# Supplementary Material (ESI) for CrystEngComm # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Shan Gao' _publ_contact_author_email SHANGAO67@YAHOO.COM _publ_section_title ; A series of three-dimensional lanthanide metal-organic frameworks with biphenylethene-4,4'-dicarboxylic acid: Hydrothermal syntheses, structures and luminescence ; loop_ _publ_author_name 'Gao Shan' 'Zhao-Peng Deng.' 'Li-Hua Huo.' 'Huan-Yu Wang.' 'Hui Zhao.' # Attachment 'B905736F.cif' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 716183' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 O6 Sm' _chemical_formula_sum 'C17 H11 O6 Sm' _chemical_formula_weight 461.61 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' Sm Sm -0.1638 3.4418 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.142(3) _cell_length_b 12.882(3) _cell_length_c 6.9096(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.74(3) _cell_angle_gamma 90.00 _cell_volume 1522.6(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20696 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _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 2.014 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 892 _exptl_absorpt_coefficient_mu 3.888 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.415 _exptl_absorpt_correction_T_max 0.506 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23783 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.16 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3470 _reflns_number_gt 3232 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.3646P] 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 3470 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0540 _refine_ls_wR_factor_gt 0.0518 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 Sm1 Sm 0.452018(7) 0.371296(9) 0.385562(18) 0.01454(6) Uani 1 1 d . . . O1 O 0.38657(12) 0.38628(15) 0.0863(3) 0.0233(4) Uani 1 1 d . . . O2 O 0.34904(11) 0.24555(15) -0.0838(3) 0.0254(4) Uani 1 1 d . . . O3 O -0.41498(13) 0.38259(17) 0.3151(4) 0.0387(6) Uani 1 1 d . . . O4 O -0.36678(12) 0.53205(16) 0.4379(4) 0.0327(5) Uani 1 1 d . . . O5 O 0.49152(12) 0.21115(15) 0.2196(3) 0.0252(4) Uani 1 1 d . . . O6 O 0.52874(13) 0.05074(15) 0.1874(3) 0.0293(5) Uani 1 1 d . . . C1 C 0.33432(15) 0.3264(2) 0.0081(4) 0.0189(5) Uani 1 1 d . . . C2 C 0.25056(16) 0.3522(2) 0.0340(4) 0.0201(5) Uani 1 1 d . . . C3 C 0.19216(16) 0.2818(2) -0.0279(4) 0.0250(6) Uani 1 1 d . . . H3A H 0.2053 0.2225 -0.0953 0.030 Uiso 1 1 calc R . . C4 C 0.11512(17) 0.2992(3) 0.0100(5) 0.0304(7) Uani 1 1 d . . . H4A H 0.0769 0.2517 -0.0326 0.036 Uiso 1 1 calc R . . C5 C 0.09397(17) 0.3880(2) 0.1122(5) 0.0267(6) Uani 1 1 d . . . C6 C 0.15244(18) 0.4596(2) 0.1667(5) 0.0282(6) Uani 1 1 d . . . H6A H 0.1391 0.5204 0.2290 0.034 Uiso 1 1 calc R . . C7 C 0.22981(17) 0.4420(2) 0.1301(4) 0.0246(6) Uani 1 1 d . . . H7A H 0.2679 0.4902 0.1698 0.030 Uiso 1 1 calc R . . C8 C 0.01399(18) 0.4078(3) 0.1672(5) 0.0321(7) Uani 1 1 d . . . H8A H 0.0052 0.4723 0.2222 0.039 Uiso 1 1 calc R . . C9 C -0.04767(19) 0.3444(3) 0.1477(5) 0.0341(7) Uani 1 1 d . . . H9A H -0.0402 0.2796 0.0929 0.041 Uiso 1 1 calc R . . C10 C -0.12644(18) 0.3693(2) 0.2063(5) 0.0279(7) Uani 1 1 d . . . C11 C -0.18895(18) 0.3029(3) 0.1532(5) 0.0337(7) Uani 1 1 d . . . H11A H -0.1798 0.2422 0.0853 0.040 Uiso 1 1 calc R . . C12 C -0.26465(18) 0.3265(3) 0.2006(5) 0.0317(7) Uani 1 1 d . . . H12A H -0.3056 0.2817 0.1644 0.038 Uiso 1 1 calc R . . C13 C -0.27917(16) 0.4167(2) 0.3016(4) 0.0244(6) Uani 1 1 d . . . C14 C -0.21744(17) 0.4830(2) 0.3556(5) 0.0280(6) Uani 1 1 d . . . H14A H -0.2269 0.5438 0.4228 0.034 Uiso 1 1 calc R . . C15 C -0.14220(18) 0.4590(3) 0.3100(5) 0.0310(7) Uani 1 1 d . . . H15A H -0.1014 0.5034 0.3492 0.037 Uiso 1 1 calc R . . C16 C -0.35972(16) 0.4461(2) 0.3554(5) 0.0268(6) Uani 1 1 d . . . C17 C 0.52406(19) 0.1306(2) 0.2879(5) 0.0245(6) Uani 1 1 d . . . H17A H 0.5450 0.1305 0.4155 0.029 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 Sm1 0.01158(8) 0.01152(8) 0.02080(8) -0.00153(4) 0.00311(6) -0.00077(4) O1 0.0174(10) 0.0231(10) 0.0294(11) 0.0017(8) 0.0012(9) -0.0002(8) O2 0.0198(10) 0.0231(10) 0.0333(11) -0.0054(8) 0.0022(9) 0.0067(8) O3 0.0201(11) 0.0331(12) 0.0642(17) -0.0207(11) 0.0137(12) -0.0068(9) O4 0.0203(10) 0.0268(11) 0.0524(14) -0.0154(10) 0.0140(10) -0.0031(8) O5 0.0251(10) 0.0163(9) 0.0343(11) -0.0035(8) 0.0021(9) 0.0027(8) O6 0.0358(12) 0.0191(10) 0.0324(11) -0.0050(8) -0.0033(10) 0.0079(9) C1 0.0152(13) 0.0208(13) 0.0207(13) 0.0043(10) 0.0026(11) 0.0034(10) C2 0.0157(13) 0.0224(13) 0.0221(13) 0.0000(10) 0.0008(11) 0.0030(10) C3 0.0186(13) 0.0262(14) 0.0305(15) -0.0062(12) 0.0046(12) 0.0018(11) C4 0.0179(14) 0.0355(17) 0.0375(17) -0.0063(13) 0.0011(13) -0.0024(12) C5 0.0167(14) 0.0365(16) 0.0274(15) 0.0009(12) 0.0051(12) 0.0062(12) C6 0.0249(15) 0.0288(15) 0.0311(16) -0.0052(12) 0.0026(13) 0.0084(12) C7 0.0184(13) 0.0257(14) 0.0298(15) -0.0026(11) 0.0018(12) 0.0019(11) C8 0.0220(15) 0.0404(18) 0.0345(17) 0.0000(14) 0.0058(14) 0.0098(13) C9 0.0220(16) 0.0401(18) 0.0410(18) -0.0040(15) 0.0075(14) 0.0084(13) C10 0.0151(14) 0.0390(18) 0.0300(16) -0.0002(12) 0.0049(13) 0.0038(11) C11 0.0257(16) 0.0319(16) 0.0443(19) -0.0102(14) 0.0082(15) 0.0057(12) C12 0.0209(15) 0.0302(16) 0.0447(19) -0.0110(14) 0.0069(14) -0.0033(12) C13 0.0175(13) 0.0261(14) 0.0303(15) -0.0038(11) 0.0059(12) -0.0004(11) C14 0.0198(14) 0.0301(15) 0.0344(16) -0.0100(12) 0.0046(13) -0.0016(11) C15 0.0171(14) 0.0394(18) 0.0369(17) -0.0079(14) 0.0041(13) -0.0046(12) C16 0.0151(13) 0.0273(15) 0.0392(17) -0.0087(12) 0.0100(13) -0.0011(11) C17 0.0238(15) 0.0222(14) 0.0274(15) -0.0023(11) 0.0001(13) 0.0026(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sm1 O1 2.295(2) . ? Sm1 O4 2.325(2) 3_566 ? Sm1 O2 2.3400(19) 4_566 ? Sm1 O3 2.367(2) 1_655 ? Sm1 O6 2.393(2) 2_655 ? Sm1 O5 2.4759(19) . ? Sm1 O5 2.591(2) 4_566 ? Sm1 O6 2.594(2) 4_566 ? Sm1 C17 2.968(3) 4_566 ? O1 C1 1.276(3) . ? O2 C1 1.254(3) . ? O2 Sm1 2.3400(19) 4_565 ? O3 C16 1.269(4) . ? O3 Sm1 2.367(2) 1_455 ? O4 C16 1.255(3) . ? O4 Sm1 2.325(2) 3_566 ? O5 C17 1.255(3) . ? O5 Sm1 2.591(2) 4_565 ? O6 C17 1.247(3) . ? O6 Sm1 2.393(2) 2_645 ? O6 Sm1 2.594(2) 4_565 ? C1 C2 1.496(4) . ? C2 C7 1.391(4) . ? C2 C3 1.397(4) . ? C3 C4 1.381(4) . ? C3 H3A 0.9300 . ? C4 C5 1.404(4) . ? C4 H4A 0.9300 . ? C5 C6 1.396(4) . ? C5 C8 1.469(4) . ? C6 C7 1.385(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.335(5) . ? C8 H8A 0.9300 . ? C9 C10 1.470(4) . ? C9 H9A 0.9300 . ? C10 C15 1.396(4) . ? C10 C11 1.401(4) . ? C11 C12 1.393(4) . ? C11 H11A 0.9300 . ? C12 C13 1.386(4) . ? C12 H12A 0.9300 . ? C13 C14 1.391(4) . ? C13 C16 1.502(4) . ? C14 C15 1.382(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 Sm1 2.968(3) 4_565 ? C17 H17A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sm1 O4 98.08(8) . 3_566 ? O1 Sm1 O2 78.94(7) . 4_566 ? O4 Sm1 O2 78.08(8) 3_566 4_566 ? O1 Sm1 O3 103.32(9) . 1_655 ? O4 Sm1 O3 136.20(7) 3_566 1_655 ? O2 Sm1 O3 143.20(7) 4_566 1_655 ? O1 Sm1 O6 78.18(7) . 2_655 ? O4 Sm1 O6 72.13(8) 3_566 2_655 ? O2 Sm1 O6 139.07(7) 4_566 2_655 ? O3 Sm1 O6 75.49(8) 1_655 2_655 ? O1 Sm1 O5 77.60(7) . . ? O4 Sm1 O5 152.80(7) 3_566 . ? O2 Sm1 O5 74.72(7) 4_566 . ? O3 Sm1 O5 70.11(7) 1_655 . ? O6 Sm1 O5 131.43(7) 2_655 . ? O1 Sm1 O5 157.09(7) . 4_566 ? O4 Sm1 O5 83.61(8) 3_566 4_566 ? O2 Sm1 O5 79.09(7) 4_566 4_566 ? O3 Sm1 O5 90.52(9) 1_655 4_566 ? O6 Sm1 O5 123.50(7) 2_655 4_566 ? O5 Sm1 O5 90.43(4) . 4_566 ? O1 Sm1 O6 152.13(6) . 4_566 ? O4 Sm1 O6 70.97(8) 3_566 4_566 ? O2 Sm1 O6 121.49(7) 4_566 4_566 ? O3 Sm1 O6 72.35(8) 1_655 4_566 ? O6 Sm1 O6 74.08(8) 2_655 4_566 ? O5 Sm1 O6 123.73(7) . 4_566 ? O5 Sm1 O6 49.69(6) 4_566 4_566 ? O1 Sm1 C17 173.55(8) . 4_566 ? O4 Sm1 C17 75.54(9) 3_566 4_566 ? O2 Sm1 C17 100.39(8) 4_566 4_566 ? O3 Sm1 C17 81.12(9) 1_655 4_566 ? O6 Sm1 C17 98.67(7) 2_655 4_566 ? O5 Sm1 C17 108.49(7) . 4_566 ? O5 Sm1 C17 24.93(7) 4_566 4_566 ? O6 Sm1 C17 24.77(7) 4_566 4_566 ? O1 Sm1 Sm1 116.91(5) . 3_666 ? O4 Sm1 Sm1 66.62(5) 3_566 3_666 ? O2 Sm1 Sm1 142.58(5) 4_566 3_666 ? O3 Sm1 Sm1 69.64(5) 1_655 3_666 ? O6 Sm1 Sm1 38.78(5) 2_655 3_666 ? O5 Sm1 Sm1 139.40(5) . 3_666 ? O5 Sm1 Sm1 84.86(5) 4_566 3_666 ? O6 Sm1 Sm1 35.30(4) 4_566 3_666 ? C17 Sm1 Sm1 59.94(5) 4_566 3_666 ? C1 O1 Sm1 128.28(18) . . ? C1 O2 Sm1 139.28(18) . 4_565 ? C16 O3 Sm1 135.23(19) . 1_455 ? C16 O4 Sm1 142.49(19) . 3_566 ? C17 O5 Sm1 129.99(19) . . ? C17 O5 Sm1 94.60(17) . 4_565 ? Sm1 O5 Sm1 133.69(9) . 4_565 ? C17 O6 Sm1 158.3(2) . 2_645 ? C17 O6 Sm1 94.63(18) . 4_565 ? Sm1 O6 Sm1 105.92(8) 2_645 4_565 ? O2 C1 O1 123.9(2) . . ? O2 C1 C2 118.2(2) . . ? O1 C1 C2 117.9(2) . . ? C7 C2 C3 119.0(3) . . ? C7 C2 C1 121.3(3) . . ? C3 C2 C1 119.5(2) . . ? C4 C3 C2 120.7(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 118.0(3) . . ? C6 C5 C8 118.8(3) . . ? C4 C5 C8 123.2(3) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C2 120.1(3) . . ? C6 C7 H7A 120.0 . . ? C2 C7 H7A 120.0 . . ? C9 C8 C5 127.8(3) . . ? C9 C8 H8A 116.1 . . ? C5 C8 H8A 116.1 . . ? C8 C9 C10 125.1(3) . . ? C8 C9 H9A 117.5 . . ? C10 C9 H9A 117.5 . . ? C15 C10 C11 118.0(3) . . ? C15 C10 C9 122.2(3) . . ? C11 C10 C9 119.7(3) . . ? C12 C11 C10 120.9(3) . . ? C12 C11 H11A 119.6 . . ? C10 C11 H11A 119.6 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.4(3) . . ? C12 C13 C16 122.3(3) . . ? C14 C13 C16 118.3(3) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C10 121.1(3) . . ? C14 C15 H15A 119.4 . . ? C10 C15 H15A 119.4 . . ? O4 C16 O3 125.2(3) . . ? O4 C16 C13 116.9(3) . . ? O3 C16 C13 117.9(3) . . ? O6 C17 O5 121.0(3) . . ? O6 C17 Sm1 60.61(16) . 4_565 ? O5 C17 Sm1 60.47(16) . 4_565 ? O6 C17 H17A 119.5 . . ? O5 C17 H17A 119.5 . . ? Sm1 C17 H17A 178.0 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Sm1 O1 C1 -90.8(2) 3_566 . . . ? O2 Sm1 O1 C1 -14.7(2) 4_566 . . . ? O3 Sm1 O1 C1 127.6(2) 1_655 . . . ? O6 Sm1 O1 C1 -160.6(2) 2_655 . . . ? O5 Sm1 O1 C1 61.8(2) . . . . ? O5 Sm1 O1 C1 1.9(3) 4_566 . . . ? O6 Sm1 O1 C1 -155.0(2) 4_566 . . . ? Sm1 Sm1 O1 C1 -158.7(2) 3_666 . . . ? O1 Sm1 O5 C17 -165.8(3) . . . . ? O4 Sm1 O5 C17 -82.2(3) 3_566 . . . ? O2 Sm1 O5 C17 -84.0(3) 4_566 . . . ? O3 Sm1 O5 C17 84.9(3) 1_655 . . . ? O6 Sm1 O5 C17 132.5(2) 2_655 . . . ? O5 Sm1 O5 C17 -5.5(3) 4_566 . . . ? O6 Sm1 O5 C17 33.9(3) 4_566 . . . ? C17 Sm1 O5 C17 12.0(2) 4_566 . . . ? Sm1 Sm1 O5 C17 77.1(3) 3_666 . . . ? O1 Sm1 O5 Sm1 -4.68(11) . . . 4_565 ? O4 Sm1 O5 Sm1 78.8(2) 3_566 . . 4_565 ? O2 Sm1 O5 Sm1 77.06(12) 4_566 . . 4_565 ? O3 Sm1 O5 Sm1 -113.98(14) 1_655 . . 4_565 ? O6 Sm1 O5 Sm1 -66.40(15) 2_655 . . 4_565 ? O5 Sm1 O5 Sm1 155.62(9) 4_566 . . 4_565 ? O6 Sm1 O5 Sm1 -164.99(10) 4_566 . . 4_565 ? C17 Sm1 O5 Sm1 173.13(11) 4_566 . . 4_565 ? Sm1 Sm1 O5 Sm1 -121.79(9) 3_666 . . 4_565 ? Sm1 O2 C1 O1 20.0(5) 4_565 . . . ? Sm1 O2 C1 C2 -157.7(2) 4_565 . . . ? Sm1 O1 C1 O2 -84.5(3) . . . . ? Sm1 O1 C1 C2 93.1(3) . . . . ? O2 C1 C2 C7 -178.4(3) . . . . ? O1 C1 C2 C7 3.8(4) . . . . ? O2 C1 C2 C3 5.9(4) . . . . ? O1 C1 C2 C3 -171.9(3) . . . . ? C7 C2 C3 C4 -1.7(5) . . . . ? C1 C2 C3 C4 174.1(3) . . . . ? C2 C3 C4 C5 -0.3(5) . . . . ? C3 C4 C5 C6 2.6(5) . . . . ? C3 C4 C5 C8 -176.2(3) . . . . ? C4 C5 C6 C7 -3.1(5) . . . . ? C8 C5 C6 C7 175.8(3) . . . . ? C5 C6 C7 C2 1.1(5) . . . . ? C3 C2 C7 C6 1.3(4) . . . . ? C1 C2 C7 C6 -174.4(3) . . . . ? C6 C5 C8 C9 -172.1(3) . . . . ? C4 C5 C8 C9 6.7(6) . . . . ? C5 C8 C9 C10 179.9(3) . . . . ? C8 C9 C10 C15 -7.6(6) . . . . ? C8 C9 C10 C11 170.7(3) . . . . ? C15 C10 C11 C12 0.8(5) . . . . ? C9 C10 C11 C12 -177.6(3) . . . . ? C10 C11 C12 C13 0.0(5) . . . . ? C11 C12 C13 C14 -0.2(5) . . . . ? C11 C12 C13 C16 179.7(3) . . . . ? C12 C13 C14 C15 -0.3(5) . . . . ? C16 C13 C14 C15 179.7(3) . . . . ? C13 C14 C15 C10 1.2(5) . . . . ? C11 C10 C15 C14 -1.4(5) . . . . ? C9 C10 C15 C14 177.0(3) . . . . ? Sm1 O4 C16 O3 14.3(6) 3_566 . . . ? Sm1 O4 C16 C13 -165.4(2) 3_566 . . . ? Sm1 O3 C16 O4 -7.5(6) 1_455 . . . ? Sm1 O3 C16 C13 172.3(2) 1_455 . . . ? C12 C13 C16 O4 -176.4(3) . . . . ? C14 C13 C16 O4 3.6(5) . . . . ? C12 C13 C16 O3 3.8(5) . . . . ? C14 C13 C16 O3 -176.2(3) . . . . ? Sm1 O6 C17 O5 -163.5(4) 2_645 . . . ? Sm1 O6 C17 O5 -2.2(3) 4_565 . . . ? Sm1 O6 C17 Sm1 -161.3(6) 2_645 . . 