0069(19) 0.017(3) O7 0.0276(16) 0.0153(14) 0.0174(13) 0.0029(11) -0.0048(14) 0.0028(14) C7 0.019(3) 0.039(3) 0.018(2) 0.001(2) -0.0016(19) 0.006(2) C8 0.014(2) 0.002(2) 0.015(2) -0.0003(17) -0.0046(19) 0.0025(19) C9 0.012(2) 0.011(2) 0.014(2) 0.0038(17) -0.0004(18) 0.0026(18) C10 0.022(2) 0.010(2) 0.014(2) -0.0006(16) -0.0033(17) -0.0015(17) C11 0.027(3) 0.016(2) 0.017(2) -0.0054(18) -0.009(2) 0.000(2) C12 0.017(2) 0.017(2) 0.041(3) -0.002(2) -0.008(2) -0.007(2) C13 0.028(3) 0.024(3) 0.027(3) 0.003(2) 0.002(2) -0.009(2) C14 0.019(3) 0.021(3) 0.013(2) 0.0004(18) -0.0043(18) -0.0028(19) C15 0.011(2) 0.009(2) 0.021(2) -0.0048(19) 0.0011(19) -0.0082(19) C16 0.013(2) 0.010(2) 0.018(2) -0.0020(18) -0.0009(18) -0.0002(18) C17 0.015(2) 0.021(3) 0.020(2) 0.0040(19) -0.0055(19) 0.000(2) C18 0.026(3) 0.026(3) 0.030(3) 0.014(2) -0.010(2) -0.002(2) C19 0.010(3) 0.025(3) 0.054(3) 0.001(2) -0.008(2) -0.001(2) C20 0.016(3) 0.021(3) 0.036(3) -0.006(2) 0.005(2) 0.005(2) C21 0.020(3) 0.015(2) 0.021(2) -0.0012(19) 0.0015(19) 0.0009(19) C22A 0.014(5) 0.017(4) 0.013(4) 0.002(3) -0.005(4) -0.007(4) C22B 0.027(7) 0.028(6) 0.020(6) 0.000(4) 0.002(5) 0.001(5) C23A 0.011(4) 0.002(4) 0.005(3) 0.000(2) 0.002(3) 0.001(3) C23B 0.071(11) 0.070(11) 0.076(12) 0.000(5) -0.001(5) 0.000(5) _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 Y1 O5 2.252(3) . ? Y1 O1 2.273(2) . ? Y1 O3 2.283(3) . ? Y1 O4 2.310(3) 5_565 ? Y1 O2 2.328(2) 5_566 ? Y1 O7 2.332(2) . ? Y1 O6 2.349(3) 5_565 ? O1 C1 1.261(5) . ? C1 O2 1.270(5) . ? C1 C2 1.496(5) . ? S1A O7 1.488(3) . ? S1A C23A 1.741(13) . ? S1A C22A 1.805(15) . ? S1B O7 1.514(4) . ? S1B C23B 1.77(3) . ? S1B C22B 1.85(2) . ? O2 Y1 2.328(2) 5_566 ? C2 C7 1.371(6) . ? C2 C3 1.403(6) . ? O3 C8 1.272(4) . ? C3 C4 1.383(6) . ? C3 H3 0.9500 . ? O4 C8 1.253(4) . ? O4 Y1 2.310(3) 5_565 ? C4 C5 1.366(6) . ? C4 H4 0.9500 . ? O5 C15 1.253(4) . ? C5 C6 1.379(6) . ? C5 H5 0.9500 . ? O6 C15 1.252(4) . ? O6 Y1 2.349(3) 5_565 ? C6 C7 1.398(6) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.506(5) . ? C9 C14 1.384(5) . ? C9 C10 1.386(5) . ? C10 C11 1.380(5) . ? C10 H10 0.9500 . ? C11 C12 1.386(6) . ? C11 H11 0.9500 . ? C12 C13 1.402(6) . ? C12 H12 0.9500 . ? C13 C14 1.373(6) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.509(5) . ? C16 C21 1.386(5) . ? C16 C17 1.391(5) . ? C17 C18 1.386(6) . ? C17 H17 0.9500 . ? C18 C19 1.375(6) . ? C18 H18 0.9500 . ? C19 C20 1.376(5) . ? C19 H19 0.9500 . ? C20 C21 1.387(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? 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 Y1 O1 160.06(10) . . ? O5 Y1 O3 80.44(9) . . ? O1 Y1 O3 99.75(10) . . ? O5 Y1 O4 78.06(10) . 5_565 ? O1 Y1 O4 116.57(10) . 5_565 ? O3 Y1 O4 124.47(9) . 5_565 ? O5 Y1 O2 85.56(9) . 5_566 ? O1 Y1 O2 85.42(9) . 5_566 ? O3 Y1 O2 151.91(10) . 5_566 ? O4 Y1 O2 75.36(9) 5_565 5_566 ? O5 Y1 O7 83.28(10) . . ? O1 Y1 O7 77.41(9) . . ? O3 Y1 O7 76.96(9) . . ? O4 Y1 O7 147.85(10) 5_565 . ? O2 Y1 O7 77.30(10) 5_566 . ? O5 Y1 O6 124.57(9) . 5_565 ? O1 Y1 O6 74.07(9) . 5_565 ? O3 Y1 O6 75.58(9) . 5_565 ? O4 Y1 O6 75.99(9) 5_565 5_565 ? O2 Y1 O6 131.89(9) 5_566 5_565 ? O7 Y1 O6 135.90(10) . 5_565 ? C1 O1 Y1 141.0(3) . . ? O1 C1 O2 123.5(3) . . ? O1 C1 C2 119.4(4) . . ? O2 C1 C2 117.0(3) . . ? O7 S1A C23A 105.7(5) . . ? O7 S1A C22A 105.6(5) . . ? C23A S1A C22A 97.0(6) . . ? O7 S1B C23B 108.3(11) . . ? O7 S1B C22B 105.3(7) . . ? C23B S1B C22B 93.7(12) . . ? C1 O2 Y1 130.2(3) . 5_566 ? C7 C2 C3 120.0(4) . . ? C7 C2 C1 120.3(4) . . ? C3 C2 C1 119.7(4) . . ? C8 O3 Y1 141.8(3) . . ? C4 C3 C2 119.3(4) . . ? C4 C3 H3 120.4 . . ? C2 C3 H3 120.4 . . ? C8 O4 Y1 136.7(2) . 5_565 ? C5 C4 C3 120.9(4) . . ? C5 C4 H4 119.5 . . ? C3 C4 H4 119.5 . . ? C15 O5 Y1 168.2(3) . . ? C4 C5 C6 119.9(4) . . ? C4 C5 H5 120.1 . . ? C6 C5 H5 120.1 . . ? C15 O6 Y1 120.8(2) . 5_565 ? C5 C6 C7 120.3(4) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? S1A O7 S1B 53.15(15) . . ? S1A O7 Y1 136.19(17) . . ? S1B O7 Y1 131.69(17) . . ? C2 C7 C6 119.7(4) . . ? C2 C7 H7 120.2 . . ? C6 C7 H7 120.2 . . ? O4 C8 O3 125.7(4) . . ? O4 C8 C9 118.8(3) . . ? O3 C8 C9 115.5(3) . . ? C14 C9 C10 118.9(4) . . ? C14 C9 C8 121.0(3) . . ? C10 C9 C8 120.1(3) . . ? C11 C10 C9 120.7(4) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 120.1(4) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 119.6(4) . . ? C11 C12 H12 120.2 . . ? C13 C12 H12 120.2 . . ? C14 C13 C12 119.3(4) . . ? C14 C13 H13 120.4 . . ? C12 C13 H13 120.3 . . ? C13 C14 C9 121.5(4) . . ? C13 C14 H14 119.3 . . ? C9 C14 H14 119.3 . . ? O5 C15 O6 124.3(4) . . ? O5 C15 C16 117.4(4) . . ? O6 C15 C16 118.3(3) . . ? C21 C16 C17 119.3(4) . . ? C21 C16 C15 120.3(4) . . ? C17 C16 C15 120.4(4) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C19 C18 C17 119.7(4) . . ? C19 C18 H18 120.1 . . ? C17 C18 H18 120.1 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C19 C20 C21 118.8(4) . . ? C19 C20 H20 120.6 . . ? C21 C20 H20 120.6 . . ? C16 C21 C20 120.8(4) . . ? C16 C21 H21 119.6 . . ? C20 C21 H21 119.6 . . ? S1A C22A H22A 109.5 . . ? S1A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? S1A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? S1B C22B H22D 109.5 . . ? S1B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? S1B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? S1A C23A H23A 109.5 . . ? S1A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? S1A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? S1B C23B H23D 109.5 . . ? S1B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? S1B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.435 _refine_diff_density_min -0.467 _refine_diff_density_rms 0.107 # Attachment '1b.CIF' data_1b _database_code_depnum_ccdc_archive 'CCDC 649805' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tris(benzoato)(dimethylsulphoxide)terbium(III)] ; _chemical_name_common '[Tb(BA)3(DMSO)]n' _chemical_melting_point ? _chemical_formula_moiety C23H21O7S1Tb1 _chemical_formula_sum 'C23 H21 O7 S1 Tb1' _chemical_formula_weight 600.38 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M P42/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x+1/2, z+1/2' '-x+1/2, -y+1/2, z' 'y+1/2, -x, z+1/2' '-x, -y, -z' 'y, -x-1/2, -z-1/2' 'x-1/2, y-1/2, -z' '-y-1/2, x, -z-1/2' _cell_length_a 22.2964(3) _cell_length_b 22.2964(3) _cell_length_c 8.9633(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4455.92(13) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.790 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2368 _exptl_absorpt_coefficient_mu 3.310 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.3631 _exptl_absorpt_correction_T_max 0.5183 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 25474 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 6 _diffrn_reflns_theta_min 0.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5116 _reflns_number_gt 4849 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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. Refined with TWIN 0 1 0 1 0 0 0 0 -1. BASF 0.632 ; _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^)+(0.0083P)^2^+2.5270P] 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 5116 _refine_ls_number_parameters 318 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0193 _refine_ls_R_factor_gt 0.0170 _refine_ls_wR_factor_ref 0.0363 _refine_ls_wR_factor_gt 0.0353 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 Tb1 Tb -0.004640(5) 0.471621(5) 0.226480(11) 0.01020(3) Uani 1 1 d . . . O1 O -0.06049(7) 0.47087(8) 0.4427(2) 0.0162(4) Uani 1 1 d . . . C1 C -0.09604(10) 0.50400(12) 0.5145(3) 0.0131(5) Uani 1 1 d . . . S1A S 0.03188(5) 0.32922(4) 0.38595(12) 0.0169(3) Uani 0.655(2) 1 d P A 1 S1B S -0.02601(9) 0.33749(8) 0.4315(2) 0.0195(6) Uani 0.345(2) 1 d P A 2 O2 O -0.08005(7) 0.53835(8) 0.6186(2) 0.0161(4) Uani 1 1 d . . . C2 C -0.16165(10) 0.50141(13) 0.4776(3) 0.0151(5) Uani 1 1 d . . . O3 O -0.07400(8) 0.43138(8) 0.0638(2) 0.0163(4) Uani 1 1 d . . . C3 C -0.18316(12) 0.45877(12) 0.3783(3) 0.0209(6) Uani 1 1 d . . . H3 H -0.1563 0.4323 0.3293 0.025 Uiso 1 1 calc R . . O4 O -0.05245(7) 0.44241(8) -0.1787(2) 0.0160(4) Uani 1 1 d . . . C4 C -0.24486(13) 0.45523(14) 0.3513(4) 0.0327(8) Uani 1 1 d . . . H4 H -0.2599 0.4259 0.2841 0.039 Uiso 1 1 calc R . . O5 O 0.05787(8) 0.44000(8) 0.0410(2) 0.0182(4) Uani 1 1 d . . . C5 C -0.28360(12) 0.49360(16) 0.4208(3) 0.0324(8) Uani 1 1 d . . . H5 H -0.3255 0.4904 0.4029 0.039 Uiso 1 1 calc R . . O6 O 0.07832(7) 0.45200(8) -0.1985(2) 0.0168(4) Uani 1 1 d . . . C6 C -0.26254(12) 0.53672(16) 0.5162(3) 0.0333(8) Uani 1 1 d . . . H6 H -0.2896 0.5640 0.5618 0.040 Uiso 1 1 calc R . . O7 O -0.00598(9) 0.36940(7) 0.29093(19) 0.0187(4) Uani 1 1 d . . . C7 C -0.20123(12) 0.54057(14) 0.5463(3) 0.0243(7) Uani 1 1 d . . . H7 H -0.1867 0.5700 0.6139 0.029 Uiso 1 1 calc R . . C8 C -0.08403(11) 0.42298(11) -0.0729(3) 0.0133(5) Uani 1 1 d . . . C9 C -0.13915(10) 0.38715(10) -0.1119(3) 0.0133(5) Uani 1 1 d . . . C10 C -0.15883(12) 0.38332(11) -0.2586(3) 0.0162(6) Uani 1 1 d . . . H10 H -0.1356 0.4004 -0.3365 0.019 Uiso 1 1 calc R . . C11 C -0.21221(12) 0.35464(12) -0.2914(3) 0.0213(6) Uani 1 1 d . . . H11 H -0.2261 0.3529 -0.3916 0.026 Uiso 1 1 calc R . . C12 C -0.24556(12) 0.32831(12) -0.1780(4) 0.0233(6) Uani 1 1 d . . . H12 H -0.2824 0.3090 -0.2005 0.028 Uiso 1 1 calc R . . C13 C -0.22516(12) 0.33026(12) -0.0325(3) 0.0241(7) Uani 1 1 d . . . H13 H -0.2473 0.3111 0.0445 0.029 Uiso 1 1 calc R . . C14 C -0.17225(11) 0.36017(11) 0.0008(3) 0.0183(5) Uani 1 1 d . . . H14 H -0.1586 0.3622 0.1011 0.022 Uiso 1 1 calc R . . C15 C 0.09012(10) 0.43199(11) -0.0720(3) 0.0127(5) Uani 1 1 d . . . C16 C 0.14712(11) 0.39604(10) -0.0527(3) 0.0134(5) Uani 1 1 d . . . C17 C 0.16168(12) 0.37243(11) 0.0855(3) 0.0201(6) Uani 1 1 d . . . H17 H 0.1354 0.3778 0.1679 0.024 Uiso 1 1 calc R . . C18 C 0.21495(12) 0.34075(12) 0.1029(4) 0.0275(7) Uani 1 1 d . . . H18 H 0.2252 0.3246 0.1976 0.033 Uiso 1 1 calc R . . C19 C 0.25300(12) 0.33274(12) -0.0175(4) 0.0288(7) Uani 1 1 d . . . H19 H 0.2892 0.3109 -0.0053 0.035 Uiso 1 1 calc R . . C20 C 0.23857(12) 0.35630(12) -0.1548(4) 0.0255(7) Uani 1 1 d . . . H20 H 0.2648 0.3508 -0.2372 0.031 Uiso 1 1 calc R . . C21 C 0.18538(11) 0.38828(11) -0.1727(3) 0.0177(5) Uani 1 1 d . . . H21 H 0.1754 0.4047 -0.2673 0.021 Uiso 1 1 calc R . . C22A C 0.0218(9) 0.3522(8) 0.5755(18) 0.030(4) Uani 0.655(2) 1 d P A 1 H22A H 0.0412 0.3911 0.5912 0.045 Uiso 0.655(2) 1 calc PR A 1 H22B H 0.0397 0.3223 0.6422 0.045 Uiso 0.655(2) 1 calc PR A 1 H22C H -0.0212 0.3557 0.5971 0.045 Uiso 0.655(2) 1 calc PR A 1 C22B C 0.0261(16) 0.3556(16) 0.570(4) 0.030(8) Uani 0.345(2) 1 d P A 2 H22D H 0.0208 0.3976 0.6001 0.046 Uiso 0.345(2) 1 calc PR A 2 H22E H 0.0668 0.3499 0.5315 0.046 Uiso 0.345(2) 1 calc PR A 2 H22F H 0.0200 0.3295 0.6569 0.046 Uiso 0.345(2) 1 calc PR A 2 C23A C -0.0085(7) 0.2621(8) 0.393(2) 0.028(4) Uani 0.655(2) 1 d P A 1 H23A H -0.0076 0.2428 0.2946 0.043 Uiso 0.655(2) 1 calc PR A 1 H23B H -0.0502 0.2705 0.4209 0.043 Uiso 0.655(2) 1 calc PR A 1 H23C H 0.0096 0.2353 0.4669 0.043 Uiso 0.655(2) 1 calc PR A 1 C23B C -0.0064(11) 0.2591(12) 0.411(3) 0.009(4) Uani 0.345(2) 1 d PU A 2 H23D H -0.0303 0.2413 0.3307 0.013 Uiso 0.345(2) 1 calc PR A 2 H23E H -0.0146 0.2379 0.5048 0.013 Uiso 0.345(2) 1 calc PR A 2 H23F H 0.0363 0.2556 0.3870 0.013 Uiso 0.345(2) 1 calc PR A 2 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 0.00876(5) 0.01253(6) 0.00932(6) 0.00027(4) -0.00024(4) 0.00020(5) O1 0.0122(8) 0.0217(9) 0.0147(10) 0.0032(8) 0.0019(7) 0.0028(8) C1 0.0120(10) 0.0177(11) 0.0097(13) 0.0079(11) -0.0002(10) -0.0042(10) S1A 0.0178(5) 0.0158(5) 0.0169(6) 0.0022(4) -0.0006(4) -0.0003(4) S1B 0.0210(9) 0.0150(9) 0.0224(12) 0.0021(8) 0.0039(9) 0.0014(8) O2 0.0142(8) 0.0202(9) 0.0137(10) -0.0004(8) -0.0023(7) -0.0010(7) C2 0.0122(11) 0.0236(12) 0.0096(13) 0.0076(12) -0.0004(10) -0.0006(11) O3 0.0175(9) 0.0170(8) 0.0145(10) 0.0004(8) -0.0033(8) -0.0028(7) C3 0.0170(12) 0.0232(14) 0.0225(16) 0.0025(12) -0.0042(12) -0.0035(10) O4 0.0154(8) 0.0163(8) 0.0163(9) 0.0004(8) 0.0019(8) -0.0027(7) C4 0.0265(15) 0.0388(18) 0.033(2) 0.0050(15) -0.0149(14) -0.0145(13) O5 0.0162(8) 0.0223(9) 0.0161(11) -0.0040(8) 0.0008(8) 0.0018(7) C5 0.0124(12) 0.058(2) 0.0266(17) 0.0164(17) -0.0036(12) -0.0075(14) O6 0.0151(9) 0.0207(9) 0.0145(10) 0.0021(8) 0.0004(7) 0.0039(7) C6 0.0157(13) 0.062(2) 0.0226(17) 0.0070(17) 0.0038(12) 0.0125(14) O7 0.0261(10) 0.0155(8) 0.0145(10) 0.0013(7) -0.0046(8) 0.0004(8) C7 0.0190(13) 0.0387(17) 0.0151(16) -0.0031(13) -0.0007(12) 0.0040(12) C8 0.0133(11) 0.0085(11) 0.0179(15) 0.0005(10) -0.0032(11) 0.0029(9) C9 0.0131(12) 0.0097(11) 0.0170(15) -0.0005(10) -0.0018(10) 0.0018(9) C10 0.0189(12) 0.0126(11) 0.0171(15) 0.0005(10) -0.0014(11) 0.0004(10) C11 0.0234(14) 0.0186(13) 0.0218(16) -0.0015(11) -0.0114(12) -0.0012(11) C12 0.0203(13) 0.0174(13) 0.0321(18) -0.0014(13) -0.0084(13) -0.0059(10) C13 0.0227(14) 0.0235(14) 0.0261(18) 0.0036(12) 0.0019(13) -0.0086(11) C14 0.0190(13) 0.0199(13) 0.0160(15) 0.0010(11) -0.0031(11) -0.0026(10) C15 0.0116(11) 0.0113(11) 0.0152(14) -0.0019(10) -0.0017(10) -0.0017(9) C16 0.0135(11) 0.0092(11) 0.0174(15) 0.0011(10) -0.0019(10) -0.0011(9) C17 0.0189(13) 0.0194(13) 0.0220(16) 0.0034(12) -0.0010(12) -0.0015(10) C18 0.0238(14) 0.0232(14) 0.036(2) 0.0102(13) -0.0111(13) 0.0015(12) C19 0.0163(13) 0.0199(14) 0.050(2) 0.0002(14) -0.0074(14) 0.0039(11) C20 0.0171(13) 0.0228(14) 0.037(2) -0.0084(14) 0.0027(13) 0.0048(10) C21 0.0166(12) 0.0157(12) 0.0208(15) -0.0013(11) 0.0008(11) 0.0002(10) C22A 0.052(8) 0.024(6) 0.015(7) -0.006(6) 0.003(5) -0.003(5) C22B 0.044(13) 0.026(11) 0.022(13) 0.023(10) -0.012(10) -0.007(9) C23A 0.039(5) 0.019(4) 0.027(7) 0.007(4) -0.006(4) 0.001(3) C23B 0.015(5) 0.005(5) 0.007(5) 0.001(4) -0.001(4) -0.003(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 O5 2.2813(17) . ? Tb1 O1 2.3035(17) . ? Tb1 O3 2.3071(18) . ? Tb1 O4 2.3405(17) 5_565 ? Tb1 O7 2.3515(16) . ? Tb1 O2 2.3547(17) 5_566 ? Tb1 O6 2.3795(17) 5_565 ? O1 C1 1.261(3) . ? C1 O2 1.258(3) . ? C1 C2 1.501(3) . ? S1A O7 1.497(2) . ? S1A C23A 1.748(17) . ? S1A C22A 1.789(15) . ? S1B O7 1.514(3) . ? S1B C22B 1.75(3) . ? S1B C23B 1.81(3) . ? O2 Tb1 2.3547(17) 5_566 ? C2 C7 1.386(4) . ? C2 C3 1.388(4) . ? O3 C8 1.260(3) . ? C3 C4 1.399(4) . ? C3 H3 0.9500 . ? O4 C8 1.258(3) . ? O4 Tb1 2.3405(17) 5_565 ? C4 C5 1.366(5) . ? C4 H4 0.9500 . ? O5 C15 1.255(3) . ? C5 C6 1.369(5) . ? C5 H5 0.9500 . ? O6 C15 1.246(3) . ? O6 Tb1 2.3795(17) 5_565 ? C6 C7 1.396(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.507(3) . ? C9 C14 1.388(4) . ? C9 C10 1.388(4) . ? C10 C11 1.383(4) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 C13 1.382(4) . ? C12 H12 0.9500 . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.512(3) . ? C16 C21 1.384(4) . ? C16 C17 1.384(4) . ? C17 C18 1.391(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.376(4) . ? C19 H19 0.9500 . ? C20 C21 1.393(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22A H22A 0.9800 . ? C22A H22B 0.9800 . ? C22A H22C 0.9800 . ? C22B H22D 0.9800 . ? C22B H22E 0.9800 . ? C22B H22F 0.9800 . ? C23A H23A 0.9800 . ? C23A H23B 0.9800 . ? C23A H23C 0.9800 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? 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 Tb1 O1 160.25(6) . . ? O5 Tb1 O3 80.14(6) . . ? O1 Tb1 O3 99.58(6) . . ? O5 Tb1 O4 77.73(6) . 5_565 ? O1 Tb1 O4 116.99(6) . 5_565 ? O3 Tb1 O4 124.58(6) . 5_565 ? O5 Tb1 O7 83.53(7) . . ? O1 Tb1 O7 77.26(6) . . ? O3 Tb1 O7 76.69(6) . . ? O4 Tb1 O7 147.74(6) 5_565 . ? O5 Tb1 O2 84.88(6) . 5_566 ? O1 Tb1 O2 86.37(6) . 5_566 ? O3 Tb1 O2 150.88(6) . 5_566 ? O4 Tb1 O2 75.46(6) 5_565 5_566 ? O7 Tb1 O2 76.92(6) . 5_566 ? O5 Tb1 O6 124.48(6) . 5_565 ? O1 Tb1 O6 73.78(6) . 5_565 ? O3 Tb1 O6 75.46(6) . 5_565 ? O4 Tb1 O6 76.71(6) 5_565 5_565 ? O7 Tb1 O6 135.31(6) . 5_565 ? O2 Tb1 O6 133.12(6) 5_566 5_565 ? C1 O1 Tb1 139.95(16) . . ? O2 C1 O1 123.9(2) . . ? O2 C1 C2 117.6(2) . . ? O1 C1 C2 118.5(2) . . ? O7 S1A C23A 104.0(6) . . ? O7 S1A C22A 107.4(6) . . ? C23A S1A C22A 98.4(9) . . ? O7 S1B C22B 106.7(13) . . ? O7 S1B C23B 107.4(9) . . ? C22B S1B C23B 97.7(14) . . ? C1 O2 Tb1 127.36(16) . 5_566 ? C7 C2 C3 119.8(2) . . ? C7 C2 C1 119.9(2) . . ? C3 C2 C1 120.3(2) . . ? C8 O3 Tb1 142.34(16) . . ? C2 C3 C4 119.3(3) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C8 O4 Tb1 136.41(16) . 5_565 ? C5 C4 C3 120.5(3) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C15 O5 Tb1 169.21(17) . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C15 O6 Tb1 119.86(16) . 5_565 ? C5 C6 C7 120.0(3) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? S1A O7 S1B 53.97(10) . . ? S1A O7 Tb1 135.46(11) . . ? S1B O7 Tb1 131.57(12) . . ? C2 C7 C6 119.9(3) . . ? C2 C7 H7 120.0 . . ? C6 C7 H7 120.0 . . ? O4 C8 O3 125.6(2) . . ? O4 C8 C9 117.6(2) . . ? O3 C8 C9 116.7(2) . . ? C14 C9 C10 119.6(2) . . ? C14 C9 C8 119.6(2) . . ? C10 C9 C8 120.7(2) . . ? C11 C10 C9 120.1(3) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.0(3) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C12 C13 C14 119.9(3) . . ? C12 C13 H13 120.1 . . ? C14 C13 H13 120.1 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? O6 C15 O5 124.2(2) . . ? O6 C15 C16 118.1(2) . . ? O5 C15 C16 117.7(2) . . ? C21 C16 C17 120.2(2) . . ? C21 C16 C15 119.7(2) . . ? C17 C16 C15 120.1(2) . . ? C16 C17 C18 119.6(3) . . ? C16 C17 H17 120.2 . . ? C18 C17 H17 120.2 . . ? C19 C18 C17 120.1(3) . . ? C19 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C20 C19 C18 120.3(3) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.8(3) . . ? C19 C20 H20 120.1 . . ? C21 C20 H20 120.1 . . ? C16 C21 C20 119.9(3) . . ? C16 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? S1A C22A H22A 109.5 . . ? S1A C22A H22B 109.5 . . ? H22A C22A H22B 109.5 . . ? S1A C22A H22C 109.5 . . ? H22A C22A H22C 109.5 . . ? H22B C22A H22C 109.5 . . ? S1B C22B H22D 109.5 . . ? S1B C22B H22E 109.5 . . ? H22D C22B H22E 109.5 . . ? S1B C22B H22F 109.5 . . ? H22D C22B H22F 109.5 . . ? H22E C22B H22F 109.5 . . ? S1A C23A H23A 109.5 . . ? S1A C23A H23B 109.5 . . ? H23A C23A H23B 109.5 . . ? S1A C23A H23C 109.5 . . ? H23A C23A H23C 109.5 . . ? H23B C23A H23C 109.5 . . ? S1B C23B H23D 109.5 . . ? S1B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? S1B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.484 _refine_diff_density_min -0.436 _refine_diff_density_rms 0.081 # Attachment '2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 649806' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[(aqua)tris(benzoato)(dimethylformamide)yttrium(III)] ; _chemical_name_common '[Y(BA)3(H2O)(DMF)]2' _chemical_melting_point ? _chemical_formula_moiety C48H48N2O16Y2 _chemical_formula_sum 'C48 H48 N2 O16 Y2' _chemical_formula_weight 1086.70 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' 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' Y Y -2.7962 3.5667 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.5806(6) _cell_length_b 8.3012(12) _cell_length_c 24.9731(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.617(6) _cell_angle_gamma 90.00 _cell_volume 2351.6(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.535 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 2.529 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4629 _exptl_absorpt_correction_T_max 0.8840 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 64282 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1135 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6882 _reflns_number_gt 4422 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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. Crystal was non-merohedrally twinned. Deconvoluted with Cell_Now with three components. Refined against HLKF5 file (BASF = 0.333 and 0.228) ; _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^)+(0.0581P)^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 64429 _refine_ls_number_parameters 317 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0502 _refine_ls_wR_factor_ref 0.1230 _refine_ls_wR_factor_gt 0.1128 _refine_ls_goodness_of_fit_ref 0.880 _refine_ls_restrained_S_all 0.880 _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 Y1 Y 0.591109(14) 0.816559(16) 0.056740(5) 0.01203(4) Uani 1 1 d . . . O1 O 0.76884(8) 0.91458(11) 0.12698(4) 0.0164(2) Uani 1 1 d . . . N1 N 0.88172(11) 0.46037(14) 0.05723(5) 0.0189(3) Uani 1 1 d . . . C1 C 0.71817(13) 1.04894(17) 0.12678(5) 0.0131(3) Uani 1 1 d . . . H1O H 0.5274(19) 0.633(2) -0.0412(8) 0.085(9) Uiso 1 1 d . . . O2 O 0.61537(9) 1.07060(11) 0.09823(4) 0.0156(2) Uani 1 1 d . . . C2 C 0.77728(12) 1.18871(17) 0.15924(5) 0.0124(3) Uani 1 1 d . . . H2O H 0.4671(14) 0.7624(18) -0.0526(6) 0.028(5) Uiso 1 1 d . . . O3 O 0.55598(8) 0.73094(10) 0.14197(3) 0.0146(2) Uani 1 1 d . . . C3 C 0.89618(13) 1.18606(19) 0.18199(5) 0.0182(3) Uani 1 1 d . . . H3 H 0.9396 1.0930 0.1797 0.022 Uiso 1 1 calc R . . O4 O 0.46803(8) 0.58688(11) 0.07183(4) 0.0153(2) Uani 1 1 d . . . C4 C 0.95146(14) 1.32027(19) 0.20821(6) 0.0236(4) Uani 1 1 d . . . H4 H 1.0318 1.3178 0.2232 0.028 Uiso 1 1 calc R . . O5 O 0.73119(8) 0.91007(11) 0.00835(4) 0.0175(2) Uani 1 1 d . . . C5 C 0.88663(15) 1.45817(18) 0.21205(6) 0.0260(4) Uani 1 1 d . . . H5 H 0.9238 1.5494 0.2290 0.031 Uiso 1 1 calc R . . O6 O 0.58587(9) 1.05855(11) -0.03751(4) 0.0159(2) Uani 1 1 d . . . C6 C 0.76780(15) 1.46114(18) 0.19091(6) 0.0272(4) Uani 1 1 d . . . H6 H 0.7241 1.5530 0.1946 0.033 Uiso 1 1 calc R . . O7 O 0.71537(9) 0.59997(11) 0.05878(4) 0.0173(2) Uani 1 1 d . . . C7 C 0.71326(13) 1.32797(17) 0.16420(5) 0.0199(3) Uani 1 1 d . . . H7 H 0.6329 1.3311 0.1493 0.024 Uiso 1 1 calc R . . O8 O 0.51796(10) 0.71420(14) -0.03013(4) 0.0168(3) Uani 1 1 d . . . C8 C 0.48668(13) 0.61852(16) 0.12262(6) 0.0127(3) Uani 1 1 d . . . C9 C 0.42568(13) 0.52448(16) 0.16001(5) 0.0137(3) Uani 1 1 d . . . C10 C 0.45045(13) 0.55918(17) 0.21551(6) 0.0198(4) Uani 1 1 d . . . H10 H 0.5060 0.6376 0.2291 0.024 Uiso 1 1 calc R . . C11 C 0.39246(14) 0.47690(18) 0.25069(6) 0.0225(4) Uani 1 1 d . . . H11 H 0.4099 0.4991 0.2880 0.027 Uiso 1 1 calc R . . C12 C 0.30940(14) 0.36286(17) 0.23046(6) 0.0242(4) Uani 1 1 d . . . H12 H 0.2695 0.3094 0.2540 0.029 Uiso 1 1 calc R . . C13 C 0.28455(13) 0.32673(18) 0.17511(6) 0.0237(4) Uani 1 1 d . . . H13 H 0.2291 0.2481 0.1616 0.028 Uiso 1 1 calc R . . C14 C 0.34260(13) 0.40821(16) 0.14000(6) 0.0184(4) Uani 1 1 d . . . H14 H 0.3257 0.3847 0.1028 0.022 Uiso 1 1 calc R . . C15 C 0.68784(14) 0.99783(16) -0.03167(6) 0.0135(3) Uani 1 1 d . . . C16 C 0.76226(13) 1.03414(16) -0.07270(5) 0.0116(3) Uani 1 1 d . . . C17 C 0.88202(13) 1.00412(16) -0.05943(6) 0.0155(4) Uani 1 1 d . . . H17 H 0.9137 0.9511 -0.0270 0.019 Uiso 1 1 calc R . . C18 C 0.95568(14) 1.05244(17) -0.09411(6) 0.0212(4) Uani 1 1 d . . . H18 H 1.0366 1.0363 -0.0842 0.025 Uiso 1 1 calc R . . C19 C 0.90735(15) 1.12467(17) -0.14336(6) 0.0248(4) Uani 1 1 d . . . H19 H 0.9562 1.1575 -0.1667 0.030 Uiso 1 1 calc R . . C20 C 0.78779(15) 1.14830(17) -0.15819(6) 0.0264(4) Uani 1 1 d . . . H20 H 0.7558 1.1939 -0.1919 0.032 Uiso 1 1 calc R . . C21 C 0.71480(14) 1.10451(16) -0.12305(6) 0.0205(4) Uani 1 1 d . . . H21 H 0.6340 1.1220 -0.1330 0.025 Uiso 1 1 calc R . . C22 C 0.82339(14) 0.58354(17) 0.07214(6) 0.0186(4) Uani 1 1 d . . . H22 H 0.8661 0.6626 0.0940 0.022 Uiso 1 1 calc R . . C23 C 1.00857(13) 0.44157(19) 0.07660(6) 0.0291(4) Uani 1 1 d . . . H23A H 1.0347 0.3454 0.0613 0.044 Uiso 0.50 1 calc PR . . H23B H 1.0258 0.4339 0.1158 0.044 Uiso 0.50 1 calc PR . . H23C H 1.0487 0.5330 0.0655 0.044 Uiso 0.50 1 calc PR . . H23D H 1.0381 0.5295 0.1004 0.044 Uiso 0.50 1 calc PR . . H23E H 1.0470 0.4410 0.0459 0.044 Uiso 0.50 1 calc PR . . H23F H 1.0240 0.3419 0.0962 0.044 Uiso 0.50 1 calc PR . . C24 C 0.81961(14) 0.33258(17) 0.02304(6) 0.0267(4) Uani 1 1 d . . . H24A H 0.8753 0.2534 0.0161 0.040 Uiso 0.50 1 calc PR . . H24B H 0.7789 0.3773 -0.0110 0.040 Uiso 0.50 1 calc PR . . H24C H 0.7637 0.2828 0.0415 0.040 Uiso 0.50 1 calc PR . . H24D H 0.7367 0.3556 0.0149 0.040 Uiso 0.50 1 calc PR . . H24E H 0.8330 0.2317 0.0421 0.040 Uiso 0.50 1 calc PR . . H24F H 0.8482 0.3263 -0.0104 0.040 Uiso 0.50 1 calc PR . . 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 Y1 0.01519(8) 0.00745(7) 0.01401(7) -0.00061(7) 0.00423(5) 0.00017(7) O1 0.0190(6) 0.0103(6) 0.0200(5) -0.0019(4) 0.0043(5) 0.0028(5) N1 0.0184(8) 0.0122(7) 0.0255(7) -0.0020(6) 0.0036(6) 0.0028(6) C1 0.0134(9) 0.0128(8) 0.0152(8) 0.0026(7) 0.0077(7) 0.0000(7) O2 0.0155(6) 0.0099(5) 0.0188(5) -0.0017(4) -0.0029(5) 0.0003(5) C2 0.0138(9) 0.0124(8) 0.0106(7) -0.0010(7) 0.0015(6) 0.0004(7) O3 0.0190(6) 0.0091(5) 0.0158(5) -0.0016(4) 0.0036(4) -0.0048(5) C3 0.0181(9) 0.0162(8) 0.0196(8) -0.0029(7) 0.0021(7) 0.0020(8) O4 0.0207(6) 0.0124(6) 0.0137(5) -0.0016(4) 0.0057(5) -0.0031(5) C4 0.0194(9) 0.0237(9) 0.0249(8) 0.0008(8) -0.0021(7) -0.0032(9) O5 0.0221(7) 0.0145(6) 0.0162(5) 0.0028(5) 0.0045(5) -0.0015(5) C5 0.0372(12) 0.0116(9) 0.0232(9) -0.0051(7) -0.0082(8) -0.0046(8) O6 0.0134(6) 0.0108(5) 0.0241(6) -0.0074(4) 0.0053(5) -0.0003(5) C6 0.0355(12) 0.0120(9) 0.0275(9) -0.0054(7) -0.0093(8) 0.0105(8) O7 0.0149(7) 0.0121(6) 0.0248(6) 0.0002(4) 0.0038(5) 0.0034(5) C7 0.0198(9) 0.0153(8) 0.0201(8) -0.0044(7) -0.0068(7) 0.0070(8) O8 0.0239(7) 0.0088(7) 0.0157(6) -0.0009(5) -0.0011(5) 0.0049(5) C8 0.0108(9) 0.0081(8) 0.0192(8) 0.0020(6) 0.0033(7) 0.0057(7) C9 0.0137(9) 0.0083(8) 0.0197(8) 0.0039(6) 0.0049(7) 0.0050(7) C10 0.0250(10) 0.0143(9) 0.0215(8) 0.0019(7) 0.0080(7) 0.0022(7) C11 0.0277(11) 0.0237(9) 0.0175(8) 0.0067(7) 0.0080(7) 0.0072(8) C12 0.0208(10) 0.0222(10) 0.0335(10) 0.0170(7) 0.0142(8) 0.0057(8) C13 0.0186(9) 0.0177(9) 0.0352(9) 0.0051(8) 0.0065(7) -0.0018(8) C14 0.0216(10) 0.0146(9) 0.0195(8) 0.0029(7) 0.0053(7) 0.0026(7) C15 0.0170(10) 0.0067(8) 0.0162(8) -0.0080(6) 0.0014(7) -0.0066(7) C16 0.0151(9) 0.0065(8) 0.0138(7) -0.0012(6) 0.0043(6) 0.0012(6) C17 0.0181(10) 0.0136(8) 0.0157(8) -0.0012(6) 0.0057(7) -0.0003(7) C18 0.0177(10) 0.0202(9) 0.0280(9) -0.0035(7) 0.0098(8) -0.0002(7) C19 0.0364(12) 0.0157(9) 0.0283(9) 0.0022(7) 0.0210(8) 0.0009(8) C20 0.0386(12) 0.0237(10) 0.0200(8) 0.0076(7) 0.0132(8) 0.0133(8) C21 0.0231(10) 0.0169(9) 0.0216(9) -0.0029(7) 0.0052(7) 0.0087(7) C22 0.0253(11) 0.0099(8) 0.0199(8) -0.0021(7) 0.0030(8) -0.0027(8) C23 0.0212(11) 0.0282(10) 0.0370(10) 0.0007(8) 0.0036(8) 0.0046(8) C24 0.0327(11) 0.0166(9) 0.0318(9) -0.0098(8) 0.0087(8) -0.0005(8) _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 Y1 O6 2.2604(10) 3_675 ? Y1 O7 2.2970(10) . ? Y1 O8 2.3250(10) . ? Y1 O2 2.3415(9) . ? Y1 O5 2.3419(9) . ? Y1 O3 2.3558(9) . ? Y1 O4 2.4546(9) . ? Y1 O1 2.5537(9) . ? Y1 C8 2.7701(14) . ? Y1 C1 2.8124(15) . ? Y1 O6 3.0857(10) . ? Y1 Y1 4.3990(4) 3_675 ? O1 C1 1.2598(16) . ? N1 C22 1.3198(17) . ? N1 C24 1.4575(17) . ? N1 C23 1.4595(18) . ? C1 O2 1.2713(16) . ? C1 C2 1.4995(19) . ? C2 C3 1.3798(18) . ? C2 C7 1.3923(18) . ? O3 C8 1.2618(15) . ? C3 C4 1.3825(19) . ? C3 H3 0.9300 . ? O4 C8 1.2707(15) . ? C4 C5 1.383(2) . ? C4 H4 0.9300 . ? O5 C15 1.2567(15) . ? C5 C6 1.371(2) . ? C5 H5 0.9300 . ? O6 C15 1.2651(16) . ? O6 Y1 2.2604(10) 3_675 ? C6 C7 1.3771(19) . ? C6 H6 0.9300 . ? O7 C22 1.2356(16) . ? C7 H7 0.9300 . ? O8 H1O 0.75(2) . ? O8 H2O 0.830(15) . ? C8 C9 1.4985(18) . ? C9 C14 1.3832(19) . ? C9 C10 1.3878(18) . ? C10 C11 1.3883(19) . ? C10 H10 0.9300 . ? C11 C12 1.372(2) . ? C11 H11 0.9300 . ? C12 C13 1.387(2) . ? C12 H12 0.9300 . ? C13 C14 1.3842(19) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 C16 1.4964(18) . ? C16 C17 1.3821(18) . ? C16 C21 1.3950(18) . ? C17 C18 1.3914(18) . ? C17 H17 0.9300 . ? C18 C19 1.381(2) . ? C18 H18 0.9300 . ? C19 C20 1.373(2) . ? C19 H19 0.9300 . ? C20 C21 1.3839(19) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C23 H23D 0.9600 . ? C23 H23E 0.9600 . ? C23 H23F 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24 H24D 0.9600 . ? C24 H24E 0.9600 . ? C24 H24F 0.9600 . ? 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 Y1 O7 154.27(3) 3_675 . ? O6 Y1 O8 79.92(4) 3_675 . ? O7 Y1 O8 81.00(4) . . ? O6 Y1 O2 72.77(3) 3_675 . ? O7 Y1 O2 132.56(4) . . ? O8 Y1 O2 136.95(4) . . ? O6 Y1 O5 115.53(3) 3_675 . ? O7 Y1 O5 76.99(3) . . ? O8 Y1 O5 78.45(4) . . ? O2 Y1 O5 84.03(3) . . ? O6 Y1 O3 90.93(3) 3_675 . ? O7 Y1 O3 88.01(3) . . ? O8 Y1 O3 129.49(4) . . ? O2 Y1 O3 84.21(3) . . ? O5 Y1 O3 146.08(3) . . ? O6 Y1 O4 81.91(3) 3_675 . ? O7 Y1 O4 76.65(3) . . ? O8 Y1 O4 75.26(3) . . ? O2 Y1 O4 130.79(3) . . ? O5 Y1 O4 145.15(3) . . ? O3 Y1 O4 54.25(3) . . ? O6 Y1 O1 124.80(3) 3_675 . ? O7 Y1 O1 79.60(3) . . ? O8 Y1 O1 148.13(4) . . ? O2 Y1 O1 53.19(3) . . ? O5 Y1 O1 72.70(3) . . ? O3 Y1 O1 74.78(3) . . ? O4 Y1 O1 123.69(3) . . ? O6 Y1 C8 85.00(4) 3_675 . ? O7 Y1 C8 82.46(4) . . ? O8 Y1 C8 102.52(4) . . ? O2 Y1 C8 107.43(4) . . ? O5 Y1 C8 159.05(4) . . ? O3 Y1 C8 26.98(3) . . ? O4 Y1 C8 27.30(3) . . ? O1 Y1 C8 99.73(4) . . ? O6 Y1 C1 98.97(4) 3_675 . ? O7 Y1 C1 106.03(4) . . ? O8 Y1 C1 151.37(4) . . ? O2 Y1 C1 26.60(3) . . ? O5 Y1 C1 76.32(3) . . ? O3 Y1 C1 78.98(4) . . ? O4 Y1 C1 133.20(3) . . ? O1 Y1 C1 26.60(3) . . ? C8 Y1 C1 105.90(4) . . ? O6 Y1 O6 70.22(3) 3_675 . ? O7 Y1 O6 116.26(3) . . ? O8 Y1 O6 65.08(3) . . ? O2 Y1 O6 74.54(3) . . ? O5 Y1 O6 45.56(3) . . ? O3 Y1 O6 154.84(3) . . ? O4 Y1 O6 134.42(3) . . ? O1 Y1 O6 101.88(3) . . ? C8 Y1 O6 153.58(3) . . ? C1 Y1 O6 87.44(3) . . ? O6 Y1 Y1 41.31(2) 3_675 3_675 ? O7 Y1 Y1 140.65(2) . 3_675 ? O8 Y1 Y1 67.33(3) . 3_675 ? O2 Y1 Y1 70.17(2) . 3_675 ? O5 Y1 Y1 74.36(2) . 3_675 ? O3 Y1 Y1 130.03(2) . 3_675 ? O4 Y1 Y1 114.75(2) . 3_675 ? O1 Y1 Y1 115.95(2) . 3_675 ? C8 Y1 Y1 125.69(3) . 3_675 ? C1 Y1 Y1 92.80(3) . 3_675 ? O6 Y1 Y1 28.917(18) . 