4_565 ? Sm1 O5 C17 O6 168.6(2) . . . . ? Sm1 O5 C17 O6 2.2(3) 4_565 . . . ? Sm1 O5 C17 Sm1 166.4(2) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.220 _refine_diff_density_min -1.001 _refine_diff_density_rms 0.107 #===END data_complex2 _database_code_depnum_ccdc_archive 'CCDC 716184' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Eu O6' _chemical_formula_sum 'C17 H11 Eu O6' _chemical_formula_weight 463.22 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.138(3) _cell_length_b 12.861(3) _cell_length_c 6.8991(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.74(3) _cell_angle_gamma 90.00 _cell_volume 1517.4(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12980 _cell_measurement_theta_min 3.17 _cell_measurement_theta_max 27.42 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.028 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 4.164 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.449 _exptl_absorpt_correction_T_max 0.655 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14669 _diffrn_reflns_av_R_equivalents 0.0537 _diffrn_reflns_av_sigmaI/netI 0.0457 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3462 _reflns_number_gt 3235 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.0186P)^2^+1.0339P] 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 3462 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0252 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0553 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.009 _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 Eu1 Eu 1.047827(7) 0.871289(8) 0.614273(16) 0.01372(6) Uani 1 1 d . . . O1 O 1.00875(11) 0.78885(12) 0.2807(3) 0.0226(4) Uani 1 1 d . . . O2 O 0.97112(12) 0.94964(13) 0.3123(3) 0.0266(4) Uani 1 1 d . . . O3 O 0.91502(13) 0.88237(14) 0.6848(4) 0.0355(5) Uani 1 1 d . . . O4 O 0.86690(11) 1.03241(14) 0.5619(3) 0.0298(4) Uani 1 1 d . . . O5 O 0.15071(10) 0.74548(13) 1.0836(3) 0.0229(4) Uani 1 1 d . . . O6 O 0.11330(12) 0.88630(13) 0.9141(3) 0.0209(4) Uani 1 1 d . . . C1 C 0.85966(16) 0.9459(2) 0.6442(4) 0.0252(6) Uani 1 1 d . . . C2 C 0.77934(15) 0.9170(2) 0.6987(4) 0.0226(5) Uani 1 1 d . . . C3 C 0.76432(17) 0.8264(2) 0.7993(4) 0.0286(6) Uani 1 1 d . . . H3A H 0.8051 0.7812 0.8351 0.034 Uiso 1 1 calc R . . C4 C 0.68899(17) 0.8028(2) 0.8466(4) 0.0306(6) Uani 1 1 d . . . H4A H 0.6799 0.7420 0.9145 0.037 Uiso 1 1 calc R . . C5 C 0.62618(18) 0.86927(19) 0.7937(5) 0.0267(6) Uani 1 1 d . . . C6 C 0.64218(17) 0.9589(2) 0.6892(4) 0.0298(6) Uani 1 1 d . . . H6A H 0.6014 1.0032 0.6491 0.036 Uiso 1 1 calc R . . C7 C 0.71711(16) 0.9831(2) 0.6445(4) 0.0263(6) Uani 1 1 d . . . H7A H 0.7264 1.0441 0.5774 0.032 Uiso 1 1 calc R . . C8 C 0.54781(17) 0.8448(2) 0.8517(5) 0.0309(6) Uani 1 1 d . . . H8A H 0.5404 0.7798 0.9068 0.037 Uiso 1 1 calc R . . C9 C 0.48601(17) 0.9079(2) 0.8322(4) 0.0295(6) Uani 1 1 d . . . H9A H 0.4946 0.9724 0.7766 0.035 Uiso 1 1 calc R . . C10 C 0.40610(17) 0.8880(2) 0.8875(4) 0.0254(6) Uani 1 1 d . . . C11 C 0.38483(16) 0.7992(2) 0.9892(4) 0.0270(6) Uani 1 1 d . . . H11A H 0.4229 0.7513 1.0310 0.032 Uiso 1 1 calc R . . C12 C 0.30800(15) 0.7822(2) 1.0281(4) 0.0231(5) Uani 1 1 d . . . H12A H 0.2951 0.7231 1.0968 0.028 Uiso 1 1 calc R . . C13 C 0.24920(15) 0.85202(19) 0.9661(4) 0.0184(5) Uani 1 1 d . . . C14 C 0.27009(16) 0.94205(19) 0.8696(4) 0.0236(5) Uani 1 1 d . . . H14A H 0.2320 0.9903 0.8293 0.028 Uiso 1 1 calc R . . C15 C 0.34760(17) 0.9596(2) 0.8337(4) 0.0262(6) Uani 1 1 d . . . H15A H 0.3610 1.0208 0.7722 0.031 Uiso 1 1 calc R . . C16 C 0.16551(15) 0.82658(18) 0.9911(4) 0.0173(5) Uani 1 1 d . . . C17 C 0.97625(18) 0.86964(16) 0.2114(4) 0.0218(6) Uani 1 1 d . . . H17A H 0.9558 0.8698 0.0832 0.026 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 Eu1 0.01326(9) 0.01071(8) 0.01728(9) 0.00130(4) 0.00160(6) 0.00068(4) O1 0.0248(10) 0.0151(8) 0.0279(10) -0.0049(7) 0.0017(8) 0.0033(7) O2 0.0333(11) 0.0162(8) 0.0294(11) -0.0024(7) -0.0045(9) 0.0063(8) O3 0.0181(11) 0.0308(11) 0.0591(16) 0.0206(9) 0.0142(10) 0.0084(8) O4 0.0205(10) 0.0262(10) 0.0437(12) 0.0150(8) 0.0109(9) 0.0039(8) O5 0.0191(9) 0.0221(8) 0.0274(10) 0.0055(7) 0.0012(8) -0.0046(7) O6 0.0179(10) 0.0207(8) 0.0240(10) -0.0009(7) -0.0006(8) -0.0001(7) C1 0.0193(13) 0.0249(13) 0.0325(15) 0.0073(11) 0.0090(11) 0.0027(11) C2 0.0167(12) 0.0264(13) 0.0251(14) 0.0044(10) 0.0054(11) -0.0011(11) C3 0.0208(14) 0.0279(14) 0.0375(17) 0.0097(12) 0.0043(12) 0.0012(12) C4 0.0234(15) 0.0302(14) 0.0388(17) 0.0103(12) 0.0067(13) -0.0044(12) C5 0.0178(15) 0.0350(16) 0.0276(16) -0.0005(10) 0.0046(12) -0.0037(10) C6 0.0195(14) 0.0375(15) 0.0325(16) 0.0074(12) 0.0034(12) 0.0036(12) C7 0.0199(13) 0.0292(13) 0.0304(15) 0.0090(11) 0.0054(11) 0.0028(11) C8 0.0211(15) 0.0373(15) 0.0350(17) 0.0020(13) 0.0073(12) -0.0078(13) C9 0.0220(15) 0.0366(15) 0.0305(16) 0.0009(12) 0.0063(12) -0.0093(13) C10 0.0189(14) 0.0345(14) 0.0231(14) -0.0025(11) 0.0035(12) -0.0065(11) C11 0.0177(13) 0.0335(14) 0.0298(15) 0.0055(11) 0.0017(11) 0.0018(11) C12 0.0195(13) 0.0248(12) 0.0249(14) 0.0063(10) 0.0019(11) -0.0012(10) C13 0.0156(13) 0.0219(11) 0.0175(13) 0.0003(9) 0.0005(10) -0.0040(10) C14 0.0223(13) 0.0237(12) 0.0247(14) 0.0030(10) 0.0008(11) -0.0028(11) C15 0.0256(14) 0.0257(13) 0.0273(15) 0.0049(10) 0.0024(11) -0.0072(11) C16 0.0170(12) 0.0176(11) 0.0172(12) -0.0038(9) 0.0005(10) -0.0018(10) C17 0.0217(14) 0.0206(13) 0.0224(14) -0.0025(9) -0.0038(12) 0.0035(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 Eu1 O6 2.296(2) 1_655 ? Eu1 O4 2.3191(19) 3_776 ? Eu1 O5 2.3362(17) 4_675 ? Eu1 O3 2.363(2) . ? Eu1 O2 2.3848(17) 3_776 ? Eu1 O1 2.4715(17) 4_576 ? Eu1 O1 2.5824(19) . ? Eu1 O2 2.594(2) . ? Eu1 C17 2.964(3) . ? Eu1 C16 3.236(3) 1_655 ? O1 C17 1.258(3) . ? O1 Eu1 2.4715(17) 4_575 ? O2 C17 1.249(3) . ? O2 Eu1 2.3848(17) 3_776 ? O3 C1 1.269(3) . ? O4 C1 1.259(3) . ? O4 Eu1 2.3191(19) 3_776 ? O5 C16 1.257(3) . ? O5 Eu1 2.3362(17) 4_476 ? O6 C16 1.269(3) . ? O6 Eu1 2.296(2) 1_455 ? C1 C2 1.497(4) . ? C2 C3 1.389(4) . ? C2 C7 1.396(4) . ? C3 C4 1.386(4) . ? C3 H3A 0.9300 . ? C4 C5 1.404(4) . ? C4 H4A 0.9300 . ? C5 C6 1.397(4) . ? C5 C8 1.461(4) . ? C6 C7 1.376(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.334(4) . ? C8 H8A 0.9300 . ? C9 C10 1.468(4) . ? C9 H9A 0.9300 . ? C10 C15 1.394(4) . ? C10 C11 1.400(4) . ? C11 C12 1.378(4) . ? C11 H11A 0.9300 . ? C12 C13 1.396(3) . ? C12 H12A 0.9300 . ? C13 C14 1.394(4) . ? C13 C16 1.492(3) . ? C14 C15 1.386(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 Eu1 3.236(3) 1_455 ? C17 H17A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O6 Eu1 O4 98.02(7) 1_655 3_776 ? O6 Eu1 O5 78.94(7) 1_655 4_675 ? O4 Eu1 O5 77.92(7) 3_776 4_675 ? O6 Eu1 O3 103.31(9) 1_655 . ? O4 Eu1 O3 136.40(6) 3_776 . ? O5 Eu1 O3 143.17(6) 4_675 . ? O6 Eu1 O2 78.04(6) 1_655 3_776 ? O4 Eu1 O2 72.23(7) 3_776 3_776 ? O5 Eu1 O2 138.94(6) 4_675 3_776 ? O3 Eu1 O2 75.62(7) . 3_776 ? O6 Eu1 O1 77.47(6) 1_655 4_576 ? O4 Eu1 O1 152.56(6) 3_776 4_576 ? O5 Eu1 O1 74.65(6) 4_675 4_576 ? O3 Eu1 O1 70.17(6) . 4_576 ? O2 Eu1 O1 131.40(7) 3_776 4_576 ? O6 Eu1 O1 157.00(6) 1_655 . ? O4 Eu1 O1 83.56(7) 3_776 . ? O5 Eu1 O1 78.97(6) 4_675 . ? O3 Eu1 O1 90.63(8) . . ? O2 Eu1 O1 123.69(6) 3_776 . ? O1 Eu1 O1 90.54(3) 4_576 . ? O6 Eu1 O2 152.04(6) 1_655 . ? O4 Eu1 O2 71.05(7) 3_776 . ? O5 Eu1 O2 121.54(6) 4_675 . ? O3 Eu1 O2 72.38(8) . . ? O2 Eu1 O2 74.13(7) 3_776 . ? O1 Eu1 O2 123.94(6) 4_576 . ? O1 Eu1 O2 49.85(6) . . ? O6 Eu1 C17 173.40(7) 1_655 . ? O4 Eu1 C17 75.45(8) 3_776 . ? O5 Eu1 C17 100.32(7) 4_675 . ? O3 Eu1 C17 81.27(9) . . ? O2 Eu1 C17 98.76(6) 3_776 . ? O1 Eu1 C17 108.75(6) 4_576 . ? O1 Eu1 C17 25.03(6) . . ? O2 Eu1 C17 24.83(6) . . ? O6 Eu1 C16 17.99(6) 1_655 1_655 ? O4 Eu1 C16 97.75(7) 3_776 1_655 ? O5 Eu1 C16 61.58(6) 4_675 1_655 ? O3 Eu1 C16 113.80(8) . 1_655 ? O2 Eu1 C16 95.01(6) 3_776 1_655 ? O1 Eu1 C16 69.66(6) 4_576 1_655 ? O1 Eu1 C16 139.01(6) . 1_655 ? O2 Eu1 C16 166.17(6) . 1_655 ? C17 Eu1 C16 161.83(7) . 1_655 ? O6 Eu1 Eu1 116.87(4) 1_655 3_776 ? O4 Eu1 Eu1 66.73(5) 3_776 3_776 ? O5 Eu1 Eu1 142.54(5) 4_675 3_776 ? O3 Eu1 Eu1 69.73(5) . 3_776 ? O2 Eu1 Eu1 38.88(5) 3_776 3_776 ? O1 Eu1 Eu1 139.57(4) 4_576 3_776 ? O1 Eu1 Eu1 84.96(4) . 3_776 ? O2 Eu1 Eu1 35.25(4) . 3_776 ? C17 Eu1 Eu1 59.95(4) . 3_776 ? C16 Eu1 Eu1 133.31(4) 1_655 3_776 ? C17 O1 Eu1 129.66(18) . 4_575 ? C17 O1 Eu1 94.72(16) . . ? Eu1 O1 Eu1 133.92(8) 4_575 . ? C17 O2 Eu1 158.39(18) . 3_776 ? C17 O2 Eu1 94.43(16) . . ? Eu1 O2 Eu1 105.87(7) 3_776 . ? C1 O3 Eu1 135.19(17) . . ? C1 O4 Eu1 142.40(18) . 3_776 ? C16 O5 Eu1 139.27(16) . 4_476 ? C16 O6 Eu1 128.04(16) . 1_455 ? O4 C1 O3 125.0(2) . . ? O4 C1 C2 116.9(2) . . ? O3 C1 C2 118.1(2) . . ? C3 C2 C7 118.8(2) . . ? C3 C2 C1 122.5(2) . . ? C7 C2 C1 118.7(2) . . ? C4 C3 C2 120.5(3) . . ? C4 C3 H3A 119.8 . . ? C2 C3 H3A 119.8 . . ? C3 C4 C5 121.0(3) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C6 C5 C4 117.7(3) . . ? C6 C5 C8 122.3(3) . . ? C4 C5 C8 120.0(3) . . ? C7 C6 C5 121.3(3) . . ? C7 C6 H6A 119.3 . . ? C5 C6 H6A 119.3 . . ? C6 C7 C2 120.7(2) . . ? C6 C7 H7A 119.6 . . ? C2 C7 H7A 119.6 . . ? C9 C8 C5 125.4(3) . . ? C9 C8 H8A 117.3 . . ? C5 C8 H8A 117.3 . . ? C8 C9 C10 128.0(3) . . ? C8 C9 H9A 116.0 . . ? C10 C9 H9A 116.0 . . ? C15 C10 C11 117.8(3) . . ? C15 C10 C9 118.8(2) . . ? C11 C10 C9 123.4(3) . . ? C12 C11 C10 120.7(3) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C13 121.2(2) . . ? C11 C12 H12A 119.4 . . ? C13 C12 H12A 119.4 . . ? C14 C13 C12 118.6(2) . . ? C14 C13 C16 121.1(2) . . ? C12 C13 C16 120.2(2) . . ? C15 C14 C13 120.0(2) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C10 121.7(2) . . ? C14 C15 H15A 119.1 . . ? C10 C15 H15A 119.1 . . ? O5 C16 O6 123.7(2) . . ? O5 C16 C13 117.9(2) . . ? O6 C16 C13 118.4(2) . . ? O5 C16 Eu1 114.79(16) . 1_455 ? C13 C16 Eu1 114.92(16) . 1_455 ? O2 C17 O1 120.9(3) . . ? O2 C17 Eu1 60.73(15) . . ? O1 C17 Eu1 60.26(15) . . ? O2 C17 H17A 119.5 . . ? O1 C17 H17A 119.5 . . ? Eu1 C17 H17A 177.7 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O6 Eu1 O1 C17 -164.52(18) 1_655 . . . ? O4 Eu1 O1 C17 -69.16(18) 3_776 . . . ? O5 Eu1 O1 C17 -148.05(18) 4_675 . . . ? O3 Eu1 O1 C17 67.52(17) . . . . ? O2 Eu1 O1 C17 -5.5(2) 3_776 . . . ? O1 Eu1 O1 C17 137.70(15) 4_576 . . . ? O2 Eu1 O1 C17 1.43(17) . . . . ? C16 Eu1 O1 C17 -163.58(16) 1_655 . . . ? Eu1 Eu1 O1 C17 -2.06(17) 3_776 . . . ? O6 Eu1 O1 Eu1 1.1(2) 1_655 . . 4_575 ? O4 Eu1 O1 Eu1 96.45(11) 3_776 . . 4_575 ? O5 Eu1 O1 Eu1 17.55(10) 4_675 . . 4_575 ? O3 Eu1 O1 Eu1 -126.87(11) . . . 4_575 ? O2 Eu1 O1 Eu1 160.06(10) 3_776 . . 4_575 ? O1 Eu1 O1 Eu1 -56.70(14) 4_576 . . 4_575 ? O2 Eu1 O1 Eu1 167.04(15) . . . 4_575 ? C17 Eu1 O1 Eu1 165.6(2) . . . 4_575 ? C16 Eu1 O1 Eu1 2.03(16) 1_655 . . 4_575 ? Eu1 Eu1 O1 Eu1 163.55(10) 3_776 . . 4_575 ? O6 Eu1 O2 C17 166.89(17) 1_655 . . . ? O4 Eu1 O2 C17 96.29(19) 3_776 . . . ? O5 Eu1 O2 C17 34.3(2) 4_675 . . . ? O3 Eu1 O2 C17 -107.88(18) . . . . ? O2 Eu1 O2 C17 172.5(2) 3_776 . . . ? O1 Eu1 O2 C17 -57.9(2) 4_576 . . . ? O1 Eu1 O2 C17 -1.44(17) . . . . ? C16 Eu1 O2 C17 133.4(3) 1_655 . . . ? Eu1 Eu1 O2 C17 172.5(2) 3_776 . . . ? O6 Eu1 O2 Eu1 -5.64(19) 1_655 . . 3_776 ? O4 Eu1 O2 Eu1 -76.24(8) 3_776 . . 3_776 ? O5 Eu1 O2 Eu1 -138.18(7) 4_675 . . 3_776 ? O3 Eu1 O2 Eu1 79.59(9) . . . 3_776 ? O2 Eu1 O2 Eu1 0.0 3_776 . . 3_776 ? O1 Eu1 O2 Eu1 129.60(7) 4_576 . . 3_776 ? O1 Eu1 O2 Eu1 -173.97(12) . . . 3_776 ? C17 Eu1 O2 Eu1 -172.5(2) . . . 3_776 ? C16 Eu1 O2 Eu1 -39.2(3) 1_655 . . 3_776 ? O6 Eu1 O3 C1 115.6(3) 1_655 . . . ? O4 Eu1 O3 C1 -1.6(4) 3_776 . . . ? O5 Eu1 O3 C1 -155.2(3) 4_675 . . . ? O2 Eu1 O3 C1 41.9(3) 3_776 . . . ? O1 Eu1 O3 C1 -173.2(3) 4_576 . . . ? O1 Eu1 O3 C1 -82.9(3) . . . . ? O2 Eu1 O3 C1 -35.7(3) . . . . ? C17 Eu1 O3 C1 -59.6(3) . . . . ? C16 Eu1 O3 C1 131.0(3) 1_655 . . . ? Eu1 Eu1 O3 C1 1.5(3) 3_776 . . . ? Eu1 O4 C1 O3 14.8(5) 3_776 . . . ? Eu1 O4 C1 C2 -165.6(2) 3_776 . . . ? Eu1 O3 C1 O4 -7.9(5) . . . . ? Eu1 O3 C1 C2 172.5(2) . . . . ? O4 C1 C2 C3 -176.5(3) . . . . ? O3 C1 C2 C3 3.1(4) . . . . ? O4 C1 C2 C7 4.2(4) . . . . ? O3 C1 C2 C7 -176.2(3) . . . . ? C7 C2 C3 C4 -0.7(5) . . . . ? C1 C2 C3 C4 180.0(3) . . . . ? C2 C3 C4 C5 0.3(5) . . . . ? C3 C4 C5 C6 1.0(5) . . . . ? C3 C4 C5 C8 -177.6(3) . . . . ? C4 C5 C6 C7 -1.9(5) . . . . ? C8 C5 C6 C7 176.7(3) . . . . ? C5 C6 C7 C2 1.5(5) . . . . ? C3 C2 C7 C6 -0.2(4) . . . . ? C1 C2 C7 C6 179.2(3) . . . . ? C6 C5 C8 C9 -7.7(5) . . . . ? C4 C5 C8 C9 170.9(3) . . . . ? C5 C8 C9 C10 -179.9(3) . . . . ? C8 C9 C10 C15 -172.5(3) . . . . ? C8 C9 C10 C11 6.3(5) . . . . ? C15 C10 C11 C12 2.3(4) . . . . ? C9 C10 C11 C12 -176.5(3) . . . . ? C10 C11 C12 C13 0.6(4) . . . . ? C11 C12 C13 C14 -2.4(4) . . . . ? C11 C12 C13 C16 173.5(2) . . . . ? C12 C13 C14 C15 1.3(4) . . . . ? C16 C13 C14 C15 -174.5(2) . . . . ? C13 C14 C15 C10 1.6(4) . . . . ? C11 C10 C15 C14 -3.4(4) . . . . ? C9 C10 C15 C14 175.5(3) . . . . ? Eu1 O5 C16 O6 20.4(4) 4_476 . . . ? Eu1 O5 C16 C13 -157.74(18) 4_476 . . . ? Eu1 O5 C16 Eu1 -17.4(3) 4_476 . . 1_455 ? Eu1 O6 C16 O5 -85.0(3) 1_455 . . . ? Eu1 O6 C16 C13 93.1(2) 1_455 . . . ? C14 C13 C16 O5 -178.3(2) . . . . ? C12 C13 C16 O5 5.9(4) . . . . ? C14 C13 C16 O6 3.4(4) . . . . ? C12 C13 C16 O6 -172.3(2) . . . . ? C14 C13 C16 Eu1 41.4(3) . . . 1_455 ? C12 C13 C16 Eu1 -134.4(2) . . . 1_455 ? Eu1 O2 C17 O1 162.8(4) 3_776 . . . ? Eu1 O2 C17 O1 2.6(3) . . . . ? Eu1 O2 C17 Eu1 160.1(6) 3_776 . . . ? Eu1 O1 C17 O2 -169.2(2) 4_575 . . . ? Eu1 O1 C17 O2 -2.7(3) . . . . ? Eu1 O1 C17 Eu1 -166.6(2) 4_575 . . . ? O4 Eu1 C17 O2 -76.23(17) 3_776 . . . ? O5 Eu1 C17 O2 -150.74(17) 4_675 . . . ? O3 Eu1 C17 O2 66.59(18) . . . . ? O2 Eu1 C17 O2 -7.3(2) 3_776 . . . ? O1 Eu1 C17 O2 132.10(17) 4_576 . . . ? O1 Eu1 C17 O2 177.4(3) . . . . ? C16 Eu1 C17 O2 -146.12(18) 1_655 . . . ? Eu1 Eu1 C17 O2 -4.98(15) 3_776 . . . ? O4 Eu1 C17 O1 106.37(18) 3_776 . . . ? O5 Eu1 C17 O1 31.86(18) 4_675 . . . ? O3 Eu1 C17 O1 -110.80(17) . . . . ? O2 Eu1 C17 O1 175.33(17) 3_776 . . . ? O1 Eu1 C17 O1 -45.29(16) 4_576 . . . ? O2 Eu1 C17 O1 -177.4(3) . . . . ? C16 Eu1 C17 O1 36.5(3) 1_655 . . . ? Eu1 Eu1 C17 O1 177.63(19) 3_776 . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.999 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.122 #===END data_complex3 _database_code_depnum_ccdc_archive 'CCDC 716185' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Gd O6' _chemical_formula_sum 'C17 H11 Gd O6' _chemical_formula_weight 468.51 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' Gd Gd -0.1653 3.9035 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.125(3) _cell_length_b 12.821(3) _cell_length_c 6.8828(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.58(3) _cell_angle_gamma 90.00 _cell_volume 1508.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12662 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.063 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_absorpt_coefficient_mu 4.428 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.348 _exptl_absorpt_correction_T_max 0.486 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14342 _diffrn_reflns_av_R_equivalents 0.0770 _diffrn_reflns_av_sigmaI/netI 0.0609 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3436 _reflns_number_gt 3146 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+2.3646P] 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 3436 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0327 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0725 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.013 _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 Gd1 Gd 0.452586(8) 0.371336(10) 0.38619(2) 0.01280(8) Uani 1 1 d . . . O1 O 0.38758(15) 0.38683(18) 0.0877(4) 0.0189(5) Uani 1 1 d . . . O2 O 0.35057(13) 0.24563(18) -0.0821(4) 0.0221(5) Uani 1 1 d . . . O3 O -0.41477(17) 0.3816(2) 0.3176(5) 0.0349(7) Uani 1 1 d . . . O4 O -0.36692(14) 0.5327(2) 0.4385(4) 0.0287(6) Uani 1 1 d . . . O5 O 0.49147(14) 0.21135(18) 0.2187(4) 0.0213(5) Uani 1 1 d . . . O6 O 0.52835(15) 0.05018(18) 0.1875(4) 0.0255(6) Uani 1 1 d . . . C1 C 0.33556(18) 0.3269(2) 0.0105(5) 0.0148(6) Uani 1 1 d . . . C2 C 0.2517(2) 0.3530(3) 0.0357(5) 0.0186(7) Uani 1 1 d . . . C3 C 0.1929(2) 0.2819(3) -0.0268(5) 0.0224(7) Uani 1 1 d . . . H3A H 0.2060 0.2226 -0.0953 0.027 Uiso 1 1 calc R . . C4 C 0.1157(2) 0.2991(3) 0.0123(6) 0.0266(8) Uani 1 1 d . . . H4A H 0.0776 0.2509 -0.0288 0.032 Uiso 1 1 calc R . . C5 C 0.0945(2) 0.3883(3) 0.1130(6) 0.0245(8) Uani 1 1 d . . . C6 C 0.1527(2) 0.4604(3) 0.1673(6) 0.0258(8) Uani 1 1 d . . . H6A H 0.1391 0.5217 0.2293 0.031 Uiso 1 1 calc R . . C7 C 0.2304(2) 0.4430(3) 0.1310(5) 0.0223(7) Uani 1 1 d . . . H7A H 0.2683 0.4918 0.1707 0.027 Uiso 1 1 calc R . . C8 C 0.0144(2) 0.4086(3) 0.1681(6) 0.0292(8) Uani 1 1 d . . . H8A H 0.0055 0.4734 0.2231 0.035 Uiso 1 1 calc R . . C9 C -0.0475(2) 0.3444(3) 0.1482(6) 0.0305(8) Uani 1 1 d . . . H9A H -0.0399 0.2793 0.0930 0.037 Uiso 1 1 calc R . . C10 C -0.1260(2) 0.3692(3) 0.2069(6) 0.0260(9) Uani 1 1 d . . . C11 C -0.1887(2) 0.3020(3) 0.1546(6) 0.0310(9) Uani 1 1 d . . . H11A H -0.1794 0.2407 0.0876 0.037 Uiso 1 1 calc R . . C12 C -0.2645(2) 0.3258(3) 0.2015(6) 0.0277(8) Uani 1 1 d . . . H12A H -0.3053 0.2805 0.1656 0.033 Uiso 1 1 calc R . . C13 C -0.2794(2) 0.4169(3) 0.3019(5) 0.0212(7) Uani 1 1 d . . . C14 C -0.2176(2) 0.4837(3) 0.3555(5) 0.0247(8) Uani 1 1 d . . . H14A H -0.2271 0.5449 0.4226 0.030 Uiso 1 1 calc R . . C15 C -0.1422(2) 0.4595(3) 0.3095(6) 0.0288(8) Uani 1 1 d . . . H15A H -0.1015 0.5044 0.3478 0.035 Uiso 1 1 calc R . . C16 C -0.3598(2) 0.4458(3) 0.3564(6) 0.0231(7) Uani 1 1 d . . . C17 C 0.5232(2) 0.1308(2) 0.2881(6) 0.0207(8) Uani 1 1 d . . . H17A H 0.5435 0.1308 0.4166 0.025 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 Gd1 0.00920(11) 0.00966(11) 0.01970(12) -0.00121(5) 0.00224(7) -0.00068(5) O1 0.0132(12) 0.0212(12) 0.0218(13) 0.0005(10) -0.0021(10) -0.0011(9) O2 0.0154(12) 0.0195(12) 0.0312(13) -0.0053(10) 0.0003(10) 0.0047(9) O3 0.0160(14) 0.0314(15) 0.059(2) -0.0218(13) 0.0135(14) -0.0061(11) O4 0.0153(12) 0.0254(13) 0.0468(16) -0.0154(12) 0.0120(12) -0.0029(10) O5 0.0184(12) 0.0146(11) 0.0309(13) -0.0037(10) 0.0024(10) 0.0023(9) O6 0.0310(14) 0.0143(12) 0.0303(14) -0.0035(10) -0.0037(12) 0.0061(10) C1 0.0122(15) 0.0154(15) 0.0171(15) 0.0035(12) 0.0025(12) 0.0027(12) C2 0.0136(17) 0.0188(15) 0.0237(18) 0.0005(13) 0.0024(14) 0.0044(13) C3 0.0175(16) 0.0226(17) 0.0274(18) -0.0069(14) 0.0042(14) 0.0010(14) C4 0.0140(17) 0.032(2) 0.034(2) -0.0072(16) 0.0024(15) -0.0016(15) C5 0.0153(18) 0.0341(19) 0.0245(19) 0.0016(15) 0.0042(15) 0.0044(15) C6 0.0220(18) 0.0249(18) 0.0306(19) -0.0047(15) 0.0034(15) 0.0080(14) C7 0.0167(16) 0.0231(17) 0.0269(18) -0.0039(14) 0.0013(14) 0.0012(14) C8 0.0177(18) 0.037(2) 0.033(2) -0.0015(17) 0.0063(16) 0.0079(16) C9 0.0166(18) 0.038(2) 0.038(2) -0.0045(18) 0.0090(17) 0.0069(17) C10 0.0146(19) 0.034(2) 0.030(2) -0.0007(14) 0.0058(16) 0.0036(13) C11 0.0190(18) 0.029(2) 0.046(2) -0.0118(17) 0.0084(17) 0.0035(15) C12 0.0152(17) 0.027(2) 0.041(2) -0.0110(17) 0.0062(16) -0.0005(15) C13 0.0147(16) 0.0233(17) 0.0263(18) -0.0045(14) 0.0057(14) -0.0002(14) C14 0.0169(17) 0.0259(18) 0.0319(19) -0.0098(15) 0.0061(15) -0.0020(14) C15 0.0134(16) 0.037(2) 0.036(2) -0.0099(17) 0.0045(15) -0.0047(15) C16 0.0134(16) 0.0223(17) 0.034(2) -0.0074(15) 0.0077(15) -0.0021(14) C17 0.0192(19) 0.0204(18) 0.0221(18) -0.0024(12) -0.0016(16) 0.0020(12) _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 Gd1 O1 2.283(3) . ? Gd1 O4 2.311(2) 3_566 ? Gd1 O2 2.323(2) 4_566 ? Gd1 O3 2.352(3) 1_655 ? Gd1 O6 2.375(2) 2_655 ? Gd1 O5 2.465(2) . ? Gd1 O5 2.572(2) 4_566 ? Gd1 O6 2.581(3) 4_566 ? Gd1 C17 2.949(4) 4_566 ? O1 C1 1.268(4) . ? O2 C1 1.257(4) . ? O2 Gd1 2.323(2) 4_565 ? O3 C16 1.266(4) . ? O3 Gd1 2.352(3) 1_455 ? O4 C16 1.259(4) . ? O4 Gd1 2.311(2) 3_566 ? O5 C17 1.248(4) . ? O5 Gd1 2.572(2) 4_565 ? O6 C17 1.250(4) . ? O6 Gd1 2.375(2) 2_645 ? O6 Gd1 2.581(3) 4_565 ? C1 C2 1.494(5) . ? C2 C7 1.388(5) . ? C2 C3 1.406(5) . ? C3 C4 1.383(5) . ? C3 H3A 0.9300 . ? C4 C5 1.397(5) . ? C4 H4A 0.9300 . ? C5 C6 1.393(5) . ? C5 C8 1.470(5) . ? C6 C7 1.387(5) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.342(6) . ? C8 H8A 0.9300 . ? C9 C10 1.463(5) . ? C9 H9A 0.9300 . ? C10 C15 1.393(5) . ? C10 C11 1.406(5) . ? C11 C12 1.390(5) . ? C11 H11A 0.9300 . ? C12 C13 1.390(5) . ? C12 H12A 0.9300 . ? C13 C14 1.392(5) . ? C13 C16 1.496(5) . ? C14 C15 1.385(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 Gd1 2.949(4) 4_565 ? C17 H17A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Gd1 O4 97.68(10) . 3_566 ? O1 Gd1 O2 79.24(9) . 4_566 ? O4 Gd1 O2 77.82(9) 3_566 4_566 ? O1 Gd1 O3 103.72(11) . 1_655 ? O4 Gd1 O3 136.66(9) 3_566 1_655 ? O2 Gd1 O3 142.78(9) 4_566 1_655 ? O1 Gd1 O6 77.86(8) . 2_655 ? O4 Gd1 O6 72.41(10) 3_566 2_655 ? O2 Gd1 O6 139.24(9) 4_566 2_655 ? O3 Gd1 O6 75.86(9) 1_655 2_655 ? O1 Gd1 O5 77.43(8) . . ? O4 Gd1 O5 152.36(8) 3_566 . ? O2 Gd1 O5 74.54(9) 4_566 . ? O3 Gd1 O5 70.14(8) 1_655 . ? O6 Gd1 O5 131.20(9) 2_655 . ? O1 Gd1 O5 157.08(8) . 4_566 ? O4 Gd1 O5 83.83(9) 3_566 4_566 ? O2 Gd1 O5 78.75(8) 4_566 4_566 ? O3 Gd1 O5 90.12(11) 1_655 4_566 ? O6 Gd1 O5 123.81(8) 2_655 4_566 ? O5 Gd1 O5 90.61(4) . 4_566 ? O1 Gd1 O6 151.82(8) . 4_566 ? O4 Gd1 O6 71.14(9) 3_566 4_566 ? O2 Gd1 O6 121.31(9) 4_566 4_566 ? O3 Gd1 O6 72.31(10) 1_655 4_566 ? O6 Gd1 O6 74.11(9) 2_655 4_566 ? O5 Gd1 O6 124.29(8) . 4_566 ? O5 Gd1 O6 49.94(8) 4_566 4_566 ? O1 Gd1 C17 173.26(10) . 4_566 ? O4 Gd1 C17 75.65(10) 3_566 4_566 ? O2 Gd1 C17 99.95(9) 4_566 4_566 ? O3 Gd1 C17 81.02(11) 1_655 4_566 ? O6 Gd1 C17 98.95(9) 2_655 4_566 ? O5 Gd1 C17 108.89(9) . 4_566 ? O5 Gd1 C17 24.94(8) 4_566 4_566 ? O6 Gd1 C17 25.02(8) 4_566 4_566 ? O1 Gd1 Gd1 116.66(6) . 3_666 ? O4 Gd1 Gd1 66.91(6) 3_566 3_666 ? O2 Gd1 Gd1 142.52(6) 4_566 3_666 ? O3 Gd1 Gd1 69.83(6) 1_655 3_666 ? O6 Gd1 Gd1 38.85(6) 2_655 3_666 ? O5 Gd1 Gd1 139.71(6) . 3_666 ? O5 Gd1 Gd1 85.09(5) 4_566 3_666 ? O6 Gd1 Gd1 35.26(5) 4_566 3_666 ? C17 Gd1 Gd1 60.16(6) 4_566 3_666 ? C1 O1 Gd1 127.9(2) . . ? C1 O2 Gd1 139.6(2) . 4_565 ? C16 O3 Gd1 135.1(2) . 1_455 ? C16 O4 Gd1 142.0(2) . 3_566 ? C17 O5 Gd1 129.3(2) . . ? C17 O5 Gd1 94.7(2) . 4_565 ? Gd1 O5 Gd1 134.16(10) . 4_565 ? C17 O6 Gd1 158.7(2) . 2_645 ? C17 O6 Gd1 94.2(2) . 4_565 ? Gd1 O6 Gd1 105.89(9) 2_645 4_565 ? O2 C1 O1 123.7(3) . . ? O2 C1 C2 118.2(3) . . ? O1 C1 C2 118.1(3) . . ? C7 C2 C3 118.6(3) . . ? C7 C2 C1 121.6(3) . . ? C3 C2 C1 119.6(3) . . ? C4 C3 C2 120.8(3) . . ? C4 C3 H3A 119.6 . . ? C2 C3 H3A 119.6 . . ? C3 C4 C5 120.5(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C6 C5 C4 118.2(3) . . ? C6 C5 C8 118.5(3) . . ? C4 C5 C8 123.2(4) . . ? C7 C6 C5 121.5(3) . . ? C7 C6 H6A 119.2 . . ? C5 C6 H6A 119.2 . . ? C6 C7 C2 120.2(3) . . ? C6 C7 H7A 119.9 . . ? C2 C7 H7A 119.9 . . ? C9 C8 C5 127.6(4) . . ? C9 C8 H8A 116.2 . . ? C5 C8 H8A 116.2 . . ? C8 C9 C10 125.0(4) . . ? C8 C9 H9A 117.5 . . ? C10 C9 H9A 117.5 . . ? C15 C10 C11 117.8(4) . . ? C15 C10 C9 122.4(4) . . ? C11 C10 C9 119.8(3) . . ? C12 C11 C10 121.0(4) . . ? C12 C11 H11A 119.5 . . ? C10 C11 H11A 119.5 . . ? C13 C12 C11 120.2(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.2(3) . . ? C12 C13 C16 122.2(3) . . ? C14 C13 C16 118.5(3) . . ? C15 C14 C13 120.4(3) . . ? C15 C14 H14A 119.8 . . ? C13 C14 H14A 119.8 . . ? C14 C15 C10 121.3(3) . . ? C14 C15 H15A 119.3 . . ? C10 C15 H15A 119.3 . . ? O4 C16 O3 125.3(3) . . ? O4 C16 C13 116.6(3) . . ? O3 C16 C13 118.1(3) . . ? O6 C17 O5 121.1(4) . . ? O6 C17 Gd1 60.78(19) . 4_565 ? O5 C17 Gd1 60.35(19) . 4_565 ? O6 C17 H17A 119.5 . . ? O5 C17 H17A 119.5 . . ? Gd1 C17 H17A 177.6 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Gd1 O1 C1 -90.5(3) 3_566 . . . ? O2 Gd1 O1 C1 -14.5(3) 4_566 . . . ? O3 Gd1 O1 C1 127.5(3) 1_655 . . . ? O6 Gd1 O1 C1 -160.6(3) 2_655 . . . ? O5 Gd1 O1 C1 61.8(3) . . . . ? O5 Gd1 O1 C1 1.8(4) 4_566 . . . ? O6 Gd1 O1 C1 -154.5(2) 4_566 . . . ? Gd1 Gd1 O1 C1 -158.5(2) 3_666 . . . ? O1 Gd1 O5 C17 -165.3(3) . . . . ? O4 Gd1 O5 C17 -82.8(4) 3_566 . . . ? O2 Gd1 O5 C17 -83.2(3) 4_566 . . . ? O3 Gd1 O5 C17 84.9(3) 1_655 . . . ? O6 Gd1 O5 C17 133.5(3) 2_655 . . . ? O5 Gd1 O5 C17 -5.0(3) 4_566 . . . ? O6 Gd1 O5 C17 34.5(3) 4_566 . . . ? C17 Gd1 O5 C17 12.3(3) 4_566 . . . ? Gd1 Gd1 O5 C17 78.1(3) 3_666 . . . ? O1 Gd1 O5 Gd1 -4.78(14) . . . 4_565 ? O4 Gd1 O5 Gd1 77.7(3) 3_566 . . 4_565 ? O2 Gd1 O5 Gd1 77.36(14) 4_566 . . 4_565 ? O3 Gd1 O5 Gd1 -114.60(17) 1_655 . . 4_565 ? O6 Gd1 O5 Gd1 -65.99(18) 2_655 . . 4_565 ? O5 Gd1 O5 Gd1 155.50(11) 4_566 . . 4_565 ? O6 Gd1 O5 Gd1 -165.00(12) 4_566 . . 4_565 ? C17 Gd1 O5 Gd1 172.80(14) 4_566 . . 4_565 ? Gd1 Gd1 O5 Gd1 -121.39(11) 3_666 . . 4_565 ? Gd1 O2 C1 O1 20.5(6) 4_565 . . . ? Gd1 O2 C1 C2 -157.8(3) 4_565 . . . ? Gd1 O1 C1 O2 -84.7(4) . . . . ? Gd1 O1 C1 C2 93.6(3) . . . . ? O2 C1 C2 C7 -178.0(3) . . . . ? O1 C1 C2 C7 3.6(5) . . . . ? O2 C1 C2 C3 6.2(5) . . . . ? O1 C1 C2 C3 -172.2(3) . . . . ? C7 C2 C3 C4 -2.5(6) . . . . ? C1 C2 C3 C4 173.4(3) . . . . ? C2 C3 C4 C5 0.7(6) . . . . ? C3 C4 C5 C6 1.9(6) . . . . ? C3 C4 C5 C8 -176.7(4) . . . . ? C4 C5 C6 C7 -2.9(6) . . . . ? C8 C5 C6 C7 175.9(4) . . . . ? C5 C6 C7 C2 1.1(6) . . . . ? C3 C2 C7 C6 1.6(5) . . . . ? C1 C2 C7 C6 -174.2(3) . . . . ? C6 C5 C8 C9 -172.4(4) . . . . ? C4 C5 C8 C9 6.3(7) . . . . ? C5 C8 C9 C10 179.8(4) . . . . ? C8 C9 C10 C15 -7.0(7) . . . . ? C8 C9 C10 C11 171.2(4) . . . . ? C15 C10 C11 C12 0.9(6) . . . . ? C9 C10 C11 C12 -177.4(4) . . . . ? C10 C11 C12 C13 -0.1(7) . . . . ? C11 C12 C13 C14 -0.3(6) . . . . ? C11 C12 C13 C16 -179.8(4) . . . . ? C12 C13 C14 C15 -0.1(6) . . . . ? C16 C13 C14 C15 179.4(4) . . . . ? C13 C14 C15 C10 0.9(6) . . . . ? C11 C10 C15 C14 -1.2(6) . . . . ? C9 C10 C15 C14 177.0(4) . . . . ? Gd1 O4 C16 O3 14.0(7) 3_566 . . . ? Gd1 O4 C16 C13 -165.8(3) 3_566 . . . ? Gd1 O3 C16 O4 -6.3(7) 1_455 . . . ? Gd1 O3 C16 C13 173.4(3) 1_455 . . . ? C12 C13 C16 O4 -176.5(4) . . . . ? C14 C13 C16 O4 4.0(5) . . . . ? C12 C13 C16 O3 3.7(6) . . . . ? C14 C13 C16 O3 -175.8(4) . . . . ? Gd1 O6 C17 O5 -163.6(5) 2_645 . . . ? Gd1 O6 C17 O5 -2.8(4) 4_565 . . . ? Gd1 O6 C17 Gd1 -160.9(8) 2_645 . . 4_565 ? Gd1 O5 C17 O6 168.9(3) . . . . ? Gd1 O5 C17 O6 2.8(4) 4_565 . . . ? Gd1 O5 C17 Gd1 166.1(3) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.722 _refine_diff_density_min -1.473 _refine_diff_density_rms 0.165 #===END data_complex4 _database_code_depnum_ccdc_archive 'CCDC 716186' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 O6 Tb' _chemical_formula_sum 'C17 H11 O6 Tb' _chemical_formula_weight 470.18 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' 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.106(3) _cell_length_b 12.758(3) _cell_length_c 6.8875(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.57(3) _cell_angle_gamma 90.00 _cell_volume 1500.1(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 10373 _cell_measurement_theta_min 3.18 _cell_measurement_theta_max 27.44 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.082 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 4.746 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.570 _exptl_absorpt_correction_T_max 0.681 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 14358 _diffrn_reflns_av_R_equivalents 0.0789 _diffrn_reflns_av_sigmaI/netI 0.0649 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.45 _reflns_number_total 3436 _reflns_number_gt 2775 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.0331P)^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 3436 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0469 _refine_ls_R_factor_gt 0.0356 _refine_ls_wR_factor_ref 0.0843 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.952966(12) 0.629006(15) 0.88706(3) 0.01822(9) Uani 1 1 d . . . O1 O 0.8884(2) 0.6130(2) 0.5903(5) 0.0238(7) Uani 1 1 d . . . O2 O 0.85133(19) 0.7544(2) 0.4193(5) 0.0254(8) Uani 1 1 d . . . O3 O 0.1330(2) 0.4667(3) 0.9405(6) 0.0337(9) Uani 1 1 d . . . O4 O 0.0851(2) 0.6188(3) 0.8228(7) 0.0407(10) Uani 1 1 d . . . O5 O 0.99124(19) 0.7883(2) 0.7190(5) 0.0258(8) Uani 1 1 d . . . O6 O 1.0274(2) 0.9508(2) 0.6854(5) 0.0307(8) Uani 1 1 d . . . C1 C 0.8356(3) 0.6724(4) 0.5114(7) 0.0221(10) Uani 1 1 d . . . C2 C 0.7521(3) 0.6460(3) 0.5352(7) 0.0223(10) Uani 1 1 d . . . C3 C 0.7306(3) 0.5561(4) 0.6321(7) 0.0264(11) Uani 1 1 d . . . H3 H 0.7685 0.5073 0.6730 0.032 Uiso 1 1 calc R . . C4 C 0.6528(3) 0.5389(4) 0.6683(8) 0.0277(11) Uani 