3_675 ? C1 O1 Y1 88.23(8) . . ? C22 N1 C24 120.60(13) . . ? C22 N1 C23 121.83(13) . . ? C24 N1 C23 117.48(12) . . ? O1 C1 O2 120.68(13) . . ? O1 C1 C2 121.42(13) . . ? O2 C1 C2 117.89(12) . . ? O1 C1 Y1 65.17(7) . . ? O2 C1 Y1 55.57(7) . . ? C2 C1 Y1 172.61(10) . . ? C1 O2 Y1 97.83(8) . . ? C3 C2 C7 118.80(13) . . ? C3 C2 C1 121.28(13) . . ? C7 C2 C1 119.81(13) . . ? C8 O3 Y1 95.13(8) . . ? C2 C3 C4 120.71(14) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C8 O4 Y1 90.31(8) . . ? C3 C4 C5 119.59(15) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C15 O5 Y1 113.28(9) . . ? C6 C5 C4 120.33(14) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C15 O6 Y1 173.02(10) . 3_675 ? C15 O6 Y1 77.18(8) . . ? Y1 O6 Y1 109.78(3) 3_675 . ? C5 C6 C7 119.93(14) . . ? C5 C6 H6 120.0 . . ? C7 C6 H6 120.0 . . ? C22 O7 Y1 133.48(9) . . ? C6 C7 C2 120.60(14) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? Y1 O8 H1O 128.6(16) . . ? Y1 O8 H2O 122.0(10) . . ? H1O O8 H2O 108.8(18) . . ? O3 C8 O4 120.15(12) . . ? O3 C8 C9 119.34(12) . . ? O4 C8 C9 120.50(13) . . ? O3 C8 Y1 57.89(7) . . ? O4 C8 Y1 62.39(7) . . ? C9 C8 Y1 174.97(10) . . ? C14 C9 C10 119.63(13) . . ? C14 C9 C8 121.28(12) . . ? C10 C9 C8 119.04(13) . . ? C9 C10 C11 120.07(14) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C12 C11 C10 119.94(14) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 120.39(14) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 119.74(15) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C9 C14 C13 120.22(13) . . ? C9 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? O5 C15 O6 122.47(13) . . ? O5 C15 C16 117.93(13) . . ? O6 C15 C16 119.58(13) . . ? C17 C16 C21 119.06(13) . . ? C17 C16 C15 119.21(12) . . ? C21 C16 C15 121.66(14) . . ? C16 C17 C18 120.68(14) . . ? C16 C17 H17 119.7 . . ? C18 C17 H17 119.7 . . ? C19 C18 C17 119.34(15) . . ? C19 C18 H18 120.3 . . ? C17 C18 H18 120.3 . . ? C20 C19 C18 120.51(14) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? C19 C20 C21 120.19(14) . . ? C19 C20 H20 119.9 . . ? C21 C20 H20 119.9 . . ? C20 C21 C16 120.10(15) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? O7 C22 N1 123.86(14) . . ? O7 C22 H22 118.1 . . ? N1 C22 H22 118.1 . . ? N1 C23 H23A 109.5 . . ? N1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N1 C23 H23D 109.5 . . ? H23A C23 H23D 141.1 . . ? H23B C23 H23D 56.3 . . ? H23C C23 H23D 56.3 . . ? N1 C23 H23E 109.5 . . ? H23A C23 H23E 56.3 . . ? H23B C23 H23E 141.1 . . ? H23C C23 H23E 56.3 . . ? H23D C23 H23E 109.5 . . ? N1 C23 H23F 109.5 . . ? H23A C23 H23F 56.3 . . ? H23B C23 H23F 56.3 . . ? H23C C23 H23F 141.1 . . ? H23D C23 H23F 109.5 . . ? H23E C23 H23F 109.5 . . ? N1 C24 H24A 109.5 . . ? N1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N1 C24 H24D 109.5 . . ? H24A C24 H24D 141.1 . . ? H24B C24 H24D 56.3 . . ? H24C C24 H24D 56.3 . . ? N1 C24 H24E 109.5 . . ? H24A C24 H24E 56.3 . . ? H24B C24 H24E 141.1 . . ? H24C C24 H24E 56.3 . . ? H24D C24 H24E 109.5 . . ? N1 C24 H24F 109.5 . . ? H24A C24 H24F 56.3 . . ? H24B C24 H24F 56.3 . . ? H24C C24 H24F 141.1 . . ? H24D C24 H24F 109.5 . . ? H24E C24 H24F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H1O O4 0.75(2) 1.98(2) 2.7249(15) 173(2) 3_665 O8 H2O O2 0.830(15) 1.922(16) 2.7221(15) 161.6(15) 3_675 C22 H22 O1 0.93 2.59 3.1898(17) 122.9 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.218 _refine_diff_density_min -0.895 _refine_diff_density_rms 0.108 # Attachment '3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 649807' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tri(2-methylbenzoato)yttrium] ; _chemical_name_common '[Y(2-MeBA)3]n' _chemical_melting_point ? _chemical_formula_moiety C24H21O6Y1 _chemical_formula_sum 'C24 H21 O6 Y1' _chemical_formula_weight 494.32 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.0308(3) _cell_length_b 13.9735(6) _cell_length_c 19.0422(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2136.89(15) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.537 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 2.767 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6658 _exptl_absorpt_correction_T_max 0.8090 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 10998 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0743 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.59 _diffrn_reflns_theta_max 27.48 _reflns_number_total 4742 _reflns_number_gt 4172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.004(4) _refine_ls_number_reflns 4742 _refine_ls_number_parameters 283 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0360 _refine_ls_R_factor_gt 0.0279 _refine_ls_wR_factor_ref 0.0594 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 0.803 _refine_ls_restrained_S_all 0.803 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.27247(3) 0.214301(15) -0.006699(12) 0.01302(6) Uani 1 1 d . . . O1 O 0.1615(2) 0.08926(12) 0.06278(9) 0.0215(4) Uani 1 1 d . . . C1 C 0.0464(3) 0.13817(18) 0.08912(13) 0.0162(5) Uani 1 1 d . . . O2 O 0.00730(19) 0.21808(13) 0.05918(8) 0.0160(3) Uani 1 1 d . . . C2 C -0.0379(3) 0.11032(18) 0.15546(13) 0.0159(5) Uani 1 1 d . . . O3 O 0.1298(2) 0.16951(12) -0.10388(9) 0.0199(4) Uani 1 1 d . . . C3 C -0.0292(3) 0.01651(18) 0.18281(14) 0.0189(6) Uani 1 1 d . . . O4 O -0.1126(2) 0.24368(13) -0.09507(9) 0.0244(4) Uani 1 1 d . . . C4 C -0.1092(4) -0.00075(19) 0.24665(14) 0.0232(6) Uani 1 1 d . . . H4 H -0.1058 -0.0633 0.2661 0.028 Uiso 1 1 calc R . . O5 O 0.2014(2) 0.36927(11) -0.01586(9) 0.0210(4) Uani 1 1 d . . . C5 C -0.1930(4) 0.0704(2) 0.28236(14) 0.0258(6) Uani 1 1 d . . . H5 H -0.2462 0.0564 0.3257 0.031 Uiso 1 1 calc R . . O6 O -0.0495(2) 0.40772(12) 0.02255(10) 0.0226(4) Uani 1 1 d . . . C6 C -0.1996(4) 0.1627(2) 0.25502(13) 0.0271(6) Uani 1 1 d . . . H6 H -0.2575 0.2119 0.2793 0.032 Uiso 1 1 calc R . . C7 C -0.1216(3) 0.1817(2) 0.19249(13) 0.0222(6) Uani 1 1 d . . . H7 H -0.1247 0.2448 0.1740 0.027 Uiso 1 1 calc R . . C8 C 0.0561(3) -0.06540(19) 0.14636(15) 0.0248(6) Uani 1 1 d . . . H8A H 0.0381 -0.1244 0.1731 0.037 Uiso 1 1 calc R . . H8B H 0.1758 -0.0523 0.1432 0.037 Uiso 1 1 calc R . . H8C H 0.0101 -0.0728 0.0990 0.037 Uiso 1 1 calc R . . C9 C -0.0062(3) 0.19783(17) -0.12963(13) 0.0185(6) Uani 1 1 d . . . C10 C -0.0469(3) 0.1802(2) -0.20573(13) 0.0210(6) Uani 1 1 d . . . C11 C 0.0187(4) 0.1042(2) -0.24428(16) 0.0254(6) Uani 1 1 d . . . C12 C -0.0283(4) 0.0973(2) -0.31581(15) 0.0328(7) Uani 1 1 d . . . H12 H 0.0138 0.0461 -0.3434 0.039 Uiso 1 1 calc R . . C13 C -0.1327(4) 0.1624(2) -0.34599(16) 0.0363(8) Uani 1 1 d . . . H13 H -0.1611 0.1560 -0.3942 0.044 Uiso 1 1 calc R . . C14 C -0.1984(4) 0.2382(2) -0.30741(15) 0.0353(8) Uani 1 1 d . . . H14 H -0.2709 0.2834 -0.3286 0.042 Uiso 1 1 calc R . . C15 C -0.1553(4) 0.2457(2) -0.23762(14) 0.0280(7) Uani 1 1 d . . . H15 H -0.2001 0.2965 -0.2104 0.034 Uiso 1 1 calc R . . C16 C 0.1306(4) 0.0305(2) -0.21361(16) 0.0358(8) Uani 1 1 d . . . H16A H 0.2379 0.0597 -0.2017 0.054 Uiso 1 1 calc R . . H16B H 0.1480 -0.0209 -0.2478 0.054 Uiso 1 1 calc R . . H16C H 0.0796 0.0041 -0.1711 0.054 Uiso 1 1 calc R . . C17 C 0.0988(3) 0.42776(16) 0.01008(13) 0.0158(5) Uani 1 1 d . . . C18 C 0.1599(3) 0.52597(16) 0.02809(12) 0.0138(5) Uani 1 1 d . . . C19 C 0.0517(3) 0.60238(17) 0.04285(13) 0.0154(5) Uani 1 1 d . . . C20 C 0.1227(3) 0.69070(17) 0.05986(13) 0.0194(6) Uani 1 1 d . . . H20 H 0.0515 0.7436 0.0690 0.023 Uiso 1 1 calc R . . C21 C 0.2927(3) 0.70358(18) 0.06382(13) 0.0230(6) Uani 1 1 d . . . H21 H 0.3371 0.7643 0.0763 0.028 Uiso 1 1 calc R . . C22 C 0.3982(3) 0.6280(2) 0.04961(14) 0.0241(6) Uani 1 1 d . . . H22 H 0.5154 0.6362 0.0526 0.029 Uiso 1 1 calc R . . C23 C 0.3321(3) 0.54058(18) 0.03108(13) 0.0195(6) Uani 1 1 d . . . H23 H 0.4050 0.4892 0.0201 0.023 Uiso 1 1 calc R . . C24 C -0.1350(3) 0.59480(19) 0.04338(14) 0.0221(6) Uani 1 1 d . . . H24A H -0.1702 0.5540 0.0825 0.033 Uiso 1 1 calc R . . H24B H -0.1730 0.5668 -0.0010 0.033 Uiso 1 1 calc R . . H24C H -0.1835 0.6587 0.0490 0.033 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 Y1 0.01133(10) 0.01182(9) 0.01590(11) -0.00166(10) 0.00058(10) 0.00002(8) O1 0.0230(10) 0.0169(9) 0.0245(10) 0.0021(8) 0.0072(8) 0.0028(7) C1 0.0123(13) 0.0181(13) 0.0180(14) -0.0033(10) -0.0028(11) -0.0059(10) O2 0.0149(9) 0.0167(8) 0.0165(9) 0.0034(8) -0.0009(7) -0.0013(7) C2 0.0114(13) 0.0217(13) 0.0147(13) 0.0005(10) -0.0041(10) -0.0002(10) O3 0.0195(10) 0.0225(10) 0.0175(10) -0.0030(8) -0.0024(8) -0.0004(8) C3 0.0176(14) 0.0222(14) 0.0169(14) 0.0018(10) -0.0031(11) -0.0030(11) O4 0.0245(11) 0.0303(11) 0.0183(10) -0.0028(8) 0.0034(9) 0.0057(8) C4 0.0256(17) 0.0237(14) 0.0204(15) 0.0045(11) -0.0044(12) -0.0053(11) O5 0.0246(9) 0.0134(8) 0.0250(10) -0.0006(7) 0.0067(9) 0.0021(7) C5 0.0278(17) 0.0354(16) 0.0142(13) 0.0030(11) 0.0012(12) -0.0049(13) O6 0.0148(9) 0.0134(9) 0.0396(12) -0.0028(8) -0.0018(8) -0.0013(7) C6 0.0322(17) 0.0339(16) 0.0151(13) -0.0011(11) -0.0005(13) 0.0096(13) C7 0.0246(16) 0.0228(14) 0.0193(14) 0.0022(11) -0.0007(12) 0.0050(12) C8 0.0313(17) 0.0175(14) 0.0258(16) 0.0058(11) 0.0024(13) -0.0008(11) C9 0.0225(14) 0.0152(14) 0.0176(13) 0.0002(10) 0.0026(11) -0.0072(10) C10 0.0173(15) 0.0296(15) 0.0162(14) -0.0023(11) 0.0031(12) -0.0079(12) C11 0.0210(15) 0.0277(15) 0.0277(16) -0.0041(12) 0.0050(13) -0.0062(12) C12 0.0307(18) 0.050(2) 0.0180(16) -0.0060(13) 0.0049(13) -0.0117(15) C13 0.0359(19) 0.055(2) 0.0182(16) -0.0043(15) 0.0019(14) -0.0138(16) C14 0.0348(19) 0.0430(19) 0.0283(16) 0.0108(13) -0.0059(14) -0.0043(14) C15 0.0308(17) 0.0317(16) 0.0216(15) -0.0012(12) 0.0002(13) -0.0060(12) C16 0.042(2) 0.0356(18) 0.0303(18) -0.0085(14) 0.0031(15) 0.0023(14) C17 0.0193(13) 0.0140(11) 0.0142(13) 0.0017(10) -0.0011(12) 0.0001(8) C18 0.0164(13) 0.0135(12) 0.0114(13) 0.0001(9) -0.0002(10) 0.0001(9) C19 0.0183(14) 0.0166(13) 0.0113(13) 0.0013(10) 0.0013(11) -0.0012(10) C20 0.0266(15) 0.0143(13) 0.0174(14) 0.0004(10) -0.0015(12) 0.0026(10) C21 0.0320(15) 0.0160(13) 0.0210(13) 0.0002(10) -0.0023(12) -0.0062(12) C22 0.0201(15) 0.0265(15) 0.0255(16) 0.0020(12) -0.0009(12) -0.0079(12) C23 0.0188(14) 0.0206(14) 0.0190(15) 0.0001(10) 0.0024(11) 0.0021(11) C24 0.0194(15) 0.0182(14) 0.0285(15) -0.0014(11) 0.0009(13) 0.0037(11) _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 Y1 O4 2.2253(17) 3 ? Y1 O6 2.2455(16) 3 ? Y1 O5 2.2461(16) . ? Y1 O3 2.2647(17) . ? Y1 O2 2.3341(16) 3 ? Y1 O1 2.3661(17) . ? Y1 O2 2.4721(16) . ? Y1 C1 2.785(3) . ? Y1 Y1 4.1453(2) 3 ? O1 C1 1.254(3) . ? C1 O2 1.293(3) . ? C1 C2 1.485(3) . ? O2 Y1 2.3341(16) 3_455 ? C2 C7 1.394(4) . ? C2 C3 1.412(3) . ? O3 C9 1.261(3) . ? C3 C4 1.396(4) . ? C3 C8 1.504(4) . ? O4 C9 1.255(3) . ? O4 Y1 2.2253(17) 3_455 ? C4 C5 1.380(4) . ? C4 H4 0.9500 . ? O5 C17 1.261(3) . ? C5 C6 1.392(4) . ? C5 H5 0.9500 . ? O6 C17 1.246(3) . ? O6 Y1 2.2455(16) 3_455 ? C6 C7 1.371(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.506(4) . ? C10 C11 1.394(4) . ? C10 C15 1.402(4) . ? C11 C12 1.417(4) . ? C11 C16 1.487(4) . ? C12 C13 1.365(5) . ? C12 H12 0.9500 . ? C13 C14 1.392(4) . ? C13 H13 0.9500 . ? C14 C15 1.377(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.497(3) . ? C18 C23 1.399(4) . ? C18 C19 1.405(3) . ? C19 C20 1.397(3) . ? C19 C24 1.504(4) . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.380(4) . ? C21 H21 0.9500 . ? C22 C23 1.378(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 Y1 O6 93.06(7) 3 3 ? O4 Y1 O5 85.33(6) 3 . ? O6 Y1 O5 152.05(6) 3 . ? O4 Y1 O3 173.89(6) 3 . ? O6 Y1 O3 90.14(6) 3 . ? O5 Y1 O3 94.27(6) . . ? O4 Y1 O2 86.04(6) 3 3 ? O6 Y1 O2 74.66(6) 3 3 ? O5 Y1 O2 77.39(6) . 3 ? O3 Y1 O2 99.83(6) . 3 ? O4 Y1 O1 82.20(6) 3 . ? O6 Y1 O1 75.78(6) 3 . ? O5 Y1 O1 131.27(6) . . ? O3 Y1 O1 93.56(6) . . ? O2 Y1 O1 147.44(6) 3 . ? O4 Y1 O2 84.82(6) 3 . ? O6 Y1 O2 129.26(6) 3 . ? O5 Y1 O2 78.46(6) . . ? O3 Y1 O2 89.13(6) . . ? O2 Y1 O2 154.771(16) 3 . ? O1 Y1 O2 53.66(6) . . ? O4 Y1 C1 78.50(7) 3 . ? O6 Y1 C1 102.30(7) 3 . ? O5 Y1 C1 104.69(7) . . ? O3 Y1 C1 95.74(7) . . ? O2 Y1 C1 164.11(6) 3 . ? O1 Y1 C1 26.62(6) . . ? O2 Y1 C1 27.65(6) . . ? O4 Y1 Y1 58.74(5) 3 3 ? O6 Y1 Y1 64.80(4) 3 3 ? O5 Y1 Y1 91.08(4) . 3 ? O3 Y1 Y1 127.36(5) . 3 ? O2 Y1 Y1 31.38(4) 3 3 ? O1 Y1 Y1 120.55(5) . 3 ? O2 Y1 Y1 142.94(4) . 3 ? C1 Y1 Y1 133.08(5) . 3 ? C1 O1 Y1 95.67(15) . . ? O1 C1 O2 118.3(2) . . ? O1 C1 C2 122.2(2) . . ? O2 C1 C2 119.4(2) . . ? O1 C1 Y1 57.72(13) . . ? O2 C1 Y1 62.58(13) . . ? C2 C1 Y1 162.65(17) . . ? C1 O2 Y1 137.30(16) . 3_455 ? C1 O2 Y1 89.77(14) . . ? Y1 O2 Y1 119.17(6) 3_455 . ? C7 C2 C3 120.1(2) . . ? C7 C2 C1 117.6(2) . . ? C3 C2 C1 122.3(2) . . ? C9 O3 Y1 132.01(16) . . ? C4 C3 C2 117.3(2) . . ? C4 C3 C8 118.7(2) . . ? C2 C3 C8 124.0(2) . . ? C9 O4 Y1 150.94(17) . 3_455 ? C5 C4 C3 121.9(3) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.0 . . ? C17 O5 Y1 139.49(15) . . ? C4 C5 C6 120.1(3) . . ? C4 C5 H5 119.9 . . ? C6 C5 H5 119.9 . . ? C17 O6 Y1 138.89(16) . 3_455 ? C7 C6 C5 119.1(3) . . ? C7 C6 H6 120.4 . . ? C5 C6 H6 120.4 . . ? C6 C7 C2 121.4(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? C3 C8 H8A 109.5 . . ? C3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 O3 123.1(2) . . ? O4 C9 C10 116.1(2) . . ? O3 C9 C10 120.7(2) . . ? C11 C10 C15 120.2(3) . . ? C11 C10 C9 123.3(3) . . ? C15 C10 C9 116.4(2) . . ? C10 C11 C12 117.3(3) . . ? C10 C11 C16 123.3(3) . . ? C12 C11 C16 119.4(3) . . ? C13 C12 C11 121.5(3) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 121.2(3) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C15 C14 C13 118.2(3) . . ? C15 C14 H14 120.9 . . ? C13 C14 H14 120.9 . . ? C14 C15 C10 121.6(3) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? C11 C16 H16A 109.5 . . ? C11 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C11 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 123.6(2) . . ? O6 C17 C18 118.4(2) . . ? O5 C17 C18 118.0(2) . . ? C23 C18 C19 119.5(2) . . ? C23 C18 C17 117.8(2) . . ? C19 C18 C17 122.7(2) . . ? C20 C19 C18 117.8(2) . . ? C20 C19 C24 117.9(2) . . ? C18 C19 C24 124.4(2) . . ? C21 C20 C19 122.1(2) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 119.8(2) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C23 C22 C21 119.5(2) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C18 121.4(2) . . ? C22 C23 H23 119.3 . . ? C18 C23 H23 119.3 . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.400 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.060 # Attachment '4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 649808' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[tris(3-methylbenzoato)(dimethylformamide)yttrium(III)] ; _chemical_name_common SH7DMF _chemical_melting_point ? _chemical_formula_moiety 'C54 H60 N2 O16 Y2' _chemical_formula_sum 'C54 H60 N2 O16 Y2' _chemical_formula_weight 1170.86 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' Y Y -2.7962 3.5667 '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 27.125(5) _cell_length_b 8.6116(17) _cell_length_c 23.062(5) _cell_angle_alpha 90.00 _cell_angle_beta 105.10(3) _cell_angle_gamma 90.00 _cell_volume 5200.8(18) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 2.293 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6570 _exptl_absorpt_correction_T_max 0.8031 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 24782 _diffrn_reflns_av_R_equivalents 0.1552 _diffrn_reflns_av_sigmaI/netI 0.0971 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 34 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5955 _reflns_number_gt 4228 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0574P)^2^+1.6550P] 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 5955 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1323 _refine_ls_wR_factor_gt 0.1168 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.039 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.055278(12) 0.68727(3) 0.046880(16) 0.02054(12) Uani 1 1 d . . . O1 O 0.08868(8) 0.4331(2) 0.06057(10) 0.0205(5) Uani 1 1 d . A . N1 N 0.05249(14) 1.0468(5) 0.18523(17) 0.0529(11) Uani 1 1 d . . . C1 C 0.12185(12) 0.4617(4) 0.10970(14) 0.0209(7) Uani 1 1 d . A . O2 O 0.12305(8) 0.5922(3) 0.13427(11) 0.0272(6) Uani 1 1 d . A . C2 C 0.16041(12) 0.3385(4) 0.13599(15) 0.0219(7) Uani 1 1 d . . . O3 O 0.13276(9) 0.7778(2) 0.03282(14) 0.0315(6) Uani 1 1 d . A . C3 C 0.20640(13) 0.3773(4) 0.17555(15) 0.0273(8) Uani 1 1 d . A . H3 H 0.2127 0.4821 0.1881 0.033 Uiso 1 1 calc R . . O4 O 0.06668(9) 0.9245(3) -0.00892(17) 0.0495(9) Uani 1 1 d . A . C4 C 0.24362(13) 0.2655(5) 0.19732(16) 0.0279(8) Uani 1 1 d . . . O5 O 0.00751(10) 0.5894(3) 0.10744(12) 0.0391(7) Uani 1 1 d . A . C5 C 0.23305(14) 0.1129(4) 0.17927(16) 0.0294(8) Uani 1 1 d . A . H5 H 0.2579 0.0349 0.1941 0.035 Uiso 1 1 calc R . . O6 O -0.03973(10) 0.4190(3) 0.04525(12) 0.0348(6) Uani 1 1 d . . . C6 C 0.18684(14) 0.0720(4) 0.14000(18) 0.0335(9) Uani 1 1 d . . . H6 H 0.1800 -0.0332 0.1283 0.040 Uiso 1 1 calc R A . C7 C 0.15084(13) 0.1861(4) 0.11803(17) 0.0285(8) Uani 1 1 d . A . H7 H 0.1194 0.1594 0.0904 0.034 Uiso 1 1 calc R . . O7A O 0.0576(2) 0.9050(7) 0.1026(3) 0.0238(15) Uani 0.552(9) 1 d P A 1 O7B O 0.0595(3) 0.8615(11) 0.1290(4) 0.0260(18) Uani 0.448(9) 1 d P A 2 O8 O -0.02689(10) 0.7848(3) 0.00392(14) 0.0293(6) Uani 1 1 d . A . C8 C 0.29552(15) 0.3088(5) 0.2367(2) 0.0433(11) Uani 1 1 d . A . H8A H 0.2993 0.4220 0.2374 0.065 Uiso 1 1 calc R . . H8B H 0.3221 0.2616 0.2207 0.065 Uiso 1 1 calc R . . H8C H 0.2988 0.2709 0.2776 0.065 Uiso 1 1 calc R . . C9 C 0.11424(13) 0.8936(4) 0.0008(2) 0.0321(9) Uani 1 1 d . A . C10 C 0.14801(12) 0.9910(3) -0.02552(17) 0.0230(7) Uani 1 1 d . . . C11 C 0.20023(12) 0.9619(3) -0.00914(16) 0.0216(7) Uani 1 1 d . A . H11 H 0.2134 0.8815 0.0188 0.026 Uiso 1 1 calc R . . C12 C 0.23355(13) 1.0486(4) -0.03303(16) 0.0232(7) Uani 1 1 d . . . C13 C 0.21296(14) 1.1664(4) -0.07313(17) 0.0293(8) Uani 1 1 d . A . H13 H 0.2351 1.2288 -0.0891 0.035 Uiso 1 1 calc R . . C14 C 0.16101(14) 1.1952(4) -0.09039(17) 0.0295(8) Uani 1 1 d . . . H14 H 0.1479 1.2755 -0.1184 0.035 Uiso 1 1 calc R A . C15 C 0.12820(13) 1.1076(4) -0.06704(17) 0.0259(8) Uani 1 1 d . A . H15 H 0.0925 1.1264 -0.0791 0.031 Uiso 1 1 calc R . . C16 C 0.28972(13) 1.0130(4) -0.01641(18) 0.0311(8) Uani 1 1 d . A . H16A H 0.2965 0.9293 -0.0421 0.047 Uiso 1 1 calc R . . H16B H 0.3005 0.9803 0.0257 0.047 Uiso 1 1 calc R . . H16C H 0.3088 1.1060 -0.0220 0.047 Uiso 1 1 calc R . . C17 C -0.02996(13) 0.4982(5) 0.09249(16) 0.0297(9) Uani 1 1 d . . . C18 C -0.06400(13) 0.4840(4) 0.13457(15) 0.0265(8) Uani 1 1 d . A . C19 C -0.10626(13) 0.3851(4) 0.12137(16) 0.0270(8) Uani 1 1 d . . . H19 H -0.1143 0.3280 0.0849 0.032 Uiso 1 1 calc R A . C20 C -0.13679(13) 0.3693(4) 0.16146(16) 0.0259(8) Uani 1 1 d . A . C21 C -0.12406(13) 0.4534(4) 0.21440(16) 0.0280(8) Uani 1 1 d . . . H21 H -0.1444 0.4436 0.2421 0.034 Uiso 1 1 calc R A . C22 C -0.08190(13) 0.5521(4) 0.22787(17) 0.0295(8) Uani 1 1 d . A . H22 H -0.0735 0.6083 0.2646 0.035 Uiso 1 1 calc R . . C23 C -0.05232(13) 0.5680(4) 0.18764(16) 0.0293(8) Uani 1 1 d . . . H23 H -0.0239 0.6367 0.1964 0.035 Uiso 1 1 calc R A . C24 C -0.18288(15) 0.2638(5) 0.14719(19) 0.0365(9) Uani 1 1 d . . . H24A H -0.2094 0.3082 0.1141 0.055 Uiso 1 1 calc R A . H24B H -0.1960 0.2534 0.1828 0.055 Uiso 1 1 calc R . . H24C H -0.1731 0.1613 0.1354 0.055 Uiso 1 1 calc R . . C25A C 0.0692(3) 0.9101(8) 0.1580(4) 0.0204(17) Uani 0.552(9) 1 d P A 1 H25A H 0.0882 0.8292 0.1817 0.024 Uiso 0.552(9) 1 calc PR A 1 C25B C 0.0384(3) 0.9878(8) 0.1323(3) 0.021(2) Uani 0.448(9) 1 d P A 2 H25B H 0.0145 1.0353 0.0995 0.025 Uiso 0.448(9) 1 calc PR A 2 C26A C 0.0658(5) 1.0170(13) 0.2565(5) 0.038(3) Uani 0.448(9) 1 d P A 2 H26A H 0.0756 1.1152 0.2778 0.057 Uiso 0.224(5) 1 calc PR A 2 H26B H 0.0941 0.9430 0.2681 0.057 Uiso 0.224(5) 1 calc PR A 2 H26C H 0.0357 0.9745 0.2670 0.057 Uiso 0.224(5) 1 calc PR A 2 H26D H 0.0613 0.9066 0.2642 0.057 Uiso 0.224(5) 1 calc PR A 2 H26E H 0.0428 1.0788 0.2739 0.057 Uiso 0.224(5) 1 calc PR A 2 H26F H 0.1012 1.0473 0.2750 0.057 Uiso 0.224(5) 1 calc PR A 2 H2O H -0.0459(16) 0.732(5) -0.014(2) 0.035(13) Uiso 1 1 d . . . H1O H -0.0383(17) 0.872(6) 0.010(2) 0.058(15) Uiso 1 1 d . . . C26B C 0.0869(4) 1.0366(10) 0.2365(5) 0.047(3) Uani 0.552(9) 1 d P A 1 H26G H 0.1137 1.1138 0.2379 0.070 Uiso 0.552(9) 1 calc PR A 1 H26H H 0.1019 0.9323 0.2407 0.070 Uiso 0.552(9) 1 calc PR A 1 H26I H 0.0710 1.0559 0.2694 0.070 Uiso 0.552(9) 1 calc PR A 1 C27A C 0.0241(3) 1.1536(11) 0.1592(4) 0.043(2) Uani 0.552(9) 1 d P A 1 H27A H 0.0149 1.1353 0.1158 0.065 Uiso 0.552(9) 1 calc PR A 1 H27B H 0.0421 1.2531 0.1680 0.065 Uiso 0.552(9) 1 calc PR A 1 H27C H -0.0069 1.1564 0.1735 0.065 Uiso 0.552(9) 1 calc PR A 1 C27B C 0.0267(4) 1.2304(11) 0.1792(5) 0.029(2) Uani 0.448(9) 1 d P A 2 H27D H 0.0527 1.3063 0.1759 0.044 Uiso 0.448(9) 1 calc PR A 2 H27E H 0.0147 1.2533 0.2149 0.044 Uiso 0.448(9) 1 calc PR A 2 H27F H -0.0021 1.2362 0.1433 0.044 Uiso 0.448(9) 1 calc PR A 2 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 Y1 0.01887(18) 0.01320(15) 0.0337(2) -0.00423(14) 0.01434(13) -0.00109(12) O1 0.0216(11) 0.0200(10) 0.0187(12) 0.0021(10) 0.0030(9) -0.0004(9) N1 0.040(2) 0.088(3) 0.033(2) -0.038(2) 0.0143(17) -0.020(2) C1 0.0194(16) 0.0327(17) 0.0128(16) 0.0037(15) 0.0082(12) -0.0008(14) O2 0.0222(12) 0.0409(14) 0.0183(12) -0.0111(11) 0.0048(9) 0.0039(11) C2 0.0162(16) 0.0369(18) 0.0147(16) 0.0049(15) 0.0078(12) 0.0014(14) O3 0.0211(12) 0.0188(11) 0.0594(19) 0.0143(12) 0.0190(12) 0.0043(9) C3 0.0293(19) 0.0401(19) 0.0147(17) -0.0017(16) 0.0099(14) 0.0073(16) O4 0.0199(14) 0.0173(11) 0.116(3) 0.0237(15) 0.0253(16) 0.0064(10) C4 0.0234(18) 0.045(2) 0.0154(16) -0.0039(17) 0.0051(13) 0.0078(16) O5 0.0242(14) 0.0717(19) 0.0259(14) 0.0145(14) 0.0147(11) 0.0053(14) C5 0.0293(19) 0.0368(19) 0.0228(19) 0.0117(17) 0.0080(15) 0.0079(16) O6 0.0361(15) 0.0516(16) 0.0222(14) 0.0117(13) 0.0175(11) 0.0199(12) C6 0.037(2) 0.0316(18) 0.032(2) 0.0145(18) 0.0082(17) -0.0043(17) C7 0.0237(18) 0.0346(19) 0.0259(19) 0.0129(17) 0.0044(14) -0.0018(15) O7A 0.027(3) 0.020(3) 0.027(4) -0.005(2) 0.011(3) 0.000(2) O7B 0.031(4) 0.023(4) 0.026(6) -0.013(3) 0.009(4) 0.000(3) O8 0.0190(13) 0.0181(12) 0.0510(19) -0.0015(13) 0.0093(12) 0.0006(11) C8 0.031(2) 0.050(2) 0.041(2) -0.016(2) -0.0051(17) 0.0161(19) C9 0.0213(18) 0.0182(16) 0.060(3) 0.0061(17) 0.0157(17) 0.0003(14) C10 0.0220(17) 0.0140(14) 0.034(2) -0.0002(15) 0.0099(14) -0.0007(13) C11 0.0249(18) 0.0160(14) 0.0266(18) 0.0028(14) 0.0112(14) 0.0015(13) C12 0.0273(18) 0.0192(15) 0.0282(19) -0.0037(15) 0.0164(15) -0.0033(13) C13 0.040(2) 0.0239(16) 0.033(2) 0.0058(16) 0.0249(17) 0.0029(15) C14 0.040(2) 0.0261(17) 0.0266(19) 0.0098(16) 0.0158(16) 0.0104(16) C15 0.0268(18) 0.0221(16) 0.030(2) 0.0005(15) 0.0086(15) 0.0044(14) C16 0.0264(19) 0.0326(18) 0.040(2) 0.0077(18) 0.0185(17) -0.0009(15) C17 0.0260(19) 0.049(2) 0.0183(18) 0.0197(18) 0.0134(15) 0.0206(18) C18 0.0235(18) 0.042(2) 0.0185(17) 0.0109(16) 0.0131(14) 0.0144(16) C19 0.0278(19) 0.0387(19) 0.0185(17) 0.0064(16) 0.0128(14) 0.0111(16) C20 0.0268(18) 0.0303(17) 0.0250(19) 0.0093(16) 0.0145(15) 0.0103(15) C21 0.0301(19) 0.0371(19) 0.0236(19) 0.0080(17) 0.0191(15) 0.0082(16) C22 0.031(2) 0.040(2) 0.0210(18) 0.0039(17) 0.0136(15) 0.0069(17) C23 0.0213(17) 0.045(2) 0.0235(19) 0.0079(18) 0.0097(14) 0.0050(16) C24 0.039(2) 0.042(2) 0.035(2) -0.0009(19) 0.0214(18) -0.0039(18) C25A 0.025(4) 0.014(3) 0.024(4) 0.001(3) 0.009(3) -0.002(3) C25B 0.028(5) 0.017(3) 0.021(4) 0.000(3) 0.010(3) 0.001(3) C26A 0.061(8) 0.033(5) 0.025(5) -0.005(4) 0.018(5) 0.008(5) C26B 0.049(6) 0.032(4) 0.046(6) -0.007(4) -0.012(5) 0.012(4) C27A 0.063(6) 0.041(5) 0.026(4) 0.002(4) 0.012(4) 0.025(4) C27B 0.048(6) 0.015(4) 0.027(5) -0.001(4) 0.014(4) 0.012(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 Y1 O6 2.250(3) 5_565 ? Y1 O7A 2.264(6) . ? Y1 O5 2.298(3) . ? Y1 O3 2.342(2) . ? Y1 O8 2.346(3) . ? Y1 O1 2.358(2) . ? Y1 O7B 2.394(9) . ? Y1 O4 2.476(3) . ? Y1 O2 2.486(2) . ? Y1 C9 2.780(3) . ? Y1 C1 2.788(3) . ? O1 C1 1.274(4) . ? N1 C27A 1.248(9) . ? N1 C25B 1.286(8) . ? N1 C26B 1.305(9) . ? N1 C25A 1.462(8) . ? N1 C26A 1.610(11) . ? N1 C27B 1.720(9) . ? C1 O2 1.255(4) . ? C1 C2 1.502(5) . ? C2 C7 1.380(5) . ? C2 C3 1.381(5) . ? O3 C9 1.264(4) . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? O4 C9 1.278(4) . ? C4 C5 1.386(5) . ? C4 C8 1.510(5) . ? O5 C17 1.259(5) . ? C5 C6 1.387(5) . ? C5 H5 0.9500 . ? O6 C17 1.254(4) . ? O6 Y1 2.250(3) 5_565 ? C6 C7 1.385(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O7A C25A 1.234(11) . ? O7B C25B 1.242(11) . ? O8 H2O 0.73(5) . ? O8 H1O 0.84(5) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.484(5) . ? C10 C11 1.391(4) . ? C10 C15 1.395(5) . ? C11 C12 1.392(4) . ? C11 H11 0.9500 . ? C12 C13 1.388(5) . ? C12 C16 1.503(5) . ? C13 C14 1.383(5) . ? C13 H13 0.9500 . ? C14 C15 1.379(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.509(5) . ? C18 C23 1.385(5) . ? C18 C19 1.397(5) . ? C19 C20 1.399(5) . ? C19 H19 0.9500 . ? C20 C21 1.383(5) . ? C20 C24 1.511(5) . ? C21 C22 1.394(5) . ? C21 H21 0.9500 . ? C22 C23 1.382(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25A H25A 0.9500 . ? C25B H25B 0.9500 . ? C26A H26A 0.9800 . ? C26A H26B 0.9800 . ? C26A H26C 0.9800 . ? C26A H26D 0.9800 . ? C26A H26E 0.9800 . ? C26A H26F 0.9800 . ? C26B H26G 0.9800 . ? C26B H26H 0.9800 . ? C26B H26I 0.9800 . ? C27A H27A 0.9800 . ? C27A H27B 0.9800 . ? C27A H27C 0.9800 . ? C27B H27D 0.9800 . ? C27B H27E 0.9800 . ? C27B H27F 0.9800 . ? 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 Y1 O7A 147.47(19) 5_565 . ? O6 Y1 O5 115.33(10) 5_565 . ? O7A Y1 O5 84.01(18) . . ? O6 Y1 O3 87.64(10) 5_565 . ? O7A Y1 O3 84.84(17) . . ? O5 Y1 O3 150.98(10) . . ? O6 Y1 O8 79.81(10) 5_565 . ? O7A Y1 O8 79.97(17) . . ? O5 Y1 O8 76.35(10) . . ? O3 Y1 O8 127.63(9) . . ? O6 Y1 O1 73.73(8) 5_565 . ? O7A Y1 O1 137.71(18) . . ? O5 Y1 O1 80.56(9) . . ? O3 Y1 O1 90.00(7) . . ? O8 Y1 O1 132.71(9) . . ? O6 Y1 O7B 163.7(2) 5_565 . ? O7A Y1 O7B 17.11(18) . . ? O5 Y1 O7B 70.6(2) . . ? O3 Y1 O7B 92.3(2) . . ? O8 Y1 O7B 87.4(2) . . ? O1 Y1 O7B 122.5(2) . . ? O6 Y1 O4 82.12(11) 5_565 . ? O7A Y1 O4 67.9(2) . . ? O5 Y1 O4 141.72(10) . . ? O3 Y1 O4 54.23(8) . . ? O8 Y1 O4 73.67(9) . . ? O1 Y1 O4 137.68(9) . . ? O7B Y1 O4 84.7(2) . . ? O6 Y1 O2 123.26(8) 5_565 . ? O7A Y1 O2 84.71(18) . . ? O5 Y1 O2 78.55(9) . . ? O3 Y1 O2 73.80(9) . . ? O8 Y1 O2 151.73(9) . . ? O1 Y1 O2 53.75(8) . . ? O7B Y1 O2 72.1(2) . . ? O4 Y1 O2 121.79(9) . . ? O6 Y1 C9 83.36(11) 5_565 . ? O7A Y1 C9 75.75(18) . . ? O5 Y1 C9 159.73(11) . . ? O3 Y1 C9 26.88(9) . . ? O8 Y1 C9 100.82(10) . . ? O1 Y1 C9 113.90(9) . . ? O7B Y1 C9 89.3(2) . . ? O4 Y1 C9 27.37(9) . . ? O2 Y1 C9 98.20(10) . . ? O6 Y1 C1 98.27(9) 5_565 . ? O7A Y1 C1 111.35(18) . . ? O5 Y1 C1 79.63(9) . . ? O3 Y1 C1 79.67(9) . . ? O8 Y1 C1 152.19(9) . . ? O1 Y1 C1 27.05(9) . . ? O7B Y1 C1 97.7(2) . . ? O4 Y1 C1 133.89(8) . . ? O2 Y1 C1 26.76(8) . . ? C9 Y1 C1 106.54(10) . . ? C1 O1 Y1 95.61(19) . . ? C27A N1 C25B 80.9(6) . . ? C27A N1 C26B 133.8(7) . . ? C25B N1 C26B 143.1(7) . . ? C27A N1 C25A 127.5(6) . . ? C26B N1 C25A 96.1(6) . . ? C27A N1 C26A 123.7(7) . . ? C25B N1 C26A 147.1(6) . . ? C25A N1 C26A 107.4(6) . . ? C25B N1 C27B 105.8(6) . . ? C26B N1 C27B 108.4(6) . . ? C25A N1 C27B 150.6(5) . . ? C26A N1 C27B 102.0(6) . . ? O2 C1 O1 120.2(3) . . ? O2 C1 C2 121.1(3) . . ? O1 C1 C2 118.6(3) . . ? O2 C1 Y1 63.11(17) . . ? O1 C1 Y1 57.35(16) . . ? C2 C1 Y1 172.1(2) . . ? C1 O2 Y1 90.13(19) . . ? C7 C2 C3 119.7(3) . . ? C7 C2 C1 119.6(3) . . ? C3 C2 C1 120.7(3) . . ? C9 O3 Y1 96.2(2) . . ? C2 C3 C4 121.1(4) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? C9 O4 Y1 89.7(2) . . ? C5 C4 C3 118.3(3) . . ? C5 C4 C8 120.2(3) . . ? C3 C4 C8 121.4(4) . . ? C17 O5 Y1 127.2(2) . . ? C4 C5 C6 121.2(3) . . ? C4 C5 H5 119.4 . . ? C6 C5 H5 119.4 . . ? C17 O6 Y1 170.7(2) . 5_565 ? C7 C6 C5 119.3(3) . . ? C7 C6 H6 120.3 . . ? C5 C6 H6 120.3 . . ? C2 C7 C6 120.4(3) . . ? C2 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C25A O7A Y1 125.3(5) . . ? C25B O7B Y1 132.1(7) . . ? Y1 O8 H2O 118(3) . . ? Y1 O8 H1O 127(3) . . ? H2O O8 H1O 114(5) . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O4 119.8(3) . . ? O3 C9 C10 119.4(3) . . ? O4 C9 C10 120.8(3) . . ? O3 C9 Y1 56.88(17) . . ? O4 C9 Y1 62.97(18) . . ? C10 C9 Y1 174.7(2) . . ? C11 C10 C15 120.0(3) . . ? C11 C10 C9 118.7(3) . . ? C15 C10 C9 121.3(3) . . ? C10 C11 C12 121.1(3) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 117.8(3) . . ? C13 C12 C16 121.6(3) . . ? C11 C12 C16 120.6(3) . . ? C14 C13 C12 121.7(3) . . ? C14 C13 H13 119.1 . . ? C12 C13 H13 119.1 . . ? C15 C14 C13 120.1(3) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 119.3(3) . . ? C14 C15 H15 120.3 . . ? C10 C15 H15 120.3 . . ? C12 C16 H16A 109.5 . . ? C12 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C12 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O6 C17 O5 123.4(3) . . ? O6 C17 C18 119.3(4) . . ? O5 C17 C18 117.4(3) . . ? C23 C18 C19 119.8(3) . . ? C23 C18 C17 119.3(3) . . ? C19 C18 C17 120.9(3) . . ? C18 C19 C20 120.6(3) . . ? C18 C19 H19 119.7 . . ? C20 C19 H19 119.7 . . ? C21 C20 C19 118.5(3) . . ? C21 C20 C24 120.6(3) . . ? C19 C20 C24 120.9(3) . . ? C20 C21 C22 121.2(3) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 119.8(4) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.1(3) . . ? C22 C23 H23 119.9 . . ? C18 C23 H23 119.9 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O7A C25A N1 116.7(6) . . ? O7A C25A H25A 121.7 . . ? N1 C25A H25A 121.7 . . ? O7B C25B N1 112.1(8) . . ? O7B C25B H25B 123.9 . . ? N1 C25B H25B 123.9 . . ? N1 C26A H26A 109.5 . . ? N1 C26A H26B 109.5 . . ? H26A C26A H26B 109.5 . . ? N1 C26A H26C 109.5 . . ? H26A C26A H26C 109.5 . . ? H26B C26A H26C 109.5 . . ? N1 C26A H26D 109.5 . . ? H26A C26A H26D 141.1 . . ? H26B C26A H26D 56.3 . . ? H26C C26A H26D 56.3 . . ? N1 C26A H26E 109.5 . . ? H26A C26A H26E 56.3 . . ? H26B C26A H26E 141.1 . . ? H26C C26A H26E 56.3 . . ? H26D C26A H26E 109.5 . . ? N1 C26A H26F 109.5 . . ? H26A C26A H26F 56.3 . . ? H26B C26A H26F 56.3 . . ? H26C C26A H26F 141.1 . . ? H26D C26A H26F 109.5 . . ? H26E C26A H26F 109.5 . . ? N1 C26B H26G 109.5 . . ? N1 C26B H26H 109.5 . . ? N1 C26B H26I 109.5 . . ? N1 C27A H27A 109.5 . . ? N1 C27A H27B 109.5 . . ? N1 C27A H27C 109.5 . . ? N1 C27B H27D 109.5 . . ? N1 C27B H27E 109.5 . . ? H27D C27B H27E 109.5 . . ? N1 C27B H27F 109.5 . . ? H27D C27B H27F 109.5 . . ? H27E C27B H27F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H2O O1 0.73(5) 1.97(5) 2.691(4) 171(4) 5_565 O8 H1O O4 0.84(5) 1.91(5) 2.741(4) 170(5) 5_575 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.342 _refine_diff_density_min -1.815 _refine_diff_density_rms 0.115 # Attachment '5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 649809' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[(aqua)(dimethylsulphoxide)tris(3-methylbenzoate)yttrium (III)].dmso solvate ; _chemical_name_common '[Y(3-MeBA)3(DMSO)(H2O)]2.2DMSO' _chemical_melting_point ? _chemical_formula_moiety 'C52 H58 O16 S2 Y2,2(C2 O1 H6 S1)' _chemical_formula_sum 'C56 H70 O18 S4 Y2' _chemical_formula_weight 1337.