1 1 d . . . H4 H 0.6392 0.4776 0.7312 0.033 Uiso 1 1 calc R . . C5 C 0.5948(3) 0.6105(4) 0.6132(8) 0.0285(11) Uani 1 1 d . . . C6 C 0.6169(3) 0.7003(4) 0.5122(8) 0.0304(12) Uani 1 1 d . . . H6 H 0.5789 0.7490 0.4709 0.036 Uiso 1 1 calc R . . C7 C 0.6937(3) 0.7175(4) 0.4735(7) 0.0249(10) Uani 1 1 d . . . H7 H 0.7070 0.7772 0.4056 0.030 Uiso 1 1 calc R . . C8 C 0.5145(3) 0.5914(4) 0.6678(8) 0.0338(12) Uani 1 1 d . . . H8 H 0.5054 0.5264 0.7229 0.041 Uiso 1 1 calc R . . C9 C 0.4527(3) 0.6557(4) 0.6485(9) 0.0363(13) Uani 1 1 d . . . H9 H 0.4601 0.7211 0.5928 0.044 Uiso 1 1 calc R . . C10 C 0.3740(3) 0.6308(4) 0.7085(8) 0.0284(12) Uani 1 1 d . . . C11 C 0.3577(3) 0.5400(4) 0.8110(8) 0.0320(12) Uani 1 1 d . . . H11 H 0.3983 0.4947 0.8499 0.038 Uiso 1 1 calc R . . C12 C 0.2824(3) 0.5161(4) 0.8556(8) 0.0297(11) Uani 1 1 d . . . H12 H 0.2727 0.4543 0.9217 0.036 Uiso 1 1 calc R . . C13 C 0.2204(3) 0.5832(4) 0.8030(7) 0.0254(11) Uani 1 1 d . . . C14 C 0.2361(3) 0.6747(4) 0.7048(9) 0.0347(13) Uani 1 1 d . . . H14 H 0.1955 0.7210 0.6710 0.042 Uiso 1 1 calc R . . C15 C 0.3110(3) 0.6981(4) 0.6565(9) 0.0369(13) Uani 1 1 d . . . H15 H 0.3201 0.7594 0.5884 0.044 Uiso 1 1 calc R . . C16 C 0.1413(3) 0.5547(4) 0.8590(8) 0.0273(11) Uani 1 1 d . . . C17 C 1.0232(3) 0.8707(3) 0.7869(8) 0.0279(12) Uani 1 1 d . . . H17 H 1.0440 0.8715 0.9149 0.034 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 0.01673(14) 0.01668(14) 0.02177(14) 0.00130(9) 0.00549(9) 0.00084(8) O1 0.0190(17) 0.0249(16) 0.0278(18) -0.0008(15) 0.0032(15) 0.0016(14) O2 0.0188(17) 0.0277(16) 0.0300(19) 0.0048(14) 0.0045(15) -0.0035(13) O3 0.0222(19) 0.0297(18) 0.051(2) 0.0161(17) 0.0130(18) 0.0022(15) O4 0.022(2) 0.036(2) 0.066(3) 0.0233(19) 0.014(2) 0.0057(16) O5 0.0247(18) 0.0185(15) 0.0347(19) 0.0036(15) 0.0047(16) -0.0005(14) O6 0.042(2) 0.0195(16) 0.0300(19) 0.0053(15) -0.0027(18) -0.0036(15) C1 0.021(2) 0.025(2) 0.020(2) -0.006(2) 0.004(2) -0.003(2) C2 0.021(2) 0.026(2) 0.021(2) -0.001(2) 0.005(2) -0.0038(19) C3 0.022(2) 0.028(2) 0.029(3) 0.004(2) 0.003(2) -0.004(2) C4 0.024(3) 0.032(3) 0.028(3) 0.005(2) 0.002(2) -0.007(2) C5 0.019(3) 0.042(3) 0.024(3) 0.004(2) 0.006(2) -0.006(2) C6 0.023(3) 0.035(3) 0.033(3) 0.008(2) 0.004(2) 0.005(2) C7 0.023(3) 0.029(2) 0.024(2) 0.006(2) 0.007(2) -0.001(2) C8 0.025(3) 0.044(3) 0.035(3) -0.004(3) 0.013(2) -0.010(2) C9 0.025(3) 0.039(3) 0.047(3) 0.003(3) 0.012(3) -0.007(2) C10 0.024(3) 0.036(3) 0.026(3) -0.001(2) 0.009(2) -0.005(2) C11 0.017(2) 0.041(3) 0.038(3) 0.010(3) 0.004(2) 0.003(2) C12 0.026(3) 0.032(3) 0.033(3) 0.004(2) 0.013(2) 0.000(2) C13 0.019(2) 0.031(3) 0.027(3) 0.005(2) 0.007(2) -0.002(2) C14 0.026(3) 0.031(3) 0.049(4) 0.009(3) 0.012(3) 0.001(2) C15 0.026(3) 0.040(3) 0.046(3) 0.013(3) 0.010(3) -0.002(2) C16 0.021(2) 0.032(2) 0.030(3) 0.004(2) 0.006(2) 0.001(2) C17 0.020(3) 0.034(3) 0.030(3) 0.003(2) 0.004(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Tb1 O1 2.271(3) . ? Tb1 O3 2.298(3) 3_667 ? Tb1 O2 2.309(3) 4_576 ? Tb1 O4 2.334(4) 1_655 ? Tb1 O6 2.357(3) 2_746 ? Tb1 O5 2.448(3) . ? Tb1 O6 2.560(3) 4_576 ? Tb1 O5 2.565(3) 4_576 ? Tb1 C17 2.935(6) 4_576 ? O1 C1 1.275(6) . ? O2 C1 1.261(6) . ? O2 Tb1 2.309(3) 4_575 ? O3 C16 1.267(6) . ? O3 Tb1 2.298(3) 3_667 ? O4 C16 1.275(6) . ? O4 Tb1 2.334(4) 1_455 ? O5 C17 1.261(5) . ? O5 Tb1 2.565(3) 4_575 ? O6 C17 1.243(6) . ? O6 Tb1 2.357(3) 2_756 ? O6 Tb1 2.560(3) 4_575 ? C1 C2 1.487(7) . ? C2 C3 1.388(6) . ? C2 C7 1.398(6) . ? C3 C4 1.387(7) . ? C3 H3 0.9300 . ? C4 C5 1.384(7) . ? C4 H4 0.9300 . ? C5 C6 1.405(7) . ? C5 C8 1.466(7) . ? C6 C7 1.374(7) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.339(8) . ? C8 H8 0.9300 . ? C9 C10 1.466(8) . ? C9 H9 0.9300 . ? C10 C11 1.394(7) . ? C10 C15 1.408(7) . ? C11 C12 1.377(7) . ? C11 H11 0.9300 . ? C12 C13 1.393(6) . ? C12 H12 0.9300 . ? C13 C14 1.383(7) . ? C13 C16 1.476(7) . ? C14 C15 1.377(7) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C17 Tb1 2.935(6) 4_575 ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Tb1 O3 97.25(13) . 3_667 ? O1 Tb1 O2 79.49(12) . 4_576 ? O3 Tb1 O2 77.45(12) 3_667 4_576 ? O1 Tb1 O4 104.27(15) . 1_655 ? O3 Tb1 O4 136.62(12) 3_667 1_655 ? O2 Tb1 O4 142.96(11) 4_576 1_655 ? O1 Tb1 O6 77.89(11) . 2_746 ? O3 Tb1 O6 72.61(13) 3_667 2_746 ? O2 Tb1 O6 139.46(12) 4_576 2_746 ? O4 Tb1 O6 75.71(13) 1_655 2_746 ? O1 Tb1 O5 77.20(11) . . ? O3 Tb1 O5 152.13(11) 3_667 . ? O2 Tb1 O5 74.69(12) 4_576 . ? O4 Tb1 O5 70.49(11) 1_655 . ? O6 Tb1 O5 130.91(12) 2_746 . ? O1 Tb1 O6 151.20(10) . 4_576 ? O3 Tb1 O6 71.11(12) 3_667 4_576 ? O2 Tb1 O6 121.24(12) 4_576 4_576 ? O4 Tb1 O6 72.00(14) 1_655 4_576 ? O6 Tb1 O6 73.51(13) 2_746 4_576 ? O5 Tb1 O6 125.13(11) . 4_576 ? O1 Tb1 O5 157.19(11) . 4_576 ? O3 Tb1 O5 83.92(12) 3_667 4_576 ? O2 Tb1 O5 78.54(11) 4_576 4_576 ? O4 Tb1 O5 89.76(14) 1_655 4_576 ? O6 Tb1 O5 123.63(11) 2_746 4_576 ? O5 Tb1 O5 91.10(6) . 4_576 ? O6 Tb1 O5 50.33(11) 4_576 4_576 ? O1 Tb1 C17 172.84(12) . 4_576 ? O3 Tb1 C17 75.74(14) 3_667 4_576 ? O2 Tb1 C17 100.11(13) 4_576 4_576 ? O4 Tb1 C17 80.41(15) 1_655 4_576 ? O6 Tb1 C17 98.32(12) 2_746 4_576 ? O5 Tb1 C17 109.67(12) . 4_576 ? O6 Tb1 C17 24.96(11) 4_576 4_576 ? O5 Tb1 C17 25.38(11) 4_576 4_576 ? O1 Tb1 Tb1 116.34(8) . 3_767 ? O3 Tb1 Tb1 67.10(8) 3_667 3_767 ? O2 Tb1 Tb1 142.31(9) 4_576 3_767 ? O4 Tb1 Tb1 69.62(8) 1_655 3_767 ? O6 Tb1 Tb1 38.52(8) 2_746 3_767 ? O5 Tb1 Tb1 139.94(8) . 3_767 ? O6 Tb1 Tb1 34.99(7) 4_576 3_767 ? O5 Tb1 Tb1 85.21(7) 4_576 3_767 ? C17 Tb1 Tb1 59.85(9) 4_576 3_767 ? C1 O1 Tb1 128.5(3) . . ? C1 O2 Tb1 140.2(3) . 4_575 ? C16 O3 Tb1 142.4(3) . 3_667 ? C16 O4 Tb1 136.6(3) . 1_455 ? C17 O5 Tb1 129.7(3) . . ? C17 O5 Tb1 93.9(3) . 4_575 ? Tb1 O5 Tb1 134.58(14) . 4_575 ? C17 O6 Tb1 157.9(3) . 2_756 ? C17 O6 Tb1 94.7(3) . 4_575 ? Tb1 O6 Tb1 106.49(13) 2_756 4_575 ? O2 C1 O1 122.7(4) . . ? O2 C1 C2 118.7(4) . . ? O1 C1 C2 118.6(4) . . ? C3 C2 C7 118.7(5) . . ? C3 C2 C1 121.7(4) . . ? C7 C2 C1 119.5(4) . . ? C4 C3 C2 120.2(5) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C5 C4 C3 121.7(5) . . ? C5 C4 H4 119.1 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 117.6(5) . . ? C4 C5 C8 119.2(5) . . ? C6 C5 C8 123.2(5) . . ? C7 C6 C5 121.1(5) . . ? C7 C6 H6 119.5 . . ? C5 C6 H6 119.5 . . ? C6 C7 C2 120.7(5) . . ? C6 C7 H7 119.7 . . ? C2 C7 H7 119.7 . . ? C9 C8 C5 128.3(5) . . ? C9 C8 H8 115.8 . . ? C5 C8 H8 115.8 . . ? C8 C9 C10 124.9(5) . . ? C8 C9 H9 117.6 . . ? C10 C9 H9 117.6 . . ? C11 C10 C15 117.5(5) . . ? C11 C10 C9 122.7(5) . . ? C15 C10 C9 119.8(5) . . ? C12 C11 C10 121.1(5) . . ? C12 C11 H11 119.4 . . ? C10 C11 H11 119.4 . . ? C11 C12 C13 120.9(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 118.6(5) . . ? C14 C13 C16 123.0(4) . . ? C12 C13 C16 118.4(4) . . ? C15 C14 C13 120.9(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C10 121.0(5) . . ? C14 C15 H15 119.5 . . ? C10 C15 H15 119.5 . . ? O3 C16 O4 123.4(5) . . ? O3 C16 C13 117.7(4) . . ? O4 C16 C13 118.9(4) . . ? O6 C17 O5 121.0(5) . . ? O6 C17 Tb1 60.4(3) . 4_575 ? O5 C17 Tb1 60.7(3) . 4_575 ? O6 C17 H17 119.5 . . ? O5 C17 H17 119.5 . . ? Tb1 C17 H17 178.2 4_575 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 Tb1 O1 C1 89.9(4) 3_667 . . . ? O2 Tb1 O1 C1 14.2(4) 4_576 . . . ? O4 Tb1 O1 C1 -128.1(4) 1_655 . . . ? O6 Tb1 O1 C1 160.3(4) 2_746 . . . ? O5 Tb1 O1 C1 -62.4(4) . . . . ? O6 Tb1 O1 C1 153.4(4) 4_576 . . . ? O5 Tb1 O1 C1 -1.7(6) 4_576 . . . ? Tb1 Tb1 O1 C1 157.9(4) 3_767 . . . ? O1 Tb1 O5 C17 165.3(4) . . . . ? O3 Tb1 O5 C17 84.1(5) 3_667 . . . ? O2 Tb1 O5 C17 82.9(4) 4_576 . . . ? O4 Tb1 O5 C17 -84.3(4) 1_655 . . . ? O6 Tb1 O5 C17 -133.5(4) 2_746 . . . ? O6 Tb1 O5 C17 -34.8(5) 4_576 . . . ? O5 Tb1 O5 C17 5.1(4) 4_576 . . . ? C17 Tb1 O5 C17 -12.6(4) 4_576 . . . ? Tb1 Tb1 O5 C17 -78.8(4) 3_767 . . . ? O1 Tb1 O5 Tb1 4.69(19) . . . 4_575 ? O3 Tb1 O5 Tb1 -76.5(3) 3_667 . . 4_575 ? O2 Tb1 O5 Tb1 -77.7(2) 4_576 . . 4_575 ? O4 Tb1 O5 Tb1 115.1(2) 1_655 . . 4_575 ? O6 Tb1 O5 Tb1 65.9(2) 2_746 . . 4_575 ? O6 Tb1 O5 Tb1 164.55(16) 4_576 . . 4_575 ? O5 Tb1 O5 Tb1 -155.55(15) 4_576 . . 4_575 ? C17 Tb1 O5 Tb1 -173.22(19) 4_576 . . 4_575 ? Tb1 Tb1 O5 Tb1 120.59(15) 3_767 . . 4_575 ? Tb1 O2 C1 O1 -19.3(8) 4_575 . . . ? Tb1 O2 C1 C2 158.4(3) 4_575 . . . ? Tb1 O1 C1 O2 84.3(6) . . . . ? Tb1 O1 C1 C2 -93.3(5) . . . . ? O2 C1 C2 C3 178.9(5) . . . . ? O1 C1 C2 C3 -3.3(7) . . . . ? O2 C1 C2 C7 -6.6(7) . . . . ? O1 C1 C2 C7 171.2(4) . . . . ? C7 C2 C3 C4 -0.8(7) . . . . ? C1 C2 C3 C4 173.8(5) . . . . ? C2 C3 C4 C5 -1.2(8) . . . . ? C3 C4 C5 C6 2.3(8) . . . . ? C3 C4 C5 C8 -175.7(5) . . . . ? C4 C5 C6 C7 -1.4(8) . . . . ? C8 C5 C6 C7 176.4(5) . . . . ? C5 C6 C7 C2 -0.5(8) . . . . ? C3 C2 C7 C6 1.6(7) . . . . ? C1 C2 C7 C6 -173.1(5) . . . . ? C4 C5 C8 C9 171.7(6) . . . . ? C6 C5 C8 C9 -6.1(9) . . . . ? C5 C8 C9 C10 -179.5(5) . . . . ? C8 C9 C10 C11 6.7(9) . . . . ? C8 C9 C10 C15 -171.1(6) . . . . ? C15 C10 C11 C12 1.4(8) . . . . ? C9 C10 C11 C12 -176.3(5) . . . . ? C10 C11 C12 C13 -1.3(9) . . . . ? C11 C12 C13 C14 0.0(8) . . . . ? C11 C12 C13 C16 -178.6(5) . . . . ? C12 C13 C14 C15 1.2(9) . . . . ? C16 C13 C14 C15 179.7(5) . . . . ? C13 C14 C15 C10 -1.2(9) . . . . ? C11 C10 C15 C14 -0.2(8) . . . . ? C9 C10 C15 C14 177.6(6) . . . . ? Tb1 O3 C16 O4 -13.8(9) 3_667 . . . ? Tb1 O3 C16 C13 166.4(4) 3_667 . . . ? Tb1 O4 C16 O3 5.3(9) 1_455 . . . ? Tb1 O4 C16 C13 -175.0(4) 1_455 . . . ? C14 C13 C16 O3 176.8(5) . . . . ? C12 C13 C16 O3 -4.7(8) . . . . ? C14 C13 C16 O4 -3.0(8) . . . . ? C12 C13 C16 O4 175.5(5) . . . . ? Tb1 O6 C17 O5 165.6(6) 2_756 . . . ? Tb1 O6 C17 O5 2.1(5) 4_575 . . . ? Tb1 O6 C17 Tb1 163.5(10) 2_756 . . 4_575 ? Tb1 O5 C17 O6 -168.4(4) . . . . ? Tb1 O5 C17 O6 -2.1(5) 4_575 . . . ? Tb1 O5 C17 Tb1 -166.3(4) . . . 4_575 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.729 _refine_diff_density_min -1.459 _refine_diff_density_rms 0.172 #===END data_complex5 _database_code_depnum_ccdc_archive 'CCDC 716187' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Er O6' _chemical_formula_sum 'C17 H11 Er O6' _chemical_formula_weight 478.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Er Er -0.2586 4.9576 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 17.060(3) _cell_length_b 12.622(3) _cell_length_c 6.8426(14) _cell_angle_alpha 90.00 _cell_angle_beta 93.46(3) _cell_angle_gamma 90.00 _cell_volume 1470.7(5) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 20377 _cell_measurement_theta_min 3.23 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 5.738 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.268 _exptl_absorpt_correction_T_max 0.402 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23023 _diffrn_reflns_av_R_equivalents 0.0922 _diffrn_reflns_av_sigmaI/netI 0.0606 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 27.44 _reflns_number_total 3363 _reflns_number_gt 3153 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^+1.0642P] 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 3363 _refine_ls_number_parameters 217 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0246 _refine_ls_R_factor_gt 0.0231 _refine_ls_wR_factor_ref 0.0595 _refine_ls_wR_factor_gt 0.0585 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _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 Er1 Er 0.453613(6) 0.371102(7) 0.388226(15) 0.01238(6) Uani 1 1 d . . . O1 O 0.38996(12) 0.38864(14) 0.0948(3) 0.0179(4) Uani 1 1 d . . . O2 O 0.35341(11) 0.24542(14) -0.0785(3) 0.0197(4) Uani 1 1 d . . . O3 O -0.41554(15) 0.37983(15) 0.3242(4) 0.0326(6) Uani 1 1 d . . . O4 O -0.36760(12) 0.53372(14) 0.4432(3) 0.0263(5) Uani 1 1 d . . . O5 O 0.49124(12) 0.21280(13) 0.2170(3) 0.0206(4) Uani 1 1 d . . . O6 O 0.52638(13) 0.04869(14) 0.1840(3) 0.0237(4) Uani 1 1 d . . . C1 C 0.33787(16) 0.3274(2) 0.0148(4) 0.0154(5) Uani 1 1 d . . . C2 C 0.25396(17) 0.3540(2) 0.0377(4) 0.0168(5) Uani 1 1 d . . . C3 C 0.19524(16) 0.2816(2) -0.0250(4) 0.0205(6) Uani 1 1 d . . . H3A H 0.2089 0.2213 -0.0932 0.025 Uiso 1 1 calc R . . C4 C 0.11751(18) 0.2985(2) 0.0128(4) 0.0249(6) Uani 1 1 d . . . H4A H 0.0795 0.2493 -0.0294 0.030 Uiso 1 1 calc R . . C5 C 0.09558(19) 0.3893(2) 0.1146(4) 0.0228(6) Uani 1 1 d . . . C6 C 0.15391(17) 0.4630(2) 0.1684(4) 0.0234(6) Uani 1 1 d . . . H6A H 0.1400 0.5254 0.2296 0.028 Uiso 1 1 calc R . . C7 C 0.23163(17) 0.4456(2) 0.1332(4) 0.0205(6) Uani 1 1 d . . . H7A H 0.2694 0.4955 0.1735 0.025 Uiso 1 1 calc R . . C8 C 0.01549(18) 0.4089(3) 0.1699(4) 0.0272(6) Uani 1 1 d . . . H8A H 0.0064 0.4748 0.2251 0.033 Uiso 1 1 calc R . . C9 C -0.04677(19) 0.3436(3) 0.1508(5) 0.0297(7) Uani 1 1 d . . . H9A H -0.0390 0.2772 0.0961 0.036 Uiso 1 1 calc R . . C10 C -0.1256(2) 0.3683(2) 0.2091(5) 0.0251(7) Uani 1 1 d . . . C11 C -0.18817(19) 0.2994(2) 0.1589(5) 0.0287(7) Uani 1 1 d . . . H11A H -0.1785 0.2369 0.0926 0.034 Uiso 1 1 calc R . . C12 C -0.26431(18) 0.3228(2) 0.2065(5) 0.0261(6) Uani 1 1 d . . . H12A H -0.3050 0.2760 0.1722 0.031 Uiso 1 1 calc R . . C13 C -0.27981(16) 0.4159(2) 0.3054(4) 0.0196(5) Uani 1 1 d . . . C14 C -0.21800(17) 0.4845(2) 0.3564(4) 0.0235(6) Uani 1 1 d . . . H14A H -0.2278 0.5472 0.4221 0.028 Uiso 1 1 calc R . . C15 C -0.14258(17) 0.4606(2) 0.3106(4) 0.0262(6) Uani 1 1 d . . . H15A H -0.1020 0.5069 0.3481 0.031 Uiso 1 1 calc R . . C16 C -0.36017(17) 0.4452(2) 0.3612(4) 0.0221(6) Uani 1 1 d . . . C17 C 0.5224(2) 0.13008(17) 0.2863(5) 0.0196(6) Uani 1 1 d . . . H17A H 0.5427 0.1293 0.4155 0.024 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 Er1 0.01072(10) 0.00864(8) 0.01794(9) -0.00112(3) 0.00213(6) -0.00060(3) O1 0.0139(11) 0.0188(9) 0.0206(10) 0.0015(8) -0.0016(8) -0.0012(7) O2 0.0159(10) 0.0165(9) 0.0266(10) -0.0039(7) 0.0006(8) 0.0044(7) O3 0.0188(13) 0.0257(11) 0.0548(16) -0.0183(9) 0.0144(12) -0.0061(8) O4 0.0161(10) 0.0211(10) 0.0428(12) -0.0132(9) 0.0116(9) -0.0022(8) O5 0.0207(11) 0.0124(8) 0.0287(10) -0.0038(7) 0.0021(8) 0.0015(7) O6 0.0288(12) 0.0139(9) 0.0282(10) -0.0028(8) -0.0005(9) 0.0064(8) C1 0.0110(13) 0.0179(12) 0.0171(12) 0.0059(10) -0.0008(10) 0.0017(10) C2 0.0141(15) 0.0172(11) 0.0193(13) 0.0006(10) 0.0018(11) 0.0045(10) C3 0.0172(14) 0.0205(13) 0.0239(14) -0.0037(10) 0.0011(11) 0.0019(10) C4 0.0172(15) 0.0288(15) 0.0289(15) -0.0039(12) 0.0025(12) -0.0013(11) C5 0.0146(16) 0.0313(14) 0.0227(14) 0.0021(12) 0.0022(12) 0.0060(11) C6 0.0195(15) 0.0238(13) 0.0273(14) -0.0026(11) 0.0040(12) 0.0055(11) C7 0.0174(14) 0.0197(13) 0.0245(13) -0.0031(10) 0.0008(11) 0.0012(10) C8 0.0193(17) 0.0327(16) 0.0299(16) -0.0023(13) 0.0054(12) 0.0068(13) C9 0.0214(17) 0.0323(15) 0.0362(17) -0.0029(14) 0.0082(13) 0.0060(14) C10 0.0179(18) 0.0290(17) 0.0287(16) 0.0006(10) 0.0041(14) 0.0038(10) C11 0.0241(17) 0.0255(14) 0.0374(17) -0.0071(12) 0.0086(13) 0.0051(12) C12 0.0187(16) 0.0238(15) 0.0363(17) -0.0081(12) 0.0050(13) -0.0026(11) C13 0.0143(14) 0.0209(13) 0.0240(14) -0.0026(10) 0.0048(11) 0.0009(10) C14 0.0185(15) 0.0242(13) 0.0280(14) -0.0066(11) 0.0044(11) -0.0019(11) C15 0.0142(15) 0.0327(15) 0.0319(16) -0.0071(12) 0.0032(12) -0.0045(11) C16 0.0138(14) 0.0220(13) 0.0310(15) -0.0059(11) 0.0057(12) -0.0013(10) C17 0.0221(18) 0.0180(14) 0.0188(14) -0.0025(9) 0.0012(13) 0.0016(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 Er1 O1 2.235(2) . ? Er1 O4 2.2654(19) 3_566 ? Er1 O2 2.2768(18) 4_566 ? Er1 O3 2.303(2) 1_655 ? Er1 O6 2.3249(18) 2_655 ? Er1 O5 2.4224(18) . ? Er1 O6 2.521(2) 4_566 ? Er1 O5 2.5336(19) 4_566 ? Er1 C17 2.900(3) 4_566 ? O1 C1 1.276(3) . ? O2 C1 1.253(3) . ? O2 Er1 2.2768(18) 4_565 ? O3 C16 1.268(3) . ? O3 Er1 2.303(2) 1_455 ? O4 C16 1.261(3) . ? O4 Er1 2.2654(19) 3_566 ? O5 C17 1.252(3) . ? O5 Er1 2.5336(19) 4_565 ? O6 C17 1.247(3) . ? O6 Er1 2.3249(18) 2_645 ? O6 Er1 2.521(2) 4_565 ? C1 C2 1.488(4) . ? C2 C7 1.392(4) . ? C2 C3 1.404(4) . ? C3 C4 1.383(4) . ? C3 H3A 0.9300 . ? C4 C5 1.404(4) . ? C4 H4A 0.9300 . ? C5 C6 1.395(4) . ? C5 C8 1.460(4) . ? C6 C7 1.379(4) . ? C6 H6A 0.9300 . ? C7 H7A 0.9300 . ? C8 C9 1.345(5) . ? C8 H8A 0.9300 . ? C9 C10 1.459(4) . ? C9 H9A 0.9300 . ? C10 C15 1.396(4) . ? C10 C11 1.403(4) . ? C11 C12 1.390(4) . ? C11 H11A 0.9300 . ? C12 C13 1.390(4) . ? C12 H12A 0.9300 . ? C13 C14 1.392(4) . ? C13 C16 1.491(4) . ? C14 C15 1.376(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C17 Er1 2.900(3) 4_565 ? C17 H17A 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Er1 O4 96.34(8) . 3_566 ? O1 Er1 O2 80.03(7) . 4_566 ? O4 Er1 O2 77.19(7) 3_566 4_566 ? O1 Er1 O3 104.38(9) . 1_655 ? O4 Er1 O3 137.43(7) 3_566 1_655 ? O2 Er1 O3 142.38(7) 4_566 1_655 ? O1 Er1 O6 77.48(7) . 2_655 ? O4 Er1 O6 72.84(7) 3_566 2_655 ? O2 Er1 O6 139.88(7) 4_566 2_655 ? O3 Er1 O6 75.94(7) 1_655 2_655 ? O1 Er1 O5 77.04(7) . . ? O4 Er1 O5 151.94(7) 3_566 . ? O2 Er1 O5 74.82(7) 4_566 . ? O3 Er1 O5 70.08(7) 1_655 . ? O6 Er1 O5 130.23(7) 2_655 . ? O1 Er1 O6 150.47(6) . 4_566 ? O4 Er1 O6 71.40(7) 3_566 4_566 ? O2 Er1 O6 121.02(7) 4_566 4_566 ? O3 Er1 O6 72.39(8) 1_655 4_566 ? O6 Er1 O6 73.26(8) 2_655 4_566 ? O5 Er1 O6 125.97(6) . 4_566 ? O1 Er1 O5 157.25(7) . 4_566 ? O4 Er1 O5 84.64(7) 3_566 4_566 ? O2 Er1 O5 78.04(7) 4_566 4_566 ? O3 Er1 O5 89.56(9) 1_655 4_566 ? O6 Er1 O5 123.99(6) 2_655 4_566 ? O5 Er1 O5 91.40(4) . 4_566 ? O6 Er1 O5 50.89(6) 4_566 4_566 ? O1 Er1 C17 172.41(7) . 4_566 ? O4 Er1 C17 76.23(9) 3_566 4_566 ? O2 Er1 C17 99.57(7) 4_566 4_566 ? O3 Er1 C17 80.63(9) 1_655 4_566 ? O6 Er1 C17 98.53(7) 2_655 4_566 ? O5 Er1 C17 110.25(7) . 4_566 ? O6 Er1 C17 25.39(6) 4_566 4_566 ? O5 Er1 C17 25.51(6) 4_566 4_566 ? O1 Er1 Er1 115.74(5) . 3_666 ? O4 Er1 Er1 67.48(5) 3_566 3_666 ? O2 Er1 Er1 142.27(5) 4_566 3_666 ? O3 Er1 Er1 70.05(5) 1_655 3_666 ? O6 Er1 Er1 38.36(5) 2_655 3_666 ? O5 Er1 Er1 140.05(5) . 3_666 ? O6 Er1 Er1 34.90(4) 4_566 3_666 ? O5 Er1 Er1 85.71(4) 4_566 3_666 ? C17 Er1 Er1 60.21(5) 4_566 3_666 ? C1 O1 Er1 127.86(16) . . ? C1 O2 Er1 140.16(18) . 4_565 ? C16 O3 Er1 135.42(18) . 1_455 ? C16 O4 Er1 141.50(18) . 3_566 ? C17 O5 Er1 128.57(19) . . ? C17 O5 Er1 93.82(17) . 4_565 ? Er1 O5 Er1 135.55(8) . 4_565 ? C17 O6 Er1 157.98(19) . 2_645 ? C17 O6 Er1 94.51(18) . 4_565 ? Er1 O6 Er1 106.74(8) 2_645 4_565 ? O2 C1 O1 123.8(2) . . ? O2 C1 C2 118.3(2) . . ? O1 C1 C2 117.9(2) . . ? C7 C2 C3 118.3(3) . . ? C7 C2 C1 121.9(3) . . ? C3 C2 C1 119.6(2) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3A 119.4 . . ? C2 C3 H3A 119.4 . . ? C3 C4 C5 120.4(3) . . ? C3 C4 H4A 119.8 . . ? C5 C4 H4A 119.8 . . ? C6 C5 C4 117.9(3) . . ? C6 C5 C8 118.9(3) . . ? C4 C5 C8 123.2(3) . . ? C7 C6 C5 121.8(3) . . ? C7 C6 H6A 119.1 . . ? C5 C6 H6A 119.1 . . ? C6 C7 C2 120.5(3) . . ? C6 C7 H7A 119.8 . . ? C2 C7 H7A 119.8 . . ? C9 C8 C5 128.1(3) . . ? C9 C8 H8A 116.0 . . ? C5 C8 H8A 116.0 . . ? C8 C9 C10 125.3(3) . . ? C8 C9 H9A 117.4 . . ? C10 C9 H9A 117.4 . . ? C15 C10 C11 117.5(3) . . ? C15 C10 C9 122.5(3) . . ? C11 C10 C9 120.0(3) . . ? C12 C11 C10 121.2(3) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C13 C12 C11 120.1(3) . . ? C13 C12 H12A 119.9 . . ? C11 C12 H12A 119.9 . . ? C12 C13 C14 119.0(3) . . ? C12 C13 C16 122.6(2) . . ? C14 C13 C16 118.4(2) . . ? C15 C14 C13 120.7(3) . . ? C15 C14 H14A 119.7 . . ? C13 C14 H14A 119.7 . . ? C14 C15 C10 121.5(3) . . ? C14 C15 H15A 119.3 . . ? C10 C15 H15A 119.3 . . ? O4 C16 O3 124.9(3) . . ? O4 C16 C13 116.9(2) . . ? O3 C16 C13 118.3(2) . . ? O6 C17 O5 120.7(3) . . ? O6 C17 Er1 60.09(16) . 4_565 ? O5 C17 Er1 60.67(16) . 4_565 ? O6 C17 H17A 119.6 . . ? O5 C17 H17A 119.6 . . ? Er1 C17 H17A 177.9 4_565 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Er1 O1 C1 -91.2(2) 3_566 . . . ? O2 Er1 O1 C1 -15.4(2) 4_566 . . . ? O3 Er1 O1 C1 126.3(2) 1_655 . . . ? O6 Er1 O1 C1 -162.0(2) 2_655 . . . ? O5 Er1 O1 C1 61.1(2) . . . . ? O6 Er1 O1 C1 -154.12(19) 4_566 . . . ? O5 Er1 O1 C1 0.1(3) 4_566 . . . ? Er1 Er1 O1 C1 -159.2(2) 3_666 . . . ? O1 Er1 O5 C17 -164.7(3) . . . . ? O4 Er1 O5 C17 -85.7(3) 3_566 . . . ? O2 Er1 O5 C17 -81.6(2) 4_566 . . . ? O3 Er1 O5 C17 84.6(3) 1_655 . . . ? O6 Er1 O5 C17 134.4(2) 2_655 . . . ? O6 Er1 O5 C17 35.9(3) 4_566 . . . ? O5 Er1 O5 C17 -4.4(3) 4_566 . . . ? C17 Er1 O5 C17 13.1(2) 4_566 . . . ? Er1 Er1 O5 C17 80.6(3) 3_666 . . . ? O1 Er1 O5 Er1 -5.46(11) . . . 4_565 ? O4 Er1 O5 Er1 73.5(2) 3_566 . . 4_565 ? O2 Er1 O5 Er1 77.55(12) 4_566 . . 4_565 ? O3 Er1 O5 Er1 -116.22(14) 1_655 . . 4_565 ? O6 Er1 O5 Er1 -66.38(16) 2_655 . . 4_565 ? O6 Er1 O5 Er1 -164.88(9) 4_566 . . 4_565 ? O5 Er1 O5 Er1 154.76(9) 4_566 . . 4_565 ? C17 Er1 O5 Er1 172.34(11) 4_566 . . 4_565 ? Er1 Er1 O5 Er1 -120.25(10) 3_666 . . 4_565 ? Er1 O2 C1 O1 20.0(4) 4_565 . . . ? Er1 O2 C1 C2 -158.55(19) 4_565 . . . ? Er1 O1 C1 O2 -83.7(3) . . . . ? Er1 O1 C1 C2 94.8(3) . . . . ? O2 C1 C2 C7 -177.7(2) . . . . ? O1 C1 C2 C7 3.6(4) . . . . ? O2 C1 C2 C3 7.2(4) . . . . ? O1 C1 C2 C3 -171.5(2) . . . . ? C7 C2 C3 C4 -2.3(4) . . . . ? C1 C2 C3 C4 173.0(3) . . . . ? C2 C3 C4 C5 0.3(4) . . . . ? C3 C4 C5 C6 2.5(4) . . . . ? C3 C4 C5 C8 -176.2(3) . . . . ? C4 C5 C6 C7 -3.5(4) . . . . ? C8 C5 C6 C7 175.3(3) . . . . ? C5 C6 C7 C2 1.5(4) . . . . ? C3 C2 C7 C6 1.4(4) . . . . ? C1 C2 C7 C6 -173.8(3) . . . . ? C6 C5 C8 C9 -172.4(3) . . . . ? C4 C5 C8 C9 6.3(5) . . . . ? C5 C8 C9 C10 -179.9(3) . . . . ? C8 C9 C10 C15 -6.7(5) . . . . ? C8 C9 C10 C11 171.7(3) . . . . ? C15 C10 C11 C12 0.7(5) . . . . ? C9 C10 C11 C12 -177.7(3) . . . . ? C10 C11 C12 C13 0.1(5) . . . . ? C11 C12 C13 C14 -0.4(5) . . . . ? C11 C12 C13 C16 -179.7(3) . . . . ? C12 C13 C14 C15 -0.2(4) . . . . ? C16 C13 C14 C15 179.1(3) . . . . ? C13 C14 C15 C10 1.2(5) . . . . ? C11 C10 C15 C14 -1.4(5) . . . . ? C9 C10 C15 C14 177.1(3) . . . . ? Er1 O4 C16 O3 12.5(5) 3_566 . . . ? Er1 O4 C16 C13 -167.2(2) 3_566 . . . ? Er1 O3 C16 O4 -4.5(5) 1_455 . . . ? Er1 O3 C16 C13 175.1(2) 1_455 . . . ? C12 C13 C16 O4 -177.1(3) . . . . ? C14 C13 C16 O4 3.5(4) . . . . ? C12 C13 C16 O3 3.2(4) . . . . ? C14 C13 C16 O3 -176.1(3) . . . . ? Er1 O6 C17 O5 -167.4(4) 2_645 . . . ? Er1 O6 C17 O5 -2.4(3) 4_565 . . . ? Er1 O6 C17 Er1 -164.9(6) 2_645 . . 4_565 ? Er1 O5 C17 O6 168.0(2) . . . . ? Er1 O5 C17 O6 2.4(3) 4_565 . . . ? Er1 O5 C17 Er1 165.6(2) . . . 4_565 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.657 _refine_diff_density_min -1.039 _refine_diff_density_rms 0.143 #===END data_complex6 _database_code_depnum_ccdc_archive 'CCDC 716188' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H11 Eu O6' _chemical_formula_sum 'C17 H11 Eu O6' _chemical_formula_weight 463.22 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' Eu Eu -0.1578 3.6682 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 16.1997(11) _cell_length_b 12.1675(6) _cell_length_c 7.4866(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.014(2) _cell_angle_gamma 90.00 _cell_volume 1448.50(14) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 12680 _cell_measurement_theta_min 3.07 _cell_measurement_theta_max 25.00 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.124 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 4.362 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.381 _exptl_absorpt_correction_T_max 0.539 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 13680 _diffrn_reflns_av_R_equivalents 0.0720 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2552 _reflns_number_gt 2258 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.1605P)^2^+5.0215P] 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 2552 _refine_ls_number_parameters 218 _refine_ls_number_restraints 138 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0578 _refine_ls_wR_factor_ref 0.1949 _refine_ls_wR_factor_gt 0.1932 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.036 _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 Eu1 Eu 0.51472(3) 0.67382(3) 0.44102(6) 0.0119(3) Uani 1 1 d . . . O1 O 0.5905(5) 0.6714(4) 0.1899(12) 0.0192(18) Uani 1 1 d U . . O2 O 0.6568(5) 0.8086(6) 0.0789(12) 0.0294(18) Uani 1 1 d U . . O3 O 0.3867(4) 0.7540(6) 0.4839(9) 0.0278(15) Uani 1 1 d U . . O4 O 0.4178(4) 0.8854(5) 0.6882(8) 0.0219(13) Uani 1 1 d U . . O5 O 0.5040(5) 0.8470(6) 0.2718(11) 0.0283(16) Uani 1 1 d U . . O6 O 0.4455(4) 0.9793(4) 0.1042(8) 0.0170(13) Uani 1 1 d U . . C1 C 0.6592(5) 0.7180(7) 0.1610(12) 0.0198(18) Uani 1 1 d U . . C2 C 0.7440(7) 0.6680(6) 0.2330(16) 0.018(2) Uani 1 1 d U . . C3 C 0.8157(5) 0.7221(7) 0.2009(13) 0.0216(19) Uani 1 1 d U . . H3 H 0.8104 0.7867 0.1333 0.026 Uiso 1 1 calc R . . C4 C 0.8958(8) 0.6793(7) 0.2705(18) 0.025(3) Uani 1 1 d U . . H4 H 0.9434 0.7159 0.2493 0.030 Uiso 1 1 calc R . . C5 C 0.9045(6) 0.5829(8) 0.3707(12) 0.0224(18) Uani 1 1 d U . . C6 C 0.8315(6) 0.5264(7) 0.3973(14) 0.025(2) Uani 1 1 d U . . H6 H 0.8363 0.4604 0.4614 0.030 Uiso 1 1 calc R . . C7 C 0.7528(6) 0.5694(7) 0.3278(13) 0.022(2) Uani 1 1 d U . . H7 H 0.7050 0.5316 0.3450 0.027 Uiso 1 1 calc R . . C8 C 0.9897(6) 0.5448(8) 0.4484(14) 0.026(2) Uani 1 1 d U . . H8 H 1.0339 0.5872 0.4238 0.031 Uiso 1 1 calc R . . C9 C 0.3659(7) 0.8312(7) 0.5788(16) 0.020(2) Uani 1 1 d U . . C10 C 0.2758(6) 0.8631(8) 0.5508(12) 0.0197(17) Uani 1 1 d U . . C11 C 0.2512(6) 0.9547(8) 0.6348(14) 0.026(2) Uani 1 1 d U . . H11 H 0.2918 0.9971 0.7085 0.031 Uiso 1 1 calc R . . C12 C 0.1677(8) 0.9850(9) 0.6124(17) 0.038(3) Uani 1 1 d U . . H12 H 0.1533 1.0480 0.6699 0.045 Uiso 1 1 calc R . . C13 C 0.1052(6) 0.9237(7) 0.5063(13) 0.0248(19) Uani 1 1 d U . . C14 C 0.1301(8) 0.8292(7) 0.4174(19) 0.028(3) Uani 1 1 d U . . H14 H 0.0899 0.7880 0.3403 0.033 Uiso 1 1 calc R . . C15 C 0.2131(6) 0.7990(9) 0.4452(15) 0.0238(19) Uani 1 1 d U . . H15 H 0.2281 0.7345 0.3928 0.029 Uiso 1 1 calc R . . C16 C 0.0161(6) 0.9540(9) 0.4744(14) 0.028(2) Uani 1 1 d U . . H16 H -0.0217 0.9034 0.4118 0.034 Uiso 1 1 calc R . . C17 C 0.4645(6) 0.9314(7) 0.2607(13) 0.0239(19) Uani 1 1 d U . . H17 H 0.4481 0.9614 0.3626 0.029 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 Eu1 0.0147(4) 0.0099(4) 0.0110(4) 0.00036(11) 0.0021(2) 0.00032(11) O1 0.019(4) 0.011(3) 0.026(4) 0.001(2) 0.000(3) -0.0041(18) O2 0.026(4) 0.035(3) 0.028(4) 0.014(3) 0.007(3) 0.005(3) O3 0.022(3) 0.031(3) 0.030(4) -0.005(3) 0.004(3) 0.006(3) O4 0.018(3) 0.025(3) 0.022(3) 0.002(3) 0.001(2) -0.001(2) O5 0.025(4) 0.036(2) 0.028(4) 0.011(3) 0.004(3) 0.005(3) O6 0.024(3) 0.015(3) 0.011(3) 0.002(2) 0.003(3) 0.002(2) C1 0.014(4) 0.021(4) 0.024(4) -0.005(4) 0.004(3) 0.003(3) C2 0.014(5) 0.019(5) 0.021(5) -0.003(3) 0.004(4) 0.001(3) C3 0.016(4) 0.024(4) 0.026(4) 0.006(4) 0.006(3) 0.002(3) C4 0.023(5) 0.026(5) 0.026(6) 0.002(3) 0.004(4) -0.003(3) C5 0.021(4) 0.028(4) 0.019(4) 0.001(3) 0.007(3) 0.005(3) C6 0.025(4) 0.019(4) 0.028(5) 0.006(3) 0.000(4) 0.006(3) C7 0.021(4) 0.022(4) 0.025(4) 0.004(4) 0.004(3) 0.007(3) C8 0.020(4) 0.025(4) 0.032(5) 0.003(4) 0.003(3) 0.006(3) C9 0.018(5) 0.031(5) 0.015(5) 0.007(3) 0.011(4) 0.006(3) C10 0.021(4) 0.021(4) 0.019(4) 0.001(4) 0.009(3) 0.000(4) C11 0.025(4) 0.022(4) 0.029(5) 0.001(4) 0.001(4) 0.001(4) C12 0.038(5) 0.031(5) 0.044(6) -0.010(4) 0.007(5) 0.011(4) C13 0.020(4) 0.025(4) 0.030(5) 0.003(4) 0.005(4) 0.006(3) C14 0.022(5) 0.026(5) 0.034(6) -0.008(3) 0.003(5) 0.000(3) C15 0.020(4) 0.021(4) 0.031(5) 0.005(4) 0.007(4) 0.003(4) C16 0.025(5) 0.030(4) 0.030(4) 0.003(4) 0.008(4) 0.004(3) C17 0.030(4) 0.024(4) 0.020(4) -0.002(3) 0.009(4) -0.008(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 Eu1 O4 2.330(6) 4_575 ? Eu1 O2 2.346(8) 4_576 ? Eu1 O3 2.369(6) . ? Eu1 O1 2.434(8) . ? Eu1 O5 2.447(7) . ? Eu1 O6 2.493(5) 2_645 ? Eu1 O5 2.528(8) 4_576 ? Eu1 O6 2.598(6) 4_576 ? Eu1 O1 2.766(7) 4_576 ? Eu1 C1 2.907(9) 4_576 ? Eu1 C17 2.961(9) 4_576 ? Eu1 C9 3.266(12) 4_575 ? O1 C1 1.303(12) . ? O1 Eu1 2.766(7) 4_575 ? O2 C1 1.259(11) . ? O2 Eu1 2.346(8) 4_575 ? O3 C9 1.261(12) . ? O4 C9 1.245(14) . ? O4 Eu1 2.330(6) 4_576 ? O5 C17 1.204(12) . ? O5 Eu1 2.528(8) 4_575 ? O6 C17 1.292(11) . ? O6 Eu1 2.493(5) 2_655 ? O6 Eu1 2.598(6) 4_575 ? C1 C2 1.505(13) . ? C1 Eu1 2.907(9) 4_575 ? C2 C7 1.387(13) . ? C2 C3 1.396(13) . ? C3 C4 1.403(15) . ? C3 H3 0.9300 . ? C4 C5 1.385(14) . ? C4 H4 0.9300 . ? C5 C6 1.415(13) . ? C5 C8 1.466(13) . ? C6 C7 1.384(13) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C8 1.34(2) 3_766 ? C8 H8 0.9300 . ? C9 C10 1.486(14) . ? C9 Eu1 3.266(12) 4_576 ? C10 C11 1.375(13) . ? C10 C15 1.400(15) . ? C11 C12 1.381(16) . ? C11 H11 0.9300 . ? C12 C13 1.381(16) . ? C12 H12 0.9300 . ? C13 C14 1.424(13) . ? C13 C16 1.464(13) . ? C14 C15 1.372(16) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C16 1.32(2) 3_576 ? C16 H16 0.9300 . ? C17 Eu1 2.961(9) 4_575 ? C17 H17 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 Eu1 O2 146.9(2) 4_575 4_576 ? O4 Eu1 O3 76.5(2) 4_575 . ? O2 Eu1 O3 135.5(2) 4_576 . ? O4 Eu1 O1 74.3(2) 4_575 . ? O2 Eu1 O1 75.2(3) 4_576 . ? O3 Eu1 O1 133.9(2) . . ? O4 Eu1 O5 82.9(3) 4_575 . ? O2 Eu1 O5 96.7(3) 4_576 . ? O3 Eu1 O5 74.8(2) . . ? O1 Eu1 O5 66.9(2) . . ? O4 Eu1 O6 75.4(2) 4_575 2_645 ? O2 Eu1 O6 83.6(2) 4_576 2_645 ? O3 Eu1 O6 131.7(2) . 