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 '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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5731(17) _cell_length_b 12.059(2) _cell_length_c 16.072(3) _cell_angle_alpha 106.75(3) _cell_angle_beta 96.04(2) _cell_angle_gamma 102.04(3) _cell_volume 1531.6(6) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.089 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.6433 _exptl_absorpt_correction_T_max 0.7164 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD' _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 19635 _diffrn_reflns_av_R_equivalents 0.0639 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.82 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6991 _reflns_number_gt 6041 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0620P)^2^+1.1282P] 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 6991 _refine_ls_number_parameters 459 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1127 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Y1 Y 0.65003(3) 0.37864(2) 0.426560(16) 0.01214(9) Uani 1 1 d . . . S1 S 0.87001(8) 0.22641(7) 0.52916(5) 0.02003(16) Uani 1 1 d . . . O1 O 0.8879(2) 0.46200(17) 0.37225(12) 0.0167(4) Uani 1 1 d . . . C1 C 0.8253(3) 0.3962(2) 0.29312(18) 0.0147(5) Uani 1 1 d . . . H2O H 0.770(4) 0.593(3) 0.581(2) 0.020(8) Uiso 1 1 d . . . O2 O 0.6876(2) 0.32477(17) 0.27679(12) 0.0183(4) Uani 1 1 d . . . C2 C 0.9141(3) 0.4076(3) 0.21927(18) 0.0173(5) Uani 1 1 d . . . S2A S 0.32848(15) 0.13535(14) 0.04965(8) 0.0497(5) Uani 0.893(4) 1 d P A 1 H1O H 0.894(5) 0.542(3) 0.574(2) 0.027(9) Uiso 1 1 d . . . O3 O 0.5022(2) 0.16834(18) 0.36680(14) 0.0225(4) Uani 1 1 d . B . C3 C 0.8522(3) 0.3303(3) 0.13425(19) 0.0204(6) Uani 1 1 d . . . H3 H 0.7567 0.2682 0.1239 0.024 Uiso 1 1 calc R . . O4 O 0.3651(2) 0.30412(17) 0.37071(13) 0.0189(4) Uani 1 1 d . B . C4 C 0.9290(4) 0.3429(3) 0.06352(19) 0.0244(6) Uani 1 1 d . . . O5 O 0.5667(2) 0.53638(17) 0.40874(13) 0.0181(4) Uani 1 1 d . . . C5 C 1.0669(4) 0.4366(3) 0.0813(2) 0.0290(7) Uani 1 1 d . . . H5 H 1.1190 0.4481 0.0340 0.035 Uiso 1 1 calc R . . O6 O 0.4391(2) 0.67832(18) 0.45642(12) 0.0192(4) Uani 1 1 d . . . C6 C 1.1299(4) 0.5131(3) 0.1661(2) 0.0308(7) Uani 1 1 d . . . H6 H 1.2249 0.5757 0.1765 0.037 Uiso 1 1 calc R . . O7 O 0.8476(2) 0.28861(18) 0.46068(13) 0.0200(4) Uani 1 1 d . . . C7 C 1.0548(3) 0.4987(3) 0.2358(2) 0.0238(6) Uani 1 1 d . . . H7 H 1.0986 0.5502 0.2943 0.029 Uiso 1 1 calc R . . O8 O 0.8031(2) 0.53482(19) 0.55066(13) 0.0190(4) Uani 1 1 d . . . C8 C 0.8620(5) 0.2589(4) -0.0286(2) 0.0406(9) Uani 1 1 d . . . H8A H 0.8771 0.3030 -0.0709 0.061 Uiso 1 1 calc R . . H8B H 0.7462 0.2237 -0.0335 0.061 Uiso 1 1 calc R . . H8C H 0.9191 0.1951 -0.0415 0.061 Uiso 1 1 calc R . . O9 O 0.4650(4) 0.1742(3) 0.00727(19) 0.0563(8) Uani 1 1 d . . . C9 C 0.3703(3) 0.1949(3) 0.35385(18) 0.0202(6) Uani 1 1 d . . . C10A C 0.2239(7) 0.0940(5) 0.3195(3) 0.0163(11) Uani 0.777(7) 1 d P B 1 C10B C 0.196(2) 0.1177(16) 0.3064(12) 0.010(4) Uani 0.223(7) 1 d PU B 2 C11A C 0.0786(5) 0.1140(4) 0.2868(3) 0.0194(10) Uani 0.777(7) 1 d P B 1 H11A H 0.0750 0.1936 0.2909 0.023 Uiso 0.777(7) 1 calc PR B 1 C11B C 0.177(2) -0.0010(14) 0.2980(10) 0.018(3) Uani 0.223(7) 1 d PU B 2 H11B H 0.2654 -0.0267 0.3201 0.022 Uiso 0.223(7) 1 calc PR B 2 C12A C -0.0608(5) 0.0229(6) 0.2484(3) 0.0207(10) Uani 0.777(7) 1 d P B 1 C12B C 0.025(3) -0.0875(18) 0.2565(11) 0.025(5) Uani 0.223(7) 1 d P B 2 C13A C -0.0499(8) -0.0931(5) 0.2432(3) 0.0248(11) Uani 0.777(7) 1 d P B 1 H13A H -0.1423 -0.1581 0.2164 0.030 Uiso 0.777(7) 1 calc PR B 1 C13B C -0.097(3) -0.041(3) 0.2290(16) 0.044(6) Uani 0.223(7) 1 d P B 2 H13B H -0.1981 -0.0952 0.1992 0.053 Uiso 0.223(7) 1 calc PR B 2 C14A C 0.0927(6) -0.1158(4) 0.2760(3) 0.0249(10) Uani 0.777(7) 1 d P B 1 H14A H 0.0962 -0.1952 0.2726 0.030 Uiso 0.777(7) 1 calc PR B 1 C14B C -0.085(2) 0.083(2) 0.2419(16) 0.055(6) Uani 0.223(7) 1 d P B 2 H14B H -0.1720 0.1129 0.2233 0.066 Uiso 0.223(7) 1 calc PR B 2 C15A C 0.2290(6) -0.0229(4) 0.3136(3) 0.0197(9) Uani 0.777(7) 1 d P B 1 H15A H 0.3267 -0.0385 0.3355 0.024 Uiso 0.777(7) 1 calc PR B 1 C15B C 0.0710(13) 0.1581(9) 0.2853(6) 0.023(4) Uani 0.223(7) 1 d PU B 2 H15B H 0.0859 0.2422 0.3000 0.027 Uiso 0.223(7) 1 calc PR B 2 S2B S 0.2729(13) 0.1842(9) 0.0296(6) 0.055(4) Uani 0.107(4) 1 d PR A 2 C16A C -0.2159(5) 0.0473(4) 0.2140(3) 0.0311(11) Uani 0.777(7) 1 d P B 1 H16A H -0.2754 0.0701 0.2624 0.047 Uiso 0.777(7) 1 calc PR B 1 H16B H -0.2825 -0.0249 0.1682 0.047 Uiso 0.777(7) 1 calc PR B 1 H16C H -0.1910 0.1126 0.1888 0.047 Uiso 0.777(7) 1 calc PR B 1 C16B C 0.004(2) -0.2156(13) 0.2417(11) 0.038(4) Uani 0.223(7) 1 d P B 2 H16D H -0.0631 -0.2402 0.2822 0.058 Uiso 0.223(7) 1 calc PR B 2 H16E H 0.1102 -0.2321 0.2525 0.058 Uiso 0.223(7) 1 calc PR B 2 H16F H -0.0490 -0.2604 0.1806 0.058 Uiso 0.223(7) 1 calc PR B 2 C17 C 0.5080(3) 0.6211(2) 0.39981(17) 0.0139(5) Uani 1 1 d . . . C18 C 0.5214(3) 0.6556(2) 0.31762(17) 0.0149(5) Uani 1 1 d . . . C19 C 0.5793(3) 0.5871(3) 0.24819(18) 0.0201(6) Uani 1 1 d . . . H19 H 0.6125 0.5186 0.2533 0.024 Uiso 1 1 calc R . . C20 C 0.5896(3) 0.6174(3) 0.17067(19) 0.0227(6) Uani 1 1 d . . . C21 C 0.5380(3) 0.7168(3) 0.1643(2) 0.0240(6) Uani 1 1 d . . . H21 H 0.5420 0.7378 0.1118 0.029 Uiso 1 1 calc R . . C22 C 0.4808(4) 0.7859(3) 0.2333(2) 0.0276(7) Uani 1 1 d . . . H22 H 0.4466 0.8539 0.2279 0.033 Uiso 1 1 calc R . . C23 C 0.4731(3) 0.7564(3) 0.3108(2) 0.0218(6) Uani 1 1 d . . . H23 H 0.4353 0.8045 0.3584 0.026 Uiso 1 1 calc R . . C24 C 0.6590(5) 0.5454(4) 0.0975(2) 0.0395(9) Uani 1 1 d . . . H24A H 0.6416 0.5709 0.0453 0.059 Uiso 1 1 calc R . . H24B H 0.6053 0.4603 0.0826 0.059 Uiso 1 1 calc R . . H24C H 0.7755 0.5580 0.1168 0.059 Uiso 1 1 calc R . . C25 C 1.0795(4) 0.2277(3) 0.5414(2) 0.0302(7) Uani 1 1 d . . . H25A H 1.1446 0.3090 0.5738 0.045 Uiso 1 1 calc R . . H25B H 1.1093 0.2011 0.4830 0.045 Uiso 1 1 calc R . . H25C H 1.0998 0.1736 0.5743 0.045 Uiso 1 1 calc R . . C26 C 0.7852(5) 0.0720(3) 0.4701(3) 0.0429(9) Uani 1 1 d . . . H26A H 0.6668 0.0562 0.4581 0.064 Uiso 1 1 calc R . . H26B H 0.8166 0.0237 0.5056 0.064 Uiso 1 1 calc R . . H26C H 0.8255 0.0511 0.4143 0.064 Uiso 1 1 calc R . . C27 C 0.4017(6) 0.0594(4) 0.1201(3) 0.0455(11) Uani 0.893(4) 1 d P A 1 H27A H 0.4170 -0.0170 0.0840 0.068 Uiso 0.893(4) 1 calc PR A 1 H27B H 0.3227 0.0444 0.1581 0.068 Uiso 0.893(4) 1 calc PR A 1 H27C H 0.5053 0.1090 0.1569 0.068 Uiso 0.893(4) 1 calc PR A 1 C28A C 0.3191(6) 0.2592(6) 0.1356(4) 0.098(5) Uani 0.893(4) 1 d P A 1 H28A H 0.2800 0.3162 0.1113 0.147 Uiso 0.893(4) 1 calc PR A 1 H28B H 0.4272 0.2977 0.1714 0.147 Uiso 0.893(4) 1 calc PR A 1 H28C H 0.2446 0.2335 0.1726 0.147 Uiso 0.893(4) 1 calc PR A 1 C28B C 0.3191(6) 0.2592(6) 0.1356(4) 0.05(2) Uani 0.107(4) 1 d P A 2 H28D H 0.3938 0.3369 0.1449 0.078 Uiso 0.107(4) 1 calc PR A 2 H28E H 0.3707 0.2139 0.1669 0.078 Uiso 0.107(4) 1 calc PR A 2 H28F H 0.2201 0.2715 0.1583 0.078 Uiso 0.107(4) 1 calc PR A 2 C29 C 0.155(5) 0.067(4) 0.024(3) 0.060(12) Uani 0.107(4) 1 d P A 2 H29A H 0.1215 0.0169 -0.0382 0.090 Uiso 0.107(4) 1 calc PR A 2 H29B H 0.0599 0.0845 0.0484 0.090 Uiso 0.107(4) 1 calc PR A 2 H29C H 0.2087 0.0251 0.0572 0.090 Uiso 0.107(4) 1 calc PR A 2 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 Y1 0.01084(13) 0.01507(14) 0.01348(13) 0.00752(10) 0.00329(9) 0.00483(9) S1 0.0201(3) 0.0254(4) 0.0221(4) 0.0138(3) 0.0058(3) 0.0120(3) O1 0.0134(8) 0.0240(10) 0.0146(9) 0.0079(8) 0.0040(7) 0.0054(8) C1 0.0129(12) 0.0167(13) 0.0191(13) 0.0092(11) 0.0046(10) 0.0077(10) O2 0.0170(9) 0.0205(10) 0.0167(9) 0.0056(8) 0.0053(7) 0.0023(8) C2 0.0160(12) 0.0234(15) 0.0198(14) 0.0122(11) 0.0072(10) 0.0112(11) S2A 0.0381(6) 0.0727(10) 0.0299(6) 0.0187(6) 0.0001(5) -0.0046(6) O3 0.0221(10) 0.0200(11) 0.0278(11) 0.0089(9) 0.0096(8) 0.0060(8) C3 0.0192(13) 0.0240(15) 0.0219(14) 0.0100(12) 0.0069(11) 0.0083(11) O4 0.0133(9) 0.0208(10) 0.0206(10) 0.0048(8) 0.0016(7) 0.0033(8) C4 0.0283(15) 0.0337(17) 0.0162(14) 0.0093(12) 0.0082(11) 0.0144(13) O5 0.0176(9) 0.0208(10) 0.0213(10) 0.0137(8) 0.0022(7) 0.0071(8) C5 0.0235(15) 0.050(2) 0.0230(15) 0.0203(15) 0.0126(12) 0.0138(14) O6 0.0204(9) 0.0259(11) 0.0191(10) 0.0140(8) 0.0091(8) 0.0099(8) C6 0.0184(14) 0.049(2) 0.0287(17) 0.0207(15) 0.0076(12) 0.0017(13) O7 0.0192(9) 0.0234(11) 0.0249(10) 0.0149(9) 0.0055(8) 0.0106(8) C7 0.0192(13) 0.0348(17) 0.0185(14) 0.0121(13) 0.0030(11) 0.0044(12) O8 0.0123(9) 0.0247(11) 0.0183(10) 0.0026(8) 0.0005(8) 0.0081(8) C8 0.055(2) 0.045(2) 0.0202(16) 0.0070(15) 0.0142(15) 0.0120(18) O9 0.070(2) 0.070(2) 0.0399(16) 0.0316(15) 0.0224(14) 0.0153(16) C9 0.0216(14) 0.0203(15) 0.0154(13) 0.0031(11) 0.0070(10) 0.0001(11) C10A 0.019(3) 0.019(3) 0.015(2) 0.0098(18) 0.0059(17) 0.0076(19) C10B 0.008(6) 0.009(5) 0.009(5) 0.000(4) -0.004(4) -0.001(4) C11A 0.025(2) 0.011(2) 0.023(2) 0.0056(16) 0.0061(16) 0.0037(17) C11B 0.021(5) 0.015(5) 0.019(5) 0.007(4) 0.002(4) 0.005(4) C12A 0.021(2) 0.018(3) 0.023(2) 0.008(2) 0.0015(17) 0.005(2) C12B 0.010(9) 0.041(11) 0.022(8) 0.014(7) -0.006(8) -0.001(9) C13A 0.018(3) 0.016(3) 0.035(3) 0.0045(19) -0.004(2) 0.002(2) C13B 0.027(11) 0.029(13) 0.065(14) -0.002(12) 0.011(9) 0.008(11) C14A 0.025(2) 0.015(2) 0.033(2) 0.0099(17) -0.0005(19) 0.0037(17) C14B 0.035(11) 0.048(13) 0.105(19) 0.044(13) 0.017(10) 0.026(10) C15A 0.019(2) 0.018(2) 0.025(2) 0.0113(16) 0.0010(16) 0.0065(17) C15B 0.014(5) 0.020(6) 0.027(5) 0.001(4) 0.003(4) -0.001(4) S2B 0.075(8) 0.061(7) 0.039(6) 0.029(5) -0.002(5) 0.029(6) C16A 0.019(2) 0.024(2) 0.046(3) 0.0109(19) -0.0054(17) 0.0018(16) C16B 0.042(9) 0.026(9) 0.034(9) 0.001(7) 0.014(7) -0.010(7) C17 0.0087(11) 0.0171(13) 0.0169(13) 0.0092(10) 0.0009(9) 0.0005(10) C18 0.0114(11) 0.0191(14) 0.0183(13) 0.0129(11) 0.0026(10) 0.0025(10) C19 0.0186(13) 0.0275(16) 0.0212(14) 0.0138(12) 0.0050(11) 0.0112(12) C20 0.0195(13) 0.0349(17) 0.0190(14) 0.0132(13) 0.0066(11) 0.0100(12) C21 0.0184(13) 0.0366(18) 0.0251(15) 0.0235(14) 0.0055(11) 0.0042(12) C22 0.0314(16) 0.0302(17) 0.0341(17) 0.0258(14) 0.0101(13) 0.0111(13) C23 0.0259(14) 0.0232(15) 0.0247(15) 0.0148(12) 0.0101(12) 0.0113(12) C24 0.049(2) 0.063(3) 0.0257(17) 0.0245(17) 0.0185(15) 0.0342(19) C25 0.0215(14) 0.0409(19) 0.0396(19) 0.0225(16) 0.0048(13) 0.0188(14) C26 0.052(2) 0.0246(18) 0.052(2) 0.0219(17) -0.0054(18) 0.0021(16) C27 0.066(3) 0.040(2) 0.037(2) 0.0165(19) 0.025(2) 0.012(2) C28A 0.060(6) 0.134(9) 0.112(8) 0.103(8) -0.030(6) -0.019(6) C28B 0.05(3) 0.05(3) 0.052(18) 0.02(4) 0.01(4) 0.01(4) C29 0.05(2) 0.06(3) 0.05(2) 0.01(2) -0.032(18) -0.002(19) _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 Y1 O5 2.2471(19) . ? Y1 O7 2.2942(19) . ? Y1 O6 2.3283(19) 2_666 ? Y1 O8 2.345(2) . ? Y1 O2 2.3809(19) . ? Y1 O4 2.396(2) . ? Y1 O1 2.4404(19) . ? Y1 O3 2.441(2) . ? Y1 C1 2.777(3) . ? Y1 C9 2.779(3) . ? Y1 Y1 4.6037(15) 2_666 ? S1 O7 1.517(2) . ? S1 C26 1.780(4) . ? S1 C25 1.783(3) . ? O1 C1 1.278(3) . ? C1 O2 1.259(3) . ? C1 C2 1.499(4) . ? C2 C3 1.387(4) . ? C2 C7 1.394(4) . ? S2A O9 1.475(3) . ? S2A C28A 1.741(8) . ? S2A C27 1.790(5) . ? O3 C9 1.251(3) . ? C3 C4 1.402(4) . ? C3 H3 0.9500 . ? O4 C9 1.277(3) . ? C4 C5 1.393(5) . ? C4 C8 1.505(5) . ? O5 C17 1.265(3) . ? C5 C6 1.383(5) . ? C5 H5 0.9500 . ? O6 C17 1.254(3) . ? O6 Y1 2.3283(19) 2_666 ? C6 C7 1.386(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O8 H2O 0.85(4) . ? O8 H1O 0.80(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 S2B 1.743(11) . ? C9 C10A 1.480(6) . ? C9 C10B 1.567(18) . ? C10A C15A 1.396(7) . ? C10A C11A 1.396(6) . ? C10B C15B 1.32(2) . ? C10B C11B 1.37(2) . ? C11A C12A 1.386(7) . ? C11A H11A 0.9500 . ? C11B C12B 1.44(2) . ? C11B H11B 0.9500 . ? C12A C13A 1.400(7) . ? C12A C16A 1.504(6) . ? C12B C13B 1.38(3) . ? C12B C16B 1.46(3) . ? C13A C14A 1.392(7) . ? C13A H13A 0.9500 . ? C13B C14B 1.43(3) . ? C13B H13B 0.9500 . ? C14A C15A 1.378(6) . ? C14A H14A 0.9500 . ? C14B C15B 1.42(2) . ? C14B H14B 0.9500 . ? C15A H15A 0.9500 . ? C15B H15B 0.9500 . ? S2B C29 1.52(4) . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 C18 1.503(3) . ? C18 C19 1.390(4) . ? C18 C23 1.392(4) . ? C19 C20 1.402(4) . ? C19 H19 0.9500 . ? C20 C21 1.387(4) . ? C20 C24 1.506(4) . ? C21 C22 1.384(4) . ? C21 H21 0.9500 . ? C22 C23 1.394(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28A H28A 0.9800 . ? C28A H28B 0.9800 . ? C28A H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 Y1 O7 152.31(7) . . ? O5 Y1 O6 113.27(7) . 2_666 ? O7 Y1 O6 79.67(7) . 2_666 ? O5 Y1 O8 78.11(8) . . ? O7 Y1 O8 81.47(8) . . ? O6 Y1 O8 77.11(8) 2_666 . ? O5 Y1 O2 89.00(7) . . ? O7 Y1 O2 90.08(7) . . ? O6 Y1 O2 149.29(7) 2_666 . ? O8 Y1 O2 130.23(7) . . ? O5 Y1 O4 74.86(7) . . ? O7 Y1 O4 132.71(7) . . ? O6 Y1 O4 79.43(7) 2_666 . ? O8 Y1 O4 133.14(7) . . ? O2 Y1 O4 86.90(7) . . ? O5 Y1 O1 83.69(7) . . ? O7 Y1 O1 73.43(7) . . ? O6 Y1 O1 144.56(7) 2_666 . ? O8 Y1 O1 76.46(7) . . ? O2 Y1 O1 54.27(7) . . ? O4 Y1 O1 135.99(6) . . ? O5 Y1 O3 127.14(7) . . ? O7 Y1 O3 79.36(7) . . ? O6 Y1 O3 72.85(8) 2_666 . ? O8 Y1 O3 146.70(7) . . ? O2 Y1 O3 76.84(7) . . ? O4 Y1 O3 54.02(7) . . ? O1 Y1 O3 122.72(7) . . ? O5 Y1 C1 85.82(8) . . ? O7 Y1 C1 81.00(7) . . ? O6 Y1 C1 160.32(7) 2_666 . ? O8 Y1 C1 103.62(8) . . ? O2 Y1 C1 26.88(7) . . ? O4 Y1 C1 111.67(7) . . ? O1 Y1 C1 27.39(7) . . ? O3 Y1 C1 99.96(8) . . ? O5 Y1 C9 101.50(8) . . ? O7 Y1 C9 105.72(8) . . ? O6 Y1 C9 73.76(8) 2_666 . ? O8 Y1 C9 148.01(8) . . ? O2 Y1 C9 81.48(8) . . ? O4 Y1 C9 27.29(8) . . ? O1 Y1 C9 135.52(7) . . ? O3 Y1 C9 26.74(8) . . ? C1 Y1 C9 108.28(8) . . ? O5 Y1 Y1 45.62(5) . 2_666 ? O7 Y1 Y1 138.04(5) . 2_666 ? O6 Y1 Y1 67.67(5) 2_666 2_666 ? O8 Y1 Y1 66.49(6) . 2_666 ? O2 Y1 Y1 131.17(5) . 2_666 ? O4 Y1 Y1 67.18(5) . 2_666 ? O1 Y1 Y1 120.84(5) . 2_666 ? O3 Y1 Y1 113.21(5) . 2_666 ? C1 Y1 Y1 131.09(6) . 2_666 ? C9 Y1 Y1 90.11(6) . 2_666 ? O7 S1 C26 104.20(15) . . ? O7 S1 C25 104.07(13) . . ? C26 S1 C25 99.38(18) . . ? C1 O1 Y1 91.12(15) . . ? O2 C1 O1 120.2(2) . . ? O2 C1 C2 120.1(2) . . ? O1 C1 C2 119.7(2) . . ? O2 C1 Y1 58.76(13) . . ? O1 C1 Y1 61.49(13) . . ? C2 C1 Y1 177.45(17) . . ? C1 O2 Y1 94.36(16) . . ? C3 C2 C7 120.4(3) . . ? C3 C2 C1 119.7(2) . . ? C7 C2 C1 119.8(3) . . ? O9 S2A C28A 107.3(2) . . ? O9 S2A C27 106.1(2) . . ? C28A S2A C27 94.9(2) . . ? C9 O3 Y1 91.88(17) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C9 O4 Y1 93.35(16) . . ? C5 C4 C3 117.9(3) . . ? C5 C4 C8 121.5(3) . . ? C3 C4 C8 120.7(3) . . ? C17 O5 Y1 175.09(17) . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C17 O6 Y1 125.82(17) . 2_666 ? C5 C6 C7 120.1(3) . . ? C5 C6 H6 119.9 . . ? C7 C6 H6 119.9 . . ? S1 O7 Y1 131.52(11) . . ? C6 C7 C2 119.3(3) . . ? C6 C7 H7 120.4 . . ? C2 C7 H7 120.4 . . ? Y1 O8 H2O 126(2) . . ? Y1 O8 H1O 127(2) . . ? H2O O8 H1O 107(3) . . ? C4 C8 H8A 109.5 . . ? C4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O3 C9 O4 120.7(3) . . ? O3 C9 C10A 116.5(3) . . ? O4 C9 C10A 122.8(3) . . ? O3 C9 C10B 132.4(7) . . ? O4 C9 C10B 106.4(7) . . ? O3 C9 Y1 61.37(15) . . ? O4 C9 Y1 59.36(14) . . ? C10A C9 Y1 176.5(3) . . ? C10B C9 Y1 165.0(7) . . ? C15A C10A C11A 118.5(5) . . ? C15A C10A C9 121.8(4) . . ? C11A C10A C9 119.6(4) . . ? C15B C10B C11B 120.7(16) . . ? C15B C10B C9 126.4(13) . . ? C11B C10B C9 112.4(14) . . ? C12A C11A C10A 122.9(5) . . ? C12A C11A H11A 118.5 . . ? C10A C11A H11A 118.5 . . ? C10B C11B C12B 121.3(18) . . ? C10B C11B H11B 119.4 . . ? C12B C11B H11B 119.4 . . ? C11A C12A C13A 116.6(4) . . ? C11A C12A C16A 121.7(6) . . ? C13A C12A C16A 121.6(6) . . ? C13B C12B C11B 114.9(18) . . ? C13B C12B C16B 123(2) . . ? C11B C12B C16B 122(2) . . ? C14A C13A C12A 121.8(5) . . ? C14A C13A H13A 119.1 . . ? C12A C13A H13A 119.1 . . ? C12B C13B C14B 125(2) . . ? C12B C13B H13B 117.4 . . ? C14B C13B H13B 117.4 . . ? C15A C14A C13A 119.9(4) . . ? C15A C14A H14A 120.0 . . ? C13A C14A H14A 120.0 . . ? C15B C14B C13B 113.5(16) . . ? C15B C14B H14B 123.2 . . ? C13B C14B H14B 123.2 . . ? C14A C15A C10A 120.2(5) . . ? C14A C15A H15A 119.9 . . ? C10A C15A H15A 119.9 . . ? C10B C15B C14B 123.8(15) . . ? C10B C15B H15B 118.1 . . ? C14B C15B H15B 118.1 . . ? C29 S2B O9 116.1(19) . . ? C12B C16B H16D 109.5 . . ? C12B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C12B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? O6 C17 O5 123.2(2) . . ? O6 C17 C18 118.1(2) . . ? O5 C17 C18 118.7(2) . . ? C19 C18 C23 119.8(2) . . ? C19 C18 C17 120.7(2) . . ? C23 C18 C17 119.5(2) . . ? C18 C19 C20 121.0(3) . . ? C18 C19 H19 119.5 . . ? C20 C19 H19 119.5 . . ? C21 C20 C19 118.3(3) . . ? C21 C20 C24 121.2(3) . . ? C19 C20 C24 120.5(3) . . ? C22 C21 C20 121.0(3) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C21 C22 C23 120.4(3) . . ? C21 C22 H22 119.8 . . ? C23 C22 H22 119.8 . . ? C18 C23 C22 119.3(3) . . ? C18 C23 H23 120.3 . . ? C22 C23 H23 120.3 . . ? C20 C24 H24A 109.5 . . ? C20 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C20 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S2A C27 H27A 109.5 . . ? S2A C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S2A C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S2A C28A H28A 109.5 . . ? S2A C28A H28B 109.5 . . ? H28A C28A H28B 109.5 . . ? S2A C28A H28C 109.5 . . ? H28A C28A H28C 109.5 . . ? H28B C28A H28C 109.5 . . ? S2B C29 H29A 109.5 . . ? S2B C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S2B C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H2O O4 0.85(4) 1.93(4) 2.754(3) 163(3) 2_666 O8 H1O O1 0.80(4) 1.99(4) 2.792(3) 173(3) 2_766 C8 H8B O9 0.98 2.56 3.502(5) 161.1 . C21 H21 O9 0.95 2.44 3.380(4) 168.8 2_665 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.285 _refine_diff_density_min -1.090 _refine_diff_density_rms 0.095 # Attachment '6.CIF' data_6 _database_code_depnum_ccdc_archive 'CCDC 649810' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common {[Y(4-MeBA)3(DMSO)(H2O)].DMSO}2 _chemical_melting_point ? _chemical_formula_moiety 'C56 H70 O18 S4 Y2' _chemical_formula_sum 'C56 H70 O18 S4 Y2' _chemical_formula_weight 1337.18 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.5475(4) _cell_length_b 13.4364(8) _cell_length_c 14.1992(8) _cell_angle_alpha 99.577(2) _cell_angle_beta 106.649(3) _cell_angle_gamma 102.216(2) _cell_volume 1481.45(14) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_absorpt_coefficient_mu 2.160 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5522 _exptl_absorpt_correction_T_max 0.7444 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 12131 _diffrn_reflns_av_R_equivalents 0.0499 _diffrn_reflns_av_sigmaI/netI 0.0953 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 5 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.53 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6806 _reflns_number_gt 5098 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0410P)^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 6806 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0807 _refine_ls_R_factor_gt 0.0520 _refine_ls_wR_factor_ref 0.1091 _refine_ls_wR_factor_gt 0.0978 _refine_ls_goodness_of_fit_ref 1.016 _refine_ls_restrained_S_all 1.016 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 1.18403(4) 1.06946(3) 0.41792(3) 0.00906(10) Uani 1 1 d . . . S1 S 1.27441(11) 0.88480(7) 0.25697(7) 0.0140(2) Uani 1 1 d . . . O2 O 0.9282(3) 1.12158(19) 0.38002(19) 0.0139(5) Uani 1 1 d . . . C1 C 0.9153(4) 1.1189(3) 0.2881(3) 0.0123(7) Uani 1 1 d . . . H2O H 1.228(5) 0.925(3) 0.544(3) 0.018(13) Uiso 1 1 d . . . S2 S 1.04599(12) 0.39862(9) 0.12645(8) 0.0239(2) Uani 1 1 d . . . O1 O 1.0329(3) 1.10206(19) 0.25557(19) 0.0140(5) Uani 1 1 d . . . C2 C 0.7578(4) 1.1326(3) 0.2183(3) 0.0135(8) Uani 1 1 d . . . H1O H 1.334(8) 0.917(5) 0.502(5) 0.08(2) Uiso 1 1 d . . . O3 O 1.3365(3) 1.24206(19) 0.4251(2) 0.0166(6) Uani 1 1 d . . . C3 C 0.7374(5) 1.1270(3) 0.1165(3) 0.0201(9) Uani 1 1 d . . . H3 H 0.8273 1.1189 0.0918 0.024 Uiso 1 1 calc R . . O4 O 1.4873(3) 1.15256(19) 0.51107(19) 0.0132(5) Uani 1 1 d . . . C4 C 0.5873(5) 1.1332(3) 0.0516(3) 0.0247(9) Uani 1 1 d . . . H4 H 0.5755 1.1291 -0.0177 0.030 Uiso 1 1 calc R . . O5 O 0.9812(3) 0.91139(19) 0.32447(19) 0.0141(6) Uani 1 1 d . . . C5 C 0.4531(5) 1.1453(3) 0.0844(3) 0.0193(9) Uani 1 1 d . . . O6 O 0.8445(3) 0.87403(19) 0.43169(18) 0.0148(6) Uani 1 1 d . . . C6 C 0.4751(5) 1.1546(3) 0.1867(3) 0.0184(8) Uani 1 1 d . . . H6 H 0.3865 1.1654 0.2116 0.022 Uiso 1 1 calc R . . O7 O 1.3256(3) 0.99510(19) 0.32355(18) 0.0142(6) Uani 1 1 d . . . C7 C 0.6264(4) 1.1482(3) 0.2529(3) 0.0175(8) Uani 1 1 d . . . H7 H 0.6399 1.1546 0.3226 0.021 Uiso 1 1 calc R . . O8 O 1.2675(4) 0.9483(2) 0.5089(2) 0.0155(6) Uani 1 1 d . . . C8 C 0.2883(5) 1.1483(3) 0.0115(3) 0.0295(11) Uani 1 1 d . . . H8A H 0.2674 1.1029 -0.0550 0.044 Uiso 1 1 calc R . . H8B H 0.2948 1.2205 0.0052 0.044 Uiso 1 1 calc R . . H8C H 0.1954 1.1236 0.0367 0.044 Uiso 1 1 calc R . . O9 O 1.0094(4) 0.3409(2) 0.0190(2) 0.0339(8) Uani 1 1 d . . . C9 C 1.4770(4) 1.2356(3) 0.4819(3) 0.0116(7) Uani 1 1 d . . . C10 C 1.6291(4) 1.3291(3) 0.5170(3) 0.0121(8) Uani 1 1 d . . . C11 C 1.6167(5) 1.4191(3) 0.4832(3) 0.0180(8) Uani 1 1 d . . . H11 H 1.5144 1.4197 0.4343 0.022 Uiso 1 1 calc R . . C12 C 1.7530(5) 1.5081(3) 0.5204(3) 0.0190(8) Uani 1 1 d . . . H12 H 1.7430 1.5692 0.4964 0.023 Uiso 1 1 calc R . . C13 C 1.9040(4) 1.5100(3) 0.5921(3) 0.0154(8) Uani 1 1 d . . . C14 C 1.9154(5) 1.4183(3) 0.6233(3) 0.0175(8) Uani 1 1 d . . . H14 H 2.0186 1.4171 0.6710 0.021 Uiso 1 1 calc R . . C15 C 1.7805(4) 1.3288(3) 0.5869(3) 0.0144(8) Uani 1 1 d . . . H15 H 1.7913 1.2672 0.6096 0.017 Uiso 1 1 calc R . . C16 C 2.0502(4) 1.6083(3) 0.6345(3) 0.0194(9) Uani 1 1 d . . . H16A H 2.1575 1.5891 0.6532 0.029 Uiso 1 1 calc R . . H16B H 2.0400 1.6504 0.6947 0.029 Uiso 1 1 calc R . . H16C H 2.0481 1.6491 0.5833 0.029 Uiso 1 1 calc R . . C17 C 0.8817(4) 0.8498(3) 0.3527(3) 0.0115(7) Uani 1 1 d . . . C18 C 0.8009(4) 0.7405(3) 0.2874(3) 0.0112(7) Uani 1 1 d . . . C19 C 0.8333(4) 0.7105(3) 0.1982(3) 0.0145(8) Uani 1 1 d . . . H19 H 0.9023 0.7609 0.1768 0.017 Uiso 1 1 calc R . . C20 C 0.7669(4) 0.6085(3) 0.1400(3) 0.0166(8) Uani 1 1 d . . . H20 H 0.7900 0.5898 0.0788 0.020 Uiso 1 1 calc R . . C21 C 0.6667(4) 0.5330(3) 0.1701(3) 0.0179(8) Uani 1 1 d . . . C22 C 0.6325(4) 0.5634(3) 0.2596(3) 0.0189(9) Uani 1 1 d . . . H22 H 0.5625 0.5131 0.2807 0.023 Uiso 1 1 calc R . . C23 C 0.6987(4) 0.6650(3) 0.3176(3) 0.0152(8) Uani 1 1 d . . . H23 H 0.6750 0.6840 0.3784 0.018 Uiso 1 1 calc R . . C24 C 0.5968(5) 0.4209(3) 0.1074(3) 0.0241(9) Uani 1 1 d . . . H24A H 0.4776 0.4088 0.0667 0.036 Uiso 1 1 calc R . . H24B H 0.6051 0.3729 0.1524 0.036 Uiso 1 1 calc R . . H24C H 0.6626 0.4083 0.0625 0.036 Uiso 1 1 calc R . . C25 C 1.1686(5) 0.8972(3) 0.1333(3) 0.0193(9) Uani 1 1 d . . . H25A H 1.0572 0.9075 0.1297 0.029 Uiso 1 1 calc R . . H25B H 1.1539 0.8332 0.0831 0.029 Uiso 1 1 calc R . . H25C H 1.2367 0.9576 0.1190 0.029 Uiso 1 1 calc R . . C26 C 1.4677(5) 0.8672(3) 0.2424(3) 0.0204(9) Uani 1 1 d . . . H26A H 1.5408 0.8589 0.3061 0.031 Uiso 1 1 calc R . . H26B H 1.5258 0.9286 0.2245 0.031 Uiso 1 1 calc R . . H26C H 1.4428 0.8043 0.1885 0.031 Uiso 1 1 calc R . . C27 C 1.1959(5) 0.3458(3) 0.2048(3) 0.0269(10) Uani 1 1 d . . . H27A H 1.1396 0.2742 0.2046 0.040 Uiso 1 1 calc R . . H27B H 1.2402 0.3896 0.2742 0.040 Uiso 1 1 calc R . . H27C H 1.2897 0.3447 0.1783 0.040 Uiso 1 1 calc R . . C28 C 1.1853(5) 0.5245(3) 0.1433(3) 0.0270(10) Uani 1 1 d . . . H28A H 1.1229 0.5659 0.1042 0.040 Uiso 1 1 calc R . . H28B H 1.2798 0.5158 0.1196 0.040 Uiso 1 1 calc R . . H28C H 1.2298 0.5609 0.2153 0.040 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 Y1 0.00666(16) 0.00892(18) 0.01131(18) 0.00196(13) 0.00319(12) 0.00167(12) S1 0.0136(4) 0.0141(5) 0.0147(5) 0.0029(4) 0.0052(4) 0.0044(4) O2 0.0118(12) 0.0179(14) 0.0144(14) 0.0055(11) 0.0051(10) 0.0064(10) C1 0.0113(17) 0.0068(18) 0.016(2) 0.0043(15) 0.0027(14) -0.0010(13) S2 0.0205(5) 0.0311(6) 0.0205(6) 0.0058(5) 0.0076(4) 0.0070(4) O1 0.0122(12) 0.0152(14) 0.0160(14) 0.0040(11) 0.0071(10) 0.0033(10) C2 0.0128(18) 0.0106(19) 0.0133(19) 0.0019(15) 0.0000(14) 0.0020(14) O3 0.0099(12) 0.0129(14) 0.0253(16) 0.0070(12) 0.0039(11) 0.0004(10) C3 0.020(2) 0.025(2) 0.014(2) 0.0034(17) 0.0051(16) 0.0075(17) O4 0.0117(12) 0.0111(13) 0.0166(14) 0.0054(11) 0.0039(10) 0.0024(10) C4 0.030(2) 0.028(2) 0.014(2) 0.0051(18) 0.0006(17) 0.0132(19) O5 0.0119(12) 0.0112(14) 0.0182(14) 0.0023(11) 0.0057(11) 0.0014(10) C5 0.020(2) 0.012(2) 0.021(2) 0.0017(16) -0.0012(16) 0.0075(15) O6 0.0148(13) 0.0167(14) 0.0119(13) 0.0017(11) 0.0038(10) 0.0049(10) C6 0.0168(19) 0.016(2) 0.023(2) 0.0070(17) 0.0036(16) 0.0070(15) O7 0.0136(13) 0.0134(14) 0.0139(14) -0.0020(11) 0.0060(10) 0.0026(10) C7 0.0161(19) 0.017(2) 0.020(2) 0.0064(17) 0.0052(16) 0.0050(15) O8 0.0151(14) 0.0196(16) 0.0208(16) 0.0128(13) 0.0118(12) 0.0092(12) C8 0.025(2) 0.026(3) 0.028(3) 0.002(2) -0.0055(18) 0.0110(19) O9 0.0430(18) 0.0328(19) 0.0170(16) 0.0029(14) 0.0050(14) 0.0014(15) C9 0.0109(17) 0.0128(19) 0.0129(19) 0.0036(15) 0.0062(14) 0.0036(14) C10 0.0081(17) 0.015(2) 0.0138(19) 0.0021(15) 0.0065(14) 0.0007(14) C11 0.0138(19) 0.018(2) 0.023(2) 0.0082(17) 0.0053(16) 0.0046(15) C12 0.0190(19) 0.014(2) 0.026(2) 0.0102(17) 0.0069(17) 0.0053(15) C13 0.0143(18) 0.016(2) 0.016(2) 0.0005(16) 0.0103(15) 0.0015(15) C14 0.0136(18) 0.017(2) 0.020(2) 0.0020(17) 0.0056(15) 0.0010(15) C15 0.0117(17) 0.015(2) 0.017(2) 0.0050(16) 0.0036(15) 0.0050(14) C16 0.0168(19) 0.017(2) 0.022(2) 0.0011(17) 0.0091(16) 0.0000(16) C17 0.0072(16) 0.016(2) 0.0132(19) 0.0052(15) 0.0021(14) 0.0074(14) C18 0.0078(16) 0.0130(19) 0.0115(19) 0.0038(15) 0.0004(14) 0.0038(14) C19 0.0100(17) 0.019(2) 0.0138(19) 0.0057(16) 0.0033(14) 0.0019(15) C20 0.0177(19) 0.017(2) 0.015(2) 0.0040(16) 0.0052(15) 0.0049(15) C21 0.0142(19) 0.016(2) 0.018(2) 0.0005(16) -0.0004(15) 0.0047(15) C22 0.0142(19) 0.015(2) 0.027(2) 0.0083(17) 0.0062(16) 0.0010(15) C23 0.0136(18) 0.020(2) 0.014(2) 0.0042(16) 0.0065(15) 0.0050(15) C24 0.020(2) 0.018(2) 0.028(2) 0.0000(18) 0.0049(18) 0.0012(17) C25 0.0157(19) 0.022(2) 0.017(2) 0.0026(17) 0.0023(16) 0.0043(16) C26 0.018(2) 0.028(2) 0.018(2) 0.0026(18) 0.0078(16) 0.0123(17) C27 0.023(2) 0.035(3) 0.027(2) 0.010(2) 0.0127(18) 0.0097(19) C28 0.031(2) 0.028(3) 0.024(2) 0.0057(19) 0.0090(19) 0.0108(19) _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 Y1 O6 2.244(2) 2_776 ? Y1 O7 2.292(2) . ? Y1 O5 2.337(2) . ? Y1 O8 2.343(3) . ? Y1 O3 2.378(2) . ? Y1 O2 2.379(2) . ? Y1 O4 2.456(2) . ? Y1 O1 2.458(2) . ? Y1 C9 2.781(3) . ? Y1 C1 2.783(4) . ? Y1 Y1 4.6883(7) 2_776 ? S1 O7 1.518(2) . ? S1 C26 1.782(4) . ? S1 C25 1.783(4) . ? O2 C1 1.271(4) . ? C1 O1 1.266(4) . ? C1 C2 1.493(5) . ? S2 O9 1.503(3) . ? S2 C28 1.785(4) . ? S2 C27 1.792(4) . ? C2 C7 1.389(5) . ? C2 C3 1.392(5) . ? O3 C9 1.269(4) . ? C3 C4 1.377(5) . ? C3 H3 0.9500 . ? O4 C9 1.265(4) . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? O5 C17 1.255(4) . ? C5 C6 1.390(5) . ? C5 C8 1.504(5) . ? O6 C17 1.262(4) . ? O6 Y1 2.244(2) 2_776 ? C6 C7 1.394(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? O8 H2O 0.76(4) . ? O8 H1O 0.79(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 C10 1.498(5) . ? C10 C11 1.387(5) . ? C10 C15 1.388(5) . ? C11 C12 1.383(5) . ? C11 H11 0.9500 . ? C12 C13 1.388(5) . ? C12 H12 0.9500 . ? C13 C14 1.391(5) . ? C13 C16 1.507(5) . ? C14 C15 1.380(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.498(5) . ? C18 C19 1.385(5) . ? C18 C23 1.400(5) . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 C21 1.390(5) . ? C20 H20 0.9500 . ? C21 C22 1.400(5) . ? C21 C24 1.513(5) . ? C22 C23 1.376(5) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 Y1 O7 150.40(9) 2_776 . ? O6 Y1 O5 111.99(9) 2_776 . ? O7 Y1 O5 78.37(8) . . ? O6 Y1 O8 76.60(10) 2_776 . ? O7 Y1 O8 79.21(10) . . ? O5 Y1 O8 76.91(9) . . ? O6 Y1 O3 90.60(9) 2_776 . ? O7 Y1 O3 92.07(9) . . ? O5 Y1 O3 149.54(9) . . ? O8 Y1 O3 130.10(9) . . ? O6 Y1 O2 74.54(8) 2_776 . ? O7 Y1 O2 134.95(9) . . ? O5 Y1 O2 77.99(8) . . ? O8 Y1 O2 130.64(10) . . ? O3 Y1 O2 89.39(8) . . ? O6 Y1 O4 83.51(8) 2_776 . ? O7 Y1 O4 74.37(8) . . ? O5 Y1 O4 144.76(8) . . ? O8 Y1 O4 76.41(9) . . ? O3 Y1 O4 54.11(8) . . ? O2 Y1 O4 137.24(8) . . ? O6 Y1 O1 126.49(8) 2_776 . ? O7 Y1 O1 82.66(8) . . ? O5 Y1 O1 73.89(8) . . ? O8 Y1 O1 148.13(9) . . ? O3 Y1 O1 76.24(8) . . ? O2 Y1 O1 54.09(8) . . ? O4 Y1 O1 123.24(8) . . ? O6 Y1 C9 86.71(10) 2_776 . ? O7 Y1 C9 82.46(9) . . ? O5 Y1 C9 160.46(9) . . ? O8 Y1 C9 103.27(10) . . ? O3 Y1 C9 27.07(9) . . ? O2 Y1 C9 113.99(9) . . ? O4 Y1 C9 27.04(9) . . ? O1 Y1 C9 100.04(9) . . ? O6 Y1 C1 101.02(10) 2_776 . ? O7 Y1 C1 108.57(10) . . ? O5 Y1 C1 72.70(9) . . ? O8 Y1 C1 146.04(10) . . ? O3 Y1 C1 83.42(9) . . ? O2 Y1 C1 27.10(9) . . ? O4 Y1 C1 137.46(9) . . ? O1 Y1 C1 27.06(9) . . ? C9 Y1 C1 110.46(10) . . ? O6 Y1 Y1 46.85(6) 2_776 2_776 ? O7 Y1 Y1 132.77(6) . 2_776 ? O5 Y1 Y1 65.18(6) . 2_776 ? O8 Y1 Y1 64.53(7) . 2_776 ? O3 Y1 Y1 134.25(6) . 2_776 ? O2 Y1 Y1 66.45(6) . 2_776 ? O4 Y1 Y1 121.11(6) . 2_776 ? O1 Y1 Y1 112.69(6) . 2_776 ? C9 Y1 Y1 132.99(7) . 2_776 ? C1 Y1 Y1 88.82(7) . 2_776 ? O7 S1 C26 103.98(16) . . ? O7 S1 C25 104.33(17) . . ? C26 S1 C25 100.13(18) . . ? C1 O2 Y1 94.4(2) . . ? O1 C1 O2 120.3(3) . . ? O1 C1 C2 120.4(3) . . ? O2 C1 C2 119.3(3) . . ? O1 C1 Y1 62.05(18) . . ? O2 C1 Y1 58.48(17) . . ? C2 C1 Y1 172.9(2) . . ? O9 S2 C28 106.00(19) . . ? O9 S2 C27 106.43(19) . . ? C28 S2 C27 97.9(2) . . ? C1 O1 Y1 90.9(2) . . ? C7 C2 C3 118.5(3) . . ? C7 C2 C1 120.6(3) . . ? C3 C2 C1 120.8(3) . . ? C9 O3 Y1 94.5(2) . . ? C4 C3 C2 120.2(4) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C9 O4 Y1 90.9(2) . . ? C3 C4 C5 121.8(4) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C17 O5 Y1 129.1(2) . . ? C4 C5 C6 118.2(3) . . ? C4 C5 C8 120.9(4) . . ? C6 C5 C8 121.0(4) . . ? C17 O6 Y1 172.1(2) . 2_776 ? C5 C6 C7 120.4(4) . . ? C5 C6 H6 119.8 . . ? C7 C6 H6 119.8 . . ? S1 O7 Y1 128.73(14) . . ? C2 C7 C6 120.9(4) . . ? C2 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? Y1 O8 H2O 127(3) . . ? Y1 O8 H1O 126(4) . . ? H2O O8 H1O 106(5) . . ? C5 C8 H8A 109.5 . . ? C5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? O4 C9 O3 120.5(3) . . ? O4 C9 C10 120.4(3) . . ? O3 C9 C10 119.2(3) . . ? O4 C9 Y1 62.01(18) . . ? O3 C9 Y1 58.45(17) . . ? C10 C9 Y1 176.9(2) . . ? C11 C10 C15 119.2(3) . . ? C11 C10 C9 119.7(3) . . ? C15 C10 C9 121.0(3) . . ? C12 C11 C10 120.1(4) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 121.4(4) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C14 117.6(3) . . ? C12 C13 C16 121.1(4) . . ? C14 C13 C16 121.3(3) . . ? C15 C14 C13 121.6(4) . . ? C15 C14 H14 119.2 . . ? C13 C14 H14 119.2 . . ? C14 C15 C10 119.9(4) . . ? C14 C15 H15 120.0 . . ? C10 C15 H15 120.0 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O5 C17 O6 124.5(3) . . ? O5 C17 C18 117.5(3) . . ? O6 C17 C18 118.0(3) . . ? C19 C18 C23 118.5(3) . . ? C19 C18 C17 120.5(3) . . ? C23 C18 C17 120.9(3) . . ? C20 C19 C18 121.2(3) . . ? C20 C19 H19 119.4 . . ? C18 C19 H19 119.4 . . ? C19 C20 C21 120.5(4) . . ? C19 C20 H20 119.7 . . ? C21 C20 H20 119.7 . . ? C20 C21 C22 118.4(4) . . ? C20 C21 C24 120.6(4) . . ? C22 C21 C24 121.0(4) . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.5 . . ? C21 C22 H22 119.5 . . ? C22 C23 C18 120.4(3) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? S2 C27 H27A 109.5 . . ? S2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? S2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? S2 C28 H28A 109.5 . . ? S2 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S2 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O8 H2O O2 0.76(4) 2.00(4) 2.740(4) 165(4) 2_776 O8 H1O O4 0.79(6) 1.99(6) 2.780(4) 177(6) 2_876 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.639 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.110 # Attachment '7a.CIF' data_7a _database_code_depnum_ccdc_archive 'CCDC 649811' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[tris(3-nitrobenzoate)yttrium(III)(DMF)] ; _chemical_name_common poly[(dmf)tris(3-nitrobenzoato)yttrium(III)] _chemical_melting_point ? _chemical_formula_moiety C24H19N4O13Y _chemical_formula_sum 'C24 H19 N4 O13 Y' _chemical_formula_weight 660.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2242(4) _cell_length_b 13.0741(8) _cell_length_c 13.1527(8) _cell_angle_alpha 90.801(4) _cell_angle_beta 105.040(3) _cell_angle_gamma 106.894(3) _cell_volume 1300.72(13) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.686 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 668 _exptl_absorpt_coefficient_mu 2.320 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5187 _exptl_absorpt_correction_T_max 0.7605 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 11854 _diffrn_reflns_av_R_equivalents 0.0441 _diffrn_reflns_av_sigmaI/netI 0.0810 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.40 _diffrn_reflns_theta_max 27.50 _reflns_number_total 5888 _reflns_number_gt 4405 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+0.2279P] 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 5888 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0779 _refine_ls_R_factor_gt 0.0444 _refine_ls_wR_factor_ref 0.1034 _refine_ls_wR_factor_gt 0.0913 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.75196(4) 0.95655(3) 1.00213(2) 0.01084(10) Uani 1 1 d . . . O1 O 0.5416(3) 0.94523(17) 0.83976(16) 0.0156(5) Uani 1 1 d . . . N1 N 0.2742(4) 0.9178(2) 0.4412(2) 0.0230(7) Uani 1 1 d . . . C1 C 0.4606(4) 1.0134(3) 0.8288(2) 0.0125(6) Uani 1 1 d . . . O2 O 0.4533(3) 1.06895(17) 0.90590(16) 0.0140(5) Uani 1 1 d . . . N2 N 0.3882(4) 0.6526(2) 0.6169(2) 0.0198(6) Uani 1 1 d . . . C2 C 0.3708(4) 1.0317(3) 0.7189(2) 0.0128(6) Uani 1 1 d . . . O3 O 0.3271(4) 0.8395(2) 0.4570(2) 0.0335(7) Uani 1 1 d . . . N3 N 1.4297(4) 0.6135(2) 1.2439(2) 0.0219(7) Uani 1 1 d . . . C3 C 0.3642(4) 0.9661(3) 0.6332(2) 0.0142(7) Uani 1 1 d . . . H3 H 0.4136 0.9085 0.6429 0.017 Uiso 1 1 calc R . . O4 O 0.2157(4) 0.9434(2) 0.35261(19) 0.0337(7) Uani 1 1 d . . . N4 N 0.3139(4) 0.6446(2) 0.9114(2) 0.0199(6) Uani 1 1 d . . . C4 C 0.2836(4) 0.9872(3) 0.5332(2) 0.0164(7) Uani 1 1 d . . . O5 O 0.8992(3) 0.91682(17) 0.89377(16) 0.0133(5) Uani 1 1 d . . . C5 C 0.2113(4) 1.0700(3) 0.5157(3) 0.0206(8) Uani 1 1 d . . . H5 H 0.1580 1.0827 0.4458 0.025 Uiso 1 1 calc R . . O6 O 1.1383(3) 0.91039(18) 0.85151(16) 0.0160(5) Uani 1 1 d . . . C6 C 0.2175(5) 1.1344(3) 0.6014(3) 0.0226(8) Uani 1 1 d . . . H6 H 0.1681 1.1919 0.5911 0.027 Uiso 1 1 calc R . . O7 O 0.3200(3) 0.6975(2) 0.6685(2) 0.0295(6) Uani 1 1 d . . . C7 C 0.2963(4) 1.1147(3) 0.7029(3) 0.0175(7) Uani 1 1 d . . . H7 H 0.2991 1.1585 0.7620 0.021 Uiso 1 1 calc R . . O8 O 0.3048(3) 0.5763(2) 0.55025(19) 0.0285(6) Uani 1 1 d . . . C8 C 0.9741(4) 0.8806(3) 0.8354(2) 0.0132(6) Uani 1 1 d . . . O9 O 0.9041(3) 0.85901(17) 1.11136(16) 0.0142(5) Uani 1 1 d . . . C9 C 0.8616(4) 0.7997(2) 0.7437(2) 0.0127(6) Uani 1 1 d . . . O10 O 1.1570(3) 0.88135(17) 1.06651(16) 0.0139(5) Uani 1 1 d . . . C10 C 0.6786(4) 0.7673(3) 0.7214(2) 0.0150(7) Uani 1 1 d . . . H10 H 0.6214 0.7966 0.7632 0.018 Uiso 1 1 calc R . . O11 O 1.4853(4) 0.5605(2) 1.3142(2) 0.0351(7) Uani 1 1 d . . . C11 C 0.5824(4) 0.6915(3) 0.6373(2) 0.0159(7) Uani 1 1 d . . . O12 O 1.5007(3) 0.6414(2) 1.1736(2) 0.0309(6) Uani 1 1 d . . . C12 C 0.6592(4) 0.6477(3) 0.5730(3) 0.0185(7) Uani 1 1 d . . . H12 H 0.5887 0.5960 0.5151 0.022 Uiso 1 1 calc R . . O13 O 0.5777(3) 0.77504(18) 0.95470(17) 0.0173(5) Uani 1 1 d . . . C13 C 0.8431(4) 0.6817(3) 0.5959(3) 0.0190(7) Uani 1 1 d . . . H13 H 0.8994 0.6532 0.5529 0.023 Uiso 1 1 calc R . . C14 C 0.9437(4) 0.7566(3) 0.6806(2) 0.0162(7) Uani 1 1 d . . . H14 H 1.0689 0.7790 0.6962 0.019 Uiso 1 1 calc R . . C15 C 1.0449(4) 0.8374(2) 1.1142(2) 0.0123(6) Uani 1 1 d . . . C16 C 1.0823(4) 0.7487(2) 1.1792(2) 0.0134(7) Uani 1 1 d . . . C17 C 1.2341(4) 0.7216(3) 1.1816(2) 0.0144(7) Uani 1 1 d . . . H17 H 1.3103 0.7561 1.1406 0.017 Uiso 1 1 calc R . . C18 C 1.2724(4) 0.6435(3) 1.2448(2) 0.0159(7) Uani 1 1 d . . . C19 C 1.1681(5) 0.5935(3) 1.3078(3) 0.0205(7) Uani 1 1 d . . . H19 H 1.2001 0.5421 1.3528 0.025 Uiso 1 1 calc R . . C20 C 1.0159(5) 0.6201(3) 1.3038(3) 0.0214(8) Uani 1 1 d . . . H20 H 0.9408 0.5857 1.3453 0.026 Uiso 1 1 calc R . . C21 C 0.9720(4) 0.6969(3) 1.2392(2) 0.0167(7) Uani 1 1 d . . . H21 H 0.8663 0.7140 1.2361 0.020 Uiso 1 1 calc R . . C22 C 0.4155(4) 0.7436(3) 0.9423(2) 0.0174(7) Uani 1 1 d . . . H22 H 0.3610 0.7951 0.9561 0.021 Uiso 1 1 calc R . . C23 C 0.3844(5) 0.5615(3) 0.8847(3) 0.0350(10) Uani 1 1 d . . . H23A H 0.3379 0.5392 0.8086 0.053 Uiso 1 1 calc R . . H23B H 0.3491 0.4996 0.9241 0.053 Uiso 1 1 calc R . . H23C H 0.5137 0.5894 0.9033 0.053 Uiso 1 1 calc R . . C24 C 0.1237(5) 0.6163(3) 0.8990(3) 0.0325(9) Uani 1 1 d . . . H24A H 0.0954 0.6788 0.9228 0.049 Uiso 1 1 calc R . . H24B H 0.0888 0.5571 0.9416 0.049 Uiso 1 1 calc R . . H24C H 0.0596 0.5940 0.8244 0.049 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 Y1 0.00892(14) 0.01717(17) 0.00759(16) -0.00080(11) 0.00282(10) 0.00532(12) O1 0.0122(11) 0.0204(13) 0.0121(11) -0.0005(10) 0.0004(9) 0.0043(10) N1 0.0203(15) 0.0294(18) 0.0140(16) -0.0039(13) 0.0048(12) -0.0002(14) C1 0.0056(14) 0.0160(17) 0.0124(16) 0.0001(13) 0.0013(12) -0.0009(12) O2 0.0113(11) 0.0197(12) 0.0097(11) -0.0045(9) 0.0047(8) 0.0015(9) N2 0.0162(14) 0.0216(16) 0.0174(15) -0.0009(13) -0.0006(12) 0.0044(13) C2 0.0095(14) 0.0169(17) 0.0114(16) 0.0020(13) 0.0044(12) 0.0017(13) O3 0.0477(18) 0.0328(16) 0.0219(14) -0.0057(12) 0.0099(12) 0.0153(14) N3 0.0214(15) 0.0185(16) 0.0255(17) 0.0001(13) 0.0028(13) 0.0088(13) C3 0.0129(15) 0.0174(17) 0.0129(16) 0.0001(14) 0.0056(12) 0.0034(13) O4 0.0405(16) 0.0481(18) 0.0078(13) -0.0015(12) 0.0008(11) 0.0115(14) N4 0.0170(14) 0.0177(15) 0.0206(16) -0.0001(12) 0.0023(12) 0.0012(12) C4 0.0138(16) 0.0237(18) 0.0083(16) -0.0027(14) 0.0019(12) 0.0015(14) O5 0.0126(11) 0.0213(12) 0.0088(11) -0.0028(9) 0.0042(8) 0.0083(9) C5 0.0192(17) 0.031(2) 0.0113(17) 0.0066(15) 0.0015(14) 0.0097(16) O6 0.0081(10) 0.0249(13) 0.0142(12) -0.0032(10) 0.0044(9) 0.0030(9) C6 0.0274(19) 0.030(2) 0.0175(19) 0.0094(16) 0.0080(15) 0.0171(17) O7 0.0166(13) 0.0376(16) 0.0310(15) -0.0090(13) 0.0054(11) 0.0051(12) C7 0.0195(17) 0.0222(19) 0.0140(17) 0.0000(14) 0.0075(13) 0.0086(15) O8 0.0236(13) 0.0283(15) 0.0234(14) -0.0072(12) -0.0031(11) 0.0016(12) C8 0.0163(16) 0.0163(17) 0.0076(15) -0.0003(13) 0.0036(12) 0.0055(13) O9 0.0118(11) 0.0216(13) 0.0111(11) 0.0029(10) 0.0026(9) 0.0085(9) C9 0.0148(15) 0.0144(16) 0.0090(15) 0.0013(13) 0.0022(12) 0.0054(13) O10 0.0101(10) 0.0198(12) 0.0133(12) 0.0050(10) 0.0049(9) 0.0052(9) C10 0.0158(16) 0.0186(17) 0.0113(16) 0.0007(14) 0.0031(12) 0.0070(14) O11 0.0406(16) 0.0446(18) 0.0303(16) 0.0148(14) 0.0064(13) 0.0309(14) C11 0.0126(16) 0.0175(18) 0.0154(17) 0.0014(14) 0.0017(13) 0.0031(14) O12 0.0275(14) 0.0403(17) 0.0369(16) 0.0135(13) 0.0164(12) 0.0215(13) C12 0.0251(18) 0.0156(17) 0.0137(17) -0.0014(14) 0.0049(14) 0.0049(14) O13 0.0133(11) 0.0213(13) 0.0150(12) -0.0015(10) 0.0017(9) 0.0037(10) C13 0.0285(19) 0.0188(18) 0.0144(17) -0.0007(14) 0.0110(14) 0.0099(15) C14 0.0165(16) 0.0207(18) 0.0148(17) 0.0014(14) 0.0065(13) 0.0087(14) C15 0.0105(15) 0.0130(16) 0.0093(15) -0.0013(13) -0.0013(12) 0.0010(13) C16 0.0130(15) 0.0153(17) 0.0100(16) -0.0024(13) -0.0003(12) 0.0047(13) C17 0.0137(15) 0.0171(17) 0.0122(16) -0.0009(13) 0.0027(12) 0.0050(13) C18 0.0154(16) 0.0165(17) 0.0149(17) -0.0012(14) 0.0011(13) 0.0063(14) C19 0.0276(19) 0.0168(18) 0.0152(18) 0.0020(14) 0.0017(14) 0.0073(15) C20 0.0241(18) 0.0232(19) 0.0169(18) 0.0038(15) 0.0088(14) 0.0043(15) C21 0.0165(16) 0.0175(18) 0.0155(17) 0.0007(14) 0.0048(13) 0.0041(14) C22 0.0170(17) 0.0205(18) 0.0122(17) -0.0018(14) 0.0028(13) 0.0031(14) C23 0.030(2) 0.021(2) 0.050(3) -0.0030(19) 0.0041(19) 0.0070(17) C24 0.0179(18) 0.035(2) 0.038(2) -0.0010(19) 0.0072(17) -0.0015(17) _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 Y1 O5 2.238(2) . ? Y1 O2 2.273(2) 2_677 ? Y1 O9 2.303(2) . ? Y1 O10 2.313(2) 2_777 ? Y1 O1 2.345(2) . ? Y1 O13 2.365(2) . ? Y1 O6 2.375(2) 2_777 ? Y1 O5 2.826(2) 2_777 ? Y1 C8 2.960(3) 2_777 ? Y1 Y1 3.9199(6) 2_777 ? Y1 Y1 4.5921(6) 2_677 ? O1 C1 1.247(4) . ? N1 O3 1.224(4) . ? N1 O4 1.231(4) . ? N1 C4 1.474(4) . ? C1 O2 1.263(4) . ? C1 C2 1.500(4) . ? O2 Y1 2.273(2) 2_677 ? N2 O7 1.223(3) . ? N2 O8 1.225(3) . ? N2 C11 1.478(4) . ? C2 C3 1.387(4) . ? C2 C7 1.388(4) . ? N3 O12 1.222(4) . ? N3 O11 1.236(4) . ? N3 C18 1.460(4) . ? C3 C4 1.381(4) . ? C3 H3 0.9500 . ? N4 C22 1.311(4) . ? N4 C23 1.450(5) . ? N4 C24 1.463(4) . ? C4 C5 1.375(5) . ? O5 C8 1.264(4) . ? O5 Y1 2.826(2) 2_777 ? C5 C6 1.378(5) . ? C5 H5 0.9500 . ? O6 C8 1.251(4) . ? O6 Y1 2.375(2) 2_777 ? C6 C7 1.387(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.499(4) . ? C8 Y1 2.960(3) 2_777 ? O9 C15 1.261(4) . ? C9 C10 1.388(4) . ? C9 C14 1.399(4) . ? O10 C15 1.256(4) . ? O10 Y1 2.313(2) 2_777 ? C10 C11 1.375(4) . ? C10 H10 0.9500 . ? C11 C12 1.384(4) . ? C12 C13 1.395(5) . ? C12 H12 0.9500 . ? O13 C22 1.241(4) . ? C13 C14 1.381(4) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.506(4) . ? C16 C17 1.386(4) . ? C16 C21 1.391(4) . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.382(5) . ? C19 C20 1.381(5) . ? C19 H19 0.9500 . ? C20 C21 1.391(5) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 Y1 O2 158.54(8) . 2_677 ? O5 Y1 O9 81.47(7) . . ? O2 Y1 O9 92.07(8) 2_677 . ? O5 Y1 O10 78.23(8) . 2_777 ? O2 Y1 O10 119.89(7) 2_677 2_777 ? O9 Y1 O10 132.54(8) . 2_777 ? O5 Y1 O1 80.91(7) . . ? O2 Y1 O1 92.72(8) 2_677 . ? O9 Y1 O1 143.27(8) . . ? O10 Y1 O1 74.08(7) 2_777 . ? O5 Y1 O13 83.28(8) . . ? O2 Y1 O13 75.27(8) 2_677 . ? O9 Y1 O13 74.65(8) . . ? O10 Y1 O13 142.97(8) 2_777 . ? O1 Y1 O13 71.48(8) . . ? O5 Y1 O6 127.73(8) . 2_777 ? O2 Y1 O6 71.59(7) 2_677 2_777 ? O9 Y1 O6 85.63(7) . 2_777 ? O10 Y1 O6 74.23(8) 2_777 2_777 ? O1 Y1 O6 130.22(7) . 2_777 ? O13 Y1 O6 140.53(8) . 2_777 ? O5 Y1 O5 79.18(7) . 2_777 ? O2 Y1 O5 117.55(7) 2_677 2_777 ? O9 Y1 O5 68.50(7) . 2_777 ? O10 Y1 O5 65.79(7) 2_777 2_777 ? O1 Y1 O5 137.94(7) . 2_777 ? O13 Y1 O5 141.00(7) . 2_777 ? O6 Y1 O5 49.14(6) 2_777 2_777 ? O5 Y1 C8 104.08(8) . 2_777 ? O2 Y1 C8 93.95(8) 2_677 2_777 ? O9 Y1 C8 75.59(8) . 2_777 ? O10 Y1 C8 68.62(8) 2_777 2_777 ? O1 Y1 C8 140.19(8) . 2_777 ? O13 Y1 C8 147.83(8) . 2_777 ? O6 Y1 C8 24.06(8) 2_777 2_777 ? O5 Y1 C8 25.10(7) 2_777 2_777 ? O5 Y1 Y1 45.07(5) . 2_777 ? O2 Y1 Y1 149.85(5) 2_677 2_777 ? O9 Y1 Y1 69.59(5) . 2_777 ? O10 Y1 Y1 65.67(5) 2_777 2_777 ? O1 Y1 Y1 116.42(5) . 2_777 ? O13 Y1 Y1 119.57(5) . 2_777 ? O6 Y1 Y1 82.98(5) 2_777 2_777 ? O5 Y1 Y1 34.11(4) 2_777 2_777 ? C8 Y1 Y1 59.08(6) 2_777 2_777 ? O5 Y1 Y1 141.54(5) . 2_677 ? O2 Y1 Y1 40.29(5) 2_677 2_677 ? O9 Y1 Y1 132.36(5) . 2_677 ? O10 Y1 Y1 86.13(5) 2_777 2_677 ? O1 Y1 Y1 60.97(5) . 2_677 ? O13 Y1 Y1 88.89(5) . 2_677 ? O6 Y1 Y1 79.55(5) 2_777 2_677 ? O5 Y1 Y1 125.55(4) 2_777 2_677 ? C8 Y1 Y1 102.40(6) 2_777 2_677 ? Y1 Y1 Y1 150.019(17) 2_777 2_677 ? C1 O1 Y1 117.25(19) . . ? O3 N1 O4 123.9(3) . . ? O3 N1 C4 118.5(3) . . ? O4 N1 C4 117.7(3) . . ? O1 C1 O2 123.1(3) . . ? O1 C1 C2 118.5(3) . . ? O2 C1 C2 118.5(3) . . ? C1 O2 Y1 131.2(2) . 2_677 ? O7 N2 O8 123.7(3) . . ? O7 N2 C11 118.2(3) . . ? O8 N2 C11 118.1(3) . . ? C3 C2 C7 120.0(3) . . ? C3 C2 C1 119.9(3) . . ? C7 C2 C1 120.1(3) . . ? O12 N3 O11 122.7(3) . . ? O12 N3 C18 118.8(3) . . ? O11 N3 C18 118.5(3) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C22 N4 C23 121.4(3) . . ? C22 N4 C24 120.4(3) . . ? C23 N4 C24 118.1(3) . . ? C5 C4 C3 122.8(3) . . ? C5 C4 N1 118.4(3) . . ? C3 C4 N1 118.7(3) . . ? C8 O5 Y1 171.8(2) . . ? C8 O5 Y1 83.42(18) . 2_777 ? Y1 O5 Y1 100.82(7) . 2_777 ? C4 C5 C6 118.8(3) . . ? C4 C5 H5 120.6 . . ? C6 C5 H5 120.6 . . ? C8 O6 Y1 105.23(18) . 2_777 ? C5 C6 C7 119.7(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C6 C7 C2 120.6(3) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O6 C8 O5 122.2(3) . . ? O6 C8 C9 119.2(3) . . ? O5 C8 C9 118.7(3) . . ? O6 C8 Y1 50.72(15) . 2_777 ? O5 C8 Y1 71.48(17) . 2_777 ? C9 C8 Y1 169.6(2) . 2_777 ? C15 O9 Y1 132.4(2) . . ? C10 C9 C14 120.2(3) . . ? C10 C9 C8 120.7(3) . . ? C14 C9 C8 119.1(3) . . ? C15 O10 Y1 137.6(2) . 2_777 ? C11 C10 C9 118.2(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 123.1(3) . . ? C10 C11 N2 118.3(3) . . ? C12 C11 N2 118.6(3) . . ? C11 C12 C13 118.0(3) . . ? C11 C12 H12 121.0 . . ? C13 C12 H12 121.0 . . ? C22 O13 Y1 123.3(2) . . ? C14 C13 C12 120.3(3) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C13 C14 C9 120.2(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? O10 C15 O9 126.5(3) . . ? O10 C15 C16 116.1(3) . . ? O9 C15 C16 117.5(3) . . ? C17 C16 C21 119.9(3) . . ? C17 C16 C15 118.6(3) . . ? C21 C16 C15 121.5(3) . . ? C18 C17 C16 118.6(3) . . ? C18 C17 H17 120.7 . . ? C16 C17 H17 120.7 . . ? C17 C18 C19 122.7(3) . . ? C17 C18 N3 117.9(3) . . ? C19 C18 N3 119.4(3) . . ? C20 C19 C18 118.2(3) . . ? C20 C19 H19 120.9 . . ? C18 C19 H19 120.9 . . ? C19 C20 C21 120.4(3) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C16 C21 C20 120.2(3) . . ? C16 C21 H21 119.9 . . ? C20 C21 H21 119.9 . . ? O13 C22 N4 124.9(3) . . ? O13 C22 H22 117.6 . . ? N4 C22 H22 117.6 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C22 H22 O6 0.95 2.81 3.596(4) 141.2 1_455 C22 H22 O10 0.95 2.92 3.792(4) 153.6 1_455 _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 1.360 _refine_diff_density_min -1.354 _refine_diff_density_rms 0.111 # Attachment '7b.CIF' data_7b _database_code_depnum_ccdc_archive 'CCDC 649812' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common '[Tb(3-NO2BA)3(DMF)]n' _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 N4 O13 Tb1' _chemical_formula_sum 'C24 H19 N4 O13 Tb1' _chemical_formula_weight 730.35 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.2095(2) _cell_length_b 13.1346(3) _cell_length_c 13.1596(4) _cell_angle_alpha 91.090(1) _cell_angle_beta 106.536(1) _cell_angle_gamma 104.418(2) _cell_volume 1311.26(6) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.850 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 720 _exptl_absorpt_coefficient_mu 2.774 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.5335 _exptl_absorpt_correction_T_max 0.6386 _exptl_absorpt_process_details SORTAV _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 KappaCCD' _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 18444 _diffrn_reflns_av_R_equivalents 0.1031 _diffrn_reflns_av_sigmaI/netI 0.1041 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6036 _reflns_number_gt 4729 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Hooft, 1999)' _computing_cell_refinement 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_data_reduction 'DENZO-SMN (Otwinowski & Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0480P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6036 _refine_ls_number_parameters 381 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0507 _refine_ls_wR_factor_ref 0.1109 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.74903(3) -0.00158(2) 0.54138(2) 0.01181(10) Uani 1 1 d . . . O1 O 0.9535(5) 0.1653(3) 0.5556(3) 0.0175(9) Uani 1 1 d . . . N1 N 1.2308(6) 0.5622(4) 0.5829(4) 0.0246(12) Uani 1 1 d . . . C1 C 1.0353(7) 0.1753(4) 0.4873(5) 0.0137(12) Uani 1 1 d . . . O2 O 1.0426(5) 0.0959(3) 0.4335(3) 0.0157(9) Uani 1 1 d . . . N2 N 1.1050(6) 0.3822(4) 0.8459(4) 0.0192(11) Uani 1 1 d . . . C2 C 1.1246(7) 0.2831(4) 0.4683(5) 0.0136(12) Uani 1 1 d . . . O3 O 1.1787(6) 0.5471(3) 0.6613(4) 0.0332(11) Uani 1 1 d . . . N3 N 0.0754(7) -0.2451(4) 0.8887(4) 0.0235(12) Uani 1 1 d . . . C3 C 1.1360(7) 0.3701(4) 0.5334(5) 0.0142(12) Uani 1 1 d . . . H3 H 1.0884 0.3616 0.5916 0.017 Uiso 1 1 calc R . . O4 O 1.2890(6) 0.6501(3) 0.5566(4) 0.0342(12) Uani 1 1 d . . . N4 N 1.1876(6) 0.0882(4) 0.8539(4) 0.0211(11) Uani 1 1 d . . . C4 C 1.2177(7) 0.4697(4) 0.5126(5) 0.0180(13) Uani 1 1 d . . . O5 O 0.5950(5) 0.1071(3) 0.5822(3) 0.0135(8) Uani 1 1 d . . . C5 C 1.2892(8) 0.4860(5) 0.4301(5) 0.0220(14) Uani 1 1 d . . . H5 H 1.3447 0.5553 0.4179 0.026 Uiso 1 1 calc R . . O6 O 0.3559(5) 0.1500(3) 0.5931(3) 0.0154(9) Uani 1 1 d . . . C6 C 1.2786(8) 0.3986(5) 0.3646(5) 0.0235(14) Uani 1 1 d . . . H6 H 1.3261 0.4078 0.3065 0.028 Uiso 1 1 calc R . . O7 O 1.1728(5) 0.3308(3) 0.8012(4) 0.0296(11) Uani 1 1 d . . . C7 C 1.1985(7) 0.2978(4) 0.3844(5) 0.0168(13) Uani 1 1 d . . . H7 H 1.1939 0.2382 0.3406 0.020 Uiso 1 1 calc R . . O8 O 1.1874(5) 0.4490(3) 0.9219(4) 0.0285(11) Uani 1 1 d . . . C8 C 0.5207(7) 0.1663(4) 0.6205(4) 0.0129(12) Uani 1 1 d . . . O9 O 0.6006(5) -0.1128(3) 0.6416(3) 0.0161(9) Uani 1 1 d . . . C9 C 0.6315(6) 0.2572(4) 0.7005(4) 0.0110(11) Uani 1 1 d . . . O10 O 0.3479(4) -0.0677(3) 0.6203(3) 0.0120(8) Uani 1 1 d . . . C10 C 0.8147(7) 0.2787(4) 0.7330(5) 0.0157(12) Uani 1 1 d . . . H10 H 0.8724 0.2363 0.7043 0.019 Uiso 1 1 calc R . . O11 O 0.0217(6) -0.3144(4) 0.9411(4) 0.0367(12) Uani 1 1 d . . . C11 C 0.9101(7) 0.3630(4) 0.8081(4) 0.0143(12) Uani 1 1 d . . . O12 O 0.0028(6) -0.1746(4) 0.8594(4) 0.0309(11) Uani 1 1 d . . . C12 C 0.8332(7) 0.4274(4) 0.8518(5) 0.0181(13) Uani 1 1 d . . . H12 H 0.9026 0.4855 0.9027 0.022 Uiso 1 1 calc R . . O13 O 0.9248(5) 0.0455(3) 0.7239(3) 0.0184(9) Uani 1 1 d . . . C13 C 0.6497(7) 0.4043(4) 0.8183(5) 0.0187(13) Uani 1 1 d . . . H13 H 0.5927 0.4469 0.8474 0.022 Uiso 1 1 calc R . . C14 C 0.5507(7) 0.3212(4) 0.7442(5) 0.0151(12) Uani 1 1 d . . . H14 H 0.4259 0.3068 0.7222 0.018 Uiso 1 1 calc R . . C15 C 0.4607(7) -0.1154(4) 0.6648(4) 0.0118(11) Uani 1 1 d . . . C16 C 0.4247(7) -0.1802(4) 0.7522(4) 0.0125(11) Uani 1 1 d . . . C17 C 0.2715(7) -0.1837(4) 0.7804(4) 0.0142(12) Uani 1 1 d . . . H17 H 0.1938 -0.1436 0.7461 0.017 Uiso 1 1 calc R . . C18 C 0.2347(7) -0.2453(4) 0.8577(5) 0.0168(12) Uani 1 1 d . . . C19 C 0.3399(8) -0.3080(4) 0.9089(5) 0.0214(13) Uani 1 1 d . . . H19 H 0.3085 -0.3521 0.9604 0.026 Uiso 1 1 calc R . . C20 C 0.4946(8) -0.3036(4) 0.8815(5) 0.0197(13) Uani 1 1 d . . . H20 H 0.5705 -0.3450 0.9153 0.024 Uiso 1 1 calc R . . C21 C 0.5373(7) -0.2389(4) 0.8052(4) 0.0150(12) Uani 1 1 d . . . H21 H 0.6443 -0.2347 0.7891 0.018 Uiso 1 1 calc R . . C22 C 1.0866(8) 0.0577(4) 0.7551(5) 0.0195(13) Uani 1 1 d . . . H22 H 1.1419 0.0439 0.7040 0.023 Uiso 1 1 calc R . . C23 C 1.1147(9) 0.1138(6) 0.9370(5) 0.0376(18) Uani 1 1 d . . . H23A H 1.1550 0.1901 0.9575 0.056 Uiso 1 1 calc R . . H23B H 1.1544 0.0763 0.9991 0.056 Uiso 1 1 calc R . . H23C H 0.9857 0.0921 0.9102 0.056 Uiso 1 1 calc R . . C24 C 1.3768(7) 0.0984(5) 0.8832(6) 0.0330(17) Uani 1 1 d . . . H24A H 1.4062 0.0723 0.8222 0.049 Uiso 1 1 calc R . . H24B H 1.4098 0.0568 0.9431 0.049 Uiso 1 1 calc R . . H24C H 1.4415 0.1728 0.9040 0.049 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 0.01183(15) 0.00922(14) 0.01490(16) 0.00080(10) 0.00490(11) 0.00272(10) O1 0.015(2) 0.013(2) 0.020(2) 0.0004(17) 0.0060(18) -0.0058(16) N1 0.022(3) 0.019(3) 0.026(3) -0.003(2) -0.001(2) 0.001(2) C1 0.008(3) 0.012(3) 0.020(3) -0.001(2) 0.001(2) 0.006(2) O2 0.0110(19) 0.0095(19) 0.025(2) -0.0029(17) 0.0021(17) 0.0035(15) N2 0.016(3) 0.012(2) 0.025(3) 0.000(2) 0.005(2) -0.003(2) C2 0.011(3) 0.010(3) 0.020(3) 0.008(2) 0.002(2) 0.005(2) O3 0.050(3) 0.019(2) 0.030(3) -0.007(2) 0.015(2) 0.005(2) N3 0.028(3) 0.024(3) 0.017(3) 0.000(2) 0.012(2) -0.002(2) C3 0.012(3) 0.017(3) 0.014(3) 0.003(2) 0.005(2) 0.002(2) O4 0.038(3) 0.012(2) 0.045(3) 0.000(2) 0.007(2) 0.000(2) N4 0.020(3) 0.023(3) 0.016(3) 0.001(2) 0.002(2) 0.002(2) C4 0.014(3) 0.013(3) 0.022(4) -0.001(2) 0.000(2) 0.002(2) O5 0.015(2) 0.0072(18) 0.017(2) -0.0004(16) 0.0058(16) -0.0009(15) C5 0.023(3) 0.011(3) 0.033(4) 0.012(3) 0.011(3) 0.003(2) O6 0.014(2) 0.013(2) 0.020(2) -0.0034(17) 0.0045(17) 0.0057(16) C6 0.030(3) 0.021(3) 0.029(4) 0.009(3) 0.022(3) 0.008(3) O7 0.017(2) 0.029(3) 0.038(3) -0.008(2) 0.006(2) 0.0024(19) C7 0.019(3) 0.017(3) 0.020(3) 0.010(3) 0.012(3) 0.008(2) O8 0.023(2) 0.025(2) 0.028(3) -0.008(2) 0.001(2) -0.0025(19) C8 0.020(3) 0.005(3) 0.014(3) 0.003(2) 0.006(2) 0.004(2) O9 0.015(2) 0.017(2) 0.018(2) 0.0016(17) 0.0068(17) 0.0047(16) C9 0.009(3) 0.015(3) 0.009(3) 0.006(2) 0.004(2) 0.001(2) O10 0.0122(19) 0.0093(18) 0.017(2) 0.0045(16) 0.0066(16) 0.0034(15) C10 0.020(3) 0.012(3) 0.019(3) 0.001(2) 0.010(2) 0.006(2) O11 0.044(3) 0.034(3) 0.043(3) 0.015(2) 0.033(3) 0.006(2) C11 0.014(3) 0.012(3) 0.015(3) 0.002(2) 0.005(2) 0.001(2) O12 0.029(3) 0.039(3) 0.033(3) 0.014(2) 0.019(2) 0.014(2) C12 0.021(3) 0.012(3) 0.015(3) -0.002(2) 0.002(2) -0.003(2) O13 0.016(2) 0.016(2) 0.019(2) -0.0003(17) 0.0014(17) 0.0013(16) C13 0.022(3) 0.013(3) 0.025(4) -0.001(2) 0.009(3) 0.009(2) C14 0.016(3) 0.012(3) 0.018(3) 0.001(2) 0.006(2) 0.004(2) C15 0.007(3) 0.010(3) 0.013(3) -0.002(2) 0.002(2) -0.005(2) C16 0.016(3) 0.011(3) 0.012(3) 0.002(2) 0.008(2) 0.002(2) C17 0.012(3) 0.014(3) 0.016(3) 0.001(2) 0.004(2) 0.003(2) C18 0.020(3) 0.016(3) 0.013(3) -0.002(2) 0.008(2) 0.001(2) C19 0.032(4) 0.014(3) 0.018(3) 0.002(2) 0.010(3) 0.003(3) C20 0.024(3) 0.017(3) 0.019(3) 0.002(3) 0.004(3) 0.008(2) C21 0.018(3) 0.012(3) 0.015(3) -0.002(2) 0.006(2) 0.003(2) C22 0.027(3) 0.009(3) 0.020(3) 0.000(2) 0.006(3) 0.002(2) C23 0.038(4) 0.056(5) 0.015(4) 0.000(3) 0.007(3) 0.007(4) C24 0.021(3) 0.035(4) 0.031(4) -0.002(3) -0.003(3) -0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O5 2.276(4) . ? Tb1 O2 2.307(3) 2_756 ? Tb1 O9 2.336(4) . ? Tb1 O10 2.337(4) 2_656 ? Tb1 O1 2.373(4) . ? Tb1 O13 2.400(4) . ? Tb1 O6 2.416(4) 2_656 ? Tb1 O5 2.809(3) 2_656 ? Tb1 C8 2.979(5) 2_656 ? Tb1 Tb1 3.9317(5) 2_656 ? Tb1 Tb1 4.5429(5) 2_756 ? O1 C1 1.256(7) . ? N1 O3 1.226(7) . ? N1 O4 1.231(7) . ? N1 C4 1.475(8) . ? C1 O2 1.273(6) . ? C1 C2 1.485(7) . ? O2 Tb1 2.307(3) 2_756 ? N2 O7 1.212(6) . ? N2 O8 1.230(6) . ? N2 C11 1.487(7) . ? C2 C3 1.382(8) . ? C2 C7 1.398(8) . ? N3 O11 1.223(6) . ? N3 O12 1.233(6) . ? N3 C18 1.478(7) . ? C3 C4 1.385(8) . ? C3 H3 0.9500 . ? N4 C22 1.319(7) . ? N4 C23 1.458(8) . ? N4 C24 1.461(7) . ? C4 C5 1.370(9) . ? O5 C8 1.275(6) . ? O5 Tb1 2.809(3) 2_656 ? C5 C6 1.393(9) . ? C5 H5 0.9500 . ? O6 C8 1.258(6) . ? O6 Tb1 2.416(4) 2_656 ? C6 C7 1.389(8) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.493(7) . ? C8 Tb1 2.979(5) 2_656 ? O9 C15 1.263(6) . ? C9 C10 1.394(7) . ? C9 C14 1.397(7) . ? O10 C15 1.259(6) . ? O10 Tb1 2.337(4) 2_656 ? C10 C11 1.379(7) . ? C10 H10 0.9500 . ? C11 C12 1.378(8) . ? C12 C13 1.395(8) . ? C12 H12 0.9500 . ? O13 C22 1.241(7) . ? C13 C14 1.368(8) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? C15 C16 1.497(8) . ? C16 C21 1.394(7) . ? C16 C17 1.400(7) . ? C17 C18 1.364(8) . ? C17 H17 0.9500 . ? C18 C19 1.386(8) . ? C19 C20 1.404(8) . ? C19 H19 0.9500 . ? C20 C21 1.391(8) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? 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 Tb1 O2 158.68(14) . 2_756 ? O5 Tb1 O9 81.59(13) . . ? O2 Tb1 O9 90.84(13) 2_756 . ? O5 Tb1 O10 77.68(13) . 2_656 ? O2 Tb1 O10 120.93(13) 2_756 2_656 ? O9 Tb1 O10 132.67(12) . 2_656 ? O5 Tb1 O1 79.52(13) . . ? O2 Tb1 O1 94.79(13) 2_756 . ? O9 Tb1 O1 141.54(14) . . ? O10 Tb1 O1 74.72(13) 2_656 . ? O5 Tb1 O13 83.64(13) . . ? O2 Tb1 O13 75.10(13) 2_756 . ? O9 Tb1 O13 73.84(13) . . ? O10 Tb1 O13 143.34(12) 2_656 . ? O1 Tb1 O13 71.01(13) . . ? O5 Tb1 O6 128.03(12) . 2_656 ? O2 Tb1 O6 70.79(12) 2_756 2_656 ? O9 Tb1 O6 86.26(13) . 2_656 ? O10 Tb1 O6 74.43(12) 2_656 2_656 ? O1 Tb1 O6 131.40(13) . 2_656 ? O13 Tb1 O6 140.00(12) . 2_656 ? O5 Tb1 O5 79.25(12) . 2_656 ? O2 Tb1 O5 116.64(12) 2_756 2_656 ? O9 Tb1 O5 68.94(12) . 2_656 ? O10 Tb1 O5 65.66(11) 2_656 2_656 ? O1 Tb1 O5 138.08(12) . 2_656 ? O13 Tb1 O5 140.79(12) . 2_656 ? O6 Tb1 O5 49.42(11) 2_656 2_656 ? O5 Tb1 C8 104.29(14) . 2_656 ? O2 Tb1 C8 93.05(14) 2_756 2_656 ? O9 Tb1 C8 76.08(14) . 2_656 ? O10 Tb1 C8 68.73(13) 2_656 2_656 ? O1 Tb1 C8 141.22(14) . 2_656 ? O13 Tb1 C8 147.34(14) . 2_656 ? O6 Tb1 C8 24.20(13) 2_656 2_656 ? O5 Tb1 C8 25.24(13) 2_656 2_656 ? O5 Tb1 Tb1 44.59(9) . 2_656 ? O2 Tb1 Tb1 149.28(9) 2_756 2_656 ? O9 Tb1 Tb1 70.04(9) . 2_656 ? O10 Tb1 Tb1 65.29(8) 2_656 2_656 ? O1 Tb1 Tb1 115.24(9) . 2_656 ? O13 Tb1 Tb1 119.31(9) . 2_656 ? O6 Tb1 Tb1 83.79(8) 2_656 2_656 ? O5 Tb1 Tb1 34.66(7) 2_656 2_656 ? C8 Tb1 Tb1 59.77(10) 2_656 2_656 ? O5 Tb1 Tb1 142.30(9) . 2_756 ? O2 Tb1 Tb1 40.16(10) 2_756 2_756 ? O9 Tb1 Tb1 130.98(9) . 2_756 ? O10 Tb1 Tb1 87.73(9) 2_656 2_756 ? O1 Tb1 Tb1 63.06(9) . 2_756 ? O13 Tb1 Tb1 88.19(9) . 2_756 ? O6 Tb1 Tb1 79.10(9) 2_656 2_756 ? O5 Tb1 Tb1 125.82(8) 2_656 2_756 ? C8 Tb1 Tb1 102.30(11) 2_656 2_756 ? Tb1 Tb1 Tb1 151.186(15) 2_656 2_756 ? C1 O1 Tb1 114.9(3) . . ? O3 N1 O4 124.3(5) . . ? O3 N1 C4 118.5(5) . . ? O4 N1 C4 117.2(6) . . ? O1 C1 O2 121.9(5) . . ? O1 C1 C2 118.9(5) . . ? O2 C1 C2 119.1(5) . . ? C1 O2 Tb1 131.7(3) . 2_756 ? O7 N2 O8 124.0(5) . . ? O7 N2 C11 118.5(5) . . ? O8 N2 C11 117.5(5) . . ? C3 C2 C7 119.2(5) . . ? C3 C2 C1 120.4(5) . . ? C7 C2 C1 120.3(5) . . ? O11 N3 O12 123.4(5) . . ? O11 N3 C18 119.0(5) . . ? O12 N3 C18 117.6(5) . . ? C2 C3 C4 119.0(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C22 N4 C23 121.2(5) . . ? C22 N4 C24 120.9(6) . . ? C23 N4 C24 117.9(5) . . ? C5 C4 C3 122.7(5) . . ? C5 C4 N1 118.5(5) . . ? C3 C4 N1 118.8(5) . . ? C8 O5 Tb1 170.9(4) . . ? C8 O5 Tb1 84.9(3) . 2_656 ? Tb1 O5 Tb1 100.75(12) . 2_656 ? C4 C5 C6 118.4(5) . . ? C4 C5 H5 120.8 . . ? C6 C5 H5 120.8 . . ? C8 O6 Tb1 103.9(3) . 2_656 ? C7 C6 C5 119.9(6) . . ? C7 C6 H6 120.0 . . ? C5 C6 H6 120.0 . . ? C6 C7 C2 120.7(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O6 C8 O5 121.8(5) . . ? O6 C8 C9 118.8(5) . . ? O5 C8 C9 119.4(5) . . ? O6 C8 Tb1 51.9(3) . 2_656 ? O5 C8 Tb1 69.9(3) . 2_656 ? C9 C8 Tb1 170.4(4) . 2_656 ? C15 O9 Tb1 131.9(3) . . ? C10 C9 C14 119.5(5) . . ? C10 C9 C8 120.8(5) . . ? C14 C9 C8 119.7(5) . . ? C15 O10 Tb1 139.2(4) . 