2_645 ? O1 Eu1 O6 72.66(18) . 2_645 ? O5 Eu1 O6 137.9(2) . 2_645 ? O4 Eu1 O5 127.1(2) 4_575 4_576 ? O2 Eu1 O5 79.8(3) 4_576 4_576 ? O3 Eu1 O5 71.5(2) . 4_576 ? O1 Eu1 O5 153.5(3) . 4_576 ? O5 Eu1 O5 125.58(19) . 4_576 ? O6 Eu1 O5 96.1(2) 2_645 4_576 ? O4 Eu1 O6 82.9(2) 4_575 4_576 ? O2 Eu1 O6 109.5(3) 4_576 4_576 ? O3 Eu1 O6 76.3(2) . 4_576 ? O1 Eu1 O6 132.96(17) . 4_576 ? O5 Eu1 O6 150.1(2) . 4_576 ? O6 Eu1 O6 61.9(2) 2_645 4_576 ? O5 Eu1 O6 49.5(2) 4_576 4_576 ? O4 Eu1 O1 154.3(2) 4_575 4_576 ? O2 Eu1 O1 50.9(2) 4_576 4_576 ? O3 Eu1 O1 85.2(2) . 4_576 ? O1 Eu1 O1 107.7(2) . 4_576 ? O5 Eu1 O1 75.0(2) . 4_576 ? O6 Eu1 O1 130.1(2) 2_645 4_576 ? O5 Eu1 O1 60.9(2) 4_576 4_576 ? O6 Eu1 O1 110.3(2) 4_576 4_576 ? O4 Eu1 C1 160.9(2) 4_575 4_576 ? O2 Eu1 C1 24.9(2) 4_576 4_576 ? O3 Eu1 C1 111.6(2) . 4_576 ? O1 Eu1 C1 88.4(2) . 4_576 ? O5 Eu1 C1 82.7(3) . 4_576 ? O6 Eu1 C1 107.8(2) 2_645 4_576 ? O5 Eu1 C1 71.9(2) 4_576 4_576 ? O6 Eu1 C1 115.6(2) 4_576 4_576 ? O1 Eu1 C1 26.4(2) 4_576 4_576 ? O4 Eu1 C17 106.0(2) 4_575 4_576 ? O2 Eu1 C17 94.7(3) 4_576 4_576 ? O3 Eu1 C17 71.7(2) . 4_576 ? O1 Eu1 C17 151.1(2) . 4_576 ? O5 Eu1 C17 141.9(2) . 4_576 ? O6 Eu1 C17 79.5(2) 2_645 4_576 ? O5 Eu1 C17 23.7(2) 4_576 4_576 ? O6 Eu1 C17 25.8(2) 4_576 4_576 ? O1 Eu1 C17 84.5(2) 4_576 4_576 ? C1 Eu1 C17 93.1(3) 4_576 4_576 ? O4 Eu1 C9 17.1(2) 4_575 4_575 ? O2 Eu1 C9 150.9(3) 4_576 4_575 ? O3 Eu1 C9 66.0(2) . 4_575 ? O1 Eu1 C9 76.1(3) . 4_575 ? O5 Eu1 C9 67.6(3) . 4_575 ? O6 Eu1 C9 92.2(2) 2_645 4_575 ? O5 Eu1 C9 129.3(3) 4_576 4_575 ? O6 Eu1 C9 93.5(2) 4_576 4_575 ? O1 Eu1 C9 137.2(2) 4_576 4_575 ? C1 Eu1 C9 149.9(2) 4_576 4_575 ? C17 Eu1 C9 112.9(3) 4_576 4_575 ? C1 O1 Eu1 134.1(6) . . ? C1 O1 Eu1 82.8(5) . 4_575 ? Eu1 O1 Eu1 106.7(3) . 4_575 ? C1 O2 Eu1 103.3(6) . 4_575 ? C9 O3 Eu1 135.9(7) . . ? C9 O4 Eu1 129.5(6) . 4_576 ? C17 O5 Eu1 139.0(7) . . ? C17 O5 Eu1 98.8(6) . 4_575 ? Eu1 O5 Eu1 114.2(3) . 4_575 ? C17 O6 Eu1 121.9(5) . 2_655 ? C17 O6 Eu1 93.0(5) . 4_575 ? Eu1 O6 Eu1 118.1(2) 2_655 4_575 ? O2 C1 O1 121.0(8) . . ? O2 C1 C2 118.0(8) . . ? O1 C1 C2 121.0(8) . . ? O2 C1 Eu1 51.8(5) . 4_575 ? O1 C1 Eu1 70.8(5) . 4_575 ? C2 C1 Eu1 165.2(7) . 4_575 ? C7 C2 C3 119.2(9) . . ? C7 C2 C1 122.1(9) . . ? C3 C2 C1 118.7(8) . . ? C2 C3 C4 120.1(9) . . ? C2 C3 H3 119.9 . . ? C4 C3 H3 119.9 . . ? C5 C4 C3 120.4(10) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C4 C5 C6 119.1(9) . . ? C4 C5 C8 118.2(9) . . ? C6 C5 C8 122.6(8) . . ? C7 C6 C5 119.8(8) . . ? C7 C6 H6 120.1 . . ? C5 C6 H6 120.1 . . ? C6 C7 C2 121.2(9) . . ? C6 C7 H7 119.4 . . ? C2 C7 H7 119.4 . . ? C8 C8 C5 126.7(12) 3_766 . ? C8 C8 H8 116.7 3_766 . ? C5 C8 H8 116.7 . . ? O4 C9 O3 123.1(10) . . ? O4 C9 C10 118.4(8) . . ? O3 C9 C10 118.4(10) . . ? O3 C9 Eu1 102.7(7) . 4_576 ? C10 C9 Eu1 132.1(7) . 4_576 ? C11 C10 C15 117.9(9) . . ? C11 C10 C9 120.7(9) . . ? C15 C10 C9 121.4(9) . . ? C10 C11 C12 121.6(10) . . ? C10 C11 H11 119.2 . . ? C12 C11 H11 119.2 . . ? C13 C12 C11 121.3(9) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C14 117.6(9) . . ? C12 C13 C16 123.3(9) . . ? C14 C13 C16 119.1(10) . . ? C15 C14 C13 120.2(11) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C10 121.4(10) . . ? C14 C15 H15 119.3 . . ? C10 C15 H15 119.3 . . ? C16 C16 C13 126.7(13) 3_576 . ? C16 C16 H16 116.6 3_576 . ? C13 C16 H16 116.6 . . ? O5 C17 O6 118.7(9) . . ? O5 C17 Eu1 57.5(5) . 4_575 ? O6 C17 Eu1 61.2(4) . 4_575 ? O5 C17 H17 120.7 . . ? O6 C17 H17 120.7 . . ? Eu1 C17 H17 177.5 4_575 . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 Eu1 O1 C1 160.4(8) 4_575 . . . ? O2 Eu1 O1 C1 -32.5(8) 4_576 . . . ? O3 Eu1 O1 C1 107.8(8) . . . . ? O5 Eu1 O1 C1 71.6(8) . . . . ? O6 Eu1 O1 C1 -120.3(8) 2_645 . . . ? O5 Eu1 O1 C1 -52.5(9) 4_576 . . . ? O6 Eu1 O1 C1 -135.5(7) 4_576 . . . ? O1 Eu1 O1 C1 7.2(8) 4_576 . . . ? C1 Eu1 O1 C1 -11.1(8) 4_576 . . . ? C17 Eu1 O1 C1 -104.7(8) 4_576 . . . ? C9 Eu1 O1 C1 142.8(8) 4_575 . . . ? O4 Eu1 O1 Eu1 64.1(3) 4_575 . . 4_575 ? O2 Eu1 O1 Eu1 -128.8(3) 4_576 . . 4_575 ? O3 Eu1 O1 Eu1 11.5(4) . . . 4_575 ? O5 Eu1 O1 Eu1 -24.7(3) . . . 4_575 ? O6 Eu1 O1 Eu1 143.4(3) 2_645 . . 4_575 ? O5 Eu1 O1 Eu1 -148.8(4) 4_576 . . 4_575 ? O6 Eu1 O1 Eu1 128.2(2) 4_576 . . 4_575 ? O1 Eu1 O1 Eu1 -89.1(4) 4_576 . . 4_575 ? C1 Eu1 O1 Eu1 -107.4(2) 4_576 . . 4_575 ? C17 Eu1 O1 Eu1 159.0(4) 4_576 . . 4_575 ? C9 Eu1 O1 Eu1 46.5(2) 4_575 . . 4_575 ? O4 Eu1 O3 C9 -162.3(9) 4_575 . . . ? O2 Eu1 O3 C9 7.9(11) 4_576 . . . ? O1 Eu1 O3 C9 -110.4(9) . . . . ? O5 Eu1 O3 C9 -76.1(9) . . . . ? O6 Eu1 O3 C9 141.9(8) 2_645 . . . ? O5 Eu1 O3 C9 60.5(9) 4_576 . . . ? O6 Eu1 O3 C9 111.9(9) 4_576 . . . ? O1 Eu1 O3 C9 -0.4(9) 4_576 . . . ? C1 Eu1 O3 C9 -0.5(10) 4_576 . . . ? C17 Eu1 O3 C9 85.5(9) 4_576 . . . ? C9 Eu1 O3 C9 -147.9(10) 4_575 . . . ? O4 Eu1 O5 C17 93.1(11) 4_575 . . . ? O2 Eu1 O5 C17 -120.3(11) 4_576 . . . ? O3 Eu1 O5 C17 15.2(11) . . . . ? O1 Eu1 O5 C17 169.0(12) . . . . ? O6 Eu1 O5 C17 151.9(10) 2_645 . . . ? O5 Eu1 O5 C17 -38.0(14) 4_576 . . . ? O6 Eu1 O5 C17 31.0(14) 4_576 . . . ? O1 Eu1 O5 C17 -73.8(11) 4_576 . . . ? C1 Eu1 O5 C17 -99.5(11) 4_576 . . . ? C17 Eu1 O5 C17 -13.9(12) 4_576 . . . ? C9 Eu1 O5 C17 85.1(11) 4_575 . . . ? O4 Eu1 O5 Eu1 -47.3(3) 4_575 . . 4_575 ? O2 Eu1 O5 Eu1 99.4(3) 4_576 . . 4_575 ? O3 Eu1 O5 Eu1 -125.2(4) . . . 4_575 ? O1 Eu1 O5 Eu1 28.7(3) . . . 4_575 ? O6 Eu1 O5 Eu1 11.5(5) 2_645 . . 4_575 ? O5 Eu1 O5 Eu1 -178.41(8) 4_576 . . 4_575 ? O6 Eu1 O5 Eu1 -109.3(4) 4_576 . . 4_575 ? O1 Eu1 O5 Eu1 145.9(4) 4_576 . . 4_575 ? C1 Eu1 O5 Eu1 120.1(3) 4_576 . . 4_575 ? C17 Eu1 O5 Eu1 -154.2(3) 4_576 . . 4_575 ? C9 Eu1 O5 Eu1 -55.2(3) 4_575 . . 4_575 ? Eu1 O2 C1 O1 -15.8(11) 4_575 . . . ? Eu1 O2 C1 C2 167.3(7) 4_575 . . . ? Eu1 O1 C1 O2 -93.3(11) . . . . ? Eu1 O1 C1 O2 13.1(9) 4_575 . . . ? Eu1 O1 C1 C2 83.5(10) . . . . ? Eu1 O1 C1 C2 -170.1(8) 4_575 . . . ? Eu1 O1 C1 Eu1 -106.4(6) . . . 4_575 ? O2 C1 C2 C7 178.8(9) . . . . ? O1 C1 C2 C7 1.9(15) . . . . ? Eu1 C1 C2 C7 -138(2) 4_575 . . . ? O2 C1 C2 C3 -1.9(14) . . . . ? O1 C1 C2 C3 -178.9(9) . . . . ? Eu1 C1 C2 C3 41(3) 4_575 . . . ? C7 C2 C3 C4 -2.6(15) . . . . ? C1 C2 C3 C4 178.2(9) . . . . ? C2 C3 C4 C5 0.3(16) . . . . ? C3 C4 C5 C6 1.8(16) . . . . ? C3 C4 C5 C8 -176.8(9) . . . . ? C4 C5 C6 C7 -1.8(14) . . . . ? C8 C5 C6 C7 176.8(9) . . . . ? C5 C6 C7 C2 -0.5(15) . . . . ? C3 C2 C7 C6 2.6(16) . . . . ? C1 C2 C7 C6 -178.2(9) . . . . ? C4 C5 C8 C8 178.6(14) . . . 3_766 ? C6 C5 C8 C8 0(2) . . . 3_766 ? Eu1 O4 C9 O3 -59.3(13) 4_576 . . . ? Eu1 O4 C9 C10 124.4(7) 4_576 . . . ? Eu1 O3 C9 O4 -2.5(15) . . . . ? Eu1 O3 C9 C10 173.8(6) . . . . ? Eu1 O3 C9 Eu1 -31.5(9) . . . 4_576 ? O4 C9 C10 C11 4.2(14) . . . . ? O3 C9 C10 C11 -172.3(9) . . . . ? Eu1 C9 C10 C11 41.9(12) 4_576 . . . ? O4 C9 C10 C15 -173.1(9) . . . . ? O3 C9 C10 C15 10.5(14) . . . . ? Eu1 C9 C10 C15 -135.3(8) 4_576 . . . ? C15 C10 C11 C12 -1.9(15) . . . . ? C9 C10 C11 C12 -179.2(10) . . . . ? C10 C11 C12 C13 0.9(17) . . . . ? C11 C12 C13 C14 -1.4(17) . . . . ? C11 C12 C13 C16 -178.3(10) . . . . ? C12 C13 C14 C15 3.0(17) . . . . ? C16 C13 C14 C15 -179.9(11) . . . . ? C13 C14 C15 C10 -4.2(18) . . . . ? C11 C10 C15 C14 3.6(15) . . . . ? C9 C10 C15 C14 -179.1(11) . . . . ? C12 C13 C16 C16 7(2) . . . 3_576 ? C14 C13 C16 C16 -170.3(14) . . . 3_576 ? Eu1 O5 C17 O6 -145.9(8) . . . . ? Eu1 O5 C17 O6 -2.0(9) 4_575 . . . ? Eu1 O5 C17 Eu1 -143.9(12) . . . 4_575 ? Eu1 O6 C17 O5 -124.1(8) 2_655 . . . ? Eu1 O6 C17 O5 1.9(9) 4_575 . . . ? Eu1 O6 C17 Eu1 -126.0(5) 2_655 . . 4_575 ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.920 _refine_diff_density_max 4.652 _refine_diff_density_min -3.038 _refine_diff_density_rms 0.280 #===END data_complex7 _database_code_depnum_ccdc_archive 'CCDC 716189' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 La O8' _chemical_formula_sum 'C24 H19 La O8' _chemical_formula_weight 574.30 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' La La -0.2871 2.4523 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' 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 19.867(4) _cell_length_b 5.4816(11) _cell_length_c 20.025(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.56(3) _cell_angle_gamma 90.00 _cell_volume 2067.4(8) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 24631 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.845 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1136 _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6767 _exptl_absorpt_correction_T_max 0.9015 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.000 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30183 _diffrn_reflns_av_R_equivalents 0.0459 _diffrn_reflns_av_sigmaI/netI 0.0296 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.44 _reflns_number_total 4699 _reflns_number_gt 4208 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.0207P)^2^+2.2400P] 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 4699 _refine_ls_number_parameters 310 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0564 _refine_ls_wR_factor_gt 0.0546 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 La1 La 0.623433(7) 0.46766(2) 0.122454(7) 0.01780(5) Uani 1 1 d . . . O1W O 0.73765(12) 0.4866(4) 0.23144(14) 0.0442(6) Uani 1 1 d D . . H1W1 H 0.7714(14) 0.466(7) 0.2174(18) 0.066 Uiso 1 1 d D . . H1W2 H 0.7448(19) 0.546(7) 0.2701(11) 0.066 Uiso 1 1 d D . . O2W O 0.56073(11) 0.8451(4) 0.05036(12) 0.0413(5) Uani 1 1 d D . . H2W1 H 0.5822(15) 0.917(7) 0.0270(16) 0.062 Uiso 1 1 d D . . H2W2 H 0.5193(8) 0.814(7) 0.0294(16) 0.062 Uiso 1 1 d D . . O1 O 0.42329(9) 0.6615(4) 0.00592(9) 0.0290(4) Uani 1 1 d . . . O2 O 0.49047(9) 0.4368(4) 0.09575(10) 0.0316(4) Uani 1 1 d . . . O3 O -0.11557(10) 0.6652(4) 0.28961(10) 0.0326(4) Uani 1 1 d . . . O4 O -0.10462(11) 0.2624(3) 0.29359(11) 0.0326(5) Uani 1 1 d . . . O5 O 0.70240(10) 0.1363(4) 0.10945(11) 0.0348(5) Uani 1 1 d . . . O6 O 0.70834(11) -0.2620(4) 0.09376(13) 0.0394(5) Uani 1 1 d . . . C1 C 0.43289(13) 0.5353(5) 0.06199(13) 0.0238(5) Uani 1 1 d . . . C2 C 0.37083(13) 0.5077(5) 0.08889(13) 0.0229(5) Uani 1 1 d . . . C3 C 0.36765(14) 0.3123(6) 0.13168(14) 0.0294(6) Uani 1 1 d . . . H3 H 0.4040 0.1974 0.1438 0.035 Uiso 1 1 calc R . . C4 C 0.31004(14) 0.2883(6) 0.15639(15) 0.0306(6) Uani 1 1 d . . . H4 H 0.3076 0.1539 0.1839 0.037 Uiso 1 1 calc R . . C5 C 0.25582(14) 0.4613(5) 0.14080(14) 0.0274(6) Uani 1 1 d . . . C6 C 0.25994(14) 0.6577(5) 0.09804(14) 0.0298(6) Uani 1 1 d . . . H6 H 0.2243 0.7753 0.0869 0.036 Uiso 1 1 calc R . . C7 C 0.31647(13) 0.6801(5) 0.07182(14) 0.0276(6) Uani 1 1 d . . . H7 H 0.3180 0.8107 0.0427 0.033 Uiso 1 1 calc R . . C8 C 0.19673(15) 0.4260(6) 0.16931(15) 0.0319(6) Uani 1 1 d . . . H8 H 0.2002 0.2927 0.1990 0.038 Uiso 1 1 calc R . . C9 C 0.13922(14) 0.5627(5) 0.15746(15) 0.0301(6) Uani 1 1 d . . . H9 H 0.1351 0.6941 0.1271 0.036 Uiso 1 1 calc R . . C10 C 0.08094(14) 0.5285(5) 0.18738(14) 0.0260(5) Uani 1 1 d . . . C11 C 0.07570(14) 0.3240(5) 0.22747(14) 0.0283(6) Uani 1 1 d . . . H11 H 0.1097 0.2013 0.2354 0.034 Uiso 1 1 calc R . . C12 C 0.02066(13) 0.3025(5) 0.25533(14) 0.0253(5) Uani 1 1 d . . . H12 H 0.0167 0.1626 0.2801 0.030 Uiso 1 1 calc R . . C13 C -0.02880(13) 0.4894(4) 0.24650(13) 0.0205(5) Uani 1 1 d . . . C14 C -0.02420(13) 0.6946(5) 0.20731(13) 0.0242(5) Uani 1 1 d . . . H14 H -0.0571 0.8203 0.2013 0.029 Uiso 1 1 calc R . . C15 C 0.02969(14) 0.7109(5) 0.17716(14) 0.0270(6) Uani 1 1 d . . . H15 H 0.0316 0.8458 0.1497 0.032 Uiso 1 1 calc R . . C16 C -0.08649(13) 0.4714(5) 0.27949(13) 0.0215(5) Uani 1 1 d . . . C17 C 0.73089(13) -0.0481(5) 0.09343(13) 0.0220(5) Uani 1 1 d . . . C18 C 0.79661(13) -0.0142(4) 0.07285(13) 0.0209(5) Uani 1 1 d . . . C19 C 0.83810(14) 0.1932(5) 0.09267(14) 0.0273(5) Uani 1 1 d . . . H19 H 0.8250 0.3147 0.1186 0.033 Uiso 1 1 calc R . . C20 C 0.89918(14) 0.2194(5) 0.07384(15) 0.0288(6) Uani 1 1 d . . . H20 H 0.9274 0.3571 