2_656 ? C11 C10 C9 118.3(5) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C12 C11 C10 123.2(5) . . ? C12 C11 N2 118.9(5) . . ? C10 C11 N2 117.8(5) . . ? C11 C12 C13 117.5(5) . . ? C11 C12 H12 121.2 . . ? C13 C12 H12 121.2 . . ? C22 O13 Tb1 123.6(4) . . ? C14 C13 C12 120.9(5) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C9 120.6(5) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O10 C15 O9 125.3(5) . . ? O10 C15 C16 116.9(5) . . ? O9 C15 C16 117.8(5) . . ? C21 C16 C17 118.8(5) . . ? C21 C16 C15 122.1(5) . . ? C17 C16 C15 119.0(5) . . ? C18 C17 C16 119.5(5) . . ? C18 C17 H17 120.3 . . ? C16 C17 H17 120.3 . . ? C17 C18 C19 123.2(5) . . ? C17 C18 N3 118.6(5) . . ? C19 C18 N3 118.2(5) . . ? C18 C19 C20 117.3(6) . . ? C18 C19 H19 121.4 . . ? C20 C19 H19 121.4 . . ? C21 C20 C19 120.4(5) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C16 120.7(5) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? O13 C22 N4 125.0(6) . . ? O13 C22 H22 117.5 . . ? N4 C22 H22 117.5 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C22 H22 O6 0.95 2.73 3.515(7) 139.9 1_655 C22 H22 O10 0.95 2.91 3.779(7) 153.0 1_655 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.611 _refine_diff_density_min -1.989 _refine_diff_density_rms 0.222 # Attachment '8.CIF' data_8 _database_code_depnum_ccdc_archive 'CCDC 649813' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly[hexa(3-nitrobenzoato)(dimethylsulphoxide)bis(aqua)bisyttrium (III)].DMSO solvate ; _chemical_name_common SH5DMSO _chemical_melting_point ? _chemical_formula_moiety 'C48 H46 N6 O29 S3 Y2' _chemical_formula_sum 'C48 H46 N6 O29 S3 Y2' _chemical_formula_weight 1444.91 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Y Y -2.7962 3.5667 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4247(5) _cell_length_b 16.1016(8) _cell_length_c 18.7135(6) _cell_angle_alpha 93.351(2) _cell_angle_beta 101.038(2) _cell_angle_gamma 106.429(3) _cell_volume 2935.9(2) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.634 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 2.169 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6587 _exptl_absorpt_correction_T_max 0.8287 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 22598 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0899 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 27.50 _reflns_number_total 12967 _reflns_number_gt 8913 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12967 _refine_ls_number_parameters 799 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0852 _refine_ls_R_factor_gt 0.0445 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0902 _refine_ls_goodness_of_fit_ref 0.987 _refine_ls_restrained_S_all 0.987 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Y1 Y 0.49581(3) 0.53686(2) 0.392719(16) 0.01114(8) Uani 1 1 d . . . S1 S 0.14691(9) 0.51946(6) 0.07891(5) 0.0194(2) Uani 1 1 d . . . O1 O 0.6177(2) 0.67079(14) 0.46864(11) 0.0153(5) Uani 1 1 d . . . N1 N 0.8825(4) 0.7761(3) 0.78982(18) 0.0379(9) Uani 1 1 d . . . C1 C 0.6346(3) 0.6552(2) 0.53425(17) 0.0146(7) Uani 1 1 d . . . Y2 Y 0.48210(3) 0.50845(2) 0.106440(16) 0.01117(8) Uani 1 1 d . . . S2 S 1.01685(11) 0.70438(7) 0.50372(6) 0.0332(3) Uani 1 1 d . . . O2 O 0.5914(2) 0.57907(14) 0.55139(12) 0.0172(5) Uani 1 1 d . . . N2 N 0.3290(3) 0.8234(2) 0.25433(16) 0.0267(7) Uani 1 1 d . . . C2 C 0.7061(3) 0.7297(2) 0.59319(16) 0.0140(7) Uani 1 1 d . . . S3 S -0.01483(11) 0.54115(8) 0.32547(5) 0.0349(3) Uani 1 1 d . . . O3 O 0.9215(3) 0.8387(2) 0.83766(14) 0.0489(9) Uani 1 1 d . . . N3 N 0.6976(3) 0.9595(2) 0.38857(17) 0.0276(8) Uani 1 1 d . . . C3 C 0.7633(4) 0.7168(2) 0.66296(18) 0.0196(8) Uani 1 1 d . . . H3 H 0.7589 0.6597 0.6752 0.023 Uiso 1 1 calc R . . O4 O 0.8833(4) 0.7038(2) 0.80198(16) 0.0646(11) Uani 1 1 d . . . N4 N 0.3514(3) 0.1156(2) 0.08162(17) 0.0266(8) Uani 1 1 d . . . C4 C 0.8275(4) 0.7895(2) 0.71487(17) 0.0214(8) Uani 1 1 d . . . O5 O 0.3340(2) 0.58939(15) 0.42490(11) 0.0169(5) Uani 1 1 d . . . N5 N 0.7740(3) 0.1504(2) 0.15473(19) 0.0302(8) Uani 1 1 d . . . C5 C 0.8379(4) 0.8730(3) 0.6992(2) 0.0297(10) Uani 1 1 d . . . H5 H 0.8830 0.9212 0.7359 0.036 Uiso 1 1 calc R . . O6 O 0.3153(3) 0.64836(15) 0.53203(12) 0.0210(6) Uani 1 1 d . . . N6 N 1.0223(3) 0.8499(2) 0.23642(18) 0.0314(8) Uani 1 1 d . . . C6 C 0.7821(4) 0.8858(2) 0.6297(2) 0.0289(9) Uani 1 1 d . . . H6 H 0.7891 0.9431 0.6176 0.035 Uiso 1 1 calc R . . O7 O 0.3042(3) 0.75531(19) 0.21481(14) 0.0428(8) Uani 1 1 d . . . C7 C 0.7155(4) 0.8147(2) 0.57747(19) 0.0215(8) Uani 1 1 d . . . H7 H 0.6751 0.8238 0.5298 0.026 Uiso 1 1 calc R . . O8 O 0.3515(4) 0.8947(2) 0.23185(15) 0.0506(9) Uani 1 1 d . . . C8 C 0.3269(3) 0.6524(2) 0.46720(18) 0.0155(7) Uani 1 1 d . . . O9 O 0.5817(2) 0.63227(14) 0.31724(11) 0.0178(5) Uani 1 1 d . . . C9 C 0.3358(3) 0.7371(2) 0.43504(17) 0.0161(7) Uani 1 1 d . . . O10 O 0.5697(2) 0.61918(15) 0.19689(11) 0.0183(5) Uani 1 1 d . . . C10 C 0.3255(3) 0.7402(2) 0.36082(17) 0.0172(8) Uani 1 1 d . . . H10 H 0.3116 0.6890 0.3287 0.021 Uiso 1 1 calc R . . O11 O 0.7266(3) 0.93328(17) 0.44774(14) 0.0413(8) Uani 1 1 d . . . C11 C 0.3357(4) 0.8198(2) 0.33393(18) 0.0209(8) Uani 1 1 d . . . O12 O 0.6772(3) 1.03035(16) 0.38199(14) 0.0348(7) Uani 1 1 d . . . C12 C 0.3545(4) 0.8958(2) 0.3774(2) 0.0274(9) Uani 1 1 d . . . H12 H 0.3605 0.9492 0.3572 0.033 Uiso 1 1 calc R . . O13 O 0.5224(2) 0.42455(14) 0.31569(11) 0.0165(5) Uani 1 1 d . . . C13 C 0.3643(4) 0.8917(2) 0.4523(2) 0.0275(9) Uani 1 1 d . . . H13 H 0.3774 0.9430 0.4840 0.033 Uiso 1 1 calc R . . O14 O 0.4376(2) 0.42602(15) 0.19725(11) 0.0175(5) Uani 1 1 d . . . C14 C 0.3550(4) 0.8132(2) 0.48081(19) 0.0224(8) Uani 1 1 d . . . H14 H 0.3618 0.8112 0.5320 0.027 Uiso 1 1 calc R . . O15 O 0.3491(3) 0.15740(18) 0.02964(14) 0.0320(7) Uani 1 1 d . . . C15 C 0.5900(3) 0.6637(2) 0.25778(17) 0.0133(7) Uani 1 1 d . . . O16 O 0.3072(4) 0.03602(18) 0.07701(16) 0.0490(9) Uani 1 1 d . . . C16 C 0.6311(3) 0.7602(2) 0.25887(17) 0.0136(7) Uani 1 1 d . . . O17 O 0.6161(3) 0.41407(15) 0.10720(13) 0.0217(6) Uani 1 1 d . . . C17 C 0.6522(4) 0.8137(2) 0.32384(18) 0.0169(8) Uani 1 1 d . . . H17 H 0.6456 0.7898 0.3687 0.020 Uiso 1 1 calc R . . O18 O 0.5750(3) 0.41629(16) -0.01322(13) 0.0269(6) Uani 1 1 d . . . C18 C 0.6828(4) 0.9020(2) 0.32109(18) 0.0208(8) Uani 1 1 d . . . O19 O 0.8099(3) 0.1962(2) 0.21407(15) 0.0433(8) Uani 1 1 d . . . C19 C 0.6976(4) 0.9408(2) 0.25785(19) 0.0270(9) Uani 1 1 d . . . H19 H 0.7200 1.0023 0.2585 0.032 Uiso 1 1 calc R . . O20 O 0.7749(4) 0.07468(19) 0.14676(18) 0.0542(9) Uani 1 1 d . . . C20 C 0.6787(4) 0.8874(2) 0.19370(19) 0.0235(9) Uani 1 1 d . . . H20 H 0.6892 0.9120 0.1494 0.028 Uiso 1 1 calc R . . O21 O 0.6871(2) 0.58870(15) 0.08082(12) 0.0177(5) Uani 1 1 d . . . C21 C 0.6445(4) 0.7982(2) 0.19443(17) 0.0175(8) Uani 1 1 d . . . H21 H 0.6298 0.7617 0.1500 0.021 Uiso 1 1 calc R . . O22 O 0.6888(2) 0.60916(15) -0.03667(11) 0.0176(5) Uani 1 1 d . . . C22 C 0.4802(3) 0.3893(2) 0.25048(17) 0.0143(7) Uani 1 1 d . . . O23 O 1.0847(4) 0.9262(2) 0.25769(16) 0.0573(10) Uani 1 1 d . . . C23 C 0.4781(3) 0.2956(2) 0.23591(17) 0.0135(7) Uani 1 1 d . . . O24 O 0.9942(3) 0.7951(2) 0.27702(15) 0.0482(9) Uani 1 1 d . . . C24 C 0.4204(3) 0.2506(2) 0.16624(18) 0.0158(7) Uani 1 1 d . . . H24 H 0.3878 0.2790 0.1268 0.019 Uiso 1 1 calc R . . O25 O 0.7091(2) 0.51640(15) 0.43243(11) 0.0165(5) Uani 1 1 d . . . C25 C 0.4119(4) 0.1631(2) 0.15585(19) 0.0199(8) Uani 1 1 d . . . O26 O 0.3064(2) 0.49827(16) 0.29427(12) 0.0210(6) Uani 1 1 d . . . C26 C 0.4572(4) 0.1192(2) 0.2113(2) 0.0272(9) Uani 1 1 d . . . H26 H 0.4468 0.0587 0.2028 0.033 Uiso 1 1 calc R . . O27 O 0.2842(2) 0.53432(17) 0.13144(12) 0.0240(6) Uani 1 1 d . . . C27 C 0.5187(4) 0.1657(2) 0.2802(2) 0.0247(9) Uani 1 1 d . . . H27 H 0.5544 0.1376 0.3191 0.030 Uiso 1 1 calc R . . O28 O 0.9046(3) 0.63770(18) 0.52719(15) 0.0364(7) Uani 1 1 d . . . C28 C 0.5279(4) 0.2533(2) 0.29228(18) 0.0186(8) Uani 1 1 d . . . H28 H 0.5687 0.2845 0.3397 0.022 Uiso 1 1 calc R . . O29 O 0.0810(3) 0.5464(2) 0.27339(13) 0.0340(7) Uani 1 1 d . . . C29 C 0.6149(4) 0.3836(2) 0.04371(19) 0.0184(8) Uani 1 1 d . . . C30 C 0.6564(3) 0.3029(2) 0.03478(17) 0.0140(7) Uani 1 1 d . . . C31 C 0.7028(3) 0.2680(2) 0.09749(18) 0.0149(7) Uani 1 1 d . . . H31 H 0.7166 0.2981 0.1449 0.018 Uiso 1 1 calc R . . C32 C 0.7283(4) 0.1887(2) 0.08907(19) 0.0202(8) Uani 1 1 d . . . C33 C 0.7094(4) 0.1431(3) 0.0208(2) 0.0305(10) Uani 1 1 d . . . H33 H 0.7249 0.0879 0.0165 0.037 Uiso 1 1 calc R . . C34 C 0.6674(4) 0.1801(3) -0.0408(2) 0.0320(10) Uani 1 1 d . . . H34 H 0.6565 0.1509 -0.0882 0.038 Uiso 1 1 calc R . . C35 C 0.6413(4) 0.2591(2) -0.03399(18) 0.0228(8) Uani 1 1 d . . . H35 H 0.6127 0.2840 -0.0768 0.027 Uiso 1 1 calc R . . C36 C 0.7310(3) 0.6317(2) 0.03182(18) 0.0158(7) Uani 1 1 d . . . C37 C 0.8410(3) 0.7171(2) 0.05752(17) 0.0148(7) Uani 1 1 d . . . C38 C 0.8859(3) 0.7425(2) 0.13213(18) 0.0170(8) Uani 1 1 d . . . H38 H 0.8526 0.7051 0.1662 0.020 Uiso 1 1 calc R . . C39 C 0.9806(4) 0.8237(2) 0.15606(19) 0.0234(8) Uani 1 1 d . . . C40 C 1.0327(4) 0.8800(2) 0.1090(2) 0.0300(9) Uani 1 1 d . . . H40 H 1.0963 0.9359 0.1271 0.036 Uiso 1 1 calc R . . C41 C 0.9895(4) 0.8527(3) 0.0343(2) 0.0299(9) Uani 1 1 d . . . H41 H 1.0257 0.8896 0.0006 0.036 Uiso 1 1 calc R . . C42 C 0.8938(4) 0.7721(2) 0.00847(19) 0.0200(8) Uani 1 1 d . . . H42 H 0.8643 0.7543 -0.0428 0.024 Uiso 1 1 calc R . . C43 C 0.0332(4) 0.4284(3) 0.1055(2) 0.0296(9) Uani 1 1 d . . . H43A H 0.0615 0.3764 0.0964 0.044 Uiso 1 1 calc R . . H43B H -0.0599 0.4194 0.0770 0.044 Uiso 1 1 calc R . . H43C H 0.0349 0.4391 0.1578 0.044 Uiso 1 1 calc R . . C44 C 0.0795(4) 0.6016(2) 0.10976(19) 0.0256(9) Uani 1 1 d . . . H44A H 0.0862 0.6030 0.1628 0.038 Uiso 1 1 calc R . . H44B H -0.0167 0.5885 0.0847 0.038 Uiso 1 1 calc R . . H44C H 0.1320 0.6584 0.0988 0.038 Uiso 1 1 calc R . . C45 C 0.9339(5) 0.7650(4) 0.4451(3) 0.0574(15) Uani 1 1 d . . . H45A H 0.8721 0.7260 0.4025 0.086 Uiso 1 1 calc R . . H45B H 1.0026 0.8105 0.4285 0.086 Uiso 1 1 calc R . . H45C H 0.8810 0.7921 0.4718 0.086 Uiso 1 1 calc R . . C46 C 1.0889(5) 0.7857(3) 0.5814(2) 0.0509(14) Uani 1 1 d . . . H46A H 1.0151 0.8007 0.5995 0.076 Uiso 1 1 calc R . . H46B H 1.1488 0.8379 0.5671 0.076 Uiso 1 1 calc R . . H46C H 1.1423 0.7631 0.6202 0.076 Uiso 1 1 calc R . . C47 C -0.1657(4) 0.5509(4) 0.2725(2) 0.0502(14) Uani 1 1 d . . . H47A H -0.1502 0.6107 0.2599 0.075 Uiso 1 1 calc R . . H47B H -0.2381 0.5375 0.3004 0.075 Uiso 1 1 calc R . . H47C H -0.1935 0.5101 0.2275 0.075 Uiso 1 1 calc R . . C48 C -0.0808(7) 0.4271(4) 0.3337(3) 0.093(2) Uani 1 1 d . . . H48A H -0.1051 0.3935 0.2851 0.139 Uiso 1 1 calc R . . H48B H -0.1625 0.4171 0.3545 0.139 Uiso 1 1 calc R . . H48C H -0.0109 0.4085 0.3659 0.139 Uiso 1 1 calc R . . H3O H 0.2283 0.5179 0.2908 0.056 Uiso 1 1 d . . . H4O H 0.3086 0.4880 0.2579 0.055 Uiso 1 1 d . . . H1O H 0.7005 0.4713 0.4433 0.000 Uiso 1 1 d . . . H2O H 0.7873 0.5591 0.4681 0.080 Uiso 1 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 Y1 0.01569(18) 0.00968(16) 0.00877(16) -0.00093(12) 0.00404(13) 0.00442(14) S1 0.0199(5) 0.0248(5) 0.0152(4) -0.0014(4) 0.0029(4) 0.0109(4) O1 0.0212(13) 0.0137(12) 0.0088(12) -0.0034(9) 0.0025(10) 0.0030(10) N1 0.033(2) 0.043(2) 0.0237(19) 0.0032(17) 0.0023(16) -0.0070(19) C1 0.0151(18) 0.0155(18) 0.0152(18) -0.0008(14) 0.0065(14) 0.0061(15) Y2 0.01673(18) 0.00933(16) 0.00780(16) -0.00141(12) 0.00267(13) 0.00494(14) S2 0.0258(6) 0.0338(6) 0.0367(6) -0.0051(5) 0.0044(5) 0.0074(5) O2 0.0200(13) 0.0126(13) 0.0195(13) -0.0005(10) 0.0069(10) 0.0045(11) N2 0.031(2) 0.032(2) 0.0210(17) 0.0076(15) 0.0079(15) 0.0132(16) C2 0.0161(18) 0.0169(18) 0.0084(16) -0.0027(13) 0.0040(14) 0.0040(15) S3 0.0271(6) 0.0640(8) 0.0170(5) -0.0060(5) 0.0040(4) 0.0216(6) O3 0.052(2) 0.061(2) 0.0145(15) -0.0108(14) 0.0006(14) -0.0058(18) N3 0.042(2) 0.0135(17) 0.0256(18) -0.0059(14) 0.0116(16) 0.0038(15) C3 0.021(2) 0.0187(19) 0.0178(18) 0.0039(15) 0.0087(15) 0.0001(16) O4 0.095(3) 0.040(2) 0.0363(19) 0.0123(16) -0.0195(19) 0.005(2) N4 0.032(2) 0.0186(18) 0.0269(18) -0.0108(14) 0.0112(15) 0.0043(15) C4 0.021(2) 0.029(2) 0.0091(17) -0.0004(15) 0.0041(15) -0.0002(17) O5 0.0232(14) 0.0163(13) 0.0142(12) -0.0019(10) 0.0062(10) 0.0099(11) N5 0.031(2) 0.030(2) 0.040(2) 0.0203(17) 0.0167(16) 0.0156(17) C5 0.034(2) 0.023(2) 0.022(2) -0.0130(16) 0.0078(18) -0.0060(18) O6 0.0356(16) 0.0220(14) 0.0096(12) 0.0007(10) 0.0069(11) 0.0143(12) N6 0.026(2) 0.034(2) 0.0255(19) -0.0168(16) -0.0048(15) 0.0066(17) C6 0.042(3) 0.014(2) 0.026(2) -0.0064(16) 0.0035(19) 0.0048(18) O7 0.065(2) 0.0356(18) 0.0176(15) -0.0003(13) 0.0062(14) 0.0020(16) C7 0.026(2) 0.0169(19) 0.0177(19) -0.0020(15) 0.0027(16) 0.0022(16) O8 0.097(3) 0.0353(19) 0.0358(17) 0.0200(15) 0.0299(18) 0.0315(19) C8 0.0144(18) 0.0176(18) 0.0172(18) -0.0005(14) 0.0036(14) 0.0095(15) O9 0.0311(15) 0.0103(12) 0.0111(12) 0.0000(9) 0.0078(11) 0.0031(11) C9 0.0161(18) 0.0177(19) 0.0165(18) 0.0003(14) 0.0056(14) 0.0072(15) O10 0.0301(15) 0.0127(12) 0.0099(12) -0.0030(9) 0.0047(10) 0.0038(11) C10 0.0172(19) 0.0176(19) 0.0166(18) -0.0019(14) 0.0024(15) 0.0067(15) O11 0.086(3) 0.0203(15) 0.0169(14) -0.0014(12) 0.0100(15) 0.0162(16) C11 0.023(2) 0.025(2) 0.0174(18) 0.0046(15) 0.0056(16) 0.0109(17) O12 0.061(2) 0.0127(14) 0.0324(16) -0.0027(12) 0.0128(14) 0.0134(14) C12 0.036(2) 0.018(2) 0.035(2) 0.0068(17) 0.0157(19) 0.0117(18) O13 0.0228(14) 0.0149(13) 0.0116(12) -0.0043(10) 0.0025(10) 0.0075(11) C13 0.041(3) 0.017(2) 0.025(2) -0.0044(16) 0.0092(18) 0.0096(18) O14 0.0290(15) 0.0153(13) 0.0109(12) 0.0026(10) 0.0076(10) 0.0085(11) C14 0.028(2) 0.024(2) 0.0158(18) -0.0041(15) 0.0069(16) 0.0090(18) O15 0.0426(18) 0.0293(16) 0.0214(14) -0.0084(12) 0.0044(13) 0.0104(14) C15 0.0118(18) 0.0157(18) 0.0122(17) -0.0030(14) 0.0035(14) 0.0044(14) O16 0.078(3) 0.0143(15) 0.0441(18) -0.0134(13) 0.0152(17) -0.0013(16) C16 0.0141(18) 0.0133(17) 0.0117(16) -0.0021(13) 0.0003(14) 0.0039(14) O17 0.0287(15) 0.0174(13) 0.0254(14) 0.0030(11) 0.0143(12) 0.0113(12) C17 0.023(2) 0.0125(17) 0.0144(17) 0.0022(14) 0.0052(15) 0.0042(15) O18 0.0262(15) 0.0194(14) 0.0308(15) 0.0115(12) -0.0024(12) 0.0039(12) C18 0.025(2) 0.0166(19) 0.0190(19) -0.0061(15) 0.0059(16) 0.0046(16) O19 0.061(2) 0.061(2) 0.0229(16) 0.0188(15) 0.0107(15) 0.0387(19) C19 0.042(3) 0.0126(19) 0.027(2) 0.0054(16) 0.0120(19) 0.0072(18) O20 0.068(2) 0.0228(17) 0.079(2) 0.0259(16) 0.0143(19) 0.0236(17) C20 0.037(2) 0.019(2) 0.0166(19) 0.0034(15) 0.0087(17) 0.0093(18) O21 0.0200(13) 0.0155(13) 0.0158(12) -0.0004(10) 0.0048(10) 0.0026(11) C21 0.024(2) 0.0160(18) 0.0124(17) -0.0002(14) 0.0041(15) 0.0058(16) O22 0.0256(14) 0.0157(13) 0.0099(12) -0.0039(9) 0.0025(10) 0.0054(11) C22 0.0174(19) 0.0127(17) 0.0154(18) 0.0001(14) 0.0079(14) 0.0063(15) O23 0.076(3) 0.0299(19) 0.0431(19) -0.0235(15) -0.0095(18) 0.0006(18) C23 0.0153(18) 0.0096(16) 0.0165(17) 0.0012(13) 0.0083(14) 0.0023(14) O24 0.068(2) 0.042(2) 0.0215(16) -0.0062(14) 0.0000(15) 0.0026(18) C24 0.0183(19) 0.0126(17) 0.0176(18) 0.0017(14) 0.0085(15) 0.0035(15) O25 0.0229(14) 0.0134(12) 0.0143(12) 0.0036(9) 0.0055(10) 0.0061(11) C25 0.021(2) 0.0134(18) 0.0225(19) -0.0066(15) 0.0105(16) -0.0005(16) O26 0.0234(14) 0.0304(15) 0.0130(12) -0.0027(10) 0.0039(10) 0.0151(12) C26 0.036(2) 0.0104(18) 0.042(2) 0.0055(17) 0.0188(19) 0.0102(17) O27 0.0199(14) 0.0337(16) 0.0193(13) -0.0091(11) 0.0006(11) 0.0141(12) C27 0.036(2) 0.0168(19) 0.026(2) 0.0064(16) 0.0094(18) 0.0133(18) O28 0.0268(16) 0.0275(16) 0.0420(17) -0.0030(13) -0.0060(13) -0.0018(13) C28 0.024(2) 0.0186(19) 0.0168(18) 0.0005(15) 0.0077(15) 0.0106(16) O29 0.0230(15) 0.064(2) 0.0202(14) 0.0012(13) 0.0060(12) 0.0217(15) C29 0.0157(19) 0.0156(18) 0.0224(19) 0.0070(15) 0.0024(15) 0.0027(15) C30 0.0152(18) 0.0107(17) 0.0163(17) 0.0020(13) 0.0050(14) 0.0032(14) C31 0.0166(18) 0.0149(18) 0.0139(17) 0.0008(14) 0.0055(14) 0.0047(15) C32 0.020(2) 0.021(2) 0.0239(19) 0.0098(16) 0.0096(16) 0.0085(16) C33 0.036(2) 0.021(2) 0.042(2) 0.0014(18) 0.022(2) 0.0121(19) C34 0.043(3) 0.028(2) 0.025(2) -0.0051(18) 0.0125(19) 0.010(2) C35 0.028(2) 0.028(2) 0.0130(18) 0.0019(15) 0.0041(16) 0.0083(18) C36 0.0166(19) 0.0144(18) 0.0177(18) -0.0013(14) 0.0065(15) 0.0058(15) C37 0.0160(18) 0.0144(18) 0.0147(17) -0.0018(14) 0.0021(14) 0.0075(15) C38 0.0176(19) 0.0176(19) 0.0168(18) -0.0027(14) 0.0037(15) 0.0076(16) C39 0.026(2) 0.0167(19) 0.024(2) -0.0085(16) 0.0002(17) 0.0058(17) C40 0.027(2) 0.017(2) 0.039(2) -0.0044(18) 0.0012(19) 0.0002(17) C41 0.032(2) 0.023(2) 0.035(2) 0.0080(18) 0.0135(19) 0.0045(19) C42 0.020(2) 0.020(2) 0.0189(18) 0.0016(15) 0.0064(15) 0.0038(16) C43 0.029(2) 0.027(2) 0.029(2) 0.0013(17) 0.0036(18) 0.0043(19) C44 0.027(2) 0.026(2) 0.027(2) 0.0024(17) 0.0040(17) 0.0150(18) C45 0.052(3) 0.075(4) 0.055(3) 0.028(3) 0.022(3) 0.023(3) C46 0.041(3) 0.048(3) 0.045(3) -0.010(2) 0.014(2) -0.016(2) C47 0.032(3) 0.093(4) 0.045(3) 0.030(3) 0.020(2) 0.037(3) C48 0.141(6) 0.092(5) 0.111(5) 0.066(4) 0.096(5) 0.081(5) _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 Y1 O2 2.244(2) 2_666 ? Y1 O5 2.249(2) . ? Y1 O9 2.262(2) . ? Y1 O25 2.327(2) . ? Y1 O26 2.336(2) . ? Y1 O13 2.357(2) . ? Y1 O1 2.384(2) . ? Y1 O2 2.919(2) . ? Y1 C1 3.021(3) . ? S1 O27 1.521(2) . ? S1 C43 1.769(4) . ? S1 C44 1.779(4) . ? O1 C1 1.257(4) . ? N1 O4 1.202(5) . ? N1 O3 1.227(4) . ? N1 C4 1.462(5) . ? C1 O2 1.264(4) . ? C1 C2 1.495(4) . ? Y2 O10 2.239(2) . ? Y2 O14 2.254(2) . ? Y2 O18 2.264(2) 2_665 ? Y2 O21 2.318(2) . ? Y2 O22 2.319(2) 2_665 ? Y2 O17 2.336(2) . ? Y2 O27 2.341(2) . ? Y2 C29 3.042(4) . ? S2 O28 1.502(3) . ? S2 C45 1.774(5) . ? S2 C46 1.787(4) . ? O2 Y1 2.244(2) 2_666 ? N2 O7 1.219(4) . ? N2 O8 1.222(4) . ? N2 C11 1.483(4) . ? C2 C3 1.381(4) . ? C2 C7 1.397(5) . ? S3 O29 1.514(3) . ? S3 C47 1.744(4) . ? S3 C48 1.797(6) . ? N3 O11 1.222(4) . ? N3 O12 1.227(4) . ? N3 C18 1.478(4) . ? C3 C4 1.392(5) . ? C3 H3 0.9500 . ? N4 O15 1.215(4) . ? N4 O16 1.225(4) . ? N4 C25 1.476(4) . ? C4 C5 1.373(5) . ? O5 C8 1.278(4) . ? N5 O20 1.222(4) . ? N5 O19 1.228(4) . ? N5 C32 1.466(4) . ? C5 C6 1.371(5) . ? C5 H5 0.9500 . ? O6 C8 1.246(4) . ? N6 O24 1.207(4) . ? N6 O23 1.217(4) . ? N6 C39 1.483(4) . ? C6 C7 1.381(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.509(5) . ? O9 C15 1.257(4) . ? C9 C10 1.377(4) . ? C9 C14 1.396(5) . ? O10 C15 1.258(4) . ? C10 C11 1.388(5) . ? C10 H10 0.9500 . ? C11 C12 1.374(5) . ? C12 C13 1.391(5) . ? C12 H12 0.9500 . ? O13 C22 1.256(4) . ? C13 C14 1.386(5) . ? C13 H13 0.9500 . ? O14 C22 1.260(4) . ? C14 H14 0.9500 . ? C15 C16 1.489(4) . ? C16 C17 1.391(4) . ? C16 C21 1.396(4) . ? O17 C29 1.255(4) . ? C17 C18 1.373(5) . ? C17 H17 0.9500 . ? O18 C29 1.266(4) . ? O18 Y2 2.264(2) 2_665 ? C18 C19 1.384(5) . ? C19 C20 1.382(5) . ? C19 H19 0.9500 . ? C20 C21 1.381(5) . ? C20 H20 0.9500 . ? O21 C36 1.259(4) . ? C21 H21 0.9500 . ? O22 C36 1.268(4) . ? O22 Y2 2.319(2) 2_665 ? C22 C23 1.511(4) . ? C23 C28 1.387(4) . ? C23 C24 1.389(4) . ? C24 C25 1.385(5) . ? C24 H24 0.9500 . ? O25 H1O 0.7509 . ? O25 H2O 1.0020 . ? C25 C26 1.372(5) . ? O26 H3O 0.9471 . ? O26 H4O 0.6972 . ? C26 C27 1.392(5) . ? C26 H26 0.9500 . ? C27 C28 1.387(5) . ? C27 H27 0.9500 . ? C28 H28 0.9500 . ? C29 C30 1.492(5) . ? C30 C35 1.389(5) . ? C30 C31 1.392(4) . ? C31 C32 1.383(5) . ? C31 H31 0.9500 . ? C32 C33 1.386(5) . ? C33 C34 1.383(5) . ? C33 H33 0.9500 . ? C34 C35 1.378(5) . ? C34 H34 0.9500 . ? C35 H35 0.9500 . ? C36 C37 1.502(5) . ? C37 C38 1.382(4) . ? C37 C42 1.394(5) . ? C38 C39 1.384(5) . ? C38 H38 0.9500 . ? C39 C40 1.375(5) . ? C40 C41 1.388(5) . ? C40 H40 0.9500 . ? C41 C42 1.387(5) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? 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 O2 Y1 O5 85.82(8) 2_666 . ? O2 Y1 O9 167.93(8) 2_666 . ? O5 Y1 O9 102.32(8) . . ? O2 Y1 O25 87.31(8) 2_666 . ? O5 Y1 O25 145.47(8) . . ? O9 Y1 O25 90.74(8) . . ? O2 Y1 O26 92.88(8) 2_666 . ? O5 Y1 O26 72.09(8) . . ? O9 Y1 O26 81.38(8) . . ? O25 Y1 O26 142.11(8) . . ? O2 Y1 O13 79.72(8) 2_666 . ? O5 Y1 O13 141.63(8) . . ? O9 Y1 O13 88.44(8) . . ? O25 Y1 O13 69.41(8) . . ? O26 Y1 O13 73.36(8) . . ? O2 Y1 O1 117.29(8) 2_666 . ? O5 Y1 O1 74.57(8) . . ? O9 Y1 O1 73.89(8) . . ? O25 Y1 O1 78.76(8) . . ? O26 Y1 O1 132.60(8) . . ? O13 Y1 O1 143.32(8) . . ? O2 Y1 O2 70.08(8) 2_666 . ? O5 Y1 O2 77.32(7) . . ? O9 Y1 O2 120.11(7) . . ? O25 Y1 O2 68.54(7) . . ? O26 Y1 O2 145.97(7) . . ? O13 Y1 O2 128.55(7) . . ? O1 Y1 O2 47.80(7) . . ? O2 Y1 C1 94.28(9) 2_666 . ? O5 Y1 C1 74.45(8) . . ? O9 Y1 C1 96.48(9) . . ? O25 Y1 C1 72.38(8) . . ? O26 Y1 C1 145.12(8) . . ? O13 Y1 C1 141.52(8) . . ? O1 Y1 C1 23.30(8) . . ? O2 Y1 C1 24.51(7) . . ? O27 S1 C43 105.55(16) . . ? O27 S1 C44 105.41(15) . . ? C43 S1 C44 98.33(19) . . ? C1 O1 Y1 108.1(2) . . ? O4 N1 O3 123.1(4) . . ? O4 N1 C4 118.3(3) . . ? O3 N1 C4 118.5(4) . . ? O1 C1 O2 121.9(3) . . ? O1 C1 C2 118.5(3) . . ? O2 C1 C2 119.7(3) . . ? O1 C1 Y1 48.62(16) . . ? O2 C1 Y1 73.23(17) . . ? C2 C1 Y1 167.0(2) . . ? O10 Y2 O14 84.65(8) . . ? O10 Y2 O18 98.96(9) . 2_665 ? O14 Y2 O18 153.78(9) . 2_665 ? O10 Y2 O21 74.96(8) . . ? O14 Y2 O21 131.38(8) . . ? O18 Y2 O21 74.07(9) 2_665 . ? O10 Y2 O22 154.79(9) . 2_665 ? O14 Y2 O22 81.70(8) . 2_665 ? O18 Y2 O22 84.64(8) 2_665 2_665 ? O21 Y2 O22 129.48(8) . 2_665 ? O10 Y2 O17 112.82(9) . . ? O14 Y2 O17 74.40(8) . . ? O18 Y2 O17 126.17(9) 2_665 . ? O21 Y2 O17 73.89(8) . . ? O22 Y2 O17 83.71(8) 2_665 . ? O10 Y2 O27 78.11(9) . . ? O14 Y2 O27 76.99(9) . . ? O18 Y2 O27 78.37(9) 2_665 . ? O21 Y2 O27 137.46(9) . . ? O22 Y2 O27 78.23(8) 2_665 . ? O17 Y2 O27 148.00(9) . . ? O10 Y2 C29 130.32(9) . . ? O14 Y2 C29 91.35(9) . . ? O18 Y2 C29 105.31(9) 2_665 . ? O21 Y2 C29 71.19(9) . . ? O22 Y2 C29 71.28(9) 2_665 . ? O17 Y2 C29 22.44(8) . . ? O27 Y2 C29 148.65(9) . . ? O28 S2 C45 105.8(2) . . ? O28 S2 C46 104.33(18) . . ? C45 S2 C46 98.3(3) . . ? C1 O2 Y1 164.7(2) . 2_666 ? C1 O2 Y1 82.26(18) . . ? Y1 O2 Y1 109.92(8) 2_666 . ? O7 N2 O8 123.3(3) . . ? O7 N2 C11 118.5(3) . . ? O8 N2 C11 118.2(3) . . ? C3 C2 C7 119.0(3) . . ? C3 C2 C1 121.7(3) . . ? C7 C2 C1 119.3(3) . . ? O29 S3 C47 105.15(18) . . ? O29 S3 C48 105.3(2) . . ? C47 S3 C48 96.2(3) . . ? O11 N3 O12 123.6(3) . . ? O11 N3 C18 118.4(3) . . ? O12 N3 C18 118.0(3) . . ? C2 C3 C4 118.2(3) . . ? C2 C3 H3 120.9 . . ? C4 C3 H3 120.9 . . ? O15 N4 O16 124.5(3) . . ? O15 N4 C25 118.4(3) . . ? O16 N4 C25 117.0(3) . . ? C5 C4 C3 122.7(3) . . ? C5 C4 N1 118.6(3) . . ? C3 C4 N1 118.6(3) . . ? C8 O5 Y1 138.4(2) . . ? O20 N5 O19 124.1(3) . . ? O20 N5 C32 117.7(3) . . ? O19 N5 C32 118.2(3) . . ? C6 C5 C4 118.9(3) . . ? C6 C5 H5 120.6 . . ? C4 C5 H5 120.6 . . ? O24 N6 O23 123.6(3) . . ? O24 N6 C39 118.9(3) . . ? O23 N6 C39 117.5(4) . . ? C5 C6 C7 119.6(4) . . ? C5 C6 H6 120.2 . . ? C7 C6 H6 120.2 . . ? C6 C7 C2 121.5(3) . . ? C6 C7 H7 119.3 . . ? C2 C7 H7 119.3 . . ? O6 C8 O5 124.6(3) . . ? O6 C8 C9 119.2(3) . . ? O5 C8 C9 116.2(3) . . ? C15 O9 Y1 157.0(2) . . ? C10 C9 C14 119.5(3) . . ? C10 C9 C8 120.6(3) . . ? C14 C9 C8 119.8(3) . . ? C15 O10 Y2 160.2(2) . . ? C9 C10 C11 118.5(3) . . ? C9 C10 H10 120.7 . . ? C11 C10 H10 120.7 . . ? C12 C11 C10 123.4(3) . . ? C12 C11 N2 118.3(3) . . ? C10 C11 N2 118.3(3) . . ? C11 C12 C13 117.4(3) . . ? C11 C12 H12 121.3 . . ? C13 C12 H12 121.3 . . ? C22 O13 Y1 139.4(2) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C22 O14 Y2 149.2(2) . . ? C13 C14 C9 120.6(3) . . ? C13 C14 H14 119.7 . . ? C9 C14 H14 119.7 . . ? O9 C15 O10 124.5(3) . . ? O9 C15 C16 118.5(3) . . ? O10 C15 C16 117.0(3) . . ? C17 C16 C21 119.2(3) . . ? C17 C16 C15 120.3(3) . . ? C21 C16 C15 120.6(3) . . ? C29 O17 Y2 112.3(2) . . ? C18 C17 C16 117.9(3) . . ? C18 C17 H17 121.0 . . ? C16 C17 H17 121.0 . . ? C29 O18 Y2 172.6(2) . 2_665 ? C17 C18 C19 123.7(3) . . ? C17 C18 N3 118.8(3) . . ? C19 C18 N3 117.5(3) . . ? C20 C19 C18 118.1(3) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? C21 C20 C19 119.5(3) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C36 O21 Y2 139.9(2) . . ? C20 C21 C16 121.6(3) . . ? C20 C21 H21 119.2 . . ? C16 C21 H21 119.2 . . ? C36 O22 Y2 133.1(2) . 2_665 ? O13 C22 O14 124.7(3) . . ? O13 C22 C23 117.0(3) . . ? O14 C22 C23 118.3(3) . . ? C28 C23 C24 119.8(3) . . ? C28 C23 C22 120.4(3) . . ? C24 C23 C22 119.7(3) . . ? C25 C24 C23 118.3(3) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? Y1 O25 H1O 110.1 . . ? Y1 O25 H2O 124.1 . . ? H1O O25 H2O 109.6 . . ? C26 C25 C24 122.9(3) . . ? C26 C25 N4 119.0(3) . . ? C24 C25 N4 118.1(3) . . ? Y1 O26 H3O 125.5 . . ? Y1 O26 H4O 124.9 . . ? H3O O26 H4O 104.1 . . ? C25 C26 C27 118.3(3) . . ? C25 C26 H26 120.9 . . ? C27 C26 H26 120.9 . . ? S1 O27 Y2 128.02(13) . . ? C28 C27 C26 120.0(3) . . ? C28 C27 H27 120.0 . . ? C26 C27 H27 120.0 . . ? C23 C28 C27 120.7(3) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? O17 C29 O18 123.0(3) . . ? O17 C29 C30 118.3(3) . . ? O18 C29 C30 118.6(3) . . ? O17 C29 Y2 45.28(17) . . ? O18 C29 Y2 79.2(2) . . ? C30 C29 Y2 157.6(2) . . ? C35 C30 C31 119.8(3) . . ? C35 C30 C29 121.6(3) . . ? C31 C30 C29 118.5(3) . . ? C32 C31 C30 118.3(3) . . ? C32 C31 H31 120.8 . . ? C30 C31 H31 120.8 . . ? C31 C32 C33 122.4(3) . . ? C31 C32 N5 118.8(3) . . ? C33 C32 N5 118.7(3) . . ? C34 C33 C32 118.3(4) . . ? C34 C33 H33 120.8 . . ? C32 C33 H33 120.8 . . ? C35 C34 C33 120.4(3) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 C30 120.7(3) . . ? C34 C35 H35 119.7 . . ? C30 C35 H35 119.7 . . ? O21 C36 O22 125.3(3) . . ? O21 C36 C37 116.6(3) . . ? O22 C36 C37 118.1(3) . . ? C38 C37 C42 119.8(3) . . ? C38 C37 C36 118.2(3) . . ? C42 C37 C36 121.9(3) . . ? C37 C38 C39 118.5(3) . . ? C37 C38 H38 120.7 . . ? C39 C38 H38 120.7 . . ? C40 C39 C38 123.0(3) . . ? C40 C39 N6 120.1(3) . . ? C38 C39 N6 116.9(3) . . ? C39 C40 C41 117.8(3) . . ? C39 C40 H40 121.1 . . ? C41 C40 H40 121.1 . . ? C42 C41 C40 120.6(4) . . ? C42 C41 H41 119.7 . . ? C40 C41 H41 119.7 . . ? C41 C42 C37 120.2(3) . . ? C41 C42 H42 119.9 . . ? C37 C42 H42 119.9 . . ? S1 C43 H43A 109.5 . . ? S1 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? S1 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? S1 C44 H44A 109.5 . . ? S1 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? S1 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? S2 C45 H45A 109.5 . . ? S2 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? S2 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? S2 C46 H46A 109.5 . . ? S2 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? S2 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? S3 C47 H47A 109.5 . . ? S3 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? S3 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? S3 C48 H48A 109.5 . . ? S3 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? S3 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O26 H3O O29 0.95 1.70 2.643(3) 172.5 . O26 H4O O14 0.70 2.30 2.850(3) 136.6 . O26 H4O O27 0.70 2.51 3.113(3) 145.9 . O25 H1O O6 0.75 1.98 2.727(3) 176.7 2_666 O25 H2O O28 1.00 1.66 2.660(3) 173.0 . _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.862 _refine_diff_density_min -0.654 _refine_diff_density_rms 0.096 # Attachment '9.CIF' data_9 _database_code_depnum_ccdc_archive 'CCDC 649814' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[(dimethylformamide)tris(4-nitrobenzoato)terbium (III)].4dimethylformamide ; _chemical_name_common '[Tb(4-NO2BA)3(DMF)]2.4DMF' _chemical_melting_point ? _chemical_formula_moiety C48H42N8O28Tb2,4(C3H7NO) _chemical_formula_sum C60H70N12O32Tb2 _chemical_formula_weight 1789.12 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 P21/n 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 9.6946(1) _cell_length_b 26.4487(4) _cell_length_c 14.4156(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.594(1) _cell_angle_gamma 90.00 _cell_volume 3560.24(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1800 _exptl_absorpt_coefficient_mu 2.068 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6689 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _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 17438 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0313 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.13 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8062 _reflns_number_gt 7272 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8062 _refine_ls_number_parameters 495 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0314 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0587 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.207382(12) 0.029331(4) 0.537482(8) 0.00991(4) Uani 1 1 d . . . O1 O 0.26765(19) 0.11317(7) 0.49521(13) 0.0152(4) Uani 1 1 d . . . N1 N 0.6101(3) 0.25673(10) 0.2801(2) 0.0291(6) Uani 1 1 d . . . C1 C 0.3505(3) 0.09910(10) 0.44539(17) 0.0127(5) Uani 1 1 d . . . O2 O 0.37605(18) 0.05316(7) 0.43561(13) 0.0160(4) Uani 1 1 d . . . N2 N 0.1979(4) -0.29053(10) 0.4287(2) 0.0392(7) Uani 1 1 d . . . C2 C 0.4165(3) 0.13930(10) 0.39776(17) 0.0134(5) Uani 1 1 d . . . O3 O 0.5850(3) 0.30012(9) 0.2986(2) 0.0575(9) Uani 1 1 d . . . N3 N 0.1699(2) -0.21703(9) 0.92220(16) 0.0188(5) Uani 1 1 d . . . C3 C 0.3694(3) 0.18885(10) 0.39971(19) 0.0172(5) Uani 1 1 d . . . H3 H 0.2941 0.1962 0.4282 0.021 Uiso 1 1 calc R . . O4 O 0.6884(2) 0.24570(9) 0.22956(17) 0.0349(6) Uani 1 1 d . . . N4 N 0.3828(2) 0.12924(9) 0.80019(16) 0.0180(5) Uani 1 1 d . . . C4 C 0.4316(3) 0.22756(10) 0.3604(2) 0.0208(6) Uani 1 1 d . . . H4 H 0.3999 0.2615 0.3612 0.025 Uiso 1 1 calc R . . O5 O 0.24891(19) -0.05157(7) 0.47593(13) 0.0154(4) Uani 1 1 d . . . N5 N 0.8688(2) 0.07780(9) 0.80641(16) 0.0198(5) Uani 1 1 d . . . C5 C 0.5414(3) 0.21535(11) 0.3197(2) 0.0198(6) Uani 1 1 d . . . O6 O 0.01786(18) -0.05913(7) 0.46432(13) 0.0167(4) Uani 1 1 d . . . N6 N 1.2906(3) 0.03997(9) 1.10167(17) 0.0220(5) Uani 1 1 d . . . C6 C 0.5898(3) 0.16655(11) 0.31585(19) 0.0195(6) Uani 1 1 d . . . H6 H 0.6646 0.1594 0.2867 0.023 Uiso 1 1 calc R . . O7 O 0.3115(4) -0.30618(10) 0.4186(3) 0.0797(12) Uani 1 1 d . . . C7 C 0.5268(3) 0.12830(10) 0.35549(18) 0.0162(5) Uani 1 1 d . . . H7 H 0.5586 0.0944 0.3540 0.019 Uiso 1 1 calc R . . O8 O 0.1005(3) -0.31800(9) 0.4365(2) 0.0471(7) Uani 1 1 d . . . C8 C 0.1369(3) -0.07734(10) 0.46235(17) 0.0134(5) Uani 1 1 d . . . O9 O 0.16029(19) -0.02453(7) 0.65612(13) 0.0160(4) Uani 1 1 d . . . C9 C 0.1469(3) -0.13323(10) 0.44688(17) 0.0138(5) Uani 1 1 d . . . O10 O -0.07571(18) -0.03916(7) 0.62467(12) 0.0143(4) Uani 1 1 d . . . C10 C 0.2665(3) -0.15264(10) 0.42255(19) 0.0176(5) Uani 1 1 d . . . H10 H 0.3370 -0.1303 0.4113 0.021 Uiso 1 1 calc R . . O11 O 0.2626(2) -0.21293(8) 0.99898(14) 0.0287(5) Uani 1 1 d . . . C11 C 0.2824(3) -0.20416(11) 0.4149(2) 0.0226(6) Uani 1 1 d . . . H11 H 0.3626 -0.2178 0.3975 0.027 Uiso 1 1 calc R . . O12 O 0.1046(2) -0.25630(7) 0.89556(14) 0.0238(4) Uani 1 1 d . . . C12 C 0.1785(3) -0.23551(11) 0.4331(2) 0.0245(6) Uani 1 1 d . . . O13 O 0.2635(2) 0.07734(7) 0.68148(13) 0.0189(4) Uani 1 1 d . . . C13 C 0.0583(3) -0.21735(11) 0.4563(2) 0.0239(6) Uani 1 1 d . . . H13 H -0.0114 -0.2399 0.4682 0.029 Uiso 1 1 calc R . . O14 O 0.44169(18) 0.00761(7) 0.62632(13) 0.0172(4) Uani 1 1 d . . . C14 C 0.0422(3) -0.16551(11) 0.46187(19) 0.0187(6) Uani 1 1 d . . . H14 H -0.0407 -0.1520 0.4760 0.022 Uiso 1 1 calc R . . O15 O 0.6288(2) 0.06501(8) 0.75633(15) 0.0267(5) Uani 1 1 d . . . C15 C 0.0530(3) -0.04795(10) 0.66666(17) 0.0122(5) Uani 1 1 d . . . C16 C 0.0821(3) -0.09140(10) 0.73645(17) 0.0121(5) Uani 1 1 d . . . O16A O 1.3279(7) -0.0166(2) 0.9926(3) 0.0381(15) Uani 0.509(7) 1 d P A 1 O16B O 1.1115(5) -0.0049(2) 0.9984(4) 0.0449(17) Uani 0.491(7) 1 d P A 2 C17 C -0.0055(3) -0.13397(10) 0.71683(19) 0.0168(5) Uani 1 1 d . . . H17 H -0.0853 -0.1345 0.6615 0.020 Uiso 1 1 calc R . . C18 C 0.0231(3) -0.17552(11) 0.77766(19) 0.0178(5) Uani 1 1 d . . . H18 H -0.0344 -0.2051 0.7639 0.021 Uiso 1 1 calc R . . C19 C 0.1379(3) -0.17272(10) 0.85898(18) 0.0153(5) Uani 1 1 d . . . C20 C 0.2246(3) -0.13054(10) 0.88170(18) 0.0170(5) Uani 1 1 d . . . H20 H 0.3012 -0.1294 0.9389 0.020 Uiso 1 1 calc R . . C21 C 0.1965(3) -0.08985(11) 0.81864(18) 0.0159(5) Uani 1 1 d . . . H21 H 0.2560 -0.0607 0.8318 0.019 Uiso 1 1 calc R . . C22 C 0.3206(3) 0.11860(10) 0.70938(19) 0.0165(5) Uani 1 1 d . . . H22 H 0.3194 0.1440 0.6625 0.020 Uiso 1 1 calc R . . C23 C 0.3956(3) 0.09182(12) 0.8754(2) 0.0265(6) Uani 1 1 d . . . H23A H 0.3493 0.0604 0.8472 0.040 Uiso 1 1 calc R . . H23B H 0.3491 0.1044 0.9233 0.040 Uiso 1 1 calc R . . H23C H 0.4971 0.0854 0.9064 0.040 Uiso 1 1 calc R . . C24 C 0.4537(4) 0.17753(12) 0.8274(2) 0.0322(7) Uani 1 1 d . . . H24A H 0.5571 0.1721 0.8523 0.048 Uiso 1 1 calc R . . H24B H 0.4168 0.1933 0.8774 0.048 Uiso 1 1 calc R . . H24C H 0.4351 0.1997 0.7709 0.048 Uiso 1 1 calc R . . C25 C 0.7515(3) 0.05670(11) 0.75086(19) 0.0197(6) Uani 1 1 d . . . H25 H 0.7628 0.0334 0.7032 0.024 Uiso 1 1 calc R . . C26 C 0.8613(4) 0.11289(14) 0.8818(3) 0.0386(9) Uani 1 1 d . . . H26A H 0.7622 0.1152 0.8859 0.058 Uiso 1 1 calc R . . H26B H 0.8938 0.1463 0.8672 0.058 Uiso 1 1 calc R . . H26C H 0.9228 0.1009 0.9435 0.058 Uiso 1 1 calc R . . C27 C 1.0094(3) 0.06690(13) 0.7937(2) 0.0291(7) Uani 1 1 d . . . H27A H 0.9997 0.0439 0.7391 0.044 Uiso 1 1 calc R . . H27B H 1.0691 0.0510 0.8523 0.044 Uiso 1 1 calc R . . H27C H 1.0545 0.0984 0.7814 0.044 Uiso 1 1 calc R . . C28A C 1.2431(4) 0.00605(13) 1.0324(2) 0.026(11) Uani 0.509(7) 1 d P A 1 H28A H 1.1436 -0.0014 1.0123 0.032 Uiso 0.509(7) 1 calc PR A 1 C29 C 1.4415(3) 0.05223(13) 1.1340(2) 0.0275(7) Uani 1 1 d . A . H29A H 1.4816 0.0388 1.1991 0.041 Uiso 1 1 calc R . . H29B H 1.4536 0.0890 1.1348 0.041 Uiso 1 1 calc R . . H29C H 1.4915 0.0371 1.0901 0.041 Uiso 1 1 calc R . . C30 C 1.1955(4) 0.06343(13) 1.1515(3) 0.0348(8) Uani 1 1 d . A . H30A H 1.0979 0.0507 1.1247 0.052 Uiso 1 1 calc R . . H30B H 1.1967 0.1002 1.1432 0.052 Uiso 1 1 calc R . . H30C H 1.2277 0.0552 1.2202 0.052 Uiso 1 1 calc R . . C28B C 1.2431(4) 0.00605(13) 1.0324(2) 0.030(12) Uiso 0.491(7) 1 d P A 2 H28B H 1.3112 -0.0109 1.0070 0.036 Uiso 0.491(7) 1 calc PR A 2 H2O H 0.4956 0.0269 0.6662 0.000 Uiso 1 1 d . . . H1O H 0.4953 -0.0099 0.6010 0.019 Uiso 1 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 0.00780(6) 0.00892(6) 0.01377(6) 0.00006(5) 0.00424(4) 0.00032(5) O1 0.0162(9) 0.0130(9) 0.0187(9) -0.0022(7) 0.0087(7) -0.0038(7) N1 0.0332(15) 0.0180(13) 0.0445(16) 0.0022(12) 0.0248(13) -0.0040(11) C1 0.0084(11) 0.0141(13) 0.0145(11) 0.0000(10) 0.0012(9) -0.0011(10) O2 0.0131(9) 0.0121(9) 0.0244(9) 0.0024(8) 0.0076(7) 0.0010(7) N2 0.067(2) 0.0139(13) 0.0462(17) -0.0030(13) 0.0318(16) -0.0005(14) C2 0.0123(12) 0.0133(13) 0.0142(11) -0.0002(10) 0.0026(9) -0.0029(10) O3 0.081(2) 0.0157(12) 0.103(2) -0.0022(14) 0.073(2) -0.0079(13) N3 0.0187(11) 0.0186(12) 0.0214(11) 0.0050(10) 0.0095(9) 0.0017(10) C3 0.0165(13) 0.0164(14) 0.0216(13) -0.0023(11) 0.0102(10) -0.0025(11) O4 0.0391(13) 0.0283(12) 0.0510(14) 0.0062(11) 0.0355(12) -0.0012(11) N4 0.0192(11) 0.0161(12) 0.0180(11) -0.0022(9) 0.0039(9) 0.0002(9) C4 0.0262(15) 0.0110(13) 0.0298(14) -0.0002(11) 0.0152(12) -0.0004(11) O5 0.0138(9) 0.0128(9) 0.0197(9) -0.0021(8) 0.0048(7) -0.0011(7) N5 0.0172(11) 0.0213(13) 0.0233(11) -0.0046(10) 0.0096(9) 0.0002(10) C5 0.0228(14) 0.0175(14) 0.0229(13) 0.0014(11) 0.0129(11) -0.0060(12) O6 0.0137(9) 0.0178(10) 0.0199(9) 0.0014(8) 0.0071(7) 0.0069(8) N6 0.0215(12) 0.0215(13) 0.0242(12) 0.0006(10) 0.0079(10) 0.0020(10) C6 0.0179(13) 0.0213(15) 0.0225(13) -0.0013(12) 0.0113(11) -0.0017(11) O7 0.102(3) 0.0164(13) 0.153(4) -0.0010(17) 0.090(3) 0.0150(16) C7 0.0153(12) 0.0138(13) 0.0206(12) -0.0008(11) 0.0066(10) -0.0004(10) O8 0.077(2) 0.0142(11) 0.0583(17) -0.0040(11) 0.0321(15) -0.0119(13) C8 0.0137(12) 0.0150(13) 0.0127(11) 0.0012(10) 0.0055(9) 0.0022(10) O9 0.0134(9) 0.0174(10) 0.0178(8) 0.0018(8) 0.0052(7) -0.0035(7) C9 0.0138(12) 0.0128(13) 0.0146(11) -0.0002(10) 0.0036(9) 0.0007(10) O10 0.0116(8) 0.0153(10) 0.0163(8) 0.0013(7) 0.0041(7) 0.0006(7) C10 0.0165(13) 0.0157(14) 0.0216(13) -0.0015(11) 0.0069(10) -0.0002(11) O11 0.0292(11) 0.0281(12) 0.0225(10) 0.0098(9) -0.0037(8) -0.0036(9) C11 0.0244(15) 0.0167(14) 0.0308(15) -0.0033(12) 0.0145(12) 0.0054(12) O12 0.0283(11) 0.0161(10) 0.0276(10) 0.0048(9) 0.0086(8) -0.0041(9) C12 0.0369(17) 0.0099(13) 0.0289(15) -0.0022(12) 0.0124(13) 0.0008(12) O13 0.0192(9) 0.0180(10) 0.0211(9) -0.0045(8) 0.0083(7) -0.0042(8) C13 0.0270(15) 0.0167(14) 0.0306(15) -0.0026(12) 0.0123(12) -0.0082(12) O14 0.0096(8) 0.0203(10) 0.0213(9) -0.0059(8) 0.0036(7) 0.0011(8) C14 0.0153(13) 0.0179(14) 0.0241(13) -0.0018(11) 0.0075(10) -0.0025(11) O15 0.0180(10) 0.0314(12) 0.0318(11) -0.0073(9) 0.0085(8) -0.0024(9) C15 0.0129(12) 0.0114(12) 0.0127(11) -0.0011(10) 0.0039(9) 0.0002(10) C16 0.0102(11) 0.0141(12) 0.0133(11) 0.0002(10) 0.0057(9) 0.0011(10) O16A 0.037(3) 0.046(3) 0.031(2) -0.014(2) 0.009(2) 0.003(2) O16B 0.027(3) 0.055(4) 0.045(3) 0.001(3) -0.002(2) -0.013(2) C17 0.0116(12) 0.0183(14) 0.0197(12) 0.0015(11) 0.0031(10) -0.0017(10) C18 0.0169(13) 0.0150(13) 0.0211(13) 0.0016(11) 0.0046(10) -0.0030(11) C19 0.0154(12) 0.0134(13) 0.0185(12) 0.0036(10) 0.0074(10) 0.0016(10) C20 0.0154(12) 0.0192(14) 0.0153(12) 0.0012(11) 0.0024(10) -0.0018(11) C21 0.0145(12) 0.0167(13) 0.0174(12) -0.0001(11) 0.0058(9) -0.0021(11) C22 0.0162(13) 0.0144(13) 0.0201(12) -0.0005(11) 0.0069(10) 0.0003(11) C23 0.0286(16) 0.0311(17) 0.0183(13) 0.0020(13) 0.0040(11) 0.0005(14) C24 0.0365(18) 0.0273(17) 0.0285(16) -0.0059(14) 0.0012(13) -0.0078(15) C25 0.0240(14) 0.0182(14) 0.0181(12) 0.0010(11) 0.0074(10) 0.0003(12) C26 0.0325(18) 0.040(2) 0.049(2) -0.0251(17) 0.0211(16) -0.0135(16) C27 0.0182(14) 0.0343(18) 0.0376(17) -0.0045(14) 0.0123(12) 0.0008(13) C28A 0.025(11) 0.030(12) 0.022(10) 0.001(3) 0.002(3) -0.005(3) C29 0.0251(15) 0.0286(17) 0.0275(15) 0.0003(13) 0.0047(12) -0.0034(13) C30 0.0380(19) 0.0283(18) 0.046(2) 0.0035(15) 0.0250(16) 0.0059(15) _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 2.3151(17) 3_556 ? Tb1 O10 2.3573(17) 3_556 ? Tb1 O14 2.3592(18) . ? Tb1 O9 2.3627(17) . ? Tb1 O13 2.3686(18) . ? Tb1 O5 2.3917(18) . ? Tb1 O1 2.4128(18) . ? Tb1 O2 2.5531(17) . ? O1 C1 1.269(3) . ? N1 O3 1.218(3) . ? N1 O4 1.220(3) . ? N1 C5 1.474(3) . ? C1 O2 1.255(3) . ? C1 C2 1.499(3) . ? N2 O8 1.220(4) . ? N2 O7 1.221(4) . ? N2 C12 1.471(4) . ? C2 C3 1.390(4) . ? C2 C7 1.396(3) . ? N3 O12 1.223(3) . ? N3 O11 1.229(3) . ? N3 C19 1.466(3) . ? C3 C4 1.385(4) . ? C3 H3 0.9500 . ? N4 C22 1.316(3) . ? N4 C23 1.448(4) . ? N4 C24 1.454(4) . ? C4 C5 1.383(4) . ? C4 H4 0.9500 . ? O5 C8 1.252(3) . ? N5 C25 1.325(4) . ? N5 C26 1.446(4) . ? N5 C27 1.452(3) . ? C5 C6 1.380(4) . ? O6 C8 1.257(3) . ? O6 Tb1 2.3151(17) 3_556 ? N6 C28A 1.329(4) . ? N6 C29 1.448(4) . ? N6 C30 1.452(4) . ? C6 C7 1.382(4) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.502(4) . ? O9 C15 1.254(3) . ? C9 C14 1.387(4) . ? C9 C10 1.396(3) . ? O10 C15 1.254(3) . ? O10 Tb1 2.3573(17) 3_556 ? C10 C11 1.379(4) . ? C10 H10 0.9500 . ? C11 C12 1.383(4) . ? C11 H11 0.9500 . ? C12 C13 1.382(4) . ? O13 C22 1.241(3) . ? C13 C14 1.385(4) . ? C13 H13 0.9500 . ? O14 H2O 0.8380 . ? O14 H1O 0.8483 . ? C14 H14 0.9500 . ? O15 C25 1.233(3) . ? C15 C16 1.503(3) . ? C16 C21 1.389(3) . ? C16 C17 1.393(4) . ? O16A C28A 1.273(7) . ? C17 C18 1.387(4) . ? C17 H17 0.9500 . ? C18 C19 1.384(4) . ? C18 H18 0.9500 . ? C19 C20 1.382(4) . ? C20 C21 1.388(4) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28A H28A 0.9500 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 O10 72.16(6) 3_556 3_556 ? O6 Tb1 O14 148.94(6) 3_556 . ? O10 Tb1 O14 138.66(6) 3_556 . ? O6 Tb1 O9 81.27(6) 3_556 . ? O10 Tb1 O9 128.74(6) 3_556 . ? O14 Tb1 O9 78.78(6) . . ? O6 Tb1 O13 79.70(6) 3_556 . ? O10 Tb1 O13 138.20(6) 3_556 . ? O14 Tb1 O13 72.18(6) . . ? O9 Tb1 O13 74.48(6) . . ? O6 Tb1 O5 123.56(6) 3_556 . ? O10 Tb1 O5 80.28(6) 3_556 . ? O14 Tb1 O5 75.52(6) . . ? O9 Tb1 O5 79.26(6) . . ? O13 Tb1 O5 141.52(6) . . ? O6 Tb1 O1 88.62(6) 3_556 . ? O10 Tb1 O1 75.61(6) 3_556 . ? O14 Tb1 O1 95.61(6) . . ? O9 Tb1 O1 147.56(6) . . ? O13 Tb1 O1 73.40(6) . . ? O5 Tb1 O1 130.71(6) . . ? O6 Tb1 O2 131.11(6) 3_556 . ? O10 Tb1 O2 70.26(6) 3_556 . ? O14 Tb1 O2 72.56(6) . . ? O9 Tb1 O2 147.51(6) . . ? O13 Tb1 O2 109.87(6) . . ? O5 Tb1 O2 79.03(6) . . ? O1 Tb1 O2 52.54(6) . . ? C1 O1 Tb1 96.11(15) . . ? O3 N1 O4 123.3(3) . . ? O3 N1 C5 118.5(2) . . ? O4 N1 C5 118.2(2) . . ? O2 C1 O1 121.4(2) . . ? O2 C1 C2 120.9(2) . . ? O1 C1 C2 117.7(2) . . ? C1 O2 Tb1 89.89(14) . . ? O8 N2 O7 123.7(3) . . ? O8 N2 C12 118.3(3) . . ? O7 N2 C12 118.1(3) . . ? C3 C2 C7 119.9(2) . . ? C3 C2 C1 118.5(2) . . ? C7 C2 C1 121.6(2) . . ? O12 N3 O11 123.3(2) . . ? O12 N3 C19 118.6(2) . . ? O11 N3 C19 118.1(2) . . ? C4 C3 C2 120.5(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C22 N4 C23 121.5(2) . . ? C22 N4 C24 120.9(2) . . ? C23 N4 C24 117.4(2) . . ? C5 C4 C3 118.0(3) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C8 O5 Tb1 108.63(15) . . ? C25 N5 C26 121.1(2) . . ? C25 N5 C27 121.5(2) . . ? C26 N5 C27 117.4(2) . . ? C6 C5 C4 123.0(2) . . ? C6 C5 N1 119.0(2) . . ? C4 C5 N1 118.0(3) . . ? C8 O6 Tb1 176.79(18) . 3_556 ? C28A N6 C29 120.6(3) . . ? C28A N6 C30 121.5(3) . . ? C29 N6 C30 117.8(3) . . ? C5 C6 C7 118.3(2) . . ? C5 C6 H6 120.8 . . ? C7 C6 H6 120.8 . . ? C6 C7 C2 120.2(3) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O5 C8 O6 123.4(2) . . ? O5 C8 C9 118.1(2) . . ? O6 C8 C9 118.5(2) . . ? C15 O9 Tb1 135.50(16) . . ? C14 C9 C10 120.3(2) . . ? C14 C9 C8 120.2(2) . . ? C10 C9 C8 119.4(2) . . ? C15 O10 Tb1 134.64(15) . 3_556 ? C11 C10 C9 120.1(2) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 118.3(3) . . ? C10 C11 H11 120.8 . . ? C12 C11 H11 120.8 . . ? C13 C12 C11 122.8(3) . . ? C13 C12 N2 118.7(3) . . ? C11 C12 N2 118.4(3) . . ? C22 O13 Tb1 137.15(17) . . ? C12 C13 C14 118.3(3) . . ? C12 C13 H13 120.9 . . ? C14 C13 H13 120.9 . . ? Tb1 O14 H2O 123.8 . . ? Tb1 O14 H1O 120.7 . . ? H2O O14 H1O 106.7 . . ? C13 C14 C9 120.1(3) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? O10 C15 O9 126.9(2) . . ? O10 C15 C16 116.6(2) . . ? O9 C15 C16 116.5(2) . . ? C21 C16 C17 120.0(2) . . ? C21 C16 C15 120.8(2) . . ? C17 C16 C15 119.2(2) . . ? C18 C17 C16 120.3(2) . . ? C18 C17 H17 119.8 . . ? C16 C17 H17 119.8 . . ? C19 C18 C17 118.2(2) . . ? C19 C18 H18 120.9 . . ? C17 C18 H18 120.9 . . ? C20 C19 C18 122.9(2) . . ? C20 C19 N3 119.0(2) . . ? C18 C19 N3 118.1(2) . . ? C19 C20 C21 118.1(2) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C16 120.5(2) . . ? C20 C21 H21 119.8 . . ? C16 C21 H21 119.8 . . ? O13 C22 N4 123.8(3) . . ? O13 C22 H22 118.1 . . ? N4 C22 H22 118.1 . . ? N4 C23 H23A 109.5 . . ? N4 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N4 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N4 C24 H24A 109.5 . . ? N4 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N4 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O15 C25 N5 124.9(3) . . ? O15 C25 H25 117.5 . . ? N5 C25 H25 117.5 . . ? N5 C26 H26A 109.5 . . ? N5 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N5 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N5 C27 H27A 109.5 . . ? N5 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N5 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O16A C28A N6 121.5(4) . . ? O16A C28A H28A 119.3 . . ? N6 C28A H28A 119.3 . . ? N6 C29 H29A 109.5 . . ? N6 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? N6 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N6 C30 H30A 109.5 . . ? N6 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N6 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H2O O15 0.84 1.86 2.698(3) 174.5 . O14 H1O O2 0.85 1.87 2.711(2) 170.9 3_656 C25 H25 O10 0.95 2.89 3.766(3) 153.2 1_655 C25 H25 O5 0.95 2.60 3.271(3) 128.0 3_656 C28A H28A O16B 0.95 2.44 3.346(6) 158.8 3_757 C29 H29C O16A 0.98 2.43 3.377(6) 162.7 3_857 C23 H23C O16A 0.98 2.64 3.467(6) 142.0 3_757 C26 H26B O3 0.98 2.72 3.583(4) 146.8 4_666 C27 H27C O3 0.98 2.70 3.590(4) 150.6 4_666 C30 H30B O7 0.98 2.63 3.589(4) 167.7 2_656 C29 H29B O8 0.98 2.66 3.572(4) 154.5 2_656 C13 H13 O11 0.95 2.66 3.598(4) 169.0 4 C11 H11 O12 0.95 2.45 3.376(3) 164.4 4_655 C24 H24C O12 0.98 2.60 3.569(4) 169.4 2_556 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.528 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.088 # Attachment '10a.CIF' data_10a _database_code_depnum_ccdc_archive 'CCDC 649815' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly{[bis(aqua)(dimethylsulphoxide)tris(4-nitrobenzoate)yttrium(III)] dimethylsulphoxide} ; _chemical_name_common {[(H2O)2(DMSO)(4-NO2BA)3Y]DMSO}n _chemical_melting_point ? _chemical_formula_moiety 'C25 H28 N3 O16 S2 Y1' _chemical_formula_sum 'C25 H28 N3 O16 S2 Y1' _chemical_formula_weight 779.53 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9516(3) _cell_length_b 10.5178(3) _cell_length_c 15.9228(5) _cell_angle_alpha 98.840(1) _cell_angle_beta 96.540(1) _cell_angle_gamma 107.148(2) _cell_volume 1551.09(8) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.669 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 2.095 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5665 _exptl_absorpt_correction_T_max 0.7366 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _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 16368 _diffrn_reflns_av_R_equivalents 0.0237 _diffrn_reflns_av_sigmaI/netI 0.0323 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.17 _diffrn_reflns_theta_max 27.50 _reflns_number_total 7109 _reflns_number_gt 6325 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 7109 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0338 _refine_ls_R_factor_gt 0.0270 _refine_ls_wR_factor_ref 0.0679 _refine_ls_wR_factor_gt 0.0650 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _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 Y1 Y 0.249959(16) 1.005763(16) 0.488956(10) 0.01285(5) Uani 1 1 d . . . S1 S 0.30882(5) 1.33857(5) 0.44448(3) 0.02069(10) Uani 1 1 d . . . O1 O 0.24972(13) 0.82018(13) 0.38582(8) 0.0215(3) Uani 1 1 d . . . N1 N 0.30220(19) 0.55027(17) 0.00950(11) 0.0252(4) Uani 1 1 d . . . C1 C 0.16594(18) 0.70878(18) 0.34162(11) 0.0166(3) Uani 1 1 d . . . H1O H -0.005(3) 0.809(2) 0.5136(15) 0.030(7) Uiso 1 1 d . . . S2 S 0.42586(5) 1.41423(4) 0.73564(3) 0.01998(10) Uani 1 1 d . . . O2 O 0.06195(14) 0.63270(14) 0.36527(9) 0.0244(3) Uani 1 1 d . . . N2 N -0.13912(18) 0.83831(15) -0.01910(10) 0.0214(3) Uani 1 1 d . . . C2 C 0.19844(18) 0.66691(18) 0.25253(11) 0.0158(3) Uani 1 1 d . . . H2O H 0.059(3) 0.737(3) 0.4646(19) 0.049(8) Uiso 1 1 d . . . O3 O 0.41433(16) 0.62100(16) -0.00746(10) 0.0338(3) Uani 1 1 d . . . N3 N 0.73837(16) 1.19650(15) 0.07541(10) 0.0183(3) Uani 1 1 d . . . C3 C 0.10753(19) 0.55209(18) 0.19565(12) 0.0204(4) Uani 1 1 d . . . H3 H 0.0251 0.5003 0.2120 0.024 Uiso 1 1 calc R . . H3O H 0.458(2) 1.252(3) 0.5970(16) 0.033(7) Uiso 1 1 d . . . O4 O 0.22304(19) 0.44681(15) -0.03831(10) 0.0376(4) Uani 1 1 d . . . C4 C 0.1388(2) 0.51409(19) 0.11470(12) 0.0220(4) Uani 1 1 d . . . H4 H 0.0785 0.4373 0.0763 0.026 Uiso 1 1 calc R . . H4O H 0.527(3) 1.176(3) 0.5722(17) 0.039(8) Uiso 1 1 d . . . O5 O 0.05687(13) 0.98336(14) 0.39029(8) 0.0207(3) Uani 1 1 d . . . C5 C 0.2621(2) 0.59382(19) 0.09278(12) 0.0193(4) Uani 1 1 d . . . O6 O -0.17802(13) 0.93279(13) 0.38280(8) 0.0197(3) Uani 1 1 d . . . C6 C 0.35247(19) 0.71020(18) 0.14696(12) 0.0189(4) Uani 1 1 d . . . H6 H 0.4334 0.7631 0.1298 0.023 Uiso 1 1 calc R . . O7 O -0.03372(16) 0.84298(15) -0.05265(9) 0.0290(3) Uani 1 1 d . . . C7 C 0.31963(18) 0.74608(18) 0.22731(12) 0.0175(3) Uani 1 1 d . . . H7 H 0.3793 0.8241 0.2649 0.021 Uiso 1 1 calc R . . O8 O -0.25865(16) 0.81543(18) -0.05965(9) 0.0367(4) Uani 1 1 d . . . C8 C -0.06753(18) 0.94632(16) 0.34932(11) 0.0136(3) Uani 1 1 d . . . O9 O 0.39073(12) 1.08703(13) 0.38601(8) 0.0179(3) Uani 1 1 d . . . C9 C -0.08705(17) 0.91544(16) 0.25229(11) 0.0131(3) Uani 1 1 d . . . O10 O 0.60881(13) 1.10157(14) 0.44744(8) 0.0213(3) Uani 1 1 d . . . C10 C -0.22027(18) 0.89073(17) 0.20359(11) 0.0156(3) Uani 1 1 d . . . H10 H -0.2978 0.8917 0.2310 0.019 Uiso 1 1 calc R . . O11 O 0.68221(16) 1.11401(15) 0.00873(9) 0.0292(3) Uani 1 1 d . . . C11 C -0.23826(19) 0.86454(18) 0.11413(12) 0.0177(3) Uani 1 1 d . . . H11 H -0.3269 0.8483 0.0809 0.021 Uiso 1 1 calc R . . O12 O 0.83890(14) 1.30024(14) 0.08037(9) 0.0242(3) Uani 1 1 d . . . C12 C -0.12069(19) 0.86326(17) 0.07593(11) 0.0165(3) Uani 1 1 d . . . O13 O 0.22304(12) 1.22752(13) 0.48652(8) 0.0184(3) Uani 1 1 d . . . C13 C 0.01281(19) 0.88531(18) 0.12230(12) 0.0187(4) Uani 1 1 d . . . H13 H 0.0893 0.8819 0.0945 0.022 Uiso 1 1 calc R . . O14 O 0.06923(14) 0.80449(14) 0.51174(9) 0.0186(3) Uani 1 1 d . . . C14 C 0.02947(18) 0.91263(18) 0.21125(11) 0.0173(3) Uani 1 1 d . . . H14 H 0.1186 0.9292 0.2440 0.021 Uiso 1 1 calc R . . O15 O 0.45303(14) 1.17209(15) 0.57684(9) 0.0241(3) Uani 1 1 d . . . C15 C 0.52110(17) 1.10502(16) 0.38511(11) 0.0146(3) Uani 1 1 d . . . O16 O 0.47489(14) 1.42729(14) 0.64993(9) 0.0250(3) Uani 1 1 d . . . C16 C 0.57689(17) 1.13142(16) 0.30362(11) 0.0143(3) Uani 1 1 d . . . C17 C 0.48502(18) 1.09152(17) 0.22482(12) 0.0171(3) Uani 1 1 d . . . H17 H 0.3876 1.0527 0.2230 0.021 Uiso 1 1 calc R . . C18 C 0.53737(18) 1.10906(18) 0.14909(12) 0.0175(3) Uani 1 1 d . . . H18 H 0.4771 1.0789 0.0960 0.021 Uiso 1 1 calc R . . C19 C 0.68245(18) 1.17297(17) 0.15478(11) 0.0148(3) Uani 1 1 d . . . C20 C 0.77605(18) 1.21707(17) 0.23229(11) 0.0167(3) Uani 1 1 d . . . H20 H 0.8724 1.2616 0.2341 0.020 Uiso 1 1 calc R . . C21 C 0.72317(18) 1.19347(17) 0.30698(11) 0.0159(3) Uani 1 1 d . . . H21 H 0.7848 1.2188 0.3595 0.019 Uiso 1 1 calc R . . C22 C 0.2076(2) 1.3096(2) 0.33939(14) 0.0345(5) Uani 1 1 d . . . H22A H 0.2151 1.2296 0.3047 0.052 Uiso 1 1 calc R . . H22B H 0.2438 1.3862 0.3131 0.052 Uiso 1 1 calc R . . H22C H 0.1093 1.2973 0.3438 0.052 Uiso 1 1 calc R . . C23 C 0.2730(2) 1.4885(2) 0.49041(15) 0.0312(5) Uani 1 1 d . . . H23A H 0.3212 1.5193 0.5491 0.047 Uiso 1 1 calc R . . H23B H 0.1722 1.4689 0.4888 0.047 Uiso 1 1 calc R . . H23C H 0.3065 1.5579 0.4580 0.047 Uiso 1 1 calc R . . C24 C 0.2546(2) 1.4363(2) 0.72678(16) 0.0361(5) Uani 1 1 d . . . H24A H 0.1858 1.3579 0.6897 0.054 Uiso 1 1 calc R . . H24B H 0.2576 1.5154 0.7030 0.054 Uiso 1 1 calc R . . H24C H 0.2280 1.4474 0.7829 0.054 Uiso 1 1 calc R . . C25 C 0.5248(2) 1.5704(2) 0.80564(13) 0.0308(5) Uani 1 1 d . . . H25A H 0.6232 1.5754 0.8174 0.046 Uiso 1 1 calc R . . H25B H 0.4878 1.5762 0.8587 0.046 Uiso 1 1 calc R . . H25C H 0.5170 1.6443 0.7788 0.046 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 Y1 0.01237(8) 0.01900(9) 0.00988(8) 0.00246(6) 0.00256(6) 0.00897(6) S1 0.0152(2) 0.0226(2) 0.0266(2) 0.00945(19) 0.00460(18) 0.00691(17) O1 0.0206(6) 0.0208(7) 0.0206(7) -0.0032(5) 0.0074(5) 0.0051(5) N1 0.0362(9) 0.0238(8) 0.0194(8) 0.0028(7) 0.0087(7) 0.0144(7) C1 0.0159(8) 0.0201(9) 0.0164(9) 0.0021(7) 0.0022(7) 0.0106(7) S2 0.0217(2) 0.0175(2) 0.0232(2) 0.00303(18) 0.00372(18) 0.01044(18) O2 0.0202(6) 0.0283(7) 0.0206(7) 0.0007(6) 0.0069(5) 0.0025(5) N2 0.0320(9) 0.0179(8) 0.0137(8) 0.0011(6) 0.0039(7) 0.0081(7) C2 0.0165(8) 0.0179(8) 0.0157(8) 0.0028(7) 0.0025(7) 0.0099(7) O3 0.0332(8) 0.0434(9) 0.0260(8) 0.0021(7) 0.0152(6) 0.0123(7) N3 0.0197(7) 0.0194(8) 0.0164(8) 0.0043(6) 0.0044(6) 0.0060(6) C3 0.0178(9) 0.0195(9) 0.0221(10) 0.0006(7) 0.0051(7) 0.0044(7) O4 0.0618(11) 0.0221(8) 0.0235(8) -0.0039(6) 0.0127(7) 0.0074(7) C4 0.0234(9) 0.0166(9) 0.0211(9) -0.0039(7) 0.0013(7) 0.0038(7) O5 0.0169(6) 0.0293(7) 0.0148(6) 0.0022(5) -0.0018(5) 0.0081(5) C5 0.0252(9) 0.0218(9) 0.0144(9) 0.0028(7) 0.0049(7) 0.0121(7) O6 0.0202(6) 0.0272(7) 0.0139(6) 0.0030(5) 0.0065(5) 0.0103(5) C6 0.0180(8) 0.0205(9) 0.0194(9) 0.0060(7) 0.0044(7) 0.0063(7) O7 0.0396(8) 0.0362(8) 0.0169(7) 0.0057(6) 0.0131(6) 0.0170(7) C7 0.0173(8) 0.0160(8) 0.0173(9) 0.0005(7) 0.0007(7) 0.0048(7) O8 0.0341(8) 0.0543(10) 0.0150(7) 0.0000(7) -0.0040(6) 0.0104(7) C8 0.0172(8) 0.0130(8) 0.0122(8) 0.0021(6) 0.0019(6) 0.0078(6) O9 0.0128(6) 0.0224(6) 0.0184(6) 0.0020(5) 0.0046(5) 0.0055(5) C9 0.0154(8) 0.0129(8) 0.0127(8) 0.0030(6) 0.0025(6) 0.0067(6) O10 0.0186(6) 0.0337(7) 0.0212(7) 0.0155(6) 0.0076(5) 0.0159(6) C10 0.0145(8) 0.0166(8) 0.0164(9) 0.0015(7) 0.0036(7) 0.0065(7) O11 0.0361(8) 0.0295(8) 0.0154(7) -0.0008(6) 0.0038(6) 0.0033(6) C11 0.0164(8) 0.0181(8) 0.0171(9) 0.0020(7) -0.0008(7) 0.0052(7) O12 0.0214(7) 0.0265(7) 0.0225(7) 0.0081(6) 0.0058(5) 0.0020(6) C12 0.0244(9) 0.0135(8) 0.0115(8) 0.0018(6) 0.0031(7) 0.0060(7) O13 0.0150(6) 0.0211(6) 0.0223(7) 0.0078(5) 0.0056(5) 0.0077(5) C13 0.0193(9) 0.0224(9) 0.0173(9) 0.0041(7) 0.0074(7) 0.0090(7) O14 0.0145(6) 0.0254(7) 0.0186(7) 0.0040(5) 0.0053(5) 0.0099(5) C14 0.0143(8) 0.0220(9) 0.0169(9) 0.0038(7) 0.0017(7) 0.0082(7) O15 0.0134(7) 0.0306(8) 0.0249(7) -0.0109(6) -0.0011(5) 0.0116(6) C15 0.0149(8) 0.0123(8) 0.0185(9) 0.0031(7) 0.0055(7) 0.0064(6) O16 0.0296(7) 0.0248(7) 0.0201(7) -0.0024(6) 0.0032(6) 0.0116(6) C16 0.0153(8) 0.0113(8) 0.0181(9) 0.0035(6) 0.0046(7) 0.0062(6) C17 0.0122(8) 0.0174(8) 0.0212(9) 0.0025(7) 0.0032(7) 0.0045(6) C18 0.0172(8) 0.0167(8) 0.0163(9) 0.0007(7) -0.0013(7) 0.0045(7) C19 0.0183(8) 0.0134(8) 0.0144(8) 0.0037(6) 0.0051(7) 0.0065(6) C20 0.0133(8) 0.0177(8) 0.0186(9) 0.0040(7) 0.0026(7) 0.0039(7) C21 0.0137(8) 0.0184(8) 0.0164(9) 0.0047(7) 0.0010(7) 0.0058(7) C22 0.0385(12) 0.0428(13) 0.0229(11) 0.0137(10) 0.0044(9) 0.0104(10) C23 0.0357(11) 0.0236(10) 0.0367(12) 0.0076(9) 0.0031(9) 0.0134(9) C24 0.0255(11) 0.0413(13) 0.0520(15) 0.0179(11) 0.0125(10) 0.0196(10) C25 0.0413(12) 0.0257(10) 0.0205(10) -0.0029(8) 0.0061(9) 0.0068(9) _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 Y1 O5 2.2688(12) . ? Y1 O10 2.2887(12) 2_676 ? Y1 O6 2.3022(12) 2_576 ? Y1 O1 2.3490(12) . ? Y1 O15 2.3709(14) . ? Y1 O9 2.3723(12) . ? Y1 O13 2.4305(12) . ? Y1 O14 2.4469(13) . ? S1 O13 1.5244(13) . ? S1 C23 1.784(2) . ? S1 C22 1.785(2) . ? O1 C1 1.265(2) . ? N1 O4 1.220(2) . ? N1 O3 1.230(2) . ? N1 C5 1.473(2) . ? C1 O2 1.243(2) . ? C1 C2 1.519(2) . ? S2 O16 1.5130(14) . ? S2 C25 1.773(2) . ? S2 C24 1.779(2) . ? N2 O7 1.222(2) . ? N2 O8 1.224(2) . ? N2 C12 1.476(2) . ? C2 C3 1.389(2) . ? C2 C7 1.389(2) . ? N3 O11 1.220(2) . ? N3 O12 1.2285(19) . ? N3 C19 1.464(2) . ? C3 C4 1.387(3) . ? C3 H3 0.9300 . ? C4 C5 1.383(3) . ? C4 H4 0.9300 . ? O5 C8 1.250(2) . ? C5 C6 1.379(3) . ? O6 C8 1.256(2) . ? O6 Y1 2.3022(12) 2_576 ? C6 C7 1.381(2) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.507(2) . ? O9 C15 1.257(2) . ? C9 C10 1.388(2) . ? C9 C14 1.400(2) . ? O10 C15 1.257(2) . ? O10 Y1 2.2887(12) 2_676 ? C10 C11 1.389(2) . ? C10 H10 0.9300 . ? C11 C12 1.381(2) . ? C11 H11 0.9300 . ? C12 C13 1.381(3) . ? C13 C14 1.382(2) . ? C13 H13 0.9300 . ? O14 H1O 0.76(2) . ? O14 H2O 0.92(3) . ? C14 H14 0.9300 . ? O15 H3O 0.84(3) . ? O15 H4O 0.74(3) . ? C15 C16 1.501(2) . ? C16 C17 1.392(2) . ? C16 C21 1.400(2) . ? C17 C18 1.384(2) . ? C17 H17 0.9300 . ? C18 C19 1.387(2) . ? C18 H18 0.9300 . ? C19 C20 1.383(2) . ? C20 C21 1.382(2) . ? C20 H20 0.9300 . ? C21 H21 0.9300 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? 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 Y1 O10 146.51(5) . 2_676 ? O5 Y1 O6 102.38(4) . 2_576 ? O10 Y1 O6 91.79(5) 2_676 2_576 ? O5 Y1 O1 78.66(5) . . ? O10 Y1 O1 72.38(5) 2_676 . ? O6 Y1 O1 144.13(5) 2_576 . ? O5 Y1 O15 141.70(5) . . ? O10 Y1 O15 71.25(5) 2_676 . ? O6 Y1 O15 74.25(5) 2_576 . ? O1 Y1 O15 126.51(5) . . ? O5 Y1 O9 86.78(4) . . ? O10 Y1 O9 99.12(4) 2_676 . ? O6 Y1 O9 144.55(5) 2_576 . ? O1 Y1 O9 71.02(4) . . ? O15 Y1 O9 77.56(5) . . ? O5 Y1 O13 70.57(5) . . ? O10 Y1 O13 142.91(5) 2_676 . ? O6 Y1 O13 74.51(4) 2_576 . ? O1 Y1 O13 136.10(5) . . ? O15 Y1 O13 71.87(5) . . ? O9 Y1 O13 76.62(4) . . ? O5 Y1 O14 76.24(5) . . ? O10 Y1 O14 79.19(5) 2_676 . ? O6 Y1 O14 73.16(5) 2_576 . ? O1 Y1 O14 72.35(4) . . ? O15 Y1 O14 134.70(5) . . ? O9 Y1 O14 141.94(4) . . ? O13 Y1 O14 126.53(4) . . ? O13 S1 C23 105.05(9) . . ? O13 S1 C22 104.53(9) . . ? C23 S1 C22 98.19(11) . . ? C1 O1 Y1 140.76(11) . . ? O4 N1 O3 123.96(16) . . ? O4 N1 C5 118.44(16) . . ? O3 N1 C5 117.60(16) . . ? O2 C1 O1 125.58(16) . . ? O2 C1 C2 118.62(16) . . ? O1 C1 C2 115.80(15) . . ? O16 S2 C25 104.67(9) . . ? O16 S2 C24 106.78(10) . . ? C25 S2 C24 98.53(11) . . ? O7 N2 O8 123.85(16) . . ? O7 N2 C12 117.98(16) . . ? O8 N2 C12 118.17(15) . . ? C3 C2 C7 119.72(16) . . ? C3 C2 C1 120.92(16) . . ? C7 C2 C1 119.35(16) . . ? O11 N3 O12 124.05(16) . . ? O11 N3 C19 118.71(15) . . ? O12 N3 C19 117.23(15) . . ? C4 C3 C2 120.48(17) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 118.03(17) . . ? C5 C4 H4 121.0 . . ? C3 C4 H4 121.0 . . ? C8 O5 Y1 162.58(12) . . ? C6 C5 C4 122.83(16) . . ? C6 C5 N1 118.25(16) . . ? C4 C5 N1 118.87(16) . . ? C8 O6 Y1 141.21(11) . 2_576 ? C5 C6 C7 118.21(16) . . ? C5 C6 H6 120.9 . . ? C7 C6 H6 120.9 . . ? C6 C7 C2 120.69(16) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? O5 C8 O6 125.04(16) . . ? O5 C8 C9 117.73(14) . . ? O6 C8 C9 117.24(15) . . ? C15 O9 Y1 129.38(11) . . ? C10 C9 C14 119.99(16) . . ? C10 C9 C8 120.04(15) . . ? C14 C9 C8 119.96(15) . . ? C15 O10 Y1 150.20(12) . 2_676 ? C9 C10 C11 120.25(15) . . ? C9 C10 H10 119.9 . . ? C11 C10 H10 119.9 . . ? C12 C11 C10 118.10(16) . . ? C12 C11 H11 120.9 . . ? C10 C11 H11 120.9 . . ? C13 C12 C11 123.20(16) . . ? C13 C12 N2 118.70(15) . . ? C11 C12 N2 118.11(16) . . ? S1 O13 Y1 127.53(7) . . ? C12 C13 C14 118.06(16) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? Y1 O14 H1O 116.9(18) . . ? Y1 O14 H2O 105.9(17) . . ? H1O O14 H2O 106(2) . . ? C13 C14 C9 120.38(16) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? Y1 O15 H3O 125.1(17) . . ? Y1 O15 H4O 123(2) . . ? H3O O15 H4O 105(3) . . ? O9 C15 O10 124.84(16) . . ? O9 C15 C16 117.98(15) . . ? O10 C15 C16 117.18(14) . . ? C17 C16 C21 119.97(16) . . ? C17 C16 C15 120.54(15) . . ? C21 C16 C15 119.47(16) . . ? C18 C17 C16 120.60(16) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 117.97(16) . . ? C17 C18 H18 121.0 . . ? C19 C18 H18 121.0 . . ? C20 C19 C18 122.82(16) . . ? C20 C19 N3 118.67(15) . . ? C18 C19 N3 118.50(15) . . ? C21 C20 C19 118.52(16) . . ? C21 C20 H20 120.7 . . ? C19 C20 H20 120.7 . . ? C20 C21 C16 120.03(16) . . ? C20 C21 H21 120.0 . . ? C16 C21 H21 120.0 . . ? S1 C22 H22A 109.5 . . ? S1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S1 C23 H23A 109.5 . . ? S1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S2 C24 H24A 109.5 . . ? S2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S2 C25 H25A 109.5 . . ? S2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H2O O2 0.92(3) 1.79(3) 2.7015(19) 169(3) . O15 H4O O1 0.74(3) 2.23(3) 2.9246(19) 157(3) 2_676 O15 H4O O10 0.74(3) 2.34(3) 2.8522(19) 127(2) . O14 H1O O13 0.76(2) 2.09(2) 2.8315(17) 166(2) 2_576 O15 H3O O16 0.84(3) 1.86(3) 2.6915(19) 175(3) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.373 _refine_diff_density_min -0.590 _refine_diff_density_rms 0.062 # Attachment '10b.CIF' data_10b _database_code_depnum_ccdc_archive 'CCDC 649816' _audit_creation_method SHELXL-97 _chemical_name_systematic ; poly{[bis(aqua)(dimethylsulphoxide)tris(4-nitrobenzoato)terbium (III)].dimethylsulphoxide} ; _chemical_name_common {[Tb(4-NO2BA)3(DMSO)(H2O)2].DMSO}n _chemical_melting_point ? _chemical_formula_moiety 'C25 H28 N3 O16 S2 Tb1' _chemical_formula_sum 'C25 H28 N3 O16 S2 Tb1' _chemical_formula_weight 849.