0.0885 0.035 Uiso 1 1 calc R . . C21 C 0.91910(13) 0.0444(5) 0.03355(14) 0.0244(5) Uani 1 1 d . . . C22 C 0.87550(14) -0.1616(5) 0.01204(15) 0.0304(6) Uani 1 1 d . . . H22 H 0.8868 -0.2785 -0.0163 0.036 Uiso 1 1 calc R . . C23 C 0.81602(13) -0.1917(5) 0.03274(14) 0.0270(5) Uani 1 1 d . . . H23 H 0.7886 -0.3320 0.0197 0.032 Uiso 1 1 calc R . . C24 C 0.98484(14) 0.0794(5) 0.01567(15) 0.0288(6) Uani 1 1 d . . . H24 H 1.0075 0.2291 0.0277 0.035 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 La1 0.01447(7) 0.01974(8) 0.02109(8) 0.00102(5) 0.00832(5) 0.00169(5) O1W 0.0333(12) 0.0357(12) 0.0485(14) -0.0061(10) -0.0087(11) -0.0019(9) O2W 0.0276(11) 0.0361(13) 0.0520(13) 0.0151(10) 0.0008(10) -0.0028(9) O1 0.0233(9) 0.0418(12) 0.0246(9) 0.0000(8) 0.0112(8) -0.0008(8) O2 0.0175(9) 0.0448(12) 0.0345(10) 0.0064(9) 0.0112(8) 0.0036(8) O3 0.0363(11) 0.0301(11) 0.0400(11) -0.0034(9) 0.0244(9) 0.0036(8) O4 0.0387(11) 0.0293(11) 0.0379(11) 0.0022(8) 0.0236(9) -0.0051(8) O5 0.0340(11) 0.0285(11) 0.0528(12) -0.0008(9) 0.0293(10) 0.0064(8) O6 0.0350(12) 0.0266(11) 0.0696(15) 0.0004(10) 0.0350(11) -0.0035(8) C1 0.0173(12) 0.0306(14) 0.0246(12) -0.0051(10) 0.0083(10) -0.0025(10) C2 0.0152(11) 0.0314(14) 0.0226(11) -0.0018(10) 0.0066(10) -0.0005(9) C3 0.0212(13) 0.0351(15) 0.0334(14) 0.0077(12) 0.0108(11) 0.0072(11) C4 0.0245(14) 0.0362(15) 0.0323(14) 0.0095(12) 0.0110(12) 0.0019(11) C5 0.0194(12) 0.0395(16) 0.0256(12) -0.0017(11) 0.0104(11) -0.0014(11) C6 0.0219(13) 0.0358(16) 0.0349(14) 0.0034(12) 0.0135(12) 0.0063(11) C7 0.0220(13) 0.0313(15) 0.0321(14) 0.0058(11) 0.0123(11) 0.0028(11) C8 0.0265(14) 0.0411(17) 0.0330(14) 0.0043(12) 0.0164(12) -0.0002(12) C9 0.0252(13) 0.0375(16) 0.0319(14) 0.0027(12) 0.0155(12) -0.0026(11) C10 0.0206(13) 0.0321(14) 0.0273(12) -0.0031(11) 0.0104(11) -0.0023(10) C11 0.0260(13) 0.0260(14) 0.0360(14) 0.0009(11) 0.0141(12) 0.0049(11) C12 0.0253(13) 0.0227(12) 0.0306(13) 0.0036(11) 0.0128(11) 0.0019(10) C13 0.0174(11) 0.0237(13) 0.0223(11) -0.0021(9) 0.0088(10) -0.0032(9) C14 0.0217(12) 0.0246(13) 0.0287(13) 0.0028(11) 0.0115(11) 0.0024(10) C15 0.0259(13) 0.0280(13) 0.0298(13) 0.0065(11) 0.0125(11) -0.0013(11) C16 0.0216(12) 0.0233(13) 0.0197(11) -0.0011(9) 0.0069(10) -0.0032(9) C17 0.0188(12) 0.0260(13) 0.0243(12) 0.0039(10) 0.0114(10) 0.0028(9) C18 0.0180(12) 0.0223(13) 0.0246(12) 0.0026(9) 0.0099(10) 0.0017(9) C19 0.0260(13) 0.0255(13) 0.0350(14) -0.0067(11) 0.0162(12) -0.0013(11) C20 0.0238(13) 0.0295(14) 0.0368(15) -0.0048(12) 0.0147(12) -0.0064(10) C21 0.0197(12) 0.0290(14) 0.0277(13) 0.0030(10) 0.0121(11) 0.0014(10) C22 0.0273(14) 0.0307(16) 0.0394(15) -0.0079(12) 0.0193(12) -0.0018(11) C23 0.0213(13) 0.0257(13) 0.0381(15) -0.0053(12) 0.0151(11) -0.0056(10) C24 0.0218(13) 0.0336(15) 0.0350(14) 0.0005(12) 0.0146(11) -0.0043(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag La1 O4 2.4446(19) 2 ? La1 O6 2.447(2) 1_565 ? La1 O3 2.4596(19) 2_545 ? La1 O5 2.4676(19) . ? La1 O2 2.5285(19) . ? La1 O1 2.5402(19) 3_665 ? La1 O1W 2.602(2) . ? La1 O2W 2.602(2) . ? O1W H1W1 0.81(3) . ? O1W H1W2 0.81(3) . ? O2W H2W1 0.83(3) . ? O2W H2W2 0.82(3) . ? O1 C1 1.281(3) . ? O1 La1 2.5402(19) 3_665 ? O2 C1 1.251(3) . ? O3 C16 1.256(3) . ? O3 La1 2.4596(19) 2 ? O4 C16 1.260(3) . ? O4 La1 2.4446(19) 2_545 ? O5 C17 1.249(3) . ? O6 C17 1.256(3) . ? O6 La1 2.4471(19) 1_545 ? C1 C2 1.502(3) . ? C2 C3 1.386(4) . ? C2 C7 1.393(4) . ? C3 C4 1.390(4) . ? C3 H3 0.9300 . ? C4 C5 1.394(4) . ? C4 H4 0.9300 . ? C5 C6 1.394(4) . ? C5 C8 1.472(4) . ? C6 C7 1.388(4) . ? C6 H6 0.9300 . ? C7 H7 0.9300 . ? C8 C9 1.323(4) . ? C8 H8 0.9300 . ? C9 C10 1.475(4) . ? C9 H9 0.9300 . ? C10 C15 1.395(4) . ? C10 C11 1.402(4) . ? C11 C12 1.382(4) . ? C11 H11 0.9300 . ? C12 C13 1.392(4) . ? C12 H12 0.9300 . ? C13 C14 1.391(4) . ? C13 C16 1.497(3) . ? C14 C15 1.389(3) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C17 C18 1.500(3) . ? C18 C19 1.386(4) . ? C18 C23 1.392(4) . ? C19 C20 1.388(4) . ? C19 H19 0.9300 . ? C20 C21 1.390(4) . ? C20 H20 0.9300 . ? C21 C22 1.405(4) . ? C21 C24 1.472(3) . ? C22 C23 1.381(3) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 C24 1.325(6) 3_755 ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 La1 O6 91.66(7) 2 1_565 ? O4 La1 O3 83.95(7) 2 2_545 ? O6 La1 O3 141.44(7) 1_565 2_545 ? O4 La1 O5 143.19(7) 2 . ? O6 La1 O5 84.96(7) 1_565 . ? O3 La1 O5 76.51(7) 2_545 . ? O4 La1 O2 79.14(7) 2 . ? O6 La1 O2 137.96(7) 1_565 . ? O3 La1 O2 78.82(7) 2_545 . ? O5 La1 O2 125.80(7) . . ? O4 La1 O1 142.52(7) 2 3_665 ? O6 La1 O1 89.33(7) 1_565 3_665 ? O3 La1 O1 116.78(7) 2_545 3_665 ? O5 La1 O1 74.20(7) . 3_665 ? O2 La1 O1 75.33(7) . 3_665 ? O4 La1 O1W 71.35(8) 2 . ? O6 La1 O1W 71.98(8) 1_565 . ? O3 La1 O1W 70.33(8) 2_545 . ? O5 La1 O1W 72.77(8) . . ? O2 La1 O1W 138.90(8) . . ? O1 La1 O1W 143.14(8) 3_665 . ? O4 La1 O2W 72.85(7) 2 . ? O6 La1 O2W 68.43(7) 1_565 . ? O3 La1 O2W 143.60(7) 2_545 . ? O5 La1 O2W 137.30(7) . . ? O2 La1 O2W 69.66(7) . . ? O1 La1 O2W 72.78(7) 3_665 . ? O1W La1 O2W 124.71(7) . . ? La1 O1W H1W1 107(3) . . ? La1 O1W H1W2 131(3) . . ? H1W1 O1W H1W2 118(2) . . ? La1 O2W H2W1 117(3) . . ? La1 O2W H2W2 110(3) . . ? H2W1 O2W H2W2 115.3(19) . . ? C1 O1 La1 129.87(17) . 3_665 ? C1 O2 La1 143.08(18) . . ? C16 O3 La1 145.37(17) . 2 ? C16 O4 La1 150.75(17) . 2_545 ? C17 O5 La1 167.97(19) . . ? C17 O6 La1 147.17(17) . 1_545 ? O2 C1 O1 124.2(2) . . ? O2 C1 C2 118.5(2) . . ? O1 C1 C2 117.3(2) . . ? C3 C2 C7 119.4(2) . . ? C3 C2 C1 120.2(2) . . ? C7 C2 C1 120.3(2) . . ? C2 C3 C4 119.9(3) . . ? C2 C3 H3 120.1 . . ? C4 C3 H3 120.1 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 118.1(2) . . ? C6 C5 C8 123.3(3) . . ? C4 C5 C8 118.6(3) . . ? C7 C6 C5 120.9(2) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C7 C2 120.3(3) . . ? C6 C7 H7 119.9 . . ? C2 C7 H7 119.9 . . ? C9 C8 C5 127.3(3) . . ? C9 C8 H8 116.4 . . ? C5 C8 H8 116.4 . . ? C8 C9 C10 126.9(3) . . ? C8 C9 H9 116.6 . . ? C10 C9 H9 116.6 . . ? C15 C10 C11 118.2(2) . . ? C15 C10 C9 118.7(2) . . ? C11 C10 C9 123.0(2) . . ? C12 C11 C10 120.8(2) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 120.2(2) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C14 C13 C12 119.8(2) . . ? C14 C13 C16 120.0(2) . . ? C12 C13 C16 120.3(2) . . ? C15 C14 C13 119.7(2) . . ? C15 C14 H14 120.2 . . ? C13 C14 H14 120.2 . . ? C14 C15 C10 121.2(2) . . ? C14 C15 H15 119.4 . . ? C10 C15 H15 119.4 . . ? O3 C16 O4 123.6(2) . . ? O3 C16 C13 118.1(2) . . ? O4 C16 C13 118.2(2) . . ? O5 C17 O6 124.2(2) . . ? O5 C17 C18 118.4(2) . . ? O6 C17 C18 117.4(2) . . ? C19 C18 C23 119.3(2) . . ? C19 C18 C17 120.9(2) . . ? C23 C18 C17 119.8(2) . . ? C18 C19 C20 119.9(2) . . ? C18 C19 H19 120.0 . . ? C20 C19 H19 120.0 . . ? C19 C20 C21 121.4(3) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C20 C21 C22 118.1(2) . . ? C20 C21 C24 119.3(2) . . ? C22 C21 C24 122.6(2) . . ? C23 C22 C21 120.5(3) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C22 C23 C18 120.7(3) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C24 C24 C21 127.0(3) 3_755 . ? C24 C24 H24 116.5 3_755 . ? C21 C24 H24 116.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 La1 O2 C1 82.6(3) 2 . . . ? O6 La1 O2 C1 2.3(3) 1_565 . . . ? O3 La1 O2 C1 168.5(3) 2_545 . . . ? O5 La1 O2 C1 -127.4(3) . . . . ? O1 La1 O2 C1 -69.8(3) 3_665 . . . ? O1W La1 O2 C1 126.9(3) . . . . ? O2W La1 O2 C1 7.0(3) . . . . ? O4 La1 O5 C17 151.0(8) 2 . . . ? O6 La1 O5 C17 -123.0(9) 1_565 . . . ? O3 La1 O5 C17 91.1(9) 2_545 . . . ? O2 La1 O5 C17 25.9(9) . . . . ? O1 La1 O5 C17 -32.2(8) 3_665 . . . ? O1W La1 O5 C17 164.4(9) . . . . ? O2W La1 O5 C17 -72.7(9) . . . . ? La1 O2 C1 O1 26.0(5) . . . . ? La1 O2 C1 C2 -153.2(2) . . . . ? La1 O1 C1 O2 93.9(3) 3_665 . . . ? La1 O1 C1 C2 -87.0(3) 3_665 . . . ? O2 C1 C2 C3 -24.0(4) . . . . ? O1 C1 C2 C3 156.8(3) . . . . ? O2 C1 C2 C7 155.2(3) . . . . ? O1 C1 C2 C7 -24.0(4) . . . . ? C7 C2 C3 C4 0.8(4) . . . . ? C1 C2 C3 C4 180.0(3) . . . . ? C2 C3 C4 C5 -1.9(4) . . . . ? C3 C4 C5 C6 1.5(4) . . . . ? C3 C4 C5 C8 -179.4(3) . . . . ? C4 C5 C6 C7 0.0(4) . . . . ? C8 C5 C6 C7 -179.1(3) . . . . ? C5 C6 C7 C2 -1.1(4) . . . . ? C3 C2 C7 C6 0.7(4) . . . . ? C1 C2 C7 C6 -178.5(2) . . . . ? C6 C5 C8 C9 2.7(5) . . . . ? C4 C5 C8 C9 -176.3(3) . . . . ? C5 C8 C9 C10 -178.7(3) . . . . ? C8 C9 C10 C15 170.7(3) . . . . ? C8 C9 C10 C11 -7.4(5) . . . . ? C15 C10 C11 C12 0.8(4) . . . . ? C9 C10 C11 C12 178.9(3) . . . . ? C10 C11 C12 C13 -2.8(4) . . . . ? C11 C12 C13 C14 2.3(4) . . . . ? C11 C12 C13 C16 -177.2(2) . . . . ? C12 C13 C14 C15 0.1(4) . . . . ? C16 C13 C14 C15 179.6(2) . . . . ? C13 C14 C15 C10 -2.2(4) . . . . ? C11 C10 C15 C14 1.7(4) . . . . ? C9 C10 C15 C14 -176.5(2) . . . . ? La1 O3 C16 O4 78.9(4) 2 . . . ? La1 O3 C16 C13 -103.3(3) 2 . . . ? La1 O4 C16 O3 -58.2(5) 2_545 . . . ? La1 O4 C16 C13 124.0(3) 2_545 . . . ? C14 C13 C16 O3 -21.3(3) . . . . ? C12 C13 C16 O3 158.2(2) . . . . ? C14 C13 C16 O4 156.6(2) . . . . ? C12 C13 C16 O4 -23.9(4) . . . . ? La1 O5 C17 O6 -53.3(10) . . . . ? La1 O5 C17 C18 127.2(8) . . . . ? La1 O6 C17 O5 -6.4(5) 1_545 . . . ? La1 O6 C17 C18 173.1(2) 1_545 . . . ? O5 C17 C18 C19 21.1(4) . . . . ? O6 C17 C18 C19 -158.4(3) . . . . ? O5 C17 C18 C23 -158.2(3) . . . . ? O6 C17 C18 C23 22.2(4) . . . . ? C23 C18 C19 C20 -1.5(4) . . . . ? C17 C18 C19 C20 179.2(2) . . . . ? C18 C19 C20 C21 1.8(4) . . . . ? C19 C20 C21 C22 0.1(4) . . . . ? C19 C20 C21 C24 -179.3(3) . . . . ? C20 C21 C22 C23 -2.3(4) . . . . ? C24 C21 C22 C23 177.1(3) . . . . ? C21 C22 C23 C18 2.6(4) . . . . ? C19 C18 C23 C22 -0.7(4) . . . . ? C17 C18 C23 C22 178.7(2) . . . . ? C20 C21 C24 C24 172.5(4) . . . 3_755 ? C22 C21 C24 C24 -6.8(5) . . . 3_755 ? 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 O1W H1W1 O3 0.81(3) 2.50(3) 2.942(3) 115(3) 1_655 O1W H1W2 O1W 0.81(3) 2.44(4) 2.841(3) 111(3) 2_655 O2W H2W1 O1 0.83(3) 2.40(3) 2.986(3) 129(4) 3_675 O2W H2W2 O1 0.82(3) 2.00(2) 2.777(3) 160(3) . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.789 _refine_diff_density_min -0.668 _refine_diff_density_rms 0.087 #===END data_complex8 _database_code_depnum_ccdc_archive 'CCDC 716190' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 H19 O8 Tb' _chemical_formula_sum 'C24 H19 O8 Tb' _chemical_formula_weight 594.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Tb Tb -0.1723 4.1537 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.4342(15) _cell_length_b 8.7266(17) _cell_length_c 16.572(3) _cell_angle_alpha 82.87(3) _cell_angle_beta 88.85(3) _cell_angle_gamma 71.41(3) _cell_volume 1010.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 9032 _cell_measurement_theta_min 3.12 _cell_measurement_theta_max 27.45 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.952 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 584 _exptl_absorpt_coefficient_mu 3.551 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.538 _exptl_absorpt_correction_T_max 0.659 _exptl_absorpt_process_details 'ABSCOR (Higashi, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(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 'Rigaku RAXIS-RAPID' _diffrn_measurement_method '\w scan' _diffrn_detector_area_resol_mean 10 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9921 _diffrn_reflns_av_R_equivalents 0.0401 _diffrn_reflns_av_sigmaI/netI 0.0523 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.12 _diffrn_reflns_theta_max 27.46 _reflns_number_total 4586 _reflns_number_gt 4201 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'RAPID-AUTO (Rigaku Corporation, 1998)' _computing_cell_refinement RAPID-AUTO _computing_data_reduction 'CrystalStructure (Rigaku/MSC and Rigaku Corporation, 2002)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP-II (Johnson, 1976)' _computing_publication_material SHELXL-97 _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^)+(0.0455P)^2^+0.7409P] 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 4586 _refine_ls_number_parameters 310 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0902 _refine_ls_wR_factor_gt 0.0744 _refine_ls_goodness_of_fit_ref 1.122 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean <0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Tb1 Tb 0.57430(3) 0.25573(2) 1.016565(11) 0.01774(8) Uani 1 1 d . . . O1W O 0.2297(5) 0.3458(4) 1.0029(2) 0.0300(7) Uani 1 1 d D . . H1W1 H 0.180(7) 0.416(5) 0.963(2) 0.045 Uiso 1 1 d D . . H1W2 H 0.156(6) 0.358(7) 1.043(2) 0.045 Uiso 1 1 d D . . O2W O 0.8153(5) -0.0186(4) 1.0194(3) 0.0372(9) Uani 1 1 d D . . H2W1 H 0.915(6) -0.042(6) 1.049(3) 0.056 Uiso 1 1 d D . . H2W2 H 0.794(8) -0.107(4) 1.013(4) 0.056 Uiso 1 1 d D . . O1 O 0.7883(5) 0.2776(4) 0.9048(2) 0.0283(7) Uani 1 1 d . . . O2 O 0.5459(5) 0.4994(4) 0.91572(19) 0.0260(7) Uani 1 1 d . . . O3 O 0.5228(5) 0.8480(4) 0.08913(19) 0.0279(7) Uani 1 1 d . . . O4 O 0.4745(5) 1.0989(4) 0.1191(2) 0.0266(7) Uani 1 1 d . . . O5 O 0.8249(5) 0.2610(4) 1.08809(19) 0.0283(7) Uani 1 1 d . . . O6 O 0.9615(5) 0.4358(4) 1.1247(2) 0.0310(7) Uani 1 1 d . . . C1 C 0.6782(7) 0.4116(5) 0.8729(3) 0.0219(9) Uani 1 1 d . . . C2 C 0.6851(6) 0.4625(5) 0.7841(3) 0.0217(9) Uani 1 1 d . . . C7 C 0.5625(6) 0.6096(5) 0.7482(3) 0.0223(9) Uani 1 1 d . . . H7 H 0.4827 0.6810 0.7807 0.027 Uiso 1 1 calc R . . C6 C 0.5571(7) 0.6520(5) 0.6645(3) 0.0257(9) Uani 1 1 d . . . H6 H 0.4737 0.7514 0.6417 0.031 Uiso 1 1 calc R . . C5 C 0.6750(7) 0.5475(5) 0.6142(3) 0.0228(9) Uani 1 1 d . . . C4 C 0.8009(7) 0.3998(6) 0.6514(3) 0.0289(10) Uani 1 1 d . . . H4 H 0.8834 0.3290 0.6194 0.035 Uiso 1 1 calc R . . C3 C 0.8041(7) 0.3582(6) 0.7342(3) 0.0289(10) Uani 1 1 