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9572(3) _cell_length_b 10.5317(4) _cell_length_c 15.9559(6) _cell_angle_alpha 98.894(2) _cell_angle_beta 96.585(1) _cell_angle_gamma 107.184(2) _cell_volume 1556.36(10) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.813 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 848 _exptl_absorpt_coefficient_mu 2.486 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5868 _exptl_absorpt_correction_T_max 0.8259 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 13670 _diffrn_reflns_av_R_equivalents 0.0378 _diffrn_reflns_av_sigmaI/netI 0.0635 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.34 _diffrn_reflns_theta_max 27.47 _reflns_number_total 7013 _reflns_number_gt 6007 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+1.9598P] 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 7013 _refine_ls_number_parameters 440 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0498 _refine_ls_R_factor_gt 0.0381 _refine_ls_wR_factor_ref 0.0758 _refine_ls_wR_factor_gt 0.0715 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.25093(2) 0.00667(2) -0.010938(12) 0.01396(6) Uani 1 1 d . . . S1 S 0.30819(11) 0.34055(11) -0.05521(7) 0.0224(2) Uani 1 1 d . . . O1 O 0.3955(3) -0.0984(3) 0.05538(19) 0.0251(7) Uani 1 1 d . . . N1 N 0.2605(4) -0.1970(4) 0.4247(2) 0.0211(8) Uani 1 1 d . . . C1 C 0.4822(4) -0.1039(4) 0.1176(3) 0.0162(8) Uani 1 1 d . . . H2O H 0.000(5) -0.205(5) 0.019(3) 0.020(14) Uiso 1 1 d . . . H1O H 0.061(6) -0.262(6) -0.030(4) 0.040(16) Uiso 1 1 d . . . H4O H 0.465(6) 0.269(7) 0.097(4) 0.06(2) Uiso 1 1 d . . . H3O H 0.527(6) 0.169(6) 0.073(3) 0.039(17) Uiso 1 1 d . . . S2 S 0.42508(11) 0.41462(11) 0.23615(7) 0.0212(2) Uani 1 1 d . . . O2 O 0.6119(3) -0.0882(3) 0.11720(18) 0.0203(6) Uani 1 1 d . . . N2 N 0.1393(4) 0.1619(4) 0.5196(2) 0.0226(8) Uani 1 1 d . . . C2 C 0.4241(4) -0.1312(4) 0.1986(3) 0.0141(8) Uani 1 1 d . . . O3 O 0.3159(3) -0.1141(3) 0.49169(19) 0.0309(8) Uani 1 1 d . . . N3 N 0.3021(4) -0.4485(4) -0.4901(2) 0.0264(9) Uani 1 1 d . . . C3 C 0.5152(4) -0.0909(4) 0.2772(3) 0.0186(9) Uani 1 1 d . . . H3 H 0.6147 -0.0504 0.2793 0.022 Uiso 1 1 calc R . . O4 O 0.1599(3) -0.3008(3) 0.41928(19) 0.0256(7) Uani 1 1 d . . . C4 C 0.4626(4) -0.1091(4) 0.3529(3) 0.0193(9) Uani 1 1 d . . . H4 H 0.5238 -0.0794 0.4072 0.023 Uiso 1 1 calc R . . O5 O 0.1807(3) 0.0685(3) 0.11929(18) 0.0211(6) Uani 1 1 d . . . C5 C 0.3173(4) -0.1724(4) 0.3462(3) 0.0162(8) Uani 1 1 d . . . O6 O -0.0546(3) 0.0191(3) 0.11075(18) 0.0219(7) Uani 1 1 d . . . C6 C 0.2244(4) -0.2160(4) 0.2683(3) 0.0163(8) Uani 1 1 d . . . H6 H 0.1258 -0.2613 0.2658 0.020 Uiso 1 1 calc R . . O7 O 0.2580(4) 0.1845(4) 0.5606(2) 0.0382(9) Uani 1 1 d . . . C7 C 0.2787(4) -0.1922(4) 0.1944(3) 0.0161(8) Uani 1 1 d . . . H7 H 0.2165 -0.2175 0.1406 0.019 Uiso 1 1 calc R . . O8 O 0.0334(3) 0.1572(3) 0.55335(19) 0.0299(8) Uani 1 1 d . . . C8 C 0.0698(4) 0.0550(4) 0.1517(2) 0.0146(8) Uani 1 1 d . . . O9 O 0.2514(3) -0.1813(3) -0.11342(18) 0.0215(6) Uani 1 1 d . . . C9 C 0.0870(4) 0.0857(4) 0.2489(2) 0.0130(8) Uani 1 1 d . . . O10 O 0.0623(3) -0.3677(3) -0.13526(19) 0.0232(7) Uani 1 1 d . . . C10 C -0.0282(4) 0.0882(4) 0.2895(2) 0.0175(9) Uani 1 1 d . . . H10 H -0.1191 0.0712 0.2559 0.021 Uiso 1 1 calc R . . O11 O 0.4139(4) -0.3777(3) -0.5069(2) 0.0340(8) Uani 1 1 d . . . C11 C -0.0127(4) 0.1152(4) 0.3785(3) 0.0192(9) Uani 1 1 d . . . H11 H -0.0911 0.1188 0.4066 0.023 Uiso 1 1 calc R . . O12 O 0.2228(4) -0.5527(3) -0.5378(2) 0.0390(9) Uani 1 1 d . . . C12 C 0.1206(4) 0.1367(4) 0.4249(2) 0.0165(8) Uani 1 1 d . . . O13 O 0.2215(3) 0.2286(3) -0.01424(18) 0.0196(6) Uani 1 1 d . . . C13 C 0.2384(4) 0.1361(4) 0.3872(3) 0.0177(9) Uani 1 1 d . . . H13 H 0.3288 0.1528 0.4213 0.021 Uiso 1 1 calc R . . O14 O 0.0704(3) -0.1970(3) 0.0119(2) 0.0192(7) Uani 1 1 d . . . C14 C 0.2207(4) 0.1104(4) 0.2980(2) 0.0155(8) Uani 1 1 d . . . H14 H 0.3000 0.1096 0.2702 0.019 Uiso 1 1 calc R . . O15 O 0.4556(4) 0.1773(4) 0.0755(2) 0.0289(8) Uani 1 1 d . . . C15 C 0.1656(4) -0.2928(4) -0.1588(3) 0.0162(8) Uani 1 1 d . . . O16 O 0.4747(3) 0.4287(3) 0.15100(19) 0.0255(7) Uani 1 1 d . . . C16 C 0.1986(4) -0.3332(4) -0.2473(3) 0.0162(8) Uani 1 1 d . . . C17 C 0.1071(4) -0.4484(4) -0.3044(3) 0.0218(9) Uani 1 1 d . . . H17 H 0.0226 -0.5012 -0.2881 0.026 Uiso 1 1 calc R . . C18 C 0.1396(5) -0.4855(4) -0.3849(3) 0.0233(10) Uani 1 1 d . . . H18 H 0.0789 -0.5645 -0.4241 0.028 Uiso 1 1 calc R . . C19 C 0.2621(4) -0.4051(4) -0.4068(3) 0.0190(9) Uani 1 1 d . . . C20 C 0.3527(4) -0.2890(4) -0.3525(3) 0.0187(9) Uani 1 1 d . . . H20 H 0.4355 -0.2350 -0.3698 0.022 Uiso 1 1 calc R . . C21 C 0.3199(4) -0.2533(4) -0.2722(2) 0.0174(9) Uani 1 1 d . . . H21 H 0.3806 -0.1736 -0.2338 0.021 Uiso 1 1 calc R . . C22 C 0.2089(5) 0.3127(5) -0.1600(3) 0.0348(12) Uani 1 1 d . . . H22A H 0.2163 0.2311 -0.1953 0.052 Uiso 1 1 calc R . . H22B H 0.2470 0.3910 -0.1864 0.052 Uiso 1 1 calc R . . H22C H 0.1086 0.3007 -0.1559 0.052 Uiso 1 1 calc R . . C23 C 0.2731(5) 0.4900(4) -0.0093(3) 0.0307(11) Uani 1 1 d . . . H23A H 0.3218 0.5210 0.0507 0.046 Uiso 1 1 calc R . . H23B H 0.1701 0.4703 -0.0112 0.046 Uiso 1 1 calc R . . H23C H 0.3079 0.5610 -0.0420 0.046 Uiso 1 1 calc R . . C24 C 0.5240(5) 0.5704(5) 0.3068(3) 0.0290(11) Uani 1 1 d . . . H24A H 0.6245 0.5756 0.3188 0.043 Uiso 1 1 calc R . . H24B H 0.4861 0.5757 0.3608 0.043 Uiso 1 1 calc R . . H24C H 0.5162 0.6461 0.2799 0.043 Uiso 1 1 calc R . . C25 C 0.2537(5) 0.4368(5) 0.2276(4) 0.0378(13) Uani 1 1 d . . . H25A H 0.1834 0.3573 0.1895 0.057 Uiso 1 1 calc R . . H25B H 0.2570 0.5179 0.2039 0.057 Uiso 1 1 calc R . . H25C H 0.2266 0.4474 0.2848 0.057 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 0.01482(10) 0.02175(11) 0.00672(9) 0.00097(7) 0.00178(7) 0.00892(8) S1 0.0161(5) 0.0258(6) 0.0264(6) 0.0095(5) 0.0041(4) 0.0061(4) O1 0.0201(15) 0.0413(19) 0.0279(17) 0.0210(15) 0.0111(13) 0.0211(14) N1 0.0229(19) 0.0219(19) 0.0189(19) 0.0058(16) 0.0043(15) 0.0065(16) C1 0.018(2) 0.014(2) 0.018(2) 0.0021(17) 0.0074(17) 0.0069(17) S2 0.0213(5) 0.0206(5) 0.0225(6) 0.0022(5) 0.0030(4) 0.0094(5) O2 0.0148(14) 0.0266(16) 0.0164(15) 0.0012(13) 0.0012(12) 0.0041(13) N2 0.032(2) 0.0203(19) 0.0131(18) 0.0027(15) 0.0032(16) 0.0062(17) C2 0.0141(19) 0.0096(18) 0.018(2) 0.0017(16) 0.0039(16) 0.0032(15) O3 0.0354(19) 0.0323(19) 0.0162(16) -0.0016(14) 0.0026(14) 0.0015(16) N3 0.038(2) 0.028(2) 0.0183(19) 0.0037(17) 0.0093(17) 0.0167(19) C3 0.0105(19) 0.018(2) 0.025(2) 0.0021(18) 0.0027(16) 0.0017(16) O4 0.0198(16) 0.0268(17) 0.0253(17) 0.0072(14) 0.0036(13) -0.0010(14) C4 0.020(2) 0.017(2) 0.018(2) 0.0001(17) -0.0015(17) 0.0050(18) O5 0.0195(15) 0.0305(17) 0.0140(14) 0.0006(13) 0.0056(12) 0.0102(13) C5 0.020(2) 0.014(2) 0.016(2) 0.0015(17) 0.0070(16) 0.0068(17) O6 0.0184(15) 0.0313(17) 0.0148(15) 0.0029(13) -0.0013(12) 0.0084(13) C6 0.0112(19) 0.018(2) 0.019(2) 0.0052(17) 0.0035(16) 0.0024(16) O7 0.033(2) 0.055(2) 0.0161(16) -0.0001(16) -0.0063(15) 0.0065(18) C7 0.0152(19) 0.017(2) 0.016(2) 0.0051(17) 0.0014(16) 0.0044(16) O8 0.0381(19) 0.0369(19) 0.0180(16) 0.0040(15) 0.0110(14) 0.0152(16) C8 0.021(2) 0.0127(19) 0.0109(19) 0.0037(16) 0.0017(16) 0.0061(17) O9 0.0195(15) 0.0214(16) 0.0210(16) -0.0031(13) 0.0059(12) 0.0053(13) C9 0.0164(19) 0.0146(19) 0.0084(18) 0.0017(16) 0.0022(15) 0.0059(16) O10 0.0175(15) 0.0264(17) 0.0213(16) 0.0010(14) 0.0053(12) 0.0016(13) C10 0.015(2) 0.027(2) 0.0116(19) 0.0028(18) 0.0017(16) 0.0085(18) O11 0.0326(19) 0.043(2) 0.0273(18) 0.0052(16) 0.0162(15) 0.0105(16) C11 0.021(2) 0.021(2) 0.017(2) 0.0028(18) 0.0054(17) 0.0084(18) O12 0.063(2) 0.0222(18) 0.0215(17) -0.0078(15) 0.0115(17) 0.0022(17) C12 0.024(2) 0.014(2) 0.0105(19) 0.0001(16) 0.0041(16) 0.0053(17) O13 0.0142(14) 0.0230(16) 0.0251(16) 0.0089(13) 0.0055(12) 0.0082(12) C13 0.0143(19) 0.022(2) 0.014(2) -0.0006(17) -0.0013(16) 0.0042(17) O14 0.0141(16) 0.0276(18) 0.0175(16) 0.0029(14) 0.0059(13) 0.0084(14) C14 0.0110(18) 0.020(2) 0.016(2) 0.0013(17) 0.0029(15) 0.0064(16) O15 0.0147(17) 0.034(2) 0.0296(19) -0.0178(15) -0.0055(14) 0.0116(15) C15 0.019(2) 0.018(2) 0.013(2) 0.0029(17) 0.0017(16) 0.0086(17) O16 0.0288(17) 0.0255(17) 0.0182(15) -0.0045(13) 0.0023(13) 0.0078(14) C16 0.017(2) 0.020(2) 0.015(2) 0.0056(17) 0.0040(16) 0.0102(17) C17 0.020(2) 0.020(2) 0.021(2) -0.0026(18) 0.0050(18) 0.0034(18) C18 0.024(2) 0.019(2) 0.022(2) -0.0036(18) 0.0021(18) 0.0043(19) C19 0.024(2) 0.021(2) 0.013(2) 0.0008(17) 0.0043(17) 0.0104(18) C20 0.019(2) 0.019(2) 0.017(2) 0.0015(17) 0.0025(17) 0.0038(17) C21 0.018(2) 0.019(2) 0.0103(19) -0.0009(17) -0.0006(16) 0.0030(17) C22 0.040(3) 0.041(3) 0.022(2) 0.011(2) 0.000(2) 0.011(2) C23 0.033(3) 0.024(2) 0.035(3) 0.006(2) 0.001(2) 0.010(2) C24 0.034(3) 0.029(3) 0.019(2) -0.005(2) 0.004(2) 0.008(2) C25 0.026(3) 0.042(3) 0.051(3) 0.015(3) 0.008(2) 0.016(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 O6 2.296(3) 2 ? Tb1 O1 2.318(3) . ? Tb1 O5 2.327(3) . ? Tb1 O9 2.366(3) . ? Tb1 O15 2.389(3) . ? Tb1 O2 2.401(3) 2_655 ? Tb1 O13 2.448(3) . ? Tb1 O14 2.465(3) . ? Tb1 Tb1 4.9774(4) 2_655 ? Tb1 Tb1 5.0112(4) 2 ? S1 O13 1.526(3) . ? S1 C22 1.776(5) . ? S1 C23 1.779(5) . ? O1 C1 1.259(5) . ? N1 O3 1.225(4) . ? N1 O4 1.229(4) . ? N1 C5 1.461(5) . ? C1 O2 1.254(5) . ? C1 C2 1.508(5) . ? S2 O16 1.512(3) . ? S2 C24 1.776(4) . ? S2 C25 1.782(5) . ? O2 Tb1 2.401(3) 2_655 ? N2 O7 1.220(5) . ? N2 O8 1.230(5) . ? N2 C12 1.473(5) . ? C2 C3 1.388(6) . ? C2 C7 1.388(5) . ? N3 O12 1.224(5) . ? N3 O11 1.228(5) . ? N3 C19 1.475(5) . ? C3 C4 1.388(6) . ? C3 H3 0.9500 . ? C4 C5 1.386(5) . ? C4 H4 0.9500 . ? O5 C8 1.252(5) . ? C5 C6 1.386(5) . ? O6 C8 1.251(5) . ? O6 Tb1 2.296(3) 2 ? C6 C7 1.379(5) . ? C6 H6 0.9500 . ? C7 H7 0.9500 . ? C8 C9 1.513(5) . ? O9 C15 1.279(5) . ? C9 C10 1.386(5) . ? C9 C14 1.396(5) . ? O10 C15 1.234(5) . ? C10 C11 1.385(5) . ? C10 H10 0.9500 . ? C11 C12 1.381(6) . ? C11 H11 0.9500 . ? C12 C13 1.379(5) . ? C13 C14 1.388(5) . ? C13 H13 0.9500 . ? O14 H2O 0.71(5) . ? O14 H1O 0.86(6) . ? C14 H14 0.9500 . ? O15 H4O 0.94(6) . ? O15 H3O 0.75(6) . ? C15 C16 1.511(5) . ? C16 C21 1.393(5) . ? C16 C17 1.395(6) . ? C17 C18 1.387(6) . ? C17 H17 0.9500 . ? C18 C19 1.381(6) . ? C18 H18 0.9500 . ? C19 C20 1.379(6) . ? C20 C21 1.381(6) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? 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 O1 146.77(11) 2 . ? O6 Tb1 O5 103.13(10) 2 . ? O1 Tb1 O5 90.46(10) . . ? O6 Tb1 O9 78.66(10) 2 . ? O1 Tb1 O9 72.77(11) . . ? O5 Tb1 O9 143.60(10) . . ? O6 Tb1 O15 141.36(12) 2 . ? O1 Tb1 O15 71.34(12) . . ? O5 Tb1 O15 74.36(11) . . ? O9 Tb1 O15 126.42(11) . . ? O6 Tb1 O2 85.71(10) 2 2_655 ? O1 Tb1 O2 100.51(10) . 2_655 ? O5 Tb1 O2 144.88(10) . 2_655 ? O9 Tb1 O2 71.21(10) . 2_655 ? O15 Tb1 O2 77.78(11) . 2_655 ? O6 Tb1 O13 70.71(10) 2 . ? O1 Tb1 O13 142.53(11) . . ? O5 Tb1 O13 74.96(10) . . ? O9 Tb1 O13 136.44(10) . . ? O15 Tb1 O13 71.52(11) . . ? O2 Tb1 O13 76.23(10) 2_655 . ? O6 Tb1 O14 75.96(10) 2 . ? O1 Tb1 O14 79.22(10) . . ? O5 Tb1 O14 73.50(11) . . ? O9 Tb1 O14 71.76(11) . . ? O15 Tb1 O14 135.67(12) . . ? O2 Tb1 O14 141.16(11) 2_655 . ? O13 Tb1 O14 126.60(10) . . ? O6 Tb1 Tb1 141.43(7) 2 2_655 ? O1 Tb1 Tb1 40.51(7) . 2_655 ? O5 Tb1 Tb1 115.37(7) . 2_655 ? O9 Tb1 Tb1 72.04(7) . 2_655 ? O15 Tb1 Tb1 54.81(9) . 2_655 ? O2 Tb1 Tb1 61.60(7) 2_655 2_655 ? O13 Tb1 Tb1 115.92(6) . 2_655 ? O14 Tb1 Tb1 116.26(8) . 2_655 ? O6 Tb1 Tb1 46.53(7) 2 2 ? O1 Tb1 Tb1 130.94(7) . 2 ? O5 Tb1 Tb1 57.36(7) . 2 ? O9 Tb1 Tb1 110.24(7) . 2 ? O15 Tb1 Tb1 123.31(9) . 2 ? O2 Tb1 Tb1 127.47(7) 2_655 2 ? O13 Tb1 Tb1 68.92(6) . 2 ? O14 Tb1 Tb1 57.86(8) . 2 ? Tb1 Tb1 Tb1 170.906(9) 2_655 2 ? O13 S1 C22 104.5(2) . . ? O13 S1 C23 105.4(2) . . ? C22 S1 C23 98.3(2) . . ? C1 O1 Tb1 151.9(3) . . ? O3 N1 O4 124.0(4) . . ? O3 N1 C5 118.4(3) . . ? O4 N1 C5 117.5(3) . . ? O2 C1 O1 125.1(4) . . ? O2 C1 C2 118.1(4) . . ? O1 C1 C2 116.8(3) . . ? O16 S2 C24 104.6(2) . . ? O16 S2 C25 107.0(2) . . ? C24 S2 C25 98.4(2) . . ? C1 O2 Tb1 127.1(3) . 2_655 ? O7 N2 O8 123.2(4) . . ? O7 N2 C12 118.8(4) . . ? O8 N2 C12 118.0(4) . . ? C3 C2 C7 120.3(4) . . ? C3 C2 C1 119.9(3) . . ? C7 C2 C1 119.8(4) . . ? O12 N3 O11 124.1(4) . . ? O12 N3 C19 118.4(4) . . ? O11 N3 C19 117.6(4) . . ? C2 C3 C4 120.7(4) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C5 C4 C3 117.5(4) . . ? C5 C4 H4 121.3 . . ? C3 C4 H4 121.3 . . ? C8 O5 Tb1 140.1(3) . . ? C4 C5 C6 123.0(4) . . ? C4 C5 N1 118.3(4) . . ? C6 C5 N1 118.7(4) . . ? C8 O6 Tb1 163.5(3) . 2 ? C7 C6 C5 118.4(4) . . ? C7 C6 H6 120.8 . . ? C5 C6 H6 120.8 . . ? C6 C7 C2 120.2(4) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? O6 C8 O5 125.8(4) . . ? O6 C8 C9 116.8(3) . . ? O5 C8 C9 117.5(3) . . ? C15 O9 Tb1 140.3(3) . . ? C10 C9 C14 119.8(4) . . ? C10 C9 C8 121.0(3) . . ? C14 C9 C8 119.3(3) . . ? C11 C10 C9 121.0(4) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 117.6(4) . . ? C12 C11 H11 121.2 . . ? C10 C11 H11 121.2 . . ? C13 C12 C11 123.4(4) . . ? C13 C12 N2 117.8(4) . . ? C11 C12 N2 118.8(4) . . ? S1 O13 Tb1 127.44(16) . . ? C12 C13 C14 118.0(4) . . ? C12 C13 H13 121.0 . . ? C14 C13 H13 121.0 . . ? Tb1 O14 H2O 129(4) . . ? Tb1 O14 H1O 108(4) . . ? H2O O14 H1O 104(5) . . ? C13 C14 C9 120.3(4) . . ? C13 C14 H14 119.9 . . ? C9 C14 H14 119.9 . . ? Tb1 O15 H4O 127(4) . . ? Tb1 O15 H3O 118(4) . . ? H4O O15 H3O 111(5) . . ? O10 C15 O9 125.1(4) . . ? O10 C15 C16 119.3(4) . . ? O9 C15 C16 115.6(3) . . ? C21 C16 C17 120.0(4) . . ? C21 C16 C15 119.6(4) . . ? C17 C16 C15 120.4(4) . . ? C18 C17 C16 119.9(4) . . ? C18 C17 H17 120.1 . . ? C16 C17 H17 120.1 . . ? C19 C18 C17 118.4(4) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C20 C19 C18 122.9(4) . . ? C20 C19 N3 118.3(4) . . ? C18 C19 N3 118.7(4) . . ? C19 C20 C21 118.2(4) . . ? C19 C20 H20 120.9 . . ? C21 C20 H20 120.9 . . ? C20 C21 C16 120.5(4) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? S1 C22 H22A 109.5 . . ? S1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? S1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? S1 C23 H23A 109.5 . . ? S1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? S1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? S2 C24 H24A 109.5 . . ? S2 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? S2 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S2 C25 H25A 109.5 . . ? S2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O14 H2O O13 0.71(5) 2.14(5) 2.831(4) 169(5) 2 O14 H1O O10 0.86(6) 1.87(6) 2.705(5) 165(5) . O15 H4O O16 0.94(6) 1.74(7) 2.676(5) 171(6) . O15 H3O O9 0.75(6) 2.18(6) 2.898(4) 160(6) 2_655 O15 H3O O1 0.75(6) 2.36(6) 2.855(5) 125(5) 2_655 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.211 _refine_diff_density_min -1.440 _refine_diff_density_rms 0.144 # Attachment '11a.CIF' data_11a _database_code_depnum_ccdc_archive 'CCDC 649817' _audit_creation_method SHELXL-97 _chemical_name_systematic ; di[(aqua)(dimethylformamide)tris(4-methoxybenzoato)yttrium(III)] ; _chemical_name_common '[Y(4-MeOBA)3(H2O)(DMF)]2' _chemical_melting_point ? _chemical_formula_moiety 'C54 H60 N2 O22 Y2' _chemical_formula_sum 'C54 H60 N2 O22 Y2' _chemical_formula_weight 1266.86 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3522(13) _cell_length_b 24.8189(30) _cell_length_c 14.2312(21) _cell_angle_alpha 90.00 _cell_angle_beta 106.889(6) _cell_angle_gamma 90.00 _cell_volume 2822.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.490 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1304 _exptl_absorpt_coefficient_mu 2.126 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5956 _exptl_absorpt_correction_T_max 0.7261 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _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 18257 _diffrn_reflns_av_R_equivalents 0.0982 _diffrn_reflns_av_sigmaI/netI 0.1173 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6420 _reflns_number_gt 3876 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6420 _refine_ls_number_parameters 379 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1054 _refine_ls_R_factor_gt 0.0418 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.0818 _refine_ls_goodness_of_fit_ref 0.968 _refine_ls_restrained_S_all 0.968 _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 Y1 Y 0.36684(4) -0.005537(11) 0.61644(2) 0.01323(9) Uani 1 1 d . . . O1 O 0.3470(3) 0.05568(8) 0.74009(16) 0.0190(5) Uani 1 1 d . . . C1 C 0.2050(4) 0.07397(12) 0.6944(2) 0.0154(7) Uani 1 1 d . . . O2 O 0.1287(3) 0.05677(8) 0.60890(17) 0.0179(5) Uani 1 1 d . . . C2 C 0.1305(4) 0.11740(12) 0.7414(2) 0.0173(7) Uani 1 1 d . . . O3 O -0.0838(3) 0.23418(10) 0.8757(2) 0.0364(7) Uani 1 1 d . . . C3 C 0.2190(5) 0.13700(14) 0.8327(3) 0.0251(8) Uani 1 1 d . . . H3 H 0.3276 0.1231 0.8638 0.030 Uiso 1 1 calc R . . O4 O 0.6575(3) 0.00196(8) 0.68525(15) 0.0168(5) Uani 1 1 d . . . C4 C 0.1536(5) 0.17627(13) 0.8799(3) 0.0260(8) Uani 1 1 d . . . H4 H 0.2164 0.1893 0.9425 0.031 Uiso 1 1 calc R . . O5 O 0.5319(3) -0.04469(8) 0.77455(16) 0.0178(5) Uani 1 1 d . . . C5 C -0.0044(5) 0.19618(13) 0.8348(3) 0.0255(8) Uani 1 1 d . . . O6 O 1.2952(3) -0.06475(10) 1.03252(19) 0.0317(6) Uani 1 1 d . . . C6 C -0.0938(5) 0.17804(14) 0.7421(3) 0.0321(9) Uani 1 1 d . . . H6 H -0.2012 0.1926 0.7105 0.039 Uiso 1 1 calc R . . O7 O 0.5510(3) -0.06051(8) 0.46793(16) 0.0173(5) Uani 1 1 d . . . C7 C -0.0269(5) 0.13878(13) 0.6955(3) 0.0251(8) Uani 1 1 d . . . H7 H -0.0885 0.1264 0.6321 0.030 Uiso 1 1 calc R . . O8 O 0.4392(3) -0.09292(8) 0.58022(16) 0.0190(5) Uani 1 1 d . . . C8 C -0.0037(5) 0.24957(16) 0.9746(3) 0.0411(11) Uani 1 1 d . . . H8A H -0.0721 0.2766 0.9953 0.062 Uiso 1 1 calc R . . H8B H 0.1065 0.2648 0.9793 0.062 Uiso 1 1 calc R . . H8C H 0.0095 0.2179 1.0173 0.062 Uiso 1 1 calc R . . O9 O 0.5229(3) -0.31105(8) 0.37094(18) 0.0294(6) Uani 1 1 d . . . C9 C 0.6650(4) -0.02594(12) 0.7627(2) 0.0156(7) Uani 1 1 d . . . O10 O 0.1673(3) -0.05862(8) 0.65243(17) 0.0197(5) Uani 1 1 d . . . N10 N 0.0575(4) -0.12976(11) 0.7107(2) 0.0245(7) Uani 1 1 d . . . C10 C 0.8301(4) -0.03601(12) 0.8348(2) 0.0179(7) Uani 1 1 d . . . O11 O 0.1907(3) -0.01909(10) 0.45787(18) 0.0196(5) Uani 1 1 d . . . C11 C 0.8445(5) -0.06718(13) 0.9179(2) 0.0216(8) Uani 1 1 d . A . H11 H 0.7470 -0.0820 0.9294 0.026 Uiso 1 1 calc R . . H11A H 0.222(5) -0.0141(14) 0.417(3) 0.023(12) Uiso 1 1 d . . . H11B H 0.088(5) -0.0335(14) 0.437(3) 0.033(12) Uiso 1 1 d . . . C12 C 0.9993(5) -0.07686(15) 0.9839(3) 0.0274(9) Uani 1 1 d . . . H12 H 1.0080 -0.0983 1.0405 0.033 Uiso 1 1 calc R A . C13 C 1.1427(5) -0.05520(15) 0.9676(3) 0.0304(9) Uani 1 1 d . A . C14 C 1.1293(5) -0.02381(15) 0.8847(3) 0.0277(8) Uani 1 1 d . . . H14 H 1.2265 -0.0088 0.8730 0.033 Uiso 1 1 calc R A . C15 C 0.9744(4) -0.01471(13) 0.8198(2) 0.0212(7) Uani 1 1 d . A . H15 H 0.9657 0.0067 0.7632 0.025 Uiso 1 1 calc R . . C16A C 1.3010(9) -0.1011(3) 1.1207(5) 0.0301(19) Uani 0.508(6) 1 d P A 1 H16A H 1.4171 -0.1049 1.1617 0.045 Uiso 0.508(6) 1 calc PR A 1 H16B H 1.2558 -0.1367 1.0972 0.045 Uiso 0.508(6) 1 calc PR A 1 H16C H 1.2339 -0.0850 1.1595 0.045 Uiso 0.508(6) 1 calc PR A 1 C16B C 1.4455(9) -0.0334(3) 1.0193(5) 0.0261(19) Uani 0.492(6) 1 d P A 2 H16D H 1.5470 -0.0440 1.0705 0.039 Uiso 0.492(6) 1 calc PR A 2 H16E H 1.4266 0.0053 1.0243 0.039 Uiso 0.492(6) 1 calc PR A 2 H16F H 1.4590 -0.0414 0.9546 0.039 Uiso 0.492(6) 1 calc PR A 2 C17 C 0.4958(4) -0.09874(12) 0.5079(2) 0.0147(7) Uani 1 1 d . . . C18 C 0.4988(4) -0.15455(12) 0.4683(2) 0.0155(7) Uani 1 1 d . . . C19 C 0.5577(5) -0.16367(12) 0.3879(3) 0.0227(8) Uani 1 1 d . . . H19 H 0.5926 -0.1340 0.3564 0.027 Uiso 1 1 calc R . . C20 C 0.5665(5) -0.21542(13) 0.3527(3) 0.0250(8) Uani 1 1 d . . . H20 H 0.6074 -0.2210 0.2977 0.030 Uiso 1 1 calc R . . C21 C 0.5156(4) -0.25862(12) 0.3978(3) 0.0212(8) Uani 1 1 d . . . C22 C 0.4516(5) -0.25004(13) 0.4771(3) 0.0247(8) Uani 1 1 d . . . H22 H 0.4140 -0.2797 0.5073 0.030 Uiso 1 1 calc R . . C23 C 0.4433(5) -0.19829(13) 0.5113(2) 0.0212(7) Uani 1 1 d . . . H23 H 0.3992 -0.1925 0.5649 0.025 Uiso 1 1 calc R . . C24 C 0.5784(6) -0.32084(14) 0.2864(3) 0.0380(10) Uani 1 1 d . . . H24A H 0.5785 -0.3597 0.2742 0.057 Uiso 1 1 calc R . . H24B H 0.6920 -0.3066 0.2979 0.057 Uiso 1 1 calc R . . H24C H 0.5029 -0.3029 0.2292 0.057 Uiso 1 1 calc R . . C25 C 0.1797(4) -0.09606(13) 0.7113(3) 0.0205(8) Uani 1 1 d . . . H25 H 0.2839 -0.1009 0.7601 0.025 Uiso 1 1 calc R . . C26 C -0.1059(5) -0.12355(15) 0.6379(3) 0.0307(9) Uani 1 1 d . . . H26A H -0.1818 -0.1517 0.6476 0.046 Uiso 0.50 1 calc PR . . H26B H -0.0931 -0.1267 0.5717 0.046 Uiso 0.50 1 calc PR . . H26C H -0.1521 -0.0881 0.6454 0.046 Uiso 0.50 1 calc PR . . H26D H -0.1029 -0.0926 0.5956 0.046 Uiso 0.50 1 calc PR . . H26E H -0.1915 -0.1176 0.6714 0.046 Uiso 0.50 1 calc PR . . H26F H -0.1326 -0.1563 0.5977 0.046 Uiso 0.50 1 calc PR . . C27 C 0.0756(5) -0.16780(14) 0.7907(3) 0.0335(10) Uani 1 1 d . . . H27A H -0.0262 -0.1896 0.7786 0.050 Uiso 0.50 1 calc PR . . H27B H 0.0936 -0.1481 0.8526 0.050 Uiso 0.50 1 calc PR . . H27C H 0.1716 -0.1914 0.7950 0.050 Uiso 0.50 1 calc PR . . H27D H 0.1855 -0.1631 0.8389 0.050 Uiso 0.50 1 calc PR . . H27E H 0.0657 -0.2046 0.7649 0.050 Uiso 0.50 1 calc PR . . H27F H -0.0123 -0.1613 0.8224 0.050 Uiso 0.50 1 calc PR . . 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 Y1 0.01317(15) 0.01457(16) 0.01392(15) -0.00017(12) 0.00705(11) -0.00050(15) O1 0.0158(12) 0.0240(12) 0.0187(13) -0.0013(9) 0.0074(10) 0.0024(11) C1 0.0139(17) 0.0183(16) 0.0168(18) -0.0010(13) 0.0088(14) -0.0036(15) O2 0.0156(12) 0.0175(11) 0.0227(14) -0.0031(9) 0.0087(11) -0.0005(10) C2 0.0192(18) 0.0154(16) 0.0206(19) 0.0019(13) 0.0111(15) 0.0000(15) O3 0.0355(17) 0.0347(15) 0.0415(18) -0.0171(12) 0.0149(14) 0.0094(14) C3 0.0204(19) 0.031(2) 0.023(2) -0.0034(15) 0.0059(16) 0.0051(17) O4 0.0160(11) 0.0209(12) 0.0146(11) 0.0037(9) 0.0065(9) -0.0014(10) C4 0.027(2) 0.0308(19) 0.0209(19) -0.0090(15) 0.0081(17) 0.0040(18) O5 0.0163(12) 0.0207(12) 0.0192(13) 0.0033(9) 0.0097(10) 0.0007(11) C5 0.031(2) 0.0196(18) 0.031(2) -0.0054(15) 0.0171(18) 0.0020(17) O6 0.0210(14) 0.0463(16) 0.0250(15) 0.0040(12) 0.0025(12) 0.0077(13) C6 0.026(2) 0.027(2) 0.041(3) -0.0081(17) 0.0062(19) 0.0104(19) O7 0.0197(13) 0.0116(11) 0.0217(13) 0.0015(9) 0.0079(11) -0.0029(10) C7 0.026(2) 0.0254(19) 0.024(2) -0.0073(14) 0.0065(17) 0.0025(17) O8 0.0226(13) 0.0182(12) 0.0192(13) -0.0007(9) 0.0109(11) 0.0030(11) C8 0.051(3) 0.039(2) 0.042(3) -0.0149(18) 0.026(2) 0.007(2) O9 0.0420(17) 0.0122(11) 0.0376(16) -0.0072(10) 0.0174(14) 0.0011(12) C9 0.0183(17) 0.0144(16) 0.0165(18) -0.0026(12) 0.0090(15) -0.0002(15) O10 0.0218(13) 0.0177(12) 0.0243(14) 0.0020(9) 0.0138(11) -0.0026(11) N10 0.0264(17) 0.0168(14) 0.0362(19) 0.0003(12) 0.0184(16) -0.0040(14) C10 0.0184(18) 0.0194(17) 0.0170(18) -0.0040(13) 0.0069(15) 0.0014(15) O11 0.0176(13) 0.0298(14) 0.0142(13) -0.0010(10) 0.0090(11) -0.0065(12) C11 0.025(2) 0.0209(17) 0.0209(19) 0.0017(13) 0.0098(16) 0.0011(16) C12 0.032(2) 0.030(2) 0.018(2) 0.0012(14) 0.0038(18) 0.0092(18) C13 0.024(2) 0.040(2) 0.022(2) -0.0109(16) -0.0017(17) 0.0134(19) C14 0.0171(17) 0.044(2) 0.023(2) -0.0101(17) 0.0076(15) -0.0021(19) C15 0.0172(17) 0.0307(19) 0.0164(17) -0.0031(14) 0.0060(14) -0.0007(16) C16A 0.022(4) 0.040(4) 0.025(4) 0.004(3) 0.001(3) -0.005(4) C16B 0.013(4) 0.042(5) 0.025(4) -0.001(3) 0.009(3) 0.000(3) C17 0.0107(15) 0.0142(16) 0.0184(17) -0.0004(12) 0.0031(13) 0.0001(15) C18 0.0146(17) 0.0139(16) 0.0187(17) -0.0011(12) 0.0060(15) 0.0012(14) C19 0.029(2) 0.0165(17) 0.029(2) -0.0020(14) 0.0189(17) -0.0061(17) C20 0.033(2) 0.0216(18) 0.027(2) -0.0055(14) 0.0191(18) -0.0030(17) C21 0.0231(19) 0.0138(16) 0.026(2) -0.0040(13) 0.0054(16) -0.0012(16) C22 0.036(2) 0.0138(16) 0.028(2) 0.0013(13) 0.0145(17) -0.0050(17) C23 0.0274(19) 0.0183(17) 0.0209(19) 0.0009(13) 0.0119(16) -0.0017(17) C24 0.051(3) 0.0235(19) 0.044(3) -0.0152(17) 0.021(2) 0.002(2) C25 0.0126(17) 0.0252(19) 0.027(2) 0.0004(14) 0.0107(16) 0.0016(16) C26 0.026(2) 0.030(2) 0.038(3) -0.0040(16) 0.0119(19) -0.0067(18) C27 0.041(2) 0.026(2) 0.038(2) 0.0072(16) 0.020(2) -0.002(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 Y1 O7 2.254(2) 3_656 ? Y1 O10 2.296(2) . ? Y1 O11 2.332(3) . ? Y1 O4 2.346(2) . ? Y1 O8 2.349(2) . ? Y1 O1 2.367(2) . ? Y1 O5 2.471(2) . ? Y1 O2 2.497(2) . ? Y1 C9 2.789(3) . ? Y1 C1 2.797(3) . ? O1 C1 1.260(4) . ? C1 O2 1.272(4) . ? C1 C2 1.496(4) . ? C2 C3 1.384(5) . ? C2 C7 1.392(5) . ? O3 C5 1.376(4) . ? O3 C8 1.424(5) . ? C3 C4 1.383(4) . ? C3 H3 0.9500 . ? O4 C9 1.287(4) . ? C4 C5 1.381(5) . ? C4 H4 0.9500 . ? O5 C9 1.261(4) . ? C5 C6 1.389(5) . ? O6 C13 1.360(4) . ? O6 C16B 1.534(7) . ? O6 C16A 1.535(7) . ? C6 C7 1.384(4) . ? C6 H6 0.9500 . ? O7 C17 1.260(3) . ? O7 Y1 2.254(2) 3_656 ? C7 H7 0.9500 . ? O8 C17 1.260(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C21 1.362(3) . ? O9 C24 1.430(4) . ? C9 C10 1.482(5) . ? O10 C25 1.235(4) . ? N10 C25 1.317(4) . ? N10 C27 1.453(4) . ? N10 C26 1.462(5) . ? C10 C11 1.389(4) . ? C10 C15 1.388(4) . ? O11 H11A 0.71(4) . ? O11 H11B 0.89(4) . ? C11 C12 1.381(5) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.391(5) . ? C14 C15 1.372(5) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 C18 1.498(4) . ? C18 C19 1.389(4) . ? C18 C23 1.391(4) . ? C19 C20 1.388(4) . ? C19 H19 0.9500 . ? C20 C21 1.379(4) . ? C20 H20 0.9500 . ? C21 C22 1.398(5) . ? C22 C23 1.383(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C26 H26D 0.9800 . ? C26 H26E 0.9800 . ? C26 H26F 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C27 H27D 0.9800 . ? C27 H27E 0.9800 . ? C27 H27F 0.9800 . ? 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 O7 Y1 O10 152.80(9) 3_656 . ? O7 Y1 O11 78.08(9) 3_656 . ? O10 Y1 O11 80.71(9) . . ? O7 Y1 O4 74.12(8) 3_656 . ? O10 Y1 O4 133.03(8) . . ? O11 Y1 O4 134.46(8) . . ? O7 Y1 O8 114.65(7) 3_656 . ? O10 Y1 O8 76.63(7) . . ? O11 Y1 O8 77.57(8) . . ? O4 Y1 O8 82.17(8) . . ? O7 Y1 O1 91.56(8) 3_656 . ? O10 Y1 O1 89.44(7) . . ? O11 Y1 O1 130.63(8) . . ? O4 Y1 O1 85.77(8) . . ? O8 Y1 O1 146.52(8) . . ? O7 Y1 O5 126.55(8) 3_656 . ? O10 Y1 O5 79.64(8) . . ? O11 Y1 O5 148.49(8) . . ? O4 Y1 O5 54.22(7) . . ? O8 Y1 O5 74.07(7) . . ? O1 Y1 O5 73.53(7) . . ? O7 Y1 O2 83.61(7) 3_656 . ? O10 Y1 O2 75.19(7) . . ? O11 Y1 O2 77.13(8) . . ? O4 Y1 O2 133.11(7) . . ? O8 Y1 O2 144.60(8) . . ? O1 Y1 O2 53.65(8) . . ? O5 Y1 O2 120.62(7) . . ? O7 Y1 C9 100.70(9) 3_656 . ? O10 Y1 C9 106.13(9) . . ? O11 Y1 C9 150.60(9) . . ? O4 Y1 C9 27.34(8) . . ? O8 Y1 C9 76.41(8) . . ? O1 Y1 C9 78.59(8) . . ? O5 Y1 C9 26.88(7) . . ? O2 Y1 C9 132.22(8) . . ? O7 Y1 C1 87.43(8) 3_656 . ? O10 Y1 C1 81.41(8) . . ? O11 Y1 C1 104.11(9) . . ? O4 Y1 C1 109.83(9) . . ? O8 Y1 C1 157.43(8) . . ? O1 Y1 C1 26.61(9) . . ? O5 Y1 C1 97.03(8) . . ? O2 Y1 C1 27.04(9) . . ? C9 Y1 C1 105.18(9) . . ? C1 O1 Y1 96.1(2) . . ? O1 C1 O2 120.5(3) . . ? O1 C1 C2 118.7(3) . . ? O2 C1 C2 120.8(3) . . ? O1 C1 Y1 57.29(16) . . ? O2 C1 Y1 63.20(16) . . ? C2 C1 Y1 175.8(2) . . ? C1 O2 Y1 89.75(19) . . ? C3 C2 C7 118.8(3) . . ? C3 C2 C1 119.7(3) . . ? C7 C2 C1 121.6(3) . . ? C5 O3 C8 117.2(3) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 H3 119.2 . . ? C2 C3 H3 119.2 . . ? C9 O4 Y1 95.82(19) . . ? C5 C4 C3 119.0(3) . . ? C5 C4 H4 120.5 . . ? C3 C4 H4 120.5 . . ? C9 O5 Y1 90.74(18) . . ? O3 C5 C4 124.1(3) . . ? O3 C5 C6 115.6(3) . . ? C4 C5 C6 120.3(3) . . ? C13 O6 C16B 117.8(4) . . ? C13 O6 C16A 117.3(4) . . ? C16B O6 C16A 124.5(4) . . ? C7 C6 C5 120.2(4) . . ? C7 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? C17 O7 Y1 174.8(2) . 3_656 ? C6 C7 C2 120.1(3) . . ? C6 C7 H7 120.0 . . ? C2 C7 H7 120.0 . . ? C17 O8 Y1 117.82(19) . . ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C21 O9 C24 116.8(3) . . ? O5 C9 O4 119.2(3) . . ? O5 C9 C10 121.6(3) . . ? O4 C9 C10 119.2(3) . . ? O5 C9 Y1 62.37(17) . . ? O4 C9 Y1 56.84(16) . . ? C10 C9 Y1 175.7(2) . . ? C25 O10 Y1 131.3(2) . . ? C25 N10 C27 120.2(3) . . ? C25 N10 C26 119.9(3) . . ? C27 N10 C26 119.2(3) . . ? C11 C10 C15 118.6(3) . . ? C11 C10 C9 121.1(3) . . ? C15 C10 C9 120.3(3) . . ? Y1 O11 H11A 119(3) . . ? Y1 O11 H11B 131(2) . . ? H11A O11 H11B 110(4) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 120.0(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? O6 C13 C14 120.2(4) . . ? O6 C13 C12 120.1(3) . . ? C14 C13 C12 119.8(4) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C10 121.7(3) . . ? C14 C15 H15 119.2 . . ? C10 C15 H15 119.2 . . ? O6 C16A H16A 109.5 . . ? O6 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? O6 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O6 C16B H16D 109.5 . . ? O6 C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? O6 C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? O7 C17 O8 123.8(3) . . ? O7 C17 C18 118.6(3) . . ? O8 C17 C18 117.7(3) . . ? C19 C18 C23 118.6(3) . . ? C19 C18 C17 120.6(3) . . ? C23 C18 C17 120.8(3) . . ? C20 C19 C18 121.1(3) . . ? C20 C19 H19 119.5 . . ? C18 C19 H19 119.5 . . ? C21 C20 C19 119.7(3) . . ? C21 C20 H20 120.1 . . ? C19 C20 H20 120.1 . . ? O9 C21 C20 124.5(3) . . ? O9 C21 C22 115.5(3) . . ? C20 C21 C22 120.0(3) . . ? C23 C22 C21 119.7(3) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.9(3) . . ? C22 C23 H23 119.6 . . ? C18 C23 H23 119.6 . . ? O9 C24 H24A 109.5 . . ? O9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O10 C25 N10 124.2(3) . . ? O10 C25 H25 117.9 . . ? N10 C25 H25 117.9 . . ? N10 C26 H26A 109.5 . . ? N10 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N10 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N10 C26 H26D 109.5 . . ? H26A C26 H26D 141.1 . . ? H26B C26 H26D 56.3 . . ? H26C C26 H26D 56.3 . . ? N10 C26 H26E 109.5 . . ? H26A C26 H26E 56.3 . . ? H26B C26 H26E 141.1 . . ? H26C C26 H26E 56.3 . . ? H26D C26 H26E 109.5 . . ? N10 C26 H26F 109.5 . . ? H26A C26 H26F 56.3 . . ? H26B C26 H26F 56.3 . . ? H26C C26 H26F 141.1 . . ? H26D C26 H26F 109.5 . . ? H26E C26 H26F 109.5 . . ? N10 C27 H27A 109.5 . . ? N10 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? N10 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? N10 C27 H27D 109.5 . . ? H27A C27 H27D 141.1 . . ? H27B C27 H27D 56.3 . . ? H27C C27 H27D 56.3 . . ? N10 C27 H27E 109.5 . . ? H27A C27 H27E 56.3 . . ? H27B C27 H27E 141.1 . . ? H27C C27 H27E 56.3 . . ? H27D C27 H27E 109.5 . . ? N10 C27 H27F 109.5 . . ? H27A C27 H27F 56.3 . . ? H27B C27 H27F 56.3 . . ? H27C C27 H27F 141.1 . . ? H27D C27 H27F 109.5 . . ? H27E C27 H27F 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H11B O2 0.89(4) 1.83(4) 2.725(3) 175(4) 3_556 O11 H11A O4 0.71(4) 2.02(4) 2.727(3) 172(4) 3_656 C25 H25 O5 0.95 2.46 3.091(4) 124.2 . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.730 _refine_diff_density_min -1.581 _refine_diff_density_rms 0.123 # Attachment '11b.CIF' data_11b _database_code_depnum_ccdc_archive 'CCDC 649818' _audit_creation_method SHELXL-97 _chemical_name_systematic ; bis[(dimethylformamide)tri(4-methoxybenzoato)terbium(III)] ; _chemical_name_common '[(dmf/dsmo)(4-MeOBA)3Tb]2' _chemical_melting_point ? _chemical_formula_moiety 'C53.91 H59.91 N1.91 O22 S0.09 Tb2' _chemical_formula_sum 'C53.91 H59.91 N1.91 O22 S0.09 Tb2' _chemical_formula_weight 1407.42 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3594(3) _cell_length_b 24.7689(8) _cell_length_c 14.2505(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.805(1) _cell_angle_gamma 90.00 _cell_volume 2824.60(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.655 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1408.4 _exptl_absorpt_coefficient_mu 2.567 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5547 _exptl_absorpt_correction_T_max 0.6289 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(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 'Bruker X8 Apex II CCD' _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 21372 _diffrn_reflns_av_R_equivalents 0.0207 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.55 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6468 _reflns_number_gt 5937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0178P)^2^+2.7097P] 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 6468 _refine_ls_number_parameters 397 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.0242 _refine_ls_R_factor_gt 0.0206 _refine_ls_wR_factor_ref 0.0475 _refine_ls_wR_factor_gt 0.0457 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.074 _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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.368941(12) 0.494672(4) 0.614613(7) 0.01235(4) Uani 1 1 d . . . O1 O 0.13027(18) 0.55853(6) 0.60780(11) 0.0174(3) Uani 1 1 d . . . N1 N 0.0576(2) 0.37050(8) 0.71065(15) 0.0208(5) Uani 0.953(3) 1 d P A 1 C1 C 0.2061(3) 0.57551(8) 0.69287(16) 0.0156(4) Uani 1 1 d . . . O2 O 0.34801(19) 0.55714(6) 0.73851(11) 0.0197(3) Uani 1 1 d . . . C2 C 0.1309(3) 0.61836(8) 0.74047(16) 0.0172(4) Uani 1 1 d . . . O3 O -0.0844(2) 0.73438(8) 0.87629(14) 0.0374(5) Uani 1 1 d . . . C3 C -0.0264(3) 0.63973(9) 0.69563(18) 0.0252(5) Uani 1 1 d . . . H3 H -0.0879 0.6274 0.6324 0.030 Uiso 1 1 calc R . . O4 O 0.53491(18) 0.45600(6) 0.77497(11) 0.0168(3) Uani 1 1 d . . . C4 C -0.0944(3) 0.67866(11) 0.7418(2) 0.0320(6) Uani 1 1 d . . . H4 H -0.2017 0.6932 0.7102 0.038 Uiso 1 1 calc R . . O5 O 0.66159(19) 0.50296(6) 0.68626(11) 0.0175(3) Uani 1 1 d . . . C5 C -0.0053(3) 0.69671(9) 0.83503(19) 0.0256(5) Uani 1 1 d . . . O6 O 1.2960(2) 0.43492(8) 1.03239(13) 0.0322(4) Uani 1 1 d . . . C6 C 0.1529(3) 0.67676(10) 0.87998(18) 0.0273(5) Uani 1 1 d . . . H6 H 0.2153 0.6896 0.9427 0.033 Uiso 1 1 calc R . . O7 O 0.45394(19) 0.56104(6) 0.52711(11) 0.0179(3) Uani 1 1 d . . . C7 C 0.2192(3) 0.63768(10) 0.83221(17) 0.0254(5) Uani 1 1 d . . . H7 H 0.3276 0.6238 0.8631 0.030 Uiso 1 1 calc R . . O8 O 0.5638(2) 0.59567(6) 0.41667(11) 0.0195(3) Uani 1 1 d . . . C8 C -0.0049(4) 0.74954(12) 0.9753(2) 0.0401(7) Uani 1 1 d . . . H8A H -0.0735 0.7765 0.9962 0.060 Uiso 1 1 calc R . . H8B H 0.1052 0.7649 0.9803 0.060 Uiso 1 1 calc R . . H8C H 0.0082 0.7176 1.0176 0.060 Uiso 1 1 calc R . . O9 O 0.4746(2) 0.81204(6) 0.62995(13) 0.0300(4) Uani 1 1 d . . . C9 C 0.6672(3) 0.47488(8) 0.76280(15) 0.0155(4) Uani 1 1 d . . . O10 O 0.16490(19) 0.44196(6) 0.65195(12) 0.0196(3) Uani 1 1 d . . . C10 C 0.8322(3) 0.46474(9) 0.83492(15) 0.0167(4) Uani 1 1 d . . . O11 O 0.18887(18) 0.47981(7) 0.45592(11) 0.0185(3) Uani 1 1 d . . . C11 C 0.8462(3) 0.43302(9) 0.91800(16) 0.0221(5) Uani 1 1 d . B . H11 H 0.7487 0.4181 0.9293 0.026 Uiso 1 1 calc R . . C12 C 1.0008(3) 0.42327(11) 0.98383(18) 0.0298(6) Uani 1 1 d . . . H12 H 1.0092 0.4018 1.0403 0.036 Uiso 1 1 calc R B . C13 C 1.1437(3) 0.44477(11) 0.96775(18) 0.0313(6) Uani 1 1 d . B . C14 C 1.1311(3) 0.47637(12) 0.88484(18) 0.0296(5) Uani 1 1 d . . . H14 H 1.2287 0.4911 0.8734 0.035 Uiso 1 1 calc R B . C15 C 0.9766(3) 0.48612(10) 0.81977(16) 0.0222(5) Uani 1 1 d . B . H15 H 0.9684 0.5078 0.7636 0.027 Uiso 1 1 calc R . . C16A C 1.2981(5) 0.39836(18) 1.1189(3) 0.0269(12) Uani 0.511(6) 1 d P B 1 H16D H 1.4134 0.3939 1.1604 0.040 Uiso 0.511(6) 1 calc PR B 1 H16E H 1.2516 0.3630 1.0946 0.040 Uiso 0.511(6) 1 calc PR B 1 H16F H 1.2307 0.4147 1.1574 0.040 Uiso 0.511(6) 1 calc PR B 1 H2O H 0.0867 0.4673 0.4390 0.038(8) Uiso 1 1 d R . . H1O H 0.2113 0.4883 0.4017 0.038(8) Uiso 1 1 d R . . S1 S 0.1211(5) 0.37882(18) 0.6507(3) 0.019(4) Uani 0.047(3) 1 d PR A 2 C28 C 0.1591(5) 0.35982(18) 0.7794(3) 0.055(19) Uani 0.047(3) 1 d PRU A 2 H28A H 0.2797 0.3572 0.8109 0.083 Uiso 0.047(3) 1 calc PR A 2 H28B H 0.1067 0.3248 0.7833 0.083 Uiso 0.047(3) 1 calc PR A 2 H28C H 0.1113 0.3873 0.8129 0.083 Uiso 0.047(3) 1 calc PR A 2 C16B C 1.4478(6) 0.4664(2) 1.0191(4) 0.0268(13) Uani 0.489(6) 1 d P . 2 H16A H 1.5490 0.4554 1.0700 0.040 Uiso 0.489(6) 1 calc PR B 2 H16B H 1.4297 0.5052 1.0247 0.040 Uiso 0.489(6) 1 calc PR B 2 H16C H 1.4609 0.4585 0.9544 0.040 Uiso 0.489(6) 1 calc PR B 2 C17 C 0.5072(2) 0.60054(8) 0.48900(15) 0.0149(4) Uani 1 1 d . . . C18 C 0.5034(3) 0.65590(8) 0.53057(16) 0.0155(4) Uani 1 1 d . . . C19 C 0.4435(3) 0.66418(9) 0.61044(18) 0.0226(5) Uani 1 1 d . . . H19 H 0.4088 0.6341 0.6410 0.027 Uiso 1 1 calc R . . C20 C 0.4332(3) 0.71577(9) 0.64683(18) 0.0242(5) Uani 1 1 d . . . H20 H 0.3923 0.7208 0.7018 0.029 Uiso 1 1 calc R . . C21 C 0.4831(3) 0.75966(9) 0.60218(17) 0.0216(5) Uani 1 1 d . . . C22 C 0.5478(3) 0.75188(9) 0.52336(18) 0.0258(5) Uani 1 1 d . . . H22 H 0.5850 0.7819 0.4939 0.031 Uiso 1 1 calc R . . C23 C 0.5577(3) 0.70031(9) 0.48809(17) 0.0214(5) Uani 1 1 d . . . H23 H 0.6019 0.6951 0.4344 0.026 Uiso 1 1 calc R . . C24 C 0.4174(4) 0.82124(11) 0.7138(2) 0.0385(7) Uani 1 1 d . . . H24A H 0.4169 0.8601 0.7266 0.058 Uiso 1 1 calc R . . H24B H 0.4920 0.8030 0.7708 0.058 Uiso 1 1 calc R . . H24C H 0.3039 0.8069 0.7014 0.058 Uiso 1 1 calc R . . C25 C 0.1794(3) 0.40436(10) 0.71080(18) 0.0200(5) Uani 0.953(3) 1 d P A 1 H25 H 0.2841 0.3996 0.7588 0.024 Uiso 0.953(3) 1 calc PR A 1 C26 C 0.0754(4) 0.33203(11) 0.7899(2) 0.0310(6) Uani 0.953(3) 1 d P A 1 H26A H 0.1930 0.3300 0.8288 0.047 Uiso 0.953(3) 1 calc PR A 1 H26B H 0.0377 0.2964 0.7626 0.047 Uiso 0.953(3) 1 calc PR A 1 H26C H 0.0076 0.3438 0.8320 0.047 Uiso 0.953(3) 1 calc PR A 1 C27 C -0.1062(4) 0.37653(14) 0.6395(3) 0.0273(7) Uani 0.953(3) 1 d P A 1 H27A H -0.1808 0.3958 0.6699 0.041 Uiso 0.953(3) 1 calc PR A 1 H27B H -0.1528 0.3408 0.6180 0.041 Uiso 0.953(3) 1 calc PR A 1 H27C H -0.0953 0.3970 0.5829 0.041 Uiso 0.953(3) 1 calc PR A 1 C29 C -0.098(8) 0.376(3) 0.609(4) 0.009(13) Uani 0.047(3) 1 d PU A 2 H29A H -0.1363 0.3848 0.5393 0.014 Uiso 0.047(3) 1 calc PR A 2 H29B H -0.1452 0.4017 0.6461 0.014 Uiso 0.047(3) 1 calc PR A 2 H29C H -0.1353 0.3393 0.6192 0.014 Uiso 0.047(3) 1 calc PR A 2 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 0.01048(6) 0.01380(5) 0.01225(5) -0.00009(3) 0.00245(4) -0.00064(3) O1 0.0122(7) 0.0207(7) 0.0175(8) -0.0037(6) 0.0014(6) -0.0005(6) N1 0.0180(11) 0.0205(10) 0.0245(11) 0.0024(8) 0.0070(9) -0.0020(8) C1 0.0131(10) 0.0165(10) 0.0175(10) 0.0019(8) 0.0050(9) -0.0005(8) O2 0.0151(8) 0.0253(8) 0.0165(8) -0.0023(6) 0.0013(6) 0.0042(6) C2 0.0138(11) 0.0173(10) 0.0204(11) -0.0012(8) 0.0049(9) 0.0002(8) O3 0.0317(11) 0.0390(10) 0.0398(11) -0.0176(9) 0.0079(9) 0.0098(8) C3 0.0212(12) 0.0240(11) 0.0255(12) -0.0063(9) -0.0011(10) 0.0042(9) O4 0.0137(8) 0.0201(7) 0.0165(7) 0.0025(6) 0.0041(6) -0.0006(6) C4 0.0205(13) 0.0323(13) 0.0375(15) -0.0092(11) -0.0007(11) 0.0102(10) O5 0.0128(7) 0.0249(8) 0.0141(7) 0.0018(6) 0.0027(6) -0.0016(6) C5 0.0248(13) 0.0225(11) 0.0311(13) -0.0064(10) 0.0106(11) 0.0031(9) O6 0.0182(9) 0.0495(11) 0.0229(9) 0.0026(8) -0.0036(7) 0.0065(8) C6 0.0239(13) 0.0354(13) 0.0209(12) -0.0087(10) 0.0035(10) 0.0028(10) O7 0.0172(8) 0.0146(7) 0.0195(8) 0.0011(6) 0.0013(7) -0.0024(6) C7 0.0189(12) 0.0335(13) 0.0206(12) -0.0047(10) 0.0008(10) 0.0066(10) O8 0.0227(8) 0.0168(7) 0.0196(8) -0.0023(6) 0.0070(7) 0.0008(6) C8 0.0458(18) 0.0408(16) 0.0377(15) -0.0170(13) 0.0186(14) 0.0063(13) O9 0.0396(11) 0.0153(8) 0.0346(10) -0.0060(7) 0.0101(9) 0.0026(7) C9 0.0173(11) 0.0157(9) 0.0136(10) -0.0022(8) 0.0048(9) 0.0009(8) O10 0.0157(8) 0.0221(8) 0.0223(8) 0.0030(6) 0.0075(7) -0.0004(6) C10 0.0141(11) 0.0215(10) 0.0122(10) -0.0008(8) 0.0001(8) 0.0036(8) O11 0.0120(8) 0.0298(8) 0.0132(7) -0.0019(6) 0.0029(6) -0.0048(6) C11 0.0226(12) 0.0243(11) 0.0178(11) 0.0017(9) 0.0034(10) 0.0025(9) C12 0.0329(15) 0.0331(13) 0.0181(12) 0.0016(10) -0.0011(11) 0.0116(11) C13 0.0213(13) 0.0446(15) 0.0201(12) -0.0108(11) -0.0067(10) 0.0136(11) C14 0.0152(12) 0.0475(15) 0.0244(12) -0.0106(11) 0.0032(10) 0.0011(10) C15 0.0166(11) 0.0351(12) 0.0136(10) -0.0028(9) 0.0020(9) 0.0011(9) C16A 0.019(2) 0.036(3) 0.020(2) 0.0052(19) -0.0037(19) 0.0011(19) S1 0.012(6) 0.014(6) 0.033(8) -0.003(5) 0.008(5) -0.002(4) C28 0.06(2) 0.05(2) 0.06(2) 0.001(5) 0.016(7) 0.000(5) C16B 0.010(2) 0.045(3) 0.022(3) 0.004(2) -0.001(2) 0.0023(19) C17 0.0107(10) 0.0144(9) 0.0166(10) 0.0006(8) -0.0010(8) 0.0012(7) C18 0.0119(10) 0.0147(9) 0.0178(10) -0.0005(8) 0.0010(9) -0.0006(7) C19 0.0247(12) 0.0181(10) 0.0283(12) -0.0018(9) 0.0129(10) -0.0043(9) C20 0.0266(13) 0.0229(11) 0.0265(12) -0.0063(9) 0.0130(11) -0.0021(9) C21 0.0195(12) 0.0156(10) 0.0259(12) -0.0052(9) 0.0007(10) 0.0015(8) C22 0.0375(14) 0.0141(10) 0.0266(12) 0.0000(9) 0.0106(11) -0.0042(9) C23 0.0272(12) 0.0176(10) 0.0203(11) -0.0007(8) 0.0086(10) -0.0021(9) C24 0.0524(19) 0.0248(13) 0.0407(16) -0.0156(11) 0.0174(14) 0.0016(12) C25 0.0140(12) 0.0234(12) 0.0238(13) -0.0006(10) 0.0074(10) 0.0005(9) C26 0.0334(16) 0.0262(13) 0.0354(15) 0.0096(11) 0.0130(13) -0.0020(11) C27 0.0192(15) 0.0301(15) 0.031(2) -0.0035(15) 0.0049(15) -0.0067(10) C29 0.009(14) 0.009(14) 0.008(14) 0.000(5) 0.002(6) -0.002(5) _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 O7 2.2967(15) . ? Tb1 O10 2.3285(15) . ? Tb1 O11 2.3552(15) . ? Tb1 O5 2.3717(15) . ? Tb1 O8 2.3807(15) 3_666 ? Tb1 O2 2.3919(15) . ? Tb1 O4 2.4962(15) . ? Tb1 O1 2.5259(15) . ? Tb1 C9 2.806(2) . ? Tb1 C1 2.825(2) . ? O1 C1 1.266(3) . ? N1 C25 1.318(3) . ? N1 C26 1.452(3) . ? N1 C27 1.457(4) . ? C1 O2 1.261(3) . ? C1 C2 1.493(3) . ? C2 C7 1.387(3) . ? C2 C3 1.390(3) . ? O3 C5 1.371(3) . ? O3 C8 1.425(3) . ? C3 C4 1.379(3) . ? C3 H3 0.9500 . ? O4 C9 1.258(3) . ? C4 C5 1.395(4) . ? C4 H4 0.9500 . ? O5 C9 1.283(3) . ? C5 C6 1.384(3) . ? O6 C13 1.360(3) . ? O6 C16A 1.526(5) . ? O6 C16B 1.546(5) . ? C6 C7 1.387(3) . ? C6 H6 0.9500 . ? O7 C17 1.261(3) . ? C7 H7 0.9500 . ? O8 C17 1.258(3) . ? O8 Tb1 2.3807(15) 3_666 ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C21 1.364(3) . ? O9 C24 1.428(3) . ? C9 C10 1.484(3) . ? O10 C25 1.236(3) . ? O10 S1 1.605(5) . ? C10 C15 1.391(3) . ? C10 C11 1.397(3) . ? O11 H2O 0.8747 . ? O11 H1O 0.8713 . ? C11 C12 1.381(3) . ? C11 H11 0.9500 . ? C12 C13 1.386(4) . ? C12 H12 0.9500 . ? C13 C14 1.396(4) . ? C14 C15 1.376(3) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16A H16D 0.9800 . ? C16A H16E 0.9800 . ? C16A H16F 0.9800 . ? S1 C29 1.76(7) . ? S1 C28 1.8302 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C16B H16A 0.9800 . ? C16B H16B 0.9800 . ? C16B H16C 0.9800 . ? C17 C18 1.498(3) . ? C18 C19 1.385(3) . ? C18 C23 1.393(3) . ? C19 C20 1.391(3) . ? C19 H19 0.9500 . ? C20 C21 1.383(3) . ? C20 H20 0.9500 . ? C21 C22 1.394(3) . ? C22 C23 1.384(3) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25 0.9500 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? 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 O7 Tb1 O10 152.56(5) . . ? O7 Tb1 O11 78.62(5) . . ? O10 Tb1 O11 79.91(5) . . ? O7 Tb1 O5 74.29(5) . . ? O10 Tb1 O5 133.06(5) . . ? O11 Tb1 O5 136.08(5) . . ? O7 Tb1 O8 116.37(5) . 3_666 ? O10 Tb1 O8 75.17(5) . 3_666 ? O11 Tb1 O8 78.07(5) . 3_666 ? O5 Tb1 O8 83.79(5) . 3_666 ? O7 Tb1 O2 92.17(5) . . ? O10 Tb1 O2 88.81(5) . . ? O11 Tb1 O2 130.32(5) . . ? O5 Tb1 O2 84.99(5) . . ? O8 Tb1 O2 144.88(5) 3_666 . ? O7 Tb1 O4 126.47(5) . . ? O10 Tb1 O4 79.96(5) . . ? O11 Tb1 O4 148.30(5) . . ? O5 Tb1 O4 53.70(5) . . ? O8 Tb1 O4 73.25(5) 3_666 . ? O2 Tb1 O4 73.29(5) . . ? O7 Tb1 O1 84.02(5) . . ? O10 Tb1 O1 74.77(5) . . ? O11 Tb1 O1 77.44(5) . . ? O5 Tb1 O1 131.86(5) . . ? O8 Tb1 O1 143.92(5) 3_666 . ? O2 Tb1 O1 52.97(5) . . ? O4 Tb1 O1 119.95(5) . . ? O7 Tb1 C9 100.76(6) . . ? O10 Tb1 C9 106.28(6) . . ? O11 Tb1 C9 151.35(6) . . ? O5 Tb1 C9 27.07(5) . . ? O8 Tb1 C9 76.70(6) 3_666 . ? O2 Tb1 C9 78.24(5) . . ? O4 Tb1 C9 26.64(5) . . ? O1 Tb1 C9 131.19(5) . . ? O7 Tb1 C1 88.11(6) . . ? O10 Tb1 C1 80.72(6) . . ? O11 Tb1 C1 104.04(6) . . ? O5 Tb1 C1 108.87(6) . . ? O8 Tb1 C1 155.08(6) 3_666 . ? O2 Tb1 C1 26.34(6) . . ? O4 Tb1 C1 96.56(5) . . ? O1 Tb1 C1 26.63(5) . . ? C9 Tb1 C1 104.56(6) . . ? C1 O1 Tb1 89.99(12) . . ? C25 N1 C26 120.7(2) . . ? C25 N1 C27 120.4(2) . . ? C26 N1 C27 118.2(2) . . ? O2 C1 O1 120.65(19) . . ? O2 C1 C2 118.61(19) . . ? O1 C1 C2 120.74(19) . . ? O2 C1 Tb1 57.28(10) . . ? O1 C1 Tb1 63.38(11) . . ? C2 C1 Tb1 175.88(15) . . ? C1 O2 Tb1 96.39(12) . . ? C7 C2 C3 118.5(2) . . ? C7 C2 C1 119.6(2) . . ? C3 C2 C1 121.9(2) . . ? C5 O3 C8 117.4(2) . . ? C4 C3 C2 120.8(2) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C9 O4 Tb1 90.53(12) . . ? C3 C4 C5 119.9(2) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C9 O5 Tb1 95.66(13) . . ? O3 C5 C6 124.0(2) . . ? O3 C5 C4 115.8(2) . . ? C6 C5 C4 120.1(2) . . ? C13 O6 C16A 116.3(2) . . ? C13 O6 C16B 117.9(3) . . ? C16A O6 C16B 125.4(3) . . ? C5 C6 C7 119.1(2) . . ? C5 C6 H6 120.5 . . ? C7 C6 H6 120.5 . . ? C17 O7 Tb1 172.91(14) . . ? C2 C7 C6 121.6(2) . . ? C2 C7 H7 119.2 . . ? C6 C7 H7 119.2 . . ? C17 O8 Tb1 114.12(13) . 3_666 ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C21 O9 C24 116.9(2) . . ? O4 C9 O5 120.1(2) . . ? O4 C9 C10 121.31(19) . . ? O5 C9 C10 118.60(19) . . ? O4 C9 Tb1 62.83(11) . . ? O5 C9 Tb1 57.27(11) . . ? C10 C9 Tb1 175.30(14) . . ? C25 O10 Tb1 130.04(15) . . ? S1 O10 Tb1 136.34(18) . . ? C15 C10 C11 118.8(2) . . ? C15 C10 C9 120.17(19) . . ? C11 C10 C9 121.0(2) . . ? Tb1 O11 H2O 128.5 . . ? Tb1 O11 H1O 124.9 . . ? H2O O11 H1O 106.5 . . ? C12 C11 C10 120.4(2) . . ? C12 C11 H11 119.8 . . ? C10 C11 H11 119.8 . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? O6 C13 C12 120.1(2) . . ? O6 C13 C14 120.0(2) . . ? C12 C13 C14 119.9(2) . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C10 121.1(2) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? O6 C16A H16D 109.5 . . ? O6 C16A H16E 109.5 . . ? H16D C16A H16E 109.5 . . ? O6 C16A H16F 109.5 . . ? H16D C16A H16F 109.5 . . ? H16E C16A H16F 109.5 . . ? O10 S1 C29 105(2) . . ? O10 S1 C28 105.45(16) . . ? C29 S1 C28 100.8(18) . . ? S1 C28 H28A 109.5 . . ? S1 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? S1 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O6 C16B C16B 151.5(5) . 3_867 ? O6 C16B H16A 109.5 . . ? C16B C16B H16A 94.6 3_867 . ? O6 C16B H16B 109.5 . . ? C16B C16B H16B 45.9 3_867 . ? H16A C16B H16B 109.5 . . ? O6 C16B H16C 109.5 . . ? C16B C16B H16C 74.7 3_867 . ? H16A C16B H16C 109.5 . . ? H16B C16B H16C 109.5 . . ? O8 C17 O7 122.79(19) . . ? O8 C17 C18 117.89(18) . . ? O7 C17 C18 119.32(18) . . ? C19 C18 C23 118.7(2) . . ? C19 C18 C17 120.97(19) . . ? C23 C18 C17 120.29(19) . . ? C18 C19 C20 121.2(2) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 119.4(2) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? O9 C21 C20 124.5(2) . . ? O9 C21 C22 115.5(2) . . ? C20 C21 C22 120.1(2) . . ? C23 C22 C21 119.9(2) . . ? C23 C22 H22 120.1 . . ? C21 C22 H22 120.1 . . ? C22 C23 C18 120.6(2) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? O9 C24 H24A 109.5 . . ? O9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O10 C25 N1 123.7(2) . . ? O10 C25 H25 118.2 . . ? N1 C25 H25 118.2 . . ? S1 C29 H29A 109.5 . . ? S1 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? S1 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H2O O1 0.87 1.86 2.728(2) 175.1 3_566 O11 H1O O5 0.87 1.88 2.705(2) 158.3 3_666 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.940 _refine_diff_density_min -0.782 _refine_diff_density_rms 0.073 # Attachment '12.CIF' data_12 _database_code_depnum_ccdc_archive 'CCDC 649819' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[Tb(4-MeOBA)3(DMSO)(H2O)]2' _chemical_melting_point ? _chemical_formula_moiety 'C52 H58 O22 S2 Tb2' _chemical_formula_sum 'C52 H58 O22 S2 Tb2' _chemical_formula_weight 1416.94 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.3013(2) _cell_length_b 24.6350(5) _cell_length_c 14.0564(3) _cell_angle_alpha 90.00 _cell_angle_beta 105.388(1) _cell_angle_gamma 90.00 _cell_volume 2771.52(11) _cell_formula_units_Z 2 _cell_measurement_temperature 123(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.698 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 2.685 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.4397 _exptl_absorpt_correction_T_max 0.6530 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(1) _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 'Bruker X8 Apex II CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23279 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0367 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 6359 _reflns_number_gt 5454 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART (Bruker)' _computing_cell_refinement 'Bruker SMART (Bruker)' _computing_data_reduction 'Bruker SAINT (Bruker)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _computing_publication_material 'CIFTAB (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 _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^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 6359 _refine_ls_number_parameters 376 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0340 _refine_ls_R_factor_gt 0.0258 _refine_ls_wR_factor_ref 0.0571 _refine_ls_wR_factor_gt 0.0532 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Tb1 Tb 0.364270(16) 0.491910(5) 0.618048(9) 0.01245(5) Uani 1 1 d . . . S1 S 0.11375(9) 0.37942(3) 0.64202(6) 0.02054(16) Uani 1 1 d . . . O1 O 0.1278(2) 0.55882(8) 0.61052(14) 0.0177(4) Uani 1 1 d . . . C1 C 0.2011(3) 0.57488(11) 0.6969(2) 0.0147(6) Uani 1 1 d . . . H1O H 0.218(5) 0.4850(14) 0.412(3) 0.028(11) Uiso 1 1 d . . . H2O H 0.088(6) 0.4689(17) 0.436(3) 0.055(13) Uiso 1 1 d . . . O2 O 0.3376(2) 0.55373(8) 0.74345(14) 0.0176(4) Uani 1 1 d . . . C2 C 0.1296(3) 0.61947(11) 0.7442(2) 0.0155(6) Uani 1 1 d . . . O3 O -0.0737(3) 0.74091(9) 0.88146(16) 0.0295(5) Uani 1 1 d . . . C3 C -0.0215(4) 0.64399(12) 0.6981(2) 0.0217(7) Uani 1 1 d . . . H3 H -0.0811 0.6327 0.6338 0.026 Uiso 1 1 calc R . . O4 O 0.5325(2) 0.45181(8) 0.77648(14) 0.0167(4) Uani 1 1 d . . . C4 C -0.0864(4) 0.68491(13) 0.7450(2) 0.0259(7) Uani 1 1 d . . . H4 H -0.1903 0.7013 0.7130 0.031 Uiso 1 1 calc R . . O5 O 0.6563(2) 0.50094(8) 0.68667(14) 0.0179(4) Uani 1 1 d . . . C5 C 0.0014(4) 0.70184(12) 0.8390(2) 0.0214(6) Uani 1 1 d . . . O6 O 1.2936(3) 0.43675(9) 1.02915(15) 0.0279(5) Uani 1 1 d . . . C6 C 0.1534(4) 0.67850(13) 0.8845(2) 0.0236(7) Uani 1 1 d . . . H6 H 0.2145 0.6904 0.9481 0.028 Uiso 1 1 calc R . . O7 O 0.4549(2) 0.56030(8) 0.53306(14) 0.0171(4) Uani 1 1 d . . . C7 C 0.2167(4) 0.63764(12) 0.8369(2) 0.0214(6) Uani 1 1 d . . . H7 H 0.3216 0.6218 0.8685 0.026 Uiso 1 1 calc R . . O8 O 0.5662(2) 0.59701(8) 0.42159(14) 0.0184(4) Uani 1 1 d . . . C8 C -0.0089(4) 0.74973(15) 0.9851(2) 0.0341(8) Uani 1 1 d . . . H8A H -0.0034 0.7151 1.0200 0.051 Uiso 1 1 calc R . . H8B H -0.0821 0.7748 1.0081 0.051 Uiso 1 1 calc R . . H8C H 0.1034 0.7654 0.9982 0.051 Uiso 1 1 calc R . . O9 O 0.4448(3) 0.81076(9) 0.63885(17) 0.0339(6) Uani 1 1 d . . . C9 C 0.6631(3) 0.47191(11) 0.76360(19) 0.0146(6) Uani 1 1 d . . . O10 O 0.1552(2) 0.43951(8) 0.65175(15) 0.0202(4) Uani 1 1 d . . . C10 C 0.8289(3) 0.46255(11) 0.8340(2) 0.0156(6) Uani 1 1 d . . . O11 O 0.1900(3) 0.48049(9) 0.45668(16) 0.0189(5) Uani 1 1 d . . . C11 C 0.8455(4) 0.42926(12) 0.9158(2) 0.0196(6) Uani 1 1 d . A . H11 H 0.7495 0.4123 0.9271 0.024 Uiso 1 1 calc R . . C12 C 1.0002(4) 0.42060(13) 0.9808(2) 0.0246(7) Uani 1 1 d . . . H12 H 1.0103 0.3977 1.0365 0.030 Uiso 1 1 calc R A . C13 C 1.1408(4) 0.44528(13) 0.9646(2) 0.0252(7) Uani 1 1 d . A . C14 C 1.1265(4) 0.47854(14) 0.8833(2) 0.0251(7) Uani 1 1 d . . . H14 H 1.2227 0.4954 0.8720 0.030 Uiso 1 1 calc R A . C15 C 0.9715(4) 0.48700(12) 0.8190(2) 0.0202(6) Uani 1 1 d . A . H15 H 0.9618 0.5099 0.7635 0.024 Uiso 1 1 calc R . . C16A C 1.3015(8) 0.4009(3) 1.1161(4) 0.0310(17) Uani 0.523(6) 1 d P A 2 H16A H 1.2142 0.4116 1.1475 0.047 Uiso 0.523(6) 1 calc PR A 2 H16B H 1.4113 0.4046 1.1635 0.047 Uiso 0.523(6) 1 calc PR A 2 H16C H 1.2843 0.3631 1.0941 0.047 Uiso 0.523(6) 1 calc PR A 2 C16B C 1.4411(8) 0.4684(3) 1.0151(5) 0.0231(16) Uani 0.477(6) 1 d P A 1 H16D H 1.4590 0.4596 0.9507 0.035 Uiso 0.477(6) 1 calc PR A 1 H16E H 1.5411 0.4589 1.0673 0.035 Uiso 0.477(6) 1 calc PR A 1 H16F H 1.4190 0.5074 1.0180 0.035 Uiso 0.477(6) 1 calc PR A 1 C17 C 0.5106(3) 0.60048(11) 0.4961(2) 0.0143(6) Uani 1 1 d . . . C18 C 0.5057(3) 0.65545(11) 0.5402(2) 0.0156(6) Uani 1 1 d . . . C19 C 0.4475(4) 0.66214(12) 0.6232(2) 0.0213(6) Uani 1 1 d . . . H19 H 0.4211 0.6310 0.6560 0.026 Uiso 1 1 calc R . . C20 C 0.4271(4) 0.71341(12) 0.6595(2) 0.0246(7) Uani 1 1 d . . . H20 H 0.3859 0.7173 0.7160 0.029 Uiso 1 1 calc R . . C21 C 0.4673(4) 0.75841(12) 0.6126(2) 0.0225(7) Uani 1 1 d . . . C22 C 0.5345(4) 0.75272(12) 0.5323(2) 0.0249(7) Uani 1 1 d . . . H22 H 0.5673 0.7839 0.5022 0.030 Uiso 1 1 calc R . . C23 C 0.5531(4) 0.70175(12) 0.4969(2) 0.0196(6) Uani 1 1 d . . . H23 H 0.5988 0.6979 0.4421 0.024 Uiso 1 1 calc R . . C24 C 0.3797(6) 0.81839(15) 0.7227(3) 0.0473(11) Uani 1 1 d . . . H24A H 0.2639 0.8056 0.7069 0.071 Uiso 1 1 calc R . . H24B H 0.3834 0.8570 0.7396 0.071 Uiso 1 1 calc R . . H24C H 0.4474 0.7978 0.7788 0.071 Uiso 1 1 calc R . . C25 C 0.1594(5) 0.35461(15) 0.7651(3) 0.0447(10) Uani 1 1 d . . . H25A H 0.2791 0.3587 0.7966 0.067 Uiso 1 1 calc R . . H25B H 0.1288 0.3162 0.7643 0.067 Uiso 1 1 calc R . . H25C H 0.0954 0.3753 0.8022 0.067 Uiso 1 1 calc R . . C26 C -0.1067(4) 0.37773(13) 0.6151(2) 0.0283(7) Uani 1 1 d . . . H26A H -0.1434 0.3998 0.6634 0.042 Uiso 1 1 calc R . . H26B H -0.1439 0.3402 0.6182 0.042 Uiso 1 1 calc R . . H26C H -0.1549 0.3923 0.5487 0.042 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 0.00997(7) 0.01420(7) 0.01307(7) -0.00028(5) 0.00286(5) -0.00109(5) S1 0.0157(4) 0.0199(4) 0.0273(4) -0.0033(3) 0.0080(3) -0.0031(3) O1 0.0126(11) 0.0204(10) 0.0192(10) -0.0045(8) 0.0027(8) -0.0025(8) C1 0.0129(15) 0.0155(14) 0.0162(14) 0.0013(11) 0.0048(11) -0.0038(11) O2 0.0151(11) 0.0212(11) 0.0158(10) -0.0005(8) 0.0029(8) 0.0030(8) C2 0.0129(15) 0.0160(14) 0.0181(14) 0.0007(11) 0.0051(11) -0.0018(11) O3 0.0273(13) 0.0285(12) 0.0302(13) -0.0098(10) 0.0031(10) 0.0099(10) C3 0.0205(17) 0.0228(16) 0.0183(15) -0.0029(12) -0.0011(12) 0.0007(12) O4 0.0106(10) 0.0211(10) 0.0187(10) 0.0034(8) 0.0047(8) 0.0005(8) C4 0.0217(17) 0.0234(16) 0.0283(17) -0.0015(13) -0.0009(13) 0.0078(13) O5 0.0156(11) 0.0238(11) 0.0141(10) 0.0038(8) 0.0033(8) -0.0012(8) C5 0.0219(17) 0.0195(15) 0.0238(16) -0.0018(12) 0.0081(13) 0.0009(12) O6 0.0166(12) 0.0418(14) 0.0208(11) 0.0056(10) -0.0031(9) 0.0028(10) C6 0.0211(17) 0.0285(17) 0.0195(15) -0.0053(13) 0.0025(13) 0.0004(13) O7 0.0149(11) 0.0147(10) 0.0205(10) 0.0016(8) 0.0029(8) -0.0026(8) C7 0.0175(16) 0.0265(16) 0.0189(15) -0.0015(12) 0.0024(12) 0.0051(12) O8 0.0173(11) 0.0199(11) 0.0199(11) -0.0013(8) 0.0081(8) 0.0012(8) C8 0.041(2) 0.033(2) 0.0289(19) -0.0092(15) 0.0107(16) 0.0096(15) O9 0.0470(16) 0.0175(11) 0.0341(13) -0.0053(10) 0.0055(11) 0.0050(10) C9 0.0150(15) 0.0166(13) 0.0121(13) -0.0025(10) 0.0035(11) 0.0017(11) O10 0.0163(11) 0.0202(11) 0.0269(11) -0.0025(8) 0.0107(9) -0.0052(8) C10 0.0128(15) 0.0187(15) 0.0145(13) -0.0019(11) 0.0024(11) 0.0006(11) O11 0.0107(11) 0.0318(13) 0.0141(11) -0.0020(9) 0.0030(9) -0.0045(9) C11 0.0177(16) 0.0229(16) 0.0181(15) 0.0028(12) 0.0045(12) 0.0017(12) C12 0.0290(19) 0.0269(17) 0.0160(15) 0.0017(12) 0.0026(13) 0.0064(13) C13 0.0212(17) 0.0334(18) 0.0164(15) -0.0048(13) -0.0029(13) 0.0113(14) C14 0.0150(16) 0.0377(19) 0.0213(15) -0.0022(14) 0.0026(12) 0.0005(13) C15 0.0183(16) 0.0265(16) 0.0144(14) 0.0000(12) 0.0019(12) -0.0029(12) C16A 0.024(4) 0.044(4) 0.019(3) 0.006(3) -0.006(3) 0.004(3) C16B 0.013(3) 0.033(4) 0.022(3) 0.003(3) 0.001(3) -0.003(3) C17 0.0078(14) 0.0146(14) 0.0178(14) -0.0004(10) -0.0013(11) 0.0017(10) C18 0.0099(14) 0.0173(14) 0.0183(14) -0.0006(11) 0.0013(11) -0.0002(11) C19 0.0212(17) 0.0187(15) 0.0244(16) -0.0027(12) 0.0069(13) -0.0047(12) C20 0.0267(18) 0.0227(16) 0.0252(16) -0.0031(13) 0.0086(14) 0.0027(13) C21 0.0229(17) 0.0147(14) 0.0242(16) -0.0052(12) -0.0039(13) -0.0002(12) C22 0.0277(18) 0.0153(15) 0.0294(17) 0.0036(12) 0.0034(14) -0.0031(13) C23 0.0203(16) 0.0179(15) 0.0193(15) -0.0010(11) 0.0029(12) -0.0012(12) C24 0.087(3) 0.0252(19) 0.030(2) -0.0094(15) 0.016(2) 0.012(2) C25 0.058(3) 0.029(2) 0.035(2) 0.0076(16) -0.0100(19) 0.0014(18) C26 0.0150(17) 0.0276(17) 0.0396(19) -0.0007(14) 0.0025(14) -0.0059(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 O7 2.3039(19) . ? Tb1 O10 2.3105(19) . ? Tb1 O11 2.361(2) . ? Tb1 O8 2.3692(19) 3_666 ? Tb1 O5 2.370(2) . ? Tb1 O2 2.3838(19) . ? Tb1 O4 2.4969(19) . ? Tb1 O1 2.5442(19) . ? Tb1 C9 2.809(3) . ? Tb1 C1 2.835(3) . ? S1 O10 1.518(2) . ? S1 C26 1.768(3) . ? S1 C25 1.778(4) . ? O1 C1 1.269(3) . ? C1 O2 1.261(3) . ? C1 C2 1.487(4) . ? C2 C7 1.386(4) . ? C2 C3 1.387(4) . ? O3 C5 1.367(4) . ? O3 C8 1.429(4) . ? C3 C4 1.389(4) . ? C3 H3 0.9500 . ? O4 C9 1.248(3) . ? C4 C5 1.393(4) . ? C4 H4 0.9500 . ? O5 C9 1.285(3) . ? C5 C6 1.380(4) . ? O6 C13 1.366(4) . ? O6 C16A 1.494(6) . ? O6 C16B 1.509(6) . ? C6 C7 1.386(4) . ? C6 H6 0.9500 . ? O7 C17 1.262(3) . ? C7 H7 0.9500 . ? O8 C17 1.254(3) . ? O8 Tb1 2.3692(19) 3_666 ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? O9 C21 1.367(3) . ? O9 C24 1.432(4) . ? C9 C10 1.484(4) . ? C10 C11 1.389(4) . ? C10 C15 1.393(4) . ? O11 H1O 0.74(4) . ? O11 H2O 0.87(4) . ? C11 C12 1.381(4) . ? C11 H11 0.9500 . ? C12 C13 1.387(5) . ? C12 H12 0.9500 . ? C13 C14 1.385(4) . ? C14 C15 1.378(4) . ? C14 H14 0.9500 . ? C15 H15 0.9500 . ? C16A H16A 0.9800 . ? C16A H16B 0.9800 . ? C16A H16C 0.9800 . ? C16B H16D 0.9800 . ? C16B H16E 0.9800 . ? C16B H16F 0.9800 . ? C17 C18 1.494(4) . ? C18 C19 1.387(4) . ? C18 C23 1.397(4) . ? C19 C20 1.389(4) . ? C19 H19 0.9500 . ? C20 C21 1.375(4) . ? C20 H20 0.9500 . ? C21 C22 1.393(4) . ? C22 C23 1.374(4) . ? C22 H22 0.9500 . ? C23 H23 0.9500 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? 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 O7 Tb1 O10 151.78(7) . . ? O7 Tb1 O11 77.88(7) . . ? O10 Tb1 O11 80.12(8) . . ? O7 Tb1 O8 114.88(7) . 3_666 ? O10 Tb1 O8 76.99(7) . 3_666 ? O11 Tb1 O8 77.84(7) . 3_666 ? O7 Tb1 O5 72.72(7) . . ? O10 Tb1 O5 135.39(7) . . ? O11 Tb1 O5 134.58(7) . . ? O8 Tb1 O5 84.01(7) 3_666 . ? O7 Tb1 O2 91.34(7) . . ? O10 Tb1 O2 89.04(7) . . ? O11 Tb1 O2 129.28(7) . . ? O8 Tb1 O2 147.23(6) 3_666 . ? O5 Tb1 O2 85.68(7) . . ? O7 Tb1 O4 124.72(6) . . ? O10 Tb1 O4 82.46(7) . . ? O11 Tb1 O4 149.85(7) . . ? O8 Tb1 O4 74.36(6) 3_666 . ? O5 Tb1 O4 53.46(6) . . ? O2 Tb1 O4 74.50(6) . . ? O7 Tb1 O1 81.90(7) . . ? O10 Tb1 O1 75.95(7) . . ? O11 Tb1 O1 76.59(7) . . ? O8 Tb1 O1 145.37(6) 3_666 . ? O5 Tb1 O1 130.61(6) . . ? O2 Tb1 O1 52.76(6) . . ? O4 Tb1 O1 122.42(6) . . ? O7 Tb1 C9 99.16(8) . . ? O10 Tb1 C9 108.59(8) . . ? O11 Tb1 C9 151.21(8) . . ? O8 Tb1 C9 77.63(7) 3_666 . ? O5 Tb1 C9 27.08(7) . . ? O2 Tb1 C9 79.09(7) . . ? O4 Tb1 C9 26.38(7) . . ? O1 Tb1 C9 131.80(7) . . ? O7 Tb1 C1 86.05(7) . . ? O10 Tb1 C1 81.94(7) . . ? O11 Tb1 C1 103.13(8) . . ? O8 Tb1 C1 158.44(7) 3_666 . ? O5 Tb1 C1 108.45(7) . . ? O2 Tb1 C1 26.17(7) . . ? O4 Tb1 C1 98.53(7) . . ? O1 Tb1 C1 26.59(7) . . ? C9 Tb1 C1 105.23(8) . . ? O10 S1 C26 103.86(14) . . ? O10 S1 C25 105.24(15) . . ? C26 S1 C25 98.12(18) . . ? C1 O1 Tb1 89.60(16) . . ? O2 C1 O1 120.3(3) . . ? O2 C1 C2 119.0(2) . . ? O1 C1 C2 120.7(3) . . ? O2 C1 Tb1 56.51(14) . . ? O1 C1 Tb1 63.81(14) . . ? C2 C1 Tb1 175.1(2) . . ? C1 O2 Tb1 97.32(16) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 119.2(3) . . ? C3 C2 C1 122.1(3) . . ? C5 O3 C8 117.4(2) . . ? C2 C3 C4 120.7(3) . . ? C2 C3 H3 119.6 . . ? C4 C3 H3 119.6 . . ? C9 O4 Tb1 90.88(16) . . ? C3 C4 C5 119.7(3) . . ? C3 C4 H4 120.1 . . ? C5 C4 H4 120.1 . . ? C9 O5 Tb1 95.85(16) . . ? O3 C5 C6 123.9(3) . . ? O3 C5 C4 116.1(3) . . ? C6 C5 C4 119.9(3) . . ? C13 O6 C16A 117.7(3) . . ? C13 O6 C16B 118.5(3) . . ? C16A O6 C16B 123.5(4) . . ? C5 C6 C7 119.8(3) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C17 O7 Tb1 173.34(18) . . ? C2 C7 C6 121.2(3) . . ? C2 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C17 O8 Tb1 115.21(17) . 3_666 ? O3 C8 H8A 109.5 . . ? O3 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? O3 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C21 O9 C24 117.0(3) . . ? O4 C9 O5 119.8(2) . . ? O4 C9 C10 122.0(2) . . ? O5 C9 C10 118.2(2) . . ? O4 C9 Tb1 62.74(14) . . ? O5 C9 Tb1 57.07(14) . . ? C10 C9 Tb1 175.0(2) . . ? S1 O10 Tb1 133.73(12) . . ? C11 C10 C15 118.6(3) . . ? C11 C10 C9 120.9(3) . . ? C15 C10 C9 120.5(3) . . ? Tb1 O11 H1O 124(3) . . ? Tb1 O11 H2O 131(3) . . ? H1O O11 H2O 105(4) . . ? C12 C11 C10 120.6(3) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C11 C12 C13 119.9(3) . . ? C11 C12 H12 120.0 . . ? C13 C12 H12 120.0 . . ? O6 C13 C14 120.0(3) . . ? O6 C13 C12 119.8(3) . . ? C14 C13 C12 120.2(3) . . ? C15 C14 C13 119.4(3) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C14 C15 C10 121.2(3) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O6 C16A H16A 109.5 . . ? O6 C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? O6 C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O6 C16B H16D 109.5 . . ? O6 C16B H16E 109.5 . . ? O6 C16B H16F 109.5 . . ? O8 C17 O7 123.2(3) . . ? O8 C17 C18 117.7(2) . . ? O7 C17 C18 119.1(2) . . ? C19 C18 C23 118.1(3) . . ? C19 C18 C17 120.7(3) . . ? C23 C18 C17 121.1(3) . . ? C18 C19 C20 121.4(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 119.3(3) . . ? C21 C20 H20 120.4 . . ? C19 C20 H20 120.4 . . ? O9 C21 C20 124.3(3) . . ? O9 C21 C22 115.2(3) . . ? C20 C21 C22 120.5(3) . . ? C23 C22 C21 119.6(3) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C18 121.1(3) . . ? C22 C23 H23 119.5 . . ? C18 C23 H23 119.5 . . ? O9 C24 H24A 109.5 . . ? O9 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O9 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? S1 C25 H25A 109.5 . . ? S1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? S1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? S1 C26 H26A 109.5 . . ? S1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? S1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O11 H1O O5 0.74(4) 1.97(4) 2.695(3) 167(4) 3_666 O11 H2O O1 0.87(4) 1.86(5) 2.733(3) 177(4) 3_566 _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.413 _refine_diff_density_min -0.630 _refine_diff_density_rms 0.100