d . . . H3 H 0.8871 0.2588 0.7573 0.035 Uiso 1 1 calc R . . C8 C 0.6731(7) 0.5880(6) 0.5254(3) 0.0275(10) Uani 1 1 d . . . H8 H 0.7522 0.5100 0.4958 0.033 Uiso 1 1 calc R . . C9 C 0.5682(7) 0.7263(6) 0.4838(3) 0.0304(11) Uani 1 1 d . . . H9 H 0.4923 0.8034 0.5148 0.036 Uiso 1 1 calc R . . C10 C 0.5556(7) 0.7743(6) 0.3953(3) 0.0252(9) Uani 1 1 d . . . C15 C 0.4378(7) 0.9315(5) 0.3656(3) 0.0250(9) Uani 1 1 d . . . H15 H 0.3681 0.9994 0.4021 0.030 Uiso 1 1 calc R . . C14 C 0.4233(6) 0.9870(5) 0.2839(3) 0.0215(9) Uani 1 1 d . . . H14 H 0.3480 1.0929 0.2658 0.026 Uiso 1 1 calc R . . C13 C 0.5215(6) 0.8847(5) 0.2278(3) 0.0198(8) Uani 1 1 d . . . C12 C 0.6377(7) 0.7275(5) 0.2564(3) 0.0249(9) Uani 1 1 d . . . H12 H 0.7044 0.6584 0.2198 0.030 Uiso 1 1 calc R . . C11 C 0.6538(7) 0.6747(5) 0.3385(3) 0.0252(9) Uani 1 1 d . . . H11 H 0.7322 0.5700 0.3566 0.030 Uiso 1 1 calc R . . C22 C 0.9926(7) 0.2199(6) 1.3676(3) 0.0265(10) Uani 1 1 d . . . H22 H 1.0330 0.2643 1.4092 0.032 Uiso 1 1 calc R . . C16 C 0.5035(6) 0.9469(5) 0.1395(3) 0.0206(9) Uani 1 1 d . . . C17 C 0.9021(6) 0.3160(5) 1.1403(3) 0.0216(9) Uani 1 1 d . . . C18 C 0.9226(6) 0.2302(5) 1.2253(3) 0.0195(8) Uani 1 1 d . . . C23 C 0.9797(6) 0.2962(5) 1.2888(3) 0.0230(9) Uani 1 1 d . . . H23 H 1.0094 0.3925 1.2780 0.028 Uiso 1 1 calc R . . C21 C 0.9457(6) 0.0764(5) 1.3857(3) 0.0252(9) Uani 1 1 d . . . C20 C 0.8871(6) 0.0134(5) 1.3214(3) 0.0252(9) Uani 1 1 d . . . H20 H 0.8540 -0.0813 1.3320 0.030 Uiso 1 1 calc R . . C19 C 0.8770(6) 0.0885(5) 1.2425(3) 0.0248(9) Uani 1 1 d . . . H19 H 0.8392 0.0432 1.2006 0.030 Uiso 1 1 calc R . . C24 C 0.9585(7) -0.0114(6) 1.4674(3) 0.0314(11) Uani 1 1 d . . . H24 H 0.9018 -0.0929 1.4744 0.038 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 0.02216(12) 0.01802(12) 0.01323(12) 0.00067(8) 0.00004(8) -0.00764(8) O1W 0.0238(17) 0.0365(18) 0.0227(17) 0.0028(15) 0.0016(13) -0.0023(14) O2W 0.0267(19) 0.0253(16) 0.058(3) -0.0029(18) 0.0034(17) -0.0070(14) O1 0.0313(18) 0.0276(16) 0.0212(16) 0.0049(14) -0.0012(13) -0.0053(14) O2 0.0377(19) 0.0226(15) 0.0183(15) -0.0003(13) 0.0072(13) -0.0117(14) O3 0.040(2) 0.0307(17) 0.0162(16) -0.0042(14) -0.0006(13) -0.0155(15) O4 0.0341(19) 0.0214(15) 0.0226(17) 0.0010(14) 0.0062(13) -0.0083(13) O5 0.0348(19) 0.0329(17) 0.0199(16) -0.0013(14) -0.0070(13) -0.0147(15) O6 0.040(2) 0.0364(18) 0.0201(16) 0.0049(15) -0.0012(14) -0.0202(16) C1 0.029(2) 0.0212(19) 0.016(2) -0.0020(18) 0.0001(17) -0.0094(17) C2 0.025(2) 0.021(2) 0.016(2) -0.0007(18) 0.0017(16) -0.0052(17) C7 0.025(2) 0.024(2) 0.017(2) -0.0041(18) 0.0046(17) -0.0068(17) C6 0.027(2) 0.020(2) 0.025(2) 0.0005(19) 0.0005(18) -0.0025(17) C5 0.028(2) 0.028(2) 0.0119(19) 0.0038(18) -0.0005(16) -0.0092(18) C4 0.037(3) 0.024(2) 0.021(2) -0.0008(19) 0.0025(19) -0.0024(19) C3 0.035(3) 0.024(2) 0.023(2) 0.0019(19) -0.0011(19) -0.0040(19) C8 0.037(3) 0.031(2) 0.013(2) -0.0018(19) 0.0064(18) -0.009(2) C9 0.037(3) 0.033(2) 0.017(2) -0.001(2) 0.0063(19) -0.006(2) C10 0.028(2) 0.030(2) 0.015(2) 0.0062(19) -0.0028(17) -0.0095(19) C15 0.029(2) 0.022(2) 0.023(2) -0.0037(19) 0.0028(18) -0.0066(18) C14 0.026(2) 0.0177(19) 0.019(2) 0.0000(17) -0.0008(17) -0.0055(17) C13 0.024(2) 0.022(2) 0.0136(19) 0.0009(17) -0.0009(16) -0.0091(17) C12 0.032(2) 0.020(2) 0.021(2) -0.0038(18) 0.0001(18) -0.0047(18) C11 0.033(3) 0.0171(19) 0.021(2) -0.0015(18) 0.0005(18) -0.0027(18) C22 0.030(2) 0.029(2) 0.024(2) -0.004(2) -0.0035(18) -0.0133(19) C16 0.019(2) 0.027(2) 0.017(2) 0.0021(18) 0.0008(16) -0.0115(17) C17 0.020(2) 0.024(2) 0.019(2) 0.0009(18) 0.0011(16) -0.0061(17) C18 0.017(2) 0.024(2) 0.017(2) 0.0011(17) -0.0013(15) -0.0067(16) C23 0.026(2) 0.021(2) 0.023(2) 0.0029(18) -0.0023(17) -0.0105(17) C21 0.023(2) 0.025(2) 0.025(2) -0.0005(19) 0.0013(17) -0.0053(18) C20 0.025(2) 0.024(2) 0.025(2) 0.0026(19) -0.0014(18) -0.0064(18) C19 0.026(2) 0.024(2) 0.025(2) -0.0007(19) -0.0043(18) -0.0096(18) C24 0.032(3) 0.030(2) 0.026(2) 0.005(2) 0.002(2) -0.006(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 O5 2.243(3) . ? Tb1 O3 2.296(3) 2_666 ? Tb1 O4 2.309(3) 1_546 ? Tb1 O1W 2.435(3) . ? Tb1 O2 2.441(3) 2_667 ? Tb1 O1 2.446(3) . ? Tb1 O2W 2.487(3) . ? Tb1 O2 2.491(3) . ? Tb1 C1 2.813(5) . ? O1W H1W1 0.85(4) . ? O1W H1W2 0.85(4) . ? O2W H2W1 0.85(5) . ? O2W H2W2 0.86(4) . ? O1 C1 1.254(5) . ? O2 C1 1.298(5) . ? O2 Tb1 2.441(3) 2_667 ? O3 C16 1.248(5) . ? O3 Tb1 2.296(3) 2_666 ? O4 C16 1.277(5) . ? O4 Tb1 2.309(3) 1_564 ? O5 C17 1.268(5) . ? O6 C17 1.256(6) . ? C1 C2 1.488(6) . ? C2 C7 1.385(6) . ? C2 C3 1.392(6) . ? C7 C6 1.389(6) . ? C7 H7 0.9300 . ? C6 C5 1.394(6) . ? C6 H6 0.9300 . ? C5 C4 1.405(6) . ? C5 C8 1.470(6) . ? C4 C3 1.374(7) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C8 C9 1.325(7) . ? C8 H8 0.9300 . ? C9 C10 1.472(6) . ? C9 H9 0.9300 . ? C10 C11 1.394(6) . ? C10 C15 1.405(6) . ? C15 C14 1.375(6) . ? C15 H15 0.9300 . ? C14 C13 1.399(6) . ? C14 H14 0.9300 . ? C13 C12 1.397(6) . ? C13 C16 1.489(6) . ? C12 C11 1.377(6) . ? C12 H12 0.9300 . ? C11 H11 0.9300 . ? C22 C23 1.381(6) . ? C22 C21 1.400(7) . ? C22 H22 0.9300 . ? C17 C18 1.498(6) . ? C18 C19 1.379(6) . ? C18 C23 1.394(6) . ? C23 H23 0.9300 . ? C21 C20 1.394(7) . ? C21 C24 1.460(7) . ? C20 C19 1.381(7) . ? C20 H20 0.9300 . ? C19 H19 0.9300 . ? C24 C24 1.321(10) 2_758 ? C24 H24 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O5 Tb1 O3 145.34(12) . 2_666 ? O5 Tb1 O4 94.41(13) . 1_546 ? O3 Tb1 O4 96.13(12) 2_666 1_546 ? O5 Tb1 O1W 146.03(12) . . ? O3 Tb1 O1W 68.60(13) 2_666 . ? O4 Tb1 O1W 74.60(12) 1_546 . ? O5 Tb1 O2 75.62(12) . 2_667 ? O3 Tb1 O2 136.48(12) 2_666 2_667 ? O4 Tb1 O2 92.61(11) 1_546 2_667 ? O1W Tb1 O2 72.96(12) . 2_667 ? O5 Tb1 O1 80.56(12) . . ? O3 Tb1 O1 73.91(12) 2_666 . ? O4 Tb1 O1 150.00(11) 1_546 . ? O1W Tb1 O1 124.38(12) . . ? O2 Tb1 O1 114.30(11) 2_667 . ? O5 Tb1 O2W 73.54(13) . . ? O3 Tb1 O2W 77.07(13) 2_666 . ? O4 Tb1 O2W 76.30(12) 1_546 . ? O1W Tb1 O2W 131.56(13) . . ? O2 Tb1 O2W 146.15(13) 2_667 . ? O1 Tb1 O2W 73.91(12) . . ? O5 Tb1 O2 98.05(12) . . ? O3 Tb1 O2 85.15(11) 2_666 . ? O4 Tb1 O2 156.00(12) 1_546 . ? O1W Tb1 O2 83.71(12) . . ? O2 Tb1 O2 70.94(12) 2_667 . ? O1 Tb1 O2 53.13(11) . . ? O2W Tb1 O2 126.95(12) . . ? O5 Tb1 C1 93.52(13) . . ? O3 Tb1 C1 73.58(12) 2_666 . ? O4 Tb1 C1 169.63(12) 1_546 . ? O1W Tb1 C1 102.15(13) . . ? O2 Tb1 C1 95.84(12) 2_667 . ? O1 Tb1 C1 26.42(12) . . ? O2W Tb1 C1 99.61(13) . . ? O2 Tb1 C1 27.49(11) . . ? O5 Tb1 Tb1 86.32(9) . 2_667 ? O3 Tb1 Tb1 112.85(9) 2_666 2_667 ? O4 Tb1 Tb1 126.45(8) 1_546 2_667 ? O1W Tb1 Tb1 75.75(9) . 2_667 ? O2 Tb1 Tb1 35.88(7) 2_667 2_667 ? O1 Tb1 Tb1 82.99(8) . 2_667 ? O2W Tb1 Tb1 151.35(9) . 2_667 ? O2 Tb1 Tb1 35.06(7) . 2_667 ? C1 Tb1 Tb1 60.77(9) . 2_667 ? Tb1 O1W H1W1 117(4) . . ? Tb1 O1W H1W2 124(4) . . ? H1W1 O1W H1W2 110(5) . . ? Tb1 O2W H2W1 119(4) . . ? Tb1 O2W H2W2 126(4) . . ? H2W1 O2W H2W2 109(5) . . ? C1 O1 Tb1 93.3(3) . . ? C1 O2 Tb1 147.9(3) . 2_667 ? C1 O2 Tb1 90.2(3) . . ? Tb1 O2 Tb1 109.06(12) 2_667 . ? C16 O3 Tb1 154.5(3) . 2_666 ? C16 O4 Tb1 135.8(3) . 1_564 ? C17 O5 Tb1 152.9(3) . . ? O1 C1 O2 119.8(4) . . ? O1 C1 C2 120.3(4) . . ? O2 C1 C2 119.6(4) . . ? O1 C1 Tb1 60.2(2) . . ? O2 C1 Tb1 62.3(2) . . ? C2 C1 Tb1 157.8(3) . . ? C7 C2 C3 118.4(4) . . ? C7 C2 C1 120.6(4) . . ? C3 C2 C1 120.8(4) . . ? C2 C7 C6 121.0(4) . . ? C2 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C6 C5 120.9(4) . . ? C7 C6 H6 119.6 . . ? C5 C6 H6 119.6 . . ? C6 C5 C4 117.6(4) . . ? C6 C5 C8 122.5(4) . . ? C4 C5 C8 119.9(4) . . ? C3 C4 C5 121.1(4) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C9 C8 C5 125.5(4) . . ? C9 C8 H8 117.3 . . ? C5 C8 H8 117.3 . . ? C8 C9 C10 128.6(4) . . ? C8 C9 H9 115.7 . . ? C10 C9 H9 115.7 . . ? C11 C10 C15 117.5(4) . . ? C11 C10 C9 124.5(4) . . ? C15 C10 C9 118.0(4) . . ? C14 C15 C10 121.4(4) . . ? C14 C15 H15 119.3 . . ? C10 C15 H15 119.3 . . ? C15 C14 C13 120.2(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C12 C13 C14 119.0(4) . . ? C12 C13 C16 121.6(4) . . ? C14 C13 C16 119.4(4) . . ? C11 C12 C13 120.1(4) . . ? C11 C12 H12 119.9 . . ? C13 C12 H12 119.9 . . ? C12 C11 C10 121.7(4) . . ? C12 C11 H11 119.1 . . ? C10 C11 H11 119.1 . . ? C23 C22 C21 120.9(4) . . ? C23 C22 H22 119.6 . . ? C21 C22 H22 119.6 . . ? O3 C16 O4 123.2(4) . . ? O3 C16 C13 118.8(4) . . ? O4 C16 C13 118.0(4) . . ? O6 C17 O5 124.1(4) . . ? O6 C17 C18 119.1(4) . . ? O5 C17 C18 116.8(4) . . ? C19 C18 C23 119.0(4) . . ? C19 C18 C17 120.3(4) . . ? C23 C18 C17 120.6(4) . . ? C22 C23 C18 120.5(4) . . ? C22 C23 H23 119.7 . . ? C18 C23 H23 119.7 . . ? C20 C21 C22 117.7(4) . . ? C20 C21 C24 118.7(4) . . ? C22 C21 C24 123.6(4) . . ? C19 C20 C21 121.4(4) . . ? C19 C20 H20 119.3 . . ? C21 C20 H20 119.3 . . ? C18 C19 C20 120.5(4) . . ? C18 C19 H19 119.8 . . ? C20 C19 H19 119.8 . . ? C24 C24 C21 127.4(6) 2_758 . ? C24 C24 H24 116.3 2_758 . ? C21 C24 H24 116.3 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 Tb1 O1 C1 -118.3(3) . . . . ? O3 Tb1 O1 C1 85.4(3) 2_666 . . . ? O4 Tb1 O1 C1 159.3(3) 1_546 . . . ? O1W Tb1 O1 C1 36.5(3) . . . . ? O2 Tb1 O1 C1 -48.9(3) 2_667 . . . ? O2W Tb1 O1 C1 166.2(3) . . . . ? O2 Tb1 O1 C1 -10.7(2) . . . . ? Tb1 Tb1 O1 C1 -30.9(3) 2_667 . . . ? O5 Tb1 O2 C1 82.1(3) . . . . ? O3 Tb1 O2 C1 -63.2(3) 2_666 . . . ? O4 Tb1 O2 C1 -157.3(3) 1_546 . . . ? O1W Tb1 O2 C1 -132.1(3) . . . . ? O2 Tb1 O2 C1 153.8(3) 2_667 . . . ? O1 Tb1 O2 C1 10.3(2) . . . . ? O2W Tb1 O2 C1 6.7(3) . . . . ? Tb1 Tb1 O2 C1 153.8(3) 2_667 . . . ? O5 Tb1 O2 Tb1 -71.69(15) . . . 2_667 ? O3 Tb1 O2 Tb1 143.06(15) 2_666 . . 2_667 ? O4 Tb1 O2 Tb1 48.9(3) 1_546 . . 2_667 ? O1W Tb1 O2 Tb1 74.10(14) . . . 2_667 ? O2 Tb1 O2 Tb1 0.0 2_667 . . 2_667 ? O1 Tb1 O2 Tb1 -143.45(19) . . . 2_667 ? O2W Tb1 O2 Tb1 -147.11(14) . . . 2_667 ? C1 Tb1 O2 Tb1 -153.8(3) . . . 2_667 ? O3 Tb1 O5 C17 170.5(6) 2_666 . . . ? O4 Tb1 O5 C17 -82.0(7) 1_546 . . . ? O1W Tb1 O5 C17 -13.3(8) . . . . ? O2 Tb1 O5 C17 9.5(7) 2_667 . . . ? O1 Tb1 O5 C17 127.8(7) . . . . ? O2W Tb1 O5 C17 -156.3(7) . . . . ? O2 Tb1 O5 C17 77.4(7) . . . . ? C1 Tb1 O5 C17 104.7(7) . . . . ? Tb1 Tb1 O5 C17 44.3(7) 2_667 . . . ? Tb1 O1 C1 O2 19.2(4) . . . . ? Tb1 O1 C1 C2 -154.3(4) . . . . ? Tb1 O2 C1 O1 109.4(6) 2_667 . . . ? Tb1 O2 C1 O1 -18.8(4) . . . . ? Tb1 O2 C1 C2 -77.0(7) 2_667 . . . ? Tb1 O2 C1 C2 154.7(4) . . . . ? Tb1 O2 C1 Tb1 128.3(5) 2_667 . . . ? O5 Tb1 C1 O1 60.5(3) . . . . ? O3 Tb1 C1 O1 -86.8(3) 2_666 . . . ? O4 Tb1 C1 O1 -79.3(7) 1_546 . . . ? O1W Tb1 C1 O1 -149.9(3) . . . . ? O2 Tb1 C1 O1 136.4(3) 2_667 . . . ? O2W Tb1 C1 O1 -13.4(3) . . . . ? O2 Tb1 C1 O1 161.2(4) . . . . ? Tb1 Tb1 C1 O1 144.3(3) 2_667 . . . ? O5 Tb1 C1 O2 -100.7(3) . . . . ? O3 Tb1 C1 O2 112.1(3) 2_666 . . . ? O4 Tb1 C1 O2 119.5(6) 1_546 . . . ? O1W Tb1 C1 O2 49.0(3) . . . . ? O2 Tb1 C1 O2 -24.8(3) 2_667 . . . ? O1 Tb1 C1 O2 -161.2(4) . . . . ? O2W Tb1 C1 O2 -174.6(3) . . . . ? Tb1 Tb1 C1 O2 -16.9(2) 2_667 . . . ? O5 Tb1 C1 C2 158.3(8) . . . . ? O3 Tb1 C1 C2 11.1(8) 2_666 . . . ? O4 Tb1 C1 C2 18.6(13) 1_546 . . . ? O1W Tb1 C1 C2 -52.0(8) . . . . ? O2 Tb1 C1 C2 -125.8(8) 2_667 . . . ? O1 Tb1 C1 C2 97.9(8) . . . . ? O2W Tb1 C1 C2 84.5(8) . . . . ? O2 Tb1 C1 C2 -101.0(9) . . . . ? Tb1 Tb1 C1 C2 -117.9(8) 2_667 . . . ? O1 C1 C2 C7 179.3(4) . . . . ? O2 C1 C2 C7 5.8(7) . . . . ? Tb1 C1 C2 C7 94.5(8) . . . . ? O1 C1 C2 C3 4.3(7) . . . . ? O2 C1 C2 C3 -169.2(4) . . . . ? Tb1 C1 C2 C3 -80.5(9) . . . . ? C3 C2 C7 C6 0.4(7) . . . . ? C1 C2 C7 C6 -174.6(4) . . . . ? C2 C7 C6 C5 0.0(7) . . . . ? C7 C6 C5 C4 -1.0(7) . . . . ? C7 C6 C5 C8 179.9(5) . . . . ? C6 C5 C4 C3 1.6(7) . . . . ? C8 C5 C4 C3 -179.3(5) . . . . ? C5 C4 C3 C2 -1.2(8) . . . . ? C7 C2 C3 C4 0.1(7) . . . . ? C1 C2 C3 C4 175.2(5) . . . . ? C6 C5 C8 C9 2.6(8) . . . . ? C4 C5 C8 C9 -176.5(5) . . . . ? C5 C8 C9 C10 -178.6(5) . . . . ? C8 C9 C10 C11 1.8(9) . . . . ? C8 C9 C10 C15 -177.8(5) . . . . ? C11 C10 C15 C14 -1.6(7) . . . . ? C9 C10 C15 C14 177.9(5) . . . . ? C10 C15 C14 C13 2.3(7) . . . . ? C15 C14 C13 C12 -1.7(7) . . . . ? C15 C14 C13 C16 179.8(4) . . . . ? C14 C13 C12 C11 0.3(7) . . . . ? C16 C13 C12 C11 178.9(4) . . . . ? C13 C12 C11 C10 0.3(8) . . . . ? C15 C10 C11 C12 0.3(7) . . . . ? C9 C10 C11 C12 -179.2(5) . . . . ? Tb1 O3 C16 O4 -61.0(9) 2_666 . . . ? Tb1 O3 C16 C13 121.2(6) 2_666 . . . ? Tb1 O4 C16 O3 -36.1(7) 1_564 . . . ? Tb1 O4 C16 C13 141.8(3) 1_564 . . . ? C12 C13 C16 O3 29.8(6) . . . . ? C14 C13 C16 O3 -151.7(4) . . . . ? C12 C13 C16 O4 -148.2(4) . . . . ? C14 C13 C16 O4 30.3(6) . . . . ? Tb1 O5 C17 O6 -86.6(8) . . . . ? Tb1 O5 C17 C18 93.5(7) . . . . ? O6 C17 C18 C19 -173.3(4) . . . . ? O5 C17 C18 C19 6.7(6) . . . . ? O6 C17 C18 C23 9.6(6) . . . . ? O5 C17 C18 C23 -170.5(4) . . . . ? C21 C22 C23 C18 -1.1(7) . . . . ? C19 C18 C23 C22 0.7(7) . . . . ? C17 C18 C23 C22 177.9(4) . . . . ? C23 C22 C21 C20 0.4(7) . . . . ? C23 C22 C21 C24 179.2(4) . . . . ? C22 C21 C20 C19 0.6(7) . . . . ? C24 C21 C20 C19 -178.2(4) . . . . ? C23 C18 C19 C20 0.3(7) . . . . ? C17 C18 C19 C20 -176.9(4) . . . . ? C21 C20 C19 C18 -0.9(7) . . . . ? C20 C21 C24 C24 167.0(6) . . . 2_758 ? C22 C21 C24 C24 -11.7(10) . . . 2_758 ? 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 O1W H1W1 O6 0.85(4) 1.90(4) 2.742(5) 172(6) 2_667 O1W H1W2 O6 0.85(4) 1.98(4) 2.811(5) 167(5) 1_455 O2W H2W1 O2W 0.85(5) 2.45(6) 2.917(8) 115(5) 2_757 O2W H2W1 O1 0.85(5) 2.54(4) 3.251(5) 141(5) 2_757 O2W H2W2 O1W 0.86(4) 2.19(4) 3.046(5) 174(5) 2_657 O2W H2W2 O3 0.86(4) 2.47(6) 2.932(5) 115(5) 1_546 _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.811 _refine_diff_density_min -1.548 _refine_diff